碳酸肼还原法制备亚微米球形银粉的研究  

Preparation of submicron spherical silver powder by hydrazine carbonate reduction method

作　　者：顾丽争 刘子英 孙立硕 卢苗 梁宏陆 李华锋 柳青 GU Lizheng;LIU Ziying;SUN Lishuo;LU Miao;LIANG Honglu;LI Huafeng;LIU Qing(Lucky Film Co.,Ltd.,Baoding,Hebei 071054,China)

机构地区：[1]乐凯胶片股份有限公司,河北保定071054

出　　处：《信息记录材料》2023年第9期12-15,19,共5页Information Recording Materials

摘　　要：硝酸银溶液中加入浓氨水配制成银氨溶液,加氢氧化钠调节溶液的pH为12~13,加入碳酸肼作还原剂制备超细银粉,研究了加料时间、碳酸肼与银氨的摩尔比以及保护剂聚乙烯吡咯烷酮(PVP)的分子量及添加量对超细银粉的影响。结果表明:加料时间采用2 s制备的银粉满足爆发成核、缓慢生长的模型,制备的银粉粒径均匀、形貌规则;碳酸肼与银氨的摩尔比可通过还原液的浓度调制,还原液的浓度越高,其氧化还原电位(ORP)值越低,制备的银粉的平均粒径越小,但粒径的跨度越大,形貌越趋于不规则的形状;保护剂PVP的分子量及其添加量对银粉粒径、形貌有较大的影响。当加料时间采用2 s、碳酸肼与银氨的摩尔比为0.25,保护剂PVP选用分子量5000的K12,添加量为2%时,制备的银粉的平均粒径为0.8μm、粒径的跨度为0.98,分布均匀,银粉均为球形,且形貌规则。The silver ammonia solution was prepared by adding concentrated ammonia water into the silver nitrate solution,adding sodium hydroxide to adjust the pH value of the solution to 12-13,adding hydrazine carbonate as reducing agent to prepare ultrafine silver powder.The effects of feeding time,molar ratio of hydrazine carbonate to silver ammonia,and molecular weight and adding amount of protective agent polyvinylpyrrolidone(PVP)on ultrafine silver powder were studied.The results show that the silver powder prepared with the feeding time of 2s meets the model of explosive nucleation and slow growth,and the silver powder prepared has uniform particle size and regular morphology;The molar ratio of hydrazine carbonate to silver ammonia can be modulated by the concentration of the reducing solution.The higher the concentration of the reducing solution,the lower the oxidation-reduction potential(ORP)value,the smaller the average particle size of the prepared silver powder,but the larger the span of the particle size,the more irregular the morphology tends to be;The molecular weight of the protective agent PVP and its addition have great influence on the particle size and morphology of silver powder.When the feeding time is 2s,the molar ratio of hydrazine carbonate to silver ammonia is 0.25,the protective agent PVP is K12 with molecular weight of 5000,and the addition amount is 2%,the average particle size of silver powder prepared is 0.8μm,the span of particle size is 0.98,the distribution is uniform,the silver powder is spherical,and the morphology is regular.

关 键 词：银氨溶液 碳酸肼 球形银粉 保护剂 ORP值 

分 类 号：TQ16[化学工程—高温制品工业]