• Title/Summary/Keyword: Porous microstructure

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Reaction Path of Cu2ZnSnS4 Nanoparticles by a Solvothermal Method Using Copper Acetate, Zinc Acetate, Tin Chloride and Sulfur in Diethylenetriamine Solvent

  • Chalapathy, R.B.V.;Jung, Gwang Sun;Ko, Young Min;Ahn, Byung Tae;Kown, HyukSang
    • Current Photovoltaic Research
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    • v.1 no.2
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    • pp.109-114
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    • 2013
  • $Cu_2ZnSnS_4$ (CZTS) nanoparticles were synthesized by a solvothermal method using copper (II) acetate, zinc acetate, tin chloride, and sulfur in diethylenetriamine solvent. Binary sulfide particles such as CuS, ZnS, SnS, and $SnS_2$ were obtained at $180^{\circ}C$; single-phase CZTS nanoparticles were obtained at $280^{\circ}C$. CZTS nanoparticles with spherical shape and grain size of 40 to 60 nm were obtained at $280^{\circ}C$. In the middle of 180 and $280^{\circ}C$, CZTS and ZnS phases were found. The time variation of reaction at $280^{\circ}C$ revealed that an amorphous state formed first instead of binary phases and then the amorphous phase was converted to crystalline CZTS state; it is different reaction path way from conventional solid-state reaction path of which binary phases react to form CZTS. CZTS films deposited and annealed from single-phase nanoparticles showed porous microstructure and poor adhesion. This indicates that a combination of CZTS and other flux phase is necessary to have a dense film for device fabrication.

Fabrication of Metallic Particle Dispersed Ceramic Based Nanocomposite Powders by the Spray Pyrolysis Process Using Ultrasonic Atomizer and Reduction Process

  • Choa, Y.H.;Kim, B.H.;Jeong, Y.K.;Chae, K.W.;T.Nakayama;T. Kusunose;T.Sekino;K. Niibara
    • Journal of Powder Materials
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    • v.8 no.3
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    • pp.151-156
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    • 2001
  • MgO based nanocomposite powder including ferromagnetic iron particle dispersions, which can be available for the magnetic and catalytic applications, was fabricated by the spray pyrolysis process using ultra-sonic atomizer and reduction processes. Liquid source was prepared from iron (Fe)-nitrate, as a source of Fe nano-dispersion, and magnesium (Mg)-nitrate, as a source of MgO materials, with pure water solvent. After the chamber were heated to given temperatures (500~$^800{\circ}C$), the mist of liquid droplets generated by ultrasonic atomizer carried into the chamber by a carrier gas of air, and the ist was decomposed into Fe-oxide and MgO nano-powder. The obtained powders were reduced by hydrogen atmosphere at 600~$^800{\circ}C$. The reduction behavior was investigated by thermal gravity and hygrometry. After reduction, the aggregated sub-micron Fe/MgO powders were obtained, and each aggregated powder composed of nano-sized Fe/MgO materials. By the difference of the chamber temperature, the particle size of Fe and MgO was changed in a few 10 nm levels. Also, the nano-porous Fe-MgO sub-micron powders were obtained. Through this preparation process and the evaluation of phase and microstructure, it was concluded that the Fe/MgO nanocomposite powders with high surface area and the higher coercive force were successfully fabricated.

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Characteristics of Plasma Electrolytic Oxidation Coatings on Mg-Zn-Y Alloys Prepared by Gas Atomization (가스 분사법으로 제조한 Mg-Zn-Y 합금의 플라즈마 전해 산화 피막 특성에 관한 연구)

  • Chang, Si-Young;Cho, Han-Gyoung;Lee, Du-Hyung;Kim, Taek-Soo
    • Journal of Powder Materials
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    • v.14 no.6
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    • pp.372-379
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    • 2007
  • The microstructure, mechanical and electrochemical properties of plasma electrolytic coatings (PEO) coatings on Mg-4.3 wt%Zn-1.0 wt%Y and Mg-1.0 wt%Zn-2.0 wt%Y alloys prepared by gas atomization, followed by compaction at 320 for 10 min under the pressure of 700 MPa and sintering at 380 and 420 respectively for 24 h, were investigated, which was compared with the cast Mg-1.0 wt%Zn alloy. All coatings consisting of MgO and $Mg_2SiO_4$ oxides showed porous and coarse surface features with some volcano top-like pores distributed disorderly and cracks between pores. In particular, the surface of coatings on Mg-1.0 wt%Zn-2.0 wt%Y alloy showed smaller area of pores and cracks compared to the Mg-4.3 wt%Zn-1.0 wt%Y and Mg-1.0 wt%Zn alloys. The cross section micro-hardness of coatings on the gas atomized Mg-Zn-Y alloys was higher than that on the cast Mg-1.0 wt%Zn alloy. Additionally, the coated Mg-1.0 wt%Zn-2.0 wt%Y alloy exhibited the best corrosion resistance in 3.5%NaCl solution. It could be concluded that the addition of Y has a beneficial effect on the formation of protective and hard coatings on Mg alloys by plasma electrolytic oxidation treatment.

Micromorphometric change of implant surface conditioned with tetracycline-HCI : $FBR^{(R)}$ and CeliNest surface (표면처리 시간에 따른 임프란트 미세구조의 변화 : $FBR^{(R)}$과 CellNest 표면 임프란트)

  • Chang, Dong-Wook;Park, Joon-Bong;Kwon, Young-Hyuk;Herr, Yeek;Chung, Jong-Hyuk
    • Journal of Periodontal and Implant Science
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    • v.36 no.3
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    • pp.717-729
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    • 2006
  • The present study was performed to evaluate the effect of tetracycline-BCL on the change of implant surface microstructure according to application time. Implant with pure titanium machined surface, double coated $FBR^{(R)}$ surface and oxidized CellNest surface were utilized. Implant surface was rubbed with $50mg/m{\ell}$ tetracycline-BCL solution for ${\frac{1}{2}}$, 1, $1{\frac{1}{2}}$, 2 and $2{\frac{1}{2}}$min. respectively in the test group. Then, specimens were processed for scanning electron microscopic observation. The results of this study were as follows. 1. Both test and control group showed a few shallow grooves and ridges in pure titanium machined surface implants. There were not significant differences between two groups. 2. The double coated $FBR^{(R)}$ surfaces showed fine crystalline structures. The roughness of surfaces conditioned with tetracycline-BCL was lessened relative to the application time. 3. The oxidized CellNest surfaces showed the porous structures. The surface conditioning with tetracycline-BCI influenced on its micro-morphology. In conclusion, the detoxification of the affected implant surface with $50mg/m{\ell}$ tetracycline-BCL should be applied respectively with different time according to various implant surfaces.

A Study on Sintering and mechanical Properties of Sinter/HIPed SiC Whisker/$Al_2O_3$ Composite (Sinter/HIP 공정으로 제조한 SiC whisker/$Al_2O_3$ 복합재료의 소결 및 기계적 물성에 관한 연구)

  • Lee, Chae-Hyun;Kim, Jong-Ock;Kim, Chong-Hee
    • The Journal of Natural Sciences
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    • v.8 no.1
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    • pp.53-59
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    • 1995
  • Effects of sintering additives and sintering temperatures on the sintering behavior and mechanical properties of SiC whisker reinforced alumina composites have been investigated in this study. Dense (>95% TD) composites were obtained by using 2 wt% $Y_2O_3$ as liquid phase sintering additive. But only porous composite could be obtained when the sintering additives were MgO and $TiO_2$, which were known as the sintering additives for solid state sintering of alumina. Bending strength and fracture toughness were enhanced by reinforcement of SiC whisker. It is belived from the microstructure investigation that the enhanced by strength and toughness could be attribute to the reinforcing and grain growth inhibition effects of SiC whisker. After HIP treatment, fully dense composites were obtained and further enhanced mechanical properties achieved.

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Effect of Milling Time on Pore Size and Distribution of Ti-Nb-Zr Biomaterials with Space Holder Consolidated by Spark Plasma Sintering

  • Kim, Dong-Gun;Woo, Kee-Do;Kang, Dong-Soo;Lee, Tack
    • Korean Journal of Materials Research
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    • v.24 no.2
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    • pp.111-115
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    • 2014
  • Titanium and its alloys are useful for implant materials. In this study, porous Ti-Nb-Zr biomaterials were successfully synthesized by powder metallurgy using a $NH_4HCO_3$ as space holder and $TiH_2$ as foaming agent. Consolidation of powder was accomplished by spark plasma sintering process(SPS) at $850^{\circ}C$ under 30 MPa condition. The effect of high energy milling time on pore size and distribution in Ti-Nb-Zr alloys with space holder($NH_4HCO_3$) was investigated by optical microscope(OM), scanning electron microscope(SEM) & energy dispersive spectroscopy(EDS) and X-ray diffraction(XRD). Microstructure observation revealed that, a lot of pores were uniformly distributed in the Ti-Nb-Zr alloys as size of about $30-100{\mu}m$ using mixed powder and milled powders. In addition, the pore ratio was found to be about 5-20% by image analysis, using an image analyzer(Image Pro Plus). Furthermore, the physical properties of specimens were improved with increasing milling time as results of hardness, relative density, compressive strength and Young's modulus. Particularly Young's modulus of the sintered alloy using 4h milled powder reached 52 GPa which is similar to bone elastic modulus.

High Temperature Properties of Vanadium and Molybdenum Added High Silicon Ductile Iron (바나듐과 몰리브덴이 첨가된 고규소 구상흑연주철의 고온특성)

  • Park, Heung-Il;Jeong, Hae-Yong
    • Journal of Korea Foundry Society
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    • v.27 no.5
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    • pp.203-208
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    • 2007
  • The high temperature properties of vanadium and molybdenum added high silicon ductile iron, so called V-Mo-Si ductile iron, were investigated. The (V,Mo) complex carbides and Mo carbides precipitated at the cellular boundaries of the as-cast specimens. The microhardness of the (V,Mo) carbides were in the range of 553-619, while that of the Mo carbides in the range of 341-390. The thermo-mechanical tests were carried out with a Gleeble system at 700 and $800^{\circ}C$ under vacuum condition. The tensile strengths of the specimen tested at $700^{\circ}C$ with the dynamic deformation rate of 50 mm/sec and those with the static deformation rate of 0.15 mm/sec were 235.7 and 115.3 MPa, while the reduction in area were 23.7 and 22.4%, respectively. At the high dynamic deformation rates, the tensile strength was steeply increased due to promoting the brittle fracture of pearlite in the matrix of the specimens. But the changes of the reduction in area with the deformation rates on the same specimens were negligible. The weight gain of the V-Mo-Si specimens oxidized in the air atmosphere for 6 hours at 800 and $900^{\circ}C$ were 1.1 and 4.1.%, respectively. The cross-sectional microstructure of oxidized specimens consisted of the porous external scale layer grown outside from the original surface, the dense internal scale layer grown into the original surface, the decarburized ferrite layer between the internal scale and the matrix of base metal. The (V,Mo) carbides and Mo carbides formed in the matrix of as-cast specimen did not decompose during oxidation at 900 for 24 hours in air atmosphere.

The Effect of Seawater on Hydration of Clinker Minerals (I) Effects of SO42- and Cl- ions (시멘트 클린커 광물의 수화에 미치는 해수성분의 영향 (I)SO42- 및 Cl-이온에 의한 영향)

  • 신도철;송태웅;한기성;최상흘
    • Journal of the Korean Ceramic Society
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    • v.24 no.1
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    • pp.77-85
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    • 1987
  • Hardened cement paste is mainly affected by corrosion of sulphate and chlorine ions in sea water. In this investigation, many specimens were made with the cement clinker minerals such as C3S, C3A, C4AF and their mixture according to cement composition added various blending materials. After the specimens were immersed in 4% MgSO4 and MgCl2 solutions, the product of reaction, the microstructure of specimen and Ca+2 ion leached in the solution were studied. The formation of Ca(OH)2 in the specimen of C3S is reduced relatively by adding pozzolanic admixtures. The chlorine ion is easily diffuse into the C3S specimen and produced CaCl2 compound, and it makes the specimen porous by leaching out itself into the solution. The specimen of C3A, C4AF are broken down by expanding reaction of ettringite and gypsum compound produced in the MgSO4 solution. At a later period, the ettringite is transformed into gypsum and 5MgO.2Al2O3·15H2O. The C3A in the MgCl2 solution combines chlorine ion to form Friedel's salt and prevents the diffusion reaction of chlorine ion into the specimen. Granulated slag shows inferior effect on the resistance of the specimen in MgSO4 solution by forming ettringite and gypsum, but good result in MgCl2 solution. Pozzolanic materials, on the whole, offer noticable effect on the resistance of the specimen in both solutions.

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Fabrication of NiO-Y:BaZrO3 Composite Anode for Thin Film-Protonic Ceramic Fuel Cells using Tape-Casting

  • Bae, Kiho;Noh, Ho-Sung;Jang, Dong Young;Kim, Manjin;Kim, Hyun Joong;Hong, Jongsup;Lee, Jong-Ho;Kim, Byung-Kook;Son, Ji-Won;Shim, Joon Hyung
    • Journal of the Korean Ceramic Society
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    • v.52 no.5
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    • pp.320-324
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    • 2015
  • Optimization of the fabrication process of NiO-yttrium doped barium zirconate (BZY) composite anode substrates using tape-casting for high performance thin-film protonic ceramic fuel cells (PCFCs) is investigated. The anode substrate is composed of a tens of microns-thick anode functional layer laminated over a porous anode substrate. The macro-pore structure of the anode support is induced by micron-scale polymethyl methacrylate (PMMA) pore formers. Thermal gravity analysis (TGA) and a dilatometer are used to determine the polymeric additive burn-out and sintering temperatures. Crystallinity and microstructure of the tape-cast NiO-BZY anode are analyzed after the sintering.

Effect of Reaction Conditions on the Particle Properties for Synthesis of Stabilized Zirconia by Modified Oxalate Method

  • Park, Hyun-wook;Lee, Young Jin;Kim, Jin-Ho;Jeon, Dae-Woo;Hwang, Hae Jin;Lee, Mi Jai
    • Journal of the Korean Ceramic Society
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    • v.53 no.5
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    • pp.529-534
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    • 2016
  • Nanocrystalline powder of zirconia stabilized with 8 mol% yttria (YSZ) has been synthesized through oxalate process using $ZrOCl_2{\cdot}8H_2O$ and $Y(NO_3)_3{\cdot}6H_2O$ as starting materials. Understanding of the characteristic changes of YSZ powder as a function of processing conditions is crucial in developing dense and porous microstructures required for fuel cell applications. In this research, microstructure change, surface area, particle shape and particle size were measured as a function of different processing conditions such as calcination temperature, stirring speed and concentration of starting materials. The resultant crystallite sizes were calculated by XRD-LB (X-Ray Diffraction Line-Broadening) method, BET method, and morphology of the crystal was observed in TEM and FE-SEM. The TEM examination showed that the powder synthesized with 0.7 M of YSZ concentration had a spherical morphology with sizes ranging from 20 to 40 nm. However, the powder was gradually aggregated above 1.0 M of YSZ concentration with the aggregation being intensified as the YSZ concentration was increased.