CN105154905A - Method for electrodeposition preparation of monatomic silicon from poly-silicon industry by-product based on ionic liquids - Google Patents
Method for electrodeposition preparation of monatomic silicon from poly-silicon industry by-product based on ionic liquids Download PDFInfo
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Abstract
The invention discloses a method for electrodeposition preparation of monatomic silicon from a poly-silicon industry by-product based on ionic liquids. The method comprises the following steps: in an inert atmosphere, mixing the poly-silicon industry by-product with one or more ionic liquid solvents and one or two additives for dissolution according to a mass ratio of 1:(0.3-0.9):(5-12); carrying out electrodeposition at 0-45 DEG C to obtain a silicon product, wherein an electrode system of which the cathode is a 316 stainless steel plate, a gold plated plate, or an ITO/PEN or ITO/PET flexible electrode, and the anode is a platinum plate or high-purity graphite is adopted, the current density of electrodeposition is controlled to be 60-150 A/m<2>, the distance between polar plates is 20-50 cm, the current efficiency of the silicon product is 50% or higher, and the product purity can reach 98% or higher according the analysis result of an EDX. The method has the advantages that a solution obtained after electrolysis can be recycled, the defect in resource recycling of the poly-silicon industry by-product can be overcome, the production cost is reduced, and the prepared monatomic silicon can be utilized for production of solar photovoltaic cells.
Description
Technical field
The present invention relates to a kind of innoxious, recycling processing method of polysilicon industry by product trichlorosilane/silicon tetrachloride, a kind of particularly method preparing elemental silicon based on ionic liquid electrodeposition.
Background technology
Along with the development of global photovoltaic industry, domestic polysilicon industry also achieves and develops rapidly, according to statistics, 2011, China's polysilicon output reaches 8.2 ten thousand t, occupy first place in the world, tentatively solve heavy dependence import and restrict the problem of China's theCourse of PV Industry, having established the basis of theCourse of PV Industry.By 2012, domestic polysilicon production capacity about 180,000 t/, inner digestion 14.3 ten thousand t/, once the production capacity of down-stream enterprise tentatively discharges, the consumption of polysilicon just will reach more than 20 ten thousand t/.At present, domestic production polysilicon many employings improved Siemens, this kind of production method often produces the silicon tetrachloride as by-product that 1t polysilicon will produce about 10 ~ 15t, if the core technology recycled is not up to standard, to safety and environmental hazard very large, also be that the one of resource is wasted simultaneously, therefore, carry out the recovery and utilization technology of this by product significant in environmental sound, changing waste into resources etc.
Current, in the world to SiCl
4treatment process mainly contain two kinds: one utilizes SiCl
4the thermal silica, organosilicon product etc. of production high added value; Another kind carries out hydrogenation to silicon tetrachloride under certain condition, thus be converted into the main raw material SiHCl preparing polysilicon
3.
Nineteen forty-two, first Harry Kloepfer has applied for Aerosil(gas-phase silica) production patent, SiCl
4at H
2and O
2in continuous flame, pyrohydrolysis prepares gas-phase silica.Gas-phase silica technology difficulties is synthetic furnace heat radiation, efficient cyclone manipulation and HCl desorb 3 aspects.SiCl
4prepare gas-phase silica Technology complicated, need the condition of high temperature, high pressure, equipment investment is comparatively large, from the viewpoint of economic benefit, market capacity etc., and also can only transform portion by product SiCl
4, fundamentally can not solve SiCl
4overstock problem.
SiCl
4can also other useful organosilicon product be prepared by series reaction such as alcoholysis, hydrolysis, assorted contractings and reclaim HCl.Industrial, its prior synthesizing method is batch technology, and reaction and rectifying are separately carried out, and industrial scale is little, poor product quality, and raw material availability is low, is unfavorable for that its large-scale industrial production is applied.
Under certain condition, SiCl
4with H
2can reduce and prepare trichlorosilane (SiHCl
3), the hydrogenation process of silicon tetrachloride mainly contains following several, traditional silica flour and hydrogen reduction method adopt copper base or ferrum-based catalyst, under the condition of 400 ~ 800 DEG C and 2 ~ 4MPa, are the raw material trichlorosilane producing polysilicon in fluidized-bed reactor by converting silicon tetrachloride.This Technology is more ripe, but comparatively harsh to the requirement of equipment, and this mainly due to reduction furnace internal pressure greatly and temperature is higher, exists larger security risk simultaneously; Hot hydrogenation utilizes hydrogen that silicon tetrachloride reduction is generated trichlorosilane, and adopt graphite rod as heating material in reducer, in electrically heated mode, reactor temperature is maintained about 1250 DEG C, the pressure in reactor is at 0.25 ~ 0.40MPa.Owing to adopting graphite as heating material, at high temperature graphite may react with silicon tetrachloride and hydrogen, generates chloroparaffin, if be not exclusively separated, will affect the quality of polysilicon product; Plasma hydrogenization technology is produced with hydrogenation of silicon tetrachloride at plasma technology application, in this technique, the yield of trichlorosilane is far away higher than other hydrogenation treatment method, but, what this technique adopted is radio-frequency plasma, due to the restriction by radio-frequency plasma power, cause temporarily realizing industrialized amplification and produce.
Li Yaqiong (" ionic liquid electrodeposition prepares the research of elemental silicon ", Northeastern University's master thesis, 2009) selects high-purity ionic liquid 1-butyl-3-methyl imidazolium fluoroform sulphonate as solvent, and high purity silicon tetrachloride is the galvanic deposit that silicon is carried out in silicon source.
Summary of the invention
For innoxious, the resource utilization difficult problem of current polysilicon by-product trichlorosilane/silicon tetrachloride, the object of the invention is to propose a kind of green, environmental protection prepare the method for elemental silicon based on ionic liquid galvanic deposit from polysilicon industry by product.
In the present invention, the bath deposition elemental silicon product that the efficient ionic liquid electrolysis of application clean environment firendly is silicon source with polysilicon industry by product trichlorosilane/silicon tetrachloride.Ionic liquid has the advantages such as higher stability, preferably solvability, lower vapour pressure and wider electrochemical window as " planner's solution ", desirable electrolytic solution, the semiconductor material that cannot deposit at the aqueous solution or other organic electrolyte can be obtained in ionic liquid, and ionic liquid electrodeposition method is flexibly easy, pattern and the size of semiconductor material can be controlled.The actual by product of the polysilicon industry in the present invention contains Multiple components, comprise the chloride impurities such as trichlorosilane, silicon tetrachloride and Fe, Cu, Mn, V, therefore need the ion liquid dissolving of the actual by product setting up applicable polysilicon industry, galvanic deposit system and processing method, control dissolving and the precipitation of impurity.
Technical scheme of the present invention is specifically described as follows.
Prepare a method for elemental silicon based on ionic liquid galvanic deposit from polysilicon industry by product, concrete steps are as follows:
1. in glove box, prepare electrolytic solution, stir after preparation for subsequent use; Wherein: described electrolytic solution is by ionic liquid, polycrystalline
Silicon industry by product and additive 1:(0.3-0.9 in mass ratio): (5 ~ 12) mixture forms, and described ionic liquid is selected from two fluoroform sulfimide salt ([Dmim] NTf of 1,3-methylimidazole
2), two fluoroform sulfimide salt ([Emim] NTf of 1-ethyl-3-methylimidazole
2), two fluoroform sulfimide salt ([Pmim] OTf of 1-propyl group-3-methyl
2), two fluoroform sulfimide salt ([Bmim] NTf of 1-butyl-3-Methylimidazole
2), any one or a few in 1-ethyl-3-methylimidazole trifluoro-methanyl sulfonate ([Emim] OTf); Described additive is selected from any one or two kinds in acetonitrile or propylene carbonate (PC);
2. build electrode system, its negative electrode be in 316 stainless steel plates, coated plate, ITO/PEN or ITO/PET flexible electrode any one, anode is platinum plate or high purity graphite;
3. carry out galvanic deposit chemical reaction, obtain elemental silicon; Wherein, in electrochemical reaction process, controlling current density is
60 ~ 150A/m
2, polar plate spacing is 20cm ~ 50cm, and electrodeposition time is 30min ~ 120min.
Above-mentioned steps 1. in, in described polysilicon industry by product, silicon tetrachloride and trichlorosilane accounting reach 95wt%, simultaneously containing impurity metallic elements.
Above-mentioned steps 1. before, polysilicon industry by product first through removal of impurities process, to get rid of the interference to electrochemical reaction in treating processes.Preferably, described removal of impurities process comprises heats polysilicon industry by product, makes it overflow to enter into the container of ionic liquid; And ionic liquid absorption is saturated afterwards, heating makes the muriate of silicon overflow, and use another container collection, and the impurity in by product is blocked on two steps in ionic liquid.
Above-mentioned steps 3. in temperature be 0 ~ 45 DEG C, stir speed (S.S.) is 20r/min ~ 80r/min.Adopt lesser temps in the present invention, the volatilization in controllable silicon source is conducive to being dissolved in ionic liquid, also has good electrodeposition effect at a lower temperature simultaneously.
Above-mentioned steps 3. after, also comprise the electrolytic solution that electrolysis completes and continue to dissolve polysilicon industry by product, repeat step operation 1., 2. and 3., deposition obtains the step of elemental silicon again.
Beneficial effect of the present invention is: utilize green, pollution-free, less energy-consumption, the ionic liquid electrolysis under certain condition trichlorosilane/silicon tetrachloride that can be recycled obtains elemental silicon, by the control to ion liquid dissolving system and electrochemical process, available silicon product can reach the requirement of industrial production raw material, avoid the impact of impurity in polysilicon industry by product, thus realize high level resource utilization and the harmless treatment of polysilicon industry by product.Meanwhile, this processing method is easy and simple to handle, moderate cost, environment-friendly high-efficiency, is suitable for suitability for industrialized production application.
Accompanying drawing explanation
Fig. 1 a kind ofly prepares the process flow diagram of elemental silicon based on ionic liquid galvanic deposit from polysilicon industry by product.
Fig. 2 is the pretreatment process schematic diagram of polysilicon industry by product.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.Below in conjunction with drawings and Examples, technical solution of the present invention is described in detail.
In the embodiment of the present invention, prepare the process flow diagram of elemental silicon as shown in Figure 1 based on ionic liquid galvanic deposit from polysilicon industry by product.
In the embodiment of the present invention, first by the metal ion in ion liquid dissolving polysilicon industry by product and other impurity, to get rid of the interference to electrochemical reaction in treating processes, concrete steps are as follows: 1, heat by product, make it overflow to be connected with the container of ionic liquid; 2, ionic liquid is filled in container, the by product produced by step 1 continues to pass into ionic liquid, made the muriate effusion container of silicon by heating after ionic liquid absorption is saturated, other impurity such as the heavy metal in by product can be made to be blocked in ionic liquid simultaneously, and don't introduce the purifying of other impurity realization to by product; 3, the container collection sealing of the by product after purifying is preserved, as the silicon source of preparation electrolytic solution.
Embodiment 1
It is that below 50ppm and dew point have rare gas element N at below 30ppm that the desired raw materials such as 1. dried in vacuum drying oven ionic liquid put into oxygen level
2or Ar
2in the glove box of filling, with for subsequent use;
2. the electrolytic solution that accurate formulation is silicon source with polysilicon industry by product in glove box, with two fluoroform sulfimide salt ([Dmim] NTf of ionic liquid 1,3-methylimidazole
2) and the mass ratio of polysilicon industry by product and additive acetonitrile be 1:0.6:8 preparation, stir after preparation for subsequent use;
3. under 30 DEG C of conditions, stir electrolytic solution with the speed of 50r/min, build with ITO/PET flexible electrode for negative electrode, platinum plate is the electrode system of anode;
4. the current density in electrolytic process processed is 60A/m
2, cathode-anode plate spacing is 20cm, and deposition 60min obtains elementary silicon,
Carry out SEM sign to product, regular appearance, meet the requirements, it is 98.33% that EDX records its purity, and current efficiency reaches 50.2%;
5. the electrolytic solution that electrolysis completed continues the muriate of dissolves silicon, depositing silicon product again, last deposit the silicon product obtained and can be used as industrial production raw material.
Embodiment 2
1. the desired raw materials such as ionic liquid dried in vacuum drying oven being put into oxygen level is that below 50ppm and dew point exist
Below 30ppm has rare gas element N
2or Ar
2in the glove box of filling, with for subsequent use;
2. the electrolytic solution that accurate formulation is silicon source with polysilicon industry by product in glove box, with ionic liquid 1-ethyl-3-methyl
The mass ratio of azoles trifluoro-methanyl sulfonate ([Emim] OTf) and polysilicon industry by product and additive acetonitrile is 1:0.7:8 preparation, stirs for subsequent use after preparation;
3. under 30 DEG C of conditions, stir electrolytic solution with the speed of 50r/min, build with ITO/PET flexible electrode for negative electrode, platinum plate is the electrode system of anode;
4. the current density controlled in electrolytic process is 60A/m
2, cathode-anode plate spacing is 20cm, and deposition 60min obtains elementary silicon,
Carry out SEM sign to product, regular appearance, meet the requirements, it is 98.02% that EDX records its purity, and current efficiency reaches 53.2%;
5. the electrolytic solution that electrolysis completed continues the muriate of dissolves silicon, depositing silicon product again, last deposit the silicon product obtained and can be used as industrial production raw material.
Embodiment 3
1. the desired raw materials such as ionic liquid dried in vacuum drying oven being put into oxygen level is that below 50ppm and dew point exist
Below 30ppm has rare gas element N
2or Ar
2in the glove box of filling, with for subsequent use;
2. the electrolytic solution that accurate formulation is silicon source with polysilicon industry by product in glove box, with ionic liquid 1-ethyl-3-methyl
The mass ratio of imidazolium trifluoromethane sulfonate ([Emim] OTf) and polysilicon industry by product and additive propylene carbonate is 1:0.3:10 preparation, stirs for subsequent use after preparation;
3. under 30 DEG C of conditions, stir electrolytic solution with the speed of 50r/min, build with ITO/PET flexible electrode for negative electrode, platinum plate
For the electrode system of anode;
4. the current density controlled in electrolytic process is 60A/m
2, cathode-anode plate spacing is 20cm, and deposition 60min obtains elementary silicon,
Carry out SEM sign to product, regular appearance, meet the requirements, it is 98.50% that EDX records its purity, and current efficiency reaches 55.0%;
5. the electrolytic solution that electrolysis completed continues the muriate of dissolves silicon, depositing silicon product again, last deposit the silicon product obtained and can be used as industrial production raw material.
Embodiment 4
Oxygen level put into by the required reagent such as 1. dried in vacuum drying oven ionic liquid is that below 50ppm and dew point have rare gas element N at below 30ppm
2or Ar
2in the glove box of filling, with for subsequent use;
2. the electrolytic solution that accurate formulation is silicon source with polysilicon industry by product in glove box, be 1:0.6:8 preparation with the mass ratio of ionic liquid 1-ethyl-3-methylimidazole trifluoro-methanyl sulfonate ([Emim] OTf) and polysilicon industry by product and additive acetonitrile, stir after preparation for subsequent use;
3. under 0 DEG C of condition, stir electrolytic solution with the speed of 80r/min, building with coated plate is negative electrode, and platinum plate is the electrode system of anode;
4. be working power with high-power DC power supply, the current density controlled in electrolytic process is 60A/m
2, cathode-anode plate spacing is 20cm, and deposition 60min obtains elementary silicon, and carry out SEM sign to product, regular appearance, meet the requirements, it is 98.60% that EDX records its purity, and current efficiency reaches 53.2%;
5. the electrolytic solution that electrolysis completed continues the muriate of dissolves silicon, depositing silicon product again, last deposit the silicon product obtained and can be used as industrial production raw material.
Embodiment 5
Oxygen level put into by the required reagent such as 1. dried in vacuum drying oven ionic liquid is that below 50ppm and dew point have rare gas element N at below 30ppm
2or Ar
2in the glove box of filling, with for subsequent use;
2. the electrolytic solution that accurate formulation is silicon source with polysilicon industry by product in glove box, be 1:0.6:8 preparation with the mass ratio of ionic liquid 1-ethyl-3-methylimidazole trifluoro-methanyl sulfonate ([Emim] OTf) and polysilicon industry by product and additive acetonitrile, stir after preparation for subsequent use;
3. under 30 DEG C of conditions, stir electrolytic solution with the speed of 50r/min, building with coated plate is negative electrode, and high purity graphite is the electrode system of anode;
4. the current density controlled in electrolytic process is (60A/m
2), cathode-anode plate spacing is 20cm, and bath voltage is 3.8V, and deposition 60min obtains elementary silicon, and carry out SEM sign to product, regular appearance, meet the requirements, it is 98.80% that EDX records its purity, and current efficiency reaches 55.0%;
5. the electrolytic solution that electrolysis completed continues the muriate of dissolves silicon, depositing silicon product again, last deposit the silicon product obtained and can be used as industrial production raw material.
Embodiment 6
1. required for ionic liquid dried in vacuum drying oven etc. reagent being put into oxygen level is that below 50ppm and dew point have rare gas element N at below 30ppm
2or Ar
2in the glove box of filling, with for subsequent use;
2. the electrolytic solution that in glove box, accurate formulation is silicon source with polysilicon industry by product, with ionic liquid 1-ethyl-3-methyl miaow
The mass ratio of azoles trifluoro-methanyl sulfonate ([Emim] OTf) and polysilicon industry by product and additive acetonitrile is 1:0.9:8 preparation, stirs for subsequent use after preparation;
3. under 30 DEG C of conditions, stir electrolytic solution with the speed of 50r/min, building with coated plate is negative electrode, and platinum plate is the electrode system of anode;
4. the current density in electrolytic process processed is 80A/m
2, cathode-anode plate spacing is 30cm, and deposition 120min obtains elementary silicon,
Carry out SEM sign to product, regular appearance, meet the requirements, it is 98.50% that EDX records its purity, and current efficiency reaches 52.5%;
5. the electrolytic solution that electrolysis completed continues the muriate of dissolves silicon, depositing silicon product again, last deposit the silicon product obtained and can be used as industrial production raw material.
Embodiment 7
With Li Yaqiong, (described in " ionic liquid electrodeposition prepares the research of elemental silicon ", optimal conditions carries out contrast experiment, and only analytical pure silicon tetrachloride is replaced with polysilicon industry by product in experiment, other condition remains unchanged.
1. the desired raw materials such as ionic liquid dried in vacuum drying oven being put into oxygen level is that below 50ppm and dew point have rare gas element N at below 30ppm
2or Ar
2in the glove box of filling, with for subsequent use;
2. the electrolytic solution that accurate formulation is silicon source with polysilicon industry by product in glove box, with ionic liquid 1-butyl-3-methyl
The mol ratio of imidazolium trifluoromethane sulfonate ([Bmim] OTf) and polysilicon industry by product and additive propylene carbonate is 1:1:4.2 preparation, stirs for subsequent use after preparation;
3. react under 40 DEG C of conditions, build with titanium plate for negative electrode, graphite is the electrode system of anode;
4. the current density controlled in electrolytic process is 22A/m
2, galvanic deposit 180min.
SEM observation is carried out to electrodeposit reaction pole plate, has no surface deposition silicon product; XPS analysis is carried out to it, also has no the spectrogram identical with silicon, show that this system is not suitable for the galvanic deposit of polysilicon industry by product.
Claims (6)
1. prepare a method for elemental silicon based on ionic liquid galvanic deposit from polysilicon industry by product, it is characterized in that, concrete steps are as follows:
1. in glove box, prepare electrolytic solution, stir after preparation for subsequent use; Wherein: described electrolytic solution is by ionic liquid, polycrystalline
Silicon industry by product and additive 1:(0.3-0.9 in mass ratio): (5 ~ 12) mixture forms, described ionic liquid be selected from the two fluoroform sulfimide salt of 1,3-methylimidazole, the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, the two fluoroform sulfimide salt of 1-propyl group-3-methyl, the two fluoroform sulfimide salt of 1-butyl-3-Methylimidazole, 1-ethyl-3-methylimidazole trifluoro-methanyl sulfonate any one or a few; Described additive is selected from any one or two kinds in acetonitrile or propylene carbonate;
2. build electrode system, its negative electrode be in 316 stainless steel plates, coated plate, ITO/PEN or ITO/PET flexible electrode any one, anode is platinum plate or high purity graphite;
3. carry out galvanic deposit chemical reaction, obtain elemental silicon; Wherein, in electrochemical reaction process, controlling current density is
60 ~ 150A/m
2, polar plate spacing is 20cm ~ 50cm, and electrodeposition time is 30min ~ 120min.
2. method according to claim 1, is characterized in that, step 1. in, in described polysilicon industry by product, silicon tetrachloride and trichlorosilane accounting reach 95wt%, simultaneously containing impurity metallic elements.
3. method according to claim 1, is characterized in that, step 1. before, polysilicon industry by product is first through removal of impurities process.
4. method according to claim 3, is characterized in that, described removal of impurities process comprises heats polysilicon industry by product, makes it overflow to enter into the container of ionic liquid; And ionic liquid absorption is saturated afterwards, heating makes the muriate of silicon overflow, and use another container collection, and the impurity in by product is blocked on two steps in ionic liquid.
5. method according to claim 1, is characterized in that, step 3. in electrochemical reaction process in, temperature is 0 ~ 45 DEG C, and stir speed (S.S.) is 20r/min ~ 80r/min.
6. method according to claim 1, is characterized in that, step 3. after, also comprise the electrolytic solution that electrolysis completes and continue to dissolve polysilicon industry by product, repeat step operation 1., 2. and 3., deposition obtains the step of elemental silicon again.
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Cited By (2)
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| CN110745831A (en) * | 2019-11-14 | 2020-02-04 | 李龙飞 | Method and device for removing impurities from silicon tetrachloride |
| CN114318456A (en) * | 2022-01-17 | 2022-04-12 | 桐乡市思远环保科技有限公司 | Method for electrodepositing silicon film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110745831A (en) * | 2019-11-14 | 2020-02-04 | 李龙飞 | Method and device for removing impurities from silicon tetrachloride |
| CN110745831B (en) * | 2019-11-14 | 2021-09-10 | 李龙飞 | Method and device for removing impurities from silicon tetrachloride |
| CN114318456A (en) * | 2022-01-17 | 2022-04-12 | 桐乡市思远环保科技有限公司 | Method for electrodepositing silicon film |
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