• Title/Summary/Keyword: Carbothermal reduction

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Preparation of Aluminum Nitride from an Alkoxide and its Properties (알콕사이드로부터 AlN분말의 합성 및 분말 특성)

  • 이홍림;박세민;조덕호
    • Journal of the Korean Ceramic Society
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    • v.26 no.1
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    • pp.100-108
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    • 1989
  • Aluminum hydroxides were prepared by the alkoxide hydrolysis method using Al-isopropoxide as a starting material and NH4OH as a catalytic agent. When Al-isopropoxide was hydrolyzed in a H2O-NH3 system, only Al(OH)3 was obtained over all pH values. However, AlOOH was formed besides Al(OH)3 when Al-isopropoxide was hydrolyzed in a H2O-NH3-isopropyl alcohol system. The AlOOH/Al(OH)3 ratio was increased as the isopropyl alcohol content was increased. The hydroxides, Al(OH)3 and AlOOH, obtained in this study and the commerical products, $\alpha$-Al2O3 and AlOOH were subjected to the carbothermal reduction and nitridation reaction to product AlN powder, using carbon black as a reducing agent under N2 atmosphere at various temperatures. AlN was synthesized from the obtained Al(OH)3 and the commercial AlOOH at 145$0^{\circ}C$, however, synthesized from the obtained AlOOH and the commercial alpha-alumina at 135$0^{\circ}C$. The temperature difference is assumed to be attributed to the reactivity of those powders. AlN powder prepared from the Al-isopropoxide was observed to have the narrower particle size distribution than that prepared from the commercial $\alpha$-Al2O3 or AlOOH.

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Synthesis of $\alpha$-Sialon Ceramics from an Alkoxide and Their Mechanical Properties(I) (알콕사이드로부터 $\alpha$-Sialon 세라믹스의 제조 및 기계적 성질(I))

  • 이홍림;윤창현;조덕호
    • Journal of the Korean Ceramic Society
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    • v.28 no.2
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    • pp.130-140
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    • 1991
  • The powders of the system Si3N4-Y2O3-AlN were prepared using Si(OC2H5)4 and YCl3.6H2O together with commercial AlN powder. $\alpha$-Si3N4 was prepared by the carbothermal reduction and nitridation of the hydrolyzed gel at 135$0^{\circ}C$ for 10h in N2 atmosphere. YCl3.6H2O was observed to be changed to Y2O3 during the reaction. $\alpha$-Sialon(X=0.2, 0.4, 0.6) ceramics were obtained by hot-pressing the Si3N4-Y2O3-AlN mixture at 178$0^{\circ}C$ for 1h under 30 MPa. The content of $\alpha$-Sialon increased with increasing metal solubility(x value) and $\alpha$-Sialon single phase was obtained at the metal solubility of 0.6. With increasing metal solubility, flexural strength, fracture toughness and thermal shock resistence were decreased, while the microhardness was increased. Large elongated $\beta$-Si3N4 grains were mainly observed at lower metal solubility. Mechanical prorerties of the sintered ceramics with X=0.2 were measured as follows : flexural strength ; 650 MPa, fracture toughness ; 3.63 MN/m3/2, hardness ; 14.7 GPa, thermal shock resistence temperature ; 58$0^{\circ}C$.

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Synthesis of Silicon Carbide Whiskers (II): Stacking Faults (탄화규소 휘스커의 (II): 적층결함)

  • 최헌진;이준근
    • Journal of the Korean Ceramic Society
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    • v.36 no.1
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    • pp.36-42
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    • 1999
  • Stacking faults in SiC whiskers grown by three different growth mechanisms; vapor-solid(VS), two-stage growth(TS), and vapor-liquid-solid (VLS) mechanism in the carbothermal reduction system were investigated by X-ray diffraction(XRD) and transmission electron microscopy (TEM). The content of stacking faults in SiC whiskers increased with decreasing the diameter of whiskers, i.e., the small diameter whiskers (<1 $\mu\textrm{m}$) grown by the VS, TS, and VLS mechanisms have heavy stacking faults whereas the large diameter whiskers(>2$\mu\textrm{m}$) grown by the VLS mechanism have little stacking faults. Heavy stacking faults of small diameter whiskers was probably due to the high specific lateral surface area of small diameter whiskers.

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A Synthesis of High Purity Single-Walled Carbon Nanotubes from Small Diameters of Cobalt Nanoparticles by Using Oxygen-Assisted Chemical Vapor Deposition Process

  • Byon, Hye-Ryung;Lim, Hyun-Seob;Song, Hyun-Jae;Choi, Hee-Cheul
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.2056-2060
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    • 2007
  • A successful combination of “oxygen-assisted chemical vapor deposition (CVD) process” and Co catalyst nanoparticles to grow highly pure single walled carbon nanotubes (SWNTs) was demonstrated. Recently, it was reported that addition of small amounts of oxygen during CVD process dramatically increased the purity and yield of carbon nanotubes. However, this strategy could not be applied for discrete Fe nanoparticle catalysts from which appropriate yields of SWNTs could be grown directly on solid substrates, and fabricated into field effect transistors (FETs) quite efficiently. The main reason for this failure is due to the carbothermal reduction which results in SiO2 nanotrench formation. We found that the oxygen-assisted CVD process could be successfully applied for the growth of highly pure SWNTs by switching the catalyst from Fe to Co nanoparticles. The topological morphologies and p-type transistor electrical transport properties of the grown SWNTs were examined by using atomic force microscope (AFM), Raman, and from FET devices fabricated by photolithography.

Effect of SiC Filler Content on Microstructure and Flexural Strength of Highly Porous SiC Ceramics Fabricated from Carbon-Filled Polysiloxane (SiC 필러 함량이 탄소 함유 Polysiloxane으로부터 제조된 고기공률 탄화규소 세라믹스의 미세조직과 꺾임강도에 미치는 영향)

  • Eom, Jung-Hye;Kim, Young-Wook;Song, In-Hyuck
    • Journal of the Korean Ceramic Society
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    • v.49 no.6
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    • pp.625-630
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    • 2012
  • Highly porous silicon carbide (SiC) ceramics were fabricated from polysiloxane, SiC and carbon black fillers, AlN-$Y_2O_3$ additives, and poly (ether-co-octene) (PEOc) and expandable microsphere templates. Powder mixtures with a fixed PEOc content (30 wt%) and varying SiC filler contents from 0-21 wt% were compression-molded. During the pyrolysis process, the polysiloxane was converted to SiOC, the PEOc generated a considerable degree of interconnected porosity, and the expandable microspheres generated fine cells. The polysiloxane-derived SiOC and carbon black reacted and synthesized nano-sized SiC with a carbothermal reduction during a heat-treatment. Subsequent sintering of the compacts in a nitrogen atmosphere produced highly porous SiC ceramics with porosities ranging from 78 % to 82 % and a flexura lstrength of up to ~7 MPa.

Gold/Copper Bi-Metallic Catalysts by Carbothermal Method for CO2 Reduction

  • Yoon, Hee-chan;Jung, Woo-bin;Jung, Hee-Tae
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 2019.10a
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    • pp.83-83
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    • 2019
  • Increasing the CO2 concentration in the atmosphere induce high temperature and rising sea levels. So the technology that capture and reuse of the CO2 have been recently become popular. Among other methods, CRR(CO22 reduction reaction) is typical method of CO2 reusing. Electrocatalyst can show more higher efficiencies in CRR than photocatalyst because it doesn't use nature source. Nowadays, finding high efficient electrocatalyst by controlling electronic (affected by stoichiometry) and geometric (affected by atomic arrangement) factors are very important issues. Mono-atomic electro-catalyst has limitations on controlling binding energy because each intermediate has own binding energy range. So the Multi-metallic electro-catalyst is important to stabilize intermediate at the same time. Carbon monoxide(CO) which is our target product and important feedstock of useful products. Au is known for the most high CO production metal. With copper, Not only gold/copper has advantages which is they have FCC packing for easily forming solid solution regardless of stoichiometry but also presence of adsorbed CO on Cu promotes the desorption of CO on Au because of strong repulsion. And gold/copper bi-metal catalyst can show high catalytic activity(mass activity) although it has low selectivity relatively Gold. Actually, multi-metallic catalyst structure control method is limited in the solution method which is takes a lot of time. In here, we introduce CTS(carbo thermal shock) method which is using heat to make MMNP in a few seconds for making gold-copper system. This method is very simple and efficient in terms of time(very short reaction time and using carbon substrate as a direct working electrode) and increasing reaction sites(highly dispersed and mixing alloy structures). Last one is easy to control degree of mixing and it can induce 5 or more metals in one alloy system. Gold/copper by CTS can show higher catalytic activity depending on metal ratio which is altered easily by changing simple variables. The ultimate goals are making CO2 test system by CTS which can check the selectivity depending on metal types in a very short time.

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Mechanical and Electrical Properties of Si-SiC Fabricated Using SiC-C Composite Powders Synthesized by Sol-gel Process (Sol-gel 법으로 합성된 SiC-C 복합분말을 사용하여 제조된 Si-SiC의 기계적 특성 및 전기저항 특성)

  • Youn, Sung Il;Cho, Gyung Sun;Youm, Mi Rae;Lim, Dae Soon;Park, Sang Whan
    • Journal of the Korean Ceramic Society
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    • v.51 no.5
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    • pp.459-465
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    • 2014
  • In this study, Si-SiC composites were fabricated using a Si melt infiltration method using ${\beta}$-SiC/C composite powders synthesized by the carbothermal reduction of $SiO_2-C$ precursors made from a TEOS and a phenol resin. The purity of the synthesized SiC-C composite powders was higher than 99.9993 wt% and the average particle size varied from 4 to $6{\mu}m$ with increasing carbon contents of the $SiO_2-C$ precursors. It was found that the Si-SiC composites fabricated in this study consist of ${\beta}$-SiC and residual Si, without any trace of ${\alpha}$-SiC. The 3-point bending strengths of the fabricated Si-SiC composites were measured and found to be higher than 550 MPa, although the density of the fabricated Si-SiC composite was less than $2.9g/cm^3$. The bending strengths and the densities of the fabricated Si-SiC composites were found to decrease with increasing C/Si mole ratios in the SiC-C composite powders. The specific resistivities of the Si-SiC composites fabricated using the SiC-C composite powders were less than $0.018{\Omega}cm$. With increasing C content in the SiC-C composite powders used for the fabrication of Si-SiC composites, the specific resistivity of the Si-SiC composites was found to slightly increase from 0.0157 to $0.018{\Omega}cm$.

Effects of heat-treatment temperature on carbon-based composites with added illite

  • Jeong, Eui-Gyung;Kim, Jin-Hoon;Lee, Young-Seak
    • Carbon letters
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    • v.12 no.2
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    • pp.95-101
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    • 2011
  • To investigate new applications for illite as an additive for carbon-based composites, the composites were prepared with and without illite at different heat-treatment temperatures. The effects of the heat-treatment temperature on the chemical structure, microstructure, and thermal oxidation properties of the resulting composites were studied. As the heat-treatment temperature was increased, silicon carbide SiC formation via carbothermal reduction increased until all the added illite was consumed in the case of the samples heat-treated at $2,300^{\circ}C$. This is attributed to the intimate contact between the $SiO_2$ in the illite and the phenol carbon precursor or the carbon fibers of the preform. Among composites prepared at all temperatures, those with illite addition exhibited fewer pores, voids, and interfacial cracks, resulting in larger bulk densities and lower porosities. A delay of oxidation was not observed in the illite-containing composites prepared at $2,300^{\circ}C$, suggesting that the illite itself absorbed energy for exfoliation or other physical changes. Therefore, if the illite-containing C/C composites can reach a density generally comparable to that of other C/C composites, illite may find application as a filler for C/C composites. However, in this study, the illite-containing C/C composites exhibited low density, even when prepared at a high heat-treatment temperature of $2300^{\circ}C$, although the thermal oxidation of the resulting composites was improved.

A Study on the Preparation of SiC Nano powder from the Si Waste of Solar Cell Industry (태양전지 산업(産業)에서 배출(排出)되는 Si waste로부터 SiC 분말 제조에 관한 연구(硏究))

  • Jang, Eun-Jin;Kim, Young-Hee;Lee, Yoon-Joo;Kim, Soo-Ryong;Kwon, Woo-Teck
    • Resources Recycling
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    • v.19 no.5
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    • pp.44-49
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    • 2010
  • SiC powders have been recovered from silicon-containing waste slurry by carbothermal reduction method with carbon black. Large amount of silicon-containing waste slurry is generated from Solar Cell industry. In an environmental and economic point of view, retrieve of the valuable natural resource from the silicon waste is important. In this study, SiC powder recovered by the reaction ball-milled silicon powder from waste and carbon black at $1350^{\circ}C$ for 3h under vacuum condition. Physical properties of samples have been characterized using SEM, XRD, Particle size analyzer and FT-IR spectroscopy.

Simulation of Silicon Carbide Converted Graphite by Chemical Vapor Reaction (Ⅰ) (화학적 기상 반응에 의한 탄화규소 피복 흑연의 시뮬레이션(Ⅰ))

  • Lee, Joon-Sung;Choi, Sung-Churl
    • Journal of the Korean Ceramic Society
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    • v.38 no.9
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    • pp.846-852
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    • 2001
  • A two-dimensional Monte Carlo simulation has been used to investigate the effect of the reaction temperature on the formation of the silicon carbide conversion layer near the surface of graphite substrate The carbothermal reduction of silica is the reaction mechanism of silicon carbide formation on graphite substrate by chemical vapor reaction methods. The chemical composition of silicon carbide conversion layer gradually changes from carbon to silicon carbide because gaseous reactants diffuse through micropores within graphite substrate and react with carbon at the surface of inner pores. The simulation was carried out under the condition of reaction temperature at 1900K, 2000K, 2100K and 2200K for 500MCS. It was found from the results of simulation that the thickness of silicon carbide conversion layer increases with reaction temperature.

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