CN106000594A - Pollution-free small-particle crushing method for polycrystalline silicon - Google Patents
Pollution-free small-particle crushing method for polycrystalline silicon Download PDFInfo
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- CN106000594A CN106000594A CN201610312596.8A CN201610312596A CN106000594A CN 106000594 A CN106000594 A CN 106000594A CN 201610312596 A CN201610312596 A CN 201610312596A CN 106000594 A CN106000594 A CN 106000594A
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- Prior art keywords
- silicon material
- polycrystalline silicon
- pollution
- polysilicon
- method realizing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
- B02C19/186—Use of cold or heat for disintegrating
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- Toxicology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a pollution-free small-particle crushing method for polycrystalline silicon. The problem of pollution in crushing is solved by taking a pollutant protection measure during the crushing process, and the controllability of the granularity of crushed polycrystalline silicon mixtures is realized by controlling the crushing temperature. The polycrystalline silicon mixtures crushed according to the method are uniform in size and are not polluted. Crushing operation of the polycrystalline silicon mixtures is convenient, so that labor is saved; and the particle sizes of the polycrystalline silicon mixtures crushed according to the method can be controlled to be 5 cm or below, and the fine powder rate of the polycrystalline silicon mixtures can be controlled.
Description
Technical field
The present invention relates to field of polysilicon technology, particularly relate to a kind of method realizing the pollution-free little grain breakage of polysilicon.
Background technology
In industry, breaking polycrystalline silicon many employings wolfram steel hammer crushes or jaw crushing crusher machine, and the former crushing efficiency is low, silicon
The material proportion of goods damageds are high, and can mix a small amount of metal impurities in shattering process, are unfavorable for silicon item matter；Although the latter's crushing efficiency is high,
But same broken loss is big, and broken can mix a large amount of metal impurities, it is necessary to carrying out batch pickling, cost is the highest, and pickling material
Quality is the most unstable.At present, photovoltaic industry has had a specific requirement for the granularity size of raw material polycrystalline silicon material, and domestic city
Also there is demand field to the technique of extensive pollution-free broken polysilicon.Existing patented technology does not focus on the pollution in shattering process
Problem, and the purpose of depollution only can not be reached by later stage washing, can not reach little grain breakage (granularity is little simultaneously
In 5cm) requirement.
Summary of the invention
Want along with proposing for the anti-pollution of silicon material shattering process and granularity size in the development of photovoltaic industry, industry
Ask, the present invention is directed to problem above, the pollution related in silicon material shattering process and granularity problem are proposed technical scheme, it is provided that
A kind of method realizing the pollution-free little grain breakage of polysilicon, the method is by solving some protection from contaminants measure in shattering process
Broken pollution problem, by the control to breaking temperature, it is achieved the controllability of silicon material crushed particles degree.
In order to achieve the above object, the processing method of a kind of polycrystalline silicone tube target that the present invention provides comprises the following steps:
Step 100: the polycrystalline silicon material of clean surface is put into and temperature can be warming up to 800-1000 DEG C in heating device,
And it is incubated 0.5-2h.
Step 200: be transferred in deionized water by temperature polycrystalline silicon material between 600-1000 DEG C, cools down 5-10min.
Step 300: after cooling terminates, takes out polycrystalline silicon material from water, and polycrystalline silicon material surface forms substantial amounts of crackle, crackle
Extend to inside silicon ingot along crystal boundary, find out the face that silicon material crack density is maximum.
Step 400: in clean room, two pieces of silicon material crack densities maximum in the face of touching, polycrystalline silicon material is complete along crackle
Split, it is achieved broken.
Wherein, the heating rate of described step 100 is 10-20 DEG C/min.
Wherein, described step 200 controls within 2min transfer time.
Wherein, described step 200 shifts articles for use aluminium oxide or SiO 2-ceramic class material.
Wherein, in described step 200 cooling procedure, the temperature of deionized water controls below 40 DEG C.
Wherein, the face that two pieces of silicon material crack densities of described step 400 are maximum just crashes.
The invention has the beneficial effects as follows: by the silicon material that the method is broken, its size uniformly and will not produce dirt to silicon material
Dye；It is easy to operate that the method crushes polycrystalline silicon material, saves manpower；The method crushes polycrystalline silicon material, and silicon material granularity can control to arrive
Below 5cm, silicon material fine powder rate can control.(reason is under this thermograde, and produced thermal stress can make silicon material occur
Substantial amounts of crackle, divided by maximum granularity when crack density just determines broken, experiment shows that divided by maximum granularity is about with this understanding
For 5cm).
Detailed description of the invention
Technical scheme and the technique effect reached for making to present invention solves the technical problem that, using are clearer, enumerate
The present invention is described in further detail for embodiment.It is understood that specific embodiment described herein is used only for
The explanation present invention, rather than limitation of the invention.
The polycrystalline silicon material of clean surface is put into and temperature can be warming up to 800-1000 DEG C, and is incubated by heating device
0.5-2h, can not have volatile, fine grained etc. may have the material of pollution to polycrystalline silicon material in heating device, also can not be with metal
Material directly contacts, and prevents metal impurity con.By verification experimental verification, in this temperature range, within 20kg, polycrystalline silicon material breaks
Broken size is at below 5cm.
Temperature polycrystalline silicon material between 600-1000 DEG C is transferred in deionized water, cools down 5-10min.Transfer process
In should be noted high temperature protection, and should control within 2min that (if it exceeds 2min, temperature reduces more, reaches not transfer time
To due thermal stress, crushing effect is poor), transfer articles for use must use high temperature resistant, high rigidity, aluminium oxide free of contamination to silicon material
Or SiO 2-ceramic class material.
In cooling procedure, the temperature of cooling water should control below 40 DEG C that (if not less than 40 degree, water is as cooling
Ji, temperature height is unfavorable for conduction of heat, reduces the temperature difference, thus reduces thermal stress), and bottom of gullet should do one layer of product of protection such as paving
The preferably thin silicon material of matter, prevents broken silicon material from polluting.
After cooling terminates, wear protective gloves from water, take out polycrystalline silicon material, it is found that polycrystalline silicon material surface is formed substantial amounts of
Crackle, crackle extends to inside silicon ingot along crystal boundary, finds out the face that silicon material crack density is maximum.
In clean room, touch faced by two pieces of silicon material crack densities maximums so that polycrystalline silicon material is complete along crackle
Split, it is achieved broken purpose, can according to actual needs bulk silicon material be broken into the fritter silicon material of different grain size scope, with full
Foot Production requirement.
The different warming temperature of table 1, temperature retention time and the broken size of cool time
Last it is noted that various embodiments above is only in order to illustrate technical scheme, it is not intended to limit；To the greatest extent
The present invention has been described in detail by pipe with reference to foregoing embodiments, it will be understood by those within the art that: it is right
Technical scheme described in foregoing embodiments is modified, or the most some or all of technical characteristic is carried out equivalent replaces
Change, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (6)
1. the method realizing the pollution-free little grain breakage of polysilicon, it is characterised in that comprise the following steps:
Step 100: the polycrystalline silicon material of clean surface is put into and temperature can be warming up to 800-1000 DEG C, and protect in heating device
Temperature 0.5-2h；
Step 200: be transferred in deionized water by temperature polycrystalline silicon material between 600-1000 DEG C, cools down 5-10min；
Step 300: after cooling terminates, takes out polycrystalline silicon material from water, and polycrystalline silicon material surface forms substantial amounts of crackle, and crackle is along brilliant
Boundary extends to inside silicon ingot, finds out the face that silicon material crack density is maximum；
Step 400: in clean room, two pieces of silicon material crack densities maximum in the face of touching, polycrystalline silicon material splits completely along crackle,
Realize broken.
A kind of method realizing the pollution-free little grain breakage of polysilicon the most according to claim 1, it is characterised in that described
The heating rate of step 100 is 10-20 DEG C/min.
A kind of method realizing the pollution-free little grain breakage of polysilicon the most according to claim 1, it is characterised in that described
Step 200 controls within 2min transfer time.
A kind of method realizing the pollution-free little grain breakage of polysilicon the most according to claim 1, it is characterised in that described
Step 200 shifts articles for use aluminium oxide or SiO 2-ceramic class material.
A kind of method realizing the pollution-free little grain breakage of polysilicon the most according to claim 1, it is characterised in that described
In step 200 cooling procedure, the temperature of deionized water controls below 40 DEG C.
A kind of method realizing the pollution-free little grain breakage of polysilicon the most according to claim 1, it is characterised in that described
The face of two pieces of silicon material crack densities maximums of step 400 just crashes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610312596.8A CN106000594A (en) | 2016-05-12 | 2016-05-12 | Pollution-free small-particle crushing method for polycrystalline silicon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610312596.8A CN106000594A (en) | 2016-05-12 | 2016-05-12 | Pollution-free small-particle crushing method for polycrystalline silicon |
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| CN106000594A true CN106000594A (en) | 2016-10-12 |
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| CN201610312596.8A Pending CN106000594A (en) | 2016-05-12 | 2016-05-12 | Pollution-free small-particle crushing method for polycrystalline silicon |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4871117A (en) * | 1988-03-31 | 1989-10-03 | Heliotronic Forschungs- Und Entwicklungsgesellschaft Fur Solarzellen- Gmbh | Low-contamination method for comminuting solid silicon fragments |
| CN101985226A (en) * | 2009-07-28 | 2011-03-16 | 三菱综合材料株式会社 | Method of generating cracks in polycrystalline silicon rod and crack generating apparatus |
| CN102489372A (en) * | 2011-12-12 | 2012-06-13 | 湖南顶立科技有限公司 | Method and device for breaking polycrystalline silicon rod |
| CN103172068A (en) * | 2011-12-21 | 2013-06-26 | 瓦克化学股份公司 | Polycrystalline silicon portion and method for breaking a silicon body |
| CN103253674A (en) * | 2012-02-21 | 2013-08-21 | 瓦克化学股份公司 | Chunk polycrystalline silicon and process for cleaning polycrystalline silicon chunks |
| CN105129804A (en) * | 2015-09-01 | 2015-12-09 | 中国化学工程第六建设有限公司 | Production technology for polycrystalline silicon |
-
2016
- 2016-05-12 CN CN201610312596.8A patent/CN106000594A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4871117A (en) * | 1988-03-31 | 1989-10-03 | Heliotronic Forschungs- Und Entwicklungsgesellschaft Fur Solarzellen- Gmbh | Low-contamination method for comminuting solid silicon fragments |
| CN101985226A (en) * | 2009-07-28 | 2011-03-16 | 三菱综合材料株式会社 | Method of generating cracks in polycrystalline silicon rod and crack generating apparatus |
| CN102489372A (en) * | 2011-12-12 | 2012-06-13 | 湖南顶立科技有限公司 | Method and device for breaking polycrystalline silicon rod |
| CN103172068A (en) * | 2011-12-21 | 2013-06-26 | 瓦克化学股份公司 | Polycrystalline silicon portion and method for breaking a silicon body |
| CN103253674A (en) * | 2012-02-21 | 2013-08-21 | 瓦克化学股份公司 | Chunk polycrystalline silicon and process for cleaning polycrystalline silicon chunks |
| CN105129804A (en) * | 2015-09-01 | 2015-12-09 | 中国化学工程第六建设有限公司 | Production technology for polycrystalline silicon |
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Application publication date: 20161012 |
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