• 한국세라믹학회지
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• 제41권9호
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• pp.703-708
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• 2004

앞선 논문 분말의 제조에서 정립한 $\alpha$-Si$_3$N$_4$ 분말의 제조를 위한 최적의 조성에서 반응 혼합물의 양에 따른 압력 및 생성물의 변화를 관찰하였다. 5L 반응기 내에서 반응 혼합물의 양이 100g일 때 필요한 최저 $N_2$ 압력은 60atm이었다. 그러나 반응 혼합물의 양이 200g 이상일 때부터 반응기 내부의 압력 증가로 인해 반응은 완료될 수 없었으며, 혼합물이 증가할수록 반응율은 직선적으로 감소하였다. 반응물의 양이 증가할수록 최초 반응기 내부의 $N_2$압력을 감소시킴으로써 반응을 완료시킬 수 있었으며, 500g일 때 초기 $N_2$ 압력을 약 20atm까지 감소시킴으로써 반응은 완료될 수 있었다. 반응이 중간에 멈추는 원인은 반응기 내부의 압력 증가로 인해 기화되지 못한 채 혼합물 안에 존재한 NH$_4$Cl때문인 것으로 밝혀졌다.

• 한국재료학회지
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• 제25권12호
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• pp.659-665
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• 2015

The self-propagating high temperature synthesis approach was applied to synthesize amorphous boron nano-powders in argon atmospheres. For this purpose, we investigated the characteristics of a thermally induced combustion wave in the $B_2O_3+{\alpha}Mg$ system(${\alpha}=1.0-8.0$) in an argon atmospheres. In this study, the exothermic nature of the $B_2O_3-Mg$ reaction was investigated using thermodynamic calculations. Experimental study was conducted based on the calculation data and the SHS products consisting of crystalline boron and other compounds were obtained starting with a different initial molar ratio of Mg. It was found that the $B_2O_3$ and Mg reaction system produced a high combustion temperature with a rapid combustion reaction. In order to regulate the combustion reaction, NaCl, $Na_2B_4O_7$ and $H_3BO_3$ additives were investigated as diluents. In an experimental study, it was found that all diluents effectively stabilized the reaction regime. The final product of the $B_2O_3+{\alpha}Mg$ system with 0.5 mole $Na_2B_4O_7$ was identified to be amorphous boron nano-powders(< 100 nm).

• 한국분말재료학회지
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• 제11권4호
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• pp.294-300
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• 2004

This study for preparation of aluminum nitride (AlN) with high purity was carried out by self-propagating high-temperature synthesis method in two different systems, $Al-N_{2}$ and $Al-N_{2}$-AlN, with the change of nitrogen gas pressure and dilution factor. On the occasion of $Al-N_{2}$ system, unreacted aluminum was detected in the product in spite of high nitrogen pressure, 10 MPa, This may be caused by obstructing nitrogen gas flow to inner part of molten and agglomerate of aluminum, formed in pre-heating zone. In $Al-N_{2}$-AlN system, AlN with a purity of 95% or ever can be prepared in the condition of $f_{Dil}\geq0.5$, $P_{N_{2}}\geq$ 1 MPa, and the purity can be elevated to 98% over in the condition of $f_{Dil}$ = 0.7 and $P_{N_{2}}$ = 10 MPa.

• 한국세라믹학회지
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• 제41권3호
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• pp.235-242
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• 2004

원재료로서 Si, NH$_4$Cl, NaN$_3$, NaCl을 사용하고 SHS법을 이용하여 $\alpha$-Si$_3$N$_4$ 분말을 제조하였다. NH$_4$Cl과 NaN$_3$는 첨가제로서, NaCl은 희석제로서 사용되었고 반응기내 최초 $N_2$ 압력은 60 atm이었다. $\alpha$-Si$_3$N$_4$분말을 제조함에 있어, 첨가제의 종류와 조성, 희석제의 첨가량에 따른 반응성 및 생성물의 특성을 조사하였는데, 우선 $\alpha$-Si$_3$N$_4$ 분말의 제조를 위한 최적의 반응계를 조사하였고, 최적의 반응계에서 최적의 조성을 확립하였다. 최적의 반응계는 Si-$N_2$-additive(NH$_4$C+NaN$_3$)-diluent(NaCl)이었고, 이때 최적의 조성은 38wt%Si+22.5wt%NH$_4$Cl+27.5wt%NaN$_3$+l2wt%NaCl이었다. 이 조건에서 생성된 최고 $\alpha$-Si$_3$N$_4$의 분율은 96.5wt%이었으며 생성된 분말의 입형은 길이가 약 10 $mu extrm{m}$이고 직경이 약 1 $\mu\textrm{m}$인 일방향으로 길게 성장한 부정형의 fiber 형태였다.

• 한국재료학회지
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• 제9권8호
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• pp.817-824
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• 1999

$Al_2$$O_3$-SiC 화합물 분말이 $SiO_2$, A1 그리고 C 분말들을 원료분말로 하여 SHS(self-propagating High-temperature Synthesis)법에 의해 제조되었다. 원료 분말에서의 몰비, 성형압력, 반응물의 초기온도의 영향이 생성물과 연소과정에 대해 연구되었다. $SiO_2$/A1/C계의 자전연소합성은 낮은 연소온도 때문에 $400^{\circ}C$ 이상으로 예열되어야 한다. 연소반응의 결과로서 최종생성물의 순도는 반응물의 순도보다 높았다. 이 계에서 $SiO_2$:Al:C의 적당한 몰비는 3.0:4.0:6.0이었고, free carbon은 30min 동안 $650^{\circ}C$에서 배소함으로써 제거되었다. 본 연구에서 상압소결은 $1700^{\circ}C$에서 powder bed를 사용한 표본의 분해를 제어하고 치밀한 소결체를 얻는데 매우 효과적이었다. hot-pressing으로 생성된 소결체는 이론비교밀도의 약 98%이었다.

• 한국분말재료학회지
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• 제29권1호
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• pp.47-55
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• 2022

Tungsten carbide is widely used in carbide tools. However, its production process generates a significant number of end-of-life products and by-products. Therefore, it is necessary to develop efficient recycling methods and investigate the remanufacturing of tungsten carbide using recycled materials. Herein, we have recovered 99.9% of the tungsten in cemented carbide hard scrap as tungsten oxide via an alkali leaching process. Subsequently, using the recovered tungsten oxide as a starting material, tungsten carbide has been produced by employing a self-propagating high-temperature synthesis (SHS) method. SHS is advantageous as it reduces the reaction time and is energy-efficient. Tungsten carbide with a carbon content of 6.18 wt % and a particle size of 116 nm has been successfully synthesized by optimizing the SHS process parameters, pulverization, and mixing. In this study, a series of processes for the high-efficiency recycling and quality improvement of tungsten-based materials have been developed.

• 한국세라믹학회지
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• 제48권6호
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• pp.559-564
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• 2011

In order to investigate the behavior of $SiO_2$ in the molybdenum silicide powders, crystal structure of these powders was measured by XRD, in addition, surface composition and surface phase (or chemical states) and microstructure were analysed by XPS and TEM, respectively. Mo-silicide powders containing $SiO_2$ were synthesized by SHS (Self-Propagating High-Temperature Synthesis) technique. In XRD result, according to increase of $SiO_2$ contents, the crystal structure for synthesized $MoSi_2$ powders was still typical $MoSi_2$ bct without any other phases. By XPS analysis, the surface of Mo and Si source powders was covered with $MoO_3$ and $SiO_2$, respectively, and the surface of synthesized $MoSi_2$ powder was also covered with $MoO_3$ and $SiO_2$, which were stable oxides at room temperature. However, according to increase of $SiO_2$ addition, $MoSi_2$ phase in XPS spectra decreased and $SiO_2$ phase increased relatively in synthesized $MoSi_2$ powders. From the results by XPS and XRD, we found that the existent $SiO_2$ has amorphous structure. In the microstructure, the small particulates of the synthesized products added $SiO_2$ agglomerated together to form larger clusters (from ~10 nm to ~1 ${\mu}m$). From TEM, XPS, and XRD results, we found that the out layer of agglomeration of synthesized $MoSi_2$ powder is surrounded by amorphous $SiO_2$.

• 대한금속재료학회지
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• 제50권3호
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• pp.256-262
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• 2012

This study investigated the hydrogen storage properties of Zr-Based $AB_{2-x}M_x$ metal hybride made by HCS (Hydriding Combustion Synthesis). The materials were prepared by HCS 80 wt% $AB_2$-15 wt% Mg-5 wt% Mm, HCS 80 wt% $AB_2$-20 wt% Mg and pure Zr-Based $AB_2$, These materials were activated at 298 K under 20 bar. Both HCS 80 wt% $AB_2$-20 wt% Mg and HCS 80 wt% $AB_2$-15 wt% Mg-5 wt% Mm were absorbed within 1 minute. In the case of the $AB_2$, it was perfectly absorbed within 6 minutes. Then, the materials were evaluated to obtain P-C-T (Pressure-Composition-Temperature) curves at 298K. As a result, the hydrogen storage capacity of HCS 80 wt% $AB_2$-20 wt% Mg, HCS 80 wt% $AB_2$-15 wt% Mg-5 wt% Mm and pure Zr-Based $AB_2$ were determined to be 1.2, 1.6 and 1.74 wt%, respectively. The activation energy and rate controlling step were calculated by the Johnson-Mehl Avrami equation. The activation energies of HCS 80 wt% $AB_2$-20 wt% Mg, HCS 80 wt% $AB_2$-15 wt% Mg-5 wt% Mm and pure Zr-Based $AB_2$ were 26.91, 20.45, and 60.41 kJ/mol, respectively. Also, the values of ${\eta}$ in the Johnson-Mehl Avrami equation for HCS 80 wt% $AB_2$-20 wt% Mg, HCS 80 wt% $AB_2$-15 wt% Mg-5 wt% Mm and pure Zr-Based $AB_2$ are 0.60, 0.51, and 0.44. So, the rate controlling steps which indicate hydrogen storage mechanism are an one dimensional diffusion process.