Summary of the invention
The present invention overcomes above-mentioned not enough problem, the device and processing method that provide a kind of electron beam melting to be coupled with crystal growing technology to prepare polysilicon, removes the phosphorus impurities element in silicon more efficiently, greatly reduces the total energy consumption in production process.
The technical scheme that the present invention is adopted for achieving the above object is: a kind of electron beam melting is coupled with crystal growing technology and prepares the device of polysilicon, plumbago crucible is placed with in body of heater, plumbago crucible outer wall is surrounded with graphite heating body and graphite muff from inside to outside successively, the upper graphite cover plate of graphite muff can move horizontally, and is circumscribed with hollow board slot in the side of body of heater and the parallel position place of upper graphite cover plate; Plumbago crucible bottom centre position is provided with water-cooled ingot pulling mechanism; It is built-in with refrigeration cycle water pipe; Body of heater top is led to and is provided with electron beam gun, and sidepiece upper end has inflation valve, and lower end has purging valve.
The preferred plus silicon carbide of plumbago crucible internal surface or silicon nitride coating.
Adopt electron beam melting to be coupled with crystal growing technology the processing method of the device preparing polysilicon, step is as follows:
(1) charging vacuumizes: put into plumbago crucible by after silicon material cleaning, drying, and vacuumize in body of heater;
(2) argon gas boosting is added: in body of heater, pass into argon gas boosting by inflation valve;
(3) intensification makes silicon material melt: mobile graphite cover plate covers to plumbago crucible top, is energized to silicon material is fused into silicon liquid completely to graphite heating body;
(4) electron beam melting: body of heater and electron beam gun are again vacuumized, removes the graphite cover plate on plumbago crucible, unlocking electronic rifle after setting electron beam gun power, and carry out electron beam melting to silicon liquid surface, melting terminates rear closedown electron beam gun;
(5) the long crystalline substance of crystal: mobile graphite cover plate covers to plumbago crucible top, is filled with argon gas boosting in body of heater, starts water-cooled ingot pulling mechanism and draws ingot, pulls out the thermal field of graphite heating body until long brilliant end by plumbago crucible;
(6) ingot casting annealing: control graphite heating body and temperature of thermal field is set in below silicon fusing point, start water-cooled ingot pulling mechanism, plumbago crucible is risen up into thermal field again, carries out insulation annealing;
(7) cool, blow-on gets ingot: the rate of temperature fall controlling graphite heating body, after ingot casting temperature is reduced, open purging valve, exit to equipment, then ingot casting is taken out in blow-on.
Preferred version is as follows:
To be phosphorus content be this silicon material 0.005 ~ 0.006%, metal content lower than 0.0001%, Boron contents lower than 0.000015% polycrystalline silicon material.
In step (3), the temperature rise rate of graphite heating body is 200 ~ 250 DEG C/h.
Unlocking electronic rifle in step (4), setting electron beam gun power is 90 ~ 120kw.
In step (5), water-cooled ingot pulling mechanism draws ingot speed 0.15 ~ 0.20mm/min.
In step (6), temperature of thermal field is 1200 ~ 1300 DEG C.
In step (7), rate of temperature fall is 100 ~ 150 DEG C/h.
In the present invention, plumbago crucible is put into graphite heating body, graphite heating body added graphite heat insulation sheath, plays insulation effect, and plumbago crucible can be splicing crucible simultaneously, takes taking-up ingot casting after being convenient to blow-on apart; Plumbago crucible internal surface plus silicon carbide coating, avoids silicon and graphite to react, and meanwhile, prevents sticky crucible phenomenon.Mechanical pump, lobe pump, diffusion pump and molecular pump are Vacuum Field common device, in apparatus of the present invention with the use of, process is vacuumized to body of heater and electron beam gun; In electron beam irradiation plumbago crucible, silicon melt surface, increases bath surface temperature, increases the thermograde of surface and surperficial following near zone, and the disturbance of strengthening silicon melt, strengthens the surface effects that phosphorus volatilization is removed, remove the phosphorus impurities in silicon; Upper graphite cover plate, on plumbago crucible top, in horizontal plane movement, can covering on plumbago crucible when heat fused, carry out the insulation of thermal field, when carrying out electron beam melting, being removed by upper graphite cover plate, high insulating effect, is skillfully constructed and easy to operate.
Advantage of the present invention: electron beam melting technology and long brilliant process are coupled by the method effectively, thus achieve the object realizing two kinds of production technique on the same device, graphite heating body is utilized to carry out melted silicon material, utilize electron irradiated silicon bath surface, strengthening surface volatilization effect, volatility phosphorus impurities in efficient removal silicon, then long crystalline substance is carried out, decrease fragmentation, cleaning and oven dry link, save input and the floor space of relevant device, greatly reduce energy expenditure during independent production, total energy consumption decreases beyond 30%, production efficiency can improve about 40%.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment and accompanying drawing, but the present invention is not limited to specific embodiment.
Embodiment 1:
Plumbago crucible 17 is placed with, plumbago crucible 17 internal surface plus silicon carbide coating in body of heater 5.Plumbago crucible 17 outer wall is surrounded with graphite heating body 9 and graphite muff 8 from inside to outside successively, and the upper graphite cover plate 7 of graphite muff 8 can move horizontally, and is circumscribed with hollow board slot in the side of body of heater 5 and the parallel position place of upper graphite cover plate 7; Plumbago crucible 5 bottom centre position is provided with water-cooled ingot pulling mechanism 11; It is built-in with refrigeration cycle water pipe 12; Body of heater 5 top is led to and is provided with electron beam gun 1, and sidepiece upper end has inflation valve 13, and lower end has purging valve 10.
Embodiment 2:
Adopt the device in embodiment 1 to carry out electron beam melting to be coupled with crystal growing technology and to prepare polysilicon:
(1) be 0.005% by 500kg phosphorus content, metal content 0.00009%, Boron contents be the polycrystalline silicon material of 0.000014%, utilizes cleaning equipment to clean, remove dust, the oil stain on surface, put into drying baker, dry at 80 DEG C; Silicon material after drying is put into plumbago crucible 17, plumbago crucible 17 is moved in equipment and positions; Plumbago crucible 17 is put into graphite heating body 9, and graphite heating body 9 added graphite heat insulation sheath 8, plays insulation effect.
(2) equipment is closed stove, opening device cooling circulating water device, leads to cooling circulating water by refrigeration cycle water pipe 12 to equipment; Open body of heater vacuum system, first after utilizing body of heater 5 vacuum system side mechanical pump 14 and side lobe pump 15 that body of heater vacuum is evacuated to 1Pa, close side mechanical pump 14 and side lobe pump 15, pass into argon gas, to body of heater internal pressure to 50KPa by inflation valve 13 to body of heater 5 inside.
(3) in movement, graphite cover plate 7 covers to plumbago crucible 17 top, starts water-cooled ingot pulling mechanism 11; Be energized to graphite heating body 9, temperature rise rate is 200 DEG C/h, and to 1550 DEG C of insulation 6h, silicon material melts completely.
(4) close inflation valve 13, stop applying argon gas in body of heater 5; Remove the graphite cover plate 7 on plumbago crucible 17, body of heater 5 vacuum tightness is evacuated to 8Pa by startup side mechanical pump 14 and side lobe pump 15, then side diffusion pump 16 is started, the vacuum tightness of body of heater 5 is evacuated to 0.004Pa, start upper mechanical pump 2, upper lobe pump 3 and upper molecular pump 4 simultaneously, electron beam gun 1 vacuum tightness is evacuated to 0.0004Pa.Pre-thermionic electron guns 1, is set to 800mA by heater current, to electron beam gun 1 preheating 15min, closes preheating button; Setting electron beam gun 1 power is 100kW, and unlocking electronic rifle 1, in increase power process, controls electron beam 19 energy distribution; Utilize electron beam 19 pairs of silicon melt 6 surfaces to carry out electron beam melting, increase the thermograde of silicon melt 6 surface and surperficial following near zone, the disturbance of strengthening silicon melt 6, strengthens the surface effects that phosphorus volatilization is removed, removes the phosphorus impurities in silicon; After melting 3h, the phosphorus impurities in silicon is removed efficiently, and closes electron beam gun 1.
(5) in movement, graphite cover plate 7 covers to plumbago crucible 17 top, in body of heater 5, be filled with argon gas by inflation valve 17, air pressure remains on 50KPa, starts water-cooled ingot pulling mechanism 11, draw ingot speed to be 0.15mm/min, plumbago crucible 17 is pulled out graphite heating body 9 thermal field; After plumbago crucible 17 removes graphite heating body 9 completely, close water-cooled ingot pulling mechanism 11, long brilliant end of processing.
(6) control graphite heating body 9, temperature of thermal field is set in 1300 DEG C, start water-cooled ingot pulling mechanism 11, plumbago crucible 17 is risen up into thermal field, and be incubated 3h at 1300 DEG C after, controlling graphite heating body 9 rate of temperature fall is 100 DEG C/h, make ingot casting temperature be down to 1000 DEG C, close graphite heating body 9 power supply.
(7) after 10h cools, open purging valve 10, exit to equipment, then ingot casting is taken out in blow-on.
Embodiment 3:
Adopt the device in embodiment 1 to carry out electron beam melting to be coupled with crystal growing technology and to prepare polysilicon:
(1) be 0.005% by 500kg phosphorus content, metal content is 0.00008%, Boron contents is the polycrystalline silicon material of 0.000013%, utilizes cleaning equipment to clean, remove dust, the oil stain on surface, put into drying baker, dry at 80 DEG C; Silicon material after drying is put into plumbago crucible 17, plumbago crucible 17 is moved in equipment and positions; Plumbago crucible 17 is put into graphite heating body 9, and graphite heating body 9 added graphite heat insulation sheath 8, plays insulation effect.
(2) equipment is closed stove, opening device cooling circulating water device, leads to cooling circulating water by refrigeration cycle water pipe 12 to equipment; Open body of heater vacuum system, first after utilizing body of heater 5 vacuum system side mechanical pump 14 and side lobe pump 15 that body of heater 5 vacuum is evacuated to 0.5Pa, close side mechanical pump 14 and side lobe pump 15, pass into argon gas by inflation valve 13 to body of heater 5 inside, to body of heater 5 internal pressure to 48KPa.
(3) in movement, graphite cover plate 7 covers to plumbago crucible 17 top, starts water-cooled ingot pulling mechanism 11; Be energized to graphite heating body 9, temperature rise rate 250 DEG C/h, to 1550 DEG C of insulation 5h, silicon material melts completely.
(4) close inflation valve 13, stop applying argon gas in body of heater 5; Remove the graphite cover plate 7 on plumbago crucible 17, body of heater 5 vacuum tightness is evacuated to 9Pa by startup side mechanical pump 14 and side lobe pump 15, then side diffusion pump 16 is started, the vacuum tightness of body of heater 5 is evacuated to 0.003Pa, start upper mechanical pump 2, upper lobe pump 3 and upper molecular pump 4 simultaneously, electron beam gun 1 vacuum tightness is evacuated to 0.0003Pa.Pre-thermionic electron guns 1, is set to 850mA by heater current, to electron beam gun 1 preheating 15min, closes preheating button; Setting electron beam gun 1 power is 120kW, and unlocking electronic rifle 1, in increase power process, controls electron beam 19 energy distribution; Utilize electron beam 19 pairs of silicon melt 6 surfaces to carry out electron beam melting, increase the thermograde of silicon melt 6 surface and surperficial following near zone, the disturbance of strengthening silicon melt 6, strengthens the surface effects that phosphorus volatilization is removed, removes the phosphorus impurities in silicon; After melting 3h, the phosphorus impurities in silicon is removed efficiently, and closes electron beam gun 1.
(5) in movement, graphite cover plate 7 covers to plumbago crucible 17 top, in body of heater 5, be filled with argon gas by inflation valve 13, air pressure remains on 48KPa, starts water-cooled ingot pulling mechanism 11, draw ingot speed to be 0.13mm/min, plumbago crucible 17 is pulled out graphite heating body 9 thermal field; After plumbago crucible 17 removes graphite heating body 9 completely, close water-cooled ingot pulling mechanism 11, long brilliant end of processing.
(6) graphite heating body 9 is controlled, temperature of thermal field is set in 1250 DEG C, start water-cooled ingot pulling mechanism 11, plumbago crucible 17 is risen up into thermal field again, 3.5h is incubated at 1250 DEG C, controlling graphite heating body 9 rate of temperature fall is 100 DEG C/h, makes ingot casting temperature slowly, evenly be down to 1000 DEG C, closes graphite heating body 9 power supply.
(7) after 11h cools, open purging valve 10, exit to equipment, then ingot casting is taken out in blow-on.
Embodiment 4:
Adopt the device in embodiment 1 to carry out electron beam melting to be coupled with crystal growing technology and to prepare polysilicon:
(1) be 0.005% by 500kg phosphorus content, metal content is 0.00007%, Boron contents is the polycrystalline silicon material of 0.000013%, utilizes cleaning equipment to clean, remove dust, the oil stain on surface, put into drying baker, dry at 80 DEG C; Silicon material after drying is put into plumbago crucible 17, plumbago crucible 17 is moved in equipment and positions; Plumbago crucible 17 is put into graphite heating body 9, and graphite heating body 9 added graphite heat insulation sheath 8, plays insulation effect.
(2) equipment is closed stove, opening device cooling circulating water device, leads to cooling circulating water by refrigeration cycle water pipe 12 to equipment; Open body of heater vacuum system, first after utilizing body of heater 5 vacuum system side mechanical pump 14 and side lobe pump 15 that body of heater 5 vacuum is evacuated to 0.5Pa, close side mechanical pump 14 and side lobe pump 15, pass into argon gas by inflation valve 13 to body of heater 5 inside, to body of heater 5 internal pressure to 48KPa.
(3) in movement, graphite cover plate 7 covers to plumbago crucible 17 top, starts water-cooled ingot pulling mechanism 11; Be energized to graphite heating body 9, temperature rise rate 220 DEG C/h, to 1550 DEG C of insulation 5.5h, silicon material melts completely.
(4) close inflation valve 13, stop applying argon gas in body of heater 5; Remove the graphite cover plate 7 on plumbago crucible 17, body of heater 5 vacuum tightness is evacuated to 8Pa by startup side mechanical pump 14 and side lobe pump 15, then side diffusion pump 16 is started, the vacuum tightness of body of heater 5 is evacuated to 0.003Pa, start upper mechanical pump 2, upper lobe pump 3 and upper molecular pump 4 simultaneously, electron beam gun 1 vacuum tightness is evacuated to 0.0003Pa.Pre-thermionic electron guns 1, is set to 780mA by heater current, to electron beam gun 1 preheating 15min, closes preheating button; Setting electron beam gun 1 power is 120kW, and unlocking electronic rifle 1, in increase power process, controls electron beam 19 energy distribution; Utilize electron beam 19 pairs of silicon melt 6 surfaces to carry out electron beam melting, increase the thermograde of silicon melt 6 surface and surperficial following near zone, the disturbance of strengthening silicon melt 6, strengthens the surface effects that phosphorus volatilization is removed, removes the phosphorus impurities in silicon; After melting 3h, the phosphorus impurities in silicon is removed efficiently, and closes electron beam gun 1.
(5) in movement, graphite cover plate 7 covers to plumbago crucible 17 top, in body of heater 5, be filled with argon gas by inflation valve 17, air pressure remains on 48KPa, starts water-cooled ingot pulling mechanism 11, draw ingot speed to be 0.14mm/min, plumbago crucible 17 is pulled out graphite heating body 9 thermal field; After plumbago crucible 17 removes graphite heating body 9 completely, close water-cooled ingot pulling mechanism 11 and graphite heating body 9 power supply, long brilliant end of processing.
(6) control graphite heating body 9, temperature of thermal field is set in 1200 DEG C, starts water-cooled ingot pulling mechanism 11, plumbago crucible 17 is risen up into thermal field again, at 1200 DEG C, is incubated 4h, controlling graphite heating body 9 rate of temperature fall is 120 DEG C/h, make ingot casting temperature be down to 1000 DEG C, close graphite heating body 9 power supply.
(7) after 11.5h cools, open purging valve 10, exit to equipment, then ingot casting is taken out in blow-on.
In sum, electron beam melting technology and long brilliant process are coupled by this device effectively, thus achieve the object realizing two kinds of production technique on the same device, graphite heating body is utilized to carry out melted silicon material, utilize electron irradiated silicon bath surface, strengthening surface volatilization effect, volatility phosphorus impurities in efficient removal silicon, then long crystalline substance is carried out, decrease fragmentation, cleaning and dry link, saving input and the floor space of relevant device, greatly reducing energy expenditure during independent production, total energy consumption decreases beyond 30%, and production efficiency can improve 40%.