• Title/Summary/Keyword: solution combustion synthesis

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Synthesis and characterization of AlN nanopowder by the microwave assisted carbothermal reduction and nitridation (CRN)

  • Chun, Seung-Yeop;Chun, Myoung-Pyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.5
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    • pp.223-228
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    • 2017
  • Aluminum nitride (AlN) powder was successfully synthesized at low temperature via carbothermal reduction and nitridation (CRN) assisted by microwave heating. The synthesis processes of AlN powder were investigated with X-ray diffraction, FE-SEM, FT-IR and TGA/DSC. Aluminum nitrate was used as an oxidizer and aluminum source, urea as fuel, and glucose as carbon source. These starting materials were mixed with D.I water and reacted in a flask at $100^{\circ}C$ for 20 minutes. After the reaction was finished, black foamy intermediate product was formed, which was considered to be an amorphous $Al_2O_3$ particles through intermediate product obtained by solution combustion synthesis (SCS) at the results of X-ray diffraction patterns and FT-IR. This intermediate product was nitridated at temperatures of $1300^{\circ}C$ and $1400^{\circ}C$ in $N_2$ atmosphere by a microwave heating furnace and then decarbonated at $600^{\circ}C$ for 2 hours in air. It should be noticed from FE-SEM images that as nitridated particles, identified as AlN from X-ray diffraction patterns, are covered with carbon residues. After decarbonating the nitridated powders, the spherical pure AlN powders were obtained without alumina and their particle sizes were dependent on the nitridating temperature with high temperature of $1400^{\circ}C$ giving large particles of around 70~100 nm.

A Facile Combustion Synthesis Route for Performance Enhancement of La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF6428) as a Robust Cathode Material for IT-SOFC

  • Yoo, Young-Sung;Namgung, Yeon;Bhardwaj, Aman;Song, Sun-Ju
    • Journal of the Korean Ceramic Society
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    • v.56 no.5
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    • pp.497-505
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    • 2019
  • Lanthanum-based transition metal cations containing perovskites have emerged as potential catalysts for the intermediate-temperature (600-800℃) oxygen reduction reaction (ORR). Here, we report a facile acetylacetone-assisted combustion route for the synthesis of nanostructured La0.6Sr0.4Co0.2Fe0.8O3-δ (LSCF6428) cathodes for intermediate-temperature solid-oxide fuel cells (IT-SOFCs). The as-prepared powder was analyzed by thermogravimetry analysis-differential scanning calorimetry. The powder calcined at 800℃ was characterized by X-ray diffraction, scanning electrode microscopy, energy dispersive X-ray spectroscopy, and Brunauer-Emmett-Teller surface area measurements. It was found that the porosity of the air electrode significantly increased by utilizing the nanostructured LSCF6428 instead of commercial powder. The performance of a single cell fabricated with the nanostructured LSCF6428 cathode increased by 112%, from 0.4 to 0.85 W cm-2, at 700℃. Electrochemical impedance spectroscopy showed a considerable reduction in the area-specific resistance and activation energy from 133.5 to 61.5 kJ/mol, resulting in enhanced electrocatalytic activity toward ORR and overall cell performance.

Fabrication of $ZrB_2$ Ceramics for Thermocouple Protective Tubes by SHS Process (SHS 공정에 의한 열전대 보호관용 $ZrB_2$ 세라믹스의 제조)

  • 곽철상;김상배;이윤복;박홍채;오기동
    • Journal of the Korean Ceramic Society
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    • v.34 no.11
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    • pp.1165-1172
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    • 1997
  • ZrB2 powders were prepared from a mixture of ZrO2, B2O3 and Mg by self-propagating high temperature synthesis method. The combustion product was successfully obtained from a mixture of ZrO2:B2O3:Mg=1:2:8.5 molar ratio. By-product, MgO was effectively removed by leaching with 1M HCl solution at 9$0^{\circ}C$ for over 5hours. After leaching, the Mg content was 0.86~1.42 wt%, and the mean particle size was 4.72${\mu}{\textrm}{m}$. The addition of 7.5 wt%(14Ni:1.0C) as a sintering aid greatly densified ZrB2 bodies compared with that of only Ni. The ZrB2 sintered bodies containing 7.5 wt%(14Ni:1.0C) was 94.3% of the theoretical density. In this case, ZrB2 existed as a major phase and had a bend strength of 300 MPa and a vickers hardness of 2000 kg/$\textrm{mm}^2$.

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Effect of Zine Oxide Size and Oxygen Pressure on the Magnetic Properties of (Ni, Zn) Ferrite Powders Prepared by Self-propagating High Temperature Synthesis (ZnO의 입도와 산소압이 고온연소합성법으로 제조된 Ni-Zn Ferrite 분말의 자기적 특성에 미치는 영향)

  • Choi, Yong;Cho, Nam-Ihn;Hahn, Y.D.
    • Journal of the Korean Magnetics Society
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    • v.9 no.2
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    • pp.78-84
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    • 1999
  • $(Ni, Zn)Fe_2O_4$ powders were prepared through self-propagating high temperature synthesis reaction and the effects of initial zinc oxide powder size and oxygen pressure on the magnetic properties of the final combustion products were studied. The ferrite powders were combustion synthesized with iron, iron oxide, nickel oxide, and zinc oxide powders under various oxygen pressures of 0.5~10 atmosphere after blended in n-hexane solution for 5 minutes with a spex mill, followed by dried at 120 $^{\circ}C$ in vacuum for 24 hours. The maximum combustion temperature and propagating rate were about 1250 $^{\circ}C$ and 9.8 mm/sec under the tap density, which were decreased with decreasing ZnO size and oxygen pressure. The final product had porous microstructure with spinel peaks in X-ray spectra. As the ZnO particle size in the reactant powders and oxygen pressure during the combustion reaction increase, coercive force, maximum magnetization, residual magnetization, squareness ratio were changed from 1324 Oe, 43.88 emu/g, 1.27 emu/g, 0.00034 emu/gOe, 37.8$^{\circ}C$ to 11.83 Oe, 68.87 emu/g, 1.23 emu/g, 0.00280 emu/gOe, 43.9 $^{\circ}C$ and 7.99 Oe, 75.84 emu/g, 0.791 emu/g, 0.001937 emu/gOe, 53.8 $^{\circ}C$ respectively. Considering the apparent activation energy changes with oxygen pressure, the combustion reaction significantly depended on initial oxygen pressure and ZnO particle size.

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Preparation of Fine Alumina Powder

  • Soh, Dea-Wha;Jeon, Yong-Woo;N., Korobova
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2002.07b
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    • pp.670-673
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    • 2002
  • Powder synthesis using the alkoxy precursor technique exhibits processing flexibility not available in traditional high temperature solid-state reaction. With proper process control, impurities can be reduced to very low levels. The major distinction of the present work lies in the method of accomplishing the hydrolysis reaction. In the present case, water is not added to the system. Instead the metal alkoxide/alcohol solution is heated to a temperature at which water is formed through dehydration of the alcohol solvent, causing precipitation of the corresponding metal oxide (hydroxide). The present method provides a means of producing amorphous alumina.

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A Study on Synthesis and Characterization of TiZrB$_2$ Composite by SHS Microwave (SHS 마이크로파에 의한 TiZrB$_2$ 복합재료의 합성 및 특성연구)

  • 이형복;윤영진;오유근;안주삼
    • Journal of the Korean Ceramic Society
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    • v.36 no.1
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    • pp.7-14
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    • 1999
  • TiZrB2 solid solution was synthesized using fine powders of Ti, Zr and B by SHS microwave process. The characterization of the synthesized powder and sintered bodies ws investigated. The combustion temperature and rate were increased with increasing the mole ratio of Zr in temperature profile, and showed the maximum combustion temperature and velocity values of 285$0^{\circ}C$ and 14.6mm/sec in Ti0.2Zr0.8B2 composition. Phase separation has been occured into a composite with TiB2 and ZrB2 phases from TiZrB2 solid solution, which was hot pressed sintering at 30 MPa for an hour at 190$0^{\circ}C$. At the composition of Ti0.8Zr0.2B2 the best properties has been obtained in relative density, bending strength, fracture toughness and hardness, with 99%, 680 MPa, 7.3MPa.m1/2 and 2750 Kg/$\textrm{mm}^2$ respectively.

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Preparation of Nanocrystalline ZnO Ultrafine Powder Using Ultrasonic Spraying Combustion Method (초음파분무 연소법에 의한 나노결정 ZnO 초미분체 제조)

  • Kim, Kwang-Su;Hwang, Du-Sun;Ku, Suk-Kyeon;Lee, Kang;Jeon, Chi-Jung;Lee, Eun-Gu;Kim, Sun-Jae
    • Korean Journal of Materials Research
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    • v.12 no.10
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    • pp.784-790
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    • 2002
  • For mass product of nanocrystalline ZnO ultrafine powders, self-sustaining combustion process(SCP) and ultrasonic spray combustion method(USCM) were applied at the same time. Ultrasonic spray gun was attached on top of the vertical type furnace. The droplet was sprayed into reaction zone of the furnace to form SCP which produces spherical shape with soft agglomerate crystalline ZnO particles. To characterize formed particles, fuel and oxidizing agent for SCP were used glycine and zinc nitrate or zinc hydroxide. Respectively, with changing combustion temperature and mixture ratio of oxidizing agent and fuel, the best ultrasonic spray conditions were obtained. To observe ultrasonic spray effect, two types of powder synthesis processes were compared. One was directly sprayed into furnace from the precursor solution (Type A), the other directly was heated on the hot plate without using spray gun (Type B). Powder obtained by type A was porous sponge shape with heavy agglomeration, but powder obtained using type B was finer primary particle size, spherical shape with weak agglomeration and bigger value of specific surface area. 9/ This can be due to much lower reaction temperature of type B at ignition time than type A. Synthesized nanocrystalline ZnO powders at the best ultrasonic spray conditions have primary particle size in range 20~30nm and specific surface area is about 20m$^2$/g.

Effect of Carbon on Electrode Characteristics of $LiCoO_2$ Resynthesis ($LiCoO_2$의 재합성시(再合成時) 전극특성(電極特性)에 미치는 탄소(炭素)의 영향(影響))

  • Lee, Churl-Kyoung;Park, Jeong-Kil;Sohn, Jeong-Soo
    • Resources Recycling
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    • v.16 no.6
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    • pp.10-19
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    • 2007
  • The mechanical process followed by hydrometallurgical treatment has been developed in order to recover cobalt and lithium from spent lithium ion battery. In the previous study, a citrate precursor combustion process to prepare cathodic active materials from the leaching solution was elucidated. Resynthesis of electrode materials should be more valuable in spent battery recycling. Conventional slurry mixing of $LiCoO_2$ and carbon cannot make uniform distribution, and therefore the cathode cannot reach the theoretical charge-discharge capacity and is easily degraded during the charge-discharge cycling. In this study, ultra-fine $LiCoO_2$ powders has been prepared by modification of the combustion process and fabricated the enhanced cathode by modification of mixing method of $LiCoO_2$ and carbon added.

Synthesis and Characterization of Tetrazine Derivatives as High Energy Propellants (테트라진 계열의 추진 물질 합성 연구)

  • Lee, Woonghee;Park, Youngchul;Joo, Young-Hyuk
    • Journal of the Korean Society of Propulsion Engineers
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    • v.17 no.6
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    • pp.38-47
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    • 2013
  • Traditional propellants release toxic gases during combustion that are harmful to the environment. This study describes a novel synthetic process of two high nitrogen containing tetrazines, TATTz and BTATz, which can be adapted as solid fuels for a solution to environmental concerns. The compounds were characterized by NMR, IR spectroscopy, and differential scanning calorimetry(DSC). Detonation properties were calculated with the EXPLO5 program based on calculated heats of formation and measured densities.