• Title/Summary/Keyword: Fine microstructure

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Fabrication and densification of Heusler Fe2VAl alloy powders by mechanical alloying (MA법에 의한 Heusler Fe2VAl 합금분말의 제조 및 치밀화)

  • Kim, Kwang-Duk;Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.1
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    • pp.51-57
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    • 2013
  • We have applied mechanical alloying (MA) to produce Heusler $Fe_2VAl$ thermoelectric alloy using a mixture of elemental $Fe_{50}V_{25}Al_{25}$ powders. An optimal milling and heat treatment conditions to obtain the single phase of Fe2VAl compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry (DSC) measurement. The $Fe_{50}V_{25}Al_{25}$ MA sample ball-milled for 60 hours exhibits a bcc ${\alpha}$-(Fe,V,Al) solid solution. Single phase of Heusler $Fe_2VAl$ compound can be obtained by MA of $Fe_{50}V_{25}Al_{25}$ mixture for 60 hours and subsequently heated up to $700^{\circ}C$. Sintering of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $900{\sim}1000^{\circ}C$ under 60 MPa. The Vickers hardness of bulk sample sintered at $1000^{\circ}C$ was high value of Hv 870. All compact bodies have a high relative density above 90 % with metallic glare on the surface.

Microstructure and Magnetic Properties of Rapidly Solidified Nd-Fe(-Co) and Sm-Co(-Fe) Laves Compounds (급속냉각된 Nd-Fe(-Co)와 Sm-Co(-Fe)계 Laves 화합물의 미세조직과 자기특성)

  • 이우영;최승덕;양충진
    • Journal of the Korean Magnetics Society
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    • v.1 no.1
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    • pp.17-24
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    • 1991
  • Laves phases of $NdFe_2$, $Nd{(Fe_{0.5})}_2$, $SmCo_2$ and $Sm{(Fe_{0.5}Co_{0.5})}_2$ stoichiometry were prepared using a rapid solidification technology. Low temperature magnetic properties show ferromagnetic behaviors for the $Nd{(Fe_{0.5}Co_{0.5})}_2$, $SmCo_2$ and $Sm{(Fe_{0.5}Co_{0.5})}_2$Nd(Feo,Coo,) Laves compounds while a sort of spin reorientation has been suggested for the supposed composition of $NdFe_2$ alloy. This rapidly solidified $NdFe_2$ alloy is believed to consist of metastable rhombohedral $NdFe_7$ phase plus fine particles of Nd-rich phase. Some evidence of phase transition from the mixture of unstable $NdFe_7$ compound plus Nd-rich to $Nd_2Fe_{17}$ plus Fe-Nd-O phase was obtained after annealing the $NdFe_2$, alloy. The pseudo-binary Laves compound, $Sm{(Fe_{0.5}Co_{0.5})}_2$ exhibits a high coercivityof 4 kOe at room temperature with Curie temperature of $400^{\circ}C$ while the $Nd{(Fe_{0.5}Co_{0.5})}_2$ compound shows a magnetic moment of $2.8\;{\mu}_B/f.u.$.

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A study on the preparation of $(Ba_{1-X}Sr_X)ZrO_3$ using oxalate method and its dielectric properties (수산염법에 의한 $(Ba_{1-X}Sr_X)ZrO_3$의 합성 및 그의 유전특성에 관한 연구)

  • Oh Seong Kweon;Nam Seok Baik;Byung Ha Lee
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.4 no.3
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    • pp.252-261
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    • 1994
  • The $(Ba_{1-X}Sr_X)ZrO_3$ powder showing chemically pure and fine particle size was attempted to be synthesized by the oxalate method. The objective of this study is to determine the optimum synthesis condition of stable $(Ba_{1-X}Sr_X)ZrO_3$ powder in terms of the temperatures coefficient of resonant frequency ${\tau}_f$ by examining the microstructure and dielectric properties of the synthesized powder. The six compounds (x=0, 0.2, 0.4, 0.6, 0.8, 1) of $(Ba_{1-X}Sr_X)ZrO_3$ were prepared by the oxalate method, and then calcined at $1000^{\circ}C$ to obtain the crystalline $(Ba_{1-X}Sr_X)ZrO_3$ powder. The synthesized powder showed the globular-shape and average particle size of less than $0.2 \mu\textrm{m}$. The composition of x=0.5, i.e., half of Ba was replaced by Sr, is experted to show the zero value of temperatures coefficient of capacitance ${\tau}_c$.

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Synthesis and characterization of Mg-Si thermoelectric compound subjected to mechanical alloying (기계적 합금화에 의한 Mg-Si계 열전화합물의 합성 및 평가)

  • Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.17 no.3
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    • pp.121-127
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    • 2007
  • We have applied mechanical alloying (MA) to get $Mg_2Si$ thermoelectric material with nano-sized grains. An optimal milling and heat treatment conditions to obtain the single phase of $Mg_2Si$ compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry (DSC) measurement. The $Mg_{66.7}Si_{33.3}$ MA samples ball-milled for $20{\sim}180\;hrs$ exhibit two broad exothermic heat releases around $220^{\circ}C$ and $570^{\circ}C$. On the other hand, MA sample ball-milled far 260 hrs exhibits only a sharp exothermic peak at $230^{\circ}C$ Single phase Mg2Si powder can be obtained by MA of $Mg_{66.7}Si_{33.3}$ mixture for 60 hours and subsequently heated up to $620^{\circ}C$. Sintering of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $800{\sim}900^{\circ}C$ under 50 MPa. The shrinkage of sintering sample during SPS was significant at about $200^{\circ}C$. All compact bodies have a high relative density above 94% with metallic glare on the surface.

Microstructure and Magnetic Properties of Zn1-xCoxO Thin Films Grown by Sol-Gel Process (Sol-Gel 법으로 제작한 Zn1-xCoxO 박박의 미세조직 및 자기적 특성)

  • Ko, Yoon-Duk;Tai, Weon-Pil;Kim, Eung-Kwon;Kim, Ki-Chul;Choi, Choon-Gi;Kim, Jong-Min;Song, Joon-Tae;Park, Tae-Seok;Suh, Su-Jeung;Kim, Young-Sung
    • Journal of the Korean Ceramic Society
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    • v.42 no.7 s.278
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    • pp.475-482
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    • 2005
  • Zn$_{l-x}$Co$_{x}$O (x = 0.05 - 0.20) films were grown on Coming 7059 glass by sol-gel process. A homogeneous and stable Zn$_{l-x}$Co$_{x}$O sol was prepared by dissolving zinc acetate dihydrate (Zn(CH$_{3}$COO)$_{2}$$\cdot$2H$_{2}$O), cobalt acetate tetrahydrate ((CH$_{3}$)$_{2}$$\cdot$CHOH) and aluminium chloride hexahydrate (AlCl$_{3}$ $\cdot$ 6H$_{2}$O) as solute in solution of isopropanol ((CH$_{3}$)$_{2}$$\cdot$CHOH) and monoethanolamine (MEA:H$_{2}$NCH$_{2}$CH$_{2}$OH). The films grown by spin coating method were postheated in air at 650°C for 1 h and annealed in the condition of vacuum (5 $\times$ 10$^{-6}$ Torr) at 300$^{\circ}C$ for 30 min and investigated the nature of c-axis preferred orientation and physical properties with different Co concentrations. Znl_xCOxO thin films with different Co concentrations were well oriented along the c-axis, but especially a highly c-axis oriented Zn$_{l-x}$Co$_{x}$O thin film was grown at 10 at$\%$ Co concentration. The transmittance spectra showed that Zn$_{l-x}$Co$_{x}$O thin films occur typical d-d transitions and sp-d exchange interaction became activated with increasing Co concentration. The electrical resistivity of the films at 10 at$\%$ Co had the lowest value due to the highest c-axis orientation. X-ray photoelectron spectroscopy and alternating gradient magnetometer analyses indicated that no Co metal cluster was formed, and the ferromagnetic properties appeared, respectively. The characteristics of the electrical resistivity and room temperature ferromagnetism of Zn$_{l-x}$Co$_{x}$O thin films suggested the possibility for the application to dilute magnetic semiconductors.

Preparation TiO$_2$sol using aqueous system and characteristics of its thin film (수용계를 이용한 TiO$_2$Sol의 제조와 박막의 특성)

  • 김성도;조경식;김성진
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.10 no.3
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    • pp.271-277
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    • 2000
  • Transparent $TiO_2$ thin films were prepared by the sol-gel method from titanium alkoxide aqueous solution containing large quantities of water. To prepare the aqueous system sol, the chelate compound solution were prepared from each 1 mole of titanium(IV)iso-propoxide, acetylacetone and 8 moles of isopropyl-alcohol. And then the 50 moles aqueous solution with the 0.02~0.50 moles of HCI for sol stability and the 0.3 mole of polyethylene glycol for coating adhesion were precisely dropped on the chelate compound solution. $TiO_2$thin films were fabricated by dip coating, drying and heat treatment at $400^{\circ}C$ and their characteristics were investigated by XRD, SEM and UV-visible spectrometer, The neutral sol of composition with TTIP : AcAc : IPA : $H_2O$ : PEG : HCl = 1 : 1 : 8 : 50 : 0.3 : 0.15 (molar ratio) was maintained stable sol condition and without problem for coating more than 30 days. The anatase phase $TiO_2$thin film prepared from 30 times dipping, drying and heat treating showed the flat surface and the fine microstructure of fracture surface with about 2 $\mu\textrm{m}$ thickness. Transparency of these $TiO_2$thin film was 80 % in the visible region.

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A Study on the Electrochemical Properties of LiNi0.8Co0.2-xMxO2[M=Al] Cathode Materials Prepared by Sol-Gel Method (졸-겔법에 의해 제조된 정극 활물질 LiNi0.8Co0.2-xMxO2[M=Al]의 전기화학적 특성)

  • Han, Chang-Joo;Cho, Won-Il;Cho, Byung-Won;Yun, Kyung-Suk;Jang, Ho
    • Journal of the Korean Electrochemical Society
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    • v.6 no.4
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    • pp.266-270
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    • 2003
  • The $LiN_{0.8}Co_{0.2}O_2$ has shown outstanding electrochemical properties. The microstructure of $LiN_{0.8}Co_{0.2}O_2$ cathode was investigated by using TEM (transmission electron microscopy) and X-ray diffraction techniques. The $LiN_{0.8}Co_{0.2}O_2$ was produced by sol-gel method to synthesize fine particles less than $1{\mu}m$ in the average diameter. In this study, emphasis was given to the examination and interpretation of the microstructural change during charge-discharge cycling experiments, which appeared to be one of the main causes of early degradation of rechargeable batteries. Results showed that the $1{\mu}m$ cathode produced by sol-gel method had high reversible capacity and excellent cycling stability due to its homogeneous distribution of Ni and Co cations on u atomic scale. In particular, the $1{\mu}m$ cathode did not show severe strain induced structural defects or cubic spinel disordering during cycling experiments, which had been observed in the conventional $LiCoO_2$ cathode. The $LiNi_{0.8}Co_{0.2-x}M_x[M=Al]$ compounds show good reversibility but low discharge capacity.

Development and Evaluation of Natural Hydroxyapatite Ceramics Produced by the Heat Treatment of Pig Bones

  • Lim, Ki-Taek;Kim, Jin-Woo;Kim, Jangho;Chung, Jong Hoon
    • Journal of Biosystems Engineering
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    • v.39 no.3
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    • pp.227-234
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    • 2014
  • Purpose: The aim of this research was to develop and evaluate natural hydroxyapatite (HA) ceramics produced from the heat treatment of pig bones. Methods: The properties of natural HA ceramics produced from pig bones were assessed in two parts. Firstly, the raw materials were characterized. A temperature of $1,200^{\circ}C$ was chosen as the calcination temperature. Fine bone powders (BPs) were produced via calcinations and a milling process. Sintered BPs were then characterized using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR) spectroscopy, and a 2-year in vitro degradability test. Secondly, an indirect cytotoxicity test was conducted on human osteoblast-like cells, MG63, treated with the BPs. Results: The average particle size of the BPs was $20{\pm}5{\mu}m$. FE-SEM showed a non-uniform distribution of the particle size. The phase obtained from XRD analysis confirmed the structure of HA. Elemental analysis using XRF detected phosphorus (P) and calcium (Ca) with the Ca/P ratio of 1.6. Functional groups examined by FTIR detected phosphate ($PO{_4}^{3-}$), hydroxyl ($OH^-$), and carbonate ($CO{_3}^{2-}$). The EDX, XRF, and FTIR analysis of BPs indicated the absence of organic compounds, which were completely removed after annealing at $1,200^{\circ}C$. The BPs were mostly stable in a simulated body fluid (SBF) solution for 2 years. An indirect cytotoxicity test on natural HA ceramics showed no threat to the cells. Conclusions: In conclusion, the sintering temperature of $1,200^{\circ}C$ affected the microstructure, phase, and biological characteristics of natural HA ceramics consisting of calcium phosphate. The Ca-P-based natural ceramics are bioactive materials with good biocompatibility; our results indicate that the prepared HA ceramics have great potential for agricultural and biological applications.

The Effect of Magnetic Field Annealing on the Structural and Electromagnetic Properties of Bising $Co_{82}Zr_6Mo_{12}$ Thin Films for Magnetoresistance Elements (자기저항소자의 바이어스용 $Co_{82}Zr_6Mo_{12}$ 박막의 구조 및 전자기적 특성에 미치는 자장 중 열처리의 영향)

  • 김용성;노재철;이경섭;서수정;김기출;송용진
    • Journal of the Korean Magnetics Society
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    • v.9 no.2
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    • pp.111-120
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    • 1999
  • The effects of annealing in rotating magnetic field after deposition on electromagnetic properties of $Co_{82}Zr_6Mo_{12}$ thin (200~1200 $\AA$) films prepared by RF-magnetron sputtering were investigated in terms of microstructure and surface morphology. The coercivity decreases, but $4{\pi}M_5$ does not change with increasing the film thickness. The coercivity of the films was decreased below 300 $^{\circ}C$ due to stress relief and decreasing the surface roughness, while increased at 400 $^{\circ}C$ due to partial grain growth. And then, $4{\rho}M_5$ was almost independent of annealing temperatures below 200 $^{\circ}C$, but increased from 7.4 kG to 8.0 kG at 300 $^{\circ}C$ and at 400 $^{\circ}C$, which was caused by precipitation and growth of fine Co particles in the films. The electrical resistivity of films was decreased with increasing annealing temperatures and the magnetoresistance was a negative value of nearly 0 $\mu$$\Omega$cm. After annealing at 300 $^{\circ}C$, maximum effective permeability was 1200 to the hard axis of the thin films according to high frequency change. Considering the practical application of biasing layers of the films for magnetoresistive heads, optimal annealing conditions was obtained after one hour annealing at 300 $^{\circ}C$ in 400 Oe rotating magnetic field.

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Precipitation Hardening by Holding After Simulated Complete Firing in a Metal-Ceramic Alloy of Pd-Au-Ag-Sn System (금속-세라믹용 Pd-Au-Ag-Sn계 합금의 모의소성 후 계류에 따른 석출경화)

  • Kim, Min-Jung;Shin, Hye-Jung;Kwon, Yong-Hoon;Kim, Hyung-Il;Seol, Hyo-Joung
    • Korean Journal of Dental Materials
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    • v.43 no.4
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    • pp.343-349
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    • 2016
  • This experiment was carried out to examine whether the post-firing heat treatment is effective in increasing the hardness of metal-ceramic alloy of the Pd-Au-Ag-Sn system. Precipitation hardening by holding at $600^{\circ}C$ after simulated complete porcelain firing in a metal-ceramic alloy of the Pd-Au-Ag-Sn system was examined by observing the change in hardness, crystal structure, and microstructure using a hardness test, X-ray diffraction (XRD), and field emission scanning electron microscopy (FE-SEM). The hardness of the alloy increased apparently by holding the specimen at $600^{\circ}C$ for 30 min after simulated complete porcelain firing. The formation of fine grain interior precipitates during holding at $600^{\circ}C$ caused the formation of lattice strain in the grain interior, resulting in apparent hardening. The faster cooling rate (stage 0) during simulated complete porcelain firing resulted in more effective precipitation hardening during holding at $600^{\circ}C$. From the above results, an appropriate post-firing heat treatment, such as holding at $600^{\circ}C$ for 30 min after complete porcelain firing may increase the durability of metal-ceramic prostheses composed of Pd-Au-Ag-Sn alloy.