CN106757335A - A kind of polysilicon crystal technique - Google Patents
A kind of polysilicon crystal technique Download PDFInfo
- Publication number
- CN106757335A CN106757335A CN201611083415.5A CN201611083415A CN106757335A CN 106757335 A CN106757335 A CN 106757335A CN 201611083415 A CN201611083415 A CN 201611083415A CN 106757335 A CN106757335 A CN 106757335A
- Authority
- CN
- China
- Prior art keywords
- silicon
- polysilicon
- state
- liquid
- mass fraction
- 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
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
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 present invention relates to field of polysilicon technology, especially a kind of polysilicon crystal technique；The crystallization processes include：When the silicon material in ingot furnace is in the state of the concurrent of solid-state silicon and liquid-state silicon, maintain the temperature of ingot furnace inner top, after after solid-state silicon fine melt, temperature to room temperature is gradually reduced with the speed of 5 10 DEG C/min, so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, 60 mesh are crushed to, carry out pickling, dried after cleaning, obtain product polysilicon；Due to just carrying out crystallization treatment to liquid-state silicon when silicon material is in solidliquid mixture state in the present invention, hereby it is ensured that the temperature of the liquid-state silicon in every ingot furnace is basically identical, also ensure that the latent heat contained by liquid-state silicon is consistent, so that the crystallization rate of liquid-state silicon is stable, improve the crystalline stability of liquid-state silicon.Meanwhile, the crystallization processes of the polysilicon in the present invention have process is simple, the characteristics of production efficiency is high.
Description
Technical field
The present invention relates to field of polysilicon technology, especially a kind of polysilicon crystal technique.
Background technology
With developing rapidly for photovoltaic industry, polycrystalline silicon ingot or purifying furnace is because its production capacity is high, the product quality stability of production is high
The features such as, it is used widely in photovoltaic generation industry.
When producing polycrystal silicon ingot in the prior art, when silicon material is in the melting stage, it is necessary to when silicon material is completely melt into
After liquid-state silicon, then the processing step for being crystallized.When the bulk temperature of the liquid-state silicon in ingot furnace is higher, there is more diving
Heat, so that the crystallization rate of polycrystal silicon ingot is slow, and in the presence of the phenomenon melted again after receiving a crime report.Simultaneously as every casting
Latent heat in ingot stove contained by liquid-state silicon is inconsistent, and the crystallization rate for thus resulting in liquid-state silicon is unstable, crystalline stability is poor so that
The performance of the solar battery sheet that polycrystal silicon ingot is made has differences.
The content of the invention
The purpose of the present invention is：Overcome deficiency of the prior art, there is provided a kind of crystallization rate stabilization, crystalline stability are good
Polysilicon crystal technique.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of polysilicon crystal technique, the crystallization processes include：When the silicon material in ingot furnace is in solid-state silicon and liquid-state silicon
During the state of concurrent, the temperature of ingot furnace inner top is maintained, after after solid-state silicon fine melt, progressively dropped with the speed of 5-10 DEG C/min
Low temperature is to room temperature so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, is crushed to 60 mesh, carries out pickling, is dried after cleaning
It is dry, obtain product polysilicon.
Preferably, the acid during the pickling operation is 2% hydrofluoric acid from mass fraction and mass fraction is 5%
The mixture of hydrochloric acid, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:1.5-3.
Preferably, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:1.8-
2.8。
Preferably, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:2.4.
Preferably, the pickling operation is to be sprayed at after acid mist on pending polysilicon.
Preferably, the drying temperature during drying operation is 180-240 DEG C.
Preferably, the drying temperature is 190-220 DEG C.
Preferably, the drying temperature is 200 DEG C.
Beneficial effect using technical scheme is：
Due to just carrying out crystallization treatment to liquid-state silicon when silicon material is in solidliquid mixture state in the present invention, hereby it is ensured that every
The temperature of the liquid-state silicon in ingot furnace is basically identical, also ensures that the latent heat contained by liquid-state silicon is consistent, so that liquid-state silicon
Crystallization rate stabilization, the crystalline stability that improve liquid-state silicon.Meanwhile, the crystallization processes of the polysilicon in the present invention have technique
Simply, the characteristics of production efficiency is high.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
A kind of polysilicon crystal technique, including：When the silicon material in ingot furnace is in the state of the concurrent of solid-state silicon and liquid-state silicon
When, the temperature of ingot furnace inner top is maintained, after after solid-state silicon fine melt, temperature to room is gradually reduced with the speed of 5-10 DEG C/min
Temperature so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, is crushed to 60 mesh, carries out pickling, dries after cleaning, obtains product
Polysilicon.
Wherein, the hydrochloric acid that the acid during pickling operation is 2% hydrofluoric acid from mass fraction and mass fraction is 5%
Mixture, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:1.5.
Wherein, pickling operation is to be sprayed at after acid mist on pending polysilicon.
Wherein, drying temperature during drying operation is 180 DEG C.
By purity analysis, Boron contents are 0.1ppm to the polysilicon that the present embodiment is obtained, and phosphorus content is 0.1ppm, and calcium contains
Amount is less than 0.03, and iron content is less than 0.03, reaches the requirement of solar energy level silicon.The conversion ratio of polycrystal silicon cell reaches
17.2%.
Embodiment 2
A kind of polysilicon crystal technique, including：When the silicon material in ingot furnace is in the state of the concurrent of solid-state silicon and liquid-state silicon
When, the temperature of ingot furnace inner top is maintained, after after solid-state silicon fine melt, temperature to room is gradually reduced with the speed of 5-10 DEG C/min
Temperature so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, is crushed to 60 mesh, carries out pickling, dries after cleaning, obtains product
Polysilicon.
Wherein, the hydrochloric acid that the acid during pickling operation is 2% hydrofluoric acid from mass fraction and mass fraction is 5%
Mixture, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:1.8.
Wherein, pickling operation is to be sprayed at after acid mist on pending polysilicon.
Wherein, drying temperature during drying operation is 190 DEG C.
By purity analysis, Boron contents are 0.1ppm to the polysilicon that the present embodiment is obtained, and phosphorus content is 0.1ppm, and calcium contains
Amount is less than 0.03, and iron content is less than 0.03, reaches the requirement of solar energy level silicon.The conversion ratio of polycrystal silicon cell reaches
17.4%.
Embodiment 3
A kind of polysilicon crystal technique, including：When the silicon material in ingot furnace is in the state of the concurrent of solid-state silicon and liquid-state silicon
When, the temperature of ingot furnace inner top is maintained, after after solid-state silicon fine melt, temperature to room is gradually reduced with the speed of 5-10 DEG C/min
Temperature so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, is crushed to 60 mesh, carries out pickling, dries after cleaning, obtains product
Polysilicon.
Wherein, the hydrochloric acid that the acid during pickling operation is 2% hydrofluoric acid from mass fraction and mass fraction is 5%
Mixture, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:2.4.
Wherein, pickling operation is to be sprayed at after acid mist on pending polysilicon.
Wherein, drying temperature during drying operation is 200 DEG C.
By purity analysis, Boron contents are 0.1ppm to the polysilicon that the present embodiment is obtained, and phosphorus content is 0.1ppm, and calcium contains
Amount is less than 0.03, and iron content is less than 0.03, reaches the requirement of solar energy level silicon.The conversion ratio of polycrystal silicon cell reaches
17.6%.
Embodiment 4
A kind of polysilicon crystal technique, including：When the silicon material in ingot furnace is in the state of the concurrent of solid-state silicon and liquid-state silicon
When, the temperature of ingot furnace inner top is maintained, after after solid-state silicon fine melt, temperature to room is gradually reduced with the speed of 5-10 DEG C/min
Temperature so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, is crushed to 60 mesh, carries out pickling, dries after cleaning, obtains product
Polysilicon.
Wherein, the hydrochloric acid that the acid during pickling operation is 2% hydrofluoric acid from mass fraction and mass fraction is 5%
Mixture, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:2.8.
Wherein, pickling operation is to be sprayed at after acid mist on pending polysilicon.
Wherein, drying temperature during drying operation is 220 DEG C.
By purity analysis, Boron contents are 0.1ppm to the polysilicon that the present embodiment is obtained, and phosphorus content is 0.1ppm, and calcium contains
Amount is less than 0.03, and iron content is less than 0.03, reaches the requirement of solar energy level silicon.The conversion ratio of polycrystal silicon cell reaches
17.3%.
Embodiment 5
A kind of polysilicon crystal technique, including：When the silicon material in ingot furnace is in the state of the concurrent of solid-state silicon and liquid-state silicon
When, the temperature of ingot furnace inner top is maintained, after after solid-state silicon fine melt, temperature to room is gradually reduced with the speed of 5-10 DEG C/min
Temperature so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, is crushed to 60 mesh, carries out pickling, dries after cleaning, obtains product
Polysilicon.
Wherein, the hydrochloric acid that the acid during pickling operation is 2% hydrofluoric acid from mass fraction and mass fraction is 5%
Mixture, the volume ratio of the hydrochloric acid that the mass fraction is 2% hydrofluoric acid and mass fraction is 5% is 1:3.
Wherein, pickling operation is to be sprayed at after acid mist on pending polysilicon.
Wherein, drying temperature during drying operation is 240 DEG C.
By purity analysis, Boron contents are 0.1ppm to the polysilicon that the present embodiment is obtained, and phosphorus content is 0.1ppm, and calcium contains
Amount is less than 0.03, and iron content is less than 0.03, reaches the requirement of solar energy level silicon.The conversion ratio of polycrystal silicon cell reaches
17.2%.
Embodiment 3 is preferred embodiment.
With above-mentioned according to desirable embodiment of the invention as enlightenment, by above-mentioned description, relevant staff completely may be used
Without departing from the scope of the technological thought of the present invention', to carry out various changes and amendments.The technical model of this invention
Enclose the content being not limited on specification, it is necessary to its technical scope is determined according to right.
Claims (8)
1. a kind of polysilicon crystal technique, it is characterised in that：The crystallization processes include：When the silicon material in ingot furnace is in solid-state
During the state of the concurrent of silicon and liquid-state silicon, the temperature of ingot furnace inner top is maintained, after after solid-state silicon fine melt, with 5-10 DEG C/min
Speed gradually reduce temperature to room temperature so that the liquid-state silicon crystallizes to form polycrystal silicon ingot again, is crushed to 60 mesh, carries out acid
Wash, dried after cleaning, obtain product polysilicon.
2. a kind of polysilicon crystal technique according to claim 1, it is characterised in that：Acid during the pickling operation
From the hydrofluoric acid that mass fraction is 2% and the mixture of hydrochloric acid that mass fraction is 5%, the mass fraction is 2% hydrofluoric acid
It is 1 with the volume ratio of the hydrochloric acid that mass fraction is 5%:1.5-3.
3. a kind of polysilicon crystal technique according to claim 2, it is characterised in that：The mass fraction is 2% hydrogen fluorine
Acid is 1 with the volume ratio of the hydrochloric acid that mass fraction is 5%:1.8-2.8.
4. a kind of polysilicon crystal technique according to claim 3, it is characterised in that：The mass fraction is 2% hydrogen fluorine
Acid is 1 with the volume ratio of the hydrochloric acid that mass fraction is 5%:2.4.
5. a kind of polysilicon crystal technique according to claim 1, it is characterised in that：The pickling operation is by acid mist
It is sprayed at afterwards on pending polysilicon.
6. a kind of polysilicon crystal technique according to claim 1, it is characterised in that：Drying temperature during the drying operation
Spend is 180-240 DEG C.
7. a kind of polysilicon crystal technique according to claim 6, it is characterised in that：The drying temperature is 190-220
℃。
8. a kind of polysilicon crystal technique according to claim 7, it is characterised in that：The drying temperature is 200 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611083415.5A CN106757335A (en) | 2016-11-30 | 2016-11-30 | A kind of polysilicon crystal technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611083415.5A CN106757335A (en) | 2016-11-30 | 2016-11-30 | A kind of polysilicon crystal technique |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106757335A true CN106757335A (en) | 2017-05-31 |
Family
ID=58913392
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611083415.5A Pending CN106757335A (en) | 2016-11-30 | 2016-11-30 | A kind of polysilicon crystal technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106757335A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671026A (en) * | 2009-09-29 | 2010-03-17 | 包头市山晟新能源有限责任公司 | Pickling impurity removal method and equipment and method and system for purifying polysilicon |
| CN101844768A (en) * | 2010-05-20 | 2010-09-29 | 厦门大学 | Method for removing phosphorus and boron from metallurgical-grade silicon |
| CN101935041A (en) * | 2010-09-13 | 2011-01-05 | 大连隆田科技有限公司 | Method for extracting polysilicon through electron beams and acid washing |
| CN102134075A (en) * | 2011-01-24 | 2011-07-27 | 云南乾元光能产业有限公司 | Novel method for producing solar-grade polysilicon |
| CN102701212A (en) * | 2012-05-17 | 2012-10-03 | 华南师范大学 | Method for removing boron and phosphorus and purifying industrial silicon by using metallurgic method |
| CN102757050A (en) * | 2011-04-27 | 2012-10-31 | 日鑫（永安）硅材料有限公司 | Acid cleaning purification method of metallic silicon |
| CN103693648A (en) * | 2013-12-03 | 2014-04-02 | 中国科学院过程工程研究所 | Method for enhancing wet-process chemical impurity removal of industrial silicon |
-
2016
- 2016-11-30 CN CN201611083415.5A patent/CN106757335A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671026A (en) * | 2009-09-29 | 2010-03-17 | 包头市山晟新能源有限责任公司 | Pickling impurity removal method and equipment and method and system for purifying polysilicon |
| CN101844768A (en) * | 2010-05-20 | 2010-09-29 | 厦门大学 | Method for removing phosphorus and boron from metallurgical-grade silicon |
| CN101935041A (en) * | 2010-09-13 | 2011-01-05 | 大连隆田科技有限公司 | Method for extracting polysilicon through electron beams and acid washing |
| CN102134075A (en) * | 2011-01-24 | 2011-07-27 | 云南乾元光能产业有限公司 | Novel method for producing solar-grade polysilicon |
| CN102757050A (en) * | 2011-04-27 | 2012-10-31 | 日鑫（永安）硅材料有限公司 | Acid cleaning purification method of metallic silicon |
| CN102701212A (en) * | 2012-05-17 | 2012-10-03 | 华南师范大学 | Method for removing boron and phosphorus and purifying industrial silicon by using metallurgic method |
| CN103693648A (en) * | 2013-12-03 | 2014-04-02 | 中国科学院过程工程研究所 | Method for enhancing wet-process chemical impurity removal of industrial silicon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018113478A1 (en) | Method for producing lithium hydroxide monohydrate using lithium carbonate as raw material | |
| JPS60500172A (en) | Method and apparatus for obtaining silicon from fluorosilicic acid | |
| CN105129804A (en) | Production technology for polycrystalline silicon | |
| CN102249250B (en) | Method for purifying silicon dioxide | |
| CN103361724A (en) | Boron-gallium co-doped efficient polycrystalline silicon and preparation method thereof | |
| WO2012000428A1 (en) | Method for preparing high purity silicon | |
| CN103436959A (en) | Polycrystalline silicon ingot preparation method | |
| CN102776556B (en) | Polycrystalline silicon ingot and preparation method thereof as well as polycrystalline silicon wafer | |
| CN101269804B (en) | Method for producing high-purity phosphoric acid crystal | |
| CN107268071A (en) | A kind of solar panel monocrystal silicon preparation technology | |
| CN103058235A (en) | Method of removing calcium with magnesium sulfate and high-purity magnesium sulfate | |
| CN108147386B (en) | Preparation method of dynamic crystalline lithium hexafluorophosphate | |
| CN106757335A (en) | A kind of polysilicon crystal technique | |
| CN107311892A (en) | A kind of preparation method of smart sulfanilamide (SN) | |
| CN111559750A (en) | Efficient continuous electronic-grade lithium fluoride production process | |
| CN104743779B (en) | Suitable for the preparation method of the low deformation rate crucible quartz raw material of monocrystalline production | |
| CN106542511B (en) | A kind of phosphorous acid method for crystallising | |
| CN108793170A (en) | A kind of ventilation slag making of industrial silicon is smelted combine pretreatment after acid cleaning process | |
| CN101362602A (en) | Purification processing method for drawing casting ingot cleaved bark slat and head material | |
| CN105600759A (en) | Method for improving suspension properties of photovoltaic-grade silicon nitride powder by means of grain size distribution | |
| CN105883836A (en) | Co-production method of sodium metasilicate and sodium fluoride | |
| CN209082036U (en) | A kind of polycrystalline cast ingot crucible | |
| CN104131341A (en) | High-efficient process for manufacturing polycrystalline silicon cast ingots | |
| CN103693647A (en) | Method for removing boron and phosphorus in silicon at low temperature | |
| CN109761255A (en) | A method of ice crystal, nitric acid and sodium sulphate are prepared using fluorine-containing nitric acid waste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170531 |
|
| RJ01 | Rejection of invention patent application after publication |