• Title/Summary/Keyword: high temperature X-ray diffraction

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Synthesis and characterization of AlN nanopowder by the microwave assisted carbothermal reduction and nitridation (CRN)

  • Chun, Seung-Yeop;Chun, Myoung-Pyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.27 no.5
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    • pp.223-228
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    • 2017
  • Aluminum nitride (AlN) powder was successfully synthesized at low temperature via carbothermal reduction and nitridation (CRN) assisted by microwave heating. The synthesis processes of AlN powder were investigated with X-ray diffraction, FE-SEM, FT-IR and TGA/DSC. Aluminum nitrate was used as an oxidizer and aluminum source, urea as fuel, and glucose as carbon source. These starting materials were mixed with D.I water and reacted in a flask at $100^{\circ}C$ for 20 minutes. After the reaction was finished, black foamy intermediate product was formed, which was considered to be an amorphous $Al_2O_3$ particles through intermediate product obtained by solution combustion synthesis (SCS) at the results of X-ray diffraction patterns and FT-IR. This intermediate product was nitridated at temperatures of $1300^{\circ}C$ and $1400^{\circ}C$ in $N_2$ atmosphere by a microwave heating furnace and then decarbonated at $600^{\circ}C$ for 2 hours in air. It should be noticed from FE-SEM images that as nitridated particles, identified as AlN from X-ray diffraction patterns, are covered with carbon residues. After decarbonating the nitridated powders, the spherical pure AlN powders were obtained without alumina and their particle sizes were dependent on the nitridating temperature with high temperature of $1400^{\circ}C$ giving large particles of around 70~100 nm.

A Study on Reaction Products between Cokes and Kaolinites (국산 cokes를 이용한 고급복합내화재료개발에 관한 연구)

  • 이희수;박정현;오영제
    • Journal of the Korean Ceramic Society
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    • v.15 no.1
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    • pp.28-34
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    • 1978
  • In order to develop the high refractory composite materials consisting of mullite and carborundum, Hadong kaolin and coal coke were selected as the starting materials. Silicone carbide crystals formed during the high-temperature reaction between kaolin and coke were detected by X-ray diffraction method and identified by electron diffraction. The temperature at which the amorphous silicone carbide begins to crystallize could be assumed to be about 155$0^{\circ}C$, which is the lower temperature claimed by others.

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Thermal behavior of the layered structure of decanesulfonate intercalated into the hydrated nickel compound (데칸술폰이 삽입된 니켈 화합물의 층상 구조의 열적 성질)

  • 허영덕;전태현;박용준
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.6
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    • pp.580-584
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    • 1999
  • The synthesis and characterization of intercalated compound of decansulfonate into hydrated nickel is presented. The compound shows a layered structure as determined by high temperature powder X-ray diffraction (HTXRD). The layer distance of the product is increased from 24.7 $\AA$ to 30.5 $\AA$ by increasing the temperature which is in turn accomplished by changing the structure of the intercalated nickel compound. From the X-ray diffraction data and the decanesulfonate size, the orientation of the decanesulfonate onto the nickel layer is determined. The molecular axis of the decanesulfonate with bilayer structure is tilted to the perpendicular of the nickel layer.

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Diffraction Characteristics of Mechanically Alloyed Nanocrystalline FeAl (기계적합금화한 FeAl 나노결정립의 회절특성)

  • Choi, Keun-Seob;Kim, Do-Hyang;Hong, Kyung-Tae
    • Applied Microscopy
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    • v.27 no.4
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    • pp.473-481
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    • 1997
  • Disorder-order transformation of nanocrystalline FeAl have been investigated by a combination of electron and X-ray diffraction analysis including high resolution electron microscopy and differential scanning calorimetry. Fe-50at.%Al powders mechanically alloyed for 90 hours consist of $5\sim10$ nm size grains haying either disordered b.c.c. structure or amorphous structure. X-ray and electron diffraction of mechanically alloyed FeAl powders show that disorder-order transformation occurs at the temperature range of $300^{\circ}C\sim320^{\circ}C$. Such a low-temperature ordering behavior exhibiting an exothermic reaction is attributable to the nm-scale grain structure with a large amount of defects accumulated during mechanical alloying process.

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High Pressure X-ray Diffraction Studies on a Natural Talc (천연산 활석에 대한 고압 X-선 회절연구)

  • 김영호;이지은
    • Journal of the Mineralogical Society of Korea
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    • v.12 no.1
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    • pp.1-10
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    • 1999
  • Talc (Mg3Si4O10(OH)2), one of the sheet silicate minerals, which is the hydrothermal alteration product of serpentinite at Cheongarm mine was prepared for the high pressure compressibility studies. Energy dispersive X-ray diffraction experiment was carried out using the Synchrotron Radiation with the Mao-Bell type diamond anvil cell at room temperature. Polycrystalline talc was mixed with MgO powder for pressure sensor as well as pressure medium in the sample chamber. High pressure runs were performed at pressures up to 35.2 GPa. Talc shows no phase transition within the present high pressure region. Bulk modulus of this talc was determined by the Birch-Murnaghan equation of state to be 78 GPa assuming its first pressure derivative Ko' of 4.

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Compression Study on a Synthetic Goethite (합성 괴타이트에 대한 압축실험)

  • Kim, Young-Ho;Hwang, Gil-Chan;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.4
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    • pp.325-330
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    • 2009
  • High pressure x-ray diffraction study was performed on a synthetic FeOOH-goethite to check out its compressibility at room temperature. Angular dispersive x-ray diffraction method was employed using a symmetrical diamond anvil cell with synchrotron radiation. Bulk modulus was determined to be 222.8 GPa under assumption of $K_{T'}$ of 4.0. This value is too high comparing with the previously published values from natural samples. It has been discussed the possible causes to incur its high bulk modulus value according to the production conditions.

Preparation, Structure, and Photoemission Studies on the High Temperature Superconductor $YBa_2Cu_{3-x}Ni_xO_{7-{\delta}}$

  • Choy, Jin-Ho;Choe, Won-Young
    • Bulletin of the Korean Chemical Society
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    • v.11 no.5
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    • pp.379-383
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    • 1990
  • $YBa_2Cu_{3-x}Ni_xO_{7-{\delta}}$, with x = 0.05, 0.2, 0.4, 0.7 and 1.0 had been prepared by the thermal decomposition of corresponding nitrates. Among them, the sample with x = 0.05 shows above-liquid-$N_2$ temperature superconductivity with $T_c$ of 88.7K. According to the X-ray diffraction analysis, its crystal symmetry was estimated as orthorhombic with the lattice parameters of a = 3.866${\AA}$, b = 3.893${\AA}$, c = 11.715${\AA}$. The chemical composition of the sample was determined by electron probe microanalysis and the chemical composition around its grain boundaries was carefully studied by the X-ray line scanning technique. From the observed binding energy of Ni-$2p_{3/2}$ orbital electron (B.E. = 853 eV) measured by X-ray photoelectron spectroscopy, the valency state of nickel stabilized in $YBa_2Cu_{2.95}Ni_{0.05}O_{7-{\delta}}$ oxide lattice could be determined to be Ni(II).

Mossbauer Effect on the Influences of Substituted $Al^{3+}$ of Goethit in Clay Cheju Island (제주도 찰흙에 함유된 Goethite에서 $Al^{3+}$ 치환 영향에 대한 Mossbauer 효과)

  • 강동우;김두철;고정대;홍성락;송관철
    • Journal of the Korean Magnetics Society
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    • v.7 no.4
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    • pp.196-204
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    • 1997
  • In order to study the effect of substituted $Al^{3+}$ of goethite, which was collected from Shinpyeongli in Cheju Island, we used X-ray diffractometer and Mossbauer spectrometer. In X-ray diffraction analysis, the X-ray diffraction peaks of goethite are not detected due to the high substituted Al contents of goethite. Isomer shifts indicated that the valence of Fe ions is almost oxidized trivalent of high spin state. It is believed that the contents of substituted diamagnetic $Al^{3+}$ for $Fe^{3+}$ is about 15.5 mol%. It seems that Neel temperature and saturated magnetic hyperfine field of the clay goethite are about 250 K and 498 kOe, respectively. For the temperature lower than Neel temperature, quadrupole splittings of the clay goethite are greatly influenced by $Al^{3+}$ substitution. It is believed that the high decrease of Neel temperature and magnetic hyperfine field of the clay goethite results from the magnetic dilution produced by substituting the diamagnetic $Al^{3+}$/TEX> for $Fe^{3+}$.

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Magnetic and Electrical Properties of High-Tc Superconductor $YBa_2Cu_3O_{6.87}$

  • Kim, Don;Kang, Chang-Kwon;Kim, Keu-Hong;Choi, Jae-Shi
    • Bulletin of the Korean Chemical Society
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    • v.9 no.5
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    • pp.280-282
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    • 1988
  • The structural, electrical and magnetic properties were investigated for the high-Tc superconductor $YBa_2Cu_3O_{7-x}$, where x was 0.13. The results of temperature dependence of the resistivity and the magnetization in $YBa_2Cu_3O_{6.87}$ whose structure and phase are confirmed by arialysis of X-ray powder diffraction pattern have been reported. A very sharp superconductivity transition appears at 92K in the specimen whose chemical composition is determined from redox titration, strongly suggesting that this specimen consists of a single-phase superconductor. From the results of X-ray diffraction analysis, magnetization curves, levitation and resistance measurements, it is suggested that the observed superconductivity is bulk property in nature and that the $YBa_2Cu_3O_{6.87}$ phase is responsible for the superconductivity of the present reproducible specimen.

USE OF SINGLE PRECURORS FOR THE PREP ARATION OF SILICON CARBIDE FILMS

  • Lee, Kyunf-Won;Yu, Kyu-Sang;Kim, Yun-Soo
    • Journal of the Korean institute of surface engineering
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    • v.29 no.5
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    • pp.467-473
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    • 1996
  • Heteroepitaxial growth of cubic silicon carbide films on Si(001) and Si(111) substrates at temperatures 900-$1000^{\circ}C$ has been achieved by high vacuum chemical vapor deposition using the single precursor 1, 3-disilabutane without carrying out the carbonization process of the substrate surfaces. The deposition temperature range is much lowered compared with conventiontional chemical vapor deposition where separate sources for silicon and carbon are employed. The deposition procedure is quite simple and safe. The qualities of the films were found to be very good judging from the results obtained by various characterization techniques including reflection high energy electron diffraction, X-ray diffraction, X-ray pole figure analysis, Rutherford backscattering spectrometry, Auger depth profiling, and transmission electron diffraction.

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