CN109133067A - A kind of method and device improving electron-beam smelting polysilicon efficiency - Google Patents
A kind of method and device improving electron-beam smelting polysilicon efficiency Download PDFInfo
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- CN109133067A CN109133067A CN201811202472.XA CN201811202472A CN109133067A CN 109133067 A CN109133067 A CN 109133067A CN 201811202472 A CN201811202472 A CN 201811202472A CN 109133067 A CN109133067 A CN 109133067A
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Abstract
The present invention relates to solar-grade polysilicon manufacturing field more particularly to a kind of method and devices for improving electron-beam smelting polysilicon efficiency.The present invention has melting kettle, and the joint angle between the side wall and bottom plate of melting kettle is equipped with inside inclined surface, and tilt angle is 45 ° -60 °, reduces the thickness of marginal position solidification layer in fusion process, enhances the Smelting Effect of electron beam.The present invention shortens the production time by the beam scanning pattern of different phase in control electron-beam smelting polysilicon process when device is used to improve the efficiency of electron-beam smelting polysilicon, reduces production energy consumption, improves production efficiency.
Description
Technical field
The present invention relates to solar-grade polysilicon manufacturing field more particularly to a kind of raising electron-beam smelting polysilicon efficiency
Method and device.
Background technique
Electron-beam smelting prepares the important process composition portion in the entire production procedure of solar-grade polysilicon as metallurgy method
Point, it can efficiently remove the volatile impurity in silicon (including P, O etc.).Under conventional process conditions, electron-beam smelting process compares
To examine single, electron beam does not consider beam scanning pattern, but under the conditions of high-power, silicon material is irradiated, silicon material is melted
And melting, the energy consumption in entire production process is higher, this also becomes the extensively hair application on a large scale of limitation electron-beam smelting polysilicon
One important limiting factor.
Summary of the invention
The technical problem to be solved by the present invention is under conventional process conditions, electron-beam smelting process compares single, the electronics of inspection
Beam does not consider beam scanning pattern, but under the conditions of high-power, silicon material is irradiated, fusing and melting are carried out to silicon material, entirely
Energy consumption in production process is higher, this also becomes the important limitation that limitation electron-beam smelting polysilicon extensively sends out application on a large scale
Factor.
To solve the above problems, the present invention proposes a kind of method and device for improving electron-beam smelting polysilicon efficiency, lead to
The beam scanning pattern of different phase in control electron-beam smelting polysilicon process is crossed, to improve electron-beam smelting polysilicon
Efficiency shortens the production time, reduces production energy consumption, improves production efficiency.
In order to achieve the above objectives, the present invention is realized by the following technical scheme: a kind of raising electron-beam smelting polysilicon efficiency
Device there is melting kettle as Figure 3-Figure 4, joint angle between the side wall and bottom plate of melting kettle is equipped with inside
Inclined surface, tilt angle are 45 ° -60 °, reduce the thickness of marginal position solidification layer in fusion process, enhance the melting of electron beam
Effect.
Further, melting kettle torsion shaft, melting kettle axis and mechanism are connected below melting kettle to connect by dynamic sealing
It connects, melting kettle turning hydraulic system is equipped with outside mechanism and moves horizontally motor, melting kettle is realized by hydraulic system
Turn over function manipulates moving horizontally for melting kettle by moving horizontally motor.
Further, as shown in Fig. 5-Fig. 6, the cooling water channel of melting kettle is divided into side wall water route and bottom water route totally two
Road carries out cooling processing respectively, plays the good effect that cools, while reducing the integrally-built difficulty of processing of crucible, side
Wall water route uses spiral waterway structure, and single channel water channel, cooling water enters by bottom, flowed out by top, using the water inlet mode,
It can guarantee the stability of cooling water inside water route；Bottom water route uses spiral waterway structure, and cooling water is passed through by crucible bottom
It inside crucible, is flowed out by circulating from crucible side, guarantees the homogeneity of cold-crucible bottom coohng ability, electron beam is molten
During refining, molten bath middle position temperature is higher, and such design can play cooling effect and protective effect.
Further, as shown in Figure 1, it is described improve electron-beam smelting polysilicon efficiency device further include feeding mechanism,
Furnace body, electron gun, melting kettle, solidification crucible；Feeding structure is connected to the upper end of furnace body, the side of furnace body and suction vacuum structure
It is connected, top is electron gun, downward launching electronics beam, and electron gun is connected with vacuum structure is inhaled；Furnace body is interior, electron beam irradiation side is
Melting kettle, the rear end of melting kettle are located at below the feeding port of feeding mechanism, and fluid guidance port end is located in the opening of solidification crucible
Side；Solidification crucible is set to bottom of furnace body.
Further, the suction vacuum structure of the side of the furnace body is sequentially connected mechanical pump I, lobe pump I, diffusion
Pump, the end of diffusion pump are connected with furnace body, furnace room air are taken away, construct vacuum environment；The suction vacuum knot of electron gun side
Structure is sequentially connected molecular pump, lobe pump II, mechanical pump II, and the end of molecular pump is connected with electron gun, and building electron beam is molten
Vacuum condition required for refining；The side of furnace body is equipped with charge valve.
A method of the electronics beam scanning improving electron-beam smelting polysilicon efficiency, using above-mentioned apparatus, electron beam
Scan pattern and Energy distribution be divided into 8 regions, 1-8# total energy value adds up to 100%；Wherein 1#, 2#, 3#, 4#, 5#, 6#
Outside region, 1# and the corner 6# overlay region, 5# and the corner 6# overlay region are constituted counterclockwise, and 2# is Chong Die with the corner 3#
Area, 3# and the corner 4# overlay region, make 1.5-2.5 times of the Energy distribution normal region at 4 angles of melting kettle；The region 7# with
The region 1#, 5#, 6#, 8# is adjacent, and the region 8# is adjacent with the region 2#, 3#, 4#, 7#.It is swept in melting stage scan pattern, smelt stage
Mode and casting stage scan pattern are retouched using different Energy distributions, Energy distribution is as follows:
Melting stage scan pattern: the region 1#: 5%-10%；The region 2#: 2%-3%；The region 3#: 3%-5%；The area 4#
Domain: 2%-3%；The region 5#: 5%-10%；The region 6#: 10%-15%；The region 7#: 35%-45%；The region 8#: 20%-
30%；Since silicon raw material is concentrated mainly on melting kettle rear end, it is close to increase energy of the electron beam in melting kettle back-end region
Degree, beam energy are concentrated mainly in the silicon raw material of tapered accumulation, can increase the burn-off rate of silicon raw material, meanwhile,
His area distribution has that energy density is lower, guarantees to remain to be maintained at liquid after the silicon liquid formed after melting silicon materials flows to other positions
State；
Smelt stage scan pattern: the region 1#: 7%-10%；The region 2#: 7%-10%；The region 3#: 7%-10%；The area 4#
Domain: 7%-10%；The region 5#: 7%-10%；The region 6#: 7%-10%；The region 7#: 20%-30%；The region 8#: 20%-
30%；Under the mode, the energy profile density of electron beam irradiation area is lower in melting kettle center, in melting kettle
Bottom and side wall juncture area are relatively high, in melting kettle four corners position highest, mainly due to melting kettle interposition
The cooling capacity set is weaker, and stronger close to bottom and side wall juncture area cooling capacity, the cooling capacity of four corners is most strong, electricity
Beamlet energy density distribution is corresponding, guarantees the smelting temperature in molten bath in silicon molten bath, meanwhile, reduce the stronger position of cooling capacity
Set the thickness of silicon solidification layer；
Casting stage scan pattern: the region 1#: 3%-5%；The region 2#: 6%-10%；The region 3#: 8%-12%；The area 4#
Domain: 6%-10%；The region 5#: 3%-5%；The region 6#: 2%-4%；The region 7#: 15%-20%；The region 8#: 45%-55%；
Since in silicon liquid casting process, with the increase of crucible overturning degree, silicon liquid will converge to the region close to melting kettle casting gate
Collection, increases the depth in the region silicon molten bath, to guarantee that silicon molten bath lower area is kept molten by, needs to increase electric in the region
The energy density of beamlet, meanwhile, melting kettle rear end silicon liquid is flowed to casting gate, and silicon liquid will fade away, and exposes the silicon of bottom
Solidification layer, energy needed for the region is less at this time, and back-end region energy is maintained lower energy density.
Specifically includes the following steps:
Step 1: wherein P content is 10-50ppm, O content 5- by the clean silicon material after over cleaning, drying
The blocky silicon raw material of 100ppm, total 800kg are respectively charged into the feeding mechanism of electron beam furnace；
Step 2: closing furnace, and lead to cooling circulating water to equipment, using the mechanical pump I of electron beam furnace furnace chamber vacuum system,
Furnace chamber vacuum is evacuated to 5 × 10 by lobe pump I, diffusion pump-2Pa hereinafter, using electron gun vacuum system mechanical pump II, lobe pump
II, electron gun inner vacuum is evacuated to 5 × 10 by molecular pump-3Pa is hereinafter, reach vacuum condition required for electron-beam smelting；
Step 3: being preheated to electron gun, electron gun filament electric current is set as 800-1000mA, electron gun is carried out
10-15min the pre-heat treatment, it is synchronous, during pre- thermionic electron guns, start feeding mechanism, 50kg silicon is conveyed into melting kettle
Raw material, silicon raw material are transported to tapered accumulation inside melting kettle；
Step 4: close the preheating mode of electron gun after electron gun preheats, start the irradiation mode of electron gun, if
Determining irradiation power is 150-180kW, while electron gun irradiation mode is set as " melting stage scan pattern " (electronics beam scanning
Region division is at 8 subregions, in electron beam scanning process, beam energy distribution electron beam residence time in a certain region
The percentage of intermittent scanning time is accounted for characterize, the scan period is for electron beam irradiation position from initial position according to certain movement rail
Mark scanning, since initial position, returns the time of initial position), since silicon raw material is concentrated mainly on melting kettle rear end,
Increase energy density of the electron beam in melting kettle back-end region, the silicon that beam energy is concentrated mainly on tapered accumulation is former
On material, the burn-off rate of silicon raw material can be increased, meanwhile, other area distributions have that energy density is lower, after guaranteeing melting silicon materials
The silicon liquid of formation remains to be maintained at liquid after flowing to other positions；
Energy distribution: the region 1#: 5%-10%；The region 2#: 2%-3%；The region 3#: 3%-5%；The region 4#: 2%-
3%；The region 5#: 5%-10%；The region 6#: 10%-15%；The region 7#: 35%-45%；The region 8#: 20%-30%；1-8# is total
Energy value adds up to 100%；
Step 5: forming liquid-state silicon molten bath after the silicon raw material in melting kettle is completely melt, change electronics beam scanning mould
Formula is " smelt stage scan pattern ", and the melting of 10-20min is carried out to silicon molten bath, removes volatile impurity therein；
Under the mode, the energy profile density of electron beam irradiation area is lower in melting kettle center, in melting earthenware
Crucible bottom and side wall juncture area are relatively high, in melting kettle four corners position highest, among melting kettle
The cooling capacity of position is weaker, and stronger close to bottom and side wall juncture area cooling capacity, the cooling capacity of four corners is most strong,
Beam energy Density Distribution is corresponding, guarantees the smelting temperature in molten bath in silicon molten bath, meanwhile, it is stronger to reduce cooling capacity
The thickness of position silicon solidification layer；
Energy distribution: the region 1#: 7%-10%；The region 2#: 7%-10%；The region 3#: 7%-10%；The region 4#: 7%-
10%；The region 5#: 7%-10%；The region 6#: 7%-10%；The region 7#: 20%-30%；The region 8#: 20%-30%；1-8# is total
Energy value adds up to 100%；Melting kettle four overlappings by scanning area energy density improve Energy distribution (1# and the corner 6#
Overlay region, 5# and the corner 6# overlay region, 2# and the corner 3# overlay region, 3# and the corner 4# overlay region), make 4 angles of melting kettle
Energy distribution is 1.5-2.5 times of normal region；
Step 6: silicon molten bath, after the melting of 10-20min, volatile impurity element therein is removed efficiently, open
Dynamic melting kettle turnover mechanism, the rotation of melting kettle torsion shaft drive melting kettle rotation, simultaneously, by electronics beam scanning
Mode is set as " casting stage scan pattern ", and the silicon liquid in silicon molten bath is flowed to the casting gate of melting kettle, and silicon liquid passes through casting
Mouth flows into solidification crucible, and silicon liquid fast cooling in solidification crucible solidifies, and forms solid-state silicon；
Since in silicon liquid casting process, with the increase of crucible overturning degree, silicon liquid will be to close to melting kettle casting gate
Region collect, increase the depth in the region silicon molten bath, for guarantee silicon molten bath lower area be kept molten by, need increase should
The energy density of electron beam in region, meanwhile, melting kettle rear end silicon liquid is flowed to casting gate, and silicon liquid will fade away, and is exposed
The silicon solidification layer of bottom, energy needed for the region is less at this time, and back-end region energy is maintained lower energy density；
Energy distribution: the region 1#: 3%-5%；The region 2#: 6%-10%；The region 3#: 8%-12%；The region 4#: 6%-
10%；The region 5#: 3%-5%；The region 6#: 2%-4%；The region 7#: 15%-20%；The region 8#: 45%-55%；1-8# total energy
Magnitude adds up to 100%；
Step 7: after the silicon liquid in melting kettle is dumped into solidification crucible completely, electron gun is closed, and by melting earthenware
Crucible is reset to original horizontal position；
Step 8: conveying 50kg silicon raw material into melting kettle again by feeding mechanism, the 4th step to the 7th step is repeated
Process melts silicon raw material, melting and casting process.
Step 9: after to the complete melting of silicon material in feeding mechanism, close electron gun system, to equipment and solid-state silicon into
Row cooling down.
Step 10: the solid-state silicon ingot that melting finishes is taken out in blow-on.
The beneficial effects of the present invention are:
It is more in electron-beam smelting by the feature in silicon molten bath during the melting characteristics of combination electron beam and electron-beam smelting
Crystal silicon different phase (mainly has melting silicon materials, silicon material melting, silicon liquid casting), by adjusting the scan pattern and energy of electron beam
The control to whole process is realized in distribution, by changing the control of different phase electron beam irradiation energy Density Distribution, is realized
Efficient fusion, melting and the casting process of silicon material in whole process, take full advantage of the heating feature of electron-beam smelting, shorten
The production time of whole process, reduce production energy consumption, can be realized in the case where reaching identical purification purpose, the production time by
22h originally is reduced to 19h, and total production energy consumption reduces by 18%.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
Fig. 2 is energy profile of the invention.
Fig. 3 is the side cross-sectional views of melting kettle of the present invention；
Fig. 4 is the front cross-sectional view of melting kettle of the present invention；
Fig. 5 is the side wall water-cooling structure figure of melting kettle of the present invention；
Fig. 6 is the bottom water-cooling structure figure of melting kettle of the present invention；
In figure, 1. electron guns, 2. molecular pumps, 3. lobe pumps II, 4. mechanical pumps II, 5. furnace bodies, 6. electron beams, 7. casting
Mouth, 8. silicon molten baths, 9. melting kettles, 91. water inlets, 92. water outlets, 10. solidification crucibles, 11. silicon liquids, 12. solid-state silicon, 13.
Melting kettle torsion shaft, 14. mechanical pumps I, 15. lobe pumps I, 16. diffusion pumps, 17. charge valves, 18. silicon raw materials, 19. feeders
Structure.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described.Obviously, described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Embodiment 1:
As Figure 3-Figure 4, a kind of device improving electron-beam smelting polysilicon efficiency, has melting kettle, melting earthenware
Joint angle between the side wall and bottom plate of crucible 9 is equipped with inside inclined surface, and tilt angle is 45 ° -60 °, reduces in fusion process
The thickness of marginal position solidification layer enhances the Smelting Effect of electron beam.
As shown in Figure 1, the device for improving electron-beam smelting polysilicon efficiency further includes feeding mechanism 19, furnace body 5, electricity
Sub- rifle 1, melting kettle 9, solidification crucible 10；Feeding structure 19 is connected to the upper end of furnace body 5, the side of furnace body 5 and suction vacuum knot
Structure be connected, top be electron gun 1, downward launching electronics beam 6, electron gun 1 with suction vacuum structure be connected；In furnace body 5, electron beam 6
Irradiation side is melting kettle 9, and the rear end of melting kettle 9 is located at below the feeding port of feeding mechanism 19, and fluid guidance port end is located at solidification
The overthe openings of crucible 10；Solidification crucible 10 is set to 5 bottom of furnace body.
The suction vacuum structure of the side of the furnace body 5 be sequentially connected mechanical pump I 14, lobe pump I 15, diffusion pump 16,
The end of diffusion pump is connected with furnace body, and furnace room air is taken away, constructs vacuum environment；The suction vacuum structure of 1 side of electron gun
End for sequentially connected molecular pump 2, lobe pump II 3, mechanical pump II 4, molecular pump is connected with electron gun 1, constructs electron beam
Vacuum condition required for melting；The side of furnace body 5 is equipped with charge valve 17.
A method of improving electron-beam smelting polysilicon efficiency, using above-mentioned apparatus, the scan pattern of electron beam and
Energy distribution is divided into 8 regions, and 1-8# total energy value adds up to 100%；Wherein 1#, 2#, 3#, 4#, 5#, 6# be counterclockwise
Constitute outside region, 1# and the corner 6# overlay region, 5# and the corner 6# overlay region, 2# and the corner 3# overlay region, 3# and the corner 4#
Overlay region makes 1.5-2.5 times of the Energy distribution normal region at 4 angles of melting kettle；The region 7# and the region 1#, 5#, 6#, 8#
Adjacent, the region 8# is adjacent with the region 2#, 3#, 4#, 7#.This 8 regions are according to actual conditions in production process, in conjunction with electron beam
Melting characteristics, water jacketed copper crucible cooling feature and the optimal setting that carries out, setting are excessive, increase the complexity of control, it is very few
Corresponding effect is then not achieved.It is used in melting stage scan pattern, smelt stage scan pattern and casting stage scan pattern
Different Energy distributions, Energy distribution are as follows:
Melting stage scan pattern: the region 1#: 5%-10%；The region 2#: 2%-3%；The region 3#: 3%-5%；The area 4#
Domain: 2%-3%；The region 5#: 5%-10%；The region 6#: 10%-15%；The region 7#: 35%-45%；The region 8#: 20%-
30%；Since silicon raw material is concentrated mainly on melting kettle rear end, it is close to increase energy of the electron beam in melting kettle back-end region
Degree, beam energy are concentrated mainly in the silicon raw material 18 of tapered accumulation, can increase the burn-off rate of silicon raw material 18, together
When, other area distributions have that energy density is lower, guarantee still to be able to maintain after the silicon liquid formed after melting silicon materials flows to other positions
In liquid；
Smelt stage scan pattern: the region 1#: 7%-10%；The region 2#: 7%-10%；The region 3#: 7%-10%；The area 4#
Domain: 7%-10%；The region 5#: 7%-10%；The region 6#: 7%-10%；The region 7#: 20%-30%；The region 8#: 20%-
30%；Under the mode, the energy profile density of electron beam irradiation area is lower in 9 center of melting kettle, in melting kettle
9 bottoms and side wall juncture area are relatively high, in 9 four corners position highest of melting kettle, among melting kettle 9
The cooling capacity of position is weaker, and stronger close to bottom and side wall juncture area cooling capacity, the cooling capacity of four corners is most strong,
Beam energy Density Distribution is corresponding, guarantee silicon molten bath 8 in molten bath smelting temperature, meanwhile, reduce cooling capacity compared with
The thickness of strong position silicon solidification layer；
Casting stage scan pattern: the region 1#: 3%-5%；The region 2#: 6%-10%；The region 3#: 8%-12%；The area 4#
Domain: 6%-10%；The region 5#: 3%-5%；The region 6#: 2%-4%；The region 7#: 15%-20%；The region 8#: 45%-55%；
Since in silicon liquid casting process, with the increase of crucible overturning degree, silicon liquid will converge to the region close to melting kettle casting gate
Collection, increases the depth in the region silicon molten bath, to guarantee that silicon molten bath lower area is kept molten by, needs to increase electric in the region
The energy density of beamlet, meanwhile, melting kettle rear end silicon liquid is flowed to casting gate, and silicon liquid will fade away, and exposes the silicon of bottom
Solidification layer, energy needed for the region is less at this time, and back-end region energy is maintained lower energy density.
Specifically includes the following steps:
Step 1: wherein P content is 10-50ppm, O content 5- by the clean silicon material after over cleaning, drying
The blocky silicon raw material 18 of 100ppm, total 800kg are respectively charged into the feeding mechanism 19 of electron beam furnace；
Step 2: closing furnace, and lead to cooling circulating water to equipment, utilizes the mechanical pump I of electron beam furnace furnace chamber vacuum system
14, furnace chamber vacuum is evacuated to 5 × 10 by lobe pump I 15, diffusion pump 16-2Pa hereinafter, using 1 vacuum system of electron gun mechanical pump
II 4,1 inner vacuum of electron gun is evacuated to 5 × 10 by lobe pump II 3, molecular pump 2-3Pa is hereinafter, reach required for electron-beam smelting
Vacuum condition；
Step 3: preheat to electron gun 1, set 1 heater current of electron gun as 800-1000mA, to electron gun 1 into
Row 10-15min the pre-heat treatment, it is synchronous, during pre- thermionic electron guns 1, starts feeding mechanism 19, conveyed into melting kettle 9
50kg silicon raw material 18, silicon raw material 18 are transported to the 9 tapered accumulation in inside of melting kettle；
Step 4: closing the preheating mode of electron gun 1 after electron gun 1 preheats, start the irradiation mode of electron gun 1,
Irradiation power is set as 150-180kW, while 1 irradiation mode of electron gun is set as " melting stage scan pattern " (electron beam
Scanning area is divided into 8 subregions, and in electron beam scanning process, beam energy distribution is stopped in a certain region with electron beam
Time accounts for the percentage of intermittent scanning time to characterize, and the scan period is that electron beam irradiation position is transported from initial position according to certain
Dynamic track scanning returns the time of initial position since initial position), since silicon raw material is concentrated mainly on melting kettle
Rear end, increases energy density of the electron beam in melting kettle back-end region, and beam energy is concentrated mainly on tapered accumulation
Silicon raw material 18 on, the burn-off rate of silicon raw material 18 can be increased, meanwhile, other area distributions have that energy density is lower, guarantee
The silicon liquid formed after melting silicon materials remains to be maintained at liquid after flowing to other positions；
Energy distribution: the region 1#: 5%-10%；The region 2#: 2%-3%；The region 3#: 3%-5%；The region 4#: 2%-
3%；The region 5#: 5%-10%；The region 6#: 10%-15%；The region 7#: 35%-45%；The region 8#: 20%-30%；1-8# is total
Energy value adds up to 100%；
Step 5: forming liquid-state silicon molten bath 8 after the silicon raw material in melting kettle 9 is completely melt, change electronics beam scanning
Mode is " smelt stage scan pattern ", and the melting of 10-20min is carried out to silicon molten bath 8, removes volatile impurity therein；
Under the mode, the energy profile density of electron beam irradiation area is lower in 9 center of melting kettle, in melting
9 bottom of crucible and side wall juncture area are relatively high, in 9 four corners position highest of melting kettle, mainly due to melting kettle 9
The cooling capacity in middle position is weaker, stronger close to bottom and side wall juncture area cooling capacity, the cooling capacity of four corners
Most strong, beam energy Density Distribution is corresponding, guarantees the smelting temperature in molten bath in silicon molten bath 8, meanwhile, reduce cooling energy
Thickness of the power compared with strong position silicon solidification layer；
Energy distribution: the region 1#: 7%-10%；The region 2#: 7%-10%；The region 3#: 7%-10%；The region 4#: 7%-
10%；The region 5#: 7%-10%；The region 6#: 7%-10%；The region 7#: 20%-30%；The region 8#: 20%-30%；1-8# is total
Energy value adds up to 100%；Melting kettle four overlappings by scanning area energy density improve Energy distribution (1# and the corner 6#
Overlay region, 5# and the corner 6# overlay region, 2# and the corner 3# overlay region, 3# and the corner 4# overlay region), make 4 angles of melting kettle
Energy distribution is 1.5-2.5 times of normal region；
Step 6: silicon molten bath 8, after the melting of 10-20min, volatile impurity element therein is removed efficiently,
Start 9 turnover mechanism of melting kettle, melting kettle torsion shaft 13 rotates, and drives melting kettle 9 to rotate, simultaneously, by electronics
Beam scanning mode is set as " casting stage scan pattern ", and the silicon liquid in silicon molten bath 8 is flowed to the casting gate 7 of melting kettle 9, silicon liquid
It is flowed into solidification crucible 10 by casting gate 7, the fast cooling in solidification crucible 10 of silicon liquid 11 solidifies, and forms solid-state silicon 12；
Since in silicon liquid casting process, with the increase of crucible overturning degree, silicon liquid will be to close to melting kettle casting gate
Region collect, increase the depth in the region silicon molten bath, for guarantee silicon molten bath lower area be kept molten by, need increase should
The energy density of electron beam in region, meanwhile, melting kettle rear end silicon liquid is flowed to casting gate, and silicon liquid will fade away, and is exposed
The silicon solidification layer of bottom, energy needed for the region is less at this time, and back-end region energy is maintained lower energy density；
Energy distribution: the region 1#: 3%-5%；The region 2#: 6%-10%；The region 3#: 8%-12%；The region 4#: 6%-
10%；The region 5#: 3%-5%；The region 6#: 2%-4%；The region 7#: 15%-20%；The region 8#: 45%-55%；1-8# total energy
Magnitude adds up to 100%；
Step 7: after the silicon liquid in melting kettle is dumped into solidification crucible 10 completely, electron gun is closed, and by melting
Crucible 9 is reset to original horizontal position；
Step 8: conveying 50kg silicon raw material 18 into melting kettle 9 again by feeding mechanism 19, the 4th step is repeated to the
Seven step processes melt silicon raw material 18, melting and casting process.
Step 9: electron gun system is closed, to equipment and solid-state silicon after to the complete melting of silicon material in feeding mechanism 19
12 carry out cooling down.
Step 10: the solid-state silicon ingot that melting finishes is taken out in blow-on.
Embodiment 2:
Melting kettle torsion shaft 13 is connected below melting kettle, melting kettle axis is connect with mechanism by dynamic sealing, mechanism
Outside is equipped with melting kettle turning hydraulic system and moves horizontally motor, and the overturning function of melting kettle is realized by hydraulic system
Can, moving horizontally for melting kettle is manipulated by moving horizontally motor.
Remaining is same as Example 1.
Embodiment 3:
As shown in Fig. 5-Fig. 6, the cooling water channel of melting kettle is divided into side wall water route and bottom water route is total to two-way, carries out respectively
Cooling processing, plays the good effect that cools, while reducing the integrally-built difficulty of processing of crucible, and side wall water route uses spiral shell
Rotating waterway structure, single channel water channel, cooling water are entered by the water inlet 91 of bottom, are flowed out by the water outlet 92 at top, using this
Water inlet mode can guarantee the stability of cooling water inside water route；Bottom water route uses spiral waterway structure, and cooling water is by crucible
The water inlet 91 of bottom is passed through inside crucible, is flowed out by circulating from the water outlet 92 of crucible side, guarantees cold-crucible
The homogeneity of bottom coohng ability, during electron-beam smelting, molten bath middle position temperature is higher, and such design can play
Cooling effect and protective effect.
Remaining is identical as embodiment 1 or embodiment 2.
Claims (7)
1. a kind of device for improving electron-beam smelting polysilicon efficiency, it is characterised in that: have melting kettle, the side of melting kettle
Joint angle between wall and bottom plate is equipped with inside inclined surface, and tilt angle is 45 ° -60 °.
2. improving the device of electron-beam smelting polysilicon efficiency as described in claim 1, it is characterised in that: below melting kettle
Connect melting kettle torsion shaft.
3. as described in claim 1 improve electron-beam smelting polysilicon efficiency device, it is characterised in that: melting kettle it is cold
But water route is divided into side wall water route and bottom water route is total to two-way, and side wall water route uses spiral waterway structure, single channel water channel, cooling water
Entered by bottom, is flowed out by top；Bottom water route uses spiral waterway structure, and cooling water is passed through inside crucible by crucible bottom,
It is flowed out by circulating from crucible side.
4. improving the device of electron-beam smelting polysilicon efficiency as described in claim 1, it is characterised in that: the raising electronics
The device of beam melting polysilicon efficiency further includes feeding mechanism, furnace body, electron gun, melting kettle, solidification crucible；Feeding structure connects
It connects in the upper end of furnace body, the side of furnace body is connected with vacuum structure is inhaled, and top is electron gun, downward launching electronics beam, electron gun
It is connected with vacuum structure is inhaled；Furnace body is interior, electron beam irradiation side is melting kettle, and the rear end of melting kettle is located at sending for feeding mechanism
Below material mouth, fluid guidance port end is located at the overthe openings of solidification crucible；Solidification crucible is set to bottom of furnace body.
5. improving the device of electron-beam smelting polysilicon efficiency as claimed in claim 4, it is characterised in that: the one of the furnace body
The suction vacuum structure of side is sequentially connected mechanical pump I, lobe pump I, diffusion pump, and the end of diffusion pump is connected with furnace body；Electronics
The suction vacuum structure of rifle side is sequentially connected molecular pump, lobe pump II, mechanical pump II, end and the electron gun phase of molecular pump
Even, vacuum condition required for electron-beam smelting is constructed；The side of furnace body is equipped with charge valve.
6. a kind of method for improving electron-beam smelting polysilicon efficiency, it is characterised in that: device described in claim 1 is used,
The scan pattern and Energy distribution of its electron beam are divided into 8 regions, and 1-8# total energy value adds up to 100%；Wherein 1#, 2#, 3#,
4#, 5#, 6# constitute outside region, 1# and the corner 6# overlay region, 5# and the corner 6# overlay region, 2# and the angle 3# counterclockwise
Portion overlay region, 3# and the corner 4# overlay region, the region 7# is adjacent with the region 1#, 5#, 6#, 8#, the region 8# and the region 2#, 3#, 4#, 7#
It is adjacent；It is as follows in the scan pattern of three phases:
Melting stage scan pattern: the region 1#: 5%-10%；The region 2#: 2%-3%；The region 3#: 3%-5%；The region 4#:
2%-3%；The region 5#: 5%-10%；The region 6#: 10%-15%；The region 7#: 35%-45%；The region 8#: 20%-30%；
Smelt stage scan pattern: the region 1#: 7%-10%；The region 2#: 7%-10%；The region 3#: 7%-10%；The region 4#:
7%-10%；The region 5#: 7%-10%；The region 6#: 7%-10%；The region 7#: 20%-30%；The region 8#: 20%-30%；
Casting stage scan pattern: the region 1#: 3%-5%；The region 2#: 6%-10%；The region 3#: 8%-12%；The region 4#:
6%-10%；The region 5#: 3%-5%；The region 6#: 2%-4%；The region 7#: 15%-20%；The region 8#: 45%-55%.
7. improving the method for electron-beam smelting polysilicon efficiency as claimed in claim 6, it is characterised in that: including following step
It is rapid:
Step 1: wherein P content is 10-50ppm by the clean silicon material after over cleaning, drying, O content is 5-100ppm's
Blocky silicon raw material, total 800kg are respectively charged into the feeding mechanism of electron beam furnace；
Step 2: closing furnace, and lead to cooling circulating water to equipment, utilizes the mechanical pump I of electron beam furnace furnace chamber vacuum system, Roots
I, diffusion pump are pumped, furnace chamber vacuum is evacuated to 5 × 10-2Pa hereinafter, using the mechanical pump II of electron gun vacuum system, lobe pump II,
Electron gun inner vacuum is evacuated to 5 × 10 by molecular pump-3Pa is hereinafter, reach vacuum condition required for electron-beam smelting；
Step 3: being preheated to electron gun, electron gun filament electric current is set as 800-1000mA, 10- is carried out to electron gun
15min the pre-heat treatment, it is synchronous, during pre- thermionic electron guns, start feeding mechanism, it is former that 50kg silicon is conveyed into melting kettle
Material, silicon raw material are transported to tapered accumulation inside melting kettle；
Step 4: closing the preheating mode of electron gun after electron gun preheats, start the irradiation mode of electron gun, setting is shone
Penetrating power is 150-180kW, while electron gun irradiation mode is set as " melting stage scan pattern "；Energy distribution: the area 1#
Domain: 5%-10%；The region 2#: 2%-3%；The region 3#: 3%-5%；The region 4#: 2%-3%；The region 5#: 5%-10%；The area 6#
Domain: 10%-15%；The region 7#: 35%-45%；The region 8#: 20%-30%；1-8# total energy value adds up to 100%；
Step 5: forming liquid-state silicon molten bath after the silicon raw material in melting kettle is completely melt, changing beam scanning pattern is
" smelt stage scan pattern " carries out the melting of 10-20min to silicon molten bath, removes volatile impurity therein；Energy distribution:
The region 1#: 7%-10%；The region 2#: 7%-10%；The region 3#: 7%-10%；The region 4#: 7%-10%；The region 5#: 7%-
10%；The region 6#: 7%-10%；The region 7#: 20%-30%；The region 8#: 20%-30%；1-8# total energy value adds up to
100%；Melting kettle four improves Energy distribution, 1# and the corner 6# overlay region by the overlapping of scanning area energy density, 5# with
The corner 6# overlay region, 2# and the corner 3# overlay region, 3# and the corner 4# overlay region, make the Energy distribution at 4 angles of melting kettle be positive
1.5-2.5 times of normal region；
Step 6: silicon molten bath after the melting of 10-20min, starts melting kettle turnover mechanism, the rotation of melting kettle torsion shaft
Turn, drive melting kettle rotation, simultaneously, beam scanning pattern is set as " casting stage scan pattern ", silicon molten bath
Silicon liquid to the casting gate of melting kettle flow, silicon liquid by casting gate flow into solidification crucible in, silicon liquid in solidification crucible fastly
Fast cooling solidification forms solid-state silicon；Energy distribution: the region 1#: 3%-5%；The region 2#: 6%-10%；The region 3#: 8%-
12%；The region 4#: 6%-10%；The region 5#: 3%-5%；The region 6#: 2%-4%；The region 7#: 15%-20%；The region 8#:
45%-55%；1-8# total energy value adds up to 100%；
Step 7: closing electron gun, and melting kettle is answered after the silicon liquid in melting kettle is dumped into solidification crucible completely
Position is to original horizontal position；
Step 8: conveying 50kg silicon raw material into melting kettle again by feeding mechanism, the 4th step to the 7th step process is repeated,
Silicon raw material is melted, melting and casting process.
Step 9: closing electron gun system after to the complete melting of silicon material in feeding mechanism, being dropped to equipment and solid-state silicon
Temperature is cooling.
Step 10: the solid-state silicon ingot that melting finishes is taken out in blow-on.
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| JPH10273313A (en) * | 1997-03-28 | 1998-10-13 | Kawasaki Steel Corp | Production of polycrystal silicon ingot |
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| CN104528732A (en) * | 2014-12-25 | 2015-04-22 | 大连理工大学 | Novel device and method for reducing energy consumption of electron beam melting technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10273313A (en) * | 1997-03-28 | 1998-10-13 | Kawasaki Steel Corp | Production of polycrystal silicon ingot |
| CN1276026A (en) * | 1997-10-16 | 2000-12-06 | Memc电子材料有限公司 | Process for preparing silicon melt from polysilicon charge |
| CN101318655A (en) * | 2008-06-19 | 2008-12-10 | 大连理工大学 | Method and device for removing foreign matter of phosphor in polysilicon |
| TWM461635U (en) * | 2013-04-30 | 2013-09-11 | Utech Solar Corp | Crucible unit for crystal growth |
| CN203558861U (en) * | 2013-11-12 | 2014-04-23 | 青岛隆盛晶硅科技有限公司 | Water-cooled copper crucible applied to smelting polysilicon with electron beam |
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