成果報告書詳細
管理番号20110000001309
タイトル*平成22年度中間年報 グリーン・サステイナブルケミカルプロセス基盤技術開発 規則性ナノ多孔体精密分離膜部材基盤技術の開発(6)
公開日2011/8/30
報告書年度2010 - 2010
委託先名財団法人ファインセラミックスセンター
プロジェクト番号P09010
部署名電子・材料・ナノテクノロジー部
和文要約和文要約等以下本編抜粋:1. 研究開発の内容及び成果等 (1)ゼオライト分離膜の微細構造解析手法の開発 (1~1)TEM試料作製法の検討 本プロジェクトでは、ガス分離特性を評価するためのゼオライト分離膜は、直径約1cmの円筒状アルミナ多孔体を基材としてゼオライト膜を作製している。この開発材を対象として電子顕微鏡法による微細構造解析を行う場合、円筒形状試料の外表面に薄くコーティングされたゼオライト層を対象とした電子顕微鏡用薄片試料を作製しなければならない。
英文要約In this project, we are synthesizing zeolite membranes on cylindrical porous alumina substrate samples 1 cm in diameter to evaluate the membrane’s gas separation properties. To carry out microstructural characterization of these new materials using electron microscopy, flakes of material must be prepared containing the thin zeolite layer that has been coated onto the sample’s outer surface. Such flakes were made into specimens suitable for transmission electron microscopy (TEM) using FIB and ion-beam milling techniques. The former technique, although having a narrow field of view, has the advantage that samples can be prepared which enable analysis to a depth of more than 10 μm from the membrane surface inwards towards the substrate. The aim of our research was thus to examine the methods of using FIB to prepare samples suitable for high-resolution TEM observation. Ion beam milling is also known to be a useful technique for preparing samples suitable for high-resolution TEM. However, it is very difficult to use this method on cylindrical samples. In this research we also examined methods employing ion beam milling to prepare TEM specimens from cylindrical samples, with dummy samples for this purpose provided by Noritake Co., Ltd. As a result of these investigations, we were able to determine the conditions necessary for the preparation of high-resolution TEM samples for both techniques.
The TEM methods developed in this project were used in the microstructural characterization of specimens provided by each group, and the results fed back into process R&D. The following five samples were examined: 1) Al-ZSM5 from Yamaguchi University; 2) an FAU membrane from Waseda University; 3) an MCM-22 membrane from Osaka University; 4) Seed crystals from Hitachi Zosen; and 5) a CHA-type membrane from Mitsubish Chemicals.
The anisotropy in grain growth speed of the Al-ZSM5 sample from Yamaguchi University was confirmed to be unique, with no other examples of such a phenomenon having been reported. The influence of this anisotropy on grain boundary structure, which strongly impacts the separation behavior of the membrane, is now being examined.
Also, based on TEM-EDS analysis of the sample provided by Waseda University, it was found that SiO2 (the chief component of the zeolite) penetrated to a depth of 9~10μm into the pores of the substrate. With the successful use of EDS to analyze composition to nano-order, another mid-term aim of the project was achieved.
Lastly, computational chemistry techniques are being applied to evaluate the permeability and other properties of zeolite materials examined in this project at the atomic scale. So far, adsorption isotherms of water in MOR zeolite, as well as the diffusion coefficients of water molecules, have been calculated at different temperatures.
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