太阳能电池正面银浆的制备及其性能研究
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摘要
太阳能是人类最重要的可再生能源之一,它是一种无污染、可再生、储量巨大、取之不尽、用之不竭的清洁能源,充满了诱人的前景。因此,太阳能的研究和应用已成为世界新能源研究的热点。银浆是制造太阳能电池电极的关键材料,电极银浆组成相的成分配方、性质和制备工艺直接影响着太阳能电池的物理和光电性能。本文瞄准当今世界科学与技术前沿,重点研究了太阳能电池正面银浆的主要组成相银粉和有机载体的性质和成分配方。利用化学液相还原法成功制备出适合太阳能电池正面银浆应用的高分散的微米/亚微米球形银粉,并成功优化出适合太阳能电池正面银浆应用的有机载体。同时,发现了银粉的粉末特性参数与太阳能电池性能的规律性,也发现了有机载体配方与太阳能电池丝网印刷性和电性能的相关性,以及银浆制备工艺与太阳能电池性能的相关性。主要研究结果如下：
1、研究了太阳能电池正面银浆用的高分散球形或类球形超细银粉,首次揭示了聚乙烯醇是利用化学吸附和物理吸附分散银粉的机理,从而突破了化学还原法制备银粉的技术关键。作者以硝酸银为原材料,运用化学液相还原法制备银粉。通过单因素实验和正交实验两种设计方法,优化出两种适合制备太阳能电池正面银浆的工艺。
单因素实验设计方法,探索了十一个影响银粉粒度、形貌和分散性的因素,发现规律性,成功制备出目标银粉。优化的工艺条件为：以抗坏血酸为还原剂,聚乙烯醇为分散剂,pH=7,分散剂用量为8wt%(相对硝酸银质量),12.500mL·s-1的滴液速度,200PRM的搅拌速度,还原剂溶液的初始浓度为1.177mol·L-1,硝酸银溶液初始浓度为0.294mol·L-1,分散剂加入到硝酸银溶液中,硝酸银溶液滴入到还原剂溶液中,反应温度50℃,用甘油单硬脂酸酯的乙醇溶液进行后处理改性。在该条件下,制备的银粉具有良好的分散性,形貌为球形,一次粒子的平均粒度为0.81μm,粒径分布为0.37～1.04μm,振实密度为4.9g·cm-3。在此基础上,运用紫外-可见光谱研究了以聚乙烯醇作分散剂制备银粉的分散机理,通过深入系统地分析,揭示了聚乙烯醇是利用化学吸附和物理吸附分散银粉的机理。正交实验设计方法,考察了六个因素和五个水平。优化的工艺条件为：硝酸银浓度为0.3mol·L-1,抗坏血酸浓度为1.4mol·L-1,明胶为分散剂,分散剂用量为8wt%(相对硝酸银质量),pH值为4,反应温度为50℃。在此条件下制备的银粉,形状为近球形,颗粒均匀,分散性良好,其一次粒子的平均粒度为0.89μm,分布在0.36-1.67μm之间,振实密度为5.4g·cm-3。
通过以上两种工艺制备的银粉都适合制备太阳能电池正面银浆,各有优点,前者工艺制备的银粉分散性好,而后者工艺制备的银粉振实密度高。
2、发现了银粉的分散性、振实密度及银浆的银含量对太阳能电池正面银浆的影响规律。高的分散性和振实密度有利于制备高品质的银浆,由其制备的太阳能电池正面银浆具有良好的丝网印刷性,其烧结厚膜的电极线条精密、平整、致密、孔洞率小,具有优异的导电性,从而提高了太阳能电池的光电转化效率,其单晶硅太阳能电池光电转化效率达17.803%。该新的发现还未见有文献报道。
3、优化了一个满足正银浆料所需的良好流平性、触变性和印刷性的有机载体。山该有机载体制备的太阳能电池正银浆料,兼备了良好的流平性、触变性和丝网印刷性能,该正银浆料印刷的电池电极和栅线具有大的湿重、膜厚和高宽比,每片电池湿重达0.18g,膜厚达33μm,高宽比达0.306,同时,电极和栅线与晶硅界而具有高的附着力(0.4N.mm-2)和良好的可焊性,该条件下制备的太阳能电池具有优异的光电转化效率,其单晶硅电池光电转化效率达17.963%。该配方还未见有文献报道。
4、发展了低成本、短流程正面银浆制备技术,该技术由湿态银粉直接配制浆料,最大限度地减少了银粉的团聚带来的负面影响,使电池性能进一步提高(可达18.020%)。发现制备该正银浆料的新工艺可克服银粉干燥过程加剧团聚的不利影响,摒弃了传统电子浆料生产时易使固、液混合和研磨不均匀的缺点,使得制备的正银浆料分散性更好,细度更细,提高了高精度、高分辨率、高速丝网印刷性能和增强了浆料的过网能力。
5、发现了正银浆料的丝网印刷、烘干和烧结工艺对太阳能电池电学性能和光电转换效率的重要影响规律。将各种工艺调到最佳匹配值才能最大限度的提高电池性能。
Solar energy is the most important one of the renewable energy, and it is a pollution-free, abundant, renewable energy of the future. Therefore, the study and application of solar energy is a main direction in the future of mankind. Silver paste is the key material of mading solar cells, and its ingredient, preparation process has a direct impact on physical and electrical performance of solar cell. Aimming at the frontier of science and technology of the world today, two key ingredients of solar cell silver paste, namely silver powder and organic vehicle, were investagated. Using chemical liquid-phase reduction method, micron/submicron spherical silver powder for solar cell front silver paste application was prepared. And organic vehicle for solar cell front silver paste application was optimized. At the same time, the law of silver powder characteristics parameter and solar cell performance, the relevance between organic vechicle and scree-pinting, electrical performance and the relevance between preparation processes of silver paste with solar cell performance are discovered. The main results are as follows:
1. Highly dispersive micron/submicron spherical silver powder for solar cell front silver paste is investigated. And dispersion mechanism of polyvinyl alcohol for preparing silver powder is firstly revealed, namely it is the chemical and physical adsorption, which is a key technology breakthrough of preparing silver powder by the chemical reduction method. We use silver nitrate as raw materials to prepare silver powder, using chemical liquid-phase reduction process. Through single factor experiment and orthogonal designs, we have optimized two processes preparing silver powder for the solar cell front silver paste.
For single factor experiment design, eleven factors of influencing granularity, morphology and dispersivity of silver powder are experimented. The desired silver powder is prepared successfully and its law is discovered. The process conditions:ascorbic acid as reduction agent, PVA as disperser, pH=7, disperser usage of8wt%(relativer to the mass of silver nitrate), dipping speed of12.500mL·s-1, stirring speed of200PRM, the concentration of reducion solution of1.177mol·L-1, the concentration of silver nitrate solution of0.294mol·L-1, adding disperser to silver nitrate solution, adding silver nitrate solution to reduction solution, temperature of50℃, a ethanol solution of glyceryl monostearate as posttreatment agent, as-prepared silver powder has good dispersivity, spherical shape, the average particle size of0.81μm, the distribution of0.37～1.04μm, the tap density of4.9g·cm-3. Using ultraviolet and visible spectrum, the disperser mechanism of the preparation of silver powder using polyvinyl alcohol as disperser is suggested firstly, which mechanism is the chemical and physical absorption mechanisms.
Using the orthogonal experimental design, six factors and five levels are experimented. The optimal process conditions:silver nitrate solution concentration of0.3mol·L-1, ascorbic acid solution concentration of1.4mol·L-1, gelatin as disperser, the disperser usage of8wt%(relative to the mass of silver nitrate), pH=4, the temperature of50℃. As-prepared silver powder has the nearly spherical shape, good dispersivity,0.36～1.67μm size distribution, average particle size of0.89μm and the tap density of5.4g·cm-3.
Silver powders prepared through the above two kinds of processes are all suitable for preparing front silver paste of solar cell. Each of them has its advantage. Silver powder prepared by the former process has good dispersion while the one prepared by the latter process has high tap density.
2. For the first time, a significant impact of dispersivity, tap density of silver powder and silver content in silver paste on the thick film and solar cell has discovered, and a higher dispersivity and tap density of silver powder is conducive to the preparation of the high quality silver paste, and its thick film has good screen-printing, which is helpful to increase conversion efficiency of solar cell (up to17.803%for monocrystalline silicon solar cell). This new discovery has been not reported.
3. An optimal organic vehicle formula is found. The solar cell front silver paste prepared using it has desired levelling, thixotropy and screen printing property. And the thick film has bigger wet weight (up to0.18g), thicker thickness (up to33μm) and bigger aspect ratio (up to0.306), and the thick film is even and compact. The grid has high adhesion (up to0.4N/mm2) and good solderability. The cell has higher photo-electric conversion efficiency (up to17.963%). This formula has been not reported.
4. This paper for the first time reported that wet silver powder is directly applied to prepare silver paste, which the negative impact of silver powder agglomeration is abated and improve cell efficiency (up to18.020%) by the greatest extent. This process has yet been not seen in reports.
5. By improving the preparation process of silver paste, the use of advanced mechanical method in mixxing of solid/liquid and solid/solid and gridding is more even and achieving better performance than the manual methods. At the same time, a significant impact of screen printing, coasting, sintering on the performance is discovered. Only matching the various techniques can high performance be required.
1、研究了太阳能电池正面银浆用的高分散球形或类球形超细银粉,首次揭示了聚乙烯醇是利用化学吸附和物理吸附分散银粉的机理,从而突破了化学还原法制备银粉的技术关键。作者以硝酸银为原材料,运用化学液相还原法制备银粉。通过单因素实验和正交实验两种设计方法,优化出两种适合制备太阳能电池正面银浆的工艺。
单因素实验设计方法,探索了十一个影响银粉粒度、形貌和分散性的因素,发现规律性,成功制备出目标银粉。优化的工艺条件为：以抗坏血酸为还原剂,聚乙烯醇为分散剂,pH=7,分散剂用量为8wt%(相对硝酸银质量),12.500mL·s-1的滴液速度,200PRM的搅拌速度,还原剂溶液的初始浓度为1.177mol·L-1,硝酸银溶液初始浓度为0.294mol·L-1,分散剂加入到硝酸银溶液中,硝酸银溶液滴入到还原剂溶液中,反应温度50℃,用甘油单硬脂酸酯的乙醇溶液进行后处理改性。在该条件下,制备的银粉具有良好的分散性,形貌为球形,一次粒子的平均粒度为0.81μm,粒径分布为0.37～1.04μm,振实密度为4.9g·cm-3。在此基础上,运用紫外-可见光谱研究了以聚乙烯醇作分散剂制备银粉的分散机理,通过深入系统地分析,揭示了聚乙烯醇是利用化学吸附和物理吸附分散银粉的机理。正交实验设计方法,考察了六个因素和五个水平。优化的工艺条件为：硝酸银浓度为0.3mol·L-1,抗坏血酸浓度为1.4mol·L-1,明胶为分散剂,分散剂用量为8wt%(相对硝酸银质量),pH值为4,反应温度为50℃。在此条件下制备的银粉,形状为近球形,颗粒均匀,分散性良好,其一次粒子的平均粒度为0.89μm,分布在0.36-1.67μm之间,振实密度为5.4g·cm-3。
通过以上两种工艺制备的银粉都适合制备太阳能电池正面银浆,各有优点,前者工艺制备的银粉分散性好,而后者工艺制备的银粉振实密度高。
2、发现了银粉的分散性、振实密度及银浆的银含量对太阳能电池正面银浆的影响规律。高的分散性和振实密度有利于制备高品质的银浆,由其制备的太阳能电池正面银浆具有良好的丝网印刷性,其烧结厚膜的电极线条精密、平整、致密、孔洞率小,具有优异的导电性,从而提高了太阳能电池的光电转化效率,其单晶硅太阳能电池光电转化效率达17.803%。该新的发现还未见有文献报道。
3、优化了一个满足正银浆料所需的良好流平性、触变性和印刷性的有机载体。山该有机载体制备的太阳能电池正银浆料,兼备了良好的流平性、触变性和丝网印刷性能,该正银浆料印刷的电池电极和栅线具有大的湿重、膜厚和高宽比,每片电池湿重达0.18g,膜厚达33μm,高宽比达0.306,同时,电极和栅线与晶硅界而具有高的附着力(0.4N.mm-2)和良好的可焊性,该条件下制备的太阳能电池具有优异的光电转化效率,其单晶硅电池光电转化效率达17.963%。该配方还未见有文献报道。
4、发展了低成本、短流程正面银浆制备技术,该技术由湿态银粉直接配制浆料,最大限度地减少了银粉的团聚带来的负面影响,使电池性能进一步提高(可达18.020%)。发现制备该正银浆料的新工艺可克服银粉干燥过程加剧团聚的不利影响,摒弃了传统电子浆料生产时易使固、液混合和研磨不均匀的缺点,使得制备的正银浆料分散性更好,细度更细,提高了高精度、高分辨率、高速丝网印刷性能和增强了浆料的过网能力。
5、发现了正银浆料的丝网印刷、烘干和烧结工艺对太阳能电池电学性能和光电转换效率的重要影响规律。将各种工艺调到最佳匹配值才能最大限度的提高电池性能。
Solar energy is the most important one of the renewable energy, and it is a pollution-free, abundant, renewable energy of the future. Therefore, the study and application of solar energy is a main direction in the future of mankind. Silver paste is the key material of mading solar cells, and its ingredient, preparation process has a direct impact on physical and electrical performance of solar cell. Aimming at the frontier of science and technology of the world today, two key ingredients of solar cell silver paste, namely silver powder and organic vehicle, were investagated. Using chemical liquid-phase reduction method, micron/submicron spherical silver powder for solar cell front silver paste application was prepared. And organic vehicle for solar cell front silver paste application was optimized. At the same time, the law of silver powder characteristics parameter and solar cell performance, the relevance between organic vechicle and scree-pinting, electrical performance and the relevance between preparation processes of silver paste with solar cell performance are discovered. The main results are as follows:
1. Highly dispersive micron/submicron spherical silver powder for solar cell front silver paste is investigated. And dispersion mechanism of polyvinyl alcohol for preparing silver powder is firstly revealed, namely it is the chemical and physical adsorption, which is a key technology breakthrough of preparing silver powder by the chemical reduction method. We use silver nitrate as raw materials to prepare silver powder, using chemical liquid-phase reduction process. Through single factor experiment and orthogonal designs, we have optimized two processes preparing silver powder for the solar cell front silver paste.
For single factor experiment design, eleven factors of influencing granularity, morphology and dispersivity of silver powder are experimented. The desired silver powder is prepared successfully and its law is discovered. The process conditions:ascorbic acid as reduction agent, PVA as disperser, pH=7, disperser usage of8wt%(relativer to the mass of silver nitrate), dipping speed of12.500mL·s-1, stirring speed of200PRM, the concentration of reducion solution of1.177mol·L-1, the concentration of silver nitrate solution of0.294mol·L-1, adding disperser to silver nitrate solution, adding silver nitrate solution to reduction solution, temperature of50℃, a ethanol solution of glyceryl monostearate as posttreatment agent, as-prepared silver powder has good dispersivity, spherical shape, the average particle size of0.81μm, the distribution of0.37～1.04μm, the tap density of4.9g·cm-3. Using ultraviolet and visible spectrum, the disperser mechanism of the preparation of silver powder using polyvinyl alcohol as disperser is suggested firstly, which mechanism is the chemical and physical absorption mechanisms.
Using the orthogonal experimental design, six factors and five levels are experimented. The optimal process conditions:silver nitrate solution concentration of0.3mol·L-1, ascorbic acid solution concentration of1.4mol·L-1, gelatin as disperser, the disperser usage of8wt%(relative to the mass of silver nitrate), pH=4, the temperature of50℃. As-prepared silver powder has the nearly spherical shape, good dispersivity,0.36～1.67μm size distribution, average particle size of0.89μm and the tap density of5.4g·cm-3.
Silver powders prepared through the above two kinds of processes are all suitable for preparing front silver paste of solar cell. Each of them has its advantage. Silver powder prepared by the former process has good dispersion while the one prepared by the latter process has high tap density.
2. For the first time, a significant impact of dispersivity, tap density of silver powder and silver content in silver paste on the thick film and solar cell has discovered, and a higher dispersivity and tap density of silver powder is conducive to the preparation of the high quality silver paste, and its thick film has good screen-printing, which is helpful to increase conversion efficiency of solar cell (up to17.803%for monocrystalline silicon solar cell). This new discovery has been not reported.
3. An optimal organic vehicle formula is found. The solar cell front silver paste prepared using it has desired levelling, thixotropy and screen printing property. And the thick film has bigger wet weight (up to0.18g), thicker thickness (up to33μm) and bigger aspect ratio (up to0.306), and the thick film is even and compact. The grid has high adhesion (up to0.4N/mm2) and good solderability. The cell has higher photo-electric conversion efficiency (up to17.963%). This formula has been not reported.
4. This paper for the first time reported that wet silver powder is directly applied to prepare silver paste, which the negative impact of silver powder agglomeration is abated and improve cell efficiency (up to18.020%) by the greatest extent. This process has yet been not seen in reports.
5. By improving the preparation process of silver paste, the use of advanced mechanical method in mixxing of solid/liquid and solid/solid and gridding is more even and achieving better performance than the manual methods. At the same time, a significant impact of screen printing, coasting, sintering on the performance is discovered. Only matching the various techniques can high performance be required.
引文
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