CN102345164A - Efficient preparation method of silicon cores and silicon core preparation furnace - Google Patents
Efficient preparation method of silicon cores and silicon core preparation furnace Download PDFInfo
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- CN102345164A CN102345164A CN2011103055500A CN201110305550A CN102345164A CN 102345164 A CN102345164 A CN 102345164A CN 2011103055500 A CN2011103055500 A CN 2011103055500A CN 201110305550 A CN201110305550 A CN 201110305550A CN 102345164 A CN102345164 A CN 102345164A
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Abstract
The invention relates to a preparation process in the field of silicon core preparation and in particular relates to an efficient preparation method of silicon cores. The method comprises the following steps: heating and melting polysilicon in a quartz crucible, and cooling a molten silicon melting zone; driving multiple seed crystals to move downwards so that the seed crystals contact the silicon melting zone, and adjusting the temperature of the silicon melting zone and the lifting speed of the seed crystals so that the diameter of the seed crystals becomes larger and larger gradually; when the diameter of the silicon cores is close to a target diameter, controlling the diameter of the seed crystals to be subjected to equal diameter growth; and in the later growing stage, stopping feeding, controlling the speed to separate the silicon cores from the silicon melting zone according to the diameter of the silicon cores, then placing the pulled silicon cores at the silicon core storage position of a turntable, and moving a seedholder at a seedholder position to perform fusion splicing. The method corresponds to a special silicon core preparation furnace. The corn material, offcuts and the like obtained in the polycrystalline production process can be fully utilized in the method, thus the energy consumption, investment and labor cost of a polysilicon preparation process can be reduced and the production cost of the solar-grade polysilicon can also be reduced.
Description
Technical field
The present invention relates to the preparation technology of silicon core preparation field, method and silicon core that particularly a kind of high-level efficiency prepares the silicon core prepare stove.
Background technology
In recent years, with the crystal silicon battery being developed rapidly of main photovoltaic industry, the production of polysilicon technology is also in progressive fast.The silicon core is " seed " of producing polysilicon; Its preparation method has: patterning method, zone melting; Patterning method is because facility investment is big, maintenance cost is high at present, and the silicon material cuts reasons such as loss is big and fails to be used on a large scale, but zone melting has obtained using widely.
Though it is progressive constantly that Qu Rong prepares the technology of silicon core, also has some problems.Such as, from single core furnace five core stoves till now the earliest, the quantity that draws out the silicon core in the unit time has improved quite a few times; Improved production efficiency, but the adjustment that five core high frequency heating coil structure formations take place, and new structure requires higher to operators'skills; The porous coupling effect of coil and silicon material has also produced variation simultaneously; So occur that the spoilage of high frequency heating coil is also corresponding to be increased, the diameter of silicon core is also corresponding to have diminished, and it is big that ovality becomes; And most important still silicon core deposition rate surface-area diminishes, and space availability ratio is low in the reduction furnace, and the energy consumption of reduction furnace production unit product rises; For the personnel of drawing silicon core, the energy of input is bigger, and the skilled operation degree is had relatively high expectations, and the index of fuel rod is required harshness especially.
The used single crystal growing furnace of tradition vertical pulling method can only be used to prepare monocrystalline, once only to draw one, must pass through seeding, put point, the several key steps of isodiametric growth, and need grow the brilliant line of monocrystalline, and the drawing time is longer.All be not used in the preparation polycrystalline all the time, utilize improved single crystal growing furnace to come high-level efficiency to prepare the method for polysilicon core so now designed especially.
Summary of the invention
The method and the silicon core that the object of the present invention is to provide a kind of high-level efficiency to prepare the silicon core prepare stove; This method has overcome above-mentioned shortcoming; The policrystalline silicon that can prepare circles such as major diameter, and the quantity of a drawing silicon core can also be above 5, and masterbatch is the polysilicon that utilizes exterior quality relatively poor.
The technical scheme that the present invention adopts is:
A kind of high-level efficiency prepares the method for silicon core, it is characterized in that the preparation method is following:
The first step is contained in polysilicon in the quartz crucible, and is heated to and dissolves;
In second step, the silicon after dissolving in the quartz crucible is dissolved the district lower the temperature;
The 3rd step; The past decline of the cartridge device that has many silicon seeds; Many silicon seeds under the cartridge device are contacted with the molten district of silicon, dissolve the temperature in district and the pulling speed that silicon seed makes progress through adjustment silicon, the silicon seed diameter is become gradually becomes the silicon core greatly; When silicon core diameter during near aimed dia, the diameter of control silicon core is done isodiametric growth;
The 4th step; In the later stage of process of growth, quartz crucible stops feed, looks the pulling speed that silicon core diameter size is controlled silicon seed; Making silicon core and silicon dissolve the district breaks away from; Then will draw the silicon core of accomplishing and be placed on corresponding silicon core and deposit on the position, and the silicon seed chuck that pipettes on the silicon seed chuck position carries out welding, repeat top step again.
Heating temperature is up to 1410 ℃ in the said the first step.
Be to reach the cooling slightly of the molten district of silicon in said second step through heating power being reduced 2-5kw.
Remain through the adjustment heating power in said the 3rd step and adjust the temperature that silicon dissolves the district, the pulling speed that the while silicon seed makes progress is 0-15mm/min.
The silicon core that is used for this method prepares stove; Comprise silicon seed stationary installation (being foregoing cartridge device), quartz crucible and attemperator; The silicon seed stationary installation is fixed in the quartz crucible upper end; Quartz crucible is fixed on the quartz crucible supporting apparatus of graphite system, and the quartz crucible lower end is fixedly connected with the graphite axis, and it is inner that quartz crucible, quartz crucible supporting apparatus and graphite axis are positioned at tubular attemperator.
Said silicon seed stationary installation comprises guiding wireline, silicon seed chuck, and the guiding wireline is connected with the silicon seed chuck through the web member that is provided with silicon seed chuck fixed bit.
Said silicon seed chuck fixed bit place is provided with rotating disk, and rotating disk is positioned at the upper end of silicon seed chuck, and rotating disk is provided with the silicon core and deposits position and silicon seed chuck position.
Said rotating disk drives through gear train assembly, and gear train assembly drives transmission through shaking handle wheel.
Said attemperator comprises from the interior graphite heater that sets gradually outward, heat-preservation cylinder, carbon adiabator layer and stainless steel cylinder; The height of graphite heater is lower than the height of heat-preservation cylinder, carbon adiabator layer; The height of heat-preservation cylinder, carbon adiabator layer is lower than the height of stainless steel cylinder, and the upper end of said heat-preservation cylinder, carbon adiabator layer is provided with loam cake.
The detailed process that present method prepares the silicon core is following: at first polysilicon is placed on the quartz crucible internal heating to dissolving, then the silicon in the quartz crucible is dissolved the district and lower the temperature; Driving clamping through control guiding wireline again has the silicon seed chuck of many silicon seeds to move down, and makes the molten district of silicon seed and silicon contact, and dissolves the temperature in district and the pulling speed that silicon seed makes progress through adjustment silicon, is silicon seed drawing becoming silicon core gradually; When silicon core diameter during near aimed dia, through control pulling guiding steel cable, drive silicon seed and rise, make the silicon core break away from silicon and dissolve the district; Make the silicon core on the rotating disk deposit the silicon core that the bit alignment drawing obtains through shaking handle wheel then; Making the silicon core be positioned over the silicon core deposits on the position; After placement finishes; Continue to shake handle wheel and rotate rotating disk to silicon seed chuck position, utilize silicon seed chuck fixed bit to extract the silicon seed chuck on the rotating disk then, then dissolve the district and carry out welding through silicon seed chuck to the silicon on the gear train assembly decline silicon seed chuck position; Begin the drawing of a new round subsequently, subsequent step repeats the same.
If furnace diameter is little, can utilize dividing plate that the bottom (silicon dissolves parts such as district) of body of heater is cut apart with top drawing trip segment, treat to take out the silicon core after first round drawing is accomplished, then on silicon seed chuck fixed bit, reinstall the silicon seed chuck.
It is polycrystalline that method of the present invention can draw the silicon core that obtains, and once can draw many, need not pass through fully in the pulling process pulling monocrystal seeding, put point, isodiametric growth step, draw rate is obviously fast than the speed of pulling monocrystal.
Technique effect of the present invention is following:
The present invention can make the weak point of traditional silicon core preparation method improved significantly; Make full use of corn material in the polycrystalline production process, scrap stock etc.; Help reducing polysilicon and prepare the total energy consumption in the process and reduce equipment gross investment and labour cost, will help reducing the cost of producing solar-grade polysilicon.
Description of drawings
Fig. 1 is the cross-sectional view that silicon core of the present invention prepares stove
Fig. 2 be silicon core of the present invention prepare stove the contour structures synoptic diagram of rotating disk
Description of reference numerals is following:
1---silicon seed, 2---the silicon core, 3---silicon dissolves the district, and 4---loam cake; 5---the carbon adiabator layer, 6---graphite heater, 7---heat-preservation cylinder, 8---stainless steel cylinder; 9---the graphite axis, 10---the quartz crucible supporting apparatus of graphite system, 11---quartz crucible, 12---the silicon seed chuck; 13---the guiding wireline, 14---silicon seed chuck fixed bit, 15---rotating disk, 16---the silicon core is deposited the position; 17---silicon seed chuck position, 18---handle wheel, 19---gear train assembly.
Embodiment
Below in conjunction with embodiment and accompanying drawing present method is done further detailed description.
Present method is a kind of preparation method that can draw many silicon cores simultaneously, and its step is following:
The first step is contained in polysilicon in the quartz crucible 11, and is heated to and dissolves, and melting temperature is 1410 ℃;
In second step,, reach the silicon after dissolving in the quartz crucible 11 is dissolved the purpose that district 3 lowers the temperature slightly through heating power is reduced 2-5kw;
The 3rd step; The past decline of the cartridge device that has many silicon seeds 1; Many silicon seeds 1 under the cartridge device are contacted with the molten district 3 of silicon, dissolve the temperature in district 3 and the pulling speed that silicon seed 1 makes progress through adjustment silicon, silicon seed 1 diameter is become gradually becomes silicon core 2 greatly; When silicon core 2 diameters during near aimed dia, the diameter of control silicon core 2 is done isodiametric growth; Wherein, adjust the temperature that silicon dissolves district 3 through the adjustment heating power, the pulling speed that while silicon seed 1 makes progress is 0-15mm/min;
The 4th step; In the later stage of process of growth, quartz crucible 11 stops feed, looks the pulling speed that silicon core 2 diameter are controlled silicon seed 1; Making silicon core 2 and silicon dissolve district 3 breaks away from; Then will draw the silicon core of accomplishing 2 and be placed on accordingly and deposits on the position, and the silicon seed chuck 12 that pipettes on the silicon seed chuck position 17 carries out welding, repeat top step again.
The major equipment that present method is used is that the silicon core prepares stove, and the size of quartz crucible and the feeding quantity of polysilicon are decided according to the structure formation of silicon core, diameter, length, radical, simultaneously, silicon core output also with relation is arranged in work-ing life of crucible.
As shown in Figure 1; The structure that this silicon core prepares stove is following: comprise silicon seed stationary installation, quartz crucible 11 and attemperator; The silicon seed stationary installation is fixed in quartz crucible 11 upper ends; Quartz crucible 11 is fixed on the quartz crucible supporting apparatus 10 of graphite system, and quartz crucible 11 lower ends are fixedly connected with graphite axis 9, and it is inner that quartz crucible 11, quartz crucible supporting apparatus and graphite axis 9 are positioned at tubular attemperator; Said silicon seed stationary installation comprises guiding wireline 13, seed chuck; Guiding wireline 13 is connected with silicon seed chuck 12 through the web member that is provided with silicon seed chuck fixed bit 14; Said silicon seed chuck fixed bit 14 places are provided with rotating disk 15; Rotating disk 15 is positioned at the upper end of silicon seed chuck 12, and rotating disk 15 is provided with the silicon core and deposits position 16 and silicon seed chuck position 17; Said rotating disk 15 drives through gear train assembly 19, and gear train assembly 19 drives transmission through shaking handle wheel 18; Said attemperator comprises from the interior graphite heater that sets gradually outward 6, heat-preservation cylinder 7, carbon adiabator layer 5 and stainless steel cylinder 8; The height of graphite heater 6 is lower than the height of heat-preservation cylinder 7, carbon adiabator layer 5; The height of heat-preservation cylinder 7, carbon adiabator layer 5 is lower than the height of stainless steel cylinder 8, and the upper end of said heat-preservation cylinder 7, carbon adiabator layer 5 is provided with loam cake 4.
When selecting for use solid polycrystalline seed crystal (8-10mm) to carry out the welding crystal pulling, drawing length is 2500mm, and feeding quantity is that 45-50kg just can output 90-100 root silicon core amount so.
In this method, can adopt the corn material shape polysilicon of visual appearance difference to drop in the quartz crucible 11, utilize the thermal field heating, under argon gas atmosphere as masterbatch.
Fig. 2 for the object transmission of equipment that present method is utilized, pipette a kind of modular design of part.Rotating disk 15 shakes rotation through handle wheel 18, when screens can be deposited position 16 or during silicon seed chuck position 17 to the eka-silicon core, through control silicon seed chuck fixed bit 14 go up or down motion get final product; Simultaneously; Driving rotating disk 15 rotation through gear train assembly 19 moves and puts the silicon core and deposit the object on position 16 (drawing the positions that the silicon core 2 after accomplishing is deposited), silicon seed chuck position 17 (move up and down through silicon seed chuck fixed bit 14, extract the object on the silicon seed chuck position 17).
The detailed process that present method prepares the silicon core is following: at first polysilicon is placed on quartz crucible 11 internal heating to dissolving, then the silicon in the quartz crucible 11 is dissolved district 3 and lower the temperature; Driving clamping through control guiding wireline 13 again has the silicon seed chuck 12 of many silicon seeds 1 to move down; Making silicon seed 1 and silicon dissolve district 3 contacts; Dissolving the temperature in district 3 and the pulling speed that silicon seed 1 makes progress through adjustment silicon, is that silicon seed 1 drawing becomes silicon core 2 gradually; When silicon core 2 diameters during near aimed dia, through control pulling guiding steel cable, drive silicon seed 1 and rise, make silicon core 2 break away from silicon and dissolve district 3; Make the silicon core on the rotating disk 15 deposit the silicon core 2 that position 16 aligning drawings obtain through shaking handle wheel 18 then; Making silicon core 2 be positioned over the silicon core deposits on the position 16; After placement finishes; Continue to shake handle wheel 18 and rotate rotating disk 15 to silicon seed chuck position 17, utilize silicon seed chuck fixed bit 14 to extract the silicon seed chuck 12 on the rotating disk 15 then, then dissolve district 3 and carry out welding through silicon seed chuck 12 to the silicon on the gear train assembly 19 decline silicon seed chuck positions 17; Begin the drawing of a new round subsequently, subsequent step repeats the same.
Although preceding text have carried out various detailed descriptions and explanation to the embodiment of this patent method; But should indicatedly be; We can carry out various equivalences to above-mentioned embodiment according to the conception of this patent and change and modification; When the function that it produced does not exceed spiritual that specification sheets and accompanying drawing contain yet, all should be within this patent protection domain.
Claims (10)
1. a high-level efficiency prepares the method for silicon core, it is characterized in that the preparation method is following:
The first step is contained in polysilicon in the quartz crucible (11), and is heated to and dissolves;
In second step, the silicon after dissolving in the quartz crucible (11) is dissolved district (3) lower the temperature;
The 3rd step; The past decline of the cartridge device that has many silicon seeds (1); Many silicon seeds (1) under the cartridge device are contacted with the molten district of silicon (3), dissolve the temperature in district (3) and the pulling speed that silicon seed (1) makes progress through adjustment silicon, silicon seed (1) diameter is become gradually becomes silicon core (2) greatly; When silicon core (2) diameter during near aimed dia, the diameter of control silicon core (2) is done isodiametric growth;
The 4th step; In the later stage of process of growth, quartz crucible (11) stops feed, looks the pulling speed that silicon core (2) diameter is controlled silicon seed (1); Making silicon core (2) and silicon dissolve district (3) breaks away from; Then will draw the silicon core of accomplishing (2) and be placed on accordingly and deposits on the position, and the silicon seed chuck (12) that pipettes on the silicon seed chuck position (17) carries out welding, repeat top step again.
2. a kind of high-level efficiency according to claim 1 prepares the method for silicon core, it is characterized in that: Heating temperature is up to 1410 ℃ in the said the first step.
3. a kind of high-level efficiency according to claim 1 prepares the method for silicon core, it is characterized in that: be to reach and silicon is dissolved district (3) lower the temperature slightly through heating power being reduced 2-5kw in said second step.
4. a kind of high-level efficiency according to claim 1 prepares the method for silicon core, it is characterized in that: be to adjust the temperature that silicon dissolves district (3) through the adjustment heating power in said the 3rd step, the pulling speed that while silicon seed (1) makes progress is 0-15mm/min.
5. the high-level efficiency silicon core for preparing the silicon core prepares stove; It is characterized in that: comprise silicon seed stationary installation, quartz crucible (11) and attemperator; The silicon seed stationary installation is fixed in quartz crucible (11) upper end; Quartz crucible (11) is fixed on the quartz crucible supporting apparatus (10) of graphite system, and quartz crucible (11) lower end is fixedly connected with graphite axis (9), and it is inner that quartz crucible (11), quartz crucible supporting apparatus and graphite axis (9) are positioned at tubular attemperator.
6. silicon core according to claim 5 prepares stove; It is characterized in that: said silicon seed stationary installation comprises guiding wireline (13), seed chuck, and guiding wireline (13) is connected with silicon seed chuck (12) through the web member that is provided with silicon seed chuck fixed bit (14).
7. prepare stove according to claim 5 or 6 described silicon cores; It is characterized in that: said silicon seed chuck fixed bit (14) locates to be provided with rotating disk (15); Rotating disk (15) is positioned at the upper end of silicon seed chuck (12), and rotating disk (15) is provided with the silicon core and deposits position (16) and silicon seed chuck position (17).
8. silicon core according to claim 7 prepares stove, it is characterized in that: said rotating disk (15) drives through gear train assembly (19), and gear train assembly (19) drives transmission through shaking handle wheel (18).
9. silicon core according to claim 8 prepares stove; It is characterized in that: said attemperator comprises from the interior graphite heater that sets gradually outward (6), heat-preservation cylinder (7), carbon adiabator layer (5) and stainless steel cylinder (8); The height of graphite heater (6) is lower than the height of heat-preservation cylinder (7), carbon adiabator layer (5); The height of heat-preservation cylinder (7), carbon adiabator layer (5) is lower than the height of stainless steel cylinder (8), and the upper end of said heat-preservation cylinder (7), carbon adiabator layer (5) is provided with loam cake (4).
10. silicon core according to claim 8 prepares stove, and the process that it is characterized in that preparing the silicon core is following: at first polysilicon is placed on quartz crucible (11) internal heating to dissolving, then the silicon in the quartz crucible (11) is dissolved district (3) and lower the temperature; Driving clamping through control guiding wireline (13) again has the silicon seed chuck (12) of many silicon seeds (1) to move down; Making silicon seed (1) and silicon dissolve district (3) contacts; Dissolving the temperature in district (3) and the pulling speed that silicon seed (1) makes progress through adjustment silicon, is silicon seed (1) drawing becoming silicon core (2) gradually; When silicon core (2) diameter during near aimed dia, through control pulling guiding steel cable, drive silicon seed (1) and rise, make silicon core (2) break away from silicon and dissolve district (3); Make the silicon core on the rotating disk (15) deposit the silicon core (2) that position (16) aligning drawing obtains through shaking handle wheel (18) then; Making silicon core (2) be positioned over the silicon core deposits on the position (16); After placement finishes; Continue to shake handle wheel (18) and rotate rotating disk (15) to silicon seed chuck position (17); Utilize silicon seed chuck fixed bit (14) to extract the silicon seed chuck (12) on the rotating disk (15) then, then dissolve district (3) and carry out welding through silicon seed chuck (12) to the silicon on gear train assembly (19) the decline silicon seed chuck position (17); Begin the drawing of a new round subsequently, subsequent step repeats the same.
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Cited By (5)
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| CN103553052A (en) * | 2013-10-30 | 2014-02-05 | 大连理工大学 | Polysilicon reverse solidification device and method |
| CN105154972A (en) * | 2015-08-25 | 2015-12-16 | 河南协鑫光伏科技有限公司 | Square silicon core production method |
| CN106367808A (en) * | 2015-07-24 | 2017-02-01 | 北京京运通科技股份有限公司 | Production method of silicon cores |
| CN111676510A (en) * | 2020-06-22 | 2020-09-18 | 四川永祥多晶硅有限公司 | Method for manufacturing silicon core by using non-washing-free material |
| CN111717919A (en) * | 2019-03-21 | 2020-09-29 | 新疆大全新能源股份有限公司 | Manufacturing process of silicon core for polycrystalline silicon reduction furnace |
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| CN201713605U (en) * | 2010-07-20 | 2011-01-19 | 西安理工晶体科技有限公司 | Silicon core furnace capable of drawing plurality of groups of silicon cores in one-time heating |
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| JP2009057232A (en) * | 2007-08-31 | 2009-03-19 | Covalent Materials Corp | Silicon single crystal growing method and its apparatus |
| CN101498033A (en) * | 2009-01-20 | 2009-08-05 | 刘朝轩 | Method for crystal crushed aggregate drawing silicon core and simple apparatus |
| CN201713605U (en) * | 2010-07-20 | 2011-01-19 | 西安理工晶体科技有限公司 | Silicon core furnace capable of drawing plurality of groups of silicon cores in one-time heating |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103553052A (en) * | 2013-10-30 | 2014-02-05 | 大连理工大学 | Polysilicon reverse solidification device and method |
| CN103553052B (en) * | 2013-10-30 | 2016-04-13 | 大连理工大学 | A kind of polysilicon reverse solidification device and method |
| CN106367808A (en) * | 2015-07-24 | 2017-02-01 | 北京京运通科技股份有限公司 | Production method of silicon cores |
| CN105154972A (en) * | 2015-08-25 | 2015-12-16 | 河南协鑫光伏科技有限公司 | Square silicon core production method |
| CN111717919A (en) * | 2019-03-21 | 2020-09-29 | 新疆大全新能源股份有限公司 | Manufacturing process of silicon core for polycrystalline silicon reduction furnace |
| CN111676510A (en) * | 2020-06-22 | 2020-09-18 | 四川永祥多晶硅有限公司 | Method for manufacturing silicon core by using non-washing-free material |
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