• Title/Summary/Keyword: XRD분석

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Mineralogy of Alunite from the Sungsan Mine (성산광산(聲山鑛山) 명반석(明礬石)의 광물학적(鑛物學的) 특성(特性))

  • Cho, Hyen Goo;Kim, Soo Jin
    • Journal of the Mineralogical Society of Korea
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    • v.2 no.2
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    • pp.81-89
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    • 1989
  • Alunite occurs as massive, cavity-filling and veinlets in the Cretaceous Hwangsan Formation in the Sungsan mine, Korea. It is a hydrothermal alteration product of rhyolitic tuffs, and associated with dickite, quartz and barite. The average chemical formula of alunite in the mine is $(K_{0.93}Na_{0.07})_{1.00}Al_{3.00}(SO_4)_{2.00}(OH)_6$. Atomic percentage of Na substituting for K in A site of the alunite structure varies from 5.9 to 9.2. Unit-cell volume and c dimension decrease with increasing Na atomic percentage. On the basis of thermal and high temperature XRD analyses, the decomposition of alunite into $KAl(SO_4)_2$ and $NaAl(SO_4)_2$ concomitant with the liberation of structural water (12.86%) occurs at about $550^{\circ}C$. The reconstruction of $KAl(SO_4)_2$ and $NaAl(SO_4)_2$ to $Al_2(SO_4)_3$, arcanite and thenardite, and the crystallization of ${\gamma}-Al_2O_3$ take place at about $720^{\circ}C$. The destruction of $Al_2(SO_4)_3$ structure takes place at about $760^{\circ}C$ removing 3/4 of total $SO_3$ (27.32%).

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Studies on Crystallographic and Mossbauer Spectra of the LiFe0.9Mn0.1PO4 (LiFe0.9Mn0.1PO4 물질의 결정구조 및 뫼스바우어 분광 연구)

  • Kwon, Woo-Jun;Lee, In-Kyu;Rhee, Chan-Hyuk;Kim, Sam-Jin;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.22 no.1
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    • pp.15-18
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    • 2012
  • The olivine structured $LiFe_{0.9}Mn_{0.1}PO_4$ material was prepared by solid state method, and was analyzed by x-ray diffractometer (XRD), superconducting quantum interference devices (SQUID) and Mossbauer spectroscopy. The crystal structure of $LiFe_{0.9}Mn_{0.1}PO_4$ was determined to be orthorhombic (space group: Pnma) by Rietveld refinement method. The value of N$\acute{e}$el temperature ($T_N$) for $LiFe_{0.9}Mn_{0.1}PO_4$ was determined 50 K. The temperature dependence of the magnetization curves showed magnetic phase transition from paramagnetic to antiferromagnetic at $T_N$ by SQUID measurement. M$\ddot{o}$ssbauer spectra of $LiFe_{0.9}Mn_{0.1}PO_4$ showed 2 absorption lines at temperatures above $T_N$ and showed asymmetric 8 absorption lines at temperatures below $T_N$. These spectra occurred due to the magnetic dipole and electric quardrupole interaction caused by strong crystalline field at asymmetric $FeO_6$ octahedral sites.

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.

Mössbauer Studies of Changed Interaction on Cr Ions in Chromite (Chromite 물질의 자기상호작용에 관한 뫼스바우어 분광연구)

  • Choi, Kang-Ryong;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.17 no.1
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    • pp.47-50
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    • 2007
  • [ $ZnCr_2O_4$ ] shows geometrically frustrated magnet. Recently, $CoCr_2O_4$ has been investigated for multiferroic property and dielectric anomalies by spin-current model. Polycrystalline $CoCr_2O_4$ and $CoCrFeO_4$ compounds was prepared by wet-chemical process. Crystallographic and magnetic properties of $CoCr_2O_4$ and $CoCrFeO_4$ were investigate by using the x-ray diffractometer(XRD), vibrating sample magnetometer(VSM), superconducting quantum interference device magnetometer(SQUID), and $M\"{o}ssbauer$ spectroscopy. The crystal structure was found to be single-phase cubic spinel with space group of Fd3m. The lattice constants of $CoCr_2O_4$ and $CoCrFeO_4$ $a_0$ were determined to be 8.340 and 8.377 ${\AA}$, respectively. The ferrimagnetic transition temperature for the both samples were observed at 97 K and 320 K. The $M\"{o}ssbauer$ absorption spectra at 4.2 K show that the well developed two sextets are superposed with small difference of hyperfine field($H_{hf1}=507\;and\;H_{hf2}=492\;kOe$). Isomer shift values($\delta$) of the two sextets are found to be 0.33 and 0.34 mm/s relative to the Fe metal, respectively, which are consistent with the high spin $Fe^{3+}$ charge state.

Effects of Temperature on A Synthesized Birnessite (온도 변화에 따른 합성 버네사이트 특성 변화 연구)

  • Park, Soo Oh;Kim, Young Jae;Lee, Young Jae
    • Journal of the Mineralogical Society of Korea
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    • v.26 no.2
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    • pp.81-86
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    • 2013
  • A series of birnessite was synthesized at 25, 40, 60, and $80^{\circ}C$, respectively. Intensities of XRD and the ratio of signal to noise of the peaks for samples increases with increasing temperature up to $60^{\circ}C$, whereas the intensity and ratio for a sample synthesized at $80^{\circ}C$ decrease, showing that crystallinity of the birnessite synthesized at $60^{\circ}C$ is better than that of the synthesized at $80^{\circ}C$. However, BET surface areas for these two samples show that the surface area increases 39.4 to 89.7 $m^2/g$ with increasing synthesizing temperature from 60 up to $80^{\circ}C$, indicating that a small surface area is shown in a well-crystallized birnessite rather than that of a poorly crystallized birnessite. SEM images show that morphologies for samples are seriously influenced by temperature. The morphology of the synthesized at 25 shows a round-shape, while a plate-like morphology is shown in the synthesized birnessite at $80^{\circ}C$. In addition, a porous layered structure is also shown in the synthesized birnessite at $80^{\circ}C$. These results suggest that physicochemical properties of the synthesized birnessite are sensitively affected by mechanical changes of parameters such as temperature during the synthesization.

Transition of 12CaO·7Al2O3 electrical insulator to the permanent semiconductor using via thermo-chemical reduction treatment (열 화학적 환원 처리를 이용한 절연체 12CaO·7Al2O3의 전도체로의 전환)

  • Chung, Jun-Ho;Eun, Jong-Won;Oh, Dong-Keun;Kim, Kwang-Jin;Hong, Tae-Ui;Jeong, Seong-Min;Choe, Bong-Geun;Shim, Kwang-Bo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.4
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    • pp.178-184
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    • 2010
  • The $12CaO{\cdot}7Al_2O_3$(C12A7) powders were successfully synthesized using combustion method with microwave-assistant and C12A7:H were fabricated by post-annealed process in Ar/H atmosphere. X-ray diffraction patterns and TGDSC were used for investigating to the precursors of crystalline and reaction depending on temperature. C12A7:H that was treated post-annealed process were investigated TG-MS and Hall-measurement for confirming H ions doping and checking electrical resistivity of C12A7:H. H ion substituted to $O^{2-}$ ions in the C12A7 cages were confirmed at $289.5^{\circ}C$ by TG-MS and C12A7:H calcined at $1000^{\circ}C$ in Ar/H=8:2 atmosphere for 8~10 h has low electrical resistivity about $10^2{\Omega}{\cdot}cm$ at room temperature.

Steam Reforming of Ethylene Glycol over Ni/Al2O3 Catalysts: Effect of the Preparation Method and Reduction Temperature (Ni/Al2O3 촉매를 사용한 에틸렌글리콜의 수증기 개질 반응: 촉매 제조 방법과 환원온도의 영향)

  • Choi, Dong Hyuck;Park, Jung Eun;Park, Eun Duck
    • Korean Chemical Engineering Research
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    • v.53 no.3
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    • pp.372-381
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    • 2015
  • The effect of preparation method on the catalytic activities of the $Ni/Al_2O_3$ catalysts on steam reforming of ethylene glycol was investigated. The catalysts were prepared with various preparation methods such as an incipient wetness impregnation, wet impregnation, and coprecipitation method. In the case of coprecipitation method, various precipitants such as KOH, $K_2CO_3$, and $NH_4OH$ were compared. The prepared catalysts were characterized by using $N_2$ physisorption, inductively coupled plasma-atomic emission spectroscopy, X-ray diffraction, temperatureprogrammed reduction, pulsed $H_2$ chemisorption, temperature-programmed oxidation, scanning electron microscopy, and thermogravimetric analysis. Among the catalysts reduced at 773 K, the $Ni/Al_2O_3$ catalyst prepared by a coprecipitation with KOH or $K_2CO_3$ as precipitants showed the best catalytic performance. The preparation method affected the particle size of Ni, reducibility of nickel oxides, catalytic performance (activity and stability), and types of coke formed during the reaction. The $Ni/Al_2O_3$ catalyst prepared by a coprecipitation with KOH showed the increasing catalytic activity with an increase in the reduction temperature from 773 to 1173 K because of an increase in the reduction degree of Ni oxide species even though the particle size of Ni increased with increasing reduction temperature.

Property Analysis of Ceramic Interconnect Prepared by Thermal Plasma Spray Coating Method for SOFC (Thermal Plasma Spray Coating 법에 의해 코팅된 SOFC용 세라믹 연결재 특성 분석)

  • Park, Kwang-Yeon;Pi, Seuk-Hoon;Lee, Jong-Won;Lee, Seung-Bok;Lim, Tak-Hyoung;Park, Seok-Joo;Song, Rak-Hyun;Shin, Dong-Ryul
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.710-714
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    • 2011
  • In present work, $La_{0.8}Ca_{0.2}CrO_{3}$(LCC), $La_{0.8}Sr_{0.2}CrO_{3}$(LSC) and $La_{0.8}Ca_{0.2}CrO_{0.9}Co_{0.1}O_{3}$(LCCC) ceramic interconnect layer for SOFC were prepared by using thermal plasma spray coating process. The LCC, LSC and LCCC powders were characterized by x-ray diffraction(XRD), scanning electron microscopy(SEM), particle counter and BET analysis. In addition, basic and essential properties such as the surface morphology, cross section, gas leak rate, and electrical conductivity of LCC, LSC, and LCCC layers coated by thermal plasma spray coating process were analyzed and discussed. Based on these experimental results, it can be concluded that the LCCC layer coated by thermal plasma spray coating process can be suitable as a ceramic interconnect of SOFC.

Synthesis and Defect-Structure Analysis of $ThO_2-Tm_2O_3$ Solid Solutions ($ThO_2-Tm_2O_3$ 고용체의 합성 및 결함구조해석)

  • Don Kim;Chang Kwon Kang;Keu Hong Kim;Jae Shi Choi
    • Journal of the Korean Chemical Society
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    • v.31 no.6
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    • pp.491-497
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    • 1987
  • $ThO_2-Tm_2O_3$ (TDT) solid solutions containing 1,3,5,8,10, and 15 mol% $Tm_2O_3$ were synthesized from spectroscopically pure $ThO_2$ and $Tm_2O_3$ polycrystalline powders. The TDT solid solutions were indentified to the fluorite structure by the X-ray powder technique. The values of the lattice parameter were decreased with increasing amount of $Tm_2O_3$ incorporated. But, there was no linearity for the samples containing 8, 10, and 15 mol% $Tm_2O_3$. It was concluded that these samples became incomplete solid solutions. From the intensity analyses of X-ray diffraction patterns, the residual factor was found below 0.13 even for the 15 mol% TDT system. lt was confirmed from the DTA and TGA analyses that any phase transitions did not occur under the experimental condition executed. Comparing the pycnometric density with the lattice parameter obtained from XRD, it was suggested that the predominant defect model be an oxygen vacancy.

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Characteristics and Physical Property of Tungsten(W) Related Diffusion Barrier Added Impurities (불순물을 주입한 텅스텐(W) 박막의 확산방지 특성과 박막의 물성 특성연구)

  • Kim, Soo-In;Lee, Chang-Woo
    • Journal of the Korean Vacuum Society
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    • v.17 no.6
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    • pp.518-522
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    • 2008
  • The miniaturization of device size and multilevel interlayers have been developed by ULSI circuit devices. These submicron processes cause serious problems in conventional metallization due to the solubility of silicon and metal at the interface, such as an increasing contact resistance in the contact hole and interdiffusion between metal and silicon. Therefore it is necessary to implement a barrier layer between Si and metal. Thus, the size of multilevel interconnection of ULSI devices is critical metallization schemes, and it is necessary reduce the RC time delay for device speed performance. So it is tendency to study the Cu metallization for interconnect of semiconductor processes. However, at the submicron process the interaction between Si and Cu is so strong and detrimental to the electrical performance of Si even at temperatures below $200^{\circ}C$. Thus, we suggest the tungsten-carbon-nitrogen (W-C-N) thin film for Cu diffusion barrier characterized by nano scale indentation system. Nano-indentation system was proposed as an in-situ and nanometer-order local stress analysis technique.