CN1609286A - Solar energy level silicon single crystal producing process - Google Patents
Solar energy level silicon single crystal producing process Download PDFInfo
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- CN1609286A CN1609286A CN 200410064692 CN200410064692A CN1609286A CN 1609286 A CN1609286 A CN 1609286A CN 200410064692 CN200410064692 CN 200410064692 CN 200410064692 A CN200410064692 A CN 200410064692A CN 1609286 A CN1609286 A CN 1609286A
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Abstract
The present invention relates to silicon monocrystal growing technology. The production process of solar energy level silicon monocrystal includes material sorting and processing, adding heat insulting cover to the graphite cover of the Czochrolski method single-crystal furnace, setting guide tube inside the graphite cover, setting protecting disc and cured heat insulating material in the bottom of the furnace, loading material, heating to draw silicon monocrystal, testing, slicing, rounding, and re-testing. The present invention is advanced, and has full utilization of heat energy.
Description
Technical field
The present invention relates to a kind of method for manufacturing that is used for the silicon single-crystal of solar cell, belong to the silicon monocrystal growth technology.
Background technology
Czochralski silicon monocrystal is the most basic material of manufacturing semiconducter device such as large-scale integrated circuit, also is a kind of important materials of solar cell.Since the eighties, it is very active that the research of silicon single-crystal, production and application all seem.The preparation method of silicon single-crystal, generally be monocrystalline or the polycrystalline starting material bought, add in the crucible in the single crystal growing furnace, heating, crystal pulling, by temperature, gaseous tension in the control stove, gas flow, crucible rotation, crystal rotating speed, crystal pulling rate are grown crystal in argon gas or argon-nitrogen mixed gas atmosphere.The silicon single crystal that is drawn into is tested, cut into slices, again through retest-ok product packing warehouse-in.The single crystal growing furnace of existing czochralski silicon monocrystal, hot system is open, mainly the shape and structure by well heater is aided with the thermal field drawing silicon single-crystal that outer stay-warm case insulation forms.The bottom of a whole set of hot system has only a graphite reflecting disc to prop up at furnace bottom.4 supports are arranged on the stove barrel, and graphite cover, heat preservation carbon felt use the graphite support plate rail in the stove tube.One graphite cover is arranged at hot system top, and is spacious in the stove tube.Shielding gas-argon gas is blown down just to scatter from furnace roof and is come, and is full of whole vacuum chamber, flows to venting port from all directions, and thermal losses is big.Because silicon single-crystal price height has influenced the research and development of domestic solar cell, does not particularly have large diameter silicon single-crystal, influences the solar cell photoelectric efficiency of conversion.
Summary of the invention
The purpose of this invention is to provide a kind of large diameter solar energy level silicon single crystal producing process cheaply.
Technical scheme of the present invention is: solar energy level silicon single crystal producing process, the starting material that to produce solar energy level silicon single crystal earlier carry out material sorting and processing, on the hot system top graphite cover of the single crystal growing furnace of czochralski silicon monocrystal, add insulation cover, add guide shell in the lid mouth of graphite cover, furnace bottom protection plate and solidified heat insulation material are established in the bottom of single crystal growing furnace, sorting and the material handled are prepared burden, after the shove charge, vacuumize, applying argon gas, heating, molten silicon, following seed crystal contacts with silicon liquid, and strict control is solid, the temperature of liquid interface draws silicon single-crystal 1418 ℃～1423 ℃ scopes, the silicon single crystal that is drawn into is tested, section, round as a ball, again through retest-ok product packing warehouse-in.The starting material of described solar energy level silicon single crystal are: one, the angle material polycrystalline under the graphitiferous polycrystalline on the top electrode, the cutting, the polycrystal that quality is low in particulate state, broken granulous polycrystalline, the reduction furnace; Two, the unacceptable product of production unicircuit, diode, triode monocrystalline and production solar level monocrystalline and material end to end; Three, produce unicircuit, diode, triode monocrystalline with the pot bottom material preferably of producing the solar level monocrystalline.Described material sorting is: to polycrystal, end to end material, pot bottom material classifies, by the electrical resistivity range stepping, the carbon electrode polycrystalline is wanted first carbon elimination, breaks removal graphite, selects P type, the n type material of resistivity greater than 1 Ω-cm for use.Described processing is that the surface of material end to end in the material of selecting for use is had foreign material, writing, cleans up with acetone, removes the quartz that pot bottom material speckles with; Material, pot bottom material, polycrystal add at hydrofluoric acid respectively and carry out chemical corrosion in the nitric acid liquid end to end, dry after rinsing well with deionized water again.Described batching is the situation according to product design requirement and existing select materials, calculates, arranges in pairs or groups according to classification, model, the electrical resistivity range of material, places stand-by (shove charge) respectively.
Technology of the present invention is advanced simple, add guide shell in the lid mouth of the hot system top graphite cover of single crystal growing furnace, the bottom of single crystal growing furnace is provided with furnace bottom protection plate and solidified heat insulation material, the individual layer insulation cover is become double-deck, tube, lid, cover, dish are formed a sealed whole body, and all adopt the high-quality graphite of import, adopt Japanese state-of-the-art solidified heat insulation material and curing carbon fiber heat insulation material to do lagging material, effectively stop heat energy loss.Guide shell is enclosed in the hot system as the heat of pot cover with well heater, fully guides the directed flow of argon gas, makes the freshest argon gas around silicon liquid and crystal, further plays a protective role.Graphite material and stainless steel furnace wall that solidified heat insulation material is good with heat conduction to greatest extent keep apart, and reduce thermal losses, guarantee making full use of of heat energy.
Major diameter solar energy level silicon single crystal production technique the most important thing is: a rational hot system, suitable operating procedure, stable single crystal furnace equipment.
The advance of hot system: molten silicon power 90-100KW, crystal pulling power 52 58KW
The advance of operating procedure: crystal pulling time 40-45h/ stove, yield rate 60-68%
The contrast of 8 inches of φ and 6 inches throughput of φ:
| Crystal diameter | Moon blow-on number | Charging capacity kg | Yield rate % | Finished product is counted kg |
| 6 inches of φ | ????20 | ????720 | ????65 | ????494 |
| 8 inches of φ | ????16 | ????960 | ????65 | ????624 |
| 8 inches of φ | ????18 | ????1080 | ????65 | ????702 |
Description of drawings
Figure 1 shows that the single crystal growing furnace structural representation that the present invention uses;
Figure 2 shows that process flow sheet of the present invention;
Among the figure: 1 guide shell, 2 insulation covers, 3 graphite covers, 4 lagging materials, 5 stay-warm cases, 6 well heaters, 7 stove tube water jackets, 8 quartzy crucibles, 9 silicon single-crystal, 10 furnace bottom protection plates, 11 material, 12 Recycled materials of buying, 13 are roughly selected, 14 material sortings, 15 chemical corrosions, 16 batchings, 17 shove charges, 18 pulling monocrystals, 19 tests, 20 get that sheet is round as a ball, 21 repetition measurements, 22 qualified, 23 packings, 24 are put in storage.
Embodiment
On the top graphite cover 3 of the single crystal growing furnace of existing czochralski silicon monocrystal, add insulation cover 2, add guide shell 1 in the lid mouth of graphite cover, furnace bottom protection plate 10 is established in the bottom of single crystal growing furnace, the lagging material 4 of single crystal growing furnace and the lagging material 4 below the furnace bottom protection plate all adopt solidified heat insulation material, and stay-warm case 5 adopts the carbon fiber heat insulation material.
To the angle material polycrystalline under the graphitiferous polycrystalline on the top electrode in particulate state, broken granulous polycrystalline, the reduction furnace, the cutting, the polycrystal that quality is low, carry out the sorting classification; The unacceptable product of producing unicircuit, diode, triode monocrystalline and production solar level monocrystalline is reached material end to end, carry out the sorting classification; To pot bottom material preferably at the bottom of the crucible of producing unicircuit, diode, triode monocrystalline, carry out the sorting classification, the carbon electrode polycrystalline is wanted first carbon elimination promptly to break and is ground off graphite.Select P type, the n type material of resistivity for use greater than 1 Ω-cm.There are foreign material, writing in correct tailing surface, cleans up with acetone, removes the quartz that pot bottom material speckles with.Material, pot bottom material and polycrystal add at hydrofluoric acid respectively and carry out chemical corrosion in the nitric acid liquid end to end then, dry after rinsing well with deionized water again and deliver to weighing room.There is the disposable polycrystal of buying of intact packing directly to deliver to weighing room.Classification, model, electrical resistivity range according to material are calculated, are prepared burden.In single crystal growing furnace, load onto quartzy crucible, load onto silicon materials and alloy, install other hot system, load onto seed crystal by the product design requirement, after the shove charge, blow-on, heating, crystal pulling.
The electrically heated part provides maximum output voltage 70V by the 160KVA three-phase rectifier transformer, the 0-140KW adjustable power of direct current.Form close loop control circuit by hyperthermia radiation thermopair and Continental Europe table.The infrared thermometer IRCON that is provided with by main furnace chamber side top (according to and root) ring of light signal during to crystal growth measures, measure the crystalline vary in diameter indirectly, and change the crystalline pull rate according to diameter signal, by CGC-101 crystal growth controller, control by computer, realize the isodiametric automatic growth of crystal diameter.By measurement to crystalline growth velocity, the pulling rate setting curve of brilliant lifting speed and process of growth is compared, the crystalline growth temperature is controlled, relatively the back then lowers the temperature if be slower than setting if pulling rate heats up faster than setting then.The crystal pull rate is changed by the technique initialization curve, be provided with 5 sections, 10 sections, 15 sections, 20 sections curves for selecting for use.Crystal length and scale parameter are calculated and shown by counting long signal and brilliant lifting speed signal, crystal weight is calculated according to diameter parameters.The stove tube water jacket of single crystal growing furnace leads to the refrigeration cycle water cooling.
By temperature, gaseous tension in the control stove, gas flow, quartzy crucible rotating speed, quartzy crucible raising speed, crystal rotating speed, crystal raising speed are grown crystal in argon gas or argon-nitrogen mixed gas atmosphere.The silicon single crystal that is drawn into is carried out model (P type, N type), electrical resistivity range, diameter test.Qualified after tested silicon single crystal cuts off, section, section is tested again, and carrying out that diameter exceeds standard is round as a ball, grinds off the part that exceeds standard.At last oxygen, carbon, life-span are tested and model, resistivity, diameter, length, weight and outward appearance etc. are carried out repetition measurement, calculate amount only, it is single to fill in test.Salable product packing warehouse-in.
Claims (5)
1, a kind of solar energy level silicon single crystal producing process, it is characterized in that the starting material that will produce solar energy level silicon single crystal earlier carry out material sorting and processing, on the hot system top graphite cover of the single crystal growing furnace of czochralski silicon monocrystal, add insulation cover, add guide shell in the lid mouth of graphite cover, furnace bottom protection plate and solidified heat insulation material are established in the bottom of single crystal growing furnace, sorting and the material handled are prepared burden, after the shove charge, after the shove charge, vacuumize applying argon gas, heating, molten silicon, molten silicon, following seed crystal contacts with silicon liquid, and the temperature of strict control solid-liquid interface draws silicon single-crystal for 1418 ℃～1423 ℃, the silicon single crystal that is drawn into is tested, section, round as a ball, again through retest-ok product packing warehouse-in.
2, according to claim 1 solar energy level silicon single crystal producing process, it is characterized in that the starting material of described solar energy level silicon single crystal are: one, the angle material polycrystalline under the graphitiferous polycrystalline on the top electrode, the cutting, the polycrystal that quality is low in particulate state, broken granulous polycrystalline, the reduction furnace; Two, the unacceptable product of production unicircuit, diode, triode monocrystalline and production solar level monocrystalline and material end to end; Three, produce unicircuit, diode, triode monocrystalline with the pot bottom material preferably of producing the solar level monocrystalline.
3, according to claim 1 solar energy level silicon single crystal producing process, it is characterized in that described material sorting is: to polycrystal, end to end material, pot bottom material classifies, by the electrical resistivity range stepping, the carbon electrode polycrystalline is wanted first carbon elimination, break removal graphite, select P type, the n type material of resistivity for use greater than 1 Ω-cm.
4, according to claim 1,3 solar energy level silicon single crystal producing process, it is characterized in that described processing is that the surface of material end to end in the material of selecting for use is had foreign material, writing, clean up with acetone, remove the quartz that pot bottom material speckles with; Material, pot bottom material, polycrystal add at hydrofluoric acid respectively and carry out chemical corrosion in the nitric acid liquid end to end, dry after rinsing well with deionized water again.
5, according to claim 1 solar energy level silicon single crystal producing process, it is characterized in that described batching is the situation according to product design requirement and current material, calculate, arrange in pairs or groups according to classification, model, the electrical resistivity range of material, place stand-by respectively.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008067700A1 (en) * | 2006-12-06 | 2008-06-12 | Tianjin Huanou Semiconductor Material And Technology Co., Ltd. | Dislocation-free silicon monocrystal, its preparation method and a graphite heating device used |
| CN100424234C (en) * | 2005-07-19 | 2008-10-08 | 上海九晶电子材料股份有限公司 | Formulation and preparation of solar energy grade silicon single crystal material |
| CN100562610C (en) * | 2007-04-28 | 2009-11-25 | 江苏华盛天龙光电设备股份有限公司 | guide cylinder lifting mechanism for artificial crystal growth |
| CN101838847A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101838846A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101838841A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101838842A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101851779A (en) * | 2010-06-04 | 2010-10-06 | 浙江芯能光伏科技有限公司 | Method for manufacturing monocrystalline silicon chip of solar cell |
| CN101509148B (en) * | 2008-02-15 | 2011-05-25 | 绿能科技股份有限公司 | Crystal growth furnace with slurry-discharge guide structure |
| CN102212873A (en) * | 2011-05-20 | 2011-10-12 | 浙江星宇能源科技有限公司 | Method for charging mono-crystal furnace |
| CN102220632A (en) * | 2011-06-23 | 2011-10-19 | 英利能源（中国）有限公司 | Technical method of N-type Czochralski silicon monocrystal |
| CN101660197B (en) * | 2009-06-19 | 2012-07-11 | 南安市三晶阳光电力有限公司 | Method for preparing single crystal rod by utilizing low-purity silicon |
| CN102671885A (en) * | 2012-05-18 | 2012-09-19 | 宁夏隆基硅材料有限公司 | Device and method for removing quartz from monocrystalline silicon pot material |
| CN108732307A (en) * | 2018-05-04 | 2018-11-02 | 扬州连城金晖金刚线切片研发有限公司 | A kind of list of diamond wire slice, the polycrystalline silicon rod method of inspection |
| CN109735896A (en) * | 2019-03-22 | 2019-05-10 | 内蒙古中环协鑫光伏材料有限公司 | A method of it improving monocrystalline silicon resistivity and controls precision |
-
2004
- 2004-09-20 CN CN 200410064692 patent/CN1609286A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100424234C (en) * | 2005-07-19 | 2008-10-08 | 上海九晶电子材料股份有限公司 | Formulation and preparation of solar energy grade silicon single crystal material |
| WO2008067700A1 (en) * | 2006-12-06 | 2008-06-12 | Tianjin Huanou Semiconductor Material And Technology Co., Ltd. | Dislocation-free silicon monocrystal, its preparation method and a graphite heating device used |
| CN100562610C (en) * | 2007-04-28 | 2009-11-25 | 江苏华盛天龙光电设备股份有限公司 | guide cylinder lifting mechanism for artificial crystal growth |
| CN101509148B (en) * | 2008-02-15 | 2011-05-25 | 绿能科技股份有限公司 | Crystal growth furnace with slurry-discharge guide structure |
| CN101660197B (en) * | 2009-06-19 | 2012-07-11 | 南安市三晶阳光电力有限公司 | Method for preparing single crystal rod by utilizing low-purity silicon |
| CN101838846A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101838842A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101838841A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101838847A (en) * | 2010-02-23 | 2010-09-22 | 上海汉虹精密机械有限公司 | Single crystal furnace device |
| CN101851779A (en) * | 2010-06-04 | 2010-10-06 | 浙江芯能光伏科技有限公司 | Method for manufacturing monocrystalline silicon chip of solar cell |
| CN102212873A (en) * | 2011-05-20 | 2011-10-12 | 浙江星宇能源科技有限公司 | Method for charging mono-crystal furnace |
| CN102220632A (en) * | 2011-06-23 | 2011-10-19 | 英利能源（中国）有限公司 | Technical method of N-type Czochralski silicon monocrystal |
| CN102220632B (en) * | 2011-06-23 | 2012-12-12 | 英利能源（中国）有限公司 | Technical method of N-type Czochralski silicon monocrystal |
| CN102671885A (en) * | 2012-05-18 | 2012-09-19 | 宁夏隆基硅材料有限公司 | Device and method for removing quartz from monocrystalline silicon pot material |
| CN108732307A (en) * | 2018-05-04 | 2018-11-02 | 扬州连城金晖金刚线切片研发有限公司 | A kind of list of diamond wire slice, the polycrystalline silicon rod method of inspection |
| CN109735896A (en) * | 2019-03-22 | 2019-05-10 | 内蒙古中环协鑫光伏材料有限公司 | A method of it improving monocrystalline silicon resistivity and controls precision |
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