CN103103552A - Method for preparing silicon by molten salt electrolysis - Google Patents
Method for preparing silicon by molten salt electrolysis Download PDFInfo
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- CN103103552A CN103103552A CN201110362133XA CN201110362133A CN103103552A CN 103103552 A CN103103552 A CN 103103552A CN 201110362133X A CN201110362133X A CN 201110362133XA CN 201110362133 A CN201110362133 A CN 201110362133A CN 103103552 A CN103103552 A CN 103103552A
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Abstract
The invention relates to a method for preparing silicon by molten salt electrolysis. According to the method, carbon, silicon or metal is used as a cathode, a carbon anode or inert anode is utilized to carry out electrolysis in a molten salt system. The invention is characterized in that silicon dioxide can be directly dissolved in the molten salt system, thereby being convenient for continuous electrolysis of silicon. The product of electrolysis can be a simple substance silicon or a silicon composite material. The silicon or silicon composite material obtained by electrolysis can be used as a negative pole material of a battery, and can also be used in the fields of electronics, semiconductors and the like. Besides, the method can also be used for removing impurity silicon in aluminum electrolysis.
Description
Technical field
The present invention relates to the preparation method of Si, adopt dissolving SiO
2The molten salt system Direct Electrolysis obtain Si, characteristics are to SiO
2Good solubility property is arranged, and can be so that suitability for industrialized production is carried out continuous electrolysis.Have technique simple and convenient, speed and the product pattern of producing Si are controlled, and the purity of gained Si is high, has reduced the advantages such as technical process.Prepared silicon can be used for the multiple fields such as cell negative electrode material, electronics, luminescent device, photovoltaic, belongs to nonmetal fused salt electrolysis technical field.(relate in particular to the multiple technologies such as chemical industry, metallurgical industry and fused salt electrolysis field)
Background technology
Silicon has the advantage of heavy body as lithium ion battery negative material, has broad application prospects, and generates in addition the growth requirement that the silicon with functional structure also can become the industry such as electronics.At present, Si produces main traditional Siemens Method and the Siemens Method of improvement of adopting, but has the shortcomings such as investment is large, cost is high, production efficiency is low, energy consumption is high, pollution is large, byproduct is many.Adopt novel method to carry out silicon and produce the focus of studying into people, produce the method for silicon as adopting metallurgy method, it is large that the method has output, and cost is low, is beneficial to the advantages such as industrial production, and shortcoming is that the purity of silicon is low than Siemens Method; Adopt laser ablation method can prepare silicon nanowires, the method output is large, purity is high, but apparatus expensive, product cost is high.
Adopt molten salt system to carry out Direct Electrolysis and obtain metal simple-substance, become aluminium, calcium, beryllium, lithium, sodium etc. and made the preparation method of metal with the hot reducing method difficulty, many rare metals also available fused salt electrolysis process make, as thorium, niobium, zirconium, tantalum etc., but Direct Electrolysis is produced micron and the method for submicron order Si yet there are no report from fused salt.The feldspar of having introduced in patent ZL 95193459.7 in fluoride smelt salt prepares the method for silicon, aluminium silicon or aluminium, but the pattern and the electrolysis raw material that do not have place of matchmakers to get silicon have obviously different from the present invention.And the form difference of negative electrode is larger, and the present invention does not relate to the material that forms alloy with silicon.US Patent No. 3022233 has also been put down in writing in the method for preparing silicon and technology silicide in the system of fluorochemical and silicon tetrafluoride, and negative electrode adopts metal, and same and the present invention also has obvious difference.The FFC technique (WO1999/064638) that univ cambridge uk proposes comprises the preparation method of silicon, but mainly by the solid-oxide reduction is made.But with the method for solid-oxide direct oxidation, be unfavorable for continuous production.The present invention is dissolved in silicon oxide in molten salt system, silicon electrolysis from fused salt is obtained the electrochemical method of nanometer and micron silicon, nanometer and micron silicon line (pipe) material and matrix material thereof, yet there are no report.
Summary of the invention
The present invention is based on the focus of present world silicon industrial development, the successful electrolytic process of research is produced silicon on a large amount of experimental studies bases.The purpose of this invention is to provide a kind of production method that is applicable to the silicon electrolysis, purpose is to solve the problems such as in existing technique, cost is high, production efficiency is low, energy consumption is high, pollution is large, byproduct is many.
A further object of the present invention is to provide a kind of method of producing silicon.
The present invention proposes a kind of when being applicable to method that silicon produces, and the operational condition that is applicable to this fused salt electrolysis silicon also is provided.A kind of method that another object of the present invention is to provide Novel electric enzymatic hydrolysis system and uses inert anode to carry out the silicon electrolysis.
The present invention comes to be realized by the following technical programs:
The molten salt system that the present invention proposes consists of (x) A (y) AlF
3(z) SiO
2, wherein x is the mole percent level of A, y is AlF
3Mole percent level, z is SiO
2Mole percent level, x is that 25～77%, y is that 22～50%, z is 1～25%; A is by KF, NaF, K
2SiF
6, Na
2SiF
6, AlF
3, Al
2O
3, MgF
2, CaF
2, KCl, NaCl, LiF, BaF
2Single or multiple salt form.
The molten salt system that the present invention proposes consists of (x) A (y) AlF
3(z) SiO
2, wherein x is the mole percent level of A, y is AlF
3Mole percent level, z is SiO
2Mole percent level, x is that 25～99%, y is that 0～50%, z is 1～25%; A is by KF, NaF, K
2SiF
6, Na
2SiF
6, AlF
3, Al
2O
3, MgF
2, CaF
2, KCl, NaCl, MgCl
2, CaCl
2, LiCl, LiF, BaF
2Single or multiple salt form.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and the electrolytic process negative electrode can adopt carbon as cathode material, and carbon can adopt carbon dust to press a kind of in the materials such as knot material, particulate state and blocky graphite, gac or carbon fiber.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and electrolytic process can adopt Si as cathode material, the silicon negative electrode can adopt tabular, block and granular monocrystalline or polysilicon.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and electrolytic process can adopt metal as cathode material.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and electrolytic process can adopt carbon as anode material, also can adopt inert anode, and inert anode material and inert anode material for aluminium electrolysis are similar.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and the molten salt system of proposition can be directly with SiO
2Dissolving fast, electrolysis temperature is 500 ℃～1500 ℃.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and the pole span of electrolytic process negative electrode and anode is 0.1～45cm; Can adopt the method for controlling electric current to carry out electrolysis, electrolytic current density is controlled at 0.01～5A/cm
2
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and the pole span of negative electrode and anode is 0.1～45cm; Can adopt the method for controlling voltage to carry out electrolysis, adopt control flume voltage 0.1～30V or control cathode electropotential+3～-3V (vs.Pt) carries out electrolysis.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, and the resulting silicon of electrolysis can be one or more of nanometer and the different morphologies such as micron silicon particle, silicon line, silicone tube and silica fibre, and wherein the size range of silicon is 1nm～1000 μ m.Here the size of said silicon refers to the particle diameter of silicon grain, the diameter of silicon line, silicone tube or silica fibre.
The employing fused salt electrolysis process that the present invention proposes is produced the method for silicon, also can adopt the method to be used for the removal of impurity silicon in electrolysis of aluminum and other electrolytic etching of metal fused salts.
The invention provides a kind of method that adopts fused salt electrolysis to produce silicon, the present invention is conducive to generate the silicon materials with special construction, is applicable to use in the industries such as battery cathode, electronics and semi-conductor.The invention provides a kind of preparation method of silicon, and realized carrying out continuously of electrolysis.The electrolysis temperature composite alloy inert anode of the method has service temperature widely, is fit to 500～1500 ℃.
Advantage of the present invention not only can overcome the above problems, and following advantage is arranged:
(1) silicon of the method preparation as cell negative electrode material, has heavy body, the long lifetime characteristics;
(2) characteristics of the method are that silicon-dioxide can directly be dissolved in molten salt system, are convenient to continuous electrolysis;
(3) can realize directly preparing solid-state elemental silicon or silicon composite under low temperature condition;
(4) the method also can be used for removing impurity silicon in electrolysis of aluminum in addition.
Description of drawings
Fig. 1 is the SEM figure of the silicon of electrolysis gained in embodiment 1, wherein, and a of Fig. 1: * 10000 times; The b of Fig. 1: * 20000 times; The c of Fig. 1: * 90000 times.
Fig. 2 is the silicon electrolytic process bath voltage changing conditions figure in embodiment 1.
Embodiment
The invention will be further described below by embodiment, but claim protection domain of the present invention is not constituted any limitation.
The dimensions length of described nano silicon particles refers to the length of the particle diameter of silicon grain in an embodiment; The dimensions length of silicon line, silicone tube or silica fibre refers to the length of the diameter of silicon line, silicone tube or silica fibre.
Described nanometer refers to the length of dimensions length below 100nm in an embodiment;
Described " % " is " wt% in an embodiment.
Embodiment 1
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (55%) KF (42%) AlF
3(3%) SiO
2Electrolysis temperature is 720 ℃; Take carbon as cathode and anode, pole span is 2cm; Electrolytic current density is controlled at 0.5A/cm
2The electrolytic process bath voltage is steadily 1.4V, according to SiO in fused salt
2Consumption in time replenish SiO
2, SiO
2Dissolving rapidly.Electrolysis obtains the silicon line that purity reaches 98.9wt%, and the linear looks diameter of silicon is that 150nm, length are 3～10 μ m, contains the wire micron silicon carbide of 1wt%.In embodiment 1 the SEM figure of the silicon of electrolysis gained as shown in Figure 1, wherein, a of Fig. 1: * 10000 times; The b of Fig. 1: * 20000 times; The c of Fig. 1: * 90000 times.Silicon electrolytic process bath voltage changing conditions in embodiment 1 as shown in Figure 2.
Embodiment 2
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (55%) NaF (42%) AlF
3(3%) SiO
2Electrolysis temperature is 750 ℃; Take carbon as negative electrode, take alloy as inert anode, pole span is 2cm; Electrolytic current density is controlled at 0.2A/cm
2The electrolytic process bath voltage is steadily 1.4V, and electrolysis obtains silicon nanowires and silicon nanofiber, and purity reaches 99.2wt%.
Embodiment 3
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (60%) KF (38%) AlF
3(2%) SiO
2Electrolysis temperature is 800 ℃; Take carbon as cathode and anode, pole span is 2cm; Electrolytic current density is controlled at 0.5A/cm
2The electrolytic process bath voltage is steadily 1.4V, and electrolysis obtains silicon nanoparticle, and purity reaches 99.8wt%.
Embodiment 4
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (50%) NaF (8%) Na
2SiF
6(40%) AlF
3(2%) SiO
2Electrolysis temperature is 820 ℃; Take granular graphite as negative electrode, carbon is anode, pole span is 2cm; Keeping the cathode electrode current potential in electrolytic process is 1.0V (vs.Pt), and stablizing after-current density is 0.15A/cm
2, electrolysis obtains Si-C composite material, and wherein silicon is nanotube-shaped, and purity reaches 99.2wt%.
Embodiment 5
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (60%) NaF (38%) AlF
3(2%) SiO
2Electrolysis temperature is 800 ℃; Take Mo as negative electrode, carbon is anode, pole span is 2.5cm; Electrolytic current density is controlled at 0.5A/cm
2The electrolytic process bath voltage is steadily 1.5V, and electrolysis obtains silicon nanowires and nano silicon particles, and purity reaches 99.9wt%.
Embodiment 6
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (70%) NaF (22%) K
2SiF
6(4%) CaF
2(4%) SiO
2Electrolysis temperature is 840 ℃; Take Mo as negative electrode, carbon is anode, pole span is 5cm; Bath voltage is controlled at 1.8V.Electrolysis obtains micron silicon particle and micron silicon fiber, and purity reaches 99.3wt%.
Embodiment 7
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (50%) NaF (34%) AlF
3(5%) Al
2O
3(3%) NaCl (5%) CaCl
2(3%) SiO
2Electrolysis temperature is 820 ℃; Take Mo as negative electrode, carbon is anode, pole span is 5cm; Bath voltage is controlled at 2.2V.Electrolysis obtains 100nm～2 μ m silicon grains, and purity reaches 99.3wt%.
Embodiment 8
A kind of method that adopts fused salt electrolysis to produce silicon is characterized in that: molten salt system consists of (55%) KF (40%) AlF
3(5%) Al
2O
3Electrolysis temperature is 750 ℃; Take carbon as cathode and anode, pole span is 4cm; Bath voltage is controlled at 2.2V, and Si reduction is at negative electrode, removes negative electrode and removes Si impurity in fused salt.
Claims (9)
1. molten salt system that adopts fused salt electrolysis to produce silicon, it is characterized in that: this molten salt system consists of (x) A (y) AlF
3(z) SiO
2, wherein x is the mole percent level of A, y is AlF
3Mole percent level, z is SiO
2Mole percent level, x is that 25～77%, y is that 22～50%, z is 1～25%; A is by KF, NaF, K
2SiF
6, Na
2SiF
6, Al
2O
3, MgF
2, CaF
2, KCl, NaCl, MgCl
2, CaCl
2, LiCl, LiF, BaF
2Single or multiple salt form.
2. molten salt system that adopts fused salt electrolysis to produce silicon, it is characterized in that: this molten salt system consists of (x) A (y) AlF
3(z) SiO
2, wherein x is the mole percent level of A, y is AlF
3Mole percent level, z is SiO
2Mole percent level, x is that 25～99%, y is that 0～50%, z is 1～25%; A is by KF, NaF, K
2SiF
6, Na
2SiF
6, Al
2O
3, MgF
2, CaF
2, KCl, NaCl, MgCl
2, CaCl
2, LiCl, LiF, BaF
2Single or multiple salt form.
3. method that adopts fused salt electrolysis to produce silicon, it is characterized in that: adopt claim 1 or molten salt system claimed in claim 2 as the molten salt system of fused salt electrolysis, the electrolytic process negative electrode adopts carbon, Si or metal as cathode material, and anode adopts carbon or inert anode material; Electrolysis temperature is 500 ℃～1500 ℃; The pole span of negative electrode and anode is 0.1～45cm; Adopt the method for controlling electric current to carry out electrolysis, electrolytic current density is controlled at 0.01～5A/cm
2Or method that adopt to control voltage carries out electrolysis, adopt control flume voltage 0.1～30V or control cathode electropotential+3～-3V (vs.Pt) carries out electrolysis.
4. the method for silicon is produced in employing fused salt electrolysis according to claim 3, it is characterized in that: adopt carbon as cathode material, carbon adopts powder to press knot material, granulate material or bulk material.
5. the method for silicon is produced in employing fused salt electrolysis according to claim 3, it is characterized in that: adopt carbon as cathode material, carbon adopts particulate state or blocky graphite material, particulate state or block absorbent charcoal material or particulate state or block carbon filamentary material.
6. the method for silicon is produced in employing fused salt electrolysis according to claim 3, it is characterized in that: adopt Si as cathode material, the silicon negative electrode can adopt tabular, block or granular silicon single crystal, the silicon negative electrode also can adopt tabular, block or granular polysilicon.
7. the method for silicon is produced in employing fused salt electrolysis according to claim 3, it is characterized in that: molten salt system (x) A (y) AlF
3(z) SiO
2In SiO
2Be adopt electrolysis temperature in electrolytic process be 500 ℃～1500 ℃ directly with SiO
2Be dissolved in molten salt system.
8. the method for silicon is produced in employing fused salt electrolysis according to claim 3, it is characterized in that: the resulting silicon of electrolysis is one or more in the different morphologies of silicon grain, silicon line and silicone tube, and wherein the size range of silicon is 1nm～1000 μ m.
9. the employing fused salt electrolysis claimed in claim 3 application of producing the method for silicon, it is characterized in that: the method can be used for the removal of impurity silicon in fused salt in electrolysis of aluminum and other electrolytic etching of metal.
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Cited By (11)
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| CN105019015A (en) * | 2015-07-09 | 2015-11-04 | 上海大学 | Electrochemical preparation method of amorphous silica material |
| CN105714322A (en) * | 2014-12-04 | 2016-06-29 | 北京有色金属研究总院 | Electrochemical preparation method for silicon carbide nanotube |
| CN106356521A (en) * | 2016-10-17 | 2017-01-25 | 宁夏大学 | Amorphous SiO2 based cathode material and preparation method and application thereof |
| CN107002271A (en) * | 2015-10-27 | 2017-08-01 | 新日铁住金株式会社 | Plate the manufacture method of silicon metallic plate |
| CN109468655A (en) * | 2019-01-07 | 2019-03-15 | 东北大学 | A kind of method of electrolytic preparation silicon in molten salt system |
| CN109763134A (en) * | 2018-12-27 | 2019-05-17 | 国联汽车动力电池研究院有限责任公司 | The preparation method of porous silicon |
| CN110629241A (en) * | 2019-09-16 | 2019-12-31 | 上海大学 | Silicon material manufacturing method |
| CN112144068A (en) * | 2020-08-06 | 2020-12-29 | 浙江工业大学 | System for synthesizing silicon nanofibers through in-situ electrocatalysis molten salt electrolysis by diaphragm method |
| CN113991082A (en) * | 2021-10-27 | 2022-01-28 | 昆明理工大学 | Method for preparing silicon-carbon cathode material of lithium ion battery from silica fume |
| CN117230459A (en) * | 2023-11-13 | 2023-12-15 | 中国科学院广州地球化学研究所 | In-situ preparation method and device of silicon-based nano-micron material |
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| CN103882465A (en) * | 2014-03-05 | 2014-06-25 | 江苏华富储能新技术股份有限公司 | Preparation method and application of high-purity nanometer silicon |
| CN105714322A (en) * | 2014-12-04 | 2016-06-29 | 北京有色金属研究总院 | Electrochemical preparation method for silicon carbide nanotube |
| CN105714322B (en) * | 2014-12-04 | 2017-10-10 | 北京有色金属研究总院 | A kind of electrochemical preparation method of Sic nanotube |
| CN105019015A (en) * | 2015-07-09 | 2015-11-04 | 上海大学 | Electrochemical preparation method of amorphous silica material |
| CN107002271A (en) * | 2015-10-27 | 2017-08-01 | 新日铁住金株式会社 | Plate the manufacture method of silicon metallic plate |
| CN106356521A (en) * | 2016-10-17 | 2017-01-25 | 宁夏大学 | Amorphous SiO2 based cathode material and preparation method and application thereof |
| CN109763134A (en) * | 2018-12-27 | 2019-05-17 | 国联汽车动力电池研究院有限责任公司 | The preparation method of porous silicon |
| CN109468655A (en) * | 2019-01-07 | 2019-03-15 | 东北大学 | A kind of method of electrolytic preparation silicon in molten salt system |
| CN110629241A (en) * | 2019-09-16 | 2019-12-31 | 上海大学 | Silicon material manufacturing method |
| CN110629241B (en) * | 2019-09-16 | 2021-06-22 | 上海大学 | Silicon material manufacturing method |
| CN112144068A (en) * | 2020-08-06 | 2020-12-29 | 浙江工业大学 | System for synthesizing silicon nanofibers through in-situ electrocatalysis molten salt electrolysis by diaphragm method |
| CN112144068B (en) * | 2020-08-06 | 2022-01-18 | 浙江工业大学 | System for synthesizing silicon nanofibers through in-situ electrocatalysis molten salt electrolysis by diaphragm method |
| CN113991082A (en) * | 2021-10-27 | 2022-01-28 | 昆明理工大学 | Method for preparing silicon-carbon cathode material of lithium ion battery from silica fume |
| CN113991082B (en) * | 2021-10-27 | 2024-04-16 | 昆明理工大学 | Method for preparing silicon-carbon negative electrode material of lithium ion battery by using silica fume |
| CN117230459A (en) * | 2023-11-13 | 2023-12-15 | 中国科学院广州地球化学研究所 | In-situ preparation method and device of silicon-based nano-micron material |
| CN117230459B (en) * | 2023-11-13 | 2024-02-13 | 中国科学院广州地球化学研究所 | In-situ preparation method and device of silicon-based nano-micron material |
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