CN101660209B - Method and device for reducing polysilicon cast ingot stress - Google Patents

Method and device for reducing polysilicon cast ingot stress Download PDF

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Publication number
CN101660209B
CN101660209B CN2009101121252A CN200910112125A CN101660209B CN 101660209 B CN101660209 B CN 101660209B CN 2009101121252 A CN2009101121252 A CN 2009101121252A CN 200910112125 A CN200910112125 A CN 200910112125A CN 101660209 B CN101660209 B CN 101660209B
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cast ingot
polysilicon
stress
polysilicon cast
ingot
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CN101660209A (en
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郑智雄
张伟娜
赵志跃
程香
汪健
南毅
林禹
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NANAN SANJING SUNSHINE AND POWER Co Ltd
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NANAN SANJING SUNSHINE AND POWER Co Ltd
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Abstract

The invention relates to a method and a device for reducing polysilicon cast ingot stress, wherein the method comprises the following steps of: taking polysilicon cast ingot out of a furnace chamber, then arranging the polysilicon cast ingot in an attemperator with the shape matched with that of the polysilicon cast ingot, and then taking out the polysilicon cast ingot after being placed naturally for 3 to 30 days; removing the edges of the polysilicon cast ingot immediately after taking-out, and cutting the polysilicon cast ingot into standard square ingots for preservation. The device comprises a heat holding cover and a handcart, wherein the heat holding cover has the hexahedral structure. The adoption of the method and the device causes the polysilicon cast ingot to be cooled uniformly so as to hardly generate thermal stress; and the polysilicon cast ingot is taken out after cooling, and edges thereof, wherein impurities are more concentrated, are cut off, thus reducing stress concentration caused by the impurities, and avoiding top crack generated when the impurities exist.

Description

A kind of method and apparatus that reduces polysilicon cast ingot stress
Technical field
The present invention relates to a kind of method and apparatus that reduces polysilicon cast ingot stress.
Background technology
Before 2005, annual 20000 tons of left and right sides semiconductor grade polysilicons, the about 8000-9000 ton of the solar cell consumption polysilicon of consuming in the whole world; Its ratio is 2: 1, still, and since 2005; Variation has taken place in this ratio; The usage quantity of solar cell increases greatly, and the increasing degree of polycrystalline silicon semiconductor is about 5%, and the amplitude of polycrystalline silicon used for solar battery is about 30%.2005, world's polysilicon was 2.88 ten thousand tons, increased by 5% than 2004.According to scholarly forecast, the annual requirement of world's polysilicon in 2009 will reach 6.5 ten thousand tons, and solar cell polysilicon will be above semiconductor grade polysilicon demand.
1975, Wacker company initiated casting legal system polycrystalline silicon material, and thereafter, many research groups have successively proposed multiple casting technique.These casting techniques mainly are divided into dual mode: a kind of mode be in a quartz crucible with unmelted polycrystalline silicon, then be cast in the graphite jig; Another kind of mode is that the fusing back adopts the method for directional freeze to make polysilicon in same crucible.The polysilicon quality that a kind of mode is made wherein is better.The principle of tasting with discrimination silicon with the directional freeze legal system is more, and the thermograde on the strict control vertical direction makes solid-liquid interface straight as far as possible, is orientated column polysilicon preferably thereby grow, and its electric property is even.Different with silicon single crystal, the polysilicon that casts out is rectangular parallelepiped, removes the scrap stock of minute quantity, adopts the line cutting again, and expensive material unaccounted-for (MUF) is just much few, and its cost is very low naturally, so earn widespread respect.
The casting polycrystalline silicon material has replaced the pulling of crystals silicon materials becomes topmost solar cell material, but the competition in market impels the growth technique of casting polycrystalline silicon material to need innovation constantly.Low-cost and high-level efficiency is two basic conditions that solar cell industry is able to long-time Sustainable development, and this impurity concentration that just requires to have in yield rate height and the casting polycrystalline silicon material of casting polycrystalline silicon silicon chip electrical activity is lower.So, casting polycrystalline silicon Development of Materials trend be big volumeization with increase silicon ingot as far as possible effectively utilize volume.
But, at present, when preparing solar-grade polysilicon, metallurgy method is faced with rimose problem in the polycrystalline silicon ingot casting process of cooling all the time, be that Pure Silicon Metal is volumetric expansion about 10% in process of setting because shrink different with most metal volume when solidifying.In addition, be mainly the remaining material end to end of microelectronics industry owing to make the raw material of casting polycrystalline silicon, so its intravital foreign matter content is very high.Secondly, produce a large amount of stress in the castingprocesses, possibly cause a large amount of dislocations to produce.
Summary of the invention
The object of the present invention is to provide a kind of method and apparatus that reduces polysilicon cast ingot stress.
Technical scheme provided by the invention is following:
A kind of method that reduces polysilicon cast ingot stress is characterized in that: after polycrystalline silicon ingot casting is taken out in the stove, be positioned in the attemperator with the polycrystal silicon ingot form fit placement taking-up after 3 days~30 days naturally immediately; Remove flaw-piece after the taking-up immediately, and break into standard side's ingot and preserve.
Described standard side ingot is 156mm * 156mm * 260mm, certainly, according to the section needs, also can be the rectangular parallelepiped of other shape.
Temperature when aforesaid polycrystalline silicon ingot casting is come out of the stove is 200~300 ℃.
Better, be 10~20 days aforesaid natural storage period.
A kind of attemperator that reduces polysilicon cast ingot stress comprises a stay-warm case and a handcart, and it is characterized in that: described stay-warm case is arranged on the handcart, and it is processed by common galvanized steel pipe, and there is a graphite carbon carpet veneer inboard; Described stay-warm case is shaped as the hexahedron structure that matches with the polycrystalline silicon ingot casting shape, and every adjacent face is for removably connecting; Described handcart comprises that one is used to place the flat board of stay-warm case, and one is loaded on the handle portion that is used to promote of dull and stereotyped posterior edges, and the roller that is positioned at dull and stereotyped bottom.
Described stay-warm case is fixedly connected or removably is connected on the flat board of said cart device.
Described graphite carbon felt layer thickness is 10mm~100mm.
The principle of the invention: polycrystalline silicon ingot casting is to adopt the method for directional freeze to be prepared from.Crystal be column crystal by the bottom to grown on top, lattice defect is prone to concentrate on the crystal boundary place.Whole polycrystalline silicon ingot casting is in the directional freeze process, and trace impurity is moved to the top by the bottom, so top impurity is maximum.If polysilicon directly cools off in air after taking out, speed of cooling is inhomogeneous, and it is the fastest to reach the cooling of flaw-piece place, top all around, and built-in thermal stress reaches the top diffusion to all around rapidly, and is inhomogeneous at crystal boundary and impure point diffusion.And the character of polysilicon is: pyrocondensation is cold rises.It is low to reach bottom temp all around, and bulging force appears in crystal, and internal temperature is high, convergent force occurs, so stress is easy to concentrate on crystals, section this moment can cause fragmentation rate to improve.The time of placing along with ingot casting increases; Internal stress is more slowly to diffusion all around, if inhomogeneous crystal cleavage or the section rate of directly causing of diffusion increases, as if evenly diffusion; When diffusing to the top; Run into a large amount of intensive impurity, especially accumulation of impurities is more at the top of ingot casting, can directly cause the top cracking.Because polysilicon is columnar growth in the ingot casting, untimely processing top cracking, crackle can extend to the bottom by the top, brings about great losses.
Fig. 1 explanation: ingot casting has just been taken out when being positioned in the air, and temperature is low all around, and stress is bulging force; Core temperature is high, and stress is convergent force, so fragmentation rate height when stress concentration in the centre, is prone to cause ingot casting cracking or section.
Fig. 2 explanation: the permanent placement, when temperature basically all was cooled to room temperature, stress ran into impure point and irregular crystal boundary (for example twin and twin band) by diffusion around the middle mind-set, still can produce stress concentration, and was difficult for eliminating.
After adopting the inventive method, when polycrystalline silicon ingot casting takes out, put into stay-warm case and be incubated more than 3~30 days, make its even cooling, then polycrystalline silicon ingot casting can produce thermal stresses hardly; Take out polycrystal silicon ingot after in attemperator, being cooled to room temperature; Existing side by side soon, the comparatively concentrated flaw-piece of impurity removes; Then reduced the stress concentration that impurity causes, the top that causes when avoiding impurity to exist cracking, this can place polycrystalline silicon ingot casting after the processing for a long time and does not influence performance.In addition, ingot casting is broken into standard side's ingot, help the unrelieved stress that further elimination possibly exist, so that permanent the placement.In addition, apparatus structure of the present invention is simple, and is easy to use, and ingot casting is transferred to correct position insulation cooling easily, and needn't wait until and come out of the stove after the cooling fully again, saves the PT of every stove.
Description of drawings
Stress synoptic diagram when Fig. 1 is positioned in the air for ingot casting has just taken out, wherein arrow is a stress direction;
Fig. 2 is the stress synoptic diagram after the permanent placement of ingot casting, and wherein arrow is a stress direction;
Fig. 3 is a kind of perspective view that reduces the polysilicon cast ingot stress device of the present invention;
Fig. 4 is a kind of front view that reduces the polysilicon cast ingot stress device of the present invention;
Fig. 5 is a kind of top view that reduces the polysilicon cast ingot stress device of the present invention.
Embodiment
With reference to Fig. 3 to Fig. 5, a kind of attemperator that reduces polysilicon cast ingot stress comprises insulating sections 1 and handcart part 2; Wherein insulating sections 1 comprises header board 11; Header board 11 is processed for common zinc-plated steel pipe 111, and internal surface has a graphite carbon carpet veneer 112, and its thickness is 50mm; Also comprise left plate 12 in addition, back plate 13 and right panel 14, its structure is consistent with header board 11, and plate 11~14 folding in order connects, and also comprises a upper plate and a lower plate (not shown) in addition.Header board 11, left plate 12, back plate 13 and right panel 14, and between upper plate and the lower plate, can surround a hexahedron type seal cavity.
Handcart 2 comprises a flat board 22, and dull and stereotyped 22 bottoms are equipped with four rolling 23, and posterior edges is equipped with handle 21, is used to promote whole device.
During use, earlier in go-cart, set lower plate, after polycrystalline silicon ingot casting is come out of the stove, be placed on the lower plate immediately, and place left plate 12 in order, back plate 13, right panel 14 and header board 11 cover upper plate afterwards.After polycrystalline silicon ingot casting 3 places, promote dolly 2 whole device is removed from the furnace chamber next door, can carry out the single crystal rod production of next stove.And the polycrystalline silicon ingot casting in the attemperator is cooled to the room temperature taking-up, removes the epithelium of band impurity part immediately, and breaks into the standard square and preserve.
Under the equivalent material:
Embodiment 1, do not adopt method of the present invention, the 275kg ingot casting is placed after 8 months the top cracking in air; For avoiding slice loss, abandon section.
Embodiment 2, do not adopt the inventive method, the 275kg ingot casting was placed in air after 30 days, and section goes out qualified 8000, and follow-up battery sheet is produced, and the stress section rapid wear is frangible, loses 520 again, last qualified is 7480 of battery sheets.
Embodiment 3, employing the inventive method, the 275kg ingot casting is put into attemperator immediately when coming out of the stove, be incubated after 3 days to take out, and section immediately goes out qualified 9000 behind the excision flaw-piece, and follow-up battery sheet is produced, and loses 180 again, and at last qualified is 8820 of battery sheets.
Embodiment 4, employing the inventive method, the 275kg ingot casting is put into attemperator immediately when coming out of the stove, be incubated after 14 days to take out, and section immediately goes out qualified 9200 behind the excision flaw-piece, and follow-up battery sheet is produced, and loses 100 again, and at last qualified is 9100 of battery sheets.
Embodiment 5, employing the inventive method, the 275kg ingot casting is put into attemperator immediately when coming out of the stove; Be incubated after 1 month and take out, section immediately goes out qualified 9100 behind the excision flaw-piece; Follow-up battery sheet is produced, and loses about 150 again, and at last qualified is 8950 of battery sheets.
Embodiment 6, employing the inventive method, the 275kg ingot casting is put into attemperator immediately when coming out of the stove; Be incubated after 1 month and take out, the excision flaw-piece breaks into standard side's ingot (156mm * 156mm * 260mm); Place section again after 30 days in the air, go out qualified 9050, follow-up battery sheet is produced; Lose about 180 again, at last qualified is 8870 of battery sheets.
Embodiment 7, employing the inventive method, the 275kg ingot casting is put into attemperator immediately when coming out of the stove; Be incubated after 15 days and take out, the excision flaw-piece breaks into standard side's ingot (156mm * 156mm * 260mm); Place section again after 8 months in the air, go out qualified 8800, follow-up battery sheet is produced; Lose 260 again, at last qualified is 8540 of battery sheets.
Above-mentionedly be merely a specific embodiment of the present invention, but design concept of the present invention is not limited thereto, allly utilizes this design that the present invention is carried out the change of unsubstantiality, all should belong to the behavior of invading protection domain of the present invention.

Claims (3)

1. method that reduces polysilicon cast ingot stress; It is characterized in that: polycrystalline silicon ingot casting in stove after being cooled to 200 ℃~300 ℃; Polycrystalline silicon ingot casting is taken out in stove, be positioned over immediately in the attemperator with the polycrystal silicon ingot form fit, place after 3 days~30 days naturally and take out; Remove flaw-piece after the taking-up immediately, and break into standard side's ingot and preserve.
2. a kind of method that reduces polysilicon cast ingot stress as claimed in claim 1 is characterized in that: be 10 days~20 days described natural storage period.
3. a kind of method that reduces polysilicon cast ingot stress as claimed in claim 1 is characterized in that: described standard side ingot volume is: 156mm * 156mm * 260mm.
CN2009101121252A 2009-06-25 2009-06-25 Method and device for reducing polysilicon cast ingot stress Expired - Fee Related CN101660209B (en)

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CN102094238A (en) * 2010-09-28 2011-06-15 常州天合光能有限公司 Method for reducing internal stress defect of ingot polycrystal
JP6013201B2 (en) * 2012-03-22 2016-10-25 三菱マテリアル電子化成株式会社 Polycrystalline silicon ingot and method for producing polycrystalline silicon ingot
CN103880434A (en) * 2013-11-05 2014-06-25 山东嘉诺电子有限公司 Thermal insulation device for soft magnetic ferrite magnetic core after being sintered
CN103924296A (en) * 2014-04-29 2014-07-16 常州天合光能有限公司 Polycrystal ingot crystal cooling process
CN106087054A (en) * 2016-08-26 2016-11-09 常熟华融太阳能新型材料有限公司 A kind of Novel polycrystalline silicon quartz crucible for ingot casting card article
CN109576798A (en) * 2019-01-11 2019-04-05 中国科学院福建物质结构研究所 A kind of crystal goes out slot protective device

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US4485072A (en) * 1982-02-24 1984-11-27 Apilat Vitaly Y Apparatus and method of growing and discharging single crystals
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