CN104451871A - Method of improving quality of polysilicon material - Google Patents
Method of improving quality of polysilicon material Download PDFInfo
- Publication number
- CN104451871A CN104451871A CN201410202285.7A CN201410202285A CN104451871A CN 104451871 A CN104451871 A CN 104451871A CN 201410202285 A CN201410202285 A CN 201410202285A CN 104451871 A CN104451871 A CN 104451871A
- Authority
- CN
- China
- Prior art keywords
- acid
- polycrystalline silicon
- silicon material
- silicon
- polysilicon materials
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title abstract description 12
- 229920005591 polysilicon Polymers 0.000 title abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 27
- 239000012535 impurity Substances 0.000 claims abstract description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 230000006698 induction Effects 0.000 claims abstract description 6
- 238000005554 pickling Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000002210 silicon-based material Substances 0.000 claims description 35
- 230000001737 promoting effect Effects 0.000 claims description 6
- 239000011324 bead Substances 0.000 claims description 4
- 239000000779 smoke Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052710 silicon Inorganic materials 0.000 abstract description 12
- 239000010703 silicon Substances 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract 3
- 230000001680 brushing effect Effects 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 125000006850 spacer group Chemical group 0.000 abstract 1
- 238000005266 casting Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000004484 Briquette Substances 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method of improving the quality of a polysilicon material. The method comprises the following steps: putting a plurality of polished polysilicon materials in an acid and alkali resistance soaking vessel, separating every two adjacent polysilicon materials by a spacer bar, then pouring hydrofluoric acid, and slowly pouring nitric acid after all the polysilicon materials are immersed by the acid liquid, so that the internal impurities of the polysilicon materials are reacted in the mixed acid liquid, and discharged through induction; and after reaction is finished, taking out the polysilicon materials, brushing, then soaking the polysilicon materials into the mixed acid liquid which is used in normal acid pickling for 1-2h, then taking out again, and brushing for standby. According to the method disclosed by the invention, polished silicon mixtures are corroded by strong acid so that the internal impurities of the silicon mixtures are discharged from internal gaps under induction when the strong acid is reacted with the silicon mixtures, and then the silicon mixtures are brushed to eliminate the internal impurities, so that the impurities in the silicon mixtures are controlled, the crystallization ratio of ingot and the growth success rate of silicon crystal are increased, and the quality of the silicon crystal is obviously improved.
Description
Technical field
The present invention relates to sun power crystalline silicon manufacturing technology field, particularly a kind of method improving polycrystalline silicon material quality.
Background technology
Silicon single-crystal and policrystalline silicon are the most frequently used materials of crystal silicon solar energy battery, and the polysilicon material source used in solar battery casting ingot needs to carry out removal of impurities process, and the general impurity removal process of silicon material epidermis is: first sandblasting and polishing, after carry out pickling.But ingot casting finished product is not high through the rate of being up to the standards, found by research, silicon material outward appearance after pickling impurity removal seems clean inclusion-free, smooth finish is better, the more inner impurity of silico briquette are not also got rid of external in acid cleaning process in fact, trace it to its cause, that silicon material is of short duration with the reaction times after sour contact, outside surface slight oxidation or some dirty impurity on surface can be removed, be difficult to remove to the more inner darker impurity of silicon material, such as polycrystalline flaw-piece, T1 expects, expect end to end, the glue trace existed in scrap stock, graphite, silicon carbide, the impurity such as metal-powder, all do not dispose, and these are all have influence on resistance in ingot casting process, few son, yield rate, therefore the present invention is devoted to carry out profound impurities removal process to the various material sources of the polysilicon used in large-scale ingot casting, its impurities removal effect is made to play better, thus improve its quality and degree of cleaning.
Summary of the invention
The present invention is directed to the technical problem existed in above-mentioned prior art, provide and a kind ofly can remove the impurity existed in polycrystalline silicon material as much as possible, to improve silicon material after ingot casting as effect during silicon crystal solar cell raw material, improve crystal forming rate and the turnover ratio of its product, strengthen the cleanliness factor of silicon material.
Technical scheme of the present invention is achieved in that
A kind of method promoting polycrystalline silicon material quality, step is as follows: in acid and alkali-resistance soaking container, put into the polycrystalline silicon material that polylith was polished, separate with parting bead between two pieces of adjacent polycrystalline silicon materials, then hydrofluoric acid is poured into, when acid solution submergence all polycrystalline silicon materials, slowly pour nitric acid into again, the inside impurity of polycrystalline silicon material is reacted in mix acid liquor, induction is taken out of external; After question response, taken out by polycrystalline silicon material and scrub, then the mix acid liquor putting into normal pickling soaks 1 ~ 2 hour, rear taking-up is scrubbed for subsequent use again.
As preferably, described acid and alkali-resistance soaking container is PVC soaking barrel, and parting bead is plastic strip.
As preferably, the volume proportion of hydrofluoric acid and nitric acid is 1:1, and each consumption of nitric acid is 300 ~ 400ml.Because make the reaction of generation larger pour the nitric acid of same equal portions into by 1:1 after, more difficult when processing acid mist, add that silicon material is relatively violent with the reaction of acid, silicon material itself there will be the darker phenomenon of crackle, thus each plant demand of nitric acid to control the effect when 300 ~ 400ml better at every turn.
Have employed the invention has the beneficial effects as follows of technique scheme:
Silicon material strong acid after polishing corrodes by the present invention, makes to discharge from internal voids under the induction of impurity when strong acid and silicon material react in its body, then carries out scrubbing removing; Thus achieve the control of impurity in silicon material, what be conducive to the crystal forming rate of ingot casting and silicon crystal grows into power, and crystal quality is significantly improved.
Embodiment
The specific embodiment of the present invention is as follows:
Embodiment: a kind of method promoting polycrystalline silicon material quality, step is as follows: in PVC soaking barrel, put into the polycrystalline silicon material that polylith was polished, separate with plastic strip between two pieces of adjacent polycrystalline silicon materials, then technical grade hydrofluoric acid is poured into, when hydroflouric acid immersion does not have all polycrystalline silicon materials, more slowly pour the nitric acid of 300 ~ 400ml into, the inside impurity of polycrystalline silicon material is reacted in mix acid liquor, induction is taken out of external, has white smoke occur when reacting; After question response, above-mentioned mix acid liquor is released and waits for second stage employ, polycrystalline silicon material is taken out simultaneously and scrub, the carbon block hammer being exposed at appearance for some is cleaned out, mix acid liquor and the spent acid solution of putting into normal pickling again soak 1 ~ 2 hour, and rear taking-up is scrubbed for subsequent use again.
Adopt the various material sources of aforesaid method to polysilicon to carry out profound impurities removal process, make its impurities removal effect play better, thus improve its quality and degree of cleaning.
Claims (4)
1. one kind promotes the method for polycrystalline silicon material quality, it is characterized in that step is as follows: in acid and alkali-resistance soaking container, put into the polycrystalline silicon material that polylith was polished, separate with parting bead between two pieces of adjacent polycrystalline silicon materials, then hydrofluoric acid is poured into, when acid solution submergence all polycrystalline silicon materials, slowly pour nitric acid into again, the inside impurity of polycrystalline silicon material is reacted in mix acid liquor, induction is taken out of external; After question response, taken out by polycrystalline silicon material and scrub, then the mix acid liquor putting into normal pickling soaks 1 ~ 2 hour, rear taking-up is scrubbed for subsequent use again.
2. a kind of method promoting polycrystalline silicon material quality according to claim 1, it is characterized in that: described acid and alkali-resistance soaking container is PVC soaking barrel, parting bead is plastic strip.
3. a kind of method promoting polycrystalline silicon material quality according to claim 1, is characterized in that: the volume proportion of hydrofluoric acid and nitric acid is 1:1, and each consumption of nitric acid is 300 ~ 400ml.
4. a kind of method promoting polycrystalline silicon material quality according to claim 1, is characterized in that: when the complete white smoke referring to that reaction produces of described reaction disappears.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410202285.7A CN104451871A (en) | 2014-05-14 | 2014-05-14 | Method of improving quality of polysilicon material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410202285.7A CN104451871A (en) | 2014-05-14 | 2014-05-14 | Method of improving quality of polysilicon material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104451871A true CN104451871A (en) | 2015-03-25 |
Family
ID=52898597
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410202285.7A Pending CN104451871A (en) | 2014-05-14 | 2014-05-14 | Method of improving quality of polysilicon material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104451871A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365170A (en) * | 2016-08-25 | 2017-02-01 | 泗阳瑞泰光伏材料有限公司 | Method of removing impurities from silicon ingot circulating material |
| CN107572533A (en) * | 2017-09-07 | 2018-01-12 | 晶科能源有限公司 | The minimizing technology of impurity in a kind of silicon material flaw-piece |
| CN109137065A (en) * | 2018-10-24 | 2019-01-04 | 镇江环太硅科技有限公司 | One kind is for the silicon material recovery and treatment method that gives up |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080069756A1 (en) * | 2005-01-27 | 2008-03-20 | Fumitaka Kume | Preferential Etching Method and Silicon Single Crystal Substrate |
| CN101974785A (en) * | 2010-11-03 | 2011-02-16 | 天津市环欧半导体材料技术有限公司 | Cleaning method of policrystalline silicon raw material |
| CN102295289A (en) * | 2011-06-01 | 2011-12-28 | 宁夏银星多晶硅有限责任公司 | Hydrometallurgical purification process of metal impurities in metallurgical polysilicon |
| CN102502652A (en) * | 2011-11-07 | 2012-06-20 | 江西旭阳雷迪高科技股份有限公司 | Cleaning process for polycrystalline material |
-
2014
- 2014-05-14 CN CN201410202285.7A patent/CN104451871A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080069756A1 (en) * | 2005-01-27 | 2008-03-20 | Fumitaka Kume | Preferential Etching Method and Silicon Single Crystal Substrate |
| CN101974785A (en) * | 2010-11-03 | 2011-02-16 | 天津市环欧半导体材料技术有限公司 | Cleaning method of policrystalline silicon raw material |
| CN102295289A (en) * | 2011-06-01 | 2011-12-28 | 宁夏银星多晶硅有限责任公司 | Hydrometallurgical purification process of metal impurities in metallurgical polysilicon |
| CN102502652A (en) * | 2011-11-07 | 2012-06-20 | 江西旭阳雷迪高科技股份有限公司 | Cleaning process for polycrystalline material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365170A (en) * | 2016-08-25 | 2017-02-01 | 泗阳瑞泰光伏材料有限公司 | Method of removing impurities from silicon ingot circulating material |
| CN107572533A (en) * | 2017-09-07 | 2018-01-12 | 晶科能源有限公司 | The minimizing technology of impurity in a kind of silicon material flaw-piece |
| CN109137065A (en) * | 2018-10-24 | 2019-01-04 | 镇江环太硅科技有限公司 | One kind is for the silicon material recovery and treatment method that gives up |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150325 |
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| RJ01 | Rejection of invention patent application after publication |