CN107099842A - The preparation method of monocrystalline silicon - Google Patents
The preparation method of monocrystalline silicon Download PDFInfo
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- CN107099842A CN107099842A CN201710327143.7A CN201710327143A CN107099842A CN 107099842 A CN107099842 A CN 107099842A CN 201710327143 A CN201710327143 A CN 201710327143A CN 107099842 A CN107099842 A CN 107099842A
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- layer
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- silica crucible
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- 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
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- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a kind of preparation method of monocrystalline silicon, it comprises the following steps：Barium carbonate layer is covered in the inwall bottom of silica crucible；It is then charged into silicon material and carries out pulling of crystals operation.The preparation method of above-mentioned monocrystalline silicon, due to covering barium carbonate layer in the inwall bottom of silica crucible in advance；Barium carbonate can finally form the small glaze layer of one layer of densification on the inwall of silica crucible.With the rising of silicon liquid level, the place finally contacted in inner wall of quartz crucible with silicon liquid is respectively formed this glaze layer.Due to forming the protective layer of fine and close small glaze layer, crystallization is effectively inhibited, therefore can significantly improve the service life and long brilliant yield of silica crucible.The protective layer of the small glaze layer of this densification is difficult silicon liquid is penetrated into and is peeled off.In addition, protective layer can increase the intensity of silica crucible, so as to reduce hot mastication phenomenon.Further, equilibrium segregation coefficient of the barium in silicon is very small, so do not interfere with the quality of silicon crystal bar.
Description
Technical field
The present invention relates to single silicon field, more particularly to a kind of preparation method of monocrystalline silicon.
Background technology
Vertical pulling method is the main production process of monocrystalline silicon, and silica crucible is the essential auxiliary implement of vertical pulling method.
Silica crucible is at a high temperature of crystal pulling, and with the trend for becoming silica crystals, this process is referred to as crystallization.Crystallization generally occurs
On the top layer of silica crucible.
Serious crystallization can be impacted to crystal pulling.For example, the original thickness of thinned silica crucible is reduced stone by crystallization
The intensity of English crucible, so as to easily cause silica crucible to deform.Particularly, recently as the increase of inventory, the crystal pulling time
Also corresponding extension；With the extension of crystal pulling time, it is also possible to cause the generation of material leakage.In addition, inner wall of quartz crucible is analysed
It is possible to destroy crucible internal walls original coating when brilliant, this will cause bubble layer and molten silicon below coating to react, causes
Partial particulate shape silica enters in molten silicon so that the crystal structure grown morphs and can not normally grow crystalline substance.And
And if quartz crucible surface attaches extremely small impurity, crystallization also leads to monocrystalline and interrupts rib in growth course, influences into
Product rate.
The content of the invention
Based on this, it is necessary to provide a kind of preparation method of effective monocrystalline silicon for suppressing silica crucible crystallization.
A kind of preparation method of monocrystalline silicon, comprises the following steps：
Barium carbonate layer is covered in the inwall bottom of silica crucible；It is then charged into silicon material and carries out pulling of crystals operation.
The preparation method of above-mentioned monocrystalline silicon, due to before dress silicon material pulling of crystals, in the inwall bottom thing of silica crucible
First cover barium carbonate layer；When melting silicon, barium carbonate can be decomposed to form barium monoxide, and barium monoxide can react to form silicon with silica crucible
Sour barium BaSiO3, due to barium silicate BaSiO3Presence, so as to form the small glaze of one layer of densification on the inwall of silica crucible
Layer.With the rising of silicon liquid level, the place finally contacted in inner wall of quartz crucible with silicon liquid is respectively formed this glaze layer.Due to being formed
The protective layer of fine and close small glaze layer, effectively inhibits crystallization, therefore can significantly improve the service life of silica crucible
And long brilliant yield.The protective layer of the small glaze layer of this densification is difficult silicon liquid is penetrated into and is peeled off.In addition, what is formed is fine and close small
Glaze layer protective layer can increase the intensity of silica crucible, so as to reduce hot mastication phenomenon.The carbonate of barium carbonate can become
Carbon dioxide and escape, highly basic, etch quartz earthenware will not be combined into alkali metal ion, the alkaline-earth metal ions remained in silicon material
Crucible.Further, equilibrium segregation coefficient of the barium in silicon is very small, so that concentration of the barium in silicon crystal bar is less than 2.5 × 10-9/
cm3；So do not interfere with the quality of silicon crystal bar.
In addition, using the method for the present invention, the side wall formation coating of silica crucible is not used in, with the rising of silicon liquid level,
The final place contacted in inner wall of quartz crucible with silicon liquid is respectively formed this glaze layer；Operation is simplified, industrialization is more beneficial for real
Apply.
In one of the embodiments, the barium carbonate layer is by the way that barium carbonate powder to be sprinkling upon to the inwall bottom shape of silica crucible
Into.
In one of the embodiments, the quality of the barium carbonate powder is 4.2g~7g.
In one of the embodiments, before silicon material is loaded, it is additionally included in the upper along formation hydrogen-oxygen of the silica crucible
Change barium layer.
In one of the embodiments, the hydroxide barium layer is formed by spraying.
In one of the embodiments, the mass ratio of the spray coating liquor reclaimed water of the spraying and barium hydroxide is 48~54：1.
In one of the embodiments, the thickness of the spraying is 0.2mm~0.6mm.
In one of the embodiments, the width of the spraying is 100mm~150mm.
In one of the embodiments, methods described is additionally included in during crystal pulling, and barium carbonate powder is added in lid is carried.
In one of the embodiments, the quality of the barium carbonate powder added in lid is carried is 3.4g~4g.
Brief description of the drawings
Fig. 1 is the cross section structure schematic diagram of the silica crucible component of an embodiment of the present invention vertically.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with embodiment
The present invention is further elaborated.It should be appreciated that embodiment described herein is only to explain the present invention,
It is not intended to limit the present invention.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The implication that technical staff is generally understood that is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein " and/or " including one or more
The arbitrary and all combination of related Listed Items.
A kind of preparation method of monocrystalline silicon, comprises the following steps：
Barium carbonate layer is covered in the inwall bottom of silica crucible；It is then charged into silicon material and carries out pulling of crystals operation.
Preferably, barium carbonate layer is formed by the way that barium carbonate powder to be sprinkling upon to the inwall bottom of silica crucible.In present embodiment
In, at the connection fillet of silica crucible and the bottom wall of whole silica crucible sprinkles barium carbonate powder.
In the present embodiment, the purity of barium carbonate powder is more than 99.85%.Crystal pulling effect can so be improved.
It is highly preferred that barium carbonate powder can be commercially available, it can also be prepared by oneself.The preparation side of specific barium carbonate powder
Method is as follows：Under nitrogen protection atmosphere, pure carbon dioxide generation barium carbonate is passed through in barium hydroxide solution.
Preferably, the weight of barium carbonate layer is 4.2~7g.So further improve crystal pulling effect.It is highly preferred that barium carbonate
The weight of layer is 4.6~6.5g, so more adapts to 26 cun of silica crucibles being currently mainly used.
In order to further protect silica crucible, it is preferable that before silicon material is loaded, be additionally included in silica crucible on along shape
Into hydroxide barium layer.That is, referring to Fig. 1, hydroxide barium layer 300 is located at the upper at of silica crucible 100.
Hydroxide barium layer can with the carbon dioxide reaction in air and be converted into barium carbonate, when silica crucible be heated when,
Barium carbonate, which is decomposed, produces barium monoxide, and barium monoxide can react to form barium silicate BaSiO with silica crucible3, due to barium silicate BaSiO3
Presence so that in the upper along the small glaze layer of one layer of densification is formed of silica crucible, so as to protect the upper edge of silica crucible.Due to
Hydroxide barium layer is located at the upper edge of silica crucible, so silicon liquid will not touch barium hydroxide, hydroxide barium layer will not be caused to rise
Skin drops influences crystal pulling quality in silicon liquid.The hydroxyl of reaction conversion completely simultaneously, also will not be with the alkali that is remained in silicon material
Metal ion, alkaline-earth metal ions are combined into highly basic, etch quartz crucible.
The step of hydroxide barium layer is with covering barium carbonate layer is formed, can simultaneously carry out, barium hydroxide can also be initially formed
Barium carbonate layer is covered after layer；Hydroxide barium layer is formed after can also be first covering barium carbonate layer.
It is highly preferred that hydroxide barium layer is formed by spraying.In the present embodiment, with water and the mass ratio of barium hydroxide
For 48~54：1 is configured to the spray coating liquor that uses during spraying；That is, the spray coating liquor reclaimed water and the quality of barium hydroxide of spraying
Than for 48~54：1.
In the present embodiment, the thickness of spraying is 0.2mm~0.6mm.
In the present embodiment, the width of spraying is 100mm~150mm.
Before silicon material is loaded, as shown in figure 1, having barium carbonate layer 200 on the inwall bottom of silica crucible 100；In stone
There is hydroxide barium layer 300 on the upper edge of English crucible 100.
Wherein, load silicon material and carry out pulling of crystals operation, be the core procedure for preparing monocrystalline silicon.In the present embodiment,
Specifically include following sub-step：
S1, charging：Silicon material and dopant are put into silica crucible, the species of dopant is depending on N-type or p-type.Mix
Miscellaneous dose has boron, phosphorus, antimony, arsenic etc..
S2, fusing：After charging is finished, after closing long crystal furnace and vacuumizing, high-purity argon gas is filled with, fusing is then heated to
More than temperature, by melting silicon materials.
S3, necking down：After the temperature stabilization of silicon liquid, seed crystal is slowly immersed in silicon liquid.Because seed crystal is contacted with silicon liquid
When thermal stress, seed crystal can be made to produce dislocation, these dislocations must be allowed to disappearance using necking-down Growth and fall.Necking-down Growth is by seed
Crystalline substance is quickly lifted up, and the diameter of the seed crystal grown is narrowed down to a certain size (general 4-6mm).
S4, shouldering：After necking down completion, temperature and pulling rate must be reduced so that needed for the diameter of crystal is increased to gradually
Size.
S5, isodiametric growth：After shouldering completion, the parameter such as regulation pulling rate and temperature makes boule diameter keep substantially not
Become growth, general holding boule diameter is maintained between positive and negative 2mm.
S6, ending：After isodiametric growth, the parameter such as regulation pulling rate and temperature reduces the diameter of crystal bar and makes crystal bar
Depart from silicon liquid.
It is, of course, understood that pulling of crystals operation can use operation known in those skilled in the art, herein
Repeat no more.
In order to further ensure that crystal pulling effect, it is preferable that during crystal pulling, barium carbonate powder is added in lid is carried.
It is highly preferred that the quality of the barium carbonate powder added in lid is carried is 3.4g~4g.
It is highly preferred that after the heating 70~80h when, with carry lid add barium carbonate powder.So it is more conducive to non-Cheng Jinglu
Platform is easy to crystal pulling.
The preparation method of above-mentioned monocrystalline silicon, due to before dress silicon material pulling of crystals, in the inwall bottom thing of silica crucible
First cover barium carbonate layer；When melting silicon, barium carbonate can be decomposed to form barium monoxide, and barium monoxide can react to form silicon with silica crucible
Sour barium BaSiO3, due to barium silicate BaSiO3Presence, so as to form the small glaze of one layer of densification on the inwall of silica crucible
Layer.With the rising of silicon liquid level, the place finally contacted in inner wall of quartz crucible with silicon liquid is respectively formed this glaze layer.Due to being formed
The protective layer of fine and close small glaze layer, effectively inhibits crystallization, therefore can significantly improve the service life of silica crucible
And long brilliant yield；Support is provided for multistage crystal pulling.The protective layer of the small glaze layer of this densification is difficult silicon liquid is penetrated into and is peeled off.
In addition, the fine and close small glaze layer protective layer formed can increase the intensity of silica crucible, so as to reduce hot mastication phenomenon.Carbon
The carbonate of sour barium can become carbon dioxide and escape, will not be with the alkali metal ion, the alkaline-earth metal ions knot that are remained in silicon material
Synthesize highly basic, etch quartz crucible.Further, equilibrium segregation coefficient of the barium in silicon is very small, so that barium is in silicon crystal bar
Concentration be less than 2.5 × 10-9/cm3；So do not interfere with the quality of silicon crystal bar.
In addition, using the method for the present invention, the side wall formation coating of silica crucible is not used in, with the rising of silicon liquid level,
The final place contacted in inner wall of quartz crucible with silicon liquid is respectively formed this glaze layer；Operation is simplified, industrialization is more beneficial for real
Apply.
Using method provided by the present invention, the service life of silica crucible can typically extend to 200h~250h.And if
Direct whole silica crucibles of spraying barium hydroxides, then just occurring that scaling, crystallization, deformation are serious etc. existing using 150h or so
As causing very big interference to crystal pulling.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of monocrystalline silicon, it is characterised in that comprise the following steps：
Barium carbonate layer is covered in the inwall bottom of silica crucible；It is then charged into silicon material and carries out pulling of crystals operation.
2. the preparation method of monocrystalline silicon according to claim 1, it is characterised in that the barium carbonate layer is by by barium carbonate
The inwall bottom that powder is sprinkling upon silica crucible is formed.
3. the preparation method of monocrystalline silicon according to claim 2, it is characterised in that the quality of the barium carbonate powder is 4.2g
~7g.
4. the preparation method of monocrystalline silicon according to claim 1, it is characterised in that before silicon material is loaded, be additionally included in
The upper edge of the silica crucible forms hydroxide barium layer.
5. the preparation method of monocrystalline silicon according to claim 4, it is characterised in that the hydroxide barium layer is by spraying shape
Into.
6. the preparation method of monocrystalline silicon according to claim 5, it is characterised in that the spray coating liquor reclaimed water and hydrogen of the spraying
The mass ratio of barium monoxide is 48~54：1.
7. the preparation method of monocrystalline silicon according to claim 5, it is characterised in that the thickness of the spraying be 0.2mm~
0.6mm。
8. the preparation method of monocrystalline silicon according to claim 5, it is characterised in that the width of the spraying be 100mm~
150mm。
9. the preparation method of monocrystalline silicon according to claim 1, it is characterised in that methods described is additionally included in crystal pulling process
In, barium carbonate powder is added in lid is carried.
10. the preparation method of monocrystalline silicon according to claim 9, it is characterised in that the barium carbonate added in lid is carried
The quality of powder is 3.4g~4g.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111102A (en) * | 2018-11-02 | 2019-01-01 | 宁夏富乐德石英材料有限公司 | A kind of semiconductor grade silica crucible and its manufacturing method |
| CN110552056A (en) * | 2019-10-11 | 2019-12-10 | 内蒙古中环协鑫光伏材料有限公司 | Method for improving Czochralski single crystal formation |
| CN113832537A (en) * | 2021-09-30 | 2021-12-24 | 西安奕斯伟材料科技有限公司 | Quartz crucible and crystal pulling furnace |
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| CN201762478U (en) * | 2010-08-25 | 2011-03-16 | 扬州华尔光电子材料有限公司 | Coating quartz crucible for polycrystalline silicon ingot casting |
| CN201933195U (en) * | 2010-12-28 | 2011-08-17 | 济宁润鹏光伏科技有限公司 | Double-coated quartz crucible |
| CN102199787A (en) * | 2010-03-23 | 2011-09-28 | 扬州华尔光电子材料有限公司 | Coated quartz crucible for production of solar single-crystal silicon materials |
| CN102260902A (en) * | 2011-07-15 | 2011-11-30 | 江苏晶鼎电子材料有限公司 | Method for preparing quartz crucible coating |
| CN202558962U (en) * | 2012-03-31 | 2012-11-28 | 安徽中科太阳能有限公司 | Single crystal silicon production quartz crucible adopting Czochralski method |
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| CN102199787A (en) * | 2010-03-23 | 2011-09-28 | 扬州华尔光电子材料有限公司 | Coated quartz crucible for production of solar single-crystal silicon materials |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111102A (en) * | 2018-11-02 | 2019-01-01 | 宁夏富乐德石英材料有限公司 | A kind of semiconductor grade silica crucible and its manufacturing method |
| CN110552056A (en) * | 2019-10-11 | 2019-12-10 | 内蒙古中环协鑫光伏材料有限公司 | Method for improving Czochralski single crystal formation |
| CN113832537A (en) * | 2021-09-30 | 2021-12-24 | 西安奕斯伟材料科技有限公司 | Quartz crucible and crystal pulling furnace |
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