• Title/Summary/Keyword: x-ray diffraction(XRD)

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Synthesis and Electrochemical Properties of Li[Fe0.9Mn0.1]PO4 Nanofibers as Cathode Material for Lithium Ion Battery by Electrospinning Method (전기방사를 이용한 리튬 이차전지용 양극활물질 Li[Fe0.9Mn0.1]PO4 나노 섬유의 합성 및 전기화학적 특성)

  • Kim, Cheong;Kang, Chung-Soo;Son, Jong-Tae
    • Journal of the Korean Electrochemical Society
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    • v.15 no.2
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    • pp.95-100
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    • 2012
  • $LiFePO_4$ is an attractive cathode material due to its low cost, good cyclability and safety. But it has low ionic conductivity and working voltage impose a limitation on its application for commercial products. In order to solve these problems, the iron($Fe^{2+}$)site in $LiFePO_4$ can be substituted with other transition metal ions such as $Mn^{2+}$ in pursuance of increase the working voltage. Also, reducing the size of electrode materials to nanometer scale can improve the power density because of a larger electrode-electrolyte contact area and shorter diffusion lengths for Li ions in crystals. Therefore, we chose electrospinning as a general method to prepare $Li[Fe_{0.9}Mn_{0.1}]PO_4$ to increase the surface area. Also, there have been very a few reports on the synthesis of cathode materials by electrospinning method for Lithium ion batteries. The morphology and nanostructure of the obtained $Li[Fe_{0.9}Mn_{0.1}]PO_4$ nanofibers were characterized using scanning electron microscopy(SEM). X-ray diffraction(XRD) measurements were also carried out in order to determine the structure of $Li[Fe_{0.9}Mn_{0.1}]PO_4$ nanofibers. Electrochemical properties of $Li[Fe_{0.9}Mn_{0.1}]PO_4$ were investigated with charge/discharge measurements, electrochemical impedance spectroscopy measurements(EIS).

Electrical Properties in $Pt/SrTiO_3/Pb_x(Zr_{0.52}, Ti_{0.48})O_3/SrTiO_3/Si$ Structure and the Role of $SrTiO_3$ Film as a Buffer Layer ($Pt/SrTiO_3/Pb_x(Zr_{0.52}, Ti_{0.48})O_3/SrTiO_3/Si$ 구조의 전기적 특성 분석 및 $SrTiO_3$박막의 완충층 역할에 관한 연구)

  • 김형찬;신동석;최인훈
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.11 no.6
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    • pp.436-441
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    • 1998
  • $Pt/SrTiO_3/Pb_x(Zr_{0.52}, Ti_{0.48})O_3/SrTiO_3/Si$ structure was prepared by rf-magnetron sputtering method for use in nondestructive read out ferroelectric RAM(NDRO-FEAM). PBx(Zr_{0.52}Ti_{0.48})O_3}$(PZT) and $SrTiO_3$(STO) films were deposited respectively at the temperatures of $300^{\circ}C and 500^{\circ}C$on p-Si(100) substrate. The role of the STO film as a buffer layer between the PZT film and the Si substrate was studied using X-ray diffraction (XRD), Auger electron spectroscopy (ASE), and scanning electron microscope(SEM). Structural analysis on the interfaces was carried out using a cross sectional transmission electron microscope(TEM). For PZT/Si structure, mostly Pb deficient pyrochlore phase was formed due to the serious diffusion of Pb into the Si substrate. On the other hand, for STO/PZT/STO/Si structure, the PZT film had perovskite phase and larger grain size with a little Pb interdiffusion. the interfaces of the PZT and the STO film, of the STO film and the interface layer and $SiO_2$, and of the $SiO_2$ and the Si substate had a good flatness. Across sectional TEM image showed the existence of an amorphous layer and $SiO_2$ with 7nm thickness between the STO film and the Si substrate. The electrical properties of MIFIS structure was characterized by C-V and I-V measurements. By 1MHz C-V characteristics Pt/STO(25nm)/PZT(160nm)/STO(25nm)/Si structure, memory window was about 1.2 V for and applied voltage of 5 V. Memory window increased by increasing the applied voltage and maximum voltage of memory window was 2 V for V applied. Memory window decreased by decreasing PZT film thickness to 110nm. Typical leakage current was abour $10{-8}$ A/cm for an applied voltage of 5 V.

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BaCeO3-BaZrO3 Solid Solution (BCZY) as a High Performance Electrolyte of Protonic Ceramic Fuel Cells (PCFCs) (BaCeO3-BaZrO3 고용체(BCZY) 기반 프로톤 세라믹 연료전지(PCFC)용 고성능 전해질 개발)

  • An, Hyegsoon;Shin, Dongwook;Choi, Sung Min;Lee, Jong-Ho;Son, Ji-Won;Kim, Byung-Kook;Je, Hae June;Lee, Hae-Weon;Yoon, Kyung Joong
    • Journal of the Korean Ceramic Society
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    • v.51 no.4
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    • pp.271-277
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    • 2014
  • To overcome the limitations of the solid oxide fuel cells (SOFCs) due to the high temperature operation, there has been increasing interest in proton conducting fuel cells (PCFCs) for reduction of the operating temperature to the intermediate temperature range. In present work, the perovskite $BaCe_{0.85-x}Zr_xY_{0.15}O_{3-\delta}$ (BCZY, x = 0.1, 0.3, 0.5, and 0.7) were synthesized via solid state reaction (SSR) and adopted as an electrolyte materials for PCFCs. Powder characteristics were examined using X-ray diffraction (XRD), thermogravimetric analysis (TGA) and Brunauer, Emmett and Teller (BET) surface area analysis. Single phase BCZY were obtained in all compositions, and chemical stability was improved with increasing Zr content. Anode-supported cell with $Ni-BaCe_{0.55}Z_{0.3}Y_{0.15}O_{3-\delta}$ (BCZY3) anode, BCZY3 electrolyte and BCZY3-$Ba_{0.5}Sr_{0.5}Co_{0.8}Fe_{0.2}O_{3-\delta}$ (BSCF) composite cathode was fabricated and electrochemically characterized. Open-circuit voltage (OCV) was 1.05 V, and peak power density of 370 ($mW/cm^2$) was achieved at $650^{\circ}C$.

Preparation of Na-X and Na-A Zeolites from Coal Fly Ash in a Thermoelectric Power Plant and Comparison of the Adsorption Characteristics for Cu(II) with a Commercial Zeolite (화력발전소 석탄비산재를 이용한 Na-X와 Na-A 제올라이트 제조 및 상업용 제올라이트와의 Cu(II) 흡착 특성 비교)

  • Choi, Yu-Lim;Angaru, Ganesh Kumar Reddy;Kim, Dong-Su;Ahn, Hye-Young;Kim, Dae-Ho;Choi, Chi-Dong;Reddy, Kodoru Janardhan;Yang, Jae-Kyu;Chang, Yoon-Young
    • Applied Chemistry for Engineering
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    • v.30 no.6
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    • pp.749-756
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    • 2019
  • Na-X and Na-A zeolites that give high adsorption capacity for heavy metals in an aqueous system were synthesized from the coal fly ash obtained from a thermoelectric power plant using a fusion method. The characteristics and Cu(II) adsorption capacity of the synthetic zeolites were also compared to those of using a commercial zeolite. For the selection of optimum conditions of zeolite synthesis, the effects of major parameters in the fusion method such as a dosage ratio of NaOH, aging time, hydrothermal reaction time, and also the dosage ratio of NaAlO2 (Na-A) on the characteristics and Cu(II) adsorption capacity of the synthetic zeolites were studied. For the analysis of characteristics of the synthetic zeolites, X-ray diffraction (XRD), cation exchange capacity (CEC), Brunaue-Emmett-Teller (BET) and scanning electron microscopy (SEM) were used. The optimum conditions for the synthesis of zeolites with a high adsorption capacity for cationic heavy metals including Cu(II) were the aging time of 6 h, hydrothermal reaction time of 6 h and NaOH and NaAlO2 dosage ratio of 1.5 and 0.5 (Na-A), respectively. According to the Langmuir isotherm test, maximum Cu(II) adsorption capacities of the synthetic and commercial Na-X and Na-A zeolites were found to be 90.1, 105.26, 102.05, and 109.89 mg/g, respectively. This indicates that the adsorption capacity of synthetic zeolites was comparable to commercial ones. The results of this study also suggest that the coal fly ash can be potentially used as a raw material for the zeolite synthesis.

A Study on Optimization of Nitric Acid Leaching and Roasting Process for Selective Lithium Leaching of Spent Batreries Cell Powder (폐 배터리 셀 분말의 선택적 리튬 침출을 위한 질산염화 공정 최적화 연구)

  • Jung, Yeon Jae;Park, Sung Cheol;Kim, Yong Hwan;Yoo, Bong Young;Lee, Man Seung;Son, Seong Ho
    • Resources Recycling
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    • v.30 no.6
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    • pp.43-52
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    • 2021
  • In this study, the optimal nitration process for selective lithium leaching from powder of a spent battery cell (LiNixCoyMnzO2, LiCoO2) was studied using Taguchi method. The nitration process is a method of selective lithium leaching that involves converting non-lithium nitric compounds into oxides via nitric acid leaching and roasting. The influence of pretreatment temperature, nitric acid concentration, amount of nitric acid, and roasting temperature were evaluated. The signal-to-noise ratio and analysis of variance of the results were determined using L16(44) orthogonal arrays. The findings indicated that the roasting temperature followed by the nitric acid concentration, pretreatment temperature, and amount of nitric acid used had the greatest impact on the lithium leaching ratio. Following detailed experiments, the optimal conditions were found to be 10 h of pretreatment at 700℃ with 2 ml/g of 10 M nitric acid leaching followed by 10 h of roasting at 275℃. Under these conditions, the overall recovery of lithium exceeded 80%. X-ray diffraction (XRD) analysis of the leaching residue in deionized water after roasting of lithium nitrate and other nitrate compounds was performed. This was done to determine the cause of rapid decrease in lithium leaching rate above a roasting temperature of 400℃. The results confirmed that lithium manganese oxide was formed from lithium nitrate and manganese nitrate at these temperatures, and that it did not leach in deionized water. XRD analysis was also used to confirm the recovery of pure LiNO3 from the solution that was leached during the nitration process. This was carried out by evaporating and concentrating the leached solution through solid-liquid separation.

Characteristics of Pd Catalysts for Methane Oxidation (메탄 산화를 위한 Pd 촉매의 특성)

  • Lee, Jin-Man;Yang, O-Bong;Kim, Chun-Yeong;Woo, Seong-Ihl
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.557-562
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    • 1999
  • The reaction properties of Pd. Pd-Ce and Pd-La catalysts supported on ${\gamma}-Al_2O_3$ were investigated in the oxidation reaction of methane($CH_4$) exhausted from the compressed natural gas vehicle in a U-tube flow reactor with gas hourly space velocity of $72,000h^{-1}$. The catalysts were characterized by X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS), BET surface area and hydrogen chemisorption. Pd catalyst prepared by $Pd(NO_3)_2$ as a palladium precursor and calcined at $600^{\circ}C$ showed the highest activity for a methane oxidation. Catalytic activity of calcined $Pd/{\gamma}-Al_2O_3$ in which most of palladium was converted into palladium oxide species was higher than that of reduced $Pd/{\gamma}-Al_2O_3$ in which most of palladium existed in palladium metal by XRD. As increasing the number of reaction cycles in the wide range of redox, the catalytic activity of $Pd/{\gamma}-Al_2O_3$ was decreased and the highly active window became narrower. Lanthanum oxide promoted Pd catalyst, $Pd/La/{\gamma}-Al_2O_3$ showed enhanced thermal stability compared with $Pd/{\gamma}-Al_2O_3$ even after aging at $1000^{\circ}C$, which was ascribed to the role of La as a promoter to suppress the sintering of palladium metal and ${\gamma}-Al_2O_3$ support. Almost all of methane was removed by the reaction with NO at the redox ratio of 1.2 in case of oxygen excluded steam, but that activity was significantly decreased in the steam containing oxygen.

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Mössbauer Study of Tb2Bi1GaxFe5-xO12(x=0, 1) (Tb2Bi1GaxFe5-xO12(x=0, 1)의 뫼스바우어 분광연구)

  • Park, Il-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.18 no.2
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    • pp.67-70
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    • 2008
  • $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) fabricated by sol-gel and vacuum sealed annealing process. $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) have been studied by x-ray diffraction(XRD), vibrating sample magnetometer, and $M\ddot{o}ssbauer$ spectroscopy. The crystal structures were found to be a cubic garnet structure with space group Ia3d. The determined lattice constants $a_0$ of x = 0, and 1 are $12.497\AA$, and $12.465\AA$, respectively. The distribution of gallium and iron in $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$ is studied by Rietveld refinement. Based on Rietveld refinement results, the terbium and bismuth ions occupy the 24c site, iron ions occupy the 24d, l6a site, and nonmagmetic gallium ions occupy the 16a site. In order to verify the magnetic site occupancy of iron and gallium, we have taken $M\ddot{o}ssbauer$ spectra for $Tb_2Bi_1Ga_xFe_{5-x}O_{12}$(x=0, 1) at room temperature. From the results of $M\ddot{o}ssbauer$ spectra analysis, the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 60.8 % and 39.2 %, respectively, and the absorption area ratios of Fe ions for $Tb_2Bi_1Fe_5O_{12}$ on 24d and 16a sites are 74.7 % and 25.3 %, respectively. It is noticeable that all of the nonmagnetic Ga atoms occupy the 16a site by vacuum annealing process.

Hydrothermal Mechanism of Na-A Type Zeolite from Natural Siliceous Mudstone (규질 이암으로부터 Na-A형 제올라이트 수열합성 반응기구에 대한 연구)

  • Bae, In-Kook;Jang, Young-Nam;Chae, Soo-Chun;Kim, Byoung-Gon;Ryu, Kyoung-Won;Lee, Sung-Ki
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.3
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    • pp.223-229
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    • 2007
  • The mechanism of hydrothermally synthesizing Na-A zeolite from siliceous mudstone at a $Na_2O/SiO_2$ ratio of 0.6, a $SiO_2/Al_2O_3$ 2.0 and a $H_2O/Na_2O$ 119 has been observed by IR, DTA, XRD and SEM. This mudstone is a tertiary periodic sedimentary rock and widely spreads around the Pohang area. In the early hydrothermal synthesis at $80^{\circ}C$ in an autoclave, sodium silicate and sodium aluminate were found to be preferentially reacted to generate Na-A type zeolite. Gibbsite and bayerite were also formed due to the presence of extra aluminum oxide in the feedstock. As reaction time in-creased up to 50 h, residual sodium aluminatewas reacted with siliceous mudstone, causing the Na-A zeolite crystal to grow and the hydroxylsodalite to generate. Therefore, in the $14{\sim}50\;h$ synthetic time, Na-A zeolite and hydroxylsodalite were formed. Also, if reaction time passed over 50 h, a part of the Na-A zeolite was finally redissolved and reacted with hydroxylsodalite to synthesize Na-P zeolite, generating porous surface of Na-A zeolite and disappearing hydroxylsodalite.

Electrical Properties of $Ba_{1-x}(Bi_{0.5}K_{0.5})TiO_3$ according to $(Bi_{0.5}K_{0.5})TiO_3$ for Pb-free PTC (Pb-free PTC에 있어서 $(Bi_{0.5}K_{0.5})TiO_3$ 첨가에 따른 $Ba_{1-x}(Bi_{0.5}K_{0.5})TiO_3$의 전기적특성)

  • Lee, Mi-Jai;Choi, Byung-Hyun;Paik, Jong-Hoo;Kim, Bip-Nam;Lee, Woo-Yong
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.35-36
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    • 2008
  • PTC thermistor are characterized by an increase in the electrical resistance with temperature. The PTC materials of middle Curie point were produced or that of high Curie point (above $200^{\circ}C$), it was determined that compositional modifications of $Pb^{2+}$ for $Ba^{2+}$ produce change sin the Curie point to higher temperature. PTC ceramic materials with the Curie point above $120^{\circ}C$ were prepared by adding $PbTiO_3$, PbO or $Pb_3O_4$ into $BaTiO_3$. Thereby, adding $Pb^{2+}$ into $BaTiO_3$-based PTC material to improve Tc was studied broadly, however, weal know that PbO was poisonous and prone to volatilize, then to pollute the circumstance and hurt to people, so we should dope other innocuous additives instead of lead to increase Tc of composite PTC material. In order to prepare lead-free $BaTiO_3$-based PTC with middle Curie point, the incorporation on $Bi_{1/2}K_{1/2}TiO_3$ into $BaTiO_3$-based ceramics was investigated on samples containing 0, 1, 2, 3, 4, and 50mol% of $Bi_{1/2}K_{1/2}TiO_3$. $Bi_{1/2}K_{1/2}TiO_3$ was compounded as standby material by conventional solid-state reaction technique. The starting materials were $Bi_2O_3$, $K_2CO_3$, $BaCO_3$ and $TiO_2$ powder, and using solid-state reaction method, too. The microstructures of samples were investigated by SEM, DSC, XRD and dielectric properties. Phase composition and lattice parameters were investigated by X-ray diffraction.

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Crystallographic and Magnetic Properties of KFeO2 (KFeO2 분말의 제조 및 뫼스바우어 분광학 연구)

  • Moon, Seung-Je;Shim, In-Bo;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.38-42
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    • 2007
  • The crystallographic and magnetic properties of $KFeO_2$ powder prepared by ball-mill method, have been studied by x-ray diffraction(XRD), $M\"{o}ssbauer$ spectroscopy, and vibrating sample magnetometer(VSM) measurements. The crystal structure of $KFeO_2$ powder at room temperature is determined to be an orthorhombic structure of Pbca with its lattice constants $a_0=5.557{\AA},\;b_0=11.227{\AA},\;c_0=15.890{\AA}$ by Rietveld refinement. $M\"{o}ssbauer$ spectra of $KFeO_2$ were taken at various temperatures ranging from 4.2 to 818 K. The magnetic hyperfine field and isomer shift value at 4.2 K and RT were 519 kOe, 489 kOe and 0.19 mm/s, 0.05 mm/s respectively. The average hyperfine field $H_{hf}(T)$ of the $KFeO_2$ shows a temperature dependence of $[H_{hf}(T)-H_{hf}(0)]/H_{hf}(0)=-0.36(T/T_N)^{5/2}$ for $T/T_N$<0.7, indicative of spin-wave excitation.