CN202022753U - Polycrystalline silicon purifying device - Google Patents
Polycrystalline silicon purifying device Download PDFInfo
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- CN202022753U CN202022753U CN2011200177253U CN201120017725U CN202022753U CN 202022753 U CN202022753 U CN 202022753U CN 2011200177253 U CN2011200177253 U CN 2011200177253U CN 201120017725 U CN201120017725 U CN 201120017725U CN 202022753 U CN202022753 U CN 202022753U
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- silicon liquid
- high temperature
- temperature silicon
- electromagnetic induction
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Abstract
The utility model aims to provides an improved polycrystalline silicon purifying device, which comprises an electromagnetic induction smelting unit (001), a plasma smelting furnace (200), a constant-temperature quartz guide pipe (101), an electron beam smelting furnace (305) and a directional solidification unit (401), wherein the electromagnetic induction smelting unit (001) heats and melts metallic silicon to generate high-temperature silicon liquid through electromagnetic induction; ion beams blow, oxidize and smelt the high-temperature silicon liquid under the vacuum environment; the constant-temperature quartz guide pipe (101) leads the high-temperature silicon liquid in the plasma smelting furnace (200) into the electron beam smelting furnace (305) in a constant-temperature manner; in the electron beam smelting furnace (305), high-energy electron beams bombard the high-temperature silicon liquid under the vacuum environment; and the directional solidification unit (401) enables the high-temperature silicon liquid flowed out of the electron beam smelting furnace (305) to be cooled and solidified in a directional manner and thrown uniformly. The ion beam blowing and oxidizing and electron beam smelting are carried out under the respective and independent vacuum environments, so that the optimal impurity removing and purifying technology is provided. The improved polycrystalline silicon purifying device has the advantages of simple equipment, low cost and controllable technology, decreases the intermediate pollution links, and produces solar energy level polycrystalline silicon with low energy consumption, quickness and high efficiency.
Description
Technical field
The utility model relates to the solar cell manufacturing technology, relates in particular to a kind of polysilicon purifying plant that adopts high energy beam current to smelt purifying polycrystalline silicon.
Background technology
Fossil energy limited amount on the earth will use up in 200 or three hundred years with existing energy expenditure speed.Sun power is inexhaustible clean energy, need use highly purified silicon yet make solar panel, and the maximum bottleneck of Application of Solar Energy technology is that just the production cost of HIGH-PURITY SILICON is too high at present.
It is chemical method that the method for purification of silicon has a kind of, and the representative method is Siemens Method and improvement Siemens Method, and its purification purity reaches 99.9999999-99.9999999999%, but the purification process complexity, the energy consumption height produces a large amount of pollutents, the cost of investment height.Another kind method is the physics method, the representative method is electron beam melting, ionic fluid melting or both technology bonded methods, this method of purification purification limit can only reach 99.99999%, foreign matter contents such as Fe, the Ti of the polysilicon efficiency of conversion that makes some difference, O are too high, the rapid relaxation phenomenon that also causes the polysilicon solar cell plate influences life-span of solar panel.But its equipment is simple, and technical process is few, less investment, and energy consumption is low, is a reasonable polysilicon purification research direction.
Applied Physics method purified silicon need be used high energy beam polysilicon purifying device.Existing high energy beam polysilicon purifying device, it comprises electron beam and ionic fluid melting unit, its structure principal feature is in a vacuum cavity electron beam gun and ion gun to be installed simultaneously, the advantage of this structure is that the high temperature silicon liquid after electron beam melting flows into ionic fluid melting tray, do not need to shift through exterior cooling, directly the high temperature silicon liquid through electron beam melting is carried out the ionic fluid melting, this continuous high-energy bundle melting technology adds electromagnetic induction melting and directional solidification processes, can the continuously feeding discharging, energy efficient is raised the efficiency and equipment capacity.
But, thisly place the intravital smelting process of same vacuum chamber can not effectively bring into play the advantage that two kinds of high energy beam currents are smelted electron beam gun and ion gun, influence the purity of purifying polycrystalline silicon; According to the best vacuum pressure of research electron beam melting refining effect is 10
-3-10
-5Pa, and the best vacuum pressure of ionic fluid melting refining effect is 10
-2-10
5Pa, and need in the ionic fluid melting, be blown into oxidizing gas, can improve the effect of removing polysilicon impurity.And existing electron beam gun and ion gun are placed the intravital polysilicon purifying plant of same vacuum chamber, and can't bring into play the best removal of impurities advantage of electron beam and ionic fluid melting simultaneously, maximum polysilicon purification degree is less than 99.9999%; Will increase vacuum pressure if in the ionic fluid melting, add the air blowing oxidation impurity removal process, influence the electron beam melting refining effect, therefore this technology can't be optimized technology and further improve polysilicon purity, can't reach solar-grade polysilicon greater than 99.9999% purity requirement.
The utility model content
The purpose of this utility model provides a kind of improved polysilicon purifying plant, this device with electromagnetic induction melting, ionic fluid air blowing oxidation smelt, electron beam really holds melting and four kinds of technologies of directional freeze combine, adopt continuous processing in turn the industrial silicon material to be carried out obtaining the polysilicon that purity reaches 99.9999-99.999999% after electromagnetic induction melting, the smelting of ionic fluid air blowing oxidation, electronic beam vacuum smelting, the directional freeze, owing in the ionic fluid melting, add the chemical process of air blowing oxidation, broken through the limit purity 99.9999% of physics method purifying polycrystalline silicon.
Polysilicon purifying plant of the present utility model comprises: electromagnetic induction melting unit (001) generates high temperature silicon liquid with the electromagnetic induction molten metal silicon material of heating; Plasma smelting stove (200), the ionic fluid air blowing oxidation is smelted high temperature silicon liquid under vacuum environment; Constant temperature quartz conduit (101) imports electron beam melting furnace (305) with the high temperature silicon liquid constant temperature in the plasma smelting stove (200); Electron beam melting furnace (305) bombards high temperature silicon liquid with high-power electron beam under vacuum environment; Directional freeze unit (401) makes from the effusive high temperature silicon liquid of electron beam melting furnace (305) directed cooled and solidified and even throwing under thermograde up and down.
Preferably, described electromagnetic induction melting unit (100) comprises the feed control motor, feed containers, electromagnetic induction heater and by-pass valve control.
Preferably, described plasma smelting stove (200) comprises bleeding point (206), is used to take out vacuum in the stove; Material collecting disc (207) is used to accept high temperature silicon liquid; At least one ion gun (202,205) carries out the plasma heating evaporation to high temperature silicon liquid; And at least one gas injection port (203,204), be used for air blowing oxidation high temperature silicon liquid.
Preferably, described constant temperature quartz conduit (101) comprises the electromagnetic induction coil (102) of outer wrap, and the high temperature silicon liquid that is used in the heating duct makes it keep constant temperature.
Preferably, described constant temperature quartz conduit (101) comprises charging valve (105) and flow control plate (103), is used to control the inflow velocity of high temperature silicon liquid and isolates described plasma smelting stove (200) and electron beam melting furnace (305).
Preferably, described constant temperature quartz conduit (101) has material receiving port (104) at the end that high temperature silicon liquid flows into.
Preferably, described electron beam melting furnace (305) comprises evaporating pan (304), accepts high temperature silicon liquid; Electron beam gun (301) carries out the high-power electron beam bombardment to high temperature silicon liquid; Bleeding point (303) is used to vacuumize and discharge foreign gas.
Preferably, described directional freeze unit (401) comprises cylindrical crucible, is positioned at the electromagnetic induction heating coil on described crucible top, is positioned at the water-cooled tube of described crucible bottom, and the billet withdrawal device that the silicon material is at the uniform velocity extracted out.
Preferably, in described polysilicon purifying plant, described plasma smelting stove (200) and electron beam melting furnace (305) all have view port (201,302).
Principle of the present utility model is that smelting of ionic fluid air blowing oxidation and electronic beam vacuum smelting are installed in two adjacent vacuum ovens, and middle the connection with electromagnetic induction constant temperature quartz conduit transmitted high temperature silicon liquid.The Pure Silicon Metal material is at first through the electromagnetic induction fusion of heating, and high temperature silicon liquid flows into evaporating pan in the ionic fluid air blowing oxidation smelting furnace, is blown into the mixed gas of steam, hydrogen and argon gas, and silicon liquid quickens polysilicon B, C, SiO under the bombardment of high energy ion beam
2Deng oxidation, the reduction chemical reaction of impurity, remove B, C, SiO in the polysilicon
2, impurity such as Fe, Ti, Cu.The high temperature silicon liquid of process ionic fluid air blowing oxidation smelting removal of impurities is sent to electronic beam vacuum smelting oven by the constant temperature quartz conduit and further purifies, remove the relative high impurity of silicon vapour pressure such as P, Al, BO in the polysilicon, utilize the difference of different substances segregation coefficient then, the vacuum oriented solidification technology of process is further removed the residual impurity in the silicon material again.
Characteristics of the present utility model be the ionic fluid air blowing oxidation is smelted and electron beam melting separately independently vacuum environment carry out, the removal of impurities purifying technique of optimum separately is provided.Blowing in the ionic fluid melting adds the redox reaction of chemistry, can improve the effect of removal of impurities, accelerates purifying velocity, can make the content of boron impurities (B) be reduced to less than 0.2PPM.In electron beam melting, select optimum vacuum environment and electronic beam current energy, can make the content of foreign matter of phosphor (P) reduce to 0.1PPM.Smelt and electron beam melting through ionic fluid, can both obviously reduce B, P and other foreign matter content, pass through the directional solidification technique removal of impurities again, finally can be met the high-purity polycrystalline silicon of solar panel application standard.
The beneficial effects of the utility model be this device separate the smelting technique technology utilized under the different vacuum environments separately independent optimization determined and can not improve the problem of polysilicon purity, this appliance arrangement is simple, with low cost, technology is controlled, be molten to the directional freeze operation from the input of silicon material, omnidistance realization silicon materials flow commentaries on classics in vacuum environment, pollution section in the middle of reducing has realized utilizing metallurgy method less energy-consumption, fast and efficient production solar-grade polysilicon.
Description of drawings
Fig. 1 is the structural representation of the polysilicon purifying plant of the utility model embodiment
Wherein, the 001st, electromagnetic induction melting unit, the 101st, constant temperature quartz conduit, the 102nd, electromagnetic induction coil, the 103rd, flow control plate, the 104th, material receiving port, the 105th, charging valve, the 200th, the plasma smelting stove, the 201st, A view port, the 202nd, A ion gun, the 203rd, A gas injection port, the 204th, the B gas injection port, the 205th, B ion gun, the 206th, A bleeding point, the 207th, material collecting disc, the 301st, electron beam gun, the 302nd, B view port, the 303rd, B bleeding point, the 304th, evaporating pan, the 305th, electron beam melting furnace, the 401st, directional freeze unit.
Embodiment
By describing technology contents of the present utility model, structural attitude in detail, realized purpose and effect, give explanation below in conjunction with embodiment and conjunction with figs. are detailed.
Fig. 1 is the structural representation of the polysilicon purifying plant of the utility model embodiment.With reference to shown in Figure 1, the utility model is the polysilicon purifying plant of a kind of integrated electromagnetic induction melting unit 001, plasma smelting stove 200, constant temperature quartz conduit 101, electron beam melting furnace 305, directional freeze unit 401.The mode of operation of its concrete structure and each several part explains detailedly below:
1, electromagnetic induction melting:
Electromagnetic induction melting unit 001 is positioned at the top of plasma smelting stove 200, feed control motor, feed containers, electromagnetic induction heater are wherein arranged, pour metal silico briquette material into feed containers by the feed control motor, carry out the electromagnetism heating and melting by electromagnetic induction heater, heating keeps 1500 ℃ of temperature, forms high temperature silicon liquid, and the electromagnetic induction melting unit bottom is equipped with by-pass valve control, control high temperature silicon liquid take-off rate, high temperature silicon liquid flows into the material collecting disc 207 of plasma smelting stove 200.
2, the ionic fluid air blowing oxidation is smelted:
There is an A bleeding point 206 in the left side in the plasma smelting stove 200, is used for vacuumizing in the stove, and vacuum pressure remains on 10
-2Between-the 10Pa.A material collecting disc 207 is installed in mid-way in stove, is used to accept electromagnetic induction melting unit 001 effusive high temperature silicon liquid, sends into constant temperature quartz conduit 101 from the right side outflow behind the silicon hydroful.Both sides, top incline position is installed A ion gun 202, B ion gun 205 in the stove, and power 45KW aims at material collecting disc 207, is used for the silicon liquid in the material collecting disc 207 is carried out the plasma heating evaporation.Both sides, top incline position has also been installed A gas injection port 203, B gas injection port 204 in the stove, is used to inject mixed gass such as argon gas, water vapor, hydrogen.Right side, top incline position is installed an A view port 302 in the stove, is used to observe temperature and smelting situation in the plasma smelting stove 200.
Remain on 10 at air pressure
-2In-10Pa the vacuum environment, A ion gun 202, B ion gun 202205 send high energy ion beam, high temperature silicon liquid heating for 207 li of evaporating pans, between Heating temperature 1500-1700 ℃, inject mixed gass such as argon gas, water vapor, hydrogen by gas injection port 204 simultaneously, impurity such as B, C, O, P, Fe, Ti, Cu and hydrogen, water molecules generation chemical reaction generate gasification substance, are got rid of outside the stoves by bleeding point 206.At material collecting disc 207.In plasma smelting stove 200, through plasma air blowing oxidation smelting process, the clearance height of B, C, O, B content＜0.2PPM, the content of C be less than 0.1PPM, the content summation＜2PPM of other impurity, silicon purity＞99.999% of high temperature silicon liquid.
3, constant temperature water conservancy diversion:
Constant temperature quartz conduit 101 connects plasma smelting stove 200 and electron beam melting furnace 305, material receiving port 104 is accepted the high temperature silicon liquid of plasma smelting stove 200 inner evaporating pan 207 spill-overs, flow in the constant temperature quartz conduit 101, constant temperature quartz conduit 101 outer wrap electromagnetic induction coils 102, be high temperature silicon liquid heated constant temperature in the conduit, keep 1500 ℃ of steady temperatures, the middle part has a charging valve 105 and right side outlet to have a flow control plate 103 common control high temperature silicon liquid to flow into, and isolates the vacuum environment of two different pressures of plasma smelting stove 200 and electron beam melting furnace 305.
Smelt the high temperature silicon liquid of purifying through the plasma air blowing oxidation and flow into material receiving port 104,, flow into the evaporating pan 304 of electron beam melting furnace 305 by the charging valve 105 and the flow control plate 103 of constant temperature quartz conduit 101 in material collecting disc 207 spill-overs.
4, vacuum electron beam melting:
The top is an electron beam gun 301 in electron beam melting furnace 305 stoves, power 30KW, and voltage 18KV, electron beam gun 301 is aimed at the evaporating pan 304 at middle part in the stove, is used for the high temperature silicon liquid melting in the evaporating pan 304.The angle is a B view port 302 on the interior right side of stove, temperature and melting situation in the observation stove.There is a B bleeding point 303 top, right side in the stove, is used to vacuumize, and discharges impurity waste gas, keeps vacuum pressure 10 in the stove
-3-10
-5Pa.Lower middle position is installed directional freeze unit 401 in the stove, accepts the high temperature silicon liquid of evaporating pan 304 spill-overs.
The high temperature silicon liquid that electron beam gun 301 is aimed at evaporating pan 304 carries out the high-energy electron bombardment, in temperature 1500-1700 ℃ vacuum pressure 10
-3-10
-5Under the environment of Pa, the saturated vapor pressure of silicon and impurity is different, and particularly impurity such as P, Ca, Al are bigger more than 10,000 times than the saturated vapor pressure of silicon, and under the bombardment of impurity high-energy electron, the overwhelming majority evaporates into gas, is extracted out outside the stove by vacuum-pumping equipment.The high temperature silicon liquid of the high-power electron beam melting of process electron beam melting furnace 305, the content of P, Al, Ca reduces to＜0.1PPM, the effusive high temperature silicon liquid of evaporating pan 304 spill-overs purity arrives＞and 99.9999%, other residual impurity is removed in next step directional freeze step.
5, directional freeze:
Directional freeze unit 401 is made up of cylindrical crucible, electromagnetic induction heating coil, water-cooled tube, billet withdrawal device etc., go in the cylindrical crucible through the high temperature silicon drop that the ionic fluid air blowing oxidation is smelted and two steps of electron beam melting are purified, electromagnetic induction heating coil is installed on crucible appearance top, silicon material in the heating crucible, water-cooled tube is installed in crucible appearance bottom, the silicon material is in the upper and lower two part formation temperature gradients of crucible, by billet withdrawal device the silicon material is extracted out at the uniform velocity downwards, the silicon material in the throwing extraction, cooled and solidified gradually.
In high temperature silicon liquid, the segregation coefficient of impurity is very low, impurity such as P, Fe, Cu, Ti less than 0.3, according to experimental verification, in the even process of billet withdrawal of right cylinder crucible, per hour the downward casting speed less than 20mm obtains best directional freeze impurity-eliminating effect, in directional freeze process of the present utility model, set casting speed 18mm/ hour, the high temperature silicon liquid of electromagnetic induction melting unit 001 flows into the speed of plasma smelting stove 200, the high temperature silicon flow quantity of constant temperature quartz conduit 101 controls must be controlled requirement less than casting speed.The silicon material external skins that impurity enriched is solidified at throwing, excision appearance impurity obtains high-purity polycrystalline silicon.Detect the sample of a plurality of purifications, adopt inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry, the polysilicon purity range 99.9999-99.999999% that directional freeze is produced, metallic element total impurities content＜0.1PPM, B content＜0.2PPM, P content＜0.1PPM, 0 content＜3 * 10
17CM
-3, C content＜2 * 10
16CM
-3, meet the solar-grade polysilicon requirement.
To sum up, the utility model the ionic fluid air blowing oxidation is smelted and electron beam melting separately independently vacuum environment carry out, the removal of impurities purifying technique of optimum separately is provided; Pass through the directional solidification technique removal of impurities again, finally can be met the high-purity polycrystalline silicon of solar panel application standard.The utility model equipment is simple, and is with low cost, and technology is controlled, be molten to the directional freeze operation from the input of silicon material, omnidistance realization silicon materials flow commentaries on classics in vacuum environment, pollution section in the middle of reducing has realized utilizing metallurgy method less energy-consumption, fast and efficient production solar-grade polysilicon.
The above only is embodiment of the present utility model; be not so limit claim of the present utility model; every equivalent structure or equivalent flow process conversion that utilizes the utility model specification sheets and accompanying drawing content to be done; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present utility model.
Claims (9)
1. a polysilicon purifying plant is characterized in that, comprising: electromagnetic induction melting unit (001) generates high temperature silicon liquid with the electromagnetic induction molten metal silicon material of heating; Plasma smelting stove (200), the ionic fluid air blowing oxidation is smelted high temperature silicon liquid under vacuum environment; Constant temperature quartz conduit (101) imports electron beam melting furnace (305) with the high temperature silicon liquid constant temperature in the plasma smelting stove (200); Electron beam melting furnace (305) bombards high temperature silicon liquid with high-power electron beam under vacuum environment; Directional freeze unit (401) makes from the effusive high temperature silicon liquid of electron beam melting furnace (305) directed cooled and solidified and even throwing under thermograde up and down.
2. polysilicon purifying plant according to claim 1 is characterized in that, described electromagnetic induction melting unit (100) comprises the feed control motor, feed containers, electromagnetic induction heater and by-pass valve control.
3. polysilicon purifying plant according to claim 1 is characterized in that, described plasma smelting stove (200) comprises bleeding point (206), is used to take out vacuum in the stove; Material collecting disc (207) is used to accept high temperature silicon liquid; At least one ion gun (202,205) carries out the plasma heating evaporation to high temperature silicon liquid; And at least one gas injection port (203,204), be used for air blowing oxidation high temperature silicon liquid.
4. polysilicon purifying plant according to claim 1 is characterized in that, described constant temperature quartz conduit (101) comprises the electromagnetic induction coil (102) of outer wrap, and the high temperature silicon liquid that is used in the heating duct makes it keep constant temperature.
5. polysilicon purifying plant according to claim 1, it is characterized in that, described constant temperature quartz conduit (101) comprises charging valve (105) and flow control plate (103), is used to control the inflow velocity of high temperature silicon liquid and isolates described plasma smelting stove (200) and electron beam melting furnace (305).
6. polysilicon purifying plant according to claim 1 is characterized in that, described constant temperature quartz conduit (101) has material receiving port (104) at the end that high temperature silicon liquid flows into.
7. polysilicon purifying plant according to claim 1 is characterized in that, described electron beam melting furnace (305) comprises evaporating pan (304), accepts high temperature silicon liquid; Electron beam gun (301) carries out the high-power electron beam bombardment to high temperature silicon liquid; Bleeding point (303) is used to vacuumize and discharge foreign gas.
8. polysilicon purifying plant according to claim 1, it is characterized in that described directional freeze unit (401) comprises cylindrical crucible, is positioned at the electromagnetic induction heating coil on described crucible top, be positioned at the water-cooled tube of described crucible bottom, and the billet withdrawal device that the silicon material is at the uniform velocity extracted out.
9. according to the described polysilicon purifying plant of above any claim, it is characterized in that described plasma smelting stove (200) and electron beam melting furnace (305) all have view port (201,302).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200177253U CN202022753U (en) | 2011-01-20 | 2011-01-20 | Polycrystalline silicon purifying device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200177253U CN202022753U (en) | 2011-01-20 | 2011-01-20 | Polycrystalline silicon purifying device |
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|---|---|
| CN202022753U true CN202022753U (en) | 2011-11-02 |
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ID=44847713
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|---|---|---|---|
| CN2011200177253U Expired - Fee Related CN202022753U (en) | 2011-01-20 | 2011-01-20 | Polycrystalline silicon purifying device |
Country Status (1)
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|---|---|
| CN (1) | CN202022753U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111910093A (en) * | 2020-08-24 | 2020-11-10 | 中国科学院金属研究所 | Electron beam induced layer condensation device and method for preparing high-temperature alloy difficult to deform |
| CN113584586A (en) * | 2021-08-06 | 2021-11-02 | 宁夏红日东升新能源材料有限公司 | Method and device for purifying polycrystalline silicon by centrifugal directional solidification |
-
2011
- 2011-01-20 CN CN2011200177253U patent/CN202022753U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111910093A (en) * | 2020-08-24 | 2020-11-10 | 中国科学院金属研究所 | Electron beam induced layer condensation device and method for preparing high-temperature alloy difficult to deform |
| CN111910093B (en) * | 2020-08-24 | 2024-04-09 | 中国科学院金属研究所 | Electron beam induced layer condensing device and method for preparing difficult-to-deform superalloy |
| CN113584586A (en) * | 2021-08-06 | 2021-11-02 | 宁夏红日东升新能源材料有限公司 | Method and device for purifying polycrystalline silicon by centrifugal directional solidification |
| CN113584586B (en) * | 2021-08-06 | 2024-04-26 | 宁夏红日东升新能源材料有限公司 | Centrifugal directional solidification purification method and device for polysilicon |
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|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111102 Termination date: 20160120 |
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