Ni-diamond composite powders with nickel layer of round-top type on the surface of synthetic diamond (140/170 mesh) were prepared by the electroless plating method (EN) with semi-batch reactor. The effects of nickel concentration, feeding rates of reductant, temperature, reaction time and stirring speeds on the weight percentage and morphology of deposited Ni, mean particle size and specific surface area of the composite powders were investigated by Atomic Adsortion Spectrometer, SEM-EDX, PSA and BET. It was found that nucleated Ni-P islands, acted as catalytic sites for further deposition and grown into these relatively thick layers with nodule-type on the surface of diamond by a lateral growth mechanism. The weight percentage of Ni in the composite powder increased with reaction time, feeding rate of reductant and temperature, but decreased with stirring speed. The weight percentage of Ni in Ni-diamond composite powder was 55% at 150 min., 200 rpm and 7 .

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