成果報告書詳細
管理番号20090000000279
タイトル*平成20年度中間年報 エネルギー使用合理化技術戦略的開発/エネルギー有効利用基盤技術先導研究開発/機械的非加熱合成法による機能性複合酸化物の省エネ製造プロセスの開発
公開日2009/9/17
報告書年度2008 - 2008
委託先名株式会社ホソカワ粉体技術研究所
プロジェクト番号P03033
部署名省エネルギー技術開発部 研究開発グループ
和文要約以下本編抜粋:1.研究開発の内容及び成果等 1-1.研究項目(1)「複合酸化物の非加熱合成用機械式製造装置の開発」複合酸化物ナノ粒子を、高温焼成することなく、機械的な処理によって非加熱で合成するプロセスの開発を行うために、来年度製作する非加熱合成用機械式製造装置の一次試作機の仕様を決定するために、既存実験装置を改良し、これを用いた機械的非加熱合成の基礎実験を行い、合成に必要な雰囲気・操作条件のデータの収集を行った。
英文要約Title: Development of energy-saving process to produce functional composite oxides by mechanical non-heating synthesis method (FY2008-FY2009 ) FY2008 Annual Report
For the purpose to determine the specifications of the prototype machine suitable for the production of composite oxide nanoparticles by mechanical processing without calcination at the elevated temperature, a series of preliminary trials have been conducted using modified conventional equipments under various mechanical and operational conditions. The trials were carried out to make lanthanum manganate as a sample from La2O3, and Mn3O4 powder materials with different moisture content and humidity under the atmospheric condition. As a result, it was found by the X-ray diffraction analysis that lanthanum manganate was successfully prepared with the mechanical energy less than the target value and that the intensity of the diffraction peaks of the composite oxide get higher with the increasing mechanical energy. On the basis of these results, main specifications of the prototype machine were decided to design and manufacture for the experiments in the next fiscal year. Concerning the processing conditions for the mechanical synthesis, not only mechanical ones of the milling apparatus but also other conditions such as sizes and surface status of the starting particles and atmosphere can be important factors. In the case of preparation of strontium doped lanthanum manganate (LSM), one of the starting powders La2O3 transforms to La(OH)3 when it is exposed to water. This phenomena leads to reduction of particle strength and other properties, and so accelerations in reduction of particle size and reaction of synthesis are expected. From this viewpoint, influences of water content and some other conditions on the mechanical synthesis were investigated using X-ray diffraction and other methods. As a result, the single phase LSM powders were obtained after 120 min milling when water contents in the starting powders were 0.2 and 0.8 mass%. In the case of 2.0 mass% water content, the single phase LSM was not obtained even after 120 min milling, although the LSM phase appeared and began to increase till 20 min milling. In this case, it was supposed that La2O3 and La(OH)3 formed strong agglomeration and it prevented proceeding of reaction with other component particles. On the other hand, crystal structures of the starting materials almost unchanged to create LSM phase even by 180 min milling on the dry atmospheric condition (0.1%RD). Thus it was confirmed that the single phase of LSM was able to be synthesized by the mechanical method and it was found that there was a proper range of water content for the reaction. Furthermore, preliminary experiments have been conducted to establish the procedures and find out appropriate conditions for the sintering of the composite oxides prepared by the mechanical non-heating synthesis method and for the evaluation of the properties of the sintered materials. In this fiscal year, a kind of lanthanum manganate LSM was prepared by the conventional solid reaction method under different conditions of calcination temperature and mixing ratio and then sintered after press forming to make test pieces. Various properties such as shrinkage, relative density, porosity and electroconductivity have been measured to investigate the relationship between these properties and the sintering conditions. As a result, it was found that the electroconductivity of the test pieces is dominantly determined by the relative density of the sintered sample piece and the sintering performance was greatly influenced by the mixing ratio of the raw materials.
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