CN102344143B - Physical purification method and device of metallic silicon - Google Patents
Physical purification method and device of metallic silicon Download PDFInfo
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- CN102344143B CN102344143B CN 201110216669 CN201110216669A CN102344143B CN 102344143 B CN102344143 B CN 102344143B CN 201110216669 CN201110216669 CN 201110216669 CN 201110216669 A CN201110216669 A CN 201110216669A CN 102344143 B CN102344143 B CN 102344143B
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- 238000000746 purification Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title abstract description 19
- 229910052710 silicon Inorganic materials 0.000 title abstract description 9
- 239000010703 silicon Substances 0.000 title abstract description 9
- 239000012159 carrier gas Substances 0.000 claims abstract description 29
- 230000005284 excitation Effects 0.000 claims abstract description 18
- 239000002210 silicon-based material Substances 0.000 claims abstract description 18
- 230000004888 barrier function Effects 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000004064 recycling Methods 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 235000013312 flour Nutrition 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 16
- 239000002245 particle Substances 0.000 abstract description 13
- 239000007789 gas Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 2
- 229920005591 polysilicon Polymers 0.000 abstract description 2
- 239000011863 silicon-based powder Substances 0.000 abstract 3
- 239000002184 metal Substances 0.000 abstract 1
- 210000002381 plasma Anatomy 0.000 description 25
- 239000011856 silicon-based particle Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- 239000012535 impurity Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 230000005495 cold plasma Effects 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
本发明涉及本发明涉及太阳能级多晶硅料的提纯技术领域，特别是一种金属硅的物理提纯方法及其设备，包括流化床、进料系统、等离子激励电源以及收料和气体循环装置，在流化床内采用介质阻挡放电的方法作为等离子的产生方式，用流化床对硅粉进行预热和传输，用硅粉粒度、载气预热温度和载气流速对颗粒平均处理时间进行控制，用载气预热温度、载气的气氛种类和介质阻挡放电的等离子激励电源功率对纯化效果进行控制，在流动过程中对约束在等离子体中的硅粉实现纯化，最终将提纯后的硅料从流化床末端产出。本发明的有益效果是：可以在常压和近常压的条件下提纯硅料，用于提纯的离子密度高，能量大，提纯效率高，成本低。
The present invention relates to the technical field of purification of solar-grade polysilicon materials, in particular to a physical purification method and equipment for metal silicon, including a fluidized bed, a feeding system, a plasma excitation power supply, and a material receiving and gas circulation device. The dielectric barrier discharge method is used as the plasma generation method in the fluidized bed, and the silicon powder is preheated and transported by the fluidized bed, and the average treatment time of the particles is controlled by the particle size of the silicon powder, the preheating temperature of the carrier gas and the velocity of the carrier gas. , the purification effect is controlled by the preheating temperature of the carrier gas, the type of atmosphere of the carrier gas, and the plasma excitation power of the dielectric barrier discharge. During the flow process, the silicon powder confined in the plasma is purified, and finally the purified silicon is The material is output from the end of the fluidized bed. The beneficial effects of the invention are: the silicon material can be purified under the condition of normal pressure or near normal pressure, the ion density used for purification is high, the energy is large, the purification efficiency is high, and the cost is low.
Description
Technical field
The present invention relates to the physical purification method and the equipment thereof in the purification techniques field, particularly a kind of Pure Silicon Metal of solar-grade polysilicon material.
Background technology
Crystalline silicon is to use solar cell material the most widely at present, and the solar energy level silicon material of main flow all adopts the Siemens Method preparation.For reducing material cost, there is several different methods that low-cost silicon material such as metalluragical silicon are handled at present, make it purity near 6N, meet the purity requirement of silicon solar cell, be respectively:
1. pyrocarbon one silicon and aluminium one Si reduction purification technique;
2. segregation effect of insulated grid oxidation purifying metalluragical silicon when utilizing crystallization;
3. pickling purification technique;
4. slagging scorification purification technique;
5. air-blowing and evaporation purification technique;
6. photoglow produces the cold plasma purification technique.
The pickling purification technique can carry out at normal temperatures, but its processing efficiency and effect are limited, generally handles the auxiliary of means as other;
Photoglow produces the cold plasma purification technique and also can handle at a lower temperature, (is lower than 10 but its ion density is low
10), ion energy little (less than 1eV), treatment effect is limited, in addition, its hypobaric working conditions has limited its material and has transported;
Other several methods all relate to the thawing of silicon material, need the pyroprocessing more than 1400 ℃.
Summary of the invention
Technical problem to be solved by this invention is: a kind of physical purification method and equipment thereof of Pure Silicon Metal are provided, reduce the purification difficulty, improve purification efficiency.
The present invention solves the scheme that its technical problem adopts: a kind of physical purification method of Pure Silicon Metal; The method that in fluidized-bed, adopts dielectric barrier discharge is as isoionic producing method; With fluidized-bed silica flour is carried out preheating and transmission; With silicon particle size, carrier gas preheating temperature and flow rate of carrier gas the particle average handling time is controlled; With the atmosphere kind of carrier gas preheating temperature, carrier gas and the plasma excitation power supply power of dielectric barrier discharge purification effect is controlled, in flow process, the silica flour that constrains in the plasma body is realized purifying, the silicon material after purifying the most at last is from the terminal output of fluidized-bed.
Concrete steps are following:
1) fluidized-bed integral body is evacuated to 1mTorr;
2) feed the carrier gas that is preheated to design temperature from grid distributor, and control flow velocity and adjusting pressure;
3) treat steady air current after, open the plasma excitation power supply and produce plasma, regulate the pressure of feed system and rewinding and gas-recycling plant, it is mobile that the flow field is produced, after flow velocity reached set(ting)value, feed system began continuous charging;
4) through regulating silicon particle size, carrier gas preheating temperature and flow rate of carrier gas, control particle mean residence time;
5) recycling finishes from rewinding and gas-recycling plant silicon and gas.
Carrier gas is main with rare gas element mainly, according to different impurities, selects to feed H
2, HCl, O
2In these three kinds of function gases a kind of, two kinds or all.
The median size of silicon particle size≤50 μ m.
The plasma excitation power supply is 5kV to a 10kV sine ac power supply, and the frequency of sine ac power supply is 200Hz～20kHz.
The plasma excitation power supply is a nanosecond pulse power supply.
The carrier gas preheating temperature is 800 ℃-1000 ℃.
According to the situation of silicon material itself, can implement multistage purification or repeat purification.
A kind of equipment for purifying comprises fluidized-bed, feed system, plasma excitation power supply and rewinding and gas-recycling plant, and fluidized-bed comprises grid distributor and bed body; The bed body is the closed environment of vacuum-pumping, and bed body internal surface applies the dielectric of low-k, and the parallel pole of parallel dislocation is set in the bed body; Make fluid pass plasma area with the S type, its surface-coated high-dielectric coefficient coating insulate between parallel pole and bed body; On parallel pole, add the plasma excitation power supply, between parallel pole, form dielectric barrier discharge, form plasma; The front end of fluidized-bed connects feed system, terminal rewinding and the gas-recycling plant of connecting, and carrier gas gets into the bed body through grid distributor; Silica flour gets into fluidized-bed through feed system and carries out purifying, and the silicon material after the purification is from terminal rewinding and the gas-recycling plant of getting into of fluidized-bed.
Particularly, parallel pole has three, horizontal each other parallel misalignment, and fluidized material can flow through the parts transversely S type of dislocation.
The invention has the beneficial effects as follows: can be under normal pressure and nearly non-pressurized condition the purified silicon material, the ion density that is used to purify is high, energy is big, purification efficiency is high, cost is low.Under normal pressure and nearly non-pressurized condition, dielectric barrier discharge can generate energy density reach 10 under multiple atmosphere
14Cm
-3Ion density, than high 4 to 5 one magnitude of common glow discharge plasma.In addition, its electronics average energy can reach more than the 10eV.In addition, normal pressure and nearly non-pressurized air pressure make the gas phase particle transport and become feasible.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified;
Fig. 1 is the front view of fluidized-bed of the present invention;
Fig. 2 is the vertical view of fluidized-bed of the present invention;
Among the figure, 1. feed system; 2. rewinding and gas-recycling plant; 3. grid distributor; 4. parallel pole; The bed body; 6. plasma excitation power supply.
Embodiment
A kind of physical purification method of Pure Silicon Metal; The method that in fluidized-bed, adopts dielectric barrier discharge is as isoionic producing method; (10000Pa is to normal pressure) carries out preheating and transmission with fluidized-bed to silica flour under the nearly normal pressure of atmosphere; With silicon particle size, carrier gas preheating temperature and flow rate of carrier gas the particle average handling time is controlled; Power with the plasma excitation power supply 6 of the atmosphere kind of carrier gas preheating temperature, carrier gas and dielectric barrier discharge is controlled purification effect, in flow process, the silica flour that constrains in the plasma body is realized purifying, and the silicon material after purifying the most at last is from the terminal output of fluidized-bed.
Concrete steps are following:
1) fluidized-bed integral body is evacuated to 1mTorr;
2) feed the carrier gas that is preheated to design temperature from grid distributor 3, and control flow velocity and adjusting pressure;
3) treat steady air current after, open plasma excitation power supply 6 and produce plasmas, regulate the pressure of feed system 1 and rewinding and gas-recycling plant 2, the flow field is produced flows, after flow velocity reached set(ting)value, feed system 1 began continuous charging;
4) through regulating silicon particle size, carrier gas preheating temperature and flow rate of carrier gas, control particle mean residence time;
5) recycling finishes from rewinding and gas-recycling plant 2 silicon and gas.
Carrier gas is main with rare gas element mainly, according to different impurities, selects to feed H
2, HCl, O
2In these three kinds of function gases a kind of, two kinds or all, wherein, H
2, the H ion that produces of HCl can remove P, B impurity in the silicon material.Cl, O ion can be removed the transition metal in the silicon material.
The median size of silicon particle size≤50 μ m.
Plasma excitation power supply 6 is 5kV to a 10kV sine ac power supply, and the frequency of sine ac power supply is 200Hz～20kHz.
For improving the yield of plasma high energy part, can replace sine-wave power with nanosecond pulse power supply.
The carrier gas preheating temperature is 800 ℃-1000 ℃.
According to the situation of silicon material itself, can implement multistage purification or repeat purification.
The equipment of dielectric barrier discharge is formed with common glow discharge device similar, and difference is block media and the excitation power supply between the parallel capacitance plate.This kind parallel capacitance plate discharge electrode can realize in a variety of forms that the present invention adopts the electric capacity flat board of dislocation as electrode, makes fluid pass plasma area with the S type.
Illustrated in figures 1 and 2, this equipment for purifying comprises fluidized-bed, feed system 1, plasma excitation power supply 6 and rewinding and gas-recycling plant 2, and fluidized-bed comprises grid distributor 3 and bed body 5, selects the grid distributor 3 of different percentage of open area according to particle grain size.The preheating carrier gas gets into bed body 5 through grid distributor 3, has dragged particle at last and has formed fluid.
The front end of fluidized-bed connects feed system 1; Terminal rewinding and the gas-recycling plant 2 of connecting; Carrier gas gets into bed body 5 through grid distributor 3, and silica flour gets into fluidized-bed through feed system 1 and carries out purifying, and the silicon material after the purification is from terminal rewinding and the gas-recycling plant 2 of getting into of fluidized-bed.
Embodiment 1:
Elder generation is evacuated to 1mTorr with the base vacuum of system in the present embodiment, feeds the carrier gas (Ar:H that comprises function gas then
2: HCl=98:1:1), the gas preheating temperature is 900 ℃.Regulate pressure to normal pressure, then system is applied the sine ac power supply of voltage 4kV, frequency 10kHz.Behind the discharge stability, load pending silicon material with carrier gas to system through feed system 1.Among the embodiment, silicon material powder is heated to 900 ℃ with the carrier gas meeting, is beneficial to the carrying out of solid phase diffusion in the particle.Particle median size 50 μ m.The mean residence time of particle in device is 1h, according to the situation of silicon material itself, can implement multistage purification or repeat purification.
Embodiment 2:
Present embodiment is under relatively low vacuum tightness (10
4Pa) implement experimental program, need, otherwise average handling time can corresponding shortening the refinement of further silicon material particle diameter (1 μ m).Other parameters and embodiment 1 are similar.
Claims (2)
1. equipment for purifying is characterized in that: comprise fluidized-bed, feed system, plasma excitation power supply and rewinding and gas-recycling plant, fluidized-bed comprises a grid distributor and a bed body; The bed body is the closed environment of vacuum-pumping, and bed body internal surface applies the dielectric of low-k, and the parallel pole of parallel dislocation is set in the bed body; Make fluid pass plasma area with the S type, its surface-coated high-dielectric coefficient coating insulate between parallel pole and bed body; On parallel pole, add the plasma excitation power supply; Between parallel pole, form dielectric barrier discharge, form plasma, the front end of fluidized-bed connects feed system; Terminal rewinding and the gas-recycling plant of connecting; Carrier gas gets into the bed body through grid distributor, and silica flour gets into fluidized-bed through feed system and carries out purifying, and the silicon material after the purification is from terminal rewinding and the gas-recycling plant of getting into of fluidized-bed.
2. equipment for purifying according to claim 1 is characterized in that: parallel pole has three, horizontal each other parallel misalignment, and fluidized material can flow through the parts transversely S type of dislocation.
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| CN 201110216669 CN102344143B (en) | 2011-07-30 | 2011-07-30 | Physical purification method and device of metallic silicon |
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| CN103224237B (en) * | 2013-05-23 | 2014-12-17 | 苏州金瑞晨科技有限公司 | Preparation method and device of phosphorus-doped nano silicon material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503192A (en) * | 2009-01-23 | 2009-08-12 | 晶海洋半导体材料（东海）有限公司 | Method for preparing polysilicon by plasma purification casting integrated furnace |
| CN101723377A (en) * | 2008-10-28 | 2010-06-09 | 刘铁林 | Method and device for purification of silicon |
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| US7820126B2 (en) * | 2006-08-18 | 2010-10-26 | Iosil Energy Corporation | Method and apparatus for improving the efficiency of purification and deposition of polycrystalline silicon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101723377A (en) * | 2008-10-28 | 2010-06-09 | 刘铁林 | Method and device for purification of silicon |
| CN101503192A (en) * | 2009-01-23 | 2009-08-12 | 晶海洋半导体材料（东海）有限公司 | Method for preparing polysilicon by plasma purification casting integrated furnace |
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Address after: 213031, No. 2, Tianhe Road, Xinbei Industrial Park, Jiangsu, Changzhou Patentee after: trina solar Ltd. Address before: 213031, No. 2, Tianhe Road, Xinbei Industrial Park, Jiangsu, Changzhou Patentee before: CHANGZHOU TRINA SOLAR ENERGY Co.,Ltd. Address after: 213031, No. 2, Tianhe Road, Xinbei Industrial Park, Jiangsu, Changzhou Patentee after: TRINASOLAR Co.,Ltd. Address before: 213031, No. 2, Tianhe Road, Xinbei Industrial Park, Jiangsu, Changzhou Patentee before: trina solar Ltd. |
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