节点文献
微米级可控制粒径银粉中试制备研究
The Middle Test of Micron Silver Power Which Can Be Controlled And The Study of Manufacturing
【作者】 张燕;
【导师】 董岁明;
【作者基本信息】 长安大学 , 环境工程(专业学位), 2015, 硕士
【摘要】 银粉是电子工业和电气的重要材料之一,也是电子工业中应用最广泛的一种贵金属材料,是介质、电阻、厚膜、陶瓷等电子浆料的最基本功能材料。最近几年,纳米材料和纳米微粒已经成为材料科学领域的重点研究内容。其制备方法繁多,但主要采用化学还原法制备。此论文参照文献资料,通过还原剂甘油、水合肼,还原制备微米级可控小试及中试研究。研究中通过小试阶段,借助激光粒度分析,系统考察了工艺参数对银粉形貌与粒度的影响;通过中试阶段,设计出一套适合大规模生产、操作简捷、尾气吸收良好的生产设备。综合比较小试间段与中试间段实验参数对银粉粒径的影响,优化生产工艺,能够稳定生产出大批量的、粒径分布均匀的、可控制的微米级银粉。综合本次实验的所得数据,我们优化出一种最佳条件下大规模生产微米银粉的参数:取1000g标银加入1.5L浓硝酸制作硝酸银溶液。取150g聚乙烯醇、250m L三乙醇胺、1500m L丙三醇、1000g Na OH,Na OH溶液的浓度为0.11g/L。调节蠕动泵转速为20转/分,电子搅拌器速率为180转/分。按照实验步骤进行反应,可得到粒径累积分布D10>0.4μm、D90<1.8μm,也就是绝大部分粒径分布在0.4~1.8μm之间的微米级银粉。
【Abstract】 Silver powder is an important material, and it is the most widely used in the electronics industry and it is the basic function of electronic paste material,such as: Thick film, resistance, ceramics, medium. In recent years, nano materials and nano particles has become a focus in the fie ld of materials science research content. Its preparation method is various, but mainly by chemical reduction method.With hydrazine hydrate and glycerol as reductant,this paper prepared by chemical reduction method of high dispersion, particle size contro llable silver powder. Through the small stage, study systemicly investigated the influence of process parameters on the morphology and particle size silver by means of laser particle size analysis; Through the middle stage,it designs a set of suitable for mass production, the operation simple, the tail gas absorption good production equipment.Integrated data from this experiment, we optimized the best mass production under the condition of a micron silver powder parameters : Take 1000 g the silver in 1.5 L nitric acid production of silver nitrate solution. Take 150 g polyvinyl alcohol, 250 ml triethanolamine, 250 ml of glycerol, 1000 gnaoh and the concentration of Na OH solution is 0.11 g/L. Adjust the peristaltic pump speed to 20 RPM and electronic stirrer speed is 180 RPM. Carried out in accordance with the experimental steps reaction,the available size cumulative distribution is D10 > 0.4 microns, the D90 < 1.8 mu m, that is, the vast majority of the particle size distribution between 0.4 ~ 1.8 microns mic ron grade silver powder.
【Key words】 silver; chemical reduction method; micron; glycerol; controllabled;