• Title/Summary/Keyword: Powder Morphology

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Glycothermal synthesis and characterization of $BaTiO_3$ glycolate (Glycothermal법에 의해 제조된 $BaTiO_3$ glycolate의 특성)

  • Kil, Hyun-Sig;Amar, Badrakh;Lim, Dae-Young
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2006.06a
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    • pp.286-287
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    • 2006
  • Barium titanate ($BaTiO_3$) glycolate particles were synthesized at temperature as low as $100^{\circ}C$ through glycothermal reaction by using $Ba(OH)_2{\cdot}8H_2O$ and amorphous titanium hydrous gel as precursors and ethylene glycol as solvent. The particle size and morphology of $BaTiO_3$ glycolate powders can be controlled by varying the reaction conditions such as the reaction temperature and Ba:Ti molar ratio of starting precursors. After glycothermal treatment at $220^{\circ}C$ for 24 h in 1.25:1(Ba:Ti), the average particle size of the $BaTiO_3$ glycolate powder was about 200-400 nm and low agglomeration. $BaTiO_3$ powders were formed by heat-treating the glycolate powder in air at $500-1000^{\circ}C$. As a result, the size of $BaTiO_3$ crystallites changed from around 50-300 nm. It is also demonstrated that the size and shape of $BaTiO_3$ particles investigated as a function of calcination temperature. The $BaTiO_3$ particles obtained from optimum synthesis condition were pressed, sintered and measured for the dielectric property. The $BaTiO_3$ ceramics sintered at $1250^{\circ}C$ for 2 h had 98 % of theoretical density. The ceramics have an average grain size of about $1\;{\mu}m$ and displays the high dielectric constant (~3100) and low dielectric loss (<0.1) at room temperature.

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Effect of Single and Dual Doping of Rare Earth Metal Ce and Nd Elements on Electrochemical Properties of LiNi0.83 Co0.11Mn0.06O2Cathode Lithium-ion Battery Material (리튬이온전지용 양극활물질 LiNi0.83 Co0.11Mn0.06O2의 전기화학적 특성에 미치는 Ce와 Nd 희토류 금속의 단독 혹은 이중 도핑효과)

  • Kim, Yoo-Young;Ha, Jong-Keun;Cho, Kwon-Koo
    • Journal of Powder Materials
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    • v.26 no.1
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    • pp.49-57
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    • 2019
  • Layered $LiNi_{0.83}Co_{0.11}Mn_{0.06}O_2$ cathode materials single- and dual-doped by the rare-earth elements Ce and Nd are successfully fabricated by using a coprecipitation-assisted solid-phase method. For comparison purposes, non-doping pristine $LiNi_{0.83}Co_{0.11}Mn_{0.06}O_2$ cathode material is also prepared using the same method. The crystal structure, morphology, and electrochemical performances are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) mapping, and electrochemical techniques. The XRD data demonstrates that all prepared samples maintain a typical ${\alpha}-NaFeO_2$-layered structure with the R-3m space group, and that the doped samples with Ce and/or Nd have lower cation mixing than that of pristine samples without doping. The results of SEM and EDS show that doped elements are uniformly distributed in all samples. The electrochemical performances of all doped samples are better than those of pristine samples without doping. In addition, the Ce/Nd dual-doped cathode material shows the best cycling performance and the least capacity loss. At a 10 C-rate, the electrodes of Ce/Nd dual-doped cathode material exhibit good capacity retention of 72.7, 58.5, and 45.2% after 100, 200, and 300 cycles, respectively, compared to those of pristine samples without doping (24.4, 11.1, and 8.0%).

Synthesis and Optical Property of TiO2 Nanoparticles Using a Salt-assisted Ultrasonic Spray Pyrolysis Process (염 보조 초음파 분무 열분해법을 이용한 TiO2 나노입자의 합성 및 광학적 성질)

  • Ji, Myeong-Jun;Park, Woo-Young;Yoo, Jae-Hyun;Lee, Young-In
    • Journal of Powder Materials
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    • v.26 no.1
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    • pp.34-39
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    • 2019
  • Current synthesis processes for titanium dioxide ($TiO_2$) nanoparticles require expensive precursors or templates as well as complex steps and long reaction times. In addition, these processes produce highly agglomerated nanoparticles. In this study, we demonstrate a simple and continuous approach to synthesize $TiO_2$ nanoparticles by a salt-assisted ultrasonic spray pyrolysis method. We also investigate the effect of salt content in a precursor solution on the morphology and size of synthesized products. The synthesized $TiO_2$ nanoparticles are systematically characterized by X-ray diffraction, transmission electron micrograph, and UV-Vis spectroscopy. These nanoparticles appear to have a single anatase phase and a uniform particle-size distribution with an average particle size of approximately 10 nm. By extrapolating the plots of the transformed Kubelka-Munk function versus the absorbed light energy, we determine that the energy band gap of the synthesized $TiO_2$ nanoparticles is 3.25 eV.

Effect of CaF2 Addition on the Crystallinity of Hexagonal Boron Nitride Nanoparticles (육방정 질화붕소 나노입자의 결정성에 미치는 불화칼슘 첨가의 영향)

  • Jung, Jae-Yong;Kim, Yang-Do;Kim, Young-Kuk
    • Korean Journal of Metals and Materials
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    • v.56 no.12
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    • pp.915-920
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    • 2018
  • With the development of modern microelectronics technologies, the power density of electronic devices is rapidly increasing, due to the miniaturization or integration of device elements which operate at high frequency, high power conditions. Resulting thermal problems are known to cause power leakage, device failure and deteriorated performance. To relieve heat accumulation at the interface between chips and heat sinks, thermal interface materials (TIMs) must provide efficient heat transport in the through-plane direction. We report on the enhanced thermal conduction of $Al_2O_3-based$ polymer composites, fabricated by the surface wetting and texturing of thermally conductive hexagonal boron nitride(h-BN) nanoplatelets with large anisotropy in morphology and physical properties. The thermally conductive polymer composites were prepared with hybrid fillers of $Al_2O_3$ macro beads and surface modified h-BN nanoplatelets. Hexagonal boron nitride (h-BN) has high thermal conductivity and is one of the most suitable materials for thermally conductive polymer composites, which protect electronic devices by efficient heat dissipation. In this study, we synthesized hexagonal boron nitride nanoparticles by the pyrolysis of cost effective precursors, boric acid and melamine. Through pyrolysis at $900^{\circ}C$ and subsequent annealing at $1500^{\circ}C$, hexagonal boron nitride nanoparticles with diameters of ca. 50nm were synthesized. We demonstrate that the addition of a small amount of calcium fluoride ($CaF_2$) during the preparation of the melamine borate adduct significantly enhanced the crystallinity of the h-BN and assisted the growth of nanoplatelets up to 100nm in diameters. The addition of a small amount of h-BN enhanced the thermal conductivity of the $Al_2O_3-based$ polymer composites, from 1.45W/mK to 2.33 W/mK.

Effect of Core Morphology on the Decomposition of CCI₄ over the Surface of Core/Shell Structured Fe₂O₃/MgO Composite Metal Oxides

  • 김해진;강진;박동곤;권호진;Kenneth J. Klabunde
    • Bulletin of the Korean Chemical Society
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    • v.18 no.8
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    • pp.831-840
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    • 1997
  • Core/shell structured composite metal oxides of Fe2O3/MgO were prepared by thermal decomposition of Fe(acac)3 adsorbed on the surface of MgO cores. The morphology of the composites conformed to that of the MgO used as the cores. Broad powder X-ray diffraction peaks shifted toward larger d, large BET surface area (∼350 m2/g), and the size of crystalline domains in nano range (4 nm), all corroborate to the nanocrystallinity of the Fe2O3/MgO composite which was prepared by using nanocrystalline MgO as the core. By use of microcrystalline MgO as the core, microcrystalline Fe2O3/MgO composite was prepared, and it had small BET surface area of less than 35 m2/g. AFM measurements on nanocrystalline Fe2O3/MgO showed a collection of spherical aggregates (∼80 nm dia) with a very rough surface. On the contrary, microcrystalline Fe2O3/MgO was a collection of plate-like flat crystallites with a smooth surface. The nitrogen adsorption-desorption behavior indicated that microcrystalline Fe2O3/MgO was nonporous, whereas nanocrystalline Fe2O3/MgO was mesoporous. Bimodal distribution of the pore size became unimodal as the layer of Fe2O3 was applied to nanocrystalline MgO. The macropores in a wide distribution which the nanocrystalline MgO had were absent in the nanocrystalline Fe2O3/MgO. The decomposition of CCl4 was largily enhanced by the overlayer of Fe2O3 on nanocrystalline MgO making the reaction between nanocrystalline Fe2O3/MgO and CCl4 be nearly stoichiometric. The reaction products were environmentally benign MgCl2 and CO2. Such an enhancement was not attainable with the microcrystalline samples. Even for the nanocrystalline MgO, the enhancement was not attained, if not with the Fe2O3 layer. Without the layer of Fe2O3, it was observed that the nanocrystalline domain of the MgO transformed into microcrystalline one as the decomposition of CCl4 proceeded on its surface. It appeared that the layer of Fe2O3 on the particles of nanocrystalline Fe2O3/MgO blocked the transformation of the nanocrystalline domain into microcrystalline one. Therefore, in order to attain stoichiometric reaction between CCl4 and Fe2O3/MgO core/shell structured composite metal oxide, the morphology of the core MgO has to be nanocrystalline, and also the nanocrystalline domains has to be sustained until the core was exhausted into MgCl2.

Preparation of $Pb(Sc_{1/2}Nb_{1/2})O_3$ powders by the molten salt synthesis method (용융염 합성법에 의한 $Pb(Sc_{1/2}Nb_{1/2})O_3$ 분말의 제조)

  • 박경봉
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.7 no.3
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    • pp.400-405
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    • 1997
  • Lead scandium niobate powders were prepared by a molten salt synthesis method using KCl as a flux. Variations in phase formation and particle morphology were investigated for the temperature range $700^{\circ}C$ to $850^{\circ}C$. Pure $Pb(Sc_{1/2}Nb_{1/2})O_3$ perovskite phase was formed at $850^{\circ}C$ after 2hrs and the average particle size of powder was below 0.5 $\mu\textrm{m}$. The results are discussed with respect to DTA, X-ray diffraction, and microstructural characterization data.

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Nickel Oxide Nano-Flake Films Synthesized by Chemical Bath Deposition for Electrochemical Capacitors (CBD(Chemical Bath Deposition) 법으로 제조된 전기화학식 캐패시터용 NiO 나노박편 필름)

  • Kim, Young-Ha;Park, Soo-Jin
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.06a
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    • pp.163.2-163.2
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    • 2010
  • In this work, nano-flake shaped nickel oxide (NiO) films were synthesized by chemical bath deposition technique for electrochemical capacitors. The deposition was carried out for 1 and 2 h at room temperature using nickel foam as the substrate and the current collector. The structure and morphology of prepared NiO film were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). And, electrochemical properties were characterized by cyclic voltammetry, galvanostatic charge-discharge, and AC impedence measurement. It was found that the NiO film was constructed by many interconnected NiO nano-flakes which arranged vertically to the substrate, forming a net-like structure with large pores. The open macropores may facilitate the electrolyte penetration and ion migration, resulted in the utilization of nickel oxide due to the increased surface area for electrochemical reactions. Furthermore, it was found that the deposition onto nickel foam as substrate and curent collector led to decrease of the ion transfer resistance so that its specific capacitance of a NiO film had high value than NiO nano flake powder.

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Reinvestigation of Dion-Jacobson Phases CsCa2Nb2MO9 (M = Fe and Al)

  • Hong, Young-Sik
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.853-856
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    • 2006
  • Dion-Jacobson phases $CsCa_2Nb_2FeO_9$ and $CsCa_2Nb_2AlO_9$ were reinvestigated by the Rietveld analysis of powder X-ray diffraction (XRD) method, scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). These nominal compounds, previously known as the oxygen-deficient layered perovskites with the sequences of $NbO_6-MO_4-NbO_6$ in tripled slab, in fact, were mixed phases of n = 3 Dion-Jacobson phases and impurities such as $Ca_2NbFeO_6$ and $Ca_3Al_2O_6$. The difference of morphology and chemical in-homogeneity between Dion-Jacobson phases and impurities could be clearly identified by scanning electron microscopy with energy-dispersive X-ray spectroscopy. The chemical composition of $CsCa_2Nb_2FeO_9$ was calculated into $Cs_{0.59}Ca_{2.64}Nb_{2.92}Fe_{0.81}$ in small agglomerate crystals and $Cs_{0.95}Ca_{1.97}Nb_{3.08}Fe_{0.15}$ in long plate-like crystals.

Synthesis of Nanocrystalline TiO2 by Sol-Gel Combustion Hybrid Method and Its Application to Dye Solar Cells

  • Han, Chi-Hwan;Lee, Hak-Soo;Han, Sang-Do
    • Bulletin of the Korean Chemical Society
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    • v.29 no.8
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    • pp.1495-1498
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    • 2008
  • $TiO_2$ nanopowders were synthesized by new sol-gel combustion hybrid method using acetylene black as a fuel. The dried gels exhibited autocatalytic combustion behaviour. $TiO_2$ nanopowders with an anatase structure and a narrow size distribution were obtained at 400-600 ${^{\circ}C}$. Their crystal structures were examined by powder Xray diffraction (XRD) and their morphology and crystal size were investigated by scanning electron microscopy (SEM). The crystal size of the nanopowders was found to be in the range of 15-20 nm. $TiO_2$ powders synthesized at 500 ${^{\circ}C}$ and 600 ${^{\circ}C}$ were applied to a dye solar cell. An efficiency of 5.2% for the conversion of solar energy to electricity ($J_{sc}$ = 11.79 mA/$cm^2$, $V_{oc}$ = 0.73 V, and FF = 0.58) was obtained for an AM 1.5 irradiation (100 mW/$cm^2$) using the $TiO_2$ nanopowder synthesized by the sol-gel combustion hybrid method at 500 ${^{\circ}C}$.

VLS growth of ZrO2 nanowhiskers using CVD method

  • Baek, Min-Gi;Park, Si-Jeong;Jeong, Jin-Hwan;Choe, Du-Jin
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.149-149
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    • 2016
  • Ceramic is widely known material due to its outstanding mechanical property. Besides, Zirconia(ZrO2) has a low thermal conductivity so it is advantage in a heat insulation. Because of these superior properties, ZrO2 is attracted to many fields using ultra high temperature for example vehicle engines, aerospace industry, turbine, nuclear system and so on. However brittle fracture is a disadvantage of the ZrO2. In order to overcome this problem, we can make the ceramic materials to the forms of ceramic nanoparticles, ceramic nanowhiskers and these forms can be used to an agent of composite materials. In this work, we selected Au catalyzed Vapor-Liquid-Solid mechanism to synthesize ZrO2 nanowhiskers. The ZrO2 whiskers are grown through Hot-wall Chemical Vapor Deposition(Hot wall CVD) using ZrCl4 as a powder source and Au film as a catalyst. This Hot wall CVD method is known to comparatively cost effective. The synthesis condition is a temperature of $1100^{\circ}C$, a pressure of 760torr(1atm) and carrier gas(Ar) flow of 500sccm. To observe the morphology of ZrO2 scanning electron microscopy is used and to identify the crystal structure x-ray diffraction is used.

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