Proceedings of the Korean Powder Metallurgy Institute Conference (한국분말야금학회:학술대회논문집)
The Korean Powder Metallurgy & Materials Institute
- Semi Annual
Domain
- Materials > Plastic Deformation Process/Powders
2006.09a
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An update and the latest results on molten metal atomization using a Pressure-Gas-Atomizer will be given. This atomizer combines a swirl-pressure atomizer, to generate a liquid hollow cone film and a gas atomizer to atomize the film and/or the fragments of the film. The paper is focused on powder production, but this atomization system is also applicable for deposition purposes. Different alloys (Sn, SnCu) were atomized to study the characteristics of the Pressure-Gas-Atomizer.
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Based on theoretical analysis, a new general equation of mean particle size applicable to both conventional atomization methods and new atomization processes is presented. In gas atomization, it is equivalent with and can be changed into Lubanska Equation. In centrifugal atomization, it can be changed into the equations that are currently the most widely used. In water atomization, it is similar to the equation proposed by Grandzol and Tallmadge. According to the universal equation, new correlations for mean particle size in novel atomization processes such as Hybrid Atomization and Multistage Atomization were proposed and agreed with our experimental data well.
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Hybrid atomization is a new atomization technique that combines gas atomization with centrifugal atomization. This process can produce fine, spherical powders economically with a mean size of about 10 m diameter and a tight size distribution.
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The use of hot gas in melt atomization has been widely reported, but little detailed experimental data on its precise effects and no satisfactory theory to explain them have been published. In this paper the authors present experimental data on the atomization of metals with gas at temperatures from ambient to 1000C, a semi-empirical equation relating particle size to gas temperature and flow rate, and an analysis of the gas dynamics of the atomization process that allows some insight into the process.
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The spherical and high quality Titanium fine powder "Tilop" has been produced with gas atomization furnace, Sumitomo Titanium Corporation originally designed. Recently, a new process which can produce Ti-alloy(Ti-6Al-4V) powders by utilizing our gas atomization process, of which raw material is sponge titanium pre-mixed with alloy chips or granules has been also developed. The particle size of gas atomized Ti-alloy powder and the mechanical properties of sintered Ti-alloy compacts prepared by metal injection molding were discussed in this study.
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In this study, a new laval type nozzle was designed and manufactured. Using this nozzle tin powder was produced in close coupled system by using nitrogen gas at different operating conditions. The results showed that the increasing the gas pressure up to 1.47 MPa reduced the mean powder size down to 11.39 microns with a gas/melt mass flow rate ratio of 2.0. Powders are spherical in shape and have smooth surfaces.
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In order to obtain spherical fine powder, we have developed a new method of high-pressure water atomization system using swirl water jet with the swirl angle
$(\omega)$ . The effect of nozzle apex angle$(\theta)$ upon the morphology of atomized powders was investigated. Molten copper was atomized by this method, with$\omega=0.2$ rad (swirl water jet) and$\omega=0$ rad (conical water jet). It was found that the median diameter$(D_{50})$ of atomized powders decreased with decreasing$(\theta)$ down to 0.35 rad in each$\omega$ , but under${\theta}<\;0.35$ rad,$D_{50}$ increased abruptly with decreasing$\theta$ for$\omega=0$ rad, while it was still decreased with decreasing$(\theta)$ for$\omega=0.2$ rad. -
To improve the properties of fine metal powder, such as particle size distribution and geometric standard deviation, this work was done at various atomizing conditions. The new atomization mechanism and the correlation equation were proposed to estimate the mean particle diameter.
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Through different projects, CETIM and its scientific and industrial partners have evaluated the potential of the High Velocityy Compaction Technology in terms of materials and component shape. Various kinds of powder materials were studied: metals, ceramics and polymers. The HVC process was used with success to manufacture gears, large parts and multilevel components. Due to the high density of HVC parts, the green machining process enables shapes to be produced that would otherwise be impossible to compact and components to be produced with very hard sintered and homogeneous materials.
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High velocity compaction (HVC) is a production technique with capacity to significantly improve the mechanical properties of powder metallurgy (PM) parts. Investigated here are green body data such as density, tensile strength, radial springback, ejection force and surface flatness. Comparisons are performed with conventional compaction using the same pressing conditions. Cylindrical samples of a pre-alloyed water atomized iron powder are used in this experimental investigation. The HVC process in this study resulted in a better compressibility curve and lower ejection force compared to conventional quasi static pressing. Vertical scanning interferometry measurements show that the HVC process gives flatter sample surfaces.
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High-Speed Centrifugal Compaction Process is one of slip-using compacting method originally developed for processing of oxide ceramics. In this study, we apply the HCP to ultra-fine (0.1 micron) WC powder. Organic liquid of heptane was chosen as dispersing media to avoid possible oxidation of WC. The mixing apparatus was a key to obtain dense compacts. Only the slips mixed by high energy planetary ball mill were packed up to 55% by the HCP, and sintered to almost full density at 1673 K without any sintering aids. This sintered compact marked Vickers hardness of Hv 2750 at maximum.
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Capping mechanisms during the compaction of pharmaceutical powders were explored. Both experimental and numerical investigations were performed. For the experimental study, an X-ray Computed Microtomography system has also used to examine the internal failure patterns of the tablets produced using a compaction simulator. Finite element (FE) methods have also been used to analyse the powder compaction. The experimental and numerical studies have shown that the shear bands developed at the early stage of unloading appear to be responsible for the occurrence of capping. It has also been found that the capping patterns depend on the compact shape.
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High-Speed Centrifugal Compaction Process (HCP) is a wet compacting method, in which powders are compacted under a huge centrifugal force. The HCP was well applied to small alumina specimens, but the compact easily cracked when we applied the HCP to other materials. We clarified how the cracks introduced and found that the formation of such a flow pattern was related to the Colioli's force in the centrifugal field.
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In a multi-action tooling system, which is usually used for the powder compaction process to fabricate the complex multilevel parts, crack formation is crucially detrimental and should be avoided. Among various process factors, tool shape is an important factor to prevent the crack formation during powder compaction process. In this work, the effects of different tool shapes were investigated through the experimental oberservation of pore distribution in real products and the finite element analysis of residual stresses. The results were interpreted based on non-uniform powder density in the compacted parts.
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Processing and properties of high power piezoelectric transformer (PT) fabricated by PIM with nano-sized piezoelectric powders are demonstrated. The high power characteristics of a PMed dome-shaped PT were examined by the lighting test for a 55watt PL lamp. The 55watt PL lamp was successfully driven by the PIMed PT with sustaining efficiency higher than 98%. The transformer with ring/dot area ratio of 2.1 exhibited the maximum properties in terms of output power, efficiency and temperature stability.
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The development of Micro MIM as a new manufacturing process for metallic micro parts made of advanced functional materials has been the subject of considerable research over the last years. This paper addresses important quality aspects on processing of new materials by Micro-MIM. Three examples of new functional materials that can be processed are reviewed in this paper. The first example is two-component-Micro-MIM to obtain multi-functional devices. A micro positioning encoder consisting of a magnetic / non-magnetic material combination is presented. The second issue is series production of the replicate of the smallest human bone in the ear (stapes) from Titanium as an example of medical application. Quality assurance and reproducibility in terms of injection moulding parameters are addressed. In the third part, first results on the processing of the shape memory alloy NiTi by Micro-MIM are presented. Potential applications include biocompatible devices and transportation, for example automotive and aerospace. Processing routes and initial microstructures obtained are discussed.
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This study aims to investigate the usage of nano-scale particles in a micro metal injection molding (
$\mu$ -MIM) process. Nanoscale particle is effective to improve transcription and surface roughness in small structure. Moreover, the effects of hybrid micro/nano particles, Cu/Cu and SUS/Cu were investigated. Small dumbbell specimens were produced using various feedstocks prepared by changing binder content and fraction of nano-scale Cu particle (0.3 and$0.13{\mu}m$ in particle size). The effects of adding the fraction of nano-scale Cu powder on the melt viscosity of the feedstock, microstructure, density and tensile strength of sintered parts were discussed. -
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The relationship between the powder particle size change and a mechanical property of the Metal Injection Molding (MIM) product was examined in detail. The XRD results indicate that the diffraction peaks of BCC appeared in compacts of powder particle size of 4 to
$10{\mu}m$ as well as the bulk SUS630. However, the diffraction peaks from both BCC and FCC were observed in the compact with powder size less than$3{\mu}m$ . TEM observation revealed that the powder with those BCC/FCC two phase structure have a finely dispersed$SiO_2$ precipitates. Because the Si is ferrite stabilizing element, decrease of Si composition in the matrix phase by the$SiO_2$ precipitation resulted in formation of the retained austenite. Therefore, controlling the elements such as Si as well as oxygen decrease is very important to obtain a normal microstructure in ultra-fine powder$(<3{\mu}m)$ injection molding. -
Small powder size is very useful in achieving detailed structures. STS 316 nanopowders with an average diameter of 100 nm and
$5{\mu}m$ were utilized to produce feedstock. The mixing behavior of the feedstock indicated that the nanoparticle feedstock produced the highest mixing torque at various powder loading compared to the micropowder feedstock. The nanoparticles feedstocks showed that elastic properties are dominant in flow behavior and high viscosity. Conversely the micropowders feedstocks, viscous properties are dominant in flow behavior and less viscosity, nanopowders feedstock perform lower flow activation energy than feedstock with bigger particles. -
The production method of micro sacrificial plastic mold insert metal injection molding, namely
${\mu}-SPiMIM$ process has been proposed to solve specific problems involving the miniaturization of MIM. Two types of sacrificial plastic molds (SP-mold) with fine structures were used: 1) PMMA resist, 2) PMMA mold injected into Ni-electroform, which is a typical LIGA (${\underline{L}}ithographie-{\underline{G}}alvanoformung-{\underline{A}}bformung$ ) process. Stainless steel 316L feedstock was injection-molded into the SP-molds with multi-pillar structures. This study focused on the effects of metal particle size and processing conditions on the shrinkage, transcription and surface roughness of sintered parts. -
Atre, Sundar V.;Wu, Carl L.;Hwang, Chul-Jin;Zauner, Rudolf;Park, Seong-Jin;German, Randall M. 45
In recent years, micro powder injection molding$(\mu-PIM)$ is being explored as an economical fabrication method for microcomponents in microsystems technology (MST). Technical and economic comparison was performed for$\mu-PIM$ processes. Molding experiment and simulation during the filling process were performed to evaluate several different geometries and processing conditions. The influence of material parameters and process conditions on mold filling were examined as a function of features size using microchannels as an example. It was found that the heat conductivity and viscosity of feedstock, geometry and mold temperature were the most critical parameters for complete filling of micro features. -
Oridinal thermal spray process has developed into two ways, namely, temperature dominated represented by plasma spraying, and velocity dominated represented by HVOF. It is common for both that the particle materials sprayed are basically in melted or half melted condition. New process has developed recently, that is, Cold Spray and Aerosol Deposition. Particle's heating is limited in CS lower than half of the material's melting point. Moreover, exactly no heating is loaded in AD process. Through the investigation on common feature for these three spraying processes, potential of new material process - Particle Deposition, PD - is considered and proposed.
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$Ti(Al,\;O)-Al_2O_3$ ] composite powders were produced by high energy mechanical milling of a mixture of Al and$TiO_2$ powders followed by a combustion reaction. The powders were subsequently thermally sprayed on H13 steel substrates. Microstructural examination was conducted on the composite powders and thermally sprayed coatings, using X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The performance of the coatings was evaluated in terms of micro-hardness and thermal fatigue. The thermally sprayed coatings performed very well in the preliminary thermal fatigue tests and showed no wetting tendency to molten aluminum. -
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$Ti_{45}Zr_{38}Ni_{17}$ ] powders were thermally sprayed onto mild steel substrates in air and under a reduced pressure of argon. Several oxides were formed after thermally-spraying the mechanically-alloyed powders in air. After spraying in a reduced pressure of argon, the coating layers obtained from the gently mixed powders consisted of the elemental metals, but an amorphous phase primarily appeared in the thermally-sprayed mechanically-alloyed powders, which transformed into the icosahedral quasicrystal phase and a minor$Ti_2Ni-type$ crystal phase after annealing at 828 K. The Vickers hardness and the contact angle with pure water for the quasicrystal layers were about 7 GPa and$92^{\circ}$ respectively. -
Ti-Zr-Ni coatings deposited by low vacuum plasma spray technique consisted of nanometer-sized
$W-Ti_{50}Zr_{35}Ni_{15}$ 1/1 cubic approximant and TiZrNi Laves phases as well as a low volume fraction of$ZrO_2$ phase. The shift of composition during deposition of the quasicrystalline powders and the presence of$ZrO_2$ phases are believed to be responsible for the reduced corrosion performances evaluated by means of electrochemical tests in a Hanks' Balance Salt Solution at$37^{\circ}C$ . -
Hwang, S.Y.;Kim, J.H.;Kim, H.J.;Seong, B.G.;Jun, H.W.;Lee, H.W.;Seok, H.K.;Lee, C.;Yang, H.;Baik, K.H. 55
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Porosity in spray-formed materials is an important issue, but the formation of porosity is not completely understood. The paper gives some examples picked from literature, which show some general correlations between process parameters and porosity. To improve the understanding of porosity formation it is necessary to know more about the conditions of the droplets and the deposit at the point of impingement. Determining the impact conditions is a challenge because usually they are not constant with time and some values are difficult to measure. Our experiments show a strong correlation between the deposit surface temperature and the porosity. The average impact angle weighted by the local particle mass flux is also an important parameter.
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In Spray Forming, specific enthalpy is a key parameter in the deposition process as it influences the thermal condition of the impinging droplets as well as that of the deposit surface. An empirical model for the distribution of specific enthalpy in the spray cone was developed as an easy to handle alternative to numerical models with which the descriptive partial differential equations are solved numerically. The model results were compared with the experimental data to validate its applicability.
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In this contribution, we attempted a theoretical analysis on the validity of the widely-accepted idea that rough and singular surfaces can coexist in a crystal at equilibrium. By manipulating the Cahn and Hoffman capillarity vector, the conclusion that a crystal at equilibrium should be composed either of singular surfaces or of rough ones was reached.
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Both densification and grain growth are driven by the reduction of the interfacial area, kinetics of which depends strongly on the interface structure. Abnormal grain coarsening in the system of singular solid/liquid interface such as WC-Co alloys was explained by the growth mechanism of 2-dimensional nucleation. Based on this concept, the marked inhibition of coarsening of WC grains by VC addition can be approached by the increase in the step free energy, which increases the barrier of 2-dimensional nucleation. The activated sintering in tungsten powders can be approached by the interface structure change induced by the addition of a small amount of nickel.
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Anisotropic constitutive equations for sintering of metal powder compacts have been formulated from a linear viscous transversely-isotropic model in which an anisotropic sintering stress has been introduced to describe free sintering densification kinetics. The identification of material parameters defined in the model, has been achieved from thermomechanical experiments performed on 316L stainless steel warm-compacted powder in a dilatometer allowing controlled compressive loading.
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The master sintering curve (MSC) is derived from densification data over a range of heating rates and temperatures. To improve the accuracy, several modifications were proposed: multi-phase MSC for solid state sintering with phase changes, MSC for liquid phase sintering, and MSC with consideration of grain growth. The developed MSC models were applied to several material systems such as molybdenum, stainless steels, and tungsten heavy alloys (WHA), in order to evaluate the effect of compaction pressure, phase change, grain growth, and composition on densification, to classify regions having different sintering mechanism, and to help engineer design, optimize, and monitor sintering cycles.
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When an alloy such as Ni-W is liquid phase sintered, heavy solid W particles sedimentate to the bottom of the container, provided that their volume fraction is less than a critical value. The sintering process evolves typically in two stages, diffusiondriven macrosegregation sedimentation followed by true sedimentation. During macrosegregation sedimentation, the overall solid volume fraction decreases concurrently with elimination of liquid concentration gradient. However, in the second stage of true sedimentation, the average solid volume fraction in the mushy zone increases with time. It is proposed that the true sedimentation results from particle rearrangement for higher packing efficiency.
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Growth behavior and kinetics of grains in a liquid matrix has been studied by computer simulation for various physical and processing conditions. The kinetics of growing and dissolving grains were considered to follow those of single crystals in a matrix. Depending on the shape of crystals, rounded or faceted, different kinetic equations were adopted for growing grains and an identical equation for dissolving grains. Effects of such critical parameters as step free energy, temperature, and liquid volume fraction were evaluated.
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The error function can be calculated based on the Simpson method through a subroutine program. An integration program by FORTRAN language was made for diffusion equations of extended source with infinite extent and limited extent. The results on some alloying elements such as C, Co, Cr, Mn, Mo, Ni and V's diffusion in iron, showed the diffusion distance for Ni and Mo can only be
$1{\sim}3\;{\mu}m$ and more distance for Co at common sintering temperature of$1120^{\circ}C$ . To refine the particle size of the added elements down to a scale of micrometers is an effective way to get homogeneous distribution. -
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New PM route via bulk mechanical alloying is developed to fabricate the solid solution semi-conductive materials with
$Mg_2Si_{1-x}Ge_x$ and$Mg_2Si_{1-y}Sn_y$ for 0 < x, y < 1 and to investigate their thermoelectric materials. Since$Mg_2Si$ is n-type and both$Mg_2Ge$ and$Mg_2Sn$ are p-type, pn-transition takes place at the specified range of germanium content, x, and tin content, y. Through optimization of chemical composition, solid-solution type thermoelectric semi-conductive materials are designed both for n-and p-type materials. -
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From a viewpoint of heat stress at high temperatures and contact thermal resistance, it is confirmed that the optimal structure is the skeleton structure using Cu substrate on the cooling side, which has excellent heat conductivity and the optimal installation method is to adopt a carbon sheet and a mica sheet to the high temperature side, where Si grease is applied to the low temperature side, under pressurized condition. The power of the developed modules indicated 0.5W in an
$FeSi_2$ module and 3.8 W with a SiGe module at 823K, respectively. -
This paper presents the influence of the compositions of sintered Ti-Ni alloys on their thermo-mechanical properties. The Ti-Ni alloys having various compositions from 50at%Ni to 51at%Ni were sintered using elemental Ti and Ni powders by a pulse-current pressure sintering equipment. The deformation resistance in stress-strain curves increased with an increase in Ni content. In the case of Ti-50at%Ni, tensile strength and elongation were more than 500 MPa and 7%, respectively. The increase in Ni content also makes the transformation temperatures lower. The deformation resistance at a test temperature change from 293K and 353K in isothermal tensile test increased with elevating test temperature.
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Processing of W-Cu graded materials from attritor-milled W-CuO mixtures is described. The powder reduction steps are investigated by TG and XRD analyses and by microstructural observations (SEM, TEM). Sintering of reduced powder with different compositions is analysed by dilatometry. Sintering behaviour of the graded component processed by co-compaction of a 10/20/30wt%Cu multi-layer material is briefly discussed. Liquid Cu migration is observed and smooths the composition gradient. Perspectives to control this migration are discussed.
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A theoretical model is applied to the analysis of thermomechanical properties of
$Al-SiC_p$ FGMs in this study. Functionally graded$Al-SiC_p$ composites ($Al-SiC_p$ FGMs) consisted with 10 layers gradually changing volume fractions of Al and$SiC_p$ were fabricated using the pressureless infiltration technique.$Al-SiC_p$ FGMs plates of total thickness of 3mm, 5mm and 7mm with fairly uniform distribution and compositional gradient of$SiC_p$ reinforcement in the Al matrix throughout the thickness was successfully fabricated. The curvature of$Al-SiC_p$ FGM plates was measured to check the internal stress distribution predicted via a theoretical model for the analysis of thermo-mechanical deformation. The evolution of curvature and also internal stresses in response to temperature variations could be predicted for the different combinations of geometric thickness of FGM plates. Theoretical prediction of thermally induced stress distribution makes it possible to design FGM structures without any critical failure during the usage of them. -
Ceramic-Metal Functionally Graded Materials (FGM) are of great interest for application as Thermal Barrier Coating (TBC) or Wear Resistant Coating (WRC). Spark Plasma Sintering (SPS) is a promising techniques for time-saving consolidation of laminated/graduated powder systems: SPS is a pressure-assisted electrical sintering method which directly applies a pulsed DC current as heat source. In the present work, production of
$Al_2O_3-Ni$ FGMs by means of Spark Plasma Sintering is considered; effect of sintering condition on density, hardness and fracture toughness is studied. Problems correlated to this new processing technology are discussed. -
Austenitic stainless steel has been used as a corrosion resistance material. However, austenitic stainless steel has poor wear resistance property due to its low hardness. In this investigation, we apply powder composite process to obtain hard layer of Stainless steel. The composite material was fabricated from planetary ball milled SUS316L stainless steel powder and WC powder and then sintered by Pulsed Current Sintering (PCS) method. We also added TiC powder as a hard particle in WC layer. Evaluations of wear properties were performed by pin-on-disk wear testing machine, and a remarkable improvement in wear resistance property was obtained.
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Metallic foams have a combination of attractive properties such as high specific mechanical properties and good energy absorption characteristics. This paper presents the properties of steel foam sandwiches produced using powder metallurgy approach. Metallic powder, solid polymeric binder and a foaming agent are dry-mixed and molded into the desired shape. The molded powder mix is then heat-treated to foam, debind and sinter the material. The resulting material has an open cell structure with high porosity. The structure and properties of sandwiches specimens produced with the process are presented and discussed.
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A novel production method for porous metal components has been developed by applying powder space holder (PSH) method to metal powder injection molding (MIM) process. The PSH-MIM method has an industrial competitive advantage that is capable of net-shape manufacturing the micro-sized porous metal products with complicated shapes and controlled porosity and pore size. In this study, the small impeller with homogeneous micro-porous structure was manufactured by the PSH-MIM method. The effects of combinations in size and fraction of PMMA particle on dimensional tolerance and variation of sintered porous specimens were investigated. It was concluded that the PSH-MIM method could manufacture commercially microporous metal components with high dimensional accuracy.
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Shimizu, Toru;Hanada, Kotarou;Adachi, Satoru;Katoh, Masahito;Hatsukano, Kanichi;Matsuzaki, Kunio 95
Stainless steel sludge is generated as a waste in the grinding process, and the possibility of recycling stainless steel is considered here. In this study, we considered the possibility of using the stainless steel sludge as metal powder for MIM or raw material for metal foam. For the MIM process, the metal powder will need some improvement, and flotation and spheroidizing processes of the sludge are necessary. For fabrication of the metal foam, untreated sludge can be used, and steel foam about 90% porosity is produced. -
Gas-permeable metal die materials are developed using tool steel powder, packed in a mold having the insertion of orthogonally arrayed polymer wires. Linear gas-permeable channels in orthogonal array are thus developed by the burning out of the polymer wires, which yield a microstructure with wear resistance value and air permeability much larger than those of the conventional gas-permeable die material.
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Cellular metals based on Iron have been intensively investigated during the last two decades. Because of the significant decreasing of the structural density of Iron based cellular structures, numerous technologies have been developed for their manufacturing. Besides the tremendous weight reduction a combination with other properties like energy and noise absorption, heat insulation and mechanical damping can be achieved. This contribution will give an overview about the latest state in Iron based cellular materials, including technologies in manufacturing, properties and potential applications.
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Processing techniques for producing microcellular silicon carbide, mullite, and cordierite ceramics have been developed by a reaction method that incorporates a polysiloxane and reactive fillers. The techniques developed in this study offer substantial flexibility for producing microcellular ceramics whereby cell size, cell density, degree of interconnectivity, composition, and porosity can all be effectively controlled. It is demonstrated that the adjustment of filler composition enables the possibility of tailoring the composition and properties of the microcellular ceramics. The present results suggest that the proposed novel processing techniques are suitable for the manufacture of microcellular ceramics with high morphological uniformity.
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The low-cycle fatigue performance and fracture of the P/M Ti-Fe-Mo-Al-Nd Alloys after sintering and forging have been studied. The linear regression equation of low-cycle fatigue lifetime has been obtained; the fatigue performances are objected under two different conditions. The fatigue fracture surface is analyzed by SEM. The low-cycle fatigue behavior of the P/M titanium alloy has been discussed.
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The effect of WC or NbC addition on various properties of Ti(C0.7N0.3)-Ni cermets was investigated. The microstructure oj Ti(C0.7N0.3)-xWC-20Ni showed a typical core/rim structure, irrespective of the WC content, whereas the structure oj Ti(C0.7N0.3)-xNbC-20Ni was different and was dependent on the NbC content. The hardness (HV) and the fracture toughness (KIC) had a tendency to increase marginally, while the coercive force (HC) and the magnetic saturation
$(4{\pi}{\sigma})$ decreased gradually with an increase in WC or NbC content in the systems studied. In addition, increasing WC content in Ti(C0.7N0.3)-xWC-20Ni system, decarburization was retarded, while denitrification was accelerated -
We have studied the effect of C/Ti atomic ratio of TiCx (x=0.5, 0.75 and 1.0) raw powder on the properties of the Ti-Mo-WTiC sintered hard alloy. The decrease of C/Ti atomic ratio accelerated the densification in the sintering process. The hardness was remarkably improved up to 1350HV with decreasing the C/Ti atomic ratio because of increase of TiCx phase volume content and its fine dispersion. From the results of electro-chemical tests in acid and 3% NaCl solutions, it was obvious that every alloy had excellent corrosion resistance, which meant about 200 times better than that of WC-Co cemented carbide.
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Injection molding of corrosive super engineering plastics and engineering plastics with various fillers is conducted under severe conditions and causes corrosion and wear problems. We have developed
$Mo_2NiB_2$ boride base cermets, which have excellent corrosion-and wear-resistances, and tried to apply them into plastic molding machine parts. In this paper, the effects of V substitution for Cr on the mechanical properties, corrosion resistance and microstructure of Ni-5.0B-51.0Mo-(17.5-X)Cr-XV (mass%) model cermets were investigated. Both transverse rupture strength (TRS) and hardness increased monotonically with increasing V content and reached 2.94GPa and$87.2R_A$ at 10.0%V, respectively. The improvements of TRS and hardness were attributed to microstructural refinement. -
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$FerroTitanit^{(R)}$ ] is an extremely high alloyed PM material containing about 20 to 35 wt.% titanium based carbides. Such materials are designed to achieve a high wear resistance, but the high volume fraction of hard phases causes a comparable low ductility in case of tensile loading. In the present study the mechanical properties of different Ferro-Titanit grades (variations in chemical composition and in heat treatment) were investigated by means of tensile tests. The mechanical properties and the fracture behaviour will be related to the chemical composition, the heat treatment and the microstructure. -
Conventional high-speed steels, which are carbide decentralized materials, are used for sliding parts, but they lack sufficient hardness for some applications. Improvement of surface hardness is possible for high-Cr steels through nitriding. However, nitriding P/M parts is not advisable without sealing the porosity before treatment, as they will become brittle. However, it is difficult to seal the pores with steam treatment, because high-Cr steel has a passive film on the surface. Controlling nitriding by decreasing the amount of oxygen on the surface to be nitrided, and grinding to decrease the porosity of the surface, makes it possible to produce a material that has reasonable and sufficient hardness in the required areas.
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The development of Fe-based metal matrix composites (MMCs) with high content of hard phase has been approached by combining the use of advanced powder metallurgy techniques like high-energy milling (HEM), cold isostatic pressing (CIP) and vacuum sinterings. A 30% vol. of NbC particles was mixed with Fe powder by HEM in a planetary mill during 10h, characteristing the powder by the observation of morphology and microstructure by scanning electron microscopy (SEM). After of sintering process the variation of density, hardness,carbon content and the microstructural changes observed, permits to find the optimal conditions of processing. Afterwards, a heat treatment study was performed to study the hardenability of the composite.
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Magnetic properties of nanostructured materials are affected by the microstructures such as grain size (or particle size), internal strain and crystal structure. Thus, it is necessary to study the synthesis of nanostructured materials to make significant improvements in their magnetic properties. In this study, nanostructured Fe-20at.%Co and Fe-50at.%Co alloy powders were prepared by hydrogen reduction from the two oxide powder mixtures,
$Fe_2O_3$ and$Co_3O_4$ . Furthermore, the effect of microstructure on the magnetic properties of hydrogen reduced Fe-Co alloy powders was examined using XRD, SEM, TEM, and VSM. -
Tin oxide nanoparticles (n-SnO and
$n-SnO_2$ ) were synthesized by the inert gas condensation (IGC) method under dynamic gas flow of oxygen and argon at various conditions. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) method were used to analysis the size, shape and crystal structure of the produced powders. The synthesized particles were mostly amorphous and their size increased with increasing the partial pressure of oxygen in the processing chamber. The particles also became broader in size when higher oxygen pressures were applied. Low temperature annealing at$320^{\circ}C$ in air resulted to crystallization of the amorphous n-SnO particles to$SnO_2$ . -
Multilayer ceramic capacitor (MLCC) miniaturization has increased the demand for superfine
$BaTiO_3$ powder due to its thin dielectric layer. Hydrothermally synthesized$BaTiO_3$ powder a pseudo-cubic phase resulting in poor dielectric properties due to size effect and hydroxyl ion inclusion in the$BaTiO_3$ lattice. We attempted a superfine (lower than 100 nm) highly tetragonal$BaTiO_3$ powder via a solvothermal method without precipitating agent. The lattice parameters and the relative amounts of tetragonal and cubic phases were determined using Rietveld refinement. -
In this study, nano grain W is fabricated by Severe Plastic Deformation-Powder Metallurgy (SPD-PM) process. W powder and W-Re powder mixtures are processed by SPD-PM process, a Mechanical Milling (MM) process. As results, a nano grain structure, whose grain size is approximately 20nm, is obtained in W powder after MM for 360ks. A nano grain W compact, whose grain size 630nm, has excellent deformability above 1273K. A nano grain W-10Re compact is composed of equiaxed grain, a grain growth is restrained and has low dislocation density after the large deformation; therefore it is considered that W-Re compact shows superplasticity.
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Kvackaj, Tibor;Zemko, Michal;Kuskulic, Tomas;Kocisko, Robert;Besterci, Michal;Dobatkin, Sergej V.;Molnarova, Maria 130
In the present research work was searched the influence of severe plastic deformation (SPD) realized by ECAP (equalchannel angular pressing) on structural, mechanical and plastic properties of IF (interstitial free) steel. For physical simulation ECAP process with right angle channels$(90^{\circ})$ was used. The ECAP process was numerical simulated (namely its course of temperature, strain and stress fields and deformation forces) by FormFEM software, too. -
Optimized choice of material for two principally different types of PM components is presented. The first is characterized by high stresses in areas with high stress concentrations (for example synchronizer hubs with very sharp notches, typically <0.25mm in the pre-synchronizer slot and the inner splines). The second type has slightly larger notch radii (small spur gears and sprockets with typically notch radii between 1- 3mm). Diffusion alloyed materials are well suited for sharp notch components. Pre-alloyed materials are also well suited for applications with sharp notches if compressive residual stresses in the notch roots are created by appropriate process control. A free choice of material is available for components with the larger notch radii.
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Ancorsteel 4300, a high performance Cr-Si-Ni-Mo steel, was unveiled two years ago as the first in a series of powder metallurgy alloys that will simulate wrought steel compositions. Advantages of this alloy include good compressibility, high hardenability, and excellent dimensional stability. More important, however, is that this alloy has the ability to be effectively sintered at
$1120^{\circ}C$ and maintain oxygen contents below 500 ppm. This unique blend of performance and processing capabilities provides static and dynamic properties that exceed those of conventional powder metallurgy alloys and approach wrought gearing materials. A second Cr-Si-Ni-Mo alloy has now been developed that offers complimentary performance levels at a lower Mo content. This manuscript reviews properties of the two chromium steels with comparisons to traditional sinter-hardened and heat-treated powder metallurgy alloys. -
Crack initiation and short crack propagation was studied on the polished notched surfaces of Cr-Mo prealloy sintered steels with 7.35
$g.cm^{-3}$ sintered density. An ultrasonic resonance test system operating in push-pull mode at 20 kHz and R=-1 was used. It showed that crack initiation took place in several places, small cracks growing oriented to the local pore structure rather than to stress orientation. Their growth rate is markedly higher than the corresponding one of long cracks. Finally, several microcracks join to form a dominant crack. -
Sintered steels are materials characterized by residual porosity, whose dimension and morphology strongly affect the fatigue crack growth behaviour of the material. Prismatic specimens were pressed at
$7.0\;g/cm^3$ from Astaloy CrM powder and sintered varying the sintering temperature and the cooling rate. Optical observations allowed to evaluate the dimensions and the morphology of the porosity and the microstructural characteristics. Fatigue tests were performed to investigate the threshold zone and to calculate the Paris law. Moreover$K_{Ic}$ tests were performed to complete the investigation. Both on fatigue and$K_{Ic}$ samples a fractographic analysis was carried out to investigate the crack path and the fracture surface features. The results show that the Paris law crack growth exponent is around 6.0 for$1120^{\circ}C$ sintered and around 4.7 for$1250^{\circ}C$ sintered materials. The same dependence to process parameters is not found for$K_{Ith}$ . -
Most PM components are exposed to cyclic loading over long periods of time, yet, the fatigue performance is often at best characterized by a fully reversed bending strength. The effects of density, deviating loading modes, external notches or mean stresses must usually be estimated. The amount of available data is nowadays sufficient to come to fact-based estimates.
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Recently, automotive engines have changed to the silent chain system in order to reduce noise and to improve reliability. High contact fatigue strength is needed for the sprockets of silent chain system. As a result, a high-contact-fatigue-strength P/M material was developed using the technology of surface rolling, which densifies the surface layer of sintered parts. It was established that the contact fatigue strength of the developed material was a great improvement over that of the conventionally used sintered material.
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A developed molybdenum hybrid-alloyed steel powder is based on a molybdenum prealloyed steel powder to which molybdenum powder particles are diffusion bonded. The sintered compact made of this powder has a finer pore structure than that of the conventional molybdenum prealloyed steel powder, because the ferritic iron phase
$({\alpha}-phase)$ with a high diffusion coefficient is formed in the sintering necks where molybdenum is concentrated resulting in enhanced sintering. The rolling contact fatigue strength of the sintered and carburized compacts made of this powder improved by a factor of 3.6 compared with that of the conventional powder due to the fine pore structures. -
Tenegal, Francois;Guizard, Benoit;Reau, Adrien;Ye, Chang;Boulanger, Loic;Giraud, Sophie;Canel, Jerome 150
Laser pyrolysis is a very suitable method for the synthesis of a wide range of nanoparticles. A pilot unit based on this process has been recently developed at CEA. This paper reports results showing the possibility to produce SiC and$TiO_2$ nanoparticles at rates of respectively 1 and 0.2 kg/h and also the possibility to adjust the mean grain size of the particles and their structure by changing the laser intensity and reactants flow rates. First tests of liquid recovery have been also successfully performed to limit the risks of nanoparticles dissemination in the environement during their recovery. -
We demonstrate the methodology of engineering the multi-component ceramic nanopowder with precise morphology by nanoblast calcinations decomposition of preliminary engineered nanoreactors. Multiple explosions of just melted
$C_3H_6N_6O_6$ embedded into preliminary engineered nanoreactors break apart the agglomerates due to the highly energetic impacts of the blast waves. Also, the solid-solubility of one component into the other is enhanced by the extremely high local temperature generated during each nano-explosion in surrounding area. This methodology was applied for production of agglomeratefree nano-aggregates of$Gd_{20}Ce_{80}O_{1.95}$ with an average size of 42 nm and$LaSrGaMgO_{3-x}$ nanopowder with an average aggregate size of 83 nm. -
This study investigated a mechanism for controlling the shape of Cu nanocrystals fabricated using the polyol process, which considers the thermodynamic transition from a facetted surface to a rough surface and the growth mechanisms of nanocrystals with facetted or rough surfaces. The facetted surfaces were stable at relatively low temperatures due to the low entropy of perfectly facetted surfaces. Nanocrystals fabricated using a coordinative surfactant stabilized the facetted surface at a higher temperature than those fabricated using a non-coordinative surfactant. The growth rate of the surface under a given driving force was dependent on the surface structure, i.e., facetted or rough, and the growth of a facetted surface was a thermally activated process. Surface twins decreased the activation energy for growth of the facetted surface and resulted in rod- or wire-shaped nanocrystals
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The preparation of composite powders for plasma spraying by an in-house designed mechanofusion process is investigated. Results show that dry particle coating depends on the chemical and mechanical properties of powders. In metal/oxide and metal/oxide/carbide powder mixtures, fine ceramic particles coat the surface of the metallic coarser particles. A nearly rounded shape of the final composite particles is induced by the mechanical energy input with no formation of new phases. However with the carbide/metal powdered system, only an intimate mixture of components is achieved. It is suggested that the coating mechanism is governed by agglomeration and rolling phenomena.
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Ultrafine Au-Pb particles prepared by two method, (1) simultaneous evaporation of Au and Pb in inert gas and (2) subsequent vapor condensation of Pb in a differentially evacuated tube onto flying Au nanoparticles prepared by gasevaporation technique, were observed by electron microscopy. In the method (1), the particles that grew at the region where the two smoke masses converged, consisted of alloy phases. In the method (2), the particles consisted of two or three phases of Au,
$Au_2Pb$ ,$AuPb_2$ and Pb phases in turn from the inner part, Pb-rich particles being composed of only two phases of$AuPb_2$ and Pb. -
Seasonal changes have been recognized in particle characteristics and forming characteristics of iron powder with insulated coating for a compacted magnetic core because of its high hygroscopicity, due to its phosphate coating and resin binder additives. For this reason, particle characteristics and molding characteristics of the powder with diverse water absorbtivity have been studied. The result shows that the higher the volume of absorbed water, the worse the fluidity becomes, resulting in the reduction in both springback during the molding process and expansion reduction after the heat treatment. The requirement on dimension accuracy for the finished product can be satisfied with an additional drying process on the material powder, which contributes to maintain its water volume constant.
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A QM-ISP-4 Planetary Mill was employed to activate mechanically the mixtures of anatase and corundum at room temperature for different times. The milled powder mixtures were then sintered at
$1300^{\circ}C$ for 1 h. The XRD results showed that the milled powder mixtures were completely transformed into$Al_2TiO_5$ after sintering, except the mixtures milled for 5 and 10 hours. The SEM observations showed the typical morphology of rod-like$Al_2TiO_5$ vary in the range: widths from 0.6 to$1.2\;{\mu}m$ , and lengths from 3.0 to$6.0\;{\mu}m$ . The rod-like$Al_2TiO_5$ formation was attributed to the positive effects caused by the mechanical activation. -
Nb-Ti alloys were hydrogenated to prepare fine and contamination-free powders. Cracks were introduced in the alloys when they were annealed at 1473 K and cooled in a hydrogen atmosphere. The fragments produced by hydrogen-induced cracking are brittle and the friability enhanced with the Ti content of the alloy, which is beneficial for further refinement of particle size. We also demonstrate that Nb-Ti powders with the average particle size less than 1 m can be produced by ball milling at a temperature lower than 203 K. Furthermore, hydrogen-free powders can then be obtained by annealing above the temperature corresponding to hydrogen desorption from Nb solid solution.
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A hyrdrothermal synthesis has been developd to prepare rod-like crystals of copper oxide using copper nitrate trihydrate as a function of synthesis temperature, stirring speed and solution pH value. The properties of the fabricated crystals were studied using scanning electron microscopy, X-ray diffraction and particle size analysis. The morphology of the synthesized CuO was dependent on both the pH value of the solution and the morphology of the seed materials. Synthesized particles have regular morphologies and a uniform size distribution.
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Advanced melting technology is now being employed in the manufacture of stainless steel powders. The new process currently includes electric arc furnace (EAF) technology in concert with Argon Oxygen Decarburization (AOD), High Performance Atomizing (HPA) and hydrogen annealing. The new high performance-processing route has allowed the more consistent production of existing products, and has allowed enhanced properties, such as improved green strength and green density. This paper will review these processing changes along with the potential new products that are being developed utilizing this technology. These include high strength stainless steels such as duplex and dual phase as well as stainless steel powders used in high temperature applications such as diesel filters and fuel cells.
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The effect of the preparation factors, such as the feeding mode and rate of raw materials, the reaction temperature and the surfactant on the size distribution of molybdenum trioxide particle were investigated by orthogonal test. The optimum conditions for the preparation of
$MoO_3$ precursors are as following; opposite feeding fast, reaction temperature of$60^{\circ}C$ and adding dispersant. -
X-ray analysis on iron ores and reduced iron powders revealed that the main acid-insoluble substances were hexagonal and tetragonal quartz, another substances were sillimanite, alumina-silicate, an unnamed zeolite, all contained Si and Al. Their particle size was in the range of
$3{\sim}7\;{\mu}m$ . Statistics analysis showed that the AIC for high-grade magnetite powder was$(0.130{\pm}0.010)%$ ) during the latest five months. The predicting value for reduced iron powder should be 0.179%. However, the testing value for reduced iron powder was$(0.192{\pm}0.014)%$ . The limited difference of 0.013% might imply rare pollution coming from the reduction and milling processes. The most important step for control AIC should be the separation process of iron ore powders. -
The filling property of the binder treated iron based powder made of atomized iron powder was compared with that of the one made of reduced iron powder. The latter one showed a better filling property than the former one, although the original reduced powder showed a worse flow rate. Changing the particle size distribution of the original atomized powder from wide to narrow like the original reduced iron powder, improved the filling property of the binder treated powder. As a result, the particle size distribution of the original iron powder was found to strongly affect the filling property of the binder treated powder.
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The results of monotonic and cyclic uniaxial compression tests, in which the deviatoric component of the stress is predominant, carried out on green and recrystallized iron compacts with different levels of density are presented and discussed in order to analyse the macro and micro-mechanisms governing the mechanical behaviour of non-sintered PM materials. The plastic deformation of the particles, especially at the contact areas between neighbouring grains, produces an internal friction responsible for the main features observed in the behaviour of green metallic compacts. These results show important discrepancies with the plasticity models, Cam-Clay and Drucker-Prager Cap.
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Densification behavior of various metal and ceramic powder was investigated under cold compaction. The Cap model was proposed based on the parameters obtained from axial and radial deformation of sintered metal powder compacts under uniaxial compression and volumetric strain evolution. For ceramic powder, the parameters were obtained from deformation of green powder compacts under triaxial compression. The Cap model was implemented into a finite element program (ABAQUS) to compare with experimental data for densification behavior of various metal and ceramic powder under cold compaction.
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Cylindrical specimens with different levels of density have been submitted to uniaxial compression tests with loading and unloading cycles. The analysis of the elastic loadings shows a non linear elasticity which can be mathematically represented by means of a potential law. Results are explained by assuming that the total elastic strain is the contribution of two terms one deriving from the hertzian deformation of the contacts among particles and another that takes into account the linear elastic deformation of the powder skeleton. A simple model based in an one pore unit cell is presented to support the mathematical model.
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Densification behavior of iron powder under cold stepped compaction was studied. Experimental data were also obtained for iron powder under cold stepped compaction. The elastoplastic constitutive equation based on the yield function of Shima and Oyane was implemented into a finite element program (ABAQUS) to simulate compaction responses of iron powder during cold stepped compaction. Finite element results were compared with experimental data for densification, deformed geometry and density distribution.
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Numerical Simulation of powder die pressing is conducted on Case Study geometry. Influence of fill density distribution and punch kinematics upon green density distribution and punch loading are studied and discussed. Deviations in punch kinematics due to punch deflection influence the most the results in term of density and force.
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In contrast with the Finite Element Method, the Discrete Element Method (DEM) takes explicitly into account the particulate nature of powders. DEM exhibits some drawbacks and many advantages. Simulations can be computationally expensive and they are only able to represent a volume element. However, these simulations have the great advantage of providing a wealth of information at the microstructural level. Here we demonstrate that the method is well suited for modelling, in coordination with FEM, the compaction of ceramic
$UO_2$ particles that have been aggregated. Aggregates of individual ceramic crystallites that are strongly bonded together are represented by porous spheres. -
During cold compaction processes loose powder is pressed under tooling action in order to produce complex shaped engineering components. Here, the analysis of the plastic deformation of granular packings is of fundamental importance to the development of computer simulation models. Powders can be idealized by packing discrete particles, where each particle is a sphere meshed with finite elements. The pressing of a body centered cubic packing was compared with numerical prediction and experimental data. The global response was expressed in force-displacement curve, and the accuracy of the numerical models analyzed for high relative densities up to 0.95.
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The deformation under radial pressure of rectangular dies for metal powder compaction has been investigated by FEM. The explored variables have been: aspect ratio of die profile, ratio between diagonal of the profile and die height, insert and ring thickness, radius at die corners, interference, different insert materials, i. e. conventional HSS, HSS from powders, cemented carbide (10% Co). The analyses have ascertained the unwanted appearance of tensile normal stress on brittle materials, also "at rest", and even some dramatic changes of stress patterns as the die height increases with respect to the rectangular profile dimensions. Different materials behave differently, mainly due to difference of thermal expansion coefficients. Profile changes occur when the dies are heated up to the temperature required for warm compaction. The deformation patterns depend on compaction temperature and thermal expansion coefficients.
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With the onging trend of weight saving in automobiles, the application of light alloys is increasing. Recently, aluminum powder metallurgy has been the subject of renewed attention due to the combination of lightweight of aluminium and the efficient material utilisation of the powder metallurgical process, which offer attractive benefits to potential end-users. This study is to explore the use of warm compaction process to aluminium powder metallurgy. This paper presents a detailed study of the effect of warm compression and sintering conditions on the resultant microstructures and mechanical properties of Al-Cu-Mg-Si PM blend.
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In recent years, demands for sintered ferrous material with higher strength are increasing. To satisfy these demands, studies and commercial use of the die wall lubrication method, the warm compaction method and the combination of both methods are widely carried out to achieve high density. The die wall lubrication warm compaction method makes it possible to achieve high density by reducing internal lubricant through die wall lubrication, although the method involves several issues such as prolonged cycle time due to lubricant spraying and difficulty in spraying lubricant in the case of compacting with complicated geometry. Meanwhile, the conventional warm compaction method requiring no die wall lubricant application cannot achieve such a high density as in the case of die wall lubrication warm compaction due to higher volume of internal lubricant. However, this report discloses our study result in which the possibility of improving density is exhibited by using a lubricant type with superior dynamic ejection property that can reduce volume of lubricant additive.
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The high pressure compaction without internal lubricant and the high green density even with the pore free density were achieved by the newly developed die wall lubricant for warm compaction. This developed die wall lubricated warm compaction followed by high temperature sintering resulted in not only the superior mechanical property but also the low dimensional change. In this paper, the effects of increasing the green density on the sintered density, the dimensional change and the mechanical property are mainly discussed
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PM recent developments focus on increasing this technology's competitiveness when compared to wrought materials. Warm compaction allows the replacement of a double press double sinter process with a single warm press and sintering step, thus allowing cost and time savings. Moreover there are added benefits to consider such as reducing work in process and lessening part's logistics cost. This paper presents a successful industrial trial to replace a double press-double sinter process with a warm die compaction and sintering process. The part chosen was a high performance gear containing 0,9% wt. carbon. Sintering was conducted in a belt furnace at
$1120^{\circ}C$ in a nitrogen rich atmosphere with rapid cooling process in order to obtain a quasi fully martensitic structure with a minimum of 700HV0,1 and 450HV10 after annealing. The balance between properties and cost is favoured by the use of a singular lubricant developed in a Eureka frame project together with POMETON S.A. and die warm compaction. Warm compaction is only needed to be effective on the gear teeth, in order to achieve the required properties. Therefore only the die is actually heated. This simplified system avoids flow rate problems typically involved when using more elaborate warm compaction equipments. -
An apparatus measuring changes of various forces directly and continuously was developed by a way of direct touch between powders and transmitting force component, which can be used to study forces state of powders during warm compaction. Using the apparatus, warm compaction processes of iron-based powder materials containing different lubricants at different temperatures were studied. Results show that densification of the iron-based powder materials can be divided into four stages, in which powder movement changes from robustness to weakness, while its degree of plastic deformation changes from weakness to robustness.
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There is an increasing demand for PM-processes with the capability to produce parts of higher complexity than with conventional press and sinter technology in high production numbers. Warm-flow-compaction (WFC) makes use of improved flowability of powders when blended in an appropriate ratio with fine powder fractions and lubricating binders. Here the process is shown with examples of PM-Steels. General features possible with the process like pressing of undercuts and threaded bores are shown.
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Rhee, Byung-Ohk;Choi, Seung-Chul;Park, Jeong-Shik;Kim, Byoung-Kyu;Kim, Hyung-Soo;Kim, Sang-Woo 205
A ball-shape alumina arc-tube for low-wattage lamp was developed by the PIM process. An ultra high purity translucentgrade alumina powder was used. In injection molding process, a hot-runner type mold was developed. The translucent-grade alumina powder was extremely sensitive to contamination so that the injection molding condition and atmosphere control in the furnace should be taken care of with extreme caution. Contamination sources were pinpointed with EPMA. The arc-tube was molded in half and two halves were bonded in the middle by a new bonding technique at room temperature developed in this study. -
In this experimental work, the development of a multicomponent binder system based on high density polyethylene (HDPE) and paraffin wax for Powder Injection Molding of Alumina
$(Al_2O_3)$ parts was carried out. The optimum composition of the injection mixture was established through mixing torque measurements and a rheological study. The maximum powder loading was 58 vol%. The miscibility of organic components and the optimum injection temperature was evaluated by thermal characterization of binder and feedstock. The thermal debinding cycle was developed on the basis of thermogravimetrical analysis of the binder. After sintering the densities achieved were closed to 98% of the theoretical one. -
Organic binders are usually pre-mixed with ceramic powders to enhance the formability during the shape forming process. These binders, however, must be eliminated before sintering in order to avoid pore formation and unusual grain growth during sintering. The present work was performed to investigate the effects of residual binder on grain growth behavior during sintering of
$Pb(Mg_{1/3}Nb_{2/3})O_3-PbTiO_3$ piezoelectric ceramics. The microstructures of sintered samples were examined for various thermal processes and atmosphere at debinding. Addition of binder seems to promote abnormal grain growth especially in incompletely debinded regions and to make the grain shape change from corner-rounded to faceted. -
Production components fabricated by metal powder injection molding are analyzed for features to identify the design window for this powder technology. This reverse approach lets the designer see where PIM has a high probability to succeed. The findings show that the most suitable components tend to be less than 25 mm in size and less than 10 g in mass, are slender, and have high complexity.
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The results of investigations in screw design for metall injection molding (MIM) will be presented. The consistency of cavity pressure, metering time and MFQ (monitoring of feedstock quality; parameter measured during metering) was chosen to compare different screws. A simulation program was used to optimize the conveying and melting mechanisms in the plastification unit. The theoretical background of this simulation programm will be explained.
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To lower the cost of MIM products, the gate and runner materials and green parts with defects are usually recycled. It is necessary to understand what causes the recycled products to deteriorate. The results show that the viscosity of the 1R (recycled once) feedstock was slightly lower than that of the fresh material. However, as the number of recyclings increased, the viscosity increased, while the density decreased, and more defects were noticed duri ng solvent debinding. These deteriorations were mainly caused by the increase of the melting point of the backbone binder and the oxidation of the filler or paraffin wax.
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More and more applications or demands for machine parts etc are expected for AISI 440C (hereinafter referred to as "440C") Stainless Steel because of its characteristic features, i.e. high-strength as well as high-corrosion resistance. This research has enabled us to obtain sintered products with good quality even under a wide range of temperature by utilizing the pinning effect of NbC, improving the relevant sintering feature of 440C Stainless Steel in the MIM method.
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To understand the effect of powder characteristics on the thermal debinding behavior, PIM parts produced with powders with different particle sizes and particle shapes were examined to determine their weight losses during thermal debinding. The results show that the average diameter of the pore channel in the compact increased when the temperature increased and when coarse powders were used. However, the weight loss rates did not increase proportionally with the pore size. This suggests that the different powders that are frequently used in PIM parts do not affect the thermal debinding rate significantly. This is because the pore size is much larger than the mean free path of the decomposed gas molecules. Thus, the diffusion rates of the gases are not rate-controlling in thermal debinding. The controlling mechanism of the thermal debinding rate is the decomposition of the backbone binder in the PIM parts.
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This paper describes a Plasma Assisted Debinding and Sintering (PADS) equipment, which has been designed to process Metal Injection Molded (MIM) components. The use of a hybrid system combining a glow discharge with a conventional heating system makes debinding and sintering of MIM components, in the same heating cycle, a feasible industrial process. Characteristics as density, carbon content and mechanical properties are similar to traditionally processed MIM materials. The reduction of energy and gas consumption and shorter lead-times are economic advantages of PADS system. The clean environment of PADS is also an ecological advantage.
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In this paper, rheological characteristics of Metal Injection Moulding (MIM) feedstock using locally binder of palm stearin are presented. The feedstock consisted of 316L-grade stainless steel powder with three different particle sizes and the binders comprise palm stearin and polyethylene. The viscosity of MIM feedstock at different temperatures and shear rates was measured and evaluated. Results showed that, the feedstock containing palm stearin exhibited suitable rheological properties and suitable to produce a homogeneous feedstock that is favorable for injection molding process.
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In this present investigation, Metal Injection Moulding (MIM) of M2 High Speed Steel (HSS) parts using a wax-High Density Polyethylene (HDPE) binder is shown. The elimination of organic binder was carried out by thermal debinding under inert atmosphere. In order to keep carbon in the sample that could improve the sintering process, incomplete debinding was performed between 450 and
$600^{\circ}C$ . The specimens were sintered at temperatures between 1210 and$1280^{\circ}C$ in high vacuum atmosphere, obtaining the 98% of the theoretical density. In the samples with higher residual carbon content, the sintering window was extended up to 20 degrees and the optimum temperature was lower. -
Wu, Yunxin;Park, Seong-Jin;Heaney, Donald F.;Zou, Xin;Gai, Guosheng;Kwon, Young-Sam;German, Randall M. 227
Powder injection molding (PIM) is a suitable technology for the fabrication of complex shape titanium and its alloys, and has a great potential in many applications. This paper dealt with the injection molding of hydride dehydrogenization (HDH) titanium powder, spheroidized HDH titanium powder and gas atomized titanium powder. Rheological and thermalgravimetric behaviors were compared between the feedstocks of the three powders, and a tentative application of Ti PIM to eye frame temple and bridge was briefed. -
The global metal injection moulding industry is getting mature. The technology is on its way to grow from a niche technology to a widely accepted manufacturing process. This paper addresses the latest technological trends in MIM. Challenges in materials development as well as the current limits of the technology are discussed. Trends in processing like 2-component injection moulding and micro injection moulding are presented. The European MIM market situation is described and some key factors for business success are addressed. In the discussion of future business opportunities best practice examples are included.
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Aluminum Alloys with a content of 22 wt.-%
$Mg_2Si$ were spray formed. This alloy features by a low density and is therefore a superior material for leightweight applications. The main problem in spray forming of this type of alloy was the occurance of high porosities. First process optimizations have been performed to decrease porosity under a certain level, so that it can be closed by an extrusion process -
In this study, the plasma sprayed
$Al_2O_3$ and$Y_2O_3$ coatings have been investigated for applications of microelectronic components. The plasma sprayed coatings had a well-defined splatted lamellae microstructure, intersplat pores and a higher amount of microcracks within the splats. The plasma sprayed$Y_2O_3$ coating had a relatively lower hardness of 300-400Hv, compared to 650-800Hv for$Al_2O_3$ coating, and would be readily damaged by mechanical attacks such as erosion, wear and friction. For a reactive ion etching against F-containing plasmas, however, the$Y_2O_3$ coating had a much higher resistance than the$Al_2O_3$ coating because of the reduced erosion rate of by-products. -
Cold spraying is a fairly new coating technique, which within the last decade attracted serious attention of research groups and spray companies. As compared to thermal spraying, the low process temperatures in cold spraying result in unique coating properties, which promise new applications. Since particles impact with high kinetic energy in the solid state, new concepts to describe coating formation are requested to enable the full potential of this new technology. The present contribution gives a brief review of current models concerning bonding, supplying a description of the most influential spray parameters and consequences for new developments. With respect to spray forming by cold cold spraying, microstructures and thick, further machineable structures are presented.
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Nozzle geometry influences gas dynamics making sprayed particle behavior one of the most important parameters in cold spray process. Gas flows at the entrance convergent section of the nozzle takes place at relatively high temperature and are subsonic. Thus, this region is a very suitable environment for heating spray particle. In this study, numerical simulation and experiments were conducted to investigate the effect of nozzle contour, entrance geometry of nozzle and powder injection position at nozzle on the cold spray process. The process changes were observed through numerical simulation studies and the results were used to find a correlation with coating properties.
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Metal/diamond binary composite coatings on Al substrate without grit blasting were deposited by cold spray process with insitu powder preheating. Microstructural characterization of the as-sprayed coatings with different diamond size, strength and with/without Ti coating on diamond was carried out by OM and SEM. The assessment of basic properties such as tensile bond strength and hardness of the coatings, and the deposition efficiency was also carried out. Particular attention on the composite coatings was on the diamond fracture phenomenon during the cold spray deposition and the interface bonding between the diamond and the Fe-based metal matrix.
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NiTiZrSiSn bulk metallic glass powder was produced using inert gas atomization and then was sprayed onto a SS 41 mild steel substrate using the kinetic spraying process. Through this study, the effects of thermal energy of in-flight particle and crystallization degree by powder preheating temperature were evaluated. The deformation behavior of bulk metallic glass is very interesting and it is largely dependent on the temperature. The crystalline phase formation at impact interface was dependent on the in-flight particle temperature. In addition, variations in the impact behavior need to be considered at high strain rate and in-flight particle temperature.
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This paper investigates the characteristic of single-layered and multi-layered compacts made by selective laser sintering using titanium powder (TILOP45 and TILOP150, Sumitomo Titanium Corp.) There were few defects in smooth surface of laser sintered specimen in vacuum as compared to the laser sintered specimen in argon. Maximum tensile strength of singlelayered compact was about 200MPa. Multi-layered compacts show the density of around 75% and the adhesive bonding was not observed between layers, resulted in 70MPa of maximum bending strength and 50MPa of maximum tensile strength.
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A new approach to sintering loose packed, coarse aluminum alloy powder to full or near full density is presented. A controlled amount of water vapor is introduced into the sintering atmosphere, which disru pts the oxide film and allows metallurgical contact between particles. In addition, supersolidus liquid phase sintering is used to sinter the part to full density. Since the method is particularly applicable to uncompacted powders, it is potentially useful for sintering aluminum powder preforms manufactured by 3DPrinting and powder injection molding.
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Direct Metal Laser Sintering (DMLS) has been utilized for prototype manufacturing of functional metal components for years now. During this period the surface quality, mechanical properties, detail resolution and easiness of the process have been improved to the level suitable for direct production of complex metallic components for various applications. The paper will present the latest DMLS technology utilizing EOSINT M270 laser sintering machine and EOSTYLE support generation software for direct and rapid production of complex shaped metallic components for various purposes. The focus of the presentation will be in rapid manufacturing of customized biomedical implants and surgical devices of the latest stainless steel, titanium and cobalt-chromium-molybdenum alloys. In addition to biomedical applications, other application areas where complex metallic parts with stringent requirements are being needed will be presented.
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It is known that powder characteristics including particle size and distribution, particle shape, and chemical composition are important parameters which influence direct laser sintering of metal powders. In this paper, we introduce a first order kinetics model for densification of steel powders during laser sintering. A densification coefficient (K) is defined which express the potential of different powders to be laser-sintered to a high density dependent on their particle characteristics.
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The fabrication of complex-shaped parts out of Co-Cr-Mo alloy and 316L stainless steel by three-dimensional printing (3DP) was studied using two grades of each alloy with average particle size of 20 and
$75\;{\mu}m$ , respectively. To produce sound specimens, the proper 3DP processing parameters were determined. The sintering behavior of the powders was characterized by dilatometric analysis and by batch sintering in argon atmosphere at$1280^{\circ}$ for 2h. The 3DP process has successfully produced complex-shaped biomedical parts with total porosity of 12-25% and homogenous pore structure, which could be suitable for tissue growth into the pores. -
Powder library of pseudo four components Li-Ni-Co-Ti compounds were prepared for exploring the composition region with the single phase of the layer-type structure by using combinatorial high-throuput preparation system "M-ist Combi" based on electrostatic spray deposition method. The new layer-type compounds were found wider composition region than the previous report. This process is promising way to find multi component functional materials.
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3D printing of NiTi alloys has been successfully achieved. A novel printing process has been developed and used, which consists in selective deposition of a solvent on a granule bed. The granules are composed of metal powders and thermoplastic binder, which are mixed and sieved by conventional methods. A sound green strength is obtained after solvent evaporation. Sintered parts exhibit good density, proper phase composition and shape memory behaviour.
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New powder compaction process, in which a Bingham semi-solid/fluid mold is utilized, is developed to fabricate micro parts. In the present process, a powder material is filled as slurry in a solid wax mold, dried and compressed. The wax is heated during compaction and becomes semi-solid state, which can acts as a pressurized medium for isostatic compaction. Since the compacted micro parts are very fragile, the mold's temperature is controlled to higher than its melting point during unloading, to avoid breakage of the compacts. To demonstrate effectiveness of this process, some micro compacts of alumina are shown as examples.
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The behaviour of steel powder compacts during sintering has been investigated by dilatometry and X-ray computed microtomography. Dilatometry measurements showed that the anisotropic deformation results from various phenomena arising at different moments of the cycle including the delubrication stage. Microtomography provided 3D images of the microstructure induced by prior die pressing and its changes throughout sintering. Finally a schematic description of the main phenomena responsible for the deformation of metal powder compacts during sintering is proposed.
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The free sintering of metallic powders blended with non sintering inclusions is investigated by the Discrete Element Method (DEM). Each particle, whatever its nature (metallic or inclusion) is modeled as a sphere that interacts with its neighbors. We investigate the retarding effect of the inclusions on the sintering kinetics. Also, we present a simple coarsening model for the metallic particles, which allows large particles to grow at the expense of the smallest.
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The directions of further developments in the modeling of sintering are pointed out, including multi-scale modeling of sintering, on-line sintering damage criteria, particle agglomeration, sintering with phase transformations. A true multi-scale approach is applied for the development of a new meso-macro methodology for modeling of sintering. The developed macroscopic level computational framework envelopes the mesoscopic simulators. No closed forms of constitutive relationships are assumed for the parameters of the material. The model framework is able to predict the final dimensions of the sintered specimen on a global scale and identify the granular structure in any localized area for prediction of the material properties.
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Zimmerman, Darin T.;Johnson, Earnie J.;Ma, JunKun;Miskovsky, Nicholas M.;Weisel, Gary J.;Weiss, Brock L. 266
We present a systematic study of the heating and pre-sintering behavior of porous copper powder metal compacts. We employ a TE102 single mode microwave system to position the samples in the separated electric field (E) or magnetic field (H) anti-node of the cavity. We observe significant differences in the heating, pre-sintering, and microstructure evolution of the samples due to the individual fields. We note that sample history (whether heated first in the E-field or H-field) greatly effects a difference in heating trends and subsequent heating behavior and does not appear to be solely a thermal process. -
Preparation processing of sintered silicon nitride ceramics was emphatically investigated with Self-Propagating High-Temperature Synthesis (SHS) of silicon nitride prepared by ourselves as raw material. The results indicate that good sinter ability can be obtained with cheaply SHS of silicon nitride preparing silicon nitride materials. The cost of silicon nitride materials will be lowered.
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Nd-Fe-B type powder was sintered using spark plasma sintering method. Fabricated compact sintered at the temperature of
$700\;^{\circ}C$ , is found to be a composite magnet with Nd-Fe-Co-B and${\alpha}-Fe$ . The compact sintered at$700\;^{\circ}C$ shows slightly low coercivity and large remanent magnetization comparing to the compact sintered at$600^{\circ}C$ due to the formation of${\alpha}-Fe$ phase, resulting in the large maximum energy product. Maximum energy product tends to decrease with decreasing thickness of sintered compacts below 0.5 mm in thickness. -
A new process of pulsed electric current sintering was developed. It combines compaction with activated sintering effectively and can manufacture bulky nano-crystalline materials very quickly. A nano-structured steel is obtained with high relative density and hardness by this process. The average grain size of iron matrix is 58nm and the carbide particulate size is less than 100 nm. The densification temperature of ball-milled powders is approximately
$200^{\circ}C$ lower than that of blended powders. When the sintering temperature increases, the density of as-sintered specimen increases but the hardness of as-sintered specimen first increases and then decreases. -
The sintering behavior of titanium-titanium nitride nanocomposite powders has been studied by dilatometry. Titanium. titanium nitride nanocomposite powders were produced by the reactive milling of micron sized titanium powder
$(12\;{\mu}m)$ in nitrogen atmosphere. The Ti-TiN nanocomposite powders milled for various durations along with the initial micron sized Ti powders were then sintered in the temperature range of$450-1000^{\circ}C$ by a constant rate of heating$(10^{\circ}C/min)$ . The linear shrinkage, shrinkage rate, activation energy for sintering and microstructure has been studied and discussed as a function of milling time. -
In order to accelerate the sintering of Al-Bronze powder covered with passive oxide film, we focused on the way to add Al-Ca fluoride consisting of
$AlF_3$ and$CaF_2$ , examined the effect of the$CaF_2$ mixing rate in Al-Ca fluoride, the amount of the added Al-Ca fluoride and the sintering temperature on sintering properties of Al-Bronze powder and considered the mechanism of the sintering acceleration. Al-Bronze powder was sintered most effectively by adding Al-Ca fluoride with the$CaF_2$ mixing rate of 20mass%. If the amount of added fluoride was over 0.05mass% and the sintering temperature was over 1123K, the sintering acceleration of the Al-Bronze powder appears. Regarding the mechanism of the sintering acceleration, it was presumed that$Al_2O_3$ film on the surface of the Al-Bronze particles was removed in the process of the formation of gaseous AlOF by the reaction with$AlF_3$ , and the reaction was accelerated further by the presence of the liquid phase which is formed in Al-Ca fluoride. -
The increasing demand for automotive industries to reduce the weight of the vehicles has led to a growing usage of Al alloy powder metallurgy (P/M) parts. In order to control the sintered microstructure and mechanical properties of the aluminium alloy powder metallurgical (P/M) parts, it is essential to establish a fundamental understanding of the microstructural development during the sintering process. This paper presents a detailed study of the effect of temperature and initial starting materials on the evolution of microstructure during the sintering of Al-Cu-Mg-Si blends for PM.
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Powder grades pre-alloyed with 1.5-3 wt% chromium can be successfully sintered at the conventional temperature
$1120^{\circ}C$ although well-monitored sintering atmospheres are required to avoid oxidation. Mechanical properties of the Cr-alloyed PM grades are enhanced by a higher sintering temperature in the range$1120-1250^{\circ}C$ , due to positive effects from pore rounding, increased density and more effective oxide reduction. Astaloy CrM (Fe-3 wt% Cr-0.5 wt% Mo) with 0.6 wt% graphite added obtains an ultimate tensile strength of 1470 MPa and an impact strength of 31 J at density$7.1\;g/cm^3$ , after sintering at$1250^{\circ}C$ followed by cooling at$2.5^{\circ}C/s$ and tempering. -
Densification behavior of nano-agglomerate powder during pressureless sintering of Fe-Ni nanopowder was investigated in terms of diffusion kinetics and microstructural development. To understand the role of agglomerate boundary for sintering process, densification kinetics of Fe-Ni nano-agglomerate powder with different agglomerate size was investigated. It was found that activation energy for densification was lower in the small-sized agglomerate powder. The increase in the volume fraction of inter-agglomerate boundary acting as high diffusion path might be responsible for the enhanced diffusion process.
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The nano-sized Fe powders were prepared by plasma arc discharge process using pure Fe rod. The microstructure and the sintering behavior of the prepared nanopowders were evaluated. The prepared Fe nanopowders had nearly spherical shapes and consisted of metallic core and oxide shell structures. The higher volume shrinkage at low sintering temperature was observed due to the reduction of surface oxide. The nanopowders showed 6 times higher densification rate and more significant isotropic shrinkage behavior than those of micron sized Fe powders.
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Two approaches for the fabrication of tailored powder composites with specially distributed pore-grain structure and chemical composition are investigated. Electrophoretic Deposition (EPD) followed by microwave sintering is employed to obtain functionally graded materials (FGM) by in-situ controlling the deposition bath suspension composition.
$Al_2O_3/ZrO_2$ and zeolite FGM are successfully synthesized using this technique. In order to fabricate an aligned porous structure, unidirectional freezing followed by freeze drying and sintering is employed. By controlling the temperature gradient during freezing of powder slurry, a unidirectional ice-ceramic structure is obtained. The frozen specimen is then subjected to freeze drying to sublimate the ice. The obtained capillary-porous ceramic specimen is consolidated by sintering. The sintering of the graded structure is modeled by the continuum theory of sintering. -
[
$SrTiO_3$ ] is usually added as shifters in order to move the$T_C$ of$BaTiO_3$ to lower temperatures because it is well established that the$T_C$ of$BaTiO_3$ decreases linearly with a solid solution of$Sr^{+2}$ in place of$Ba^{+2}$ . It is not fully understood yet, however, how$SrTiO_3$ influences on the peak value of the dielectric constant$(\varepsilon_{max})$ at the$T_C$ of$BaTiO_3$ . This research reports the effect of$SrTiO_3$ addition on εmax at the$T_C$ of$BaTiO_3$ ceramics. Based on the chemical composition and the grain size dependence of the dielectric property of$BaTiO_3$ ceramics, functionally graded$(Ba,Sr)TiO_3$ composites were designed and fabricated. Multi-layered$(Ba,Sr)TiO_3$ composites with a compositional gradient of$SrTiO_3$ exhibited a low temperature coefficient and high dielectric constant in a wide temperature range. -
A steel/cemented carbide couple is selected to generate a tough/hard two layers material. Sintering temperature and composition are deduced from phase equilibria, and experimental studies are used to determine optimal conditions. Liquid migration from the hard layer to the tough one is observed. Microstructure evolution during sintering of the tough material (TEM, SEM, image analysis) evidences coupled mechanisms of pore reduction and WC dissolution. Liquid migration, as well as interface crack formation due to differential densification are limited by suitable temperature and time conditions.
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Laser Powder Deposition (LPD) is a technology capable of modifying a metallic structure by adding the appropriate material to perform a desired function. LPD offers a unique fabrication technique that allows the use of soft (tough) materials as base structures. Through LPD a hard material can be applied to the base material with little thermal input (minimal dilution and heat-affected-zone {HAZ}), thus providing the function of a heat treatment or other surface modifications. These surface modifications have been evaluated through standard wear testing (ASTM G-65), surface hardness (Rc), micro-hardness (vickers), and optical microscopy.
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High hardness of P/M parts can be obtained in the cooling section of the sintering furnace by using sinter hardenable materials, thus the post-sintering heat treatment can be eliminated. However, the sinter hardened materials would have difficulties in secondary machining if it is required, which will limit the applications of sinter hardenable materials in the machined parts. Recent development in warm compaction technology can enable us not only to achieve the high green density up to
$7.4\;g/cm^3$ , but also the high green strength which is needed for green machining. Therefore by using warm compaction technology, the green machining can be applied to sinter hardenable materials for the high density, strength and hardness P/M parts. In the present study, a pre-alloyed steel powder, ATOMET4601, was used by mixing with 2.0% copper, 1.0% nickel, 0.9% graphite and a proprietary lubricant using a binder treatment process - FLOMET. The specimens were compacted and green machined with different machining parameters. The machined surface finish and part integrity were evaluated in selecting the optimal conditions for green machining. The possibility of applying the green machining to the high-density structural parts was explored. -
Free-machining agent 'KSX' contains complex calcium oxide is developed. The effect of admix ratio of KSX on mechanical properties and machinability with two different cutting speeds is reported. KSX displays improved machinability without deterioration of mechanical properties up to 0.3mass% addition. It was observed that KSX is effective with a small addition of 0.1mass% at slower cutting speed, and increased of admix ratio is effective at faster cutting speed.
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Machining of sinter-hardened PM steels provides a challenge for part makers. To facilitate machining of these materials, a new additive (MA) has been developed to increase tool life during the machining process. Hard turning tests were performed to evaluate the effect of this new additive. Sintered compacts with the MA additive were compared to compacts without a machining aid and to compacts that contained the MnS additive. This paper discusses the improvement in machinability with this new additive in sinter-hardenable PM steels.
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Machinability and machining mechanism were examined in the case where resin impregnation treatment was conducted to the Mo-Co hardening particle dispersed iron-based sintered alloy. As a result, the force required for machining decreased significantly compared with the case where resin impregnation treatment was not conducted. This effect is considered to be attributable to the embrittlement of cutting chips produced by the minimization of the cut material deformation.
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The mechanical properties of ferrous powder metallurgy (P/M) materials are directly related to their microstructure. Ferrous P/M materials with sufficient hardenability will develop microstructures containing significant percentages of martensite in the as-sintered condition. Recently, sinter-hardening has developed into a highly cost effective production method through hardened P/M parts without the need for additional heat-treatments. This paper reviews the advances of sinter-hardening as well as some key processing parameters such as sintering temperature, cooling rate, tempering required to produce high quality sinter-hardened components. Specific topics including effect of alloying elements, alloying methods, and the Characterization and observation of microstructure are discussed.
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The sinter-bonding behavior of iron based powder mixtures was investigated. To produce the green compacts to be joined the following powders based on
$H{\ddot{o}}gan{\ddot{a}}s$ AB grade NC 100.24 plain iron powder were used: NC 100.24 as delivered, PNC 30, PNC 60 and NC 100.24 + 4%Cu powder mixtures. Dimensional behaviour of all those materials during the sintering cycle was monitored by dilatometry. Simple ring shaped specimens as the outer parts and cylindrical as the inner parts were pressed. The influence of parts' composition on joining strength was established. Diffusion of alloying elements: copper and phosphorous, across the bonding surface was controlled by metallography, SEM and microanalysis. -
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Porous titanium implants can be produced by powder metallurgy in combination with suitable space holder materials. Various mechanical experiments were done to characterize this material regarding the influence of the processing parameters on microstructure and mechanical properties taking into account the properties of the human bone. In this paper, the anistropic behaviour of uniaxially compacted samples was analysed in compression tests and compared to the behaviour of isostatically pressed samples. The failure of the struts of the porous titanium and the crack- initiation and -growth was examined by in-situ SEM analysis.
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The primary aim pursued by the preparation of separation membrane is the preparation of the membrane thin as well as with no defect. The field-flow fractionation deposition is a new molding technology which can overcome the traditional disadvantages such as multi-preparation to the preparation of great area of separation membrane with no defect. Therefor the mainly ingredients which influence the appearance and performance of titanium membrane layer are investigated by scanning electricity mirror (SEM) as well as porous material testing instrument: powder performance prepared and confected; selection of supporting body; sintering system such as temperature and time. It is shown that the membrane thickness can be controlled at
$50{\mu}m$ or so; the filtration precision mainly rests with powder performance and selection of supporting body and little sintering system -
The paper presents some results regarding the obtaining of some copper heat pipes with a porous copper internal layer for electronic components cooling. The heat pipes were realized by sintering of spherical copper powders of
$90{\div}125\;{\mu}m$ size directly on the internal side of a copper pipe of 18 mm in diameter. The obtained pipes were then brazed in order to obtain a heat pipe of 0.5 m in length. After that, the heat pipe was sealed and filled with a small quantity of distilled water as working fluid. To establish the total heat transport coefficient and the thermal flow transferred at the evaporator, some external devices were realized to allow the heating of the evaporator and the cooling of the condenser. Water heat pipes are explored in the intermediate temperature range of 303 up to 500 K. Test data are reported for copper water heat pipe, which was tested under different orientations. The obtained results show that the water heat pipe has a good thermal transfer performance in the temperatures range between 345 and 463 K. -
The thermal dissipation performance of sintered heat pipes is usually determined by the capillarity and permeability of the Cu powder wicks. Since the capillary provided by the Cu powder is usually large enough to draw water from the condenser end to the evaporator end, the permeability has become the controlling factor. In this study, Cu powders with different particle sizes and shapes were loosely sintered, and their permeabilities were compared. The results show that more complicated shapes, finer particle sizes, lower porosities, and rougher pore surfaces give lower permeability and thermal dissipation.
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Nano-structured ceramics, which consist of structural elements with nanometer-size crystallites, are expected to show various unusual properties. We developed the novel nano-structured ceramics which consists of
$Si_3N_4$ and TiN and a self-lubricant material. The ceramics was fabricated by powder metallurgy process using mechano-chemical grinding process and short-time sintering process. Each grain size of matrix and the self-lubricant particle was under about 50 nm and a few namometer. It showed high wear resistance and low friction coefficient by controlling of microstructure. -
The nanostructure control of
$Si_3N_4$ ceramics can be achieved by using fine starting powder and retardation of grain growth. The spark plasma sintering technique is useful to retard the grain growth by rapid heating. In the present work, the change of microstructure was investigated with emphasis on the particle size of starting powder, the amount of sintering additive and the heating schedule. The rapid heating by spark plasma sintering gave the fine microstructure consisting of equiaxed grains with the same size as starting particles. The spark plasma sintering of$Si_3N_4$ fine powder was effective to control the microstrucutre on nano-meter level. -
Using
$6wt%Y_2O_3-2wt%Al_2O_3$ as sintering additives and Si as a raw powder, the continuously porous in-situ$Si_2N_2O-Si_3N_4$ bodies were fabricated by multi-pass extrusion process and their microstructures were investigated depending on the addition of carbon (0-9wt%) in the mixture powder. The introduction of$Si_2N_2O$ fibers observed in the unidirectional continuous pores as well as in the pore-frame regions of the nitrided bodies can be an effective method in increasing the filtration efficiency. In the case of no carbon addition, the network type$Si_2N_2O$ fibers with high aspect ratio appeared in the continuous pores with diameters of 150-200 nm. However, in the case of 9wt% C addition, the fibers were found without any network type and had diameters of 200-250 nm. -
We have demonstrated that textured
$Al_2O_3-mullite-SiC$ nanocomposites can be fabricated by slip casting followed by partial oxidation - reaction sintering of mixed suspensions of$Al_2O_3$ and SiC powders in a high magnetic field. The sintered density was changed by the degree of oxidation at 1200C and 1300C. The degree of orientation of alumina in the nanocomposite was examined on the basis of the X-ray diffraction patterns and scanning electron micrographs. It is confirmed that alumina-oriented nanocomposites were fabricated. The three-point bending strength at room temperature was observed for the nanocomposites. -
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Fabrication of a nano-laminar ceramic composite by sintering thin ceramic plates was examined. Silver-coated glass flakes with a thickness of less than
$1{\mu}m$ were consolidated by pulsed current sintering or hotpressing to obtain model composites. The samples sintered at the optimum conditions were fairly dense, and the flakes were aligned by uniaxial press. The metal coating remained on the flakes through the sintering process, and became an interface layer between the flakes. No crack propagation through the transverse direction of the lamellar was observed in the indentation test. The possibilities of high resistance against crack propagation was suggested. -
The driving forces and the probable processes of WC-Co grain growth are reanalysed from recent data of interface energy and microstructure. Grain growth is driven by the disappearing of the high energy WC/WC and WC/Co interfaces with habit planes different from {0001},
${10\bar{1}0}$ and${11\bar{2}0}$ facets and by the area decrease of the WC/WC and WC/Co interfaces with {0001} and${10\bar{1}0}$ habit planes. Grain growth mainly results of dissolution-precipitation. Abnormal grains are likely formed by defects assisted nucleation. -
WC/WC interface in VC mono-doped WC-10mass%Co submicro-grained hardmetals of
$0.5\;{\mu}m$ was investigated together with WC/Co interface by using HRTEM and XMA. The thickness of V-rich layer and the analytical value of V at WC/WC interface were almost the same as those at WC/Co interfaces. These results, etc., suggested that the V-rich layers at both interfaces were not generated by an equilibrium segregation mechanism in the sintering stage, but generated by a preferential precipitation mechanism during the solidification of Co liquid phase in the cooling stage. Based on this suggestion, we succeeded in developing a nano-grained hardmetal with 100 nm$(0.1\;{\mu}m)$ . -
During sintering of cemented carbides abnormal grain growth is often observed but cannot be understood from the classical LSW-theory. A model based on 2-D nucleation of new crystalline layers and a grain-size distribution function is formulated and the equations are solved numerically. Experimental studies and computer simulations show that the initial grain size distribution has a strong effect on the grain growth behavior. For example, a fine-grained powder can grow past a coarser powder.
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The solubility of Cr in cubic carbides in the systems WC-Co-TaC and WC-Co-ZrC has been determined using equilibrium samples. Thermodynamic calculations were used to design the alloys through extrapolations of Gibbs energy expressions. The alloys were designed to have a microstructure containing the following phases: WC, liquid,
$M_7C_3$ , graphite and cubic carbide. The alloys were investigated using scanning electron microscopy and analyzed using energy-dispersive X-ray spectrometry. The present work shows how the Cr solubility depends on which cubic carbide former that is present. The WC-Co-Cr-Zr alloy has no detectable amount of Cr whereas the WC-Co-Cr-Ta alloy has 12% Cr in the cubic carbide. -
High functional micro devices are demanded in a variety of fields. For realising such demands, development of high-precision micro-components installed in the devices are needed. To achieve high-precision in the mold processing of micro-components, the development of mold materials, i.e., the development of WC-Co hardmetal with higher hardness and fracture strength is essential, together with the developments of processing technology of high precision mold and mold-forming technology of high precision micro-components, etc. The role of development of the finer submicro-grained hardmetal in a NEDO national project aiming the integrated development of these all technologies and some results are mainly explained.
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In order to develop the nano-sized WC powder that improved the hardness of hardmetals, carbothermal reduction of WO3 by C was examined by using the thermogravimetric analysis. At the direct carburization reaction path of
$WO_3{\rightarrow}WO_{2.72}{\rightarrow}WO_2{\rightarrow}W{\rightarrow}W_2C{\rightarrow}WC$ , the nano-sized grain was generated at the reaction stage$WO_{2.72}$ to$WO_2$ and W. For trial production, the intermediate products which consists of metal and carbide phases obtained by the first heating has been carburized to the final WC powder. We succeeded in the development of the WC powder of about 70nm. In addition, the nano-sized WC powder in which the vanadium of the most effective grain growth inhibitor was uniformly dispersed was developed. -
The linear intercept (LI) method was used to quantitatively measure the intercepts of WC grains in nano-grained WC-10Co hardmetal. When the surveyed intercept numbers of WC grain exceeded 200, the statistic data for the mean grain size of WC were reproduced. The discriminative minimal grain size of used LI method was 12 nm; the maximum intercept of WC grain was 109 nm; the average intercept of WC grains was 45 nm and the corresponding 3D mean grain size of WC was 70 nm which is agreeable with the XRD outcome.
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New manufacturing processes, such as thermochemical, mechanochemical and chemical vapor condensation processes have been developed to obtain nanostructured WC/Co materials. Nanoscale size WC/Co composite powders of near 100-150nm can be synthesizes by thermochemical and mechanochemical processes using water soluble precursors. Non-agglomerated and nano sized WC powder can be synthesized by the chemical vapor condensation process using metallorganic precursors as starting materials. In this paper, the scientific and technical issues on synthesis and consolidation of nanostructured WC/Co alloys produced by new chemical processes are introduced.
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The plastic deformation behavior of cemented carbides is related to the WC grain boundary strength. Ab initio calculations predict that Co and Mn segregate to WC/WC grain boundaries. To experimentally study the effect of Mn, a WC-Co-Mn material was manufactured and compared to a WC-Co material. The microstructure was studied using scanning electron microscopy (SEM), including electron backscatter diffraction (EBSD). Special attention was paid to the WC grain size and the frequency of special low-energy grain boundaries. Mn was found to have negligible effect on both the WC grain growth and the fraction of
$\sum2$ WC/WC boundaries in the as-sintered material. -
A solid stage sinterizacion model of the WC-Co is applied on this work. These results are compaired with the experimental data obtained for nanometric and micrometric sinter powder in an electric furnace and micrometric in a plasma reactor (using Abnormal Glow Discharge AGD). The correlations obtained allow the prediction of the sintering behavior in AGD for nanometric powder. The activation of the solid state sintering is shown with the decraease of the WC size and the use of AGD
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The effect of TiC content on oxidation behavior of the sintered WC-TiC-TaC alloys with 2 mass% TaC and different TiC amounts of 3-45 mass% was investigated through oxidation tests in air at 973K. As a result of the tests, it was revealed that with increasing TiC content in the alloys, mass changes caused by oxidation and thickness of the scale decreased. Thus, it is considered that the main component of the scales changed gradually from
$WO_3$ to$TiO_2$ with increasing TiC content in the alloys, and oxygen diffusion through the scale to the alloys was inhibited gradually. -
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Uchiyama, Yasuo;Ueno, Shuji;Sano, Hideaki;Tanaka, Hiroki;Nakahara, Kenji;Sakaguchi, Shigeya;Nakano, Osamu 355
WC-TiC-TaC binderless cemented carbide was oxidized under low partial pressure of oxygen (50ppm) at 873K for 1 to 20 h. Surface roughness was measured using atomic force microscope, and effect of TiC amount on oxidation behavior of the carbide was investigated. WC phase was oxidized more easily than WC-TiC-TaC solid solution phase. With an increase in TiC amount, WC-TiC-TaC phase increased and the oxidation resistance of the carbide increased. -
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Ru-C nano-composite films were prepared by MOCVD, and their microstructures and their electrode properties for oxygen gas sensors were investigated. Deposited films contained Ru particles of 5-20 nm in diameter dispersed in amorphous C matrix. The AC conductivities associating to the interface charge transfer between Ru-C composite electrode and YSZ electrolyte were 100-1000 times higher than that of conventional paste-Pt electrodes. The emf values of the oxygen gas concentration cell constructed from the nano-composite electrodes and YSZ electrolyte showed the Nernstian theoretical values at low temperatures around 500 K. The response time of the concentration cell was 900 s at 500 K.
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Nanostructured aluminum powders were obtained by means of planetary ball milling with methanol as the Process Control Agent (PCA). The behavior, during milling, was considered measuring the microhardness and grain size at different milling times. Bulk near-full density samples were sintered using the Spark Plasma Sintering technology with different schedules: temperature of
$500^{\circ}C$ and$550^{\circ}C$ , pressure of 30 MPa and 60 MPa and different modes of applying the pressure were changed in order to understand the behavior during sintering. All the samples retained their nanostructure with an increase of the grain size from about 46 up to 70-90 nm. -
Nano-structured tungsten carbide compacts with cobalt matrices (WC-Co) offer new opportunities for achieving superior hardness and toughness combinations. A unified modeling and simulation tool has been developed to produce maps of sintering pathways from nanocrystalline WC powder to sintered nano-structured WC-Co compacts. This tool includes (1) die compaction, (2) grain growth, (3) densification, (4) sensitivity analysis, and (5) optimization. All material parameters were obtained by curve fitting based on results with two WC-Co powders. Critical processing parameters are determined based on sensitivity analysis and are optimized to minimize grain size with high density.
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Nanostructured or partially amorphous Al-and Zr-based alloys are attractive candidates for advanced high-strength lightweight materials. Such alloys can be prepared by quenching from the melt or by powder metallurgy using mechanical attrition techniques. This work focuses on mechanically attrited powders and their consolidation into bulk specimens. Selected examples of mechanical deformation behavior are presented, revealing that the properties can be tuned within a wide range of strength and ductility as a function of size and volume fraction of the different phases.
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Carbon nanotubes (CNTs) have attracted remarkable attention as reinforcement for composites owing to their outstanding mechanical properties. The CNT/Cu nanocomposite is fabricated by a novel fabrication process named molecular level process. The novel process for fabricating CNT/Cu composite powders involves suspending CNTs in a solvent by surface functionalization, mixing Cu ions with CNT suspension, drying, calcination and reduction. The molecular level process produces CNT/Cu composite powders whereby the CNTs are homogeneously implanted within Cu powders. The mechanical properties of CNT/Cu nanocomposite, consolidated by spark plasma sintering of CNT/Cu composite powders, shows about 3 times higher strength and 2 times higher Young's modulus than those of Cu matrix.
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Kaygorodov, Anton;Rhee, Chang;Kim, Whung-Whoe;Ivanov, Viktor;Paranin, Sergey;Spirin, Alexey;Khrustov, Vladimir 368
By means of magnetic pulsed compaction and sintering of weakly aggregated alumina based nanopowders the jet forming nozzle samples for the hydroabrasive cutting were fabricated. The ceramics was obtained from pure alumina, as well as from alumina, doped by$TiO_2$ , MgO and AlMg. It was shown that the samples sintered from AlMg doped$Al_2O_3$ powder have the best mechanical properties and structural characteristics: relative density${\sim}0.97$ , channel microhardness. - 18-20 GPa, channel surface roughness${\sim}0.7\;{\mu}m$ , average crystallite size${\sim}1\;{\mu}m$ . -
The particulate strengthened
$Cu-MoSi_2$ composites were prepared by a PM process to develop novel copper based composites with reasonable strength, high thermal conductivity and low thermal expansion coefficient. Microstructure of the composites was investigated by SEM; the tensile strength, elongation, thermal conductivity and thermal expansion coefficient (CTE) of the composites were examined. A comparative analysis of mechanical and thermal properties of various Cu-matrix composites currently in use was given and the strengthening mechanisms for the$Cu-MoSi_2$ composites were discussed. -
Modern business trends call for miniaturization of electronic systems. One of the major impedances in this miniaturization is the conductive and inductive components in chips and circuit boards. Direct Write Technology can write these soft magnetic materials, thus allowing for further miniaturization of inductor devices. Another obstacle in electronics fabrication is the size limitations of thick screen-printing and the material limitations in ink jet printing. Direct Write Technologies address both of these limitations by providing feature sizes less than 20 microns with a wide range of materials possibilities. A discussion of the application of these nano-particulate materials by Direct Write Technologies will be presented.
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Three-dimensional artificial crystals with periodicity corresponding to terahertz wave lengths were fabricated by self-assembling monosized metal spherical particles. The metal crystals were weakly sintered to utilize them as templates. The metal templates were inverted to air spheres crystal embedded in dielectric resin though infiltration and etching. The resulting resin inverted crystals clearly presented the photonic stop gaps within terahertz wave region and the frequencies of the gaps were confirmed to agree well with calculation by plane wave expansion method.
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Lee, Seong;Noh, Joon-Woong;Kwon, Young-Sam;Chung, Seong-Taek;Johnson, John L.;Park, Seong-Jin;German, Randall M. 377
Thermal management technology is a critical element in all new chip generations, caused by a power multiplication combined with a size reduction. A heat sink, mounted on a base plate, requires the use of special materials possessing both high thermal conductivity (TC) and a coefficient of thermal expansion (CTE) that matches semiconductor materials as well as certain packaging ceramics. In this study, nano tungsten coated copper powder has been developed with a wide range of compositions, 90W-10Cu to 10W-90Cu. Powder technologies were used to make samples to evaluate density, TC, and CTE. Measured TC lies among theoretical values predicted by several existing models. -
Recently, in spindle motors for hard disk drive (HDD) devices, fluid dynamic bearings (FDB) with herringbone grooves have come to be used instead of ball bearings due to the demand for high density recording of the devices etc. In this study, a 5-lobe bearing with high bearing stiffness using a sintered material was developed, and the bearing performance was examined by simulated calculations and experiments. As a result, it was clarified that the 5-lobe bearing had the required performance for practical use in the spindle motor for HDD
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A comparative study is made on root bending fatigue performance of spur gears and plane bending fatigue performance of notched test bars. R = 0 root bending fatigue tests are made on small spur gears with critical root radius 1.0 mm. The results are compared to plane bending fatigue tests of 0.9 mm radius notched specimens. Results are presented for tests on 4%Ni/2%Cu/1.5%Mo prealloyed PM steel with addition of about 0.6% graphite. Predicted values from the test bars coincide well with the results obtained from the gear root fatigue tests.
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Fe-4Ni-0.5Mo-1Cu powder was selected as raw material, pressed and sinter-hardened at
$1135\;^{\circ}C$ for 30 min with rapid cooling. The density varies in the range of$7.24-7.29\;g/cm^3$ . Its fatigue properties have been tested in axial loading of alternating tensile/compressive stress at R=-1 with a servo-pulse pump. The fatigue endurance limit was measured to be 260 MPa. The microstructure showed more homogeneous bainite and martensite. Fractography displayed the fatigue cracks initiated from the pore areas near the surface. A non-typical ductile fatigue striation was found. More dimples occurred on fracture surface due to the plastic deformation, which can prohibit cracking propagation and improve its fatigue properties. -
For attaining optimum fatigue resistance of PM steels, high density levels are necessary. In this work, sintered steels Fe-1.5%Mo-0.6%C and Fe-1.5%Cr-0.2%Mo-0.6%C were produced with density levels of 7.1 to
$7.6\;g.cm^{-3}$ . Ultrasonic fatigue testing with 20 kHz was performed in push-pull mode up to 10E9 cycles. It was shown that the fatigue endurance strength is strongly improved by higher density levels, but also higher sintering temperatures are beneficial. The Cr-Mo steels proved to be superior to the plain Mo alloyed, due to a more favourable as-sintered matrix microstructure. -
The influence of porosity (P) on Young's modulus (E) and Poisson's ratio
$(\upsilon)$ of sintered steels produced from four types of steel powders was investigated. The values of E and$(\upsilon)$ depend mainly on the value of P, and those were a little affected by alloying elements. The relationships between E,$(\upsilon)$ , and P were described as following equations:$E\;=\;E_0{\cdot}(1\;-\;k_E{\cdot}P)^2$ and$\upsilon\;=\;({\upsilon}_0\;-\;\upsilon_{sub}){\cdot}(1\;-\;k_{\upsilon}{\cdot}P)2+\upsilon_{sub}$ , where subscript 0 means P = 0, and$k_E,\;k_{\upsilon}$ and${\upsilon}_{sub}$ are empirical constants. These approximate equations showed good agreement with empirical results. -
Selective surface densification is a tool for improving the mechanical properties of PM steels, such that the requirements for highly loaded gears can be matched. This paper describes the manufacturing and the properties of a helical P/M gear. The gear performance was evaluated on a 3-shaft back to back test rig, on a load bearing test rig and on a sound test bench. The results of these tests are presented and compared to data obtained from solid steel gear with identical geometry and surface quality. This comparison indicates that P/M gears have a load bearing capacity and noise level which are both well comparable to solid steel gears.
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Sintered materials have been applied widely in Valve Seat Inserts (VSI). The amount of wear on VSIs increases when used in gas (LPG, CNG) engines because of their dry environments. In this paper, two newly developed high performance VSI materials for gas engines are introduced. These materials applied new techniques, which are both high performance hard particle and new distribution method of solid lubricant, to increase wear resistance.
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Highly compressible Ni-Mo steels are attractive materials for PM due to high sinter density and ease of processing. Extra-fine Ni admixed PM steels have demonstrated improved mechanical properties and rolling contact fatigue resistance due to a more uniform microstructure and increased Ni diffusion during sintering. Sinter densities of single press single sinter XF Ni-Mo steels can approach
$7.5\;g/cm^3$ at moderate compaction pressures. Leaner alloys based on extra-fine Ni powder are possible depending on the performance requirements of the PM steel part. Extra-fine Ni steels are particularly attractive for the growing market of high performance PM gears and sprockets. -
To manufacture a flange for a compressor with a relief groove by using powder metallurgy in order to prevent deformation to the compressor in operation, powder material for the flange is charged into a mold; an ablative member having a melting point lower than that of the powder material is positioned at a place where a relief groove is to be formed; the flange is formed by compressing the powder material and the ablative member; and the formed flange is sintered at a temperature between the melting point of the powder material and the ablative member so as to melt and remove the ablative member. It made according to the new method has more excellent strength and airtight property than the conventional one. It is analyzed that the ablative member is melted and penetrated into the flange structure during the sintering process, which results in improvement of the airtight property and increase of the strength.
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In late years, from a trend for ecology of auto motive engine, low emission and low fuel consumption of engine become a social assignment. At the same time, the high output (high efficiency) is required, too. In order to meet those requirements, in comparison with conventional engines, lean A/F (Air fuel ratio) setting is becoming popular for the high performance engines of late years. Exhaust valve seat (sintered material) used in these engines has a problem in wear resistance, because it is exposed to the surroundings that is clean and a high temperature in comparison with the conventional engines. Therefore, wear mechanism with lean A/F of engine was analyzed.The exhaust valve seat (sintered material), that was superior in wear resistance, was developed.
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M390 microclean(R) of
$B{\ddot{o}}hler$ Edelstahl is a powder metallurgical plastic mould steel with a high level of corrosion and wear resistance and therefore often used in the plastics processing industry. But as a consequence of rapidly advancing developments in the plastics processing industry the required level of wear resistance of tool steels in this field is constantly rising. For that reason a new PM tool steel with higher hardness values and an increased amount of primary carbides has been developed to improve the resistance against abrasive and adhesive wear. The wear resistance of both steels against adhesive situations for components of the plastification unit of injection moulding machines has been tested with a novel method. In case of processing polyolefins with an injection moulding machine it was found that there is adhesive wear between the check-ring and the flights of the screw tip of the non-return valve under certain circumstances. The temperature in that region was measured with an infrared temperature sensor. The existence of significant peaks of that signal was used as an indicator for an adhesive wear situation. -
All-surface, all-tooth machining and roll forming of cast iron have been used to manufacture the crankshaft position sensor wheel (CPSW). However, these methods pose many problems such as difficult processing, high material cost, and low tooth precision. Thus, we developed a sintered CPSW with an improved detection ability in order to resolve the problems related with the previous methods of manufacturing CPSW by simplifying the process flow and improving tooth precision. The sintering process is introduced in this study. We conducted an experiment to compare the sintered and roll formed products and analyzed the results to evaluate the reliability of the sintering process. Furthermore, we compared and analyzed stress and displacement in the sintered and roll formed products through the "Finite Element Method(FEM)". According to the experimental and FEM results, the sintered product showed satisfactory mechanical properties. It was less expensive to process and lighter and showed better quality than the roll formed product. The results of this study could be applied to design an optimum CPSW using the sintering process.
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Sintered materials have been applied widely in Valve Seat Inserts (VSI). The demands for VSIs are not only good heat and wear resistance but also good machinability. The sintered materials, which are made of a mixture of manganese containing iron powder and certain types of sulfide powder, have superior machinability due to precipitation of the fine MnS particles in the matrix. This report introduces a new VSI material, which has both superior machinability, and wear resistance due to applies of this "MnS precipitation" technique.
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Raw materials from different sources, produced by a given process and having equal chemical composition, are supposed to be equivalent. The differences in sintering behavior have been investigated on P/M steels obtained from four diffusion-bonded powders (Fe + Ni + Cu + Mo) on atomized iron base, at the same alloy contents. Two levels of carbon and two sintering conditions have been investigated. Dimensional changes, C content, hardness, microhardness pattern, universal hardness, fractal analysis, pore features, microstructure features, and rupture strength have been compared to characterize different raw materials. The results show that the claimed equivalence is not confirmed by experimental data.
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Dimensional precision is a critical parameter in net shape processing of ferrous PM components. Sinter-hardening alloys undergo a transformation from austenite to martensite. Martensite formation expands the sintered compact, while tempering hardened steels results in shrinkage. In addition, martensitic regions with high Cu and C contents may contain large amounts of retained austenite. The presence of martensite and retained austenite, in addition to the tempering step, all play a role in the final dimensions of a component. This paper investigates the dimensional and microstructural changes to two sinter-hardening grades through different post-sintering thermal treatments.
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New applications for PM have resulted in a substantial market growth during the last decades. The clue to these components lies in the utilization of new powders and component production processes. In order to reduce development time and increase the probability for success it is essential to work in close cooperation within the whole chain from powder supplier to component supplier and component user.
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A high nitrogen PM tool steel has shown to have an excellent galling resistance due to the introduction of a high amount of a low friction phase predominantly consisting of VN. Tool making and heat treatment are according to standard procedures. An increase of tool life of more than two times compared to ordinary tool steels is found. Furthermore, the new low friction tool steel shows a potential for sintered parts with higher densities through the applica bility of increased compaction pressure or minimized lubricant amount.
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The effects of several experimental parameters on the formation of stable Ni nanoparticles dispersion were investigated. The suspensions of Ni nanoparticles were produced in organic solvents using Hypermer KD-2 as a dispersant. The transmission profiles, particle size distribution, zeta potential, and visual inspection results were used to discuss the stability of the dispersion. The optimal conditions for the formation of stable dispersion are evaluated.
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Nanostructured ceria powder was synthesized by a thermochemical process and investigated its applicability for an oxygen gas sensor. An amorphous precursor powders prepared by spray drying a cerium-nitrate solution were transformed successfully into nanostructured ceria by heat-treatment in air atmosphere. The powders were a loose agglomerated structure with extremely fine
$CeO_2$ particles about 15 nm in size, resulting in a very high specific surface area$(110\;m^2/g)$ . The oxygen sensitivity and the response time$t_{90}$ measured at sintered sample at$1000^{\circ}C$ was about -0.25 and very short, i.e.,$3{\sim}5$ seconds, respectively. -
In the present, the focus is on the synthesis of nanostructured TiC/Co composite powder by the spray thermal conversion process using titanium dioxide powder has an average particle size of 50 nm and cobalt nitrate as raw materials. The titanium-cobalt-oxygen based oxide powder prepared by the combination of the spray drying and desalting methods. The titanium-cobalt-oxygen based oxide powder carbothermally reduced by the solid carbon. The synthesized TiC-15wt.%Co composite powder at 1473K for 2 hours had an average particle size of 150 nm.
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In the present study, ultrafined Zr-V-Fe based alloy powder prepared by a plasma arc discharge process with changing process parameters. The chemical composition of synthesized powder was strongly influenced by the process parameters, especially the hydrogen volume fraction in the powder synthesis atmosphere. The synthesized powder had an average particle size of 50 nm. The synthesized Zr-V-Fe based particles had a shell-core structure composed of metal in the core and oxidse in the shell.
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Ultrasonic-milling of metal oxide nanopowders for the preparation of tungsten heavy alloys was investigated. Milling time was selected as a process variable. XRD results of metal oxide nanopowders ultrasonic-milled for 50 and 100h showed that mean crystallite size reduced with increasing milling time and there was no evidence of contamination or change of composition by impurities. It was found that nanocomposite powders reduced at
$800^{\circ}C$ in$H_2$ atmosphere had a composition of 93.1W-4.9Ni-2.0Fe by EDX analysis. Hardness of sintered samples of 50 and 100h was 390 and 463 Hv, respectively, which corresponds to the hardness of commercial products. -
The effects of reaction temperature and precursor concentration on the microstructure and magnetic properties of
${\gamma}-Fe_2O_3$ nanoparticles synthesized as final products of iron acetylacetonate in chemical vapor condensation (CVC) were investigated. Pure${\gamma}-Fe_2O_3$ phase was obtained at temperature above$900^{\circ}C$ and crystallite size of${\gamma}-Fe_2O_3$ nanoparticles decreased with lowering precursor concentration. Also, the coercivity decreases with decreasing crystallite size of nanopowder. The lowest coercivity was 7.8 Oe, which was obtained from the${\gamma}-Fe_2O_3$ nanopowder sample synthesized at precursor concentration of 0.3M. Then, the crystallite size of${\gamma}-Fe_2O_3$ nanoparticles was 8.8 nm. -
Mono-sized silicon particles were effectively fabricated by a novel way named pulsated orifice ejection method (POEM). The particles are with very narrow particles size distribution and very small standard deviation of mean particle size. There are two different types spherical silicon particles were found. One consists of many grains mainly in random boundaries. The other consists of two or three grains with only twin orientation relationships, even single crystal in cross-section was also found within this type of spherical silicon particles.
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Aluminum hydroxides were synthesized by a simple electrolytic reaction of aluminum plates. The aluminum monohydroxide, boehmite(AlO(OH)), was predominantly formed by the application of an electrical potential above 30V, while the mixture of the bayerite
$(Al(OH)_3)$ and boehmite(AlO(OH)) phases were formed below 20V. The boehmite has a clear fibrous structure which is controlled on a nanometer scale. On the contrary, the bayerite consists of the typical hourglass or semi-hourglass shaped coarse crystals as a result of an aggregation of the various crystals stacked together. The specific surface area of the boehmite nanofiber was remarkably high, reaching about$300m^2/g$ . -
Thermoelectric thick film was fabricated by screen printing process with using p-type Bi-Te-Sb powders. The powder was synthesized by melting, milling and sintering process and hydrogen reduced to enhance the thermoelectric property. The thick film of Bi-Te-Sb powder was fabricated by screen printing method and baked at the optimized conditions. The thermal conductivity, the electrical resistivity and Seeback coefficient of thick film were measured and the thermoelectric performance was analyzed in terms of film characteristics and its microstructure. Finally, the feasibility of thermoelectric thick film into micro cooling device on CPU chip was discussed in this study.
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Monosized germanium micro particles are prepared by a newly developed Pulsated Orifice Ejection Method. The obtained particles are categorized into two kinds of the microstructures as refined and coarse ones. The morphological difference is estimated to be determined by the undercooling level during nucleation. Actually, the increase in the temperature of the melt was effective in coarsening the microstructure, because the temperature of the melt intensely relates to the undercooling level. The transition temperature of coarse and refined microstructures is found to be 1300-1350K. Furthermore, a triggered nucleation could improve the crystallinity of the particles in the short separation.
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The
$Ag/TiO_{2-x}N_x$ nanoparticles were synthesized by photochemical deposition in a$TiO_{2-X}N_X$ suspension system. The prepared products were characterized by means of XRD, Uv-vis and photoluminescence spectra (PL). Its photocatalytic activity was investigated by the decomposition of methylene blue (MB) solution under illumination of visible and ultraviolet light, respectively. Compared to$TiO_{2-x}N_x$ , the photocatalytic activity of the as-prepared$Ag/TiO_{2-x}N_x$ is obviously enhanced due to the decreasing recombination of a photoexcitated electron-hole pairs. The Mechanism in which photocatalytic activity is enhanced has been discussed in detail. -
Pure and stable YAG
$(Y_3Al_5O_{12})$ powders were synthesized by a PVA (polyvinyl alcohol) polymer solution technique. PVA was used as an organic carrier for the precursor ceramic gel. The precursor gels were crystallized to YAG at relatively a low temperature of$900\;^{\circ}C$ . The synthesized powders, which have nano-sized primary particles, were soft and porous, and the porous powders were ground to sub-micron size by a simple ball milling process. The ball-milled powders were densified to 94% relative density at$1500\;^{\circ}C$ for 1h. In this study, the characteristics of the synthesized YAG powders were examined. -
Several titanate powders (
$Al_2TiO_5,\;SrTiO_3$ , etc.) were synthesized by an ethylene glycol solution route. Titanium isopropoxide and nitrate salts were dissolved in stoichiometric proportions in liquid-type ethylene glycol without any precipitation. The parent precursor sols were dried to porous gels, and then the gels were calcined and crystallized. All synthesized titanate powders had stable crystallization behavior at low temperature and high specific surface area after a simple ball-milling process. A three-component PZT$(Pb(Zr_{0.52}{\cdot}Ti_{0.48})O_3)$ powder was also synthesized successfully by the ethylene glycol method. In this study, the characteristics of the multi-component titanate powders by the ethylene glycol method are examined. -
Vacuum carbonization of nanometer tungsten powder was investigated in a simple designed apparatus. An X-Y recorder was used to plot differential thermal analysis (DTA) curves to determine starting temperature of carbonization of four samples with different specific surface area. The product was detected by X-ray Diffraction (XRD) and small angle X-ray scattering (SAXS). The results show that finer tungsten powder has lower starting temperature of carbonization. Tungsten powder, which BET surface area is
$32.97m^2/g$ , is completely carbonized to tungsten carbide at$1050^{\circ}C$ , although the starting temperature is$865^{\circ}C$ . Particle grows sharply before carbonization. -
Flying trajectories of fine particles within a size range of
$10{\sim}60{\mu}m$ were studied during centrifugal atomizing processes. A FORTRAN program was written by using increment method. Calculation results revealed that the drag force might reach very high value of 522-7800 g for fine powder of$10{\sim}60{\mu}m$ . Flying distance in horizontal direction could be shortened if the particles fly obliquely due to the huge drug force. On the other hand, very fine powder could be projected to far distances when the atmosphere flow velocity is much stronger. Fortunately such particles could be contracted within a cylinder closed to the atomizer when the atmosphere flow was weaken or retained in a limited diameter. -
Magnetic oxide-coated iron nanoparticles with the mean size ranging from 6 to 75 nm were synthesized by aerosol method using iron carbonyl as a precursor under the flowing inert gas atmosphere. Oxide shells were formed by passivation of asprepared iron particles. The influence of experimental parameters on the nanoparticles' microstructure, phase composition and growth behavior as well as magnetic properties were investigated and discussed in this study.
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This paper described the preparation method for composing high-grade synthetic diamond by water atomizing using FeNi30 powder catalyst. The objective of this article is about powder making process using super high water atomizing in the atmosphere of inert gas, and then corroded the powder with a corrosion inhibitor. Finally, FeNi30 catalyst powder with lower oxygen content and good sphericity is produced. The experiment of making diamonds by using cubic press and the performance of the diamonds are also discussed.
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The influence of Hi-flux powders characteristics on the performance of magnetic powder cores was studied. It was found that different cooling rate and nozzle configuration could change the shape and microstructure of powders. Smooth surface and spherical shape of powders were beneficial to improve DC bias performance and reduce core losses of magnetic powder core.
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We have demonstrated that textured
$Al_2O_3-mullite-SiC$ nanocomposites can be fabricated by slip casting followed by partial oxidation. reaction sintering of mixed suspensions of$Al_2O_3$ and SiC powders in a high magnetic field. The sintered density was changed by the degree of oxidation at 1200C and 1300C. The degree of orientation of alumina in the nanocomposite was examined on the basis of the X-ray diffraction patterns and scanning electron micrographs. It is confirmed that aluminaoriented nanocomposites were fabricated. The three-point bending strength at room temperature was observed for the nanocomposites. -
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N-type
$Bi_2Te_3-Sb_2Te_3$ solid solutions doped with 1$CdCl_2$ was prepared by melt spinning, crushing and vacuum sintering processes. Microstructure, bending strength and thermoelectric property were investigated as a function of the doping quantity from 0.03wt.% to 0.10wt.% and sintering temperature from$400^{\circ}C$ to$500^{\circ}C$ , and finally compared with those of conventionally fabricated alloys. The alloy showed a good structural homogeneity as well as bending strength of$3.88Kgf/mm^2$ . The highest thermoelectric figure of merit was obtained by doping 0.03wt.% and sintering at$500^{\circ}C$ . -
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Monodispersed and nano-sized Ni powders were synthesized from aqueous nickel sulfate hexahydrate
$(NiSO_4{\cdot}6H_2O)$ inside nonionic polymer network by using wet chemical reduction process. The sucrose was used as a nonionic polymer network source. The effect of reaction conditions such as the amount of sucrose and a various reaction temperature, nickel sulfate hexahydrate molarity. The influence of a nonionic polymer network on the particle size of the prepared Ni powders was characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and particle size analysis (PSA). The results showed that the obtained Ni powders were strong by dependent of the reaction conditions. In particular, the Ni powders prepared inside a nonionic polymer network had smooth spherical shape and narrow particle size distribution. -
Monodispersed and nano-sized Cu powders were synthesized from copper sulfate pentahydrate
$(CuSO_4{\cdot}5H_2O)$ inside a nonionic polymer matrix by using wet chemical reduction process. The sucrose was used as a nonionic polymer network source. The influences of a nonionic polymer matrix on the particle size of the prepared Cu powders were characterized by means of X-ray diffraction), scanning electron microscopy), and particle size analysis). The smallen Cu powders with size of approximately 100 nm was obtained with adding of 0.04M sucrose at reaction temperature of$60\;^{\circ}C$ . The particle size of the Cu powders prepared by the reduction inside polymer network was strongly dependent of the sucrose content and reaction temperature. -
The anatase particle was facetted at the free surface and a neck formation between the anatase particles prior to the phase transformation occured. This resulted in the severe lattice distortion at the region of the interface near the neck and this can act as the nucleation sites for the phase transformation. The grain growth of rutile particles after the phase transformation grew very fast by the sweeping phenomena of grain boundary. Therfore, It leaded to the microstructure without the rutile phase located in anatase particle.
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[
$TiO_2$ ] nanoparticle was synthesized by the flame method, which was controlled by varying the ratio and flow rate of gas mixtures consisting of oxygen (oxidizer), methane (fuel) and nitrogen (carrier gas). The crystalline phases of$TiO_2$ nanoparticle depended strongly on the temperature distribution in the flame, whereas the morphology was not sensitive. We proved that the anatase phase formed without the phase transformation in the flame and the rutile phase generated through several phase transformations. -
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Maghemite and hematite nanospheres were synthesized by using the Sol-gel technique. The structural properties of these nanosphere powders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and pore size distribution. Hematite phase shows crystalline structures. The mean particle size that resulted from BET and XRD analyses were 4.9 nm and 2 nm. It can be seen from transmission electron microscopy that the size of the particles are very small which is in good agreement with the FESEM and the X-ray diffraction. The BET and pore size method were employed for specific surface area determination.
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Using microwave synthesized HAp nano powder and polymethyl methacrylate (PMMA) as a pore-forming agent, the porous biphasic calcium phosphate (BCP) ceramics were fabricated depending on the sintering temperature. The synthesized HAp powders was about 70-90 nm in diameter. In the porous sintered bodies, the pores having
$150-180\;{\mu}m$ were homogeneously dispersed in the BCP matrix. Some amounts of pores interconnected due the necking of PMMA powders which will increase the osteoconductivity and ingrowth of bone-tissues while using as a bone substrate. As the sintering temperature increased, the relative density increased and showed the maximum value of 79.6%. From the SBF experiment, the maximum resorption of$Ca^{2+}$ ion was observed in the sample sintered at$1000^{\circ}C$ . -
Close-coupled atomizers are of great interest and controlling their performance parameters is critical for metal powder producing and spray forming industries. In this study, designed close-coupled nozzle systems were used to investigate the effect of the nozzle types and protrusion length of the melt delivery tube on the pressure formation at the melt delivery tube tip. The observed metal flow rate was not behaving as what was earlier assumed, namely that, deeper aspiration enhanced metal flow rate. Higher aspiration pressure at the tip of the melt delivery tube increases the stability of atomization process.
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The n-type
$(95%Bi_2Te_3-5%Bi_2Se_3)$ compound was newly fabricated by gas atomization and hot extrusion, which is considered to be a mass production technique of this alloy. The effect of powder size on thermoelectric properties of 0.04%$SbI_3$ doped$95%Bi_2Te_3-5%Bi_2Se_3$ alloy were investigated. Seebeck coefficient$({\alpha})$ and Electrical resistivity$(\rho)$ increased with increasing powder size due to the decrease in carrier concentration by oxygen content. With increasing powder size, the compressive strength of$95%Bi_2Te_3-5%Bi_2Se_3$ alloy was increased due to the relative high density. The compound with${\sim}300\;{\mu}m$ size shows the highest power factor among the four different powder sizes. The rapidly solidified and hot extruded compound using$200[\sim}300{\mu}m$ powder size shows the highest compressive strength. -
Synthesis of iron nanopowder by room-temperature electrochemical reduction process of
${\alpha}-Fe_2O_3$ nanopowder was investigated in terms of phase evolution and microstructure. As process variables, reduction time and applied voltage were changed in the range of$1{\sim}20$ h and$30{\sim}40$ V, respectively. From XRD analyses, it was found that volume of Fe phase increased with increasing reduction time and applied voltage, respectively. The crystallite size of Fe phase in all powder samples was less than 30 nm, implying that particle growth was inhibited by the reaction at room temperature. Based on the distinct equilibrium shape of crystalline particle, phase composition of nanoparticles was identified by TEM observation. -
The process of coprecipitation of biocomposite hydroxyapatite/chitosan from aqueous solution at low temperature in alkali environnement was examined. We have shown that initially we have the formation of amorphous octocalcium phosphates
$(Ca_8(HPO_4)(PO_4)_5,\;nH_2O:\;OCP)$ and the transferring from OCP to amorphous calcium phosphate$(Ca_9(PO_4)_3,\;nH_2O:\;TCP)$ , and then from TCP to calcium-deficient hydroxyapatite$(Ca_{10-X}\;(HPO_4)_X(PO_4)_{6-x}(OH)_{2-X}\;:\;ACP)$ and hydroxyapatite$(Ca_{10}(PO_4)_6(OH)_2\;:\;HAP)$ . The transformation of ACP to HAP was inhibited in the presence of chitosan. The result suggests that there is an affinity binding between ACP and chitosan and subsequently blocking the active growth site of ACP. -
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Novel bisphenol-based wholly aromatic poly(ether sulfone-ketone) copolymer containing pendant sulfonate groups were prepared by direct aromatic nucleophilic substitution polycondensation of 4,4-difluorobenzophenone, 2,2'-disodiumsulfonyl-4,4'-fluorophenylsulfone (40mole% of bisphenol A) and bisphenol A. Polymerization proceeded quantitatively to high molecular weight in N-methyl-2-pyrrolidinone at
$180^{\circ}C$ . Organic-inorganic composite membranes were obtained by mixing organic polymers with hydrophilic$SiO_2$ (ca. 20nm) obtained by sol-gel process. The polymer and a series of composite membranes were studied by FT-IR,$^1HNMR$ , differential scanning calorimetry (DSC) and thermal stability. The proton conductivity as a function of temperature decreased as$SiO_2$ content increased, but methanol permeability decreased. The nano composite membranes were found to posse all requisite properties; Ion exchange capacity (1.2meq./g), glass transition temperatures$(164-183\;^{\circ}C)$ , and low affinity towards methanol$(4.63-1.08{\times}10^{-7}\;cm^2/S)$ . -
Branched sulfonated poly(ether sulfone-ketone) copolymer was prepared with bisphenol A, 4,4-difluorobenzophenone, sulfonated chlorophenyl sulfone (40mole% of bisphenol A) and THPE (1,1,1-tris-p-hydroxyphenylethane). THPE was used 0.4 mol% of bisphenol A to synthesize branched copolymers. Organic-inorganic nano composite membranes were prepared with copolymer and a series of
$SiO_2$ nanoparticles (20 nm, 4, 7 and 10 wt%). The composite membranes were cast from dimethylsulfoxide solutions. The films were converted from the salt to acid forms with dilute hydrochloric acid. The membranes were studied by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Sorption experiments were conducted to observe the interaction of sulfonated polymers with water and methanol. Branched copolymer and nano composite membranes exhibit proton conductivities from$1.12{\times}10^{-3}$ to$6.04{\times}10^{-3}\;S/cm^2$ , water uptake from 52.9 to 62.4%, IEC from 0.81 to 1.21 meq/g and methanol diffusion coefficients from$1.2{\times}10^{-7}$ to$1.5{\times}10^{-7}\;cm^2/S$ . -
The horizontal high energy rotor ball mill (
$Simoloyer^{(R)}$ ) is used to break and activate dry solids. It is used for dry-milling and in the vertical mount for wet-milling in leaching processes. Technical electric arc furnace (EAF) dust with high contents of zinc oxide, zinc ferrite and magnetite is efficiently separated by ambient temperature leaching. The process shows promise for industrial application -
Chip breaker of cutting tool is an important feature to enhance cutting performance. Powder injection molding process was used to produce a triangular-shape cermet grooving insert which has three chip breakers. Attrition milled cermet powders were mixed with wax-based binder system in continuous twin screw extruder. Three-plate injection mold with slide cores was used to produce injection-molded parts. After molding, solvent and thermal debinding was carried out. Sintering was conducted in a batch furnace with a graphite heater. The sintered parts satisfy the requirements of dimensional tolerances and material properties.
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The kneading process and formulations of feedstock obviously affect the quality of MIM products. In the present work, the rheological behaviour of the composite MIM feedstock, metal matrix (Cu) with few additions of ceramic powders
$(Al_2O_3)$ , was measured by a self-designed/manufactured simple capillary rheometer. Experimental results show that the distribution between powders and binder is more uniformly when blending time increased. Though high powder loading will increase the feedstock viscosity, the fluidity reveals relatively stable through the load curves of extrusion. Besides, the temperature-dependence of viscosity of the feedstock approximately follows an Arrehnius equation. Basing on Taguchi's method, the kneading optimization conditions and the rheological model of the feedstock were established, respectively. -
Powder Injection Molding (PIM) has recently been recognized as an advanced manufacturing technology for low-cost mass production of metal or ceramic parts of complicated geometry. With this regards, design technology of dental scaler tip PIM mold, which has complex shape, with the help of computer-aided analysis for powder injection molding process was developed. Compter aided analysis results, such as filling pattern, weldline formation, and air vent position prediction were investigated and eventually showed good agreements with experimental results.
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With the capability of net shaping for complex 3D geometry, powder injection molding (PIM) is widely used for automotive parts, electronics and medical industry. In this study, an ultrasonic dental scaler tip produced by machining process was redesigned for the PIM process. An injection mold was designed and machined to produce the dental scaler tip by the PIM process.
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The present investigation has been performed on full densification behavior and mechanical property of the powder injection molded Fe-8wt%Ni nanoalloy powder. The net shaping process of the nanopowder was conducted by powder injection molding (PIM) process. The key-process for fabricating fully densified net-shaped nanopowder by pressureless sintering is an optimal control of agglomerate size of nanopowder. Enhanced mechanical property of PIMed Fe-Ni nanopowder is explained by grain refinement and microstructural uniformity.
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The MIM technology is an alternative process for fabricating near net shape components that usually uses gas atomised powders with small size
$(<\;20\;{\mu}m)$ and spherical shape. In this work, the possibility of changing partially or totally spherical powder by an irregular and/or coarse one that is cheaper than the former was investigated. In this way, different bronze 90/10 components were fabricated by mixing three different types of powder, gas and water atomised with different particle sizes, in order to evaluate how the particle shape and size affect the MIM process. -
This study is focused on the manufacturing technique of powder injection molding of watch case made from zirconia powder. A series of computer simulation processes were applied to the prediction of the flow pattern in the inside of the mould and defects as weld-line. The material properties of melted feedstock, including the PVT graph and thermal viscosity flowage properties were measured to obtain the input data to be used in a computer simulation. Also, a molding experiment was conducted and the results of the experiment showed a good agreement with the simulation results for flow pattern and weld line location. On the other hand, gravity and inertia effects have an influence on the velocity of the melt front because of the high density of ceramic powder particles during powder injection molding in comparison with polymer's injection molding process. In the experiment, the position of the melt front was compared with the upper gate and lower gate positions. The gravity and inertia effect could be confirmed in the experimental results.
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In this communication the development of a new metal injection moulding (MIM) system for duplex stainless steels is presented. The metal powders were prepared by premixing 316L and 430L stainless steels gas atomised powders in a ratio of 50:50. The binder used to prepare the feedstock was composed by HDPE and paraffin wax. Torque measurements of the mixture indicated that the maximum amount of metal was 68 vol%. The polymeric part was driven off by thermal debinding and the sintering was performed in low vacuum. The final densities were close to the theoretical ones.
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Correlations between in-flight particle, splat and coating microstructure of thermally sprayed Ni20Cr were investigated. Flame spray and arc spray systems were employed for spraying Ni20Cr powder and Ni20Cr wire, respectively. The results showed that the arc spray process produced a broader size distribution for both in-flight particles and splats compared to flame process. Flower-like splat morphology was obtained from the arc spray whereas a pancake-like splat was obtained by flame spray. Ni20Cr coating sprayed by arc process had a denser microstructure, lower porosity and better adhesion at the interface.
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Tungsten coatings with different interlayers onto the oxygen-free copper substrates were fabricated by atmosphere plasma spraying. The effects of different interlayers of NiCrAl, NiAl and W/Cu on bonding strength were studied. SEM, EDS and XRD were used to investigate the photographs and compositions of these coatings. The tungsten coatings with different initial particle sizes resulted in different microstructures. Oxidation was not detected in the tungsten coating, but in the interlayer, it was found by both XRD and EDS. The tungsten coating deposited directly onto the copper substrate presented higher bonding strength than those with different interlayers.
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In this study, multi-ply SiC fiber reinforced Ti-6Al-4V composites have been manufactured by plasma spraying and subsequent vacuum hot pressing. Two different sizes of Ti-6Al-4V feedstock powders were used for plasma spraying to form matrix. A considerable amount of oxygen was incorporated into as-sprayed Ti matrix during plasma spraying, and consequently caused matrix embrittlement. The use of coarse-sized feedstock powder reduced oxygen contamination, but tended to increase fiber spacing irregularity and fiber strength degradation. Longitudinal tensile strength and ductility of the composites were mainly affected by the matrix oxygen content.
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A connection between pulse-periodical laser radiation power and stability of liquid-metal contacts between powder particles during selective laser sintering (SLS) is determined based on analysis solving the problem of stability of liquid column in the gravity and capillary forces field. On the grounds of obtained relationships the optimization of pulse-periodical laser radiation power and SLS-process duration is realized, that allows to produce voluminous powder porous materials with pre-determined physical and mechanical properties and surface geometry. Results of metallographic investigations of powder porous materials of titanium powder produced with technological regimes calculated by means of obtained relationships are given in the work
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Laser additive direct deposition of metals is a new rapid manufacturing technology, which combines with computer aided design, laser cladding and rapid prototyping. The advanced technology can build fully-dense metal components directly from CAD files with neither mould nor tool. Based on the theory of this technology, a promising rapid manufacturing system called "Laser Metal Deposition Shaping (LMDS)" is being developed significantly. The microstructure and mechanical properties of the LMDS-formed samples are tested and analyzed synthetically. As a result, significant processing flexibility with the LMDS system over conventional processing capabilities is recognized, with potentially lower production cost, higher quality components, and shorter lead time.
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The
$TiB_2$ dispersion strengthened copper alloy was attracted as thermal and electrical functional material for the high mechanical strength, high thermal stability and good conductivity of$TiB_2$ . In the present study, the focus is on the synthesis of$TiB_2$ dispersed copper alloy by spark plasma sintering process using copper oxide and titanium diboride as raw materials. The mechanical, thermal and electrical properties of sintered bodies were discussed with the sintering parameters, and developed microstructure and phase of sintered bodies. -
Calcium-hexaluminate phase
$(CA_6)$ is known to be effective for the crack shielding due to the spinel block crystal structure. In this study, we focused to the control of$CA_6$ morphology for good damage tolerance behavior in alumina and zirconia/calcium-hexaluminate$(CA_6)$ composites. Calcium-hexaluminate$(CA_6)$ composites were prepared from zirconia, alumina and calcium carbornate powders. Calcium-hexaluminate$(CA_6)$ phase was obtained by the solid reaction through the formation of intermediate phase$(CA_2)$ .$CA_6$ phase showed the column type abnormal grain grown behavior composed of small blocks. Due to the typical microstructure of$CA_6$ , alumina and zirconia/calcium-hexaluminate composites provide a well controlled crack propagation behavior. -
Nanostructured Alumina - 20 vol% 3YSZ composites powder were synthesized by wet-milling technique. The starting materials were a mixture of Alumina micro-powder and 3YSZ nano-powders. Nano-crystalline grains were obtained after 24 h milling time. The nano-structured powder compacts were then processed to full density at different temperatures by high-frequency induction heat sintering (HFIHS). Effects of temperature on the mechanical and microstructure properties have been studied.
$Al_2O_3-3YSZ$ composites with higher mechanical properties and small grain size were successfully developed at relatively low temperatures through this technique. -
This paper concerned with SPS (spark plasma sintering), hot pressing of sinter nanometer WC-Co powder and discussed the density, hardness, microstructures and grain sizes of the alloys sintered. The results showed that the two sintered techniques could produce high density alloys and play well on the grain growth, but SPS could lower the sintering temperature and shorten sintering time. Besides, the hardness of the sintered cemented alloys that was dependent on the grain size and densification could also be improved.
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The effects of compaction pressure and sintering temperature on the densification of Fe-40wt%Ni alloy nanoparticles were analyzed. The Fe-Ni nanoparticles were fabricated by an arc-discharge method and then, compacted at three different pressures and sintered at 550 to
$900\;^{\circ}C$ . Densification was completed at temperature as low as$600\;^{\circ}C$ and high-pressure compaction was found to enhance densification. Densification behaviors and microstructure developments have been investigated through density measurements, electron microscopies, and hardness measurements. -
1mm-thick BLT ceramics were sintered in accordance with a bulk ceramic fabrication process. All XRD peaks detected in the sintered ceramics were indexed as the Bi-layered perovskite structure without secondary phases. Density was increased with increasing the sintering temperature up to
$1050\;^{\circ}C$ and the maximum value was about 98% of the theoretical density. The remanent polarization (2Pr) value of BLT ceramic sintered at$1050\;^{\circ}C$ was approximately$6.5\;{\mu}C/cm^2$ at the applied voltage of 4.5kV. From these results, a BLT ceramic target for plused laser deposition (PLD) system was successfully fabricated. -
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In the present work, the sintering behavior of high strength Al-5.6Zn-2.5Mg-1.6Cu (in wt.%) alloy compacts prepared from elemental powders was investigated. Microstructural evaluation was accompanied by XRD and DSC methods in order to determine the temperature and chemical composition of the liquid phases formed during sintering. It was found that three transient liquid phases are formed at 420, 439 and 450
$^{\circ}C$ . Microstructural study revealed the progressive formation of sintered contacts due to the presence of the liquid phases, although the green compact expands as a result of the melt penetration along the grain boundaries. While Zn melts at${\sim}420\;^{\circ}C$ , the intermetallic phases formed between Al and Mg were found to be responsible for the formation of liquid phase and the dimensional change at higher temperatures. -
Misawa, Tatsuya;Shikatani, Noboru;Kawakami, Yuji;Enjoji, Takashi;Ohtsu, Yasunori;Fujita, Hiroharu 538
The influence of the internal current for the ZnO ceramics on the sintering behavior by pulse current sintering (PCS) method was investigated. To clear the dependence of inner current on the sintering behavior of ZnO ceramics, direct measurement of electric resistance of ZnO specimen under sintering by SPS device was carried out. It was observed that electric resistance of specimen decreases with increase in the temperature. The electric resistance begins to decrease from the low temperature of$200^{\circ}C$ . The internal structure of sintered ZnO ceramics changed by the control of the internal current in the specimen using$Al_2O_3$ plate. -
SUS316L stainless steel, commercial pure Titanium and Ti-6Al-4V alloy powders applied by Mechanical Milling (MM) process are sintered by Hot Roll Sintering (HRS) process. Microstructure and mechanical properties of those HRS materials is investigated. The microstructures of materials produced by HRS process consist of fine grains and work-hardened structure, that is, the hybrid microstructure. Tensile test of the HRS material demonstrated the good mechanical properties. These results show that the HRS process is very effective to the improvement of mechanical properties in the SUS316L stainless steel, commercial pure Titanium and Ti-6Al-4V alloy.
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The effect of the additives,
$Y_2O_3$ and MgO, on the sintering and properties of$Al_2O_3-TiC$ composites was investigated. It is known that MgO is used as additive for improving densification and$Y_2O_3$ is applied as sintering aid. In this study, the amounts of TiC were varied in the range of 30-47 wt%. The 0.5 wt% MgO and also varied amounts of$Y_2O_3$ from 0.3 to 1 wt% were added into the composites. The sintering of$Al_2O_3-TiC$ composites was performed in a graphite-heating element furnace at different sintering temperature, 1700 and$1900\;^{\circ}C$ , for 2 hr under an argon atmosphere. The results demonstrated that the properties of the composites sintered at$1700\;^{\circ}C$ were much better than those sintered at$1900\;^{\circ}C$ . The comparisons on physical properties, mechanical properties and microstructure of composites with and without additives were reported. Comparing with other samples,$Al_2O_3-30wt%TiC$ composites with 0.5wt% MgO and$1\;wt%Y_2O_3$ exhibited the highest density of approximately 98% of theoretical and flexural strength of 302 MPa. -
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The main object of this research was to examine the effect of sintering conditions on the microstructure of tungsten heavy alloys and how the resulting modification of the microstructure can be used to optimize their mechanical properties. Alloys composed of 88%, 93% and 95% wt. of tungsten and the balance is Ni: Fe in the ratio of 7:3 were sintered at different temperatures for different sintering holding times in hydrogen atmosphere. It was shown that the mechanical properties of the alloys, and especially their ductility, are harmed when tungsten grains are contiguous.
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The corrosion performance of a powder metallurgical aluminum alloy in aeronautical environments was studied for both as sintered and heat treated states. Sintered samples were obtained by uniaxial pressing of an Al-Cu-Mg prealloyed powder followed by liquid phase sintering. The heat treatments applied were T4 and T6. Corrosion behaviour was assessed by means of potentiodynamic polarization. Results for the equivalent commercial wrought counterpart, AA2024-T3, are also presented for comparison. Similar corrosion performance was observed for both as sintered and AA2024-T3 samples, while corrosion resistance of the PM materials was improved by the heat treatment, especially in the T4 state.
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Da Silva Soares, Sergio R.;Gomes, Uilame Umbelino;Furukava, Marciano;De Souza, Carlson Pereira 552
The present study investigates the behavior of the sintering and hardness of stainless steel samples reinforced with NbC and TaC. Matrixes of pure stainless steel were compacted with addition of up to 3% wt NbC or TaC in a cylindrical die of steel$(\phi\;=\;5,0\;mm)$ at 700 MPa and sintered in an electrical resistance furnace under argon atmosphere. The sintered samples were characterized by density and hardness measurement, optical microscopy and scanning electron microscopy (SEM). The preliminary results show that the size and distribution of carbides influence in the sintering and hardness of the sintered samples. -
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The study examines hardness pattern of SH737-2Cu-.9C samples transient liquid phase sintered at different temperatures viz.
$1120^{\circ}C$ ,$1180^{\circ}C$ and$1250^{\circ}C$ , heat treated by various methods and then tempered at different temperatures. Sintered samples were characterized for density and densification parameter, and austenitized at$900^{\circ}C$ , subsequently cooled by four different methods viz. annealing, normalizing, oil and brine quenching. Hardness pattern was found minimum for air cooled and maximum for brine quenched, and samples sintered at$1250^{\circ}C$ had relatively higher hardness. The O.Q and B.Q samples were then tempered at$200^{\circ}C$ ,$400^{\circ}C$ ,$600^{\circ}C$ and$700^{\circ}C$ . Hardness pattern typically showed secondary hardness taking place, with maximum around$600^{\circ}C$ . -
In all conventional sintered PM products, the pores present are of two types, primary and secondary. Primary pores forming during compaction and latter during sintering, due to penetration of formed liquid through the matrix grain boundary. Effect of carbon addition on diffusion of Cu in SH737-2Cu system was investigated. After compaction and transient liquid phase sintering at
$1120^{\circ}C$ and$1180^{\circ}C$ , samples were characterized for densification, showing rise in sintering density and reduction in swelling on carbon addition. Quantitative microstructural characterization (shape factor and pore size) revealed bimodal distribution for 0% carbon, more rounded pores for 0.9% carbon and higher sintering temperature, and pore coarsening at higher sintering temperature. -
Powder forging is used for heavy-loaded parts (rings of rolling-contact bearings, gears etc.) production. Rolling contact fatigue is material property values of which characterize possibility of practical utilization of such parts. Rolling contact fatigue of some steels obtained out of prealloyed powders Astaloy CrM, Atomet 4601, Atomet 4901 and powder blends iron-carbon-nickel by hot forging is studied in the present paper. Effect of various kinds of heat and thermomechanical treatment on rolling contact fatigue is determined. Thermomechanical treatment provides optimal values of rolling contact fatigue. In this case steel structure contains up to 40% of retained metastable austenite which is transformed to martensite on trials. Thus typically crack is generated on residual pores and non-metallic inclusions instead of martensite zones in wrought steels.
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The effect of chemical composition of the sintering atmosphere on density, microstructure and mechanical properties of Fe-3%Mn-(Cr)-(Mo)-0.3%C steels is described. Pre-alloyed Astaloy CrM and CrL, ferromanganese and graphite were used as the starting powders. Following pressing in a rigid die, compacts were sintered at 1120 and
$1250^{\circ}C$ in atmospheres having different$H_2/N_2$ ratio and furnace cooled to room temperature. It has been found that the atmosphere composition has negligible effect on the as-sintered properties of the investigated materials. -
Sulowski, Maciej;Cias, Andrzej;Frydrych, Hanna;Frydrych, Jerzy;Olszewska, Irena;Golen, Ryszard;Sowa, Marek 563
The effect of different cooling rate on the structure and mechanical properties of Fe-3%Mn-(Cr)-(Mo)-0.3%C steels is described. Pre-alloyed Astaloy CrM and CrL, ferromanganese and graphite were used as the starting powders. Following pressing in a rigid die, compacts were sintered at$1120^{\circ}C$ and$1250^{\circ}C$ in$H_2/N_2$ atmospheres and cooled with cooling rates$1.4^{\circ}C/min$ and$6.5^{\circ}C/min$ . Convective cooled specimens were subsequently tempered at$200^{\circ}C$ for 60 and 240 minutes. -
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The characteristics of residual stresses occurring in PM steel based nickel (FLN2-4405) was investigated. The measurements of residual stresses were carried out by electrochemical layer removal technique. The values and distributions of residual stresses occurring in PM steel processed under various densities and heat treatment conditions were determined. In most of the experiments, tensile residual stresses were recorded in surface of samples. The residual stress distribution on the surface of the PM steels is affected by the heat treatment conditions and density. Maximum values of residual stresses on the surface were observed sinter hardened condition and
$7.4\;g/cm^3$ density. Minimum level of recorded tensile residual stresses are150 MPa and its maximum level is 370 MPa. -
The use of the nickel free, high nitrogen stainless steel powder and nitriding during sintering of iron based materials have been shown as an alternative way to the conventional PM stainless steels containing nickel. Nitrogen as an alloying element for iron improves in an effective way the properties of sintered alloyed steels. The powder metallurgy route is a suitable way to introduce nitrogen into these alloys and, in particular, to produce high nitrogen (close to the solubility limit) stainless steels. The paper presents and discusses the nitriding behavior of nickel-free stainless steels produced by powder metallurgy method. Alloyed melt was atomized by nitrogen and in this way nitrogen was introduced into the powder. Further nitriding occurred during sintering in a nitrogen atmosphere. For comparison, compacts having the same composition as an alloyed powder were produced from elemental powders mixture. Sintering-nitriding behaviour of investigated materials has been controlled by dilatometry, chemical and X-Ray phase analysis and metallography. Mechanical properties of sintered compacts were also measured.
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The mixed atomized iron powders with 0.3% graphite and 1% Ni powders were cold pressed and sintered at
$1200^{\circ}C$ for 30 min under pure Ar gas atmosphere. Some of the sintered specimens were intercritically annealed at$760^{\circ}C$ and quenched in water (single quenching). The other sintered specimens were first fully austenized at$890^{\circ}C$ and water quenched. These specimens were then intercritically annealed at$760^{\circ}C$ and re-quenched in water. The experimental results showed that the wear coefficient effectively decreased in the double quenched specimen. -
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Due to the increasing use that the stainless steel is getting recently in the nuclear industry, this document proposes the study of the stainless steel 316L with boron addition. With the final product, the properties of the stainless steel 316L (good mechanical properties and high corrosion resistance) with the boron neutron absorption properties are claimed to unify. The P/M technologies allow adding higher boron quantities than with the solidification conventional technologies, where segregation is produced.
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This study was conducted to improve the durability and decrease the friction of the sintered bushing used in the joints of construction equipment. Research was carried out to examine the effects of the groove pattern on the inner surface. The following results were obtained: (1) The bushing (EK Bush) with grooves on the inner diameter showed increased durability as compared to a non-grooved bushing. (2) The helical-grooved bushing showed the least amount of wear; it was 1/10 of the wear of the non-grooved bushing. (3) If the distance between grooves was decreased, then the coefficient of friction also decreased.
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We investigated that the effect of
$CaCO_3$ based compound on machinability of two types of PM steels. One is a copper steel which is selected as a general PM steel, and the other is a diffusion alloyed steel selected as a high strength PM steel. It is found that$CaCO_3$ based compound addition improves machinability in drilling of both of the PM steels. Although the compound addition degrades the mechanical properties of PM steels, it is considered that decrease of the properties can be compensated by increasing density. -
The present paper investigates the possibilities of niobium using for the mechanical properties of the common low alloyed Cu-Ni-Mo-C sintered structural steels enhancing. On both thermodynamic and experimental bases there were demonstrated the Nb nitrides/carbides/carbonitrides preferential formation in these steels during sintering in dissociated ammonia at both common and elevated temperatures. The obtained results for
$0.2\;{\div}\;1.0\;%$ fine Nb powder and 0.3% graphite additions to Distaloy AB iron base powder cold compacted and sintered in dissociated ammonia proved the expected strengthening effect, leading to higher mechanical properties of the processed steels than of the common Cu-Ni-Mo-C ones. -
This work presents mechanical properties and corrosion resistance of duplex stainless steels obtained through powder metallurgy starting from austenitic, martensitic powders by controlled addition of alloying elements in the right quantity to obtain the chemical composition of the structure similar to biphasic one. In the mixes preparations the Schaffler's diagram was taken into consideration. Prepared mixes of powders have been sintered in a vacuum furnace with argon backfilling. After sintering rapid cooling was applied using nitrogen. Corrosion properties have been studied through electrochemical methods in 1M NaCl.
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Several chemicals were studied to suppress the damage due to stress corrosion cracking (SCC) of steam generator (SG) tubes in nuclear power plants. The effects on the SCC of the compounds,
$TiO_2$ , TyzorLA and$CeB_6$ , were tested for several types of SG tubing materials. The test with the addition of$TiO_2$ and$CeB_6$ showed an effect in decreasing the SCC for the SG tubing material. However,$CeB_6$ caused some more SCC for Alloy 800. The penetration property into a crevice of the inhibitors was investigated by using Alloy 600 specimens with different gap. -
The stress corrosion cracking (SCC) susceptibility of Alloy 600 MA, Alloy 600 TT, Alloy 800, and Alloy 690 TT were investigated in a deaerated 0.01 M solution of sodium tetrathionate using reverse u-bend test samples at
$340^{\circ}C$ . The results showed that SCC occurred in all alloys, excluding Alloy 690 TT. The SCC susceptibility decreased with an increase in the chromium content of the alloys. The results of the deposits and spectra taken from an energy dispersive X-ray system confirmed the existence of a reduced sulfur causing SCC. -
Based on the comparison of structures and properties of the HS6-5-2 high speed steels made with the powder injection moulding method, pressureless forming, compacting and sintering, and commercial steels made with the ASEA-STORA method, fine carbides spread evenly in the steel matrix were found in the structure of all tested high-speed steels in the sintered state. The steels made with the pressureless forming method are characteristic of the lowest sintering temperature and the highest density, resulting from the high carbon concentration coming from the binding agent degradation.
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Manufacturers of shock absorbers are continuously innovating for improving safety and enhance comfort in cars. The PM industry, as important supplier of components for shock absorbers, has gone along with this evolution by developing the required technology. This paper presents examples of components and technology to meet demanding market requirements. They have been selected by their representative character but there are many other interesting components that we cannot show because of the limited extension of a paper.
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Porous bearings are lubricated the oil that is contained in porous metal. Then they are always used with no oil supply, because of that, widely used electric motors. But, if oil flow out less than the limit, troubles often happen. This report shows that attempt of estimating oil quantity in porous bearing by using calculation that based Reynols' equation and Darcy's law, aimed of developing long life bearing. And comparing with experimental and calculation result, we show possibility of estimating rest oil quantity in porous bearing at steadry state by calculation.
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Gas filtration at high temperature from industrial processes offers various advantages such as increasing process efficiency, improving heat recovery and materials resource recovery, etc. At the same time, it is an advanced environment protection technology. This paper describes a newly developed metallic filter element. The manufacturing process of sintered
$Fe_3Al$ metallic powder and the mechanical and filtration characteristics of this filter element were investigated. In this work, the phase constituent changes of the$Fe_3Al$ powder during sintering were studied. The newly developed filter elements were found to have excellent corrosion resistance, good thermal resistance, high strength and high filtration efficiency. -
This paper described the state of art of porous metal materials, the typical manufacturing technologies and performances of sintered metal porous materials, with emphasis on the recent research achievements of CISRI in development of porous metal materials. High performance porous metal materials, such as metallic membrane, sub-micron asymmetric composite porous metal, large dimensional and structure complicated porous metal aeration cones and tube, metallic catalytic filter elements, lotus-type porous materials, etc, have been developed. Their applications in energy industry, petrochemical industry, clean coal process and other industrial fields were introduced and discussed.
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Micro-porous nickel (Ni) with an open cell structure was fabricated by powder metallurgy. The pore size of the micro-porous Ni approximated
$30{\mu}m$ and$150{\mu}m$ . For comparison, porous Ni with a macro-porous structure were also prepared by both powder metallurgy (pore size$800{\mu}m$ ) and the traditional chemical vapour deposition method (pore size$1300{\mu}m$ ). The mechanical properties of the micro-and macro-porous Ni samples were evaluated using compressive tests. Results indicate that the micro-porous Ni samples exhibited significantly enhanced mechanical properties, compared to those of the macro-porous Ni samples. -
Recently the Marangoni convention is supposed to be an important phenomenon that significantly affects the solidification. For understanding the Marangoni convection mechanism, visualizing the convention phenomenon of molten tin with ultrasonic has been conducted. This paper reports developing a tracer material of micro metal balloon that is used in the molten system. We have succeeded in coating the surface of Shirasu-ballons with nickel by plating process. The obtained metal balloon is spherical and some characterizations were conducted.
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A porous material with a surface layer was fabricated using glass abrasive sludge and expanding agents. The glass abrasive sludges were mixed with expanding agents and compacted into pellets. These pellets were sintered in the range of
$700-900^{\circ}C$ for 20min. The sintered porous materials had a surface layer with smaller pores and inner parts with larger pores. The surface layer and pores controlled the absorption ratio and physical properties. -
The deformation behavior under three-point bend test was found to depend on the loading uniformity and the macrostructure for SiC reticulated porous ceramics (RPCs). However, this dependence of loading uniformity is alleviated by improved macrostructure with fewer flaws and clogged pores. Even, this dependence becomes less important as the struts become thicker and stronger. The bend result of RPCs with highly uniform macrostructure is in excellent agreement with the GA (Gibson and Ashby) model, but the one with un-uniform macrostructure deviates from the GA model, suggesting that the macrostructure plays an important role in deformation behavior of RPCs under bend.
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In a manufacturing technique of the sintered filter, pressureless sintering method has good permeability, it is not need the binder and lubricant used on compacting process, so it has little contamination and it is easy to control the pore size and shape but the mechanical strength is low relatively and it is difficult that parts of complicate form are manufactured. In the case of manufacturing the filter by press and sintering method, in order to be satisfactory characteristic of un-pressed filter, in this study sintered metal filter fabricated by using 30-40mesh stainless steel 316L powder and additive agents. Porosity and structure of pores, permeability and mechanical strength of the sintered filter were investigated with the variation sintering conditions. Porosity was nearly constant about
$60{\sim}70%$ , density, permeability and mechanical strength were changed markedly with quantity of additive materials and sintering conditions. -
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Investigation of influence the morphology of initial powder particles, application pore-formers for sintering of nickel powders and application of flux for sintering of aluminum was made. Using different methods was prepared material with size of porous in wide range size of pores (
$1-500{\mu}m$ ). Using the flux for gravity sintering of aluminum in air atmosphere was manufactured porous material with porosity about 45%.. -
The binder phase for TiC reinforced steel matrix composite was added in the form of elemental powders and master alloy powders. The microstructures, binder phase variation with TiC content and mechanical properties were evaluated. The addition of a type of binder phase largely effects the microstructure and mechanical properties. The binder phase variation from starting composition was observed with increase in wt% TiC content and this variation was higher when the master alloy powders were used as a binder. The response to heat treatment was decreased with an increase in TiC content due to the shift of binder phase from the starting composition.
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In this paper, we show some experimental results of binder-free WC sintered by Pulsed Electric Current Sintering (PECS) also known as Field Assisted Sintering Technology (FAST). These binder-free WC have extremely hardness and stiffness. However, these mechanical properties are dependent on the sintering condition, e.g., maximum temperature, applied pressure, etc. We show some relationship between mechanical properties and sintering condition to improve to sinter the binder-free WC.
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The behavior of hardmetals under cyclic loads is investigated. Unnotched specimens were employed to obtain practical information regarding fatigue in hardmetals. All the tested hardmetals exhibit an increase in the number of cycles until failure with a decrease in the maximum stress, i.e., the hardmetals exhibit a high fatigue sensitivity. The fatigue strength increases with the cobalt content. Although distinct fatigue limits, as observed in metals, cannot be observed, the calculated fatigue limit stress at
$10^7$ cycles is found to be approximately 70% of the flexural strength, and the stress value exhibits a linear relationship with the flexural stress. -
In the present study, the focus is on the synthesis of nanosized WC powder by the chemical vapor condensation proces. The synthesized W-C system powder by the CVC process shows W2C, W, WO3 phases and can not shows WC phase. After recarburization heat treatment under mixture gas atmosphere of argon and hydrogen gases, the synthesized W-C system powder fully transformed to the pure WC. The synthesized WC powder after recarburization heat treatment has an average particle size of 20 nm. The nano-sized WC powder can be prepared by the combination of the CVC process and heat treatment methods.
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The present work is a study on the argon gas pressure effects of Sinter/HIP sintering on microstructure and strength of different grades of TiC-NiMo cermets. Titanium carbide in the composition of different grades of TiC-NiMo cermets was ranged from 40 to 80 wt.% and the ratio of nickel to molybdenum in the initial powder composition was 1:1, 2:1 and 4:1 respectively. On the sintered alloys, the main strength characteristic, transverse rupture strength (TRS) was measured. Furthermore, the microstructure parameters of some alloys were measured and the pressure effect on pore elimination was evaluated. All the results were compared with common, vacuum sintered alloys. The TRS values of TiC-NiMo cermets could be considerably improved by using Sinter/HIP technique, for high-carbide fraction alloys and for alloys sintered at elevated temperatures.
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To investigate sliding friction and wear behaviors of WC-Co/WC-Co pairs containing different WC grain sizes, the ball-on-disc test in air were carried out, where WC grain sizes a
$0.5\;{\mu}m$ (F.G.) and$1.5\;{\mu}m$ (C.G.). The wear volume of F.G. pin for F.G. pin/C.G. disc is larger than that of F.G. pin for F.G. pin/F.G. disc due to higher friction coefficient, and the surfaces after wear test are richer in oxygen compared to those before test. Furthermore, the wear debris, which is composed of nona-scale grain, after the wear test are remarkably richer in oxygen than to those before test. -
Cr-C-Ni composites were synthesized in situ from elemental powders of Cr, Ni and C by high energy milling followed by reactive sintering. The milled powders with the grain size in nano-scale were pressed to compacts and sintered. During the following thermal treatment at first the chromium carbide was formed and then the
$Cr_3C_2-Ni$ cermets were sintered in one cycle. The interface between the binder phase and the carbide grains of the in situ composite has a good bonding strength as it is not contaminated with oxidation films or other detrimental surface reactions. -
The aim of present work is to link geometrical parameter of maximum area of structural defect
$\sqrt{area}\;_{max}$ (proposed by Y. Murakami, 1983) with surface fatigue mechanisms. Determined relations allow making predictions of surface fatigue properties of cemented carbides (WC-Co hardmetal - H15 - 85wt% WC and 15wt %Co, TiC-based cermets - T60/8 - 60wt %TiC and Fe/8wt% Ni and T70/14 - 70wt %TiC and Fe/14wt% Ni) in conditions of rolling contact and impact cycling loading. Pores considered being equivalent to small defects. Three comparative defects conditions are distinguished: surface pore, just below free surface and interior pores. The Vickers hardness of binder (as main responsible for the fracture mechanism of hardmetal and cermets) assumed to be the basis of such assumption. The estimate of this prediction has been done by analyzing the pore sizes using the statistics of extremes. The lower bound of fatigue properties can be correctly predicted by considering the maximum occurring pore size. -
In this study, the diffusion behaviors of C and Co in liquid phase sintering of WC-Co system were investigated whether these two components diffused in the same direction in case of having opposite gradient each other with not being
$\eta$ phase. The green compacts with controlled compositions in not being of$\eta$ phase and gradient composition which one is WC-5Co-1.2%C, the other is WC-XCo-0.2%C (where X = 5, 10, 15, 20, 25) were sintered at$1350^{\circ}C$ and$1400^{\circ}C$ and then the diffusion behaviors of C and Co were investigated by analyses of compositional change, also determined for microstructure and microhardness. Also, same testing was carried out on the specimens with dual layers sintered in upright and reverse positions to evaluate the effect of gravity on the diffusion in liquid Co. From the results of this study, we can find the fact that the direction of diffusion for C and Co in WC-Co system during liquid phase sintering was different and the effect of gravity for the liquid was insignificant. Also other physical properties were changed on the diffusion of elements. -
Multilayered coatings on tungsten carbide cutting tools are widely used for enhancing cutting performance. In this paper, we review the CVD TiC/TiCN multilayer as a function of the multilayer period. The TiC/TiCN multilayers in initial stage show preferred (220) orientation but shifts to (200) orientation with decreasing multilayer period. The nanohardness of TiC/TiCN multilayers were found to increase with decreasing multilayer period and shows a maximum of 23.8 GPa at a period = 33.5 nm.
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To improve the mechanical properties of WC-Co cemented carbides, the dual composite was studied. The compositions of granule and matrix were nano-sized WC-6 wt% Co(granule) and normal sized WC-20 wt% Co(matrix), respectively. The granules were grouped 50, 100 and
$150\;{\mu}m$ and mixed with WC and Co powders as the volume fractions of granule to matrix were 50 to 50, 40 to 60 and 30 to 70. These compacts were sintered at$1380^{\circ}C$ for 10 minutes in vacuum. The microstructure, transverse rupture strength and wear resistance were investigated. -
Direct reduction and carburization process was thought one of the best methods to make nano-sized WC powder. The oxide powders were mixed with graphite powder by ball milling in the compositions of WC-5,-10wt%Co. The mixture was heated at the temperatures of
$600{\sim}800^{\circ}C$ for 5 hours in Ar. The reaction time of the reduction and carburization was decreased as heating temperatures and cobalt content increased. The mean size of WC/Co composite powders was about 260 nm after the reactions. And the mean size of WC grains in WC/Co composite powders was about 38 nm after the reaction at$800^{\circ}C$ for 5 hours. -
TiC-and Ti(C,N)-based cermets are excellent in semi-and final finishing of work piece during cutting operations. Typical microstructure of the cermets is a core/rim structure. The undissolved Ti(C,N) cores contribute to their high hardness while the rim phases, (Ti,M1,M2)(C,N)-type solid solutions, play great roles in enhancing the toughness. In this paper, various ultrafine pre-mixed MeC-Ni powders were synthesized and the powders were sintered or hot pressed after mixing in order to control the size and volume fractions of core and rim phases in the system. This paper will present the factors determining the microstructure along with mechanical properties.
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Nano-sized WC particles in WC/Co composite powders were synthesized by mechanochemical method. The raw powders
$(WO_3,\;Co_3O_4,\;VC,\;Cr_3C_2$ and graphite) were mixed by planetary milling for 30 hours. The compositions were WC-10 and -20 wt% Co added VC and$Cr_3C_2$ . The direct reduction and carburization of the mixed powders were carried at$900\;^{\circ}C$ for 1 to 3 hours under flowing Ar gas. The mean size of WC particles in WC/Co composite powders was about 16 nm. The resultant powders were compacted and sintered at$1300{\sim}1360\;^{\circ}C$ for 0.5 hour. After sintering the mean size of WC particles was about 50 nm. -
The dry-milling technique was used for mixing and crushing oxides and graphite powders. The ratio of ball-to-powder was 30:1 and argon gas was filled in jar. The excess carbon was
$10{\sim}20wt%$ of the stoichiometric amount. The dry-milling was carried for 20 hours. The mixed powders were reduced and carburized at$900{\sim}980^{\circ}C$ for 3 hours flowing Ar gas in tube furnace. The dry-milled powders showed the wide diffraction patterns of X-ray. The reactions of reduction and carburization were completed in 3 hours at$980^{\circ}C$ . After the reactions, the mean size of WC particles was about 200 nm. The content of free carbon in WC/Co mixed powders was less as the reaction temperature increased. -
This paper presents a study of large grains by transmission electron microscopy in two WC-Co alloys, one W rich and one C rich. In the W rich alloy, some large grains are found in contact with the
$\eta$ phase. The C content influences the morphology of large grains: they are flatter in the C rich alloy with smoother interfaces. Whatever the C content, they contain few dislocations compared to matrix grains except often in a small area. Small WC grains are often found inside the large grains. They have likely been engulfed during the growth of the large grains owing to the low boundary energy. -
This paper introduces a special spheroidizing technology at ultra-high temperature. The conventional cast tungsten carbide (YZ) is melted at high temperature, rapidly cooled and spheroidized on a new ultra-high temperature spheroidizing equipment to prepare various grades WSC powders.
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This is about the effects deoxidization, carbonization and alloying preparation on fine grain W, WC, and grade YG8 powder reduced by "yellow tungsten oxide" and "blue tungsten oxide". The result indicates that yellow tungsten has single composition and blue tungsten oxide has complex composition. With this feature, yellow tungsten oxide got better uniformity and concentration distribution on fine particle size W and WC powder than blue tungsten oxide's. The grade alloy YG8 that made of this W or WC powder has uniform alloy construction, concentrated WC grain distribution and better alloy properties.
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One append way of liquid state inhibitor was investigated, which putting V, Cr into W-Co composite solutions in the form of ionization. After spray drying and being calcined, W-Co composite oxides could come into being. Then taking fluidization techniques, well-proportioned W-Co composite powder compounded with inhibitor could be produced in the end.
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Magnetron sputtered TiN, (Ti, Al)N and TiN/(Ti, Al)N multilayer coatings grown on cemented carbide substrates have been characterized by using electron probe microanalysis (EPMA), X-ray diffraction (XRD), scanning electron spectroscopy (SEM), nanoindentation, scratcher and cutting tests. Results show that TiN coating is bell mouth columnar structures, (Ti, Al)N coating is straight columnar structures and the modulation structure has been formed in the TiN/(Ti, Al)N multilayer coating. TiN/(Ti, Al)N multilayer coating exhibited higher hardness, better adhesion with substrate and excellent cutting performance compared with TiN and (Ti, Al)N coating.
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Development of recycling method at cemented carbide scraps was researched. Some properties of recycled cemented carbides were investigated. Recycled WC fine powder suffered the surface oxidation. Therefore it was necessary to be done by reduction treatment at 1073K-3.6ks under hydrogen atmosphere. When sintering condition at 1673K-3.6ks was treated under vacuum condition, it gained the deflective strength of about 90%, and gained hardness and sintering density about same value compared with commercial alloys. As a result, it was able to recycle only by 7 processes.
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Sintered Ti(C,N)-based cermets were treated with hot isostatic pressing (HIP) at different nitrogen pressures. The tribological properties of the treated cermets have been evaluated. The results show that a hard near-surface area rich in TiN formed after HIP treatment. The cermets treated at higher pressure had a relatively lower friction coefficient and specific wear rate. In all cases the microhardness of treated cermets is higher than that without HIP natridation. The wear mechanisms of cermets were hard particle flaking-off and ploughing. It was also found that the HIP natridation is well-suited for improving the tribological properties of cermets.
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Ur, Soon-Chul;Kwon, Joon-Chul;Choi, Moon-Kwan;Kweon, Soon-Yong;Hong, Tae-Whan;Kim, Il-Ho;Lee, Young-Geun 665
Undoped$CoSb_3$ powders were synthesized by mechanical alloying (MA) of elemental powders using a nominal stoichiometric composition. Nano-structured, single-phase skutterudite$CoSb_3$ was successfully produced by vacuum hot pressing (VHP) using MA powders without subsequent annealing. Phase transformations during synthesis were investigated using XRD, and microstructure was observed using SEM and TEM. Thermoelectric properties in terms of Seebeck coefficient, electrical conductivity, thermal conductivity and figure of merit(ZT) were systematically measured and compared with the results of analogous studies. Lattice thermal conductivity was reduced owing to increasing phone scattering in nano-structured MA$CoSb_3$ , leading to enhancement in the thermoelectric figure of merit. MA associated with VHP technique offers an alternative potential processing route for the process of skutterudite. -
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The influence of
$Eu^{3+}$ doping on the structural and morphological properties of the$Gd_2O_3:Eu^{3+}$ phosphor system, obtained ultrasonically via Spray Pyrolysis from common gadolinium and europium nitrate solutions, was studied. The particle morphology, crystalline and chemical structure were studied by XRD, SEM and EDS. TEM was applied in order to identify the structure and growth of "primary nanoparticles" and determine the presence of domains locally affected by "Moires Frames" and "Crystallite Size". The SADP allows determining the presence of a polycrystalline material with two phases in the "as-prepared" samples, and only an Ia3 phase along the thermal treatment. -
De la Torre, M. A. Lopez;Dura, O. J.;Hernandez, M.;Garcia-Cordobes, M.;Herranz, G.;Sanchez-Bautista, C.;Rodriguez, G. P. 670
We report on the mechanical and structural properties of nanocrystalline 8% and 10% mol yttria stabilized zirconia (YSZ) obtained using mechanical alloying (MA). The as-milled powders show a body-centered cubic structure with grain sizes in the nanometer scale. After uniaxial pressing and sintering the compacts exhibit good mechanical properties. We discuss the correlation of these enhanced properties with the microstructural changes induced by heat treatment. -
The influence of several experimental parameters on the formation of stable Alloy 625 nanoparticles dispersion in ethanol was investigated. Several analyzing methods were applied, like transmission profiles measured by Turbiscan, transmission electron microscopy, X-ray diffraction, gas chromatography, and particle size analyzer. The correlation among the increase of particle sizes, caused by nanoparticle coalescence and collision, concentration of dispersant and time was presented and discussed. The optimum conditions for the formation of stable dispersion are evaluated.
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Synthesis of zinc oxide nanorods, sheets and flower like structure were done by the sol-gel method using zinc acetate dihydrate and sodium hydroxide at
$80^{\circ}C$ with 12 hours refluxing time nanorods, in case of as synthesized powder, with diameter of 20-60nm. Annealing at higher temperature (300 and$500^{\circ}C$ ,) in air ambient changes the morphology to sheet and flower like structure. The standard peak of zinc oxide was observed in IR at$523cm^{-1}$ . The UV-VIS spectroscopy of zinc oxide shows a characteristic peak at 375nm. -
The effects of particle size on the surface properties of hydro-thermally synthesized barium titanate powders were investigated by means of particle size analysis, specific surface area, SEM, zeta potential and XPS. Particle sizes were measured by laser light scattering and are in the range of 150 to 1100nm. Zeta potential increased with increasing particle size and it was large minus value in the range of particle size from 500 to 900nm, which seems to be related with the dissolution of
$Ba^{2+}$ ion in these particle sizes from the analysis of surface properties by XPS. -
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Shikatani, Noboru;Misawa, Tatsuya;Ohtsu, Yasunori;Fujita, Hiroharu;Kawakami, Yuji;Enjoji, Takashi 682
Thermoelectric conversion efficiency of thermoelectric elements can be increased by using a structure combining n-type and p-type semiconductors. From the above point of view, attention was directed at ZnO as a candidate n-type semiconductor material and investigations were made. As the result, a dimensionless figure of merit ZT close to 0.28 (1073K) was obtained for specimens produced by the PCS (Pulse Current Sintering) method with addition of specified quantities of$TiO_2$ , CoO, and$Al_2O_3$ to ZnO. It was found that the interstitial$TiO_2$ in the ZnO restrains the grain growth and CoO acts onto the bond between grains. The influence of the inclusion of$TiO_2$ and CoO onto the sintering behavior also was investigated. -
In the present study, the powder metallurgical fabrication of
$Bi_{0.4}Te_3Sb_{1.6}$ thermoelectric materials has been studied with specific interest to control the microstructure by the mechanical grinding process. The$Bi_{0.4}Te_3Sb_{1.6}$ thermoelectric powders with a various particle size distribution were prepared by the combination of the mechanical milling and blending processes. The specific electric resistivity of the$Bi_{0.4}Te_3Sb_{1.6}$ sintered bodies mainly depended on the orientation of the crystal structure rather than the particle size of the raw powders. -
Park, Kwan-Ho;Kim, Mi-Jung;Jung, Jae-Yong;You, Sin-Wook;Lee, Jung-Il;Ur, Soon-Chul;Kim, Il-Ho 686
The encapsulated induction melting and hot pressing were employed to prepare Fe-doped$CoSb_3$ skutterudites and their thermoelectric properties were investigated. Single phase$\delta-CoSb_3$ was successfully obtained by the subsequent heat treatment at 773K for 24 hours. Iron atoms acted as electron acceptors by substituting cobalt atoms. Thermoelectric properties were remarkably improved by the appropriate doping.$Co_{0.7}Fe_{0.3}Sb_3$ was found as an optimum composition for best thermoelectric properties in this work. -
Kim, Mi-Jung;Park, Kwan-Ho;Jung, Jae-Yong;You, Sin-Wook;Lee, Jung-Il;Ur, Soon-Chul;Kim, Il-Ho 688
Ni-doped$CoSb_3$ was prepared by the encapsulated induction melting and hot pressing, and its doping effects on the thermoelectric properties were investigated. Single phase$\delta-CoSb_3$ was successfully obtained by the subsequent heat treatment at 773K for 24 hours. Nickel atoms acted as electron donors by substituting cobalt atoms. Thermoelectric properties were remarkably improved by the appropriate doping. -
Variable valve timing unit, which is able to decrease environmental load and improve fuel economy is loaded onto many automobiles recently. This unit consists mainly of sprocket, housing and rotor. These parts are requested different properties according to environment. We produce sintered parts for variable valve timing unit by selecting compact, sinter process and special treatment according to demanded properties. In this paper, demanded properties of sintered parts for variable valve timing unit and adopted technique to satisfy them are presented.
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Behavior of stoichiometric and near-stoichiometric NiAl at plasma spray deposition, without and with a bond coat, for coating layers realization on a low alloyed steel substrate, has been investigated. In all variants, NiAl particle melting and subsequent welding at the impact with substrate were observed, forming a relatively compact and adherent coating layer with the NiAl stability maintaining - all assuring the coating layer oxidation and corrosion resistance. Good results from these points of view, also validated through corrosion tests, were obtained for 45:55 Ni:Al composition without a bond coat but adopting an Ar protective surrounding of plasma jet.
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As a candidate for lead-free piezoelectric materials, dense
$95(Na_{0.5}K_{0.5})NbO_3-5LiTaO_3$ (NKN-5LT) ceramics were developed by conventional sintering process. Sintering temperature was lowered by adding$Li_2O$ as a sintering aid. The electrical properties of NKN-5LT ceramics were investigated as a function of$Li_2O$ concentration. At the addition of 1 mol%$Li_2O$ , electromechanical coupling factor$(k_P)$ and piezoelectric coefficient$(d_{33})$ of NKN-5LT ceramics were found to reach the highest values of 0.37 and 250 pC/N, respectively. -
This paper presents the densification and microstructure evolution of bilayer components made from 316L stainless steel and M2 High speed steel during co-sintering process. The sintering was carried out at temperatures ranging from
$1230-1320^{\circ}C$ in a reducing atmosphere. The addition of boron to 316L was examined in order to increase the densification rate and improve the sintering compatibility between the two layers. It was shown that the mismatch strain bettwen the two layers induces biaxial stresses during sintering, influencing the densification rate. The effect of boron addition was also found to be positive as it improves the bonding between the two layers. -
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Kim, Chang-Kyu;Oh, Seok-Jin;Jang, Se-Jung;Kim, Ki-Hwan;Lee, Don-Bae;Lee, Yoon-Sang;Park, Jong-Man;Park, Hee-Dae 474.1
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Souza, Carlson;Gomes, Kalyanne K. P. Gomes;Medeiros, Francisca F. P.;Cardoso, Maria C. C.;Sousa, Joao F.;Gomes, Uilame U. 479.1
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Gateaud, Arnaud;Apelian, Diran;Baum, Marc;Poskrebyshev, Grisha;Donaldson, Ian;Levee, Patrice 517.2
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Talaka, Tatsiana;Grigorieva, Tatiana;Vitiaz, Piotr;Lyakhov, Nikolay;Letsko, Andrey;Beliaev, Andrey;Barinova, Antonina 672.1
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Lomovsky, O.I.;Dudina, D.V.;Korchagin, M.A.;Kosarev, V.F.;Klinkov, S.V.;Ulianitsky, V.Yu.;Kim, J.S.;Kwon, Y.S. 680.2