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Progress in Chemistry 2022, Vol. 34 Issue (4): 926-949 DOI: 10.7536/PC210710 Previous Articles   Next Articles

• Review •

Boron Removal Method, Technology and Process for Producing Solar Grade Silicon by Metallurgical Method

Yi Zeng1, Yongsheng Ren1,2,3(), Wenhui Ma1(), Hui Chen2, Shu Zhan4, Jing Cao1   

  1. 1 Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology,Kunming 650093, China
    2 Department of Materials Engineering, The University of Tokyo, Tokyo 113-8656, Japan
    3 State Key Laboratory of Advanced Metallurgy, University of Science and Technology Beijing,Beijing 100083, China
    4 School of Computer and Information, Hefei University of Technology, Hefei 230601, China
  • Received: Revised: Online: Published:
  • Contact: Yongsheng Ren, Wenhui Ma
  • Supported by:
    Youth Fund of the National Natural Science Foundation of China(52104303); Yunnan Joint Fund of the National Natural Science Foundation of China(U1702251); Open Fund of the State Key Laboratory of Advanced Metallurgy of University of Science and Technology Beijing(KK21-07)
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As a kind of green renewable energy, solar energy has attracted wide attention, and impurity removal is a necessary purification process to obtain solar grade silicon from metallurgical grade silicon, which is very important for the preparation of silicon-based solar cells. The new technology for preparing solar grade polysilicon by the metallurgical method has become the focus of research and development because of its advantages such as low energy consumption, low cost and less pollution. However, the effective removal of boron is one of the most severe challenges we face. In this paper, the thermodynamic and kinetic properties of boron (solubility, diffusivity, diffusion coefficient, mass transfer coefficients and activity coefficient) and the research topics of boron removal in recent years (gas blowing, slag treatment, plasma treatment, acid leaching and solvent refining) are reviewed. It is found that solvent refining is a promising method to obtain high purity silicon. The enrichment rate of silicon and the removal rate of boron can reach more than 90%. Additives can strengthen the formation and precipitation of borides to improve the boron removal process, and the subsequent almost can be completely eliminated, which will not cause pollution to the refined silicon, which will be more effective in boron removal and increase the practicability of the process. At the end of the paper, several deboration processes are compared and analyzed, and the application prospect of metallurgical process is forecasted.

Contents

1 Introduction

2 Properties of boron in silicon

2.1 Solubility of boron in silicon

2.2 Diffusivity of boron in silicon

2.3 Diffusion coefficients and mass transfer coefficients of boron in silicon and slags

2.4 Activity coefficients of boron in silicon and slags

2.5 Segregation coefficients of boron between solid silicon and solvent

2.6 The technical difficulties and challenges of boron removal in silicon

3 Boron removal process

3.1 Boron removal by gas blowing

3.2 Boron removal by slag treatment

3.3 Boron removal by a united refining technique combined gas blowing with slag treatment

3.4 Boron removal by plasma refining

3.5 Boron removal by acid leaching

3.6 Boron removal by solvent refining

3.7 Application of boron removal technology by metallurgical method

4 Conclusion and prospect

Key words: solar energy, metallurgical grade silicon, boron removal, metallurgical process, silicon purification
Fig. 1 Phase equilibria in the Si-rich Si-B system
Fig. 2 Diffusion coefficients of B in Si
Table 1 Diffusion coefficients and mass transfer rates[10,11,22⇓⇓⇓⇓⇓⇓⇓~30].DSi and DS are the diffusion coefficients of B in Si and BO1.5 in slag, respectively. βSi and βS are the mass transfer coefficients of B in Si and BO1.5 in slag, respectively. δSi and δS are boundary layer thicknesses in Si and slag, respectively
Slags (mass fraction) D Si DS βSi βS δSi δS Temp. ref
Unit 10-8 m2·s-1 10-9 m2·s-1 10-6 m·s-1 10-7 m·s-1 mm mm K -
- 2.4±0.7 1687 Kodera[11]
- 1.2 1687 Garander[10]
0.63Na2O-0.37SiO2 3.66 1973 Fang et al.[22]
0.4CaO-0.4SiO2-0.2MgO 43 1923 Krystad et al.[23]
0.2CaO-0.6SiO2-0.1CaF2-0.1Al2O3 6.85 1.01 2073 Zhang et al.[24]
- 2.1 1687 Tang et al.[25]
0.5CaO-0.5SiO2 1.46 170 31.6 0.086 1823 Wu et al.[26]
0.4CaO-0.4SiO2-0.2K2CO3 243 1823 Wu et al.[27]
0.55CaO-0.45SiO2 14 1823 Nishimoto et al.[28]
0.20CaO-0.17SiO2-0.63CaCl2 8.46 250 0.34 1723 Wang et al.[29]
0.37CaO-0.63SiO2 5.24 62 0.85 1723 Wang et al.[30]
Fig. 3 Activity coefficients of B in Si
Table 2 Interaction coefficients between various elements and boron in silicon[21,31,32,34,35,37]
Interaction coefficients Results ref
ε B N 240(1723 K),80±20(1723 K),73±1(1773 K) Noguchi et al.[21] and Tanahashi et al.[31]
ε B C a -0.38±0.84(1723 K) Inoue et al.[32]
ε B B 370±140(1273 K), 120±40(1373 K), 67±20(1473 K) Yoshikawa et al.[34]
ε B A l 1313(1173 K), 970(1273 K), 610(1373 K), 400(1473 K) Yoshikawa et al.[34]
ε B S n 2506±143(1173 K) Xu et al.[37]
ε B B -159±45(1483 K), -111±28(1533 K), -96±12(1583 K);
-164±8(1723 K), -105±8(1733 K)		 Khajavi et al.[35]and Tanahashi et al.[31]
Table 3 Segregation coefficients of boron between solid silicon and eutectics[35,38⇓⇓⇓~42]
Alloys Results ref
Si 0.8 Hall[38]
Si-Al 0.22(1273 K),0.32(1373 K), 0.49(1473 K) Yoshikawa et al.[34]
Si-17 wt% Fe 0.07(1480 K) Esfahani et al.[39]
Si-Sn 0.038(1500 K, calculated) Zhao et al.[40]
Si-34 wt% Ni 20~65 Yin et al.[41]
Si-20 wt% Fe
Si-50 at% Cu
Si-50 at% Cu+Zr		 0.33(1483 K),0.41(1533 K), 0.49(1583 K)
0.29(1345 K)
0.21(1345 K)		 Khajavi et al.[35]
Ren et al.[42]
Ren et al.[42]
Fig. 4 The cross-sectional configuration of experimental setup for gas injection
Fig. 5 Mechanism of boron removal using a mixed water vapor and oxygen gases refining
Fig. 6 Mixing free energy of gaseous boric species for Ar-H2O-(H2, O2 or CO2)-B system through HSC chemistry
Fig. 7 Reaction mechanism of boron removal using CaO-SiO2 slag
Fig. 8 Phase diagram of binary CaO-SiO2 system
Fig. 9 Schematic diagram of boron removal by CaO-SiO2-ZnO ternary slag refining
Fig. 10 Research idea of united refining technique of combining gas blowing with slag treatment
Fig. 11 Boron partition versus a function of slag composition of binary CaO-SiO2 and ternary CaO-SiO2-CaF2 system
Fig. 12 Schematic diagram of synergistic separation to boron using combined slag treatment and gas blowing refining technique
Fig. 13 Mechanism of deboronization process for MG-Si purification by Ar-H2-H2O plasma refining
Fig. 14 Schematic of the experimental apparatus for solvent refining
Fig. 15 Schematic diagram of interaction between boron and additive element in Si-Al melt
Fig. 16 Ellingham diagram of partial borides
Fig. 17 Distribution coefficients of B between slag and Si-Cu alloy as a function of (a) CaO/SiO2 and (b) SiO2/Al2O3 ratios of slag equilibrated at 1773 K
Fig. 18 A schematic of the process of the dissolution of MG-Si, recrystallization of a Si grain, and segregation of impurities
Fig. 19 The B removal from Si-Al, Si-Sn, and Si-Al-Sn alloys using solvent refining methods
Table 5 Reported removal efficiency of B from Si-based alloys using solvent refining method[39,40,42,62,85,97,99,100,101,104,106,108,113,115,116,118,126,128,129,134,135,136⇓⇓⇓⇓⇓⇓⇓⇓⇓⇓⇓⇓~149]
Authors and ref Alloy system B removal efficiency P removal efficiency Si separation method
Yoshikawa and Morita et al.[97] Si-54 wt% Al 56→0.81 ppmw (98.6%) 35.8→0.93 ppmw (97.4%) Electromagnetic separation
Obinata and Komatsu et al.[136] Si-Al 120→20 ppmw (83.3%) Electrolysis separation
Yoshikawa et al.[137] Si-54 wt% Al + Ti 65.4→0.42 ppmw (99.4%) - Electromagnetic separation
Gumaste et al.[138] Si-Al 6→6 ppmw 45→15 ppmw (98.6%) Pouring+acid leaching
Gu et al.[139] Si-Al 8→1.55 ppmw (80.6%) 13→0.41 ppmw(96.8%) Pouring the residual alloy+
Acid leaching
Li et al.[140] 35 wt% Si-Al 8.33→5.25 ppmw (37.0%) 33.65→13.5 ppmw (60.0%) Super gravity separation
Hu et al.[104] Si-Sn 12.1→3.3 ppmw (Si-Sn alloy) 242.6→44.5 ppmw (Si-Sn alloy) Super gravity separation
Si-Al →0.28 ppmw (Si-Al alloy) →0.46 ppmw (Si-Al alloy)
Jie et al.[141] 30 wt% Si-Al 65→3.1 ppmw (93.4%) 68→10.8 ppmw (81.4%) Electromagnetic separation
Li et al.[135] 22.8 wt% Si-Al 14.8→3.8 ppmw (74.3%) - Acid leaching
Li et al.[134] Si-63.8 wt% Al 14.8→1.4 ppmw (90.5%) - Acid leaching
Ma and Lei et al.[99,100,142] 45 wt% Si-Al 27.9→10.8 ppmw (61.3%) 104.9→2.5 ppmw (97.6%) Electromagnetic separation
+Directional solidification
Si-54 wt% Al + Zr 65.4→0.42 ppmw (99.4%) - Electromagnetic separation
Al-46 wt% Si + Hf 58.9→1.04 ppmw (98.2%) - Electromagnetic separation
Al-46 wt% Si + Ti 58.9→0.46 ppmw (99.2%) - Electromagnetic separation
Esfahani et al.[39] Si-17 wt% Fe 27→2 ppmw (92.6%) 68→29 ppmw (57.4%) Heavy medium
Khajavi et al.[116] Si-Fe (70%, at 1583 K; 65%,
at 1483 K)		 - Acid leaching
Wu et al.[115] Si-Fe - 378.5→17.2 ppmw (95.5%) Acid leaching
Luo and Huang et al.[108,113,143] Si-Cu 3.12→1.29 ppmw (58.7%) 17.14→9.9 ppmw (42.2%) Acid leaching
Si-50 wt% Cu + 3.12→0.35 ppmw (88.8%) 17.14→7.27 ppmw (57.8%) Acid leaching
slag treatment
Si-Cu 36→27 ppmw (25%) 25→18 ppmw (28%) Directional solidification
Li et al.[62] 30 wt% Si-Cu 15→1 ppmw (93.3%) 20→1 ppmw (95%) Acid leaching
Zhang et al.[144] Si-Sn - 16.1→3.77 ppmw (85.51%) Zone melting directional
solidification method
Li et al.[128] Si-Sn+ 12.92→0.79 ppmw (93.9%) - Acid leaching
slag treatment
Ma et al.[85,145,146] Si-Sn 33→11.6 ppmw (64.8%) 37→9.7 ppmw (73.8%) Directional solidification method
Sn-84.4 wt% Si + 33→9.2 ppmw (75.1%) 36.2→9.6 ppmw (73.5%) Directional solidification method
slag treatment
Sn-26.2 wt% Si + 33→0.3 ppmw (99.1%) - Electromagnetic separation
slag treatment
Hu et al.[147] Si-Sn + Ca 10.3→3.12 ppmw (69.71%) 108.5→28.9 ppmw (73.36%) Super gravity separation
Li et al.[129,148] Si-Al-Sn 14.8→3.8 ppmw (74.3%) - Electromagnetic separation
Si-Al-Zn 14.8→3.8 ppmw(74.3%) - Acid leaching
Zhao et al.[40] 6 wt% Si-Sn 15→0.1 ppmw (99.3%) - Acid leaching
Lei et al.[149] Si-5wt% Zr 52→35 ppmw (32.7%) 51→12 ppmw (76.5%) Acid leaching
Morito et al.[118] Si-Na - 73→3.4 ppmw (95.3%) Acid leaching
Lai et al.[126] Si-Ca 8.6→3 ppmw (65.1%) 35→4 ppmw (88.6%) Acid leaching
Ren et al.[106] Si-50 at% Sn + Zr 120→31.2 ppmw (73.6%) - Directional solidification+
Acid leaching
Ren et al.[42] Si-50 at% Cu + Zr 80→5.3 ppmw (93.4%) - Directional solidification +
Acid leaching
Chen et al.[101] Al-35at% Si + V 73.6→35.5 ppma (76.8%) - Directional solidification +
Acid leaching
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