沉淀轉(zhuǎn)化法制備超細(xì)銀粉試驗(yàn)研究
發(fā)布時(shí)間:2019-03-20 21:48
【摘要】:隨著光伏產(chǎn)業(yè)在全球范圍內(nèi)的興起,晶體硅太陽能電池正銀漿料對(duì)高振實(shí)密度、平均粒徑在1μm左右、單分散球形銀粉的需求與日俱增。目前,銀粉制備工藝以液相化學(xué)還原法為主。在高過飽和度下形成的銀粉,團(tuán)聚嚴(yán)重、單分散性差、結(jié)晶度低、振實(shí)密度小,難以滿足制備晶體硅太陽能電池正銀漿料的要求。 本文提出以沉淀轉(zhuǎn)化法為銀粉合成路線,其特征在于:粉末顆粒形成的“源物質(zhì)”來源于前驅(qū)體沉淀的溶解,以實(shí)現(xiàn)體系低的過飽和度,從而制備出單分散性好、結(jié)晶度高的超細(xì)球形銀粉。采用SEM、XRD、激光粒度儀及Zeta電位儀等方法,對(duì)粉末樣品進(jìn)行表征。 采用氧化銀為前軀體制備銀粉,研究了還原劑、分散劑、溶劑、pH調(diào)節(jié)劑以及加料方式對(duì)銀粉形貌與粒度的影響,確定后續(xù)試驗(yàn)反應(yīng)體系為:以葡萄糖為還原劑,PVP為分散劑,氨水為pH調(diào)節(jié)劑,并流加料。考察了反應(yīng)條件對(duì)銀粉形貌與粒度的影響,結(jié)果表明:在偏中性pH值、較低溫度與葡萄糖濃度下,可以制備出分散性好、粒度可控的超細(xì)銀粉。在添加1%PVP(與前軀體質(zhì)量百分比,下同)為分散劑,溫度30℃,pH=8.0,葡萄糖濃度0.35 mol·L-1的反應(yīng)條件下制備出結(jié)晶度高、分散性好且粒徑在1μm左右的類球形銀粉。 以碳酸銀為前軀體,葡萄糖為還原劑,PVP為分散劑,碳酸鈉為pH調(diào)節(jié)劑,采用沉淀轉(zhuǎn)化法制備了亞微米級(jí)銀粉。考察了分散劑PVP添加量、輔助添加六偏磷酸鈉添加量以及添加檸檬酸根對(duì)銀粉形貌與粒度的影響。結(jié)果表明:PVP用量低于5%則對(duì)銀粉分散性作用不明顯;添加兩種分散劑(1.2%PVP和0.4%六偏磷酸鈉)可以制得分散性較好的亞微米級(jí)銀粉;同時(shí)添加1.2%PVP和1%檸檬酸鈉所制備銀粉粒度減小且分散性提高。
[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,
本文編號(hào):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,
本文編號(hào):2444661
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