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CN101445957B - Vacuum electron beam melting furnace for polysilicon purification - Google Patents

Vacuum electron beam melting furnace for polysilicon purification Download PDF

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Publication number
CN101445957B
CN101445957B CN200810073986XA CN200810073986A CN101445957B CN 101445957 B CN101445957 B CN 101445957B CN 200810073986X A CN200810073986X A CN 200810073986XA CN 200810073986 A CN200810073986 A CN 200810073986A CN 101445957 B CN101445957 B CN 101445957B
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electron beam
ingot
working chamber
chamber
crucible
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CN101445957A (en
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黄以平
李少林
宋宜梅
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GUILIN SHICHUANG VACUUM NC EQUIPMENT CO Ltd
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GUILIN SHICHUANG VACUUM NC EQUIPMENT CO Ltd
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Abstract

The invention provides a vacuum electron beam melting furnace for polysilicon purification. The melting furnace is characterized in that a melting chamber is square or cylindrical, a chamber wall is of a double water cooling structure or a coil water cooling structure; an electron gun is vertically and downwardly or horizontally arranged on the chamber wall of the melting chamber, a vacuum system is arranged at the rear of the melting chamber; an isolating valve is arranged between a feeding chamber and the melting chamber of a feed mechanism, and an inflation valve of an inflation system is arranged at the other side of the melting chamber; a discharge mechanism is arranged at the bottom of the melting chamber and connected with an ingot-pulling mechanism; the ingot-pulling isolating valve is arranged between discharge mechanism and the melting chamber; the melting chamber is internally provided with a water cooling crucible and a crystallizing crucible; all high-voltage devices of a high-voltage power supply of an electrical control system are arranged at a fuel tank filled with a transformer; and by adopting oil insulation of the transformer, the high-voltage power supply is connected with an electric cabinet which is connected with a console. The melting furnace has the advantages that a plurality of elements can be purified simultaneously, the production efficiency is high, energy consumption is low, energy-saving effect is excellent, and large-scale and automatic operation is easy to be implemented.

Description

Vacuum electron beam melting furnace for polysilicon purification
Technical field
The present invention relates to the equipment for purifying of polysilicon, specifically is a kind of vacuum electron beam melting furnace for polysilicon purification.
Background technology
Present global energy anxiety, the sun power demand increases considerably, and the requirement of making the high purity silicon chip of solar cell also increases considerably.Original method of purification mainly is to be raw material with silicone content greater than 99% Pure Silicon Metal, with gas phase distillation method of purification it is purified, and handles and obtains more highly purified silicon materials through solidifying again.This material is mainly used in semicon industry, section back the surplus tankage material that then can be used as solar cell use, such tankage limited amount does not satisfy the requirement of production solar cell.In addition, this method can't produce the material of contaminate environment such as a large amount of silane, muriate with avoiding.The silicon materials that are used for sun power contain impurity such as phosphorus, boron, carbon, iron, aluminium, titanium, oxygen, carbon, oxygen must be reduced to respectively below the 5-10ppm, and other impurity must be reduced to below the 0.1ppm, to guarantee required photoelectric transformation efficiency.In order to utilize solar cell more widely, this polysilicon of mass production at an easy rate.
In addition, China's publication number is CN101169311A, denomination of invention is the patent application of " electronic beam vacuum smelting oven ", a kind of electronic beam vacuum smelting oven that is used for melting refractory metal titanium is disclosed, because application is different, the equipment that this equipment and the present invention propose has very big difference on its principle and structure.
Summary of the invention
The objective of the invention is to provide a kind of can enhancing productivity, the multiple element of purifying simultaneously, but continuous production, energy consumption is low energy-conservation good, free of contamination, adopts vacuum electron beam melting furnace for polysilicon purification automatization control, that maximize.
The technical scheme that realizes the object of the invention is:
Vacuum electron beam melting furnace of the present invention, be under vacuum environment, utilize the Pure Silicon Metal of high-energy-density electron beam heating about 99% and make it fusing, by adjusting beam energy and track while scan, control polysilicon surface temperature, make vacuum tightness to change within the specific limits by the method that charges into rare gas element in addition, thereby make the phosphorus of polysilicon, impurity evaporations such as aluminium fall, silicon solution after the purification flows into the crystallization crucible, by insulation, ingot is drawn in crystallographic orientation and rotation, make the higher silicon ingot of purity, can be used for solar silicon wafers, the raw material of semi-conductor silicon chip and other industrial silicons.
A kind of vacuum electron beam melting furnace for polysilicon purification of the present invention, comprise the working chamber, electron beam gun, the electron beam Controlling System, pumped vacuum systems, electrical control system, feed mechanism, discharging mechanism, ingot pulling mechanism and automatic control system, it is characterized in that: the working chamber is square or cylindrical, locular wall is double-deck water-cooling structure or coil pipe water-cooling structure, electron beam gun is the 2-4 handle, vertically downward or level be installed on the locular wall of working chamber, pumped vacuum systems is configured in the rear of working chamber, feed mechanism is arranged on a side of working chamber, between the feeding material chamber of feed mechanism and working chamber, be provided with separation valve door, opposite side in the working chamber is fitted with the charging valve of inflation system, discharging mechanism is arranged on the bottom of working chamber, join with ingot pulling mechanism, between discharging mechanism and working chamber, be provided with and draw the ingot chamber isolation valve, be provided with cold-crucible and crystallization crucible in the working chamber, all high tension apparatus of the high-voltage power supply of electrical control system are contained in the fuel tank that fills transformer, the insulation of employing transformer oil, high-voltage power supply is connected with electrical control cubicles, and electrical control cubicles is connected with operator's console.
Described electron beam gun is made up of vacuum system, the separation valve door of electronic generator, focusing coil, deflector coil, electron beam gun.Electron beam gun power is between 30KW-300KW, and the electron beam gun acceleration voltage can be set between the 20KV-45KV, and the beam deflection angle can be the 5-30 degree.The vacuum system of electron beam gun can be made up of 1-3 level vacuum system, and every grade of vacuum system adds diffusion pump or sliding vane rotary pump by sliding vane rotary pump and adds molecular pump and form.Electronic generator is made up of filament, negative electrode, anode, grating, bunching electrode, and electronic generator chamber vacuum tightness is 10 -3-10 -4Between the Pa.Electron beam gun can be vertically downward, also can level be installed on the furnace wall, working chamber.
Described electrical control system high-voltage power supply provides beam voltage, heater current, bombarding voltage to electron beam gun.High-voltage power supply is made up of accelerating power source, heater supply, bombardment power supply, and all high tension apparatus are contained in the fuel tank shell, adopts the transformer oil insulation.High-voltage power supply power is 40-400KVA, and acceleration voltage is 20-45KV, and the high-voltage power supply voltage regulating mode can be a silicon-controlled voltage regulation mode, perhaps voltate regulator voltage regulating mode, or IGBT module voltage regulating mode, or intermediate frequency generator group voltage regulating mode.Acceleration voltage can be adjustable continuously between 0-45KV, and stability is ± 1%, and magnitude of voltage can pass through program setting, also can manual regulation.
Described electron beam Controlling System is used to control line size, bundle spot size, heating location and the track while scan of the electron beam that heats silicon.Electronic beam current can be regulated between 0-10A continuously, beam spot diameter, is between 5-30mm, heating location is whole silicon liquid place of arrival, scan mode can circular scan, square scanning, rectilinear scanning or helicon scanning, by electron beam conversion track while scan and line size, can control the liquid-state silicon surface temperature and between 1350-1500 ℃, change, help the evaporation of different impurities, also can control silicon itself simultaneously and be unlikely to loss too much according to certain rule.
Described feed mechanism is the mechanism that the silicon raw material that will purify is sent into working chamber's cold-crucible.Feeding style can be vertical feeding, also can be the straight feeding mode.Vertical feeding style generally is used for the conveying of block or Powdered silicon raw material, can realize the continuous conveying from the atmosphere to the working chamber, straight feeding generally is used for the conveying of long strip shape and bar-like raw material, Wheel-type multi-work-station structure can be made by mechanism, the 1-8 root bar stock of once can packing into, when a raw material melting finishes, another root raw material can forward the melting position to, continue melting, the straight feeding mode also can be used for the secondary smelting of silicon ingot.There is independently pumped vacuum systems in feeding material chamber, between feeding material chamber and working chamber separation valve door is arranged, and after the raw material melting is intact, can close separation valve door, adds new raw material, can not influence the vacuum tightness of working chamber, to realize continuous production.
Described cold-crucible and crystallization crucible, cold-crucible is made by copper or graphite, can make flat crucible, also can make crucible at the bottom of the circular arc.Squarely can be done in the crucible molten bath, also can do circular.Crucible is positioned at certain altitude and has opened a leakage grooves, and the height that reaches leakage grooves when liquid-state silicon will flow into the crystallization crucible along leakage grooves; The crystallization crucible is used for the directional freeze of polysilicon, and material is a copper.The crystallization crucible bottom is the end ingot of a rotation, the material of end ingot is quartz or graphite, in rotation, move downwards, make liquid-state silicon bottom directional freeze and form cylindrical silicon ingot under the cooling of water mold, speed of rotation can be 0.5-5 rev/min, pulls down ingot speed and can be 0.5-20mm/min.
Described pumped vacuum systems and inflation system, vacuum system are used to provide the silicon needed vacuum environment of purifying.Working chamber's working vacuum degree is 10 -2-10 -4Between the Pa; Inflation system is used to change the vacuum tightness of working chamber.The vacuum tightness of working chamber can be fixed, and also can change vacuum tightness by the amount of charging into of regulating inflation proportional valve control rare gas element, and vacuum tightness is 10 -2-10 -4Change with certain rule between the Pa, be beneficial to the elements vaporization of various different saturation vapour pressures, improve refining effect.
Described ingot pulling mechanism and discharge system, ingot pulling mechanism be used to realize the directional freeze of polysilicon and cast cylindrical silicon ingot, and ingot pulling mechanism moves downwards when making silicon ingot produce rotation by rotating machine, vertically draw ingot motor, screw mandrel, sealed water jacket to form.Discharge system be used for will draw ingot to finish polycrystal silicon ingot take out and draw the ingot chamber, finish whole fusion process, draw ingot to finish after, can be by closing the separation valve door that draws between ingot chamber and the working chamber, under the situation of not destroying working chamber's vacuum, take out silicon ingot and load onto new end ingot, to realize continuous production.
The situation that described video system is observed the working chamber by camera by the rotating metallic sheet that is installed on working chamber's door passes to vision signal computer or display screen again.Video system is installed in feeding material chamber simultaneously and draws the ingot chamber, so that the situation of observing feeding and drawing ingot.
Described automatization control is the program input computer that will weave in advance, and whole fusion process can be finished in automatization.
Advantage of the present invention is:
1) production efficiency height,
2) the multiple element because equipment can be purified does not simultaneously need as conventional fabrication processes each element all to be prepared a cover equipment for purifying;
3) can realize the uninterrupted production of purifying continuously.Because feeding material chamber and draw the ingot chamber all to design separation valve door and independent pumped vacuum systems, feeding and get the vacuum tightness that material can not influence the working chamber is so can realize continuous production;
4) energy expenditure is low, because beam energy density height can reach 10 5W/cm 2, heating efficiency is higher than (height) in traditional heating frequently, good energy-conserving effect;
5) owing to adopt metallurgy method to purify, can not produce pollutent as chemical method, the material of loss also can easily reclaim;
6) owing to adopt automated control technology, equipment is realized maximizing and automatization easily.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the floor plan synoptic diagram of structure of the present invention;
Fig. 3 is that Fig. 2 K is to enlarged diagram.
Among the figure: 1. electron beam gun a 2. electron beam gun b 3. electron beam a 4. electron beam b 5. working chambers 6. feed mechanisms, 7. silicon raw materials, 8. cold-crucibles, 9. crystallization crucibles, 10. charging valves, 11. end ingot 12. draws ingot chamber isolation valve 13. ingot pulling mechanisms 14. polycrystal silicon ingots 15. high-voltage power supplies 16. electrical control cubicles 17. operator's console 18. fire doors 19. pumped vacuum systems 20. video viewing systems 21. discharging mechanisms
Embodiment
With reference to Fig. 1, vacuum electron beam melting furnace for polysilicon purification of the present invention comprises electron beam gun a1, electron beam gun b2, electron beam a3, electron beam b4, working chamber 5, feed mechanism 6, cold-crucible 8, crystallization crucible 9, ingot pulling mechanism 13, high-voltage power supply 15, electrical control cubicles 16, operator's console 17, fire door 18, pumped vacuum systems 19, video viewing system 20 and discharging mechanism 21, working chamber 5 is square or cylindrical, locular wall is double-deck water-cooling structure or coil pipe water-cooling structure, electron beam gun a1 and electron beam gun b2 are the 2-4 handle, be installed in vertically downward on the locular wall of working chamber 5, the rear of working chamber 5 disposes pumped vacuum systems 19, feed mechanism 6 is arranged on a side of working chamber 5, be connected with motor, between the feeding material chamber of feed mechanism 6 and working chamber 5, be provided with separation valve door, 5 opposite side is fitted with the charging valve 10 of inflation system in the working chamber, discharging mechanism 21 is arranged on the bottom of working chamber 5, join with ingot pulling mechanism 13, between discharging mechanism 21 and working chamber 5, be provided with and draw ingot chamber isolation valve 12, be provided with cold-crucible 8 and crystallization crucible 9 in the working chamber 5, all high tension apparatus of the high-voltage power supply 15 of electrical control system are contained in the fuel tank that fills transformer, the insulation of employing transformer oil, high-voltage power supply 15 is connected with electrical control cubicles 16, and electrical control cubicles 16 is connected with operator's console 17.Production process of the present invention by computer control from the production process that is fed to discharging is:
After A, equipment vacuumize and reaches working order, incite somebody to action into strips or blocky metallic silicon raw material 7, send into copper or graphite system cold-crucible 8 or the top position that places vacuum melting chamber 5 by feed mechanism 6a;
The program of electron beam a3, the electron beam b4 that B, electron beam gun a1, electron beam gun b2 produce by establishment in advance heats the silicon raw material 7 of in the cold-crucible 8 or top position and it is melted in the cold-crucible 8;
C, charging into small amounts of inert gas by regulating proportional valve to working chamber 5, generally is argon gas, makes the vacuum tightness of working chamber 5 10 -2-10 -4Change with certain rule between the Pa, keep silicon simultaneously and become molten state;
D, by regulating line size and the track while scan of electron beam a3, electron beam b4, control polysilicon surface temperature changes according to certain rule between 1350-1500 ℃, along with electron beam a3, electron beam b4 stir silicon melt regularly, plurality of impurities will be evaporated in this process;
E, along with the raw material sent into increases, the molten silicon liquid level after the purification will reach spillway and slowly trickle in crystallization crucible 9; Continuous again charging feed kept the raw material of sending into equal substantially with the liquid-state silicon that flows away when liquid-state silicon flowed away, and finished up to melting;
After F, liquid-state silicon flowed into crystallization crucible 9, the electron beam a3, the electron beam b4 that are produced by other electron beam gun a1, electron beam gun b2 continued the scanning heating, kept its surface and were in molten state and are further purified;
Ingot moves downwards in rotation at the bottom of the rotation of G, crystallization crucible 9 bottoms, makes liquid-state silicon bottom directional freeze and form cylindrical silicon ingot under the cooling of water mold;
H, when melting end or silicon ingot reach predefined height, stop to draw ingot, close and draw ingot chamber valve 12, can under the situation of not destroying working chamber's 5 vacuum, take out silicon ingot;
When electron beam gun power was 60KW, continuous production 20 hours can be produced 38 kilograms of the cylindrical polycrystal silicon ingots of 10 diameter 100mm, length 200mm.

Claims (7)

1. vacuum electron beam melting furnace for polysilicon purification, comprise the working chamber, electron beam gun, the electron beam Controlling System, pumped vacuum systems, electrical control system, feed mechanism, discharging mechanism, ingot pulling mechanism and automatic control system, it is characterized in that: working chamber (5) are for square or cylindrical, locular wall is double-deck water-cooling structure or coil pipe water-cooling structure, electron beam gun (1,2) be the 2-4 handle, vertically downward or level be installed on the locular wall of working chamber (5), pumped vacuum systems (19) is configured in the rear of working chamber (5), feed mechanism (6) is arranged on a side of working chamber (5), between the feeding material chamber of feed mechanism (6) and working chamber (5), be provided with separation valve door, the opposite side of (5) is fitted with the charging valve (10) of inflation system in the working chamber, discharging mechanism (21) is arranged on the bottom of working chamber (5), join with ingot pulling mechanism (13), between discharging mechanism (21) and working chamber (5), be provided with and draw ingot chamber isolation valve (12), be provided with cold-crucible (8) and crystallization crucible (9) in the working chamber (5), all high tension apparatus of the high-voltage power supply of electrical control system (15) are contained in the fuel tank that fills transformer, the insulation of employing transformer oil, high-voltage power supply (15) is connected with electrical control cubicles (16), and electrical control cubicles (16) is connected with operator's console (17).
2. smelting furnace according to claim 1, it is characterized in that: described electron beam gun (1,2) power is between 30KW-300KW, electron beam gun (1,2) acceleration voltage is between 20KV-45KV, electron beam (3,4) deflection angle is the 5-30 degree, the vacuum system of electron beam gun (1,2) is made up of 1-3 level vacuum system, and every grade of vacuum system adds diffusion pump or sliding vane rotary pump by sliding vane rotary pump and adds molecular pump and form; Electronic generator chamber vacuum tightness is 10 -3-10 -4Between the Pa.
3. smelting furnace according to claim 1 is characterized in that: electronic beam current is adjustable continuously between 0-10A, and beam spot diameter, is between 5-30mm.
4. smelting furnace according to claim 1 is characterized in that: described cold-crucible (8) is made crucible at the bottom of flat crucible or the circular arc by copper or graphite, and the crucible molten bath is made square or circular.
5. smelting furnace according to claim 1, it is characterized in that: described crystallization crucible (9) is made by copper product, the bottom is the end ingot (11) of a rotation, the material of end ingot (11) is quartz or graphite, the speed of rotation of end ingot (11) is 0.5-5 rev/min, and pulling down ingot speed is 0.5-20mm/min.
6. smelting furnace according to claim 1 is characterized in that: described working chamber (5) working vacuum degree is 10 -2-10 -4Between the Pa.
7. smelting furnace according to claim 1 is characterized in that: described ingot pulling mechanism (13) is by forming with the vertical ingot motor that draws with the rotating machine that screw mandrel is connected with sealed water jacket.
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CN103435043A (en) * 2013-08-28 2013-12-11 青岛隆盛晶硅科技有限公司 Device and process method for preparing polycrystalline silicon through coupling of electron beam smelting and crystal growing technology

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CN102275929A (en) * 2010-06-10 2011-12-14 上海华巨硅材料有限公司 Method for improving purity of metallurgical silicon and apparatus for realizing method
CN102564123B (en) * 2010-12-29 2014-03-05 北京有色金属研究总院 Electron beam smelting furnace
CN102120578B (en) * 2011-01-29 2012-10-03 大连隆田科技有限公司 A method and equipment for coupling purification of polysilicon by electron beam dephosphorization and metal removal
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CN102126725B (en) * 2011-01-29 2012-12-19 大连隆田科技有限公司 A method and equipment for purifying polysilicon by electron beam shallow molten pool smelting
CN103420380B (en) * 2013-08-28 2015-06-03 青岛隆盛晶硅科技有限公司 Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology
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CN104195637B (en) * 2014-09-01 2017-02-15 大连理工大学 An electron beam melting device and method for preparing boron master alloy
CN104195636A (en) * 2014-09-01 2014-12-10 大连理工大学 A method for quickly preparing boron master alloy by metallurgical method
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CN104878448A (en) * 2015-05-15 2015-09-02 大连理工大学 An electron beam area smelting polysilicon equipment and a method for removing impurities
CN109052408A (en) * 2018-10-17 2018-12-21 大连颐和顺新材料科技有限公司 Continuous smelting method and equipment for diamond wire cutting silicon powder
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CN103435043B (en) * 2013-08-28 2015-05-27 青岛隆盛晶硅科技有限公司 Device and process method for preparing polycrystalline silicon through coupling of electron beam smelting and crystal growing technology

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