Ag 水溶液으로부터 還元反應에 의한 Ag 微粒子의 製造 硏究
Preparation of Ag Fine Particles from Aqueous Silver Solution by Reduction Reaction
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초록
국내 폐은 원료로부터 고부가가치 Ag powder를 제조하기 위한 연구의 일환으로써 ascorbic acid를 환원제로 사용한 Ag 미립자 제조실험을 수행하였다. Ag 수용액은 질산은을 10 ~ 120 mmole/l의 범위로 용해시켜 사용하였으며, Ag 미립자의 응집방지를 위한 분산제로는 Tamol NN8906 및 PVP를 각각 사용하였다. 환원반응을 통하여 제조한 Ag 미립자는 X-선 회절분석, 입도분석, SEM 및 TEM 분석을 실시하여 morphology 와 평균입도를 측정하였다. ascorbic acid에 의한 수용액중 Ag 이온의 환원반응은 10분 이내에 거의 평형상태에 도달하였으며, 완전한 Ag 이온의 환원을 위해서는 ascorbic acid 첨가량이 이론치의 1.6배가 소요되었다. 생성된 Ag 미립자의 입도분포는 bimodal 혹은 trimodal의 분포곡선을 보였으며, Ag 미립자의 평균입도는 분산제 종류 및 첨가량과 수용액중 초기 Ag 농도에 따라 달라지는 것으로 나타났다.
Abstract
A study on the preparation of Ag fine particles was performed through a reduction reaction using ascorbic acid as a reductant, which is one of the indispensable processes for the recycling of silver-bearing wastes. Silver nitrate solution in the range of 10 ~ 120mmole/l was used and Tamol NN8906 or PVP was also used as a dispersant in the preparation of Ag fine particles. Ag particles obtained from the reduction reaction in the silver solution were characterized using X-ray diffraction, particle size analyze, SEM, and TEM to determine the particle size and morphology of them. As a result, the reduction reaction of silver ions with ascorbic acid reached equilibrium within 10min. It was found that about 60% excess of ascorbic acid was required in order to reduce completely silver ions in the solution. The particle size distribution of Ag particles prepared through the reduction reaction showed typically bimodal or trimodal distribution. Especially, initial Ag concentration in the solution, the type and amount of dispersant added during the reduction reaction played an important role in determining the mean particle size of Ag particles.
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