• Journal of the Korean Ceramic Society
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• v.41 no.9
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• pp.703-708
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• 2004

The variation of the reaction pressure and reaction product during the reaction was investigated according to the total mass of the reaction mixture at the optimum composition for the preparation of u-Si3N4 powder which had been confirmed in the former investigation; 'Preparation of $\alpha$-Si$_3$N$_4$ powder in reaction system containing molten salt by SHS - part 1. synthesizing of powder'. When the total mass of the reaction mixture was 100g, the minimum pressure for a complete reaction was 60atm in 5L reactor, whereas the reaction was incomplete in the case that the mass exceeded 200g because of pressure increase. Also, as the mass of the reaction mixture increased, the reactivity linearly decreased. Hence, the complete reaction was realized by decreasing an initial $N_2$ pressure, and thus obtained minimum initial pressure was recorded 20 atm for the initial mixture of 500g. The reason of the incomplete reaction with pressure Increase was found to be that NH$_4$Cl vapour which was suppressed by the gas pressure acted as a diluent.

• Korean Journal of Materials Research
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• v.25 no.12
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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).

• Journal of Powder Materials
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• v.11 no.4
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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.

• Journal of the Korean Ceramic Society
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• v.41 no.3
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• pp.235-242
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• 2004

Si, NH$_4$Cl, NaN$_3$, NaCl, $N_2$ were used as raw materials for preparation of $\alpha$-Si$_3$N$_4$ powder. NH$_4$Cl and NaN$_3$ were used as additives, and NaCl was used as a diluent. Initial $N_2$ gas pressure in the SHS reactor was 60 atm. In preparation of $\alpha$-Si$_3$N$_4$, the reactivity and the properties of the products were examined with the various kinds of additives and the content of diluent. At first, the optimum reaction system for the preparation of $\alpha$-Si$_3$N$_4$ is examined and then the optimum composition was examined in the optimum reaction system. The optimum reaction system was Si-$N_2$-additive(NH$_4$Cl+NaN$_3$)-diluent(NaCl) and the optimum composition was 38 wt%Si+50 wt%(NH$_4$Cl+NaN$_3$)+12 wt%NaCl. The maximum fraction of $\alpha$-phase of Si$_3$N$_4$ produced in this condition was 96.5 wt% and the shape of the $\alpha$-Si$_3$N$_4$ produced in this condition was an irregular fiber with a length of 10 ${\mu}{\textrm}{m}$ and a diameter of 1 ${\mu}{\textrm}{m}$.

• Korean Journal of Materials Research
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• v.9 no.8
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• pp.817-824
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• 1999

The $Al_2$$O_3$-SiC composite powder was prepared by Self-propagating High-Temperature Synthesis(SHS) process using $SiO_2$Al and C powders as raw material. The effects of the molar ratio in raw material, compaction pressure, initial temperature of reactants on the products and combustion process were studied. Self-propagating high temperature synthesis of $SiO_2$/Al/C system should be preheated above $400^{\circ}C$ owing to the low combustion temperature. As the result of the combustion reaction, the purity of final product became better than that of reactants. In this system, the optimum molar ratio of $SiO_2$:Al:C was 3.0:4.0:6.0. The free carbon was removed by roasting at $650^{\circ}C$ for 30min. In this study, pressureless sintering was very dffective both for controlling the disintegration of specimen with powder bed and for obtaining dense sintered-body at $1700^{\circ}C$. The sintered-body produced with hot-pressing was about 98% of the theoretical relative density.

• Journal of Powder Materials
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• v.29 no.1
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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.

• Journal of the Korean Ceramic Society
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• v.48 no.6
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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 $SiO_2$.

• Korean Journal of Metals and Materials
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• v.50 no.3
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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.