• 제목/요약/키워드: high temperature X-ray diffraction

검색결과 840건 처리시간 0.031초

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

  • Chun, Seung-Yeop;Chun, Myoung-Pyo
    • 한국결정성장학회지
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    • 제27권5호
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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.

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

  • 이희수;박정현;오영제
    • 한국세라믹학회지
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    • 제15권1호
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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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데칸술폰이 삽입된 니켈 화합물의 층상 구조의 열적 성질 (Thermal behavior of the layered structure of decanesulfonate intercalated into the hydrated nickel compound)

  • 허영덕;전태현;박용준
    • 한국결정성장학회지
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    • 제9권6호
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    • pp.580-584
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    • 1999
  • 수화된 니켈에 데칸술폰이 층간 삽입된 화합물을 합성한 후 성질을 확인하였다. 화합물의 층상구조는 고온 X-선 회절 데이터로 확인하였다. 온도가 증가하면 층간 삽입된 니켈화합물의 구조가 변하는 것과 동시에 화합물의 층 거리가 24.7 $\AA$에서 30.5 $\AA$가지 증가하였다. X-선 회절 데이터와 데칸술폰의 크기로부터 니켈 층에 결합된 데칸술폰의 공간배열을 결정하였다. 이중 층 구조를 가진 데칸술폰의 분자 축은 니켈 층에 경사진 각도로 수직하게 배열되어있다.

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

  • 최근섭;김도향;홍경태
    • Applied Microscopy
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    • 제27권4호
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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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천연산 활석에 대한 고압 X-선 회절연구 (High Pressure X-ray Diffraction Studies on a Natural Talc)

  • 김영호;이지은
    • 한국광물학회지
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    • 제12권1호
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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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합성 괴타이트에 대한 압축실험 (Compression Study on a Synthetic Goethite)

  • 김영호;황길찬;김순오
    • 한국광물학회지
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    • 제22권4호
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    • pp.325-330
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    • 2009
  • 합성 FeOOH-괴타이트 분말시료에 대한 고압실험을 압축성을 검증하기 위해 상온에서 시행하였다. 방사광이용 실험장치에서 대칭다이아몬드 앤빌기기를 각분산회절방법으로 배열하여 실험을 하였다. $K_{T'}$ 값을 4.0으로 가정하였을 때, 체적탄성률은 222.8 GPa로 계산되었다. 이 값은 천연산 괴타이트로부터 얻은 기존의 값과 비교하여 볼 때 매우 높은 값으로, 시료의 생성조건에 따라 나타나는 물질의 압력에 대한 이상 거동에 대해 고찰하였다.

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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    • 제11권5호
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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).

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

  • 강동우;김두철;고정대;홍성락;송관철
    • 한국자기학회지
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    • 제7권4호
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    • pp.196-204
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    • 1997
  • 제주도 신평리 지역 논에서 채취한 찰흙에 함유된 goethite에서 $Al^{3+}$ 이 미치는 영향을 조사하기 위하여 X-선 회절 분석과 Mossbauer 분광 실험을 실시하였다. X-선 회절 분석에서 goethite 내에 치환된 Al 이온의 함량이 높아 goethite에 의한 회절 피크가 관측되지 않았다. 이성질체 이동값은 Fe 이온들이 대부분 high spin의 +3가 상태임을 나타내며, Fe$^{3+}$ 와 치환된 반자성 $Al^{3+}$ 의 치환량은 약 15.5 mol%로 추정된다. 찰흙에 함유된 goethite의 Neel 온도와 포화 초미세자기장값은 약 250 K와 약 498 kOe로 각각 나타났다. goethite의 사중극자 분열값은 Neel 온도 이하에서 $Al^{3+}$ 의 치환에 큰 영향을 받는 것으로 나타났다. 찰흙 시료에 함유된 goethite의 neel 온도와 초미세자기장값의 큰 감소는 격자내의 Fe$^{3+}$ 와 반자성 $Al^{3+}$ 의 치환에 의해 생긴 magnetic dilution에 기인한 것으로 보여진다.

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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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    • 제9권5호
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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
    • 한국표면공학회지
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    • 제29권5호
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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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