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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Abstract
The invention relates to the technical field of purification of solar-grade polycrystalline silicon materials, particularly a physical purification method and device of metallic silicon. The device comprises a fluidized bed, a feed system, a plasma excitation power supply and a material collection and gas circulation device. A dielectric barrier discharge method is used in the fluidized bed as a plasma generation way; the fluidized bed is used for preheating and transmitting silicon powder; the granule average treatment time is controlled by granularity of silicon powder, preheating temperature of carrier gas and flow rate of carrier gas; the purification effect is controlled by preheating temperature of carrier gas, atmosphere type of carrier gas and power of the plasma excitation power supply for dielectric barrier discharge; the silicon powder restricted into the plasma is purified in the flow process; and finally, the purified silicon material is output from the tail end of the fluidized bed. The invention can be used for purifying the silicon material under the atmospheric pressure or near-atmospheric pressure, and has the advantages of high density of ions for purification, high energy, high purification efficiency and low cost.
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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| 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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