| Project/Area Number |
06554028
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| Research Category |
Grant-in-Aid for Developmental Scientific Research (B)
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| Allocation Type | Single-year Grants |
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| Research Field |
Inorganic chemistry
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| Research Institution | KYOTO UNIVERSITY |
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Principal Investigator |
KOSUGE Koji Kyoto Univ., Graduate School of Sci., Prof., 大学院理学研究科, 教授 (00025371)
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| Co-Investigator(Kenkyū-buntansha) |
KATAYAMA Tyuji MAC Science, Senior Researcher, 技術研究所, 主任研究員
YOSHIMURA Kazuyoshi Kyoto Univ., Graduate School of Sci., Asso.Prof., 大学院理学研究科, 助教授 (70191640)
NAKAYAMA Noriaki Yamaguchi Univ., Dep.Engineering, Asso.Prof., 工学部, 助教授 (00164369)
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| Project Period (FY) |
1994 – 1995
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| Project Status |
Completed (Fiscal Year 1995)
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| Budget Amount *help |
¥13,000,000 (Direct Cost: ¥13,000,000)
Fiscal Year 1995: ¥900,000 (Direct Cost: ¥900,000)
Fiscal Year 1994: ¥12,100,000 (Direct Cost: ¥12,100,000)
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| Keywords | Poder X-ray / TG-DTA / SSD / Inorganic reaction |
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| Research Abstract |
The purpose of this project is to develop an apparatus which can be used for in situ and simultaneous measurements of X-ray diffraction pattern (XRD), Differential thermal analysis (DTA) and Thermo gravimetry (TG).. The most difficult point of this development is in how to construct the X-ray beam path (incident and diffracted beam) through TG-DTA apparatus with an infrared furnace. It is evident that it is impossible to have the large "windows" for the diffracted beams, because the sample on a Pt plate is surrounded by the block of infrared furnace. We adopted, accordingly, the energy dispersion system by use of white X-ray.
The beam of white X-ray (incident beam) and diffracted one has been guided by transparent quartz arms attached to the guard tube, which is also made from transparent quartz, of TG-DTA apparatus. The thin film of poly imide (capton), which is transparent to X-ray, was used as "windows" for X-ray. The incident white X-ray beam comes at an angle of about 10 degree to
… More
the surface of powder samples and the diffracted beam goes out at an angle of about 10 degree to the surface of powder samples. The energy of diffracted beam was analyzed by SSD (Ge).
To test the performance of this trial apparatus, the reaction process of (La_2O_3+CuO*La_2CuO_4) and (1/2Y_2O_3+2BaCO_3+3CuO*YBa_2Cu_3O_7) systems has been investigated in detail. Moreover, the mechanism of abnormal desorption of oxygen observed in the Li (Mn-Ni) _2O_4 system has been studied up to 1000ﾟC.As the result, the characteristics of our trial apparatus are as follows ;
(1) In the case of slow reaction, this apparatus can trace the reaction mechanism.
(2) The identification of phases is easily done for the case of having simple crystal structure. The following points have to be improved ;
(1) Because the intensity of incident white X-ray is very weak (2kW), it takes about twenty minutes to get the full diffraction patterns. This fault is easily improved by using rotor target X-ray system (18kW).
(2) Due to the limit (160eV) of energy analyzer (SSD), the resolution power of diffracted patterns is very low in comparison with the usual Debye-Sherrer method. This default is also improved by adopting the wave length dispersion method.
We are now planning to improve these default. Less
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