• Title/Summary/Keyword: Nano powder synthesis

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Synthesis and Characterization of Si-C-N Precursor by Using Chemical Vapor Condensation Method (화학기상응축법을 이용한 Si-C-N Precursor 분말의 합성 및 특성평가)

  • Kim, Hyoung-In;Kim, Dae-Jung;Hong, Jin-Seok;So, Myoung-Gi
    • Journal of the Korean Ceramic Society
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    • v.39 no.8
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    • pp.783-788
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    • 2002
  • In this study, nano-sized Si-C-N precursor powders were synthesized by Chemical Vapor Condensation Method(CVC) using TMS(Tetramethylsilane: Si($CH_3)_4$), $NH_3$ and $H_2$ gases under the various reaction conditions of the reaction temperature, TMS/$NH_3$ ratio and TMS/$H_2$ ratio. XRD and FESEM were used to analysis the crystalline phase and the average particle size of the synthesized powders. It was found that the obtained powders under the considering conditions were all spherical amorphous powder with the particle size of 87∼130 nm. The particle size was decreased as the reaction temperature increased and TMS/$NH_3$ and TMS/$H_2$ ratio decreased. As the results of EA analysis, it was found that the synthesized powders had been formed the powders composed of Si, N, C and H. Through FT-IR results, it was found that the synthesized powders were Si-C-N precursor powders with Si-C, Si-N and C-N bonds.

Electrochemical Properties of Lithium Secondary Battery and the Synthesis of Spherical Li4Ti5O12 Powder by Using TiCl4 As a Starting Material (TiCl4를 출발원료로한 구형 Li4Ti5O12 분말합성 및 리튬이차 전지특성)

  • Choi, Byung-Hyun;Ji, Mi-Jung;Kwon, Yong-Jin;Kim, Eun-Kyung;Nahm, Sahn
    • Korean Journal of Materials Research
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    • v.20 no.12
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    • pp.669-675
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    • 2010
  • One of the greatest challenges for our society is providing powerful electrochemical energy conversion and storage devices. Rechargeable lithium-ion batteries and fuel cells are among the most promising candidates in terms of energy and power density. As the starting material, $TiCl_4{\cdot}YCl_3$ solution and dispersing agent (HCP) were mixed and synthesized using ammonia as the precipitation agent, in order to prepare the nano size Y doped spherical $TiO_2$ precursor. Then, the $Li_4Ti_5O_{12}$ was synthesized using solid state reaction method through the stoichiometric mixture of Y doped spherical $TiO_2$ precursor and LiOH. The Ti mole increased the concentration of the spherical particle size due to the addition of HPC with a similar particle size distribution in a well in which $Li_4Ti_5O_{12}$ spherical particles could be obtained. The optimal synthesis conditions and the molar ratio of the Ti 0.05 mol reaction at $50^{\circ}C$ for 30 minutes and at $850^{\circ}C$ for 6 hours heat treatment time were optimized. $Li_4Ti_5O_{12}$ was prepared by the above conditions as a working electrode after generating the Coin cell; then, electrochemical properties were evaluated when the voltage range of 1.5V was flat, the initial capacity was 141 mAh/g, and cycle retention rate was 86%; also, redox reactions between 1.5 and 1.7V, which arose from the insertion and deintercalation of 0.005 mole of Y doping is not a case of doping because the C-rate characteristics were significantly better.

Effect of Processing Parameters on the Microstructure and Band Gap Energy of 1D-Na2Ti6O13 (1D-Na2Ti6O13 합성 변수에 따른 미세구조 및 밴드 갭 에너지 변화)

  • Yun, Kang-Seop;Ku, Hye-Kyung;Kang, Woo-Seung;Kim, Sun-Jae
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.8
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    • pp.664-669
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    • 2012
  • Nano-structured one-dimensional $Na_2Ti_6O_{13}$ particles were synthesized by a molten salt process. Effects of processing parameters on the microstructure and band gap energy of the $Na_2Ti_6O_{13}$ powder were studied in this paper. For the synthesis of the $Na_2Ti_6O_{13}$ particles, two different raw materials of tubular shaped Na-titanate (Na-TiNT) and spherical shaped $TiO_2$ were utilized. Synthesizing with the raw material of Na-TiNT, around 70nm thick 1D-$Na_2Ti_6O_{13}$ with the bandgap energy of 3.5 eV was obtained at $810^{\circ}C$. Below $810^{\circ}C$ or without the presence of NaCl, 1D-$Na_2Ti_6O_{13}$ was in a relatively short in length and agglomerated state. With the processing temperature increased, the thickness of the 1D-$Na_2Ti_6O_{13}$ was also observed to be increased. On the other hand, when $TiO_2$ was employed as a raw material, the mixed amount of $Na_2CO_3$ played an important role in transforming the morphology and phase of the raw material, affecting the bandgap energy of the synthesized product. Specific surface area of the synthesized 1D-$Na_2Ti_6O_{13}$ was significantly affected by the raw and mixed materials as well as processing temperature. When Na-TiNT was processed at $810^{\circ}C$ with NaCl, the specific surface area of the 1D-$Na_2Ti_6O_{13}$ showed the best value of 30.63 $m^2/g$.

Synthesis of $Fe/Al_2O_3$ and $Fe/TiO_2$ nanocomposite powder by mechanical alloying (기계적합금화에 의한 $Fe/Al_2O_3$$Fe/TiO_2$계 나노복합분말의 제조)

  • Lee, Seong-Hee;Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.19 no.4
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    • pp.202-207
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    • 2009
  • Nanocomposite formation of metal-metal oxide systems by mechanical alloying (MA) has been investigated at room temperature. The systems we chose are the $Fe_3O_4$-M (M = AI, Ti), where pure metals are used as reducing agent. It is found that $Fe/Al_2O_3$ and $Fe/TiO_2$ nanocomposite powders in which $Al_2O_3$ and $TiO_2$ are dispersed in ${\alpha}$-Fe matrix with nano-sized grains are obtained by MA of $Fe_3O_4$ with Al and Ti for 25 and 75 hours, respectively. It is suggested that the shorter MA time for the nanocomposite formation in $Fe/Al_2O_3$ is due to a large negative heat associated with the chemical reduction of magnetite by aluminum. X-ray diffraction results show that the average grain size of ${\alpha}$-Fe in $Fe/TiO_2$ nanocomposite powders is in the range of 30 nm. The change in magnetic properties also reflects the details of the solid-state reduction of magnetite by pure metals during MA.

The Study on Thermal Analysis and Thermodynamic Characteristics of Spinel Compounds(ZnCo2O4, NiCo2O4) (스피넬 구조를 가지는 전이금속화합물(ZnCo2O4, NiCo2O4)의 열적 분석 및 열역학적 특성 연구)

  • Kim, Jae-Uk;Ji, Myoung-Jin;Cha, Byung-Kwan;Kim, Chul-Hyun;Jang, Won-Cheoul;Kim, Jong-Gyu
    • Journal of the Korean Chemical Society
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    • v.54 no.2
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    • pp.192-197
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    • 2010
  • The spinel compound was obtained by the thermal decomposition of Zn-Co and Zn-Ni gel prepared by sol-gel method using oxalic acid as a chelating agent. The formation of spinel compound has been comfirmed by thermogravimetric analysis (TGA), x-ray powder diffraction (XRD) and infrared spectroscopy (IR). The particle size of 13 nm~16 nm was calculated by Scherrer's equation. The sol-gel method provides a practicable and effective route for the synthesis of the spinel compound at low temperature ($350^{\circ}C$). The kinetic parameters such as activation energy (Ea) and pre-exponential factor (A) for each compound were found by means of the Kissinger method and Arrhenius equation. The decomposition of spinel compound has an activation energy about 155 kJ/mol. Finally, the thermodynamic parameters (${\Delta}G^{\varphi}$, ${\Delta}H^{\varphi}$, ${\Delta}S^{\varphi}$) for decomposition of spinel compound was determined.