• Korean Journal of Materials Research
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• v.23 no.12
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• pp.722-726
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• 2013

Freeze drying of a porous Cu-Sn alloy with unidirectionally aligned pore channels was accomplished by using a composite powder of CuO-$SnO_2$ and camphene. Camphene slurries with CuO-$SnO_2$ content of 3, 5 and 10 vol% were prepared by mixing with a small amount of dispersant at $50^{\circ}C$. Freezing of a slurry was done at $-25^{\circ}C$ while the growth direction of the camphene was unidirectionally controlled. Pores were generated subsequently by sublimation of the camphene during drying in air for 48 h. The green bodies were hydrogen-reduced at $650^{\circ}C$ and then were sintered at $650^{\circ}C$ and $750^{\circ}C$ for 1 h. XRD analysis revealed that the CuO-$SnO_2$ powder was completely converted to Cu-Sn alloy without any reaction phases. The sintered samples showed large pores with an average size of above $100{\mu}m$ which were aligned parallel to the camphene growth direction. Also, the internal walls of the large pores had relatively small pores. The size of the large pores decreased with increasing CuO-$SnO_2$ content due to the change of the degree of powder rearrangement in the slurry. The size of the small pores decreased with increase of the sintering temperature from $650^{\circ}C$ to $750^{\circ}C$, while that of the large pores was unchanged. These results suggest that a porous alloy body with aligned large pores can be fabricated by a freeze-drying and hydrogen reduction process using oxide powders.

• Proceedings of the Korean Vacuum Society Conference
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• 2000.02a
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• pp.167-167
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• 2000

전지 재료의 충방전 과정 연구에는 X-선 분말회절(x-ray powder diffraction techniques)과 중성자회절을 많이 사용하였다. 하지만 이러한 분석기술은 long-range order의 구조에 관한 정보를 제공하는데 유용하지만 atomic scale의 구조에 관한 정보를 얻기에는 한계가 있다. Li 전지에서의 전기화학적 반응에서는 cathode 물질에 포함된 전이금속의 산화, 환원 반응에 의한 Li 이온의 intercalation (charge process)과 deintercalation (discharge process) 현상이 일어난다. 이러한 충방전 과정은 알려지지 않은 다양한 형태의 위상 변화를 동반하게 되는데 x-선 이나 중성자를 이용한 powder diffraction techniques 로는 단지 정성적인 결정학적 정보를 얻을 수 있다. 따라서 최근에 원자 단위의 local structure에 관한 정보와 electrochemical state에 관한 정보를 동시에 얻을 수 있는 X-ray Absorption Fine Structure (XAFS) 분석기술을 Li 전지분석에 활용하기 시작하였다. XAFS는 하나의 x-ray 흡수원자에 대해서 주변원자들의 원자구조에 관한 정보와 구성 원소의 electrochemical state에 관한 정보를 얻을 수 있는 분석방법이다. X-ray Induced Electron Emission Spectroscopy (XIEES)는 x-ray에 의해서 방출된 전자를 검출하여 스펙트럼을 얻는 기능을 함축적으로 나타낸 것으로, x-ray를 물질 표면에 조사하여 발생하는 광전자, Auger 전자, 이차전자 등을 전자검출기(Channel Electron Multiplier: CEM)로 검출하는 기능과, 시료를 투과한 x-ray와 시료에서 발생하는 형광 x-ray를 비례계수기로 검출하는 기능을 가지고 있다. 이러한 검출 능력을 바탕으로 EXAFS, XANES, Standing Wave Technique, Elemental Composition Analysis, DXRD, Total Reflection Technique 등을 이용하여 물질을 구성하고 있는 원소의 성분, 미세원자구조, 전자구조에 관한 정보를 얻을 수 있는 새로운 spectrometer이다. 본 연구에서는 자체 개발한 XIEES의 XAFS 기능을 이용하여 여러 가지 방법으로 제조한 LiMn2-xO4와 LiMnO2, MnO2에서 Mn K-absorption edge에 대한 chemical state 변화를 측정하였다. Absorption edge에서 chemical shift를 측정하기 위해서는 방사광 가속기 수준의 에너지 분해능(~0.3eV)이 필요하다. 이번 연구에서는 SiO2(3140) monochromator를 사용하고 여기에 맞는 적절한 parameter를 적용하여 x-ray 에너지 분해능을 포항방사광가속기 수준으로 개선하였다. XIEES에서 얻은 스펙트럼과 포항방사광가속기에서 얻은 스펙트럼을 비교하였다. Chemical shift가 일어나는 경향은 두 실험 결과가 잘 일치하였다.

• Journal of Surface Science and Engineering
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• v.50 no.1
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• pp.46-54
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• 2017

Marcel Pourbaix에 의해 만들어진 Eh-pH 도표는 화학적으로 안정한 상을 pH와 전위 (Potential or Eh)의 관점으로 도시한 것으로서 수용액 내에서 일어나는 화학반응을 부식-방식의 관점에서 이해하데 유용하게 사용되어 왔다. pH (potential of hydrogen)는 수소이온의 농도의 함수이며, Eh는 표준수소전극 (SHE, standard hydrogen electrode) 에 대한 전위를 나타낸다. 수용액에서의 도금 반응은 부식반응의 역반응이라 할 수 있으므로 도금반응도 이 도표를 이용하면 반응에 대한 열역학적 예측이 가능하다. 국내외 전기화학 및 표면공학 관련 교재들을 보면 Eh-pH 도표로 대표되는 열역학이나 분극곡선으로 대표되는 속도론에 대한 설명은 주로 부식의 관점에서 설명이 되어있어 도금을 공부하는 학생들에게는 직접적인 이해가 쉽지 않은 것이 사실이다. 저자는 출연연구소에 근무하면서 새로 들어오는 학연생(대학원생)들의 Eh-pH 도표에 대한 이해도를 알아보면 이 도표를 이해하고 이용할 줄 아는 학생이 거의 없다는 점을 안타깝게 여겨왔다. 최근에는 단순한 금속 도금이 아니라 나노 분말 합성, 반도체 물질 합성 등 여러 가지 공정기술과 응용기술이 수용액에서의 산화-환원 반응을 이용하고 있기 때문에 Eh-pH 도표의 중요성은 더해가고 있음을 느끼고 있었다. 그러던 중, 일본의 표면 처리 학술지인 표면기술(表面技術) (2013년, 64권 2호)에 'Eh-pH 도표의 표면기술에의 응용'이라는 제하의 소특집이 발간되었다. 이 소특집은 6편의 논문으로 되어 있었다. 저자는 이 소특집을 읽는 순간 이 논문들을 번역하여 표면공학회지에 소개를 하면 도금이나 전기화학을 공부하는 학생들에게 큰 도움이 될 것이라는 생각을 하였다. 본 기술해설 논문은 저자가 이 소특집에 게재된 논문을 번역하고 일부 내용은 저자의 의견으로 가감하여 표면공학회 학생 회원 및 기업의 연구원들에게 소개하기 위하여 저역을 한 것이다. 이 논문은 매 호 한편씩 소개할 예정이며, 원문을 읽고 싶다면 표면기술(表面技術)을 참조하길 바란다.

• Korean Journal of Materials Research
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• v.14 no.4
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• pp.293-299
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• 2004

Transition metal ions doped $TiO_2$ nanostructured powders were prepared with simply heating aqueous $TiOCl_2$ solutions, contained various metal ions (Ni, Al, Fe, Zr, and Nb) of 1.47 mol% added as metal-chlorides, at $100^{\circ}C$ for 4 hrs by homogeneous precipitation process under suppressing conditions of water vaporization. The characterizations for prepared $TiO_2$ powders were carried out to observe doping of metal ions, their concentrations and microstructures using XRD, UV-VIS (DRS), XPS, SEM, TEM and ICP. Also, photo-oxidative abilities were evaluated by decomposition of 4-chlorophenol (4CP) under ultraviolet light irradiations. No secondary oxide phases were formed in all the $VTiO_2$ powders, showing doping with various transition metal ions. When adding ions ($Ni^{2+}$ or$ Al^{3+ }$ and $Zr^{4+}$ ) having valance states or ionic radii greatly different from those of $Ti^{4+}$ , the $TiO_2$ powders of mixed anatase and rutile phases were formed, whereas in the case of additions of $^Fe{3+ }$ and $Nb^{ 5+}$ as well as no addition of metal ion the powders with pure rutile phase alone were formed. Among the prepared $TiO_2$ powders, Ni$^{2+}$ doped $TiO_2$ powders, containing a small amount of anatase phase, showed excellent photo-oxidative ability in 4CP decomposition because of relative decreases in electron-hole recombination and poisoning of $TiO_2$ surface during the photoreaction.n.

• Transactions of Materials Processing
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• v.27 no.1
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• pp.5-11
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• 2018

Direct energy deposition (DED) technique uses a laser heat source to deposit a metal layer on a substrate. Many researchers have used the DED technique to study the hardfacing of molds and dies. The aim of this study is to obtain high surface hardness and a sound bonding between the AISI M4 deposits and a substrate utilizing a mixed powder that contains M4 and AISI P21 powders. To prevent interfacial cracks between the M4 deposits and the substrate, the mixed powder is pre-deposited onto a JIS S45C substrate, before the deposition of M4 powders. Interfacial defects occurring between the deposits and substrate and changes in the microhardness of the intermediate layer were examined. Observations of the cross-sections of deposited specimens revealed that the interfacial cracks appeared in samples with one and two mixed layers regardless of the mixture ratio. However, the crack was removed by increasing the mixture ratio and the number of intermediate layers. Meanwhile, the microhardness in the mixed layer was found to decrease with increasing ratio of P21 powder in the mixture and that in the upper region of the deposited layers was approximately 800 HV, which was attributed to various alloying elements in the M4 powder.

• Journal of Welding and Joining
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• v.25 no.5
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• pp.45-50
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• 2007

The Ni-base superalloy GTD111 DS is used in the first stage blade of high power land-based gas turbines. Advanced repair technologies of the blade have been introduced to the gas turbine industry over recent years. The effect of the filler metal powder on Transient Liquid Phase bonding phenomenon and tensile mechanical properties was investigated on the GTD111 DS superalloy. At the filler metal powder N series, the base metal powders fully melted at the initial time and a large amount of the base metal near the bonded interlayer was dissolved by liquid inter metal. Liquid filler metal powder was eliminated by isothermal solidification which was controlled by the diffusion of B into the base metal. The solids in the bonded interlayer grew from the base metal near the bonded interlayer inward the insert metal during the isothermal solidification. The bond strength of N series filler metal powder was over 1000 MPa. and ${\gamma}'$ phase size of N series TLP bonded region was similar with base metal by influence of Ti, Al elements. At the insert metal powder M series, the Si element fluidity of the filler metal was good but microstructure irregularity on bonded region because of excessive Si element. Nuclear of solids formed not only from the base metal near the bonded interlayer but also from the remained filler metal powder in the bonded interlayer. When the isothermal solidification was finished, the content of the elements in the boned interlayer was approximately equal to that of the base metal. But boride and silicide formed in the base metal near the bonded interlayer. And these boride decreased with the increasing of holding time. The bond strength of M series filler metal powder was about 400 MPa.

• Journal of the Korean Ceramic Society
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• v.35 no.1
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• pp.23-32
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• 1998

Al2O3/Al composites were produced by immersing the sintered silica preform in molten aluminum which contained magnesium as impurity. Three distinct regions existed in the penetration behavior of molten me-tal with changing the reaction temperature. These regions are denoted as low temperature regime(75$0^{\circ}C$-85$0^{\circ}C$) intermediate regime(90$0^{\circ}C$-95$0^{\circ}C$) and high temperature regime(100$0^{\circ}C$$\leq$) In the low temperature regime the penetration speed of molten aluminum increased with increasing reaction temperature whereas it decreased in the intermediate regime due to the phase transition of alumina formed by displacement reac-tion. In the high temperature regime the penetration speed of molten aluminum was the highest at 100$0^{\circ}C$ which was 3.6 mm/hr But above 105$0^{\circ}C$ molten aluminum did not penetrate into the silica preform because of the formation of a dense spinel layer at the preform surface by magnesium in molten Al.

• Journal of the Korean Ceramic Society
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• v.50 no.6
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• pp.402-409
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• 2013

The objective of this study was to develop a synthesis process for ${\beta}$-SiC powders to reduce the synthesis temperature and to control the particle size and to prevent particle agglomeration of the synthesized ${\beta}$-SiC powders. A phenol resin and TEOS were used as the starting materials for the carbon and Si sources, respectively. $SiO_2$-C hybrid precursors with various C/Si mole ratios were fabricated using a conventional sol-gel process. ${\beta}$-SiC powders were synthesized by a carbothermal reduction process using $SiO_2$-C hybrid precursors with various C/Si mole ratios (1.6 ~ 2.5) fabricated using a sol-gel process. In this study, the effects of excess carbon and the addition of Si powders to the $SiO_2$-C hybrid precursor on the synthesis temperature and particle size of ${\beta}$-SiC were examined. It was found that the addition of metallic Si powders to the $SiO_2$/C hybrid precursor with excess carbon reduced the synthesis temperature of the ${\beta}$-SiC powders to as low as $1300^{\circ}C$. The synthesis temperature for ${\beta}$-SiC appeared to be reduced with an increase of the C/Si mole ratio in the $SiO_2$-C hybrid precursor by a direct carburization reaction between Si and excess carbon.

• Resources Recycling
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• v.26 no.3
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• pp.17-25
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• 2017

Electric arc furnace steelmaking dust has various physicochemical properties as volatile components generated in the melting process of steel scraps in an electric arc furnace, which is captured in oxide form as fine powder by reacting with oxygen in the air. In order to efficiently recycle these electric arc furnace dust, a kinetic basic experiment and a pilot production test were carried out in parallel. As a result, it was found that the electric arc furnace dust contain a large amount of Cl and alkali components, thus it was expected that the compounds have a great adverse effect on the actual operation for the recycling. It was confirmed that the volatilization behavior was progressing actively at $1100^{\circ}C$ and the electric arc furnace dust was melted at $1250^{\circ}C$. These results are the same as a result of pilot test for the formation behavior of zinc oxide and reduced iron. These results should be useful as basic data for designing the recycling plant of the electric arc furnace dust and establishing the operating conditions.

• Resources Recycling
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• v.27 no.2
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• pp.32-37
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• 2018

This study was conducted as a preliminary study for the recycling of palladium and palladium oxide. In this study, thermodynamic equations for the formation of palladium oxide (PdO) are established. Palladium chloride is dissolved into hydrochloric acid to generate a palladium chloride solution. Nanosized palladium oxide powder with an average particle size below 30 nm were generated from this raw material solution by means of a spray pyrolysis process. The palladium oxide particles were composed of a single solid crystal. The results of XRD analysis showed that only a PdO phase of the generated powder was formed. And, the specific surface area of the generated palladium powder was approximately $32m^2/g$.