• Title/Summary/Keyword: precursor particle size

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Preparation of Nano-size BaTiO3 Powders Using Glycothermal Method (Glycothermal법을 이용한 나노 사이즈 BaTiO3분말의 제조)

  • 김병규;임대영;노준석;조승범
    • Journal of the Korean Ceramic Society
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    • v.39 no.7
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    • pp.642-648
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    • 2002
  • Barium Titanate(BaTiO$_3$) nanoparticles were prepared at 22$0^{\circ}C$ through glycothermal process by using barium hydroxide and amorphous titanium hydrous gel as precursor and 1,4-butanediol and distilled water as solvent. It is demonstrated that the size of BaTiO$_3$ particles can be controlled by reaction conditions such as various content of 1,4-butanediol/distilled water volume ratio. This processing method can fabricate BaTiO$_3$ powders, which have a narrow distribution and exhibit good dispersion. The particle size of BaTiO$_3$ powders obtained by glycothermal process were about 50 nm to 200 nm on the condition that reaction temperature was 22$0^{\circ}C$ and holding time was 24 h.

Nanostructural Study of Apatite Film Biomimetically Grown in SBF (Simulated Body Fluid) (생체유사환경에서 성장된 아파타이트 층의 나노구조 연구)

  • Kim, Joung;Lee, Kap-Ho;Hong, Sun-Ig
    • Korean Journal of Materials Research
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    • v.15 no.11
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    • pp.690-696
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    • 2005
  • The ultrastructure ore of a nanostructured apatite film nucleated from solution was studied to gain insights into that of bone minerals which is the most important constituent to sustain the strength of bones. Needle-shaped apatite crystal plates with a bimodal size distribution $(\~100\;to\;\~1000 nm)$ were randomly distributed and they were found to grow parallel to the c-axis ([002]), driven by the reduction of surface energy. Between these randomly distributed needle-shaped apatite crystals which are parallel to the film, apatite crystals (20-40nm) with the normal of the grains quasi-perpendicular to the c-axis were observed. These observations suggest that the apatite film is the interwoven structure of apatite crystals with the c-axis parallel and quasi-perpendicular to the fan. In some regions, amorphous calcium phosphate, which is a precursor of apatite, was also observed. In the amorphous phase, small crystalline particle with the size of 2-3 nm were observed. These particles were quite similar, in size and shape, to those observed in the femoral trabecular bone, suggesting the nucleation of apatites by a biomimetic process in vitro is similar to that in vivo.

Hydrothermal Synthesis and Mechanical Characterization of ZrO2 by Y2O3 Stabilizer Contents (Y2O3안정화제 첨가량에 따라 수열합성법으로 제조된 ZrO2-Xmol% Y2O3분말의 합성 및 기계적 특성)

  • Lee, Hak-Joo;Kim, Taik-Nam;Bea, Sung-Chul;Go, Myung-Won;Ryu, Jae-Kyung
    • Korean Journal of Materials Research
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    • v.20 no.10
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    • pp.518-523
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    • 2010
  • In this study, partially stabilized zirconia was synthesized using a chemical $Y_2O_3$ stabilizer and hydrothermal method. First, $YCl_3-6H_2O$ and $ZrCl_2O-8H_2O$ was dissolved in distilled water. Y-TZP (a $Y_2O_3$-doped toughened zirconia polycrystalline precursor) was also prepared by conventional co-precipitates in the presence of an excess amount of $NH_4OH$ solution under a fixed pH of 12. The Y-TZP precursors were filtered and repeatedly washed with distilled water to remove $Cl^-$ ions. $ZrO_2$-Xmol%$Y_2O_3$ powder was synthesized by a hydrothermal method using Teflon Vessels at $180^{\circ}C$ for 6 h of optimized condition. The powder added with the Xmol%- $Y_2O_3$ (X = 0,1,3,5 mol%) stabilizer of the $ZrO_2$ was synthesized. The crystal phase, particle size, and morphologies were analyzed. Rectangular specimens of $33mm{\times}8mm{\times}3$ mm for three-point bend tests were used in the mechanical properties evaluation. A teragonal phase was observed in the samples, which contains more than 3 mol% $Y_2O_3$. The $3Y-ZrO_2$ agglomerated particle size was measured at $7.01{\mu}m$. The agglomerated particle was clearly observed in the sample of 5 mol % $Y_2O_3-ZrO_2$, and and the agglomerated particle size was measured at 16.4 um. However, a 20 nm particle was specifically observed by FE-SEM in the sample of 3 mol% $Y_2O_3-ZrO_2$. The highest bending fracture strength was measured as 321.3 MPa in sample of 3 mol% $Y_2O_3-ZrO_2$.

Synthesis and analysis CdSe Quantum dot with a Microfluidic Reactor Using a Combinatorial Synthesis System (조합 합성 시스템의 미세유체반응기를 이용한 CdSe 양자점 합성 및 분석)

  • Hong, Myung Hwan;Lee, Duk-Hee;Kang, Lee-Seung;Lee, Chan Gi;Kim, Bum-Sung;Kim, Nam-Hoon
    • Journal of Powder Materials
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    • v.23 no.2
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    • pp.143-148
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    • 2016
  • A microfluidic reactor with computer-controlled programmable isocratic pumps and online detectors is employed as a combinatorial synthesis system to synthesize and analyze materials for fabricating CdSe quantum dots for various applications. Four reaction condition parameters, namely, the reaction temperature, reaction time, Cd/Se compositional ratio, and precursor concentration, are combined in synthesis condition sets, and the size of the synthesized CdSe quantum dots is determined for each condition. The average time corresponding to each reaction condition for obtaining the ultraviolet-visible absorbance and photoluminescence spectra is approximately 10 min. Using the data from the combinatorial synthesis system, the effects of the reaction conditions on the synthesized CdSe quantum dots are determined. Further, the data is used to determine the relationships between the reaction conditions and the CdSe particle size. This method should aid in determining and selecting the optimal conditions for synthesizing nanoparticles for diverse applications.

Effect of solvent and precursor on the CeO2 nanoparticles fabrication (CeO2 나노 분말 합성에 미치는 용매 및 전구체의 영향)

  • Ock, Ji-Young;Son, Jeong-Hun;Bae, Dong-Sik
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.28 no.3
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    • pp.118-122
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    • 2018
  • Ceria ($CeO_2$) is a rare earth oxide, which has been widely investigated to improve the property. It is important to increase the surface area of $CeO_2$, because high surface area of $CeO_2$ can improve the catalytic ability. $CeO_2$ nanoparticles were synthesized by a solvothermal process. A discussion on the influence of solvent ratio and precursors on $CeO_2$ nanoparticles was performed. The size and degree of the agglomeration of the synthesized $CeO_2$ could be tuned by controlling those parameters. The average size and distribution of prepared $CeO_2$ powders was in the range of 3 to 13 nm and narrow, respectively. The XRD pattern showed that the synthesized $CeO_2$ powders were crystalline with cubic phase of $CeO_2$. The average particle size was calculated by Scherrer equation and FE-TEM images. The morphology of the synthesized $CeO_2$ particle was objected using FE-TEM and FE-SEM. Specific surface area of the synthesized $CeO_2$ was determined using BET (Brunauer-Emmett-Teller) equation.

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.

Preparation of LiCoO$_2$from Used Lithium Ion Battery by Hydrometallurgical Processes

  • Lee, Churl-Kyoung;Rhee, Kang-In;Yang, Dong-Hyo;Yu, Hyo-Shin
    • Proceedings of the IEEK Conference
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    • 2001.10a
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    • pp.240-244
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    • 2001
  • Recycling process involving mechanical, thermal, hydrometallurgical, and sol-gel step has been applied to recover cobalt and lithium from spent lithium ion batteries and to synthesize LiCoO$_2$from leach liquor as cathodic active materials. Electrode materials containing lithium and cobalt could be concentrated with 2-step thermal and mechanical treatment. Leaching behaviors of the lithium and cobalt in nitric acid media was investigated in terms of reaction variables. Hydrogen peroxide in 1 M HNO$_3$solution turned out to be an effective reducing agent by enhancing the leaching efficiency. O f many possible processes to produce LiCoO$_2$, the amorphous citrate precursor process (ACP) has been applied to synthesize powders with a large specific surface area and an exact stoichiometry. After leaching used LiCoO$_2$with nitric acid, the molar ratio of Li/Co in the leach liquor was adjusted at 1.1 by adding a fresh LiNO$_3$solution. Then, 1 M citric acid solution at a 100% stoichiometry was also added to prepare a gelatinous precursor. When the precursor was calcined at 95$0^{\circ}C$ for 24 hr, purely crystalline LiCoO$_2$was successfully obtained. The particle size and specific surface area of the resulting crystalline powders were 20 пm and 30 $\textrm{cm}^2$/g, respectively The LiCoO$_2$powder was proved to have good characteristics as cathode active materials in charge/discharge capacity and cyclic performance.

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Properties of Synthesis LSCF Cathode with pH Control using Oxalate Method (Oxalate법으로 합성한 LSCF의 pH 변화에 따른 공기극 특성)

  • Lee, Mi-Jai;Choi, Byung-Hyun;Kim, Sei-Ki;Lee, Mi-Jung
    • 한국신재생에너지학회:학술대회논문집
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    • 2007.11a
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    • pp.17-18
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    • 2007
  • Solid oxide fuel cells are clean, pollution-free technology for the electrochemical generation of electricity at high efficiency. Specially, the polarization resistance between electrolyte and electrode of SOFC unit cell is of importance, because it is desirable to develop SOFC operating at intermediate temperature below $800^{\circ}C$. The LSCF cathode prepared using modified oxalate method was investigated with different electrolyte. A precursor was prepared with oxalic acid, ethanol and $NH_4OH$ solution. The LSCF precursor was prepared at $80^{\circ}C$, and pH control was 2, 6, 8, 9 and 10. The precursor powder was calcined at $800^{\circ}C$, $1000^{\circ}C$ and $1200^{\circ}C$ for 4hrs. The crystal of LSCF powders show single phase at pH 2, 6, 8 and 9, and the average particle size was about $3{\mu}m$. The LSCF cathode with heat treatment at $1200^{\circ}C$ showed a plot of electric conductivity versus temperature. Unit cell prepared from the LSCF cathode, buffer layer between cathode and electrolyte and the LSGM, YSZ, ScSZ and CeSZ electrolyte. Also interface reaction between LSCF, buffer layer and electrolyte were measured by EPMA and the polarization resistance for unit cell with cycle measure using a Solatron 1260 analyzer.

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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.

Preparation and Characterization of a Layered Organic-inorganic Composite by the Electrophoretic Deposition of Plate-shaped Al2O3 Particles and Electrophoretic Resin (전기영동적층법을 통한 판상 알루미나 입자와 전기영동 수지의 배향 유무기 복합체 제조 및 물성평가)

  • Park, Hee Jeong;Lim, Hyung Mi;Choi, Sung-Churl;Kim, Younghee
    • Journal of the Korean Ceramic Society
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    • v.50 no.6
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    • pp.460-465
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    • 2013
  • Plate-shaped inorganic particles are coated onto a stainless steel substrate by the electrophoretic deposition of a precursor slurry which includes the inorganic particles of $Al_2O_3$ and polymer resin in mixed solvents to mimic the abalone shell structure, which is a composite of plate-shaped inorganic particles and organic interlayer binding materials with a layered orientation. The process parameters of the electrophoretic deposition include the voltage, coating time, and conductivity of the substrate. In addition, the suspension parameters are the particle size, concentration, viscosity, conductivity, and stability. We prepared an organic-inorganic composite coating with a high inorganic solid content by arraying the plate-shaped $Al_2O_3$ particles and electrophoretic resin via an electrophoretic deposition method. We analyzed the effect of the slurry composition and the electrophoretic deposition process parameters on the physical, mechanical and thermal properties of the coating layer, i.e., the thickness, density, particle orientation, Young's modulus and thermogravimetric analysis results.