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Catalysis of Organic..

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160 Raney® Metastable Precursorsslowly solidified specimen. In this case, the direct effect <strong>of</strong> Pd dissolved in the Cuskeleton on the conversion ratio is hard to explain clearly, because high specificsurface area contributes to the high conversion ratio. We have developed a directTEM observation method for the microstructure <strong>of</strong> leached specimens by slicing thespecimen using an ultra-microtome. Figure 8 shows an example <strong>of</strong> TEM images forCu <strong>of</strong> Pd free and 1.5mass % Pd. They have a skeletal structure composed <strong>of</strong> finegranular Cu particles. The size <strong>of</strong> Cu particles was about 30-40nm for a Pd freematerial and 10nm for a 1.5 mass %Pd added material. It suggests that the dissolvedPd in the precursor suppressed the growth <strong>of</strong> Cu particles as obstacles for therearrangement <strong>of</strong> Cu. The size obtained by direct observation by TEM was almostthe same as that evaluated by the X-ray line- broadening method.(a) Pd free (b) Pd 1.5 mass %Figure 8. TEM image <strong>of</strong> as-leached state (Raney Cu).Mechanical alloying (MA) is another process solution in addition to rapidsolidification for making a supersaturated solid. In this process, the pure powders<strong>of</strong> different elements are mixed and encapsulated in a metallic container with somesteel balls. Then, the container is rotated or vibrated for an extended time. Thepowders are cold worked by collisions <strong>of</strong> steel balls. This cold working makesmechanically alloyed powder.This process was applied to prepare Al 3 Ni precursor with 2at% Ti. The catalyticbehavior was examined for the hydrogenation <strong>of</strong> acetone in an autoclave. The rate <strong>of</strong>change <strong>of</strong> hydrogen pressure with time was evaluated, i.e. the rate <strong>of</strong> decrease from0.3MPa (initial pressure). This value is an indicator <strong>of</strong> the activity <strong>of</strong> the catalyst. It

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