氟化物熔盐体系中Si的电化学提取与提纯
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摘要
太阳级Si的低成本高效率制备是光伏产业发展的迫切需求,也是国家能源战略的重要组成部分。论文在博士点基金、湖南省研究生创新项目和中南大学优博扶植基金的资助下,以制备高纯Si和含Si合金为目标,开展氟化物熔盐体系中Si的电解提取与电解精炼研究,探讨了氟化物熔盐体系中多种组元的热力学沉积条件,研究了Si在固态电极和液态金属电极上的电化学行为,研究了Na3A1F6-SiO2体系中Si的电解提取工艺,提出并研究了Si的三层液和水平式熔盐电解精炼工艺,主要研究结果如下：
(1)基于自由能计算获得了氟化物熔盐体系中主要元素的电极电位和电沉积序,结合实际组元浓度获得了Si的单一沉积临界条件。Sr、Mg、Ca等元素因电极电位比Si负,不会与Si共沉积；而Fe、Cu、P等元素在电解质中的浓度大于理论计算获得的“极限浓度”时,会先于Si电沉积析出,从而影响沉积Si的纯度。
(2)揭示了Si在氟化物熔盐体系中的电沉积机理,建立了沉积Si在液态阴极中的传质模型,获得了低熔点合金元素扩散系数和活度系数等难以直接测量的基础数据。在Na3A1F6熔体中阳离子的还原序为Si、A1及Na,通过控制电解质中Si离子浓度和沉积电位,可以实现单质硅的沉积。Si在不同液态金属中的扩散系数差异显著,Cu-Si熔体中Si的扩散系数比A1-Si熔体中要高两个数量级。A1-Si合金中硅浓度为3.230×10-5mol/cm3时活度系数为0.387,浓度为6.457×10-5mol/cm3时活度系数为0.435。
(3)揭示了原料、电极材料和电解工艺参数对Na3A1F6-SiO2熔盐中电解提取Si的电流效率和产物纯度的影响规律。固态电极上电解硅的纯度高于99.9%,主要杂质为A1、Fe、Ti等。电解槽容量和电流的增大可显著提高电流(收集)效率,200A电解20h后阴极A1-Si合金中Si的平均含量高于18%,部分区域合金中Si含量达到40%。与冶金Si相比,以液态Al为阴极电解制备A1-Si合金所分离出单质Si纯度更高,其中杂质B和P含量分别降低到3.3和10.2ppmw,含量低于10ppmw的其它杂质元素有Ti、Ni和Cu。
(4)通过三层液熔盐电解精炼实现了Si的提纯。电解精炼过程可以在大电流密度(400mA/cm2)下平稳进行,电解阳极电流效率高于95%。与直接熔配合金相比,三层液精炼制备Al-Si合金中B和P的含量分别由32.7和32.5降低到4.8和12.4ppmw,合金总的纯度也由99.950%提高到99.987%,其中分离得到的单质Si中的B和P的含量最低分别为2.2和6.5ppmw。熔盐电解及精炼制备的Al-Si合金更适合作为合金凝固提纯制备太阳级Si的原料。
(5)发展了基于液态电极的水平式熔盐电解精炼Si的新方法,突破了三层液熔盐电解中电解质和电极材料密度差异对精炼体系的限制。水平式精炼过程在高达800mA/cm2电流密度下运行平稳,电流效率达到98.6%,水平槽型电流密度分布不均匀特点并未对电解精炼带来不利影响。以Al为阴极水平精炼Si时的收集效率较低,随着电流密度的增大,收集效率从50mA/cm2时的32%降低到400mA/cm2的15%,而以Cu-8wt%Si合金为阴极时收集效率最高可达78%。
(6)提出了从SiO2到太阳级Si的熔盐电化学-合金凝固提纯工艺原型。针对合金凝固提纯方法目前所存在的除杂效率和产品纯度问题,采用熔盐电化学方法提高合金原料纯度,同时利用水平精炼来实现高纯Al的循环利用。与西门子法相比,该工艺更简单,估算综合能耗仅为58.4kWh/kg。
Developing a low-cost solar grade (SoG) silicon feedstock is both requirement of continued rapid expansion of the photovoltaic (PV) market and a very important role in national energy security strategies. This thesis work has been funded by Specialized Research Fund for the Doctoral Program of Higher Education(Grant No.200805331120), Hunan Provincial Innovation Foundation For Postgraduate (CX2009B036) and Innovation Foundation of Central South University(2010bsxt02). After systematic analyzing of the advantages and disadvantages of "solidification refining with Al-Si melts" method, this paper focuses on the study of electrochemical preparation of high pure Si and Si alloys. The reduction potentials of elements in fluoride molten salt were calculated based on Gibbs free energy, and the electrodeposition behavior of Si on solid and liquid electrodes were studied. Furthermore, electrowinning of Si in Na3AlF6-SiO2molten salt was studied systematically considering the electrolysis parameters, electrolysis cell and composition of electrodes. Meanwhile, three-liquid-layer electrorefining and similar horizontal electrorefining of Si were proposed and carried out. The main results of the thesis can be summarized as follows:
(1) Reduction potential of each element is calculated based on the Gibbs free energy of fluoride, the conditions of co-deposition of impurities and Si in complex fluoride molten salt are also discussed. Reduction potentials of impurities such as Sr, Mg and Ca are more negative than Si, which means that they can't co-deposit with Si. When the concentration of impurities such as Fe, Cu and P are greater than the calculated minimal concentration in complex fluoride molten salt, they would be reduced prior to Si and bring bad influence on the purity of deposited Si.
(2) Si electrodeposition behavior in complex fluoride molten salt is revealed by electrochemical measurements. Silicon diffusion into liquid cathode is modelled and evolution of diffusion coefficient and Si activity with concentration is deduced by a mathematic approach based on the electrochemical results. Cyclic voltammograms (CVs) showed that the reduction order of ions in Na3AlF6-LiF melts are Si, Al and Na. Maintaining the concentration and adjusting the reduce potetial of Si ions in eletrolyte, Si can be successfully depostied without codeposition of Al and other impurities. Si diffusion coefficient in Al-Si alloy is much less than that in Cu-Si alloy. When the Si concentration in Al-Si alloy are3.230×10-5mol/cm3and6.457×10-5mol/cm3, Si activity coefficiency are0.387and0.435respectively.
(3) This study demonstrates the feasibility of continous Si alloy and very pure Si production directly from SiO2by electrowinning using liquid electrodes. The influence law of electrolysis parameters, electrolysis cell and electrodes materials on current efficiency of electrowinning and purity of deposits is revealed. Solid deposited Si is more pure than99.9%, the dominant impurities are Al, Fe and Ti. The experimental works with200A scale indicate that the average Si content in Al-Si alloy after electrolysis is found above18%, and the highest Si content in top area of solidified Al-Si alloy is near40%. Compared with the MG-Si, Si crystals in Al-Si alloy prepared from200A and20h electrolysis are much more pure, impurities such as B and P are decreased from5.1and21.4to3.3and10.2ppmw respectively. Moreover, concentration of impurities B, Ti, Ni and Cu are all less than10ppmw.
(4) Taking advantage of the knowledge of Al electrorefining, the influence law of electrolysis parameters, electrolysis cell and electrodes materials on current efficiency of electrorefining and purity of deposits is revealed. Deposited silicon particles are found embedded in electrolyte. Furthermore, with increasing operation time and current density, re-combination of silicon particles is revealed and yield a larger size Al-Si alloy ball of2cm. Compared with the smelting Al-Si alloy, electrorefined Al-Si alloy shows a remarkable reduction of B and P concentration, decreasing from32.7and32.5to4.8and12.4ppmw respectively. B and P concentration in Si crystals separated from electrorefined Al-Si alloy are as lower as2.2and6.5ppmw respectively. Al-Si alloy obtained from electrochemical methods are more appropriate as raw materials for the alloy solidification refining method.
(5) A modified horizontal electrorefining cell was developed and the uneven current density distribution does not bring bad influences on the electrochemical process. Aluminum electrorefining could run steady under current density as high as800mA/cm2and current efficiency can reach95%. Under experimental scale, Si electrorefining using horizontal cell indicates that Cu-8wt%Si alloy is more appropriate than A1acting as cathode and collecting the deposited Si.
(6) An innovative route for production of SoG-Si is raised with the combination of molten salt electrochemical method and alloy solidification physical method. Although this process isn't optimized yet, electrochemical method is believed that can satisfy the demand of high pure raw materials and recycle the high pure Al during the physical production lines. Compared with the Siemens process, this route is simple and saves a great deal of energy, only consuming less than58.4kWh per kg
(1)基于自由能计算获得了氟化物熔盐体系中主要元素的电极电位和电沉积序,结合实际组元浓度获得了Si的单一沉积临界条件。Sr、Mg、Ca等元素因电极电位比Si负,不会与Si共沉积；而Fe、Cu、P等元素在电解质中的浓度大于理论计算获得的“极限浓度”时,会先于Si电沉积析出,从而影响沉积Si的纯度。
(2)揭示了Si在氟化物熔盐体系中的电沉积机理,建立了沉积Si在液态阴极中的传质模型,获得了低熔点合金元素扩散系数和活度系数等难以直接测量的基础数据。在Na3A1F6熔体中阳离子的还原序为Si、A1及Na,通过控制电解质中Si离子浓度和沉积电位,可以实现单质硅的沉积。Si在不同液态金属中的扩散系数差异显著,Cu-Si熔体中Si的扩散系数比A1-Si熔体中要高两个数量级。A1-Si合金中硅浓度为3.230×10-5mol/cm3时活度系数为0.387,浓度为6.457×10-5mol/cm3时活度系数为0.435。
(3)揭示了原料、电极材料和电解工艺参数对Na3A1F6-SiO2熔盐中电解提取Si的电流效率和产物纯度的影响规律。固态电极上电解硅的纯度高于99.9%,主要杂质为A1、Fe、Ti等。电解槽容量和电流的增大可显著提高电流(收集)效率,200A电解20h后阴极A1-Si合金中Si的平均含量高于18%,部分区域合金中Si含量达到40%。与冶金Si相比,以液态Al为阴极电解制备A1-Si合金所分离出单质Si纯度更高,其中杂质B和P含量分别降低到3.3和10.2ppmw,含量低于10ppmw的其它杂质元素有Ti、Ni和Cu。
(4)通过三层液熔盐电解精炼实现了Si的提纯。电解精炼过程可以在大电流密度(400mA/cm2)下平稳进行,电解阳极电流效率高于95%。与直接熔配合金相比,三层液精炼制备Al-Si合金中B和P的含量分别由32.7和32.5降低到4.8和12.4ppmw,合金总的纯度也由99.950%提高到99.987%,其中分离得到的单质Si中的B和P的含量最低分别为2.2和6.5ppmw。熔盐电解及精炼制备的Al-Si合金更适合作为合金凝固提纯制备太阳级Si的原料。
(5)发展了基于液态电极的水平式熔盐电解精炼Si的新方法,突破了三层液熔盐电解中电解质和电极材料密度差异对精炼体系的限制。水平式精炼过程在高达800mA/cm2电流密度下运行平稳,电流效率达到98.6%,水平槽型电流密度分布不均匀特点并未对电解精炼带来不利影响。以Al为阴极水平精炼Si时的收集效率较低,随着电流密度的增大,收集效率从50mA/cm2时的32%降低到400mA/cm2的15%,而以Cu-8wt%Si合金为阴极时收集效率最高可达78%。
(6)提出了从SiO2到太阳级Si的熔盐电化学-合金凝固提纯工艺原型。针对合金凝固提纯方法目前所存在的除杂效率和产品纯度问题,采用熔盐电化学方法提高合金原料纯度,同时利用水平精炼来实现高纯Al的循环利用。与西门子法相比,该工艺更简单,估算综合能耗仅为58.4kWh/kg。
Developing a low-cost solar grade (SoG) silicon feedstock is both requirement of continued rapid expansion of the photovoltaic (PV) market and a very important role in national energy security strategies. This thesis work has been funded by Specialized Research Fund for the Doctoral Program of Higher Education(Grant No.200805331120), Hunan Provincial Innovation Foundation For Postgraduate (CX2009B036) and Innovation Foundation of Central South University(2010bsxt02). After systematic analyzing of the advantages and disadvantages of "solidification refining with Al-Si melts" method, this paper focuses on the study of electrochemical preparation of high pure Si and Si alloys. The reduction potentials of elements in fluoride molten salt were calculated based on Gibbs free energy, and the electrodeposition behavior of Si on solid and liquid electrodes were studied. Furthermore, electrowinning of Si in Na3AlF6-SiO2molten salt was studied systematically considering the electrolysis parameters, electrolysis cell and composition of electrodes. Meanwhile, three-liquid-layer electrorefining and similar horizontal electrorefining of Si were proposed and carried out. The main results of the thesis can be summarized as follows:
(1) Reduction potential of each element is calculated based on the Gibbs free energy of fluoride, the conditions of co-deposition of impurities and Si in complex fluoride molten salt are also discussed. Reduction potentials of impurities such as Sr, Mg and Ca are more negative than Si, which means that they can't co-deposit with Si. When the concentration of impurities such as Fe, Cu and P are greater than the calculated minimal concentration in complex fluoride molten salt, they would be reduced prior to Si and bring bad influence on the purity of deposited Si.
(2) Si electrodeposition behavior in complex fluoride molten salt is revealed by electrochemical measurements. Silicon diffusion into liquid cathode is modelled and evolution of diffusion coefficient and Si activity with concentration is deduced by a mathematic approach based on the electrochemical results. Cyclic voltammograms (CVs) showed that the reduction order of ions in Na3AlF6-LiF melts are Si, Al and Na. Maintaining the concentration and adjusting the reduce potetial of Si ions in eletrolyte, Si can be successfully depostied without codeposition of Al and other impurities. Si diffusion coefficient in Al-Si alloy is much less than that in Cu-Si alloy. When the Si concentration in Al-Si alloy are3.230×10-5mol/cm3and6.457×10-5mol/cm3, Si activity coefficiency are0.387and0.435respectively.
(3) This study demonstrates the feasibility of continous Si alloy and very pure Si production directly from SiO2by electrowinning using liquid electrodes. The influence law of electrolysis parameters, electrolysis cell and electrodes materials on current efficiency of electrowinning and purity of deposits is revealed. Solid deposited Si is more pure than99.9%, the dominant impurities are Al, Fe and Ti. The experimental works with200A scale indicate that the average Si content in Al-Si alloy after electrolysis is found above18%, and the highest Si content in top area of solidified Al-Si alloy is near40%. Compared with the MG-Si, Si crystals in Al-Si alloy prepared from200A and20h electrolysis are much more pure, impurities such as B and P are decreased from5.1and21.4to3.3and10.2ppmw respectively. Moreover, concentration of impurities B, Ti, Ni and Cu are all less than10ppmw.
(4) Taking advantage of the knowledge of Al electrorefining, the influence law of electrolysis parameters, electrolysis cell and electrodes materials on current efficiency of electrorefining and purity of deposits is revealed. Deposited silicon particles are found embedded in electrolyte. Furthermore, with increasing operation time and current density, re-combination of silicon particles is revealed and yield a larger size Al-Si alloy ball of2cm. Compared with the smelting Al-Si alloy, electrorefined Al-Si alloy shows a remarkable reduction of B and P concentration, decreasing from32.7and32.5to4.8and12.4ppmw respectively. B and P concentration in Si crystals separated from electrorefined Al-Si alloy are as lower as2.2and6.5ppmw respectively. Al-Si alloy obtained from electrochemical methods are more appropriate as raw materials for the alloy solidification refining method.
(5) A modified horizontal electrorefining cell was developed and the uneven current density distribution does not bring bad influences on the electrochemical process. Aluminum electrorefining could run steady under current density as high as800mA/cm2and current efficiency can reach95%. Under experimental scale, Si electrorefining using horizontal cell indicates that Cu-8wt%Si alloy is more appropriate than A1acting as cathode and collecting the deposited Si.
(6) An innovative route for production of SoG-Si is raised with the combination of molten salt electrochemical method and alloy solidification physical method. Although this process isn't optimized yet, electrochemical method is believed that can satisfy the demand of high pure raw materials and recycle the high pure Al during the physical production lines. Compared with the Siemens process, this route is simple and saves a great deal of energy, only consuming less than58.4kWh per kg
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