• 한국분말재료학회지
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• 제11권1호
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• pp.28-33
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• 2004

In the present study, the focus is on the analysis of carbothermal reduction of the titanium-cobalt-oxygen based oxide powder by solid carbon for the optimizing synthesis process of ultra fined TiC/Co composite powder. The titanium-cobalt-oxygen based oxide powder was prepared by the combination of the spray drying and desalting processes using the titanium dioxide powder and cobalt nitrate as the raw materials. The titanium-cobalt-oxygen based oxide powder was mixed with carbon black, and then this mixture was carbothermally reduced under a flowing argon atmosphere. The changes in the phase structure and thermal gravity of the mixture during carbothermal reduction were analysed using XRD and TGA. The synthesized titanium-cobalt-oxygen based oxide powder has a mixture of $TiO_2$ and $CoTiO_3$. This oxide powder was transformed to a mixed state of titanium car-bide and cobalt by solid carbon through four steps of carbothermal reduction steps with increasing temperature; reduction of $CoTiO_3$ to $TiO_2$ and Co, reduction of $TiO_2$, to the magneli phase($Ti_nO_{2n-1}$, n>3), reduction of the mag-neli phase($Ti_nO_{2n-1}$, n>3) to the $Ti_nO_{2n-1}$(2$\leq$n$\leq$3) phases, and reduction and carburization of the $Ti_nO_{2n-1}$(2$\leq$n$\leq$3) phases to titanium carbide.

• 한국세라믹학회지
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• 제50권6호
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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.

• 한국분말재료학회지
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• 제9권3호
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• pp.167-173
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• 2002

A new approach to produce nanostructured WC/Co composite powders by a mechanochemical process was made to improve the mechanical properties of advanced hardmetals. Homogeneous spherical W-Co salt powders were made by spray drying of aqueous solution from ammonium metatungstate($(NH_4)_6(H_2W_{12}O_{40})\cdo4H_2O$,AMT) and cobalt nitrate hexahydrate (Co(NO$_3$)$_2$.6$H_2O$). spray dried W-Co salt powders were calcined for 1 hr at $700^{\circ}C$ in atmosphere of air. The oxide powder was mixed with carbon black by ball milling and this mixture was heated with various temperatures and times in $H_2$. The $WO_3/CoWO_4$ composite oxide powders were obtained by calcinations at $700^{\circ}C$. The primary particle size of W/Co composite oxide powders by SEM was 100 nm. The reduction/carburization time decreased with increasing temperatures and carbon additions. The average size of WC particle carburized at $800^{\circ}C$ by TEM was smaller than 50 nm.

• 한국표면공학회지
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• 제26권2호
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• pp.87-107
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• 1993

The grain size of the final products of WC-Co and WC-Ni composite powders is dependent on the size of the starting material and the conditions employed for the reduction and carburization. APT-Co and -Ni com-plex salts were prepared by the substitution reaction between ammonium ions in APT and the metal ions in Co(NO3)2 and Ni(NO3)2 solutions of different concentrations(0.1 to 0.7M) at $50^{\circ}C$ and the grain sizes of the com-plex salts was $0.54~0.76\mu\textrm{m}$. The complex which calcined the complex salts at $700^{\circ}$~80$0^{\circ}C$ for 60min. were 0.2~0.5$\mu\textrm{m}$. W-Co($5.92^{\circ}C$) and -Ni(6.95%) powders which reduced the complex oxides with H2d atmo-sphere(flow rate;600cc/min.) at $700^{\circ}$~$800^{\circ}C$ for 60min. were $0.5~0.6\mu\textrm{m}$. The mean grain sizes of WC-Co and WC-Ni composite powders which carburized both complex metals of W-Co and W-Ni at $800^{\circ}C$ for 60min. were $0.5~0.6\mu\textrm{m}$, and take place the coarsening of the grain above $800^{\circ}C$ and the optmium ratio of C3H8 and H2 was 0.2 for the control of the free carbon. The effect of Co contents on the particle sizes decreased from 0.4 to $0.25\mu\textrm{m}$ with increasing the content from 2.0 to 7.6w%. The activation energies on the reductions of oxides and the formations of carbides were as follows ; W-Co : Q = 8.7 kcal/mole, W-Ni : Q = 8.1 kcal/mole, WC-Co pow-der : Q = 17.8 kcal/mole, WC-Ni powder : Q = 16.6 kcal/mole.

• 보존과학회지
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• 제38권3호
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• pp.217-233
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• 2022

경주 금척리 유적은 5세기 후반에서 6세기 전반에 조성된 금척리고분군(사적 제43호)과 매우 연접하며, 유적이 위치한 지역은 그 일대의 유력 지배세력의 무덤으로 알려져 있다. 신라성장에 일익을 담당했던 인근 유적과도 밀접한 관련성이 있을 것으로 추정되는 경주 금척리 유적에서 출토된 철기를 대상으로 금속학적 방법론을 도입한 연구를 진행하였다. 철기의 용도에 따른 제작기법 차이를 확인하기 위해 용도별로 분류하여 8점을 선정하고, 미세조직 및 비금속개재물을 연구하였다. 분석 결과 제작 공정은 탄소함량이 높은 소재를 사용하여 형상을 단조하는 방법과 탄소함량이 낮은 소재를 사용하여 형상 단조만을 하는 기법, 형상 단조 후 필요에 따라 강도를 높이기 위한 침탄작업을 실시하는 기법이 적용된 것으로 확인된다. 이후 부위별 기능을 고려한 제강법과 열처리기술을 선택적으로 적용하여 기계적 성질을 향상시켰으며 제련공정에는 저온환원법이 적용되었을 가능성이 크다. 또한 경주 중심부와 외곽에 위치한 유적에서 출토된 철기 유물과 비교해본 결과 제련 및 제작기술에서 상호 유사한 것이 확인된다.

• 자원리싸이클링
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• 제13권5호
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• pp.45-50
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• 2004

탄화철을 합성하는 공정을 수소($H_2$) 환원과 $CO-H_2$ 혼합가스에 의한 탄화의 2단계 과정으로 나누어서 수행했다. 환원종료 후 미량의 암모니아 가스를 첨가하여 환원철의 표면을 개질한 후, 탄화시간 경과별 탄화상태를 C/S 분석기(Low C/S determinator), 뫼스바우어 분광 분석기(Mossbauer spectroscopy), XRD(X-ray diffraction patterns), SEM(Scanning electron microscopy), TEM(Transmission electron microscopy), XPS(Photoelectron spectroscopy), 및 라만분광기 (Raman spectroscopy)를 사용하여 조사하였다. 연구결과, 미량의 암모니아가스로 환원철 표면을 개질함으로써 탄화철의 분해 및 유리탄소의 석출을 방지할 수 있을 뿐만아니라 6.68wt% 이상 10wt% 까지 탄소가 과고용된 상태에서도 분해되거나 유리탄소를 석출하지 않고 안정상태를 유지하였다. 이러한 결과로부터 철(Fe)과 세멘타이트(cementite, $Fe_3C$)가 혼합되지 않고 고탄화철(SIC, super iron carbide)인 Fe5C2 상태의 안정한 단일상을 얻는데 성공하였다.