Abstract
The existence of inclusions in industrial silicon seriously affects the conversion efficiency of organic silicon monomer synthesis, making it difficult to meet the requirements of polycrystalline silicon production for raw materials. In this work, the basic slag system SiO2-CaO-Al2O3 was used to remove inclusions in industrial silicon. The microstructure and chemical composition of metal inclusions formed by the main metal impurities in industrial silicon were considered, and the physical and chemical behavior and evolution process of inclusions in industrial silicon before and after refining were analyzed. The effect of the CaO/SiO2 ratio on the removal of inclusions was examined. It was found that when CaO/SiO2 = 0.38, the removal effect of metal inclusions in industrial silicon was the best; the removal rates of Fe, Al, Ca, and Ti reached 27.1%, 68.7%, 25.1% and 99.1%, respectively. This study provides an idea for industrial silicon refining technology and high-quality industrial silicon product development.
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References
Lucio CA, Angelo B, Piotr K, Marco L, Lisa R (2019) Silicon solar cells: toward the efficiency limits. Adv Phys-X 4(1):1548305
Lei Y, Ma XD, Wang Y, Chen ZY, Ren YS, Ma WH (2022) Recent progress in upgrading metallurgical-grade silicon to solar-grade silicon via pyro-metallurgical routes. Int J Miner Metall Mater 29(4):767–782
Wen JH, Deng XC, Ma WH, Wei KX, Zhang ZY, Xu FC (2019) Research progress on influence of metallurgical grade silicon quality on organosilicon monomer synth. J Kunming Univ Sci Technol (Natural Science) 44:1–7
Zhang HM, Chen ZJ, Wen JH, Ma WH, Cao SJ (2021) Effect of silica and carbon-reducing agents on Ni and Ti impurities during silicon production. Silicon 14(9):4925–4934
He YF, Ma WH, Xing AM, Xu PB, Yang X (2022) A high-efficiency and energy-saving method for purifying industrial silicon for silicone use. Silicon(online). https://doi.org/10.1007/s12633-022-02141-4
Ding Z, Wei KX, Ma WH, Wu JJ, Zhou Y, Xie KQ (2012) Boron removal from metallurgical-grade silicon using lithium containing slag. J Non-Cryst Solids 358(18–19):2708–2712
Huang LQ, Lai HX, Lu CH, Luo XT (2016) Enhancement in extraction of boron and phosphorus from metallurgical grade silicon by copper alloying and aqua regia leaching. Hydrometallurgy 161:14–21
Lu HF, Wei KX, Ma WH, Lei Y (2017) The effect of secondary refining on the removal of phosphorus from metallurgical-grade silicon by acid leaching. Metall Mater Trans B 48:2768–2780
Li S, Deng XC, Wen JH, Wei KX, Ma WH (2021) Microstructure evolution of precipitates during solidification in metallurgical grade silicon. Intermetallics 128:106987
Meteleva-Fischer YV, Yang Y, Boom R, Kuntzel H (2012) Microstructure of metallurgical grade silicon during alloying refining with calcium. Intermetallics 25:9–17
Li S, Deng XC, Wei KX, Ma WH, Wu JJ (2020) Effect of electromagnetic strengthening on microstructure of precipitates in metallurgical grade silicon. J Alloy Compd 816(C):152507
Li S, Deng XC, Zhang C, Wen JH, Wu JJ, Ma WH (2020) Leaching behavior of impurities in metallurgical grade silicon subjected to electromagnetic strengthening. J Alloy Compd 831:15488
Ciftja A, Engh TA, Tangstad M, Kvithyld A (2009) Removal of inclusions from silicon. JOM 61(11):56–61
Wang D, Wang ZK, Wang Z, Qian GY, Gong XZ, Xin L (2020) Silicon recovery from silicon sawing waste by removal of SiC impurity via CaO-SiO2-Na2O slag absorption. Sep Purif Technol 231(C):115902
Yang SC, Wan XH, Wei KX, Ma WH, Wang Z (2021) Investigation of Na2CO3-CaO-NaCl (or Na3AlF6) additives for the remanufacturing of silicon from diamond wire saw silicon powder waste. J Clean Prod 286:125525
Li YQ, Li ZT, Zhang LF, Wen X, Ren CY, Yu YL (2021) Silicon recovery from Si sawing waste through slag refining. Sep Purif Technol 274:119025
Li YQ, Pan D, Zhang LF, Li JY, Wen X (2021) Slag refining for separate-on of SiC inclusions from Si. Sep Purif Technol 279:119794
Xi FS, Cui HQ, Yang TT, Li SY, Ma WH, Chen XH, Zheng DM, Wei KX, Chen R (2020) Mechanism of enhancing Fe removal from metallurgical grade silicon by metal-assisted chemical leaching. J Mater Res Technol 9(6):12213–12222
Long X, Luo WB, Lu GH, Chen FL, Zheng XN, Zhao XF, Long SL (2022) Iron removal from metallurgical grade silicon melts using synthetic slags and oxygen injection. Materials 15(17):6042
Deng XC, Zhou L, Wei KX, Ma WH (2023) The use of vacuum refining to separate Ca, Al, and P from crude metallurgical grade silicon. Vacuum 207:111581
Xi FS, Zhang Z, Li SY, Ma WH, Chen XH, Chen ZJ et al (2021) Influence of iron, aluminium, calcium, titanium and vanadium impurities removal from silicon based on Cu-catalyzed chemical leaching. J Mater Res Technol 10:502–511
Wang Z, Ge Z, Liu JH, Qian GY, Du B (2018) The mechanism of boron removal from silicon alloy by electric field using slag treatment. Sep Purif Technol 199:134–139
Chen H, Kzk M, Ma XD, Chen ZY, Wang Y (2019) Boron removal for solar-grade silicon production by metallurgical route: a review. Sol Energy Mater Sol Cells 203:110169
Zhang C, Wei KX, Zheng DM, Ma WH, Dai YN (2017) Phosphorus removal from upgraded metallurgical-grade silicon by vacuum directional solidification. Vacuum 146:159–163
Li YQ, Zhang LF, Pan D (2022) Removal of SiC and Si3N4 inclusions in solar cell Si scraps through slag refining. High Temp Mater Process 41(1):132–136
Li YQ, Pan D, Zhang LF, Duan HJ, Lei XH, Chen W, Li JY (2022) Characterization of SiC and Si3N4 inclusions in solar cell Si scraps and their motion at the Si/slag interface. J Mater Res Technol 17:2220–2228
Hou Y, Zhang GH, Chou KC (2021) Reaction behavior of SiC with CaO-SiO2-Al2O3 slag. ISIJ Int 61(3):745–752
Anglézio JC, Servant C, Dubrous F (1990) Characterization of metallurgical grade silicon. J Mater Res 5(9):1894–1899
Anglézio JC, Servant C, Ansara I (1994) Contribution to the experimental and thermodynamic assessment of the Al-Ca-Fe-Si system-I. Al-Ca-Fe, Al- Ca-Si, Al-Fe-Si and Ca-Fe-Si systems. Calphad 18(3):273–309
Zhang ZY, Zheng T, Zhuang YX, Xing PF, Kong J et al (2022) Recovery and purification of metallurgical silicon from waste silicon slag by blowing refining. J Clean Prod 371:133655
Qiao D, Liang S, Zhao JG, Peng YX et al (2022) Study on the composition and interface of waste silicon slag after secondary refining. SILICON 14(9):5029–5034
Tang K, Eivind J, Gabriella T, Merete TA (2009) A thermochemical database for the solar cell silicon materials. Mater Trans 50(8):1978–1984
Acknowledgements
The authors wish to acknowledge the financial support on this research from the National Natural Science Foundation of China (22078140), the Talent Training Program of Yunnan of China (202005AC160041 and KKXY202252002), and Key Science and Technology Specific Projects of Yunnan Province (202202AG050012).
Funding
The authors are grateful for financial support from the National Natural Science Foundation of China (22078140), the Talent Training Program of Yunnan of China (202005AC160041 and KKXY202252002) and Key Science and Technology Specific Projects of Yunnan Province (202202AG050012).
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Zuhan Shan: Experiment development, Data Integration, Writing—original draft. Jianhua Wen: Provision of study materials, reagents, computing resources. Guiming Yang: Visualization of experimental results. Fuchang Xu: Validation, Software. Jijun Wu: Funding acquisition, Project administration. Kuixian Wei: Data curation, Supervision. Wenhui Ma: Conceptualization, Provide ideas.
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Shan, Z., Wen, J., Yang, G. et al. Inclusions Removal in Industrial Silicon by SiO2-CaO-Al2O3 Based Slag System. Silicon 15, 4889–4896 (2023). https://doi.org/10.1007/s12633-023-02404-8
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DOI: https://doi.org/10.1007/s12633-023-02404-8