沉淀转化法制备超细银粉试验研究
发布时间：2019-03-20 21:48
【摘要】：随着光伏产业在全球范围内的兴起,晶体硅太阳能电池正银浆料对高振实密度、平均粒径在1μm左右、单分散球形银粉的需求与日俱增。目前,银粉制备工艺以液相化学还原法为主。在高过饱和度下形成的银粉,团聚严重、单分散性差、结晶度低、振实密度小,难以满足制备晶体硅太阳能电池正银浆料的要求。 本文提出以沉淀转化法为银粉合成路线,其特征在于：粉末颗粒形成的“源物质”来源于前驱体沉淀的溶解,以实现体系低的过饱和度,从而制备出单分散性好、结晶度高的超细球形银粉。采用SEM、XRD、激光粒度仪及Zeta电位仪等方法,对粉末样品进行表征。 采用氧化银为前躯体制备银粉,研究了还原剂、分散剂、溶剂、pH调节剂以及加料方式对银粉形貌与粒度的影响,确定后续试验反应体系为：以葡萄糖为还原剂,PVP为分散剂,氨水为pH调节剂,并流加料。考察了反应条件对银粉形貌与粒度的影响,结果表明：在偏中性pH值、较低温度与葡萄糖浓度下,可以制备出分散性好、粒度可控的超细银粉。在添加1%PVP(与前躯体质量百分比,下同)为分散剂,温度30℃,pH=8.0,葡萄糖浓度0.35 mol·L-1的反应条件下制备出结晶度高、分散性好且粒径在1μm左右的类球形银粉。 以碳酸银为前躯体,葡萄糖为还原剂,PVP为分散剂,碳酸钠为pH调节剂,采用沉淀转化法制备了亚微米级银粉。考察了分散剂PVP添加量、辅助添加六偏磷酸钠添加量以及添加柠檬酸根对银粉形貌与粒度的影响。结果表明：PVP用量低于5%则对银粉分散性作用不明显；添加两种分散剂(1.2%PVP和0.4%六偏磷酸钠)可以制得分散性较好的亚微米级银粉；同时添加1.2%PVP和1%柠檬酸钠所制备银粉粒度减小且分散性提高。
[Abstract]:With the rise of photovoltaic industry in the world, the demand for monodisperse spherical silver powder is increasing with the development of positive silver paste for crystalline silicon solar cells with high density and average particle size of about 1 渭 m. At present, the preparation of silver powder is dominated by liquid-phase chemical reduction. The silver powder formed at high supersaturation has serious agglomeration, poor monodispersity, low crystallinity and low density, so it is difficult to meet the requirements of preparing silver paste for crystalline silicon solar cells. In this paper, the precipitation transformation method is proposed as the synthetic route of silver powder. The characteristic is that the "source material" formed by powder particles comes from the dissolution of precursor precipitation, in order to achieve low supersaturation of the system, so that the monodispersity is good. Ultra-fine spherical silver powder with high crystallinity. The powder samples were characterized by SEM,XRD, laser particle size analyzer and Zeta potentiometer. Silver powder was prepared by using silver oxide as precursor. The effects of reducing agent, dispersant, solvent, pH regulator and feeding method on the morphology and particle size of silver powder were studied. The following reaction system was determined as follows: glucose as reducing agent and PVP as dispersant. Ammonia is the pH regulator, and the feed is added. The effects of reaction conditions on the morphology and particle size of silver powder were investigated. The results showed that ultrafine silver powder with good dispersion and controllable particle size could be prepared at neutral pH, lower temperature and glucose concentration. High crystallinity was obtained by adding 1%PVP as dispersant, temperature 30 鈩，
本文编号：2444661
[Abstract]:With the rise of photovoltaic industry in the world, the demand for monodisperse spherical silver powder is increasing with the development of positive silver paste for crystalline silicon solar cells with high density and average particle size of about 1 渭 m. At present, the preparation of silver powder is dominated by liquid-phase chemical reduction. The silver powder formed at high supersaturation has serious agglomeration, poor monodispersity, low crystallinity and low density, so it is difficult to meet the requirements of preparing silver paste for crystalline silicon solar cells. In this paper, the precipitation transformation method is proposed as the synthetic route of silver powder. The characteristic is that the "source material" formed by powder particles comes from the dissolution of precursor precipitation, in order to achieve low supersaturation of the system, so that the monodispersity is good. Ultra-fine spherical silver powder with high crystallinity. The powder samples were characterized by SEM,XRD, laser particle size analyzer and Zeta potentiometer. Silver powder was prepared by using silver oxide as precursor. The effects of reducing agent, dispersant, solvent, pH regulator and feeding method on the morphology and particle size of silver powder were studied. The following reaction system was determined as follows: glucose as reducing agent and PVP as dispersant. Ammonia is the pH regulator, and the feed is added. The effects of reaction conditions on the morphology and particle size of silver powder were investigated. The results showed that ultrafine silver powder with good dispersion and controllable particle size could be prepared at neutral pH, lower temperature and glucose concentration. High crystallinity was obtained by adding 1%PVP as dispersant, temperature 30 鈩，
本文编号：2444661
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