• Title/Summary/Keyword: Single-calcination

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Synthesis of CuO nanoparticles by liquid phase precursor process (액상프리커서법에 의한 산화구리(CuO) 나노 입자의 합성)

  • Seong-Whan Shinn
    • The Journal of the Convergence on Culture Technology
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    • v.9 no.6
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    • pp.855-859
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    • 2023
  • Copper oxide (CuO) nanoparticles were successfully synthesized using a precursor in which industrial starch was impregnated with an aqueous solution of copper (II) nitrate trihydrate. The microstructure of the precursor impregnated with an aqueous solution of copper nitrate trihydrate was confirmed with a scanning electron microscope (SEM), and the particle size and the crystal structure of the copper oxide particles produced as the temperature of the heat treatment of the precursor increased was analyzed by X-ray diffraction (XRD) and the scanning electron microscope (SEM). As a result of the analysis, it was confirmed that the temperature at which the organic matter of the precursor is completely thermally decomposed is 450-490℃, and that the size and crystallinity of the copper oxide particles increased as the heat treatment temperature increased. The size of the copper oxide particles obtained through heat treatment at 500-800℃ during 1 hour was 100nm~2㎛. It was confirmed that the copper oxide crystalline phase is formed at a heat treatment temperature of 400℃, and only the copper oxide single phase existed up to 800℃. And it was also confirmed that the size of particles produced increased as the calcination temperature increased.

Study on Low-Temperature sintering of Co2Z type Ba ferrites for chip inductor (Chip inductor용 Co2Z type Ba-ferrite의 저온소결에 관한 연구)

  • 조균우;한영호;문병철
    • Journal of the Korean Magnetics Society
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    • v.12 no.5
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    • pp.195-200
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    • 2002
  • Low temperature sintering of Co$_2$Z type Ba ferrites with various oxide additives has been studied. Co$_2$Z phase was obtained by 2 step calcination and XRD peaks showed a good agreement with the peaks of the standard Co$_2$Z phase, except for some minor extra peaks. ZnO-B$_2$O$_3$ glass, ZnO-B$_2$O$_3$ and CuO, ZnO-B$_2$O$_3$ and Bi$_2$O$_3$, and ZnO-Bi$_2$O$_3$ glass were added to lower sintering temperatures. Specimens were sintered at the temperature range between 900 $^{\circ}C$ and 1000 $^{\circ}C$. In the single addition of ZnO-B$_2$O$_3$ glass, the specimen with 7.5 wt% showed the highest shrinkage. Specimens with complex addition of ZnO-B$_2$O$_3$ glass with CuO or Bi$_2$O$_3$ showed higher shrinkages and initial permeabilities than single addition of ZnO-B$_2$O$_3$ glass. Shrinkages and initial permeabilities of the specimens with ZnO-Bi$_2$O$_3$ glass were higher than those of ZnO-B$_2$O$_3$ glass addition.

Structure and Magnetic Properties on Synthesis Route of Co2Z-type Barium Hexaferrite (Co2Z-type Barium Hexaferrite의 합성방법에 따른 결정구조 및 자기적 특성)

  • Baek, In Seung;Nam, In Tak
    • Journal of the Korean Magnetics Society
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    • v.24 no.1
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    • pp.1-10
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    • 2014
  • $Co_2Z$-type barium ferrites ($Ba_3Co_2Fe_{24}O_{41}$) were synthesized using variation method. First, M-type, $Co_2Y$-type and $Co_2Z$-type synthesized by hydrothermal method. Second, M- and Y-type precursors for synthesis of $Co_2Z$ hexaferrite by hydrothermal and ball milling method. the morphology, structure and magnetic properties of the barium ferrite particles were characterized using XRD, FESEM, VSM, impedance. As a result, Single phase of M-type and $Co_2Y$-type were obtained. Manufactured powders of M+Y ball milling, M+Y hydrothermal were similar to single phase of $Co_2Z$-type hexaferrite, all powders were obtained theoretical magnetization (50 emu/g). The largest initial permeability were obtained $Co_2Z$ hexaferrite synthesized by reagent precusor, With increasing calcination temperature was lowered the initial permeability. In another synthesis didn't almost that little change could be found.

Preparation and properties of porous (Ca,Mg)0.15Zr0.7O1.7 ceramics (다공성 (Ca,Mg)0.15Zr0.7O1.7 세라믹스의 제조 및 특성)

  • Kim, Bok-Hee;Kim, Sang-Hee;Choi, Eun-Sil
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.21 no.2
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    • pp.70-74
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    • 2011
  • [ $(Ca,Mg)_{0.15}Zr_{0.7}O_{1.7}$ ]ceramics was investigated for the application to SOFC ceramic supporter with high porosity and mechanical strength. $ZrO_2$ powder was prepared by combustion method with glycine using the solution of $ZrO(NO_3)_2{\cdot}2H_2O$ dissolved into deionized water and calcination at $800^{\circ}C$ Porous $(Ca,Mg)_{0.15}Zr_{0.7}O_{1.7}$ ceramics was prepared by sintering the mixture of prepared $ZrO_2$ powder, dolomite and carbon black at $1200{\sim}1400^{\circ}C$ for 1 h. The open porosity ofthe $(Ca,Mg)_{0.15}Zr_{0.7}O_{1.7}$ ceramics sintered at $1300^{\circ}C$ was over 30 % and increased linearly with the amount of carbon black. The crystal structure of $(Ca,Mg)_{0.15}Zr_{0.7}O_{1.7}$ ceramics consisted of single cubic phase. The open pore of this ceramics was connected continuously and distributed well on the whole. This ceramics sintered at $1300^{\circ}C$ showed the porosity from 32 to 55 % and mechanical strength from 90 MPa to 30 MPa with increasing the content of added carbon black.

A Study on the Catalytic Characteristics of Oxygen Reduction in an Alkaline Fuel Cell I. Synthesis of La0.6Sr0.4Co1-xFexO3 and Reduction Reaction of Oxygen (알칼리형 연료전지에서 산소환원에 미치는 촉매 특성 연구 I. La0.6Sr0.4Co1-xFexO3의 합성과 산소환원반응)

  • Moon, Hyeung-Dae;Lee, Ho-In
    • Applied Chemistry for Engineering
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    • v.7 no.3
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    • pp.543-553
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    • 1996
  • Oxygen reduction in an alkaline fuel cell was studied by using perovskite type oxides as an oxygen electrode catalyst. The high surface area catalysts were prepared by malic acid method and had a formula of $La_{0.6}Sr_{0.4}Co_{1-x}Fe_xO_3$(x=0.00, 0.01, 0.10, 0.20, 0.35 and 0.50). From the result of XRD pattern and specific surface area due to the amount of Fe substitution and the consumption of ammonia-water, the complex formation of Fe ion with $NH_3$ was the main factor for both the phase stability of perovskite and the increase of specific surface area. Multi-step calcination was necessary to give a single phase of perovskite in catalyst precursor. The crystal structure of the catalysts was simple cubic perovskite, which was verified from the XRD patterns of the catalysts. The activity of oxygen reduction was monitored by the techniques of cyclic voltammetry, static voltage-current method, and current interruption method. The activity(current density) of oxygen reduction showed its minimum at x=0.01 and its maximum between 0.20 and 0.35 of x-value in $La_{0.6}Sr_{0.4}Co_{1-x}Fe_xO_3$. This tendency was independent of the change of surface area.

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Preparation of Al-doped NiO via Solvothermal Synthesis and its Crystal Structural and Electrical Properties (용매열 합성법을 통하여 알루미늄을 도핑한 니켈옥사이드의 제조와 그 결정구조적, 전기적 특성)

  • Hong, Sun-Ki;Ji, Mi-Jung;Lee, Min-Jin;Jung, Sung-Hun;Seol, Kwang-Hee;Choi, Byung-Hyun
    • Korean Journal of Materials Research
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    • v.22 no.11
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    • pp.631-635
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    • 2012
  • Nickel oxide was doped with a wide range of concentrations (mol%) of Aluminum (Al) by solvothermal synthesis; single-phased nano powder of nickel oxide was generated after calcination at$900^{\circ}C$. When the concentration of Al dopant was increased, the reduced intensity was confirmed through XRD analysis. Lattice parameters of the synthesized NiO powder were decreased after treatment of the dopant; parameters were increased when the concentration of Al was over the doping limit (5 mol% Al). The binding energy of $Ni^{2+}$ was chemically shifted to $Ni^{3+}$ by doping $Al^{3+}$ ion, as confirmed by the XPS analysis. The tilted structure of the synthesized NiO with 5 mol% Al dopant and the polycrystalline structure of the $Ni_{0.75}Al_{0.25}O$ were observed by HR-TEM analysis. The electrical conductivity of the newly synthesized NiO was highly improved by Al doping in the conductivity test. The electrical conductivity values of the commercial NiO and the synthesized NiO with 5 mol% Al dopant ($Ni_{0.95}Al_{0.05}O$) were 1,400 s/cm and 2,230 s/cm at $750^{\circ}C$, respectively. However, the electrical conductivity of the synthesized NiO with 10 mol% Al dopant ($Ni_{0.9}Al_{0.1}O$) decreased due to the scattering of free-electrons caused by the large number of impurity atoms; the electrical conductivity of $Ni_{0.9}Al_{0.1}O$ was 545 s/cm at $750^{\circ}C$.

Fabrication of YAG : Er3+ powders for the single crystal growth according to the synthetic temperature and flux concentration (다양한 온도조건과 flux 첨가량에 따른 단결정 성장용 YAG : Er3+ 분말 제조)

  • Park, Cheol Woo;Kang, Suk Hyun;Park, Jae Hwa;Kim, Hyun Mi;Choi, Jae Sang;Kang, Hyo Sang;Shim, Kwang Bo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.4
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    • pp.166-171
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    • 2015
  • In this study, using solid-state and flux, $Y_3Al_5O_{12}:Er^{3+}\;(YAG:Er^{3+})$ powders were successfully synthesized at low temperatures. To analyze the crystallinity of powders according to the synthesis or non-synthesis of powders and powder calcination temperatures, X-ray diffraction (XRD) was measured. In the case of pure YAG, when YAG was analyzed using the general solid-phase method, it was calcined for 12 hours at $1400^{\circ}C$ and pure YAG phase could be obtained. But when $BaF_2$ was added to YAG, YAG was synthesized at lower temperature (1000^{\circ}C$). It was thus found that the synthesis temperature could be lowered by about $400^{\circ}C$. Also, when BaF2 with an optimal concentration was added to $YAG:Er^{3+}$, the particle shape and size according to synthesis temperatures were surveyed, and corresponding luminous intensity was discussed.

Phase Formation Behavior and Charge-discharge Properties of Carbon-coated Li2MnSiO4 Cathode Materials for Lithium Rechargeable Batteries (리튬이차전지용 탄소 코팅된 Li2MnSiO4 양극활물질의 상형성 거동 및 충방전 특성)

  • Sun, Ho-Jung;Chae, Suman;Shim, Joongpyo
    • Journal of the Korean Electrochemical Society
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    • v.18 no.4
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    • pp.143-149
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    • 2015
  • Carbon-coated $Li_2MnSiO_4$ powders as the active materials for the cathode were synthesized by planetary ball milling and solid-state reaction, and their phase formation behavior and charge-discharge properties were investigated. Calcination temperature and atmosphere were controlled in order to obtain the ${\beta}-Li_2MnSiO_4$ phase, which was active electrochemically, and the carbon-coated $Li_2MnSiO_4$ active material powders with near single phase ${\beta}-Li_2MnSiO_4$ could be fabricated. The particles of the synthesized powders were secondary particles composed of primary ones of about 100 nm size. The carbon incorporation was essential to enable the Li ions to be inserted and extracted from $Li_2MnSiO_4$ active materials, and the initial capacity of 192 mAh/g could be obtained in the $Li_2MnSiO_4$ active materials with 4.8 wt% of carbon.

Synthesis and Conductive Properties of Li1+xAlxTi2-x(PO4)3 (x = 0, 0.3, 0.5) by Sol-Gel Method (Sol-Gel법에 의한 Li1+xAlxTi2-x(PO4)3 (x = 0, 0.3, 0.5)의 합성 및 전도특성)

  • Moon, Jung-In;Cho, Hong-Chan;Song, Jeong-Hwan
    • Korean Journal of Materials Research
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    • v.22 no.7
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    • pp.346-351
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    • 2012
  • $Li_{1+x}Al_xTi_{2-x}(PO_4)_3$(LATP) is a promising solid electrolyte for all-solid-state Li ion batteries. In this study, LATP is prepared through a sol-gel method using relatively the inexpensive reagents $TiCl_4$. The thermal behavior, structural characteristics, fractured surface morphology, ion conductivity, and activation energy of the LATP sintered bodies are investigated by TG-DTA, X-ray diffraction, FE-SEM, and by an impedance method. A gelation powder was calcined at $500^{\circ}C$. A single crystalline phase of the $LiTi_2(PO_4)_3$(LTP) system was obtained at a calcination temperature above $650^{\circ}C$. The obtained powder was pelletized and sintered at $900^{\circ}C$ and $1000^{\circ}C$. The LTP sintered at $900{\sim}1000^{\circ}C$ for 6 h had a relatively low apparent density of 75~80%. The LATP(x = 0.3) pellet sintered at $900^{\circ}C$ for 6 h was denser than those sintered under other conditions and showed the highest ion conductivity of $4.50{\times}10^{-5}$ S/cm at room temperature. However, the ion conductivity of LATP (x = 0.3) sintered at $1000^{\circ}C$ decreased to $1.81{\times}10^{-5}$ S/cm, leading to Li volatilization and abnormal grain growth. For LATP sintered at $900^{\circ}C$ for 6 h, x = 0.3 shows the lowest activation energy of 0.42 eV in the temperature range of room temperature to $300^{\circ}C$.

Crystal structure and microstructure of Z-type hexaferrite (Ba, La)Co2Fe24O41 by molten salt synthesis (용융염 합성법에 의한 Z형 육방정 페라이트 (Ba, La)Co2Fe24O41계의 결정구조와 미세구조)

  • Lee, Do Hyeok;Kwon, Chae-Yeon;Moon, Kyoung-Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.31 no.5
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    • pp.197-202
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    • 2021
  • Synthesis of Z-type hexaferrite Ba3Co2Fe24O41 (Ba3Z) and Ba1.5La1.5Co2Fe24O41 (Ba1.5La1.5Z) powders were tried using molten salt synthesis after primary calcination. Ba3Z calcined at 1000℃ was formed with both M-type and Y-type hexaferrite, and then Z-type was obtained when sintered with molten salt at 1150℃ and 1200℃. In the case of Ba1.5La1.5Z calcined at 1000℃, however, M-type hexaferrite, CoFe2O4 (Spinel phase), and LaFeO3 were synthesized. As a result, Z-type hexaferrite was not synthesized after sintering with molten salt. In addition, the aspect ratio of the particles decreased as the sintering temperature increased with molten salt synthesis. To obtain a single-phase Ba1.5La1.5Z with a high aspect ratio, it is expected the raw materials have to calcine below the temperature of a spinel phase formation before sintering with molten salt.