CN111518422A - Crucible bottom coating for full-melting efficient polycrystalline growth and spraying process and application thereof - Google Patents
Crucible bottom coating for full-melting efficient polycrystalline growth and spraying process and application thereof Download PDFInfo
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- CN111518422A CN111518422A CN202010342019.XA CN202010342019A CN111518422A CN 111518422 A CN111518422 A CN 111518422A CN 202010342019 A CN202010342019 A CN 202010342019A CN 111518422 A CN111518422 A CN 111518422A
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- slurry
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
- B05D3/0272—After-treatment with ovens
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- 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
- 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
Abstract
The invention discloses a crucible bottom coating for full-melting efficient polycrystalline growth, a spraying process and application thereof, wherein the coating is coated on the surface of the bottom of a crucible and comprises a slurry A coating and a slurry B coating, wherein: the coating of the slurry A is made of a mixture of silicon nitride powder, ultrapure water and silica sol, wherein the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol is =2.5-3:8-10: 1; the coating of the slurry B is made of a mixture of silicon nitride powder, ultrapure water, silica sol and mixed powder alpha, the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol to the mixed powder alpha is 2.5-3:8-10:1:0.3-0.5, the mixed powder alpha is prepared by mixing 200-mesh and 300-mesh silicon powder and silicon dioxide powder, the coating material is high in purity and less in impurities, the formed coating is high in compactness and good in blocking effect, and the spraying process is simple and easy to implement.
Description
Technical Field
The invention relates to a technology for coating the bottom of a high-efficiency polycrystalline crucible, in particular to a crucible bottom coating for full-melting high-efficiency polycrystalline growth, and belongs to the field of photovoltaic ingot polycrystalline growth.
Background
With the comprehensive popularization of diamond wire slicing and the large-scale application of new battery technologies such as PERC, HIT and the like, the efficiency and the cost of monocrystalline silicon wafers and polycrystalline silicon wafers are gradually increased, so that the improvement of the cost and the quality of the existing polycrystalline ingot casting technology is particularly important.
At present, polycrystal ingot casting technologies mainly comprise a semi-melting technology and a full-melting technology, and compared with the semi-melting technology, the full-melting technology has the advantages of being few in head-tail cutoff, high in effective utilization rate, short in ingot casting time consumption, low in unit water and electricity consumption and the like, but one of the cost advantages (few in tail cutoff) brings the defect that the number of silicon wafer black edges is slightly large, and the control difficulty of key points of the full-melting technology is high. The 3-5mm crystal flower proportion of the crystal ingot is easily reduced due to slight negligence of production control or quality control, the bottom of the crystal ingot is stuck to a crucible, even the whole ingot is scrapped, the problem of batch efficiency of silicon wafers occurs, and most enterprises in the industry adopt a semi-melting process with higher cost.
The crucible used in the existing full-melting process is a high-efficiency crucible which is manufactured by a crucible manufacturer by taking 'sand (quartz sand particles)' as a seeding layer at the bottom of a common crucible in advance as shown in figure 1, and an ingot manufacturer sprays a silicon nitride powder coating on the bottom high-efficiency layer by adopting a full-melting spraying process, wherein the silicon nitride powder coating has the same effect of protecting the crucible from being adhered to the crucible as the coating of the semi-melting spraying process, and silicon liquid and the quartz sand particles are required to be properly corroded. However, the spraying cannot be guaranteed to be completely uniform, the center and the edge of a thermal field of the ingot furnace are different, and the nucleation seeding effect at the bottom of the crucible in the full-melting process is not completely uniform, so that the process window for good nucleation seeding is relatively narrow, which is a main factor with high control difficulty of key points of the full-melting process.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a crucible bottom coating for full-melting efficient polycrystalline growth and a spraying process and application thereof.
In order to solve the technical problems, the invention provides a crucible bottom coating for full-melting efficient polycrystalline growth, which is coated on the bottom surface of a crucible and comprises a slurry A coating and a slurry B coating, wherein:
the coating of the slurry A is prepared by spraying the slurry A, wherein the slurry A is a mixture of silicon nitride powder, ultrapure water and silica sol, and the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol is =2.5-3:8-10: 1;
the coating of the slurry B is prepared by spraying the slurry B, the slurry B is a mixture of silicon nitride powder, ultrapure water, silica sol and mixed powder alpha, the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol to the mixed powder alpha is 2.5-3:8-10:1:0.3-0.5, and the mixed powder alpha is prepared by mixing 200-mesh and 300-mesh silicon powder and silicon dioxide powder.
The technical scheme of the invention is further defined as follows:
further, in the bottom coating of the crucible for full-melting high-efficiency polycrystalline growth, the silicon dioxide powder accounts for 1-10% of the mixed powder alpha by mass ratio.
In the crucible bottom coating for the full-melting efficient polycrystalline growth, the purity of the silicon powder and the silicon dioxide powder is more than 99.99 percent.
The method has the advantages that the adopted material has high purity and few impurities, the formed coating has high compactness, and the method can play a role in blocking the impurity diffusion at the bottom.
The invention also relates to a spraying process of the crucible bottom coating for full-melting efficient polycrystalline growth, which specifically comprises the following steps:
(1) setting spray gun atomization pressure to 4-4.5kgf/cm, and setting mist pressure to 4-4.5 kgf/cm;
(2) the spraying starting point and the spraying finishing point are arranged on the edge line of the crucible, the interval of each gun is 8-11cm, six temperature measuring points are selected on the surface of the crucible, one temperature measuring point is arranged on each of the four side walls of the crucible, the temperature of the two temperature measuring points at the bottom of the crucible reaches 60-90 ℃, and the bottom of the crucible is sprayed by using the slurry A;
(3) adding the slurry B when the slurry A is left at 200-.
In the spraying process of the crucible bottom coating for the full-melting efficient polycrystalline growth, the spraying process is characterized in that: slurry A and slurry B used in the spraying process are calculated according to the mass ratio: slurry B =1-1.4: 1-0.6.
The invention also relates to the application of the bottom coating of the crucible for full-melting efficient polycrystalline growth, the crucible with the coating is filled with materials, ingot casting is carried out, the surface temperature of the ingot after discharging is reduced to below 50 ℃, and the ingot is unloaded.
The invention has the beneficial effects that:
according to the invention, due to the reasons of material and particle size, nucleation and seeding conditions of quartz sand particles are different, and silicon dioxide particles in the coating play a role in auxiliary seeding at the position with poor seeding of the quartz sand particles, so that a process window is enlarged, and the ratio of crystal flowers with the diameter of 3-5mm at the bottom of a crystal ingot is increased; meanwhile, the coating main body material has high purity and less impurities, and the formed coating has high compactness and can play a role in blocking the impurity diffusion at the bottom.
The invention improves the aspects of spraying materials and spraying process, and improves the quality of the silicon wafer as follows:
(1) the area proportion of the crystal boule at the bottom of the crystal ingot with the diameter of 3-5mm is increased by 3-9%, and the silicon wafer batch verification conversion efficiency is improved by 0.02%.
(2) The red area of the ingot is reduced by 1.6mm, the corresponding black edge of the silicon wafer is reduced by 10%, and the larger the size of the silicon wafer is, the more the corresponding black edge is reduced.
Drawings
FIG. 1 is a schematic structural view of a crucible in the prior art without a sprayed coating;
FIG. 2 is a schematic structural view of a crucible after being sprayed with a coating according to an embodiment of the present invention;
in the figure: 1-crucible substrate, 2-quartz sand particles, 3, slurry A coating and 4-slurry B coating.
Detailed Description
Example 1
The crucible bottom coating for the full-melting efficient polycrystalline growth provided by the embodiment has a structure shown in fig. 2, the coating is coated on the surface of the bottom of a crucible, quartz sand particles 2 are arranged on a crucible substrate 1, a slurry A coating 3 and a slurry B coating 4 are arranged on the quartz sand particles 2, and the slurry B coating 4 is arranged on the slurry A coating 3, wherein:
the coating of the slurry A is prepared by spraying the slurry A, wherein the slurry A is a mixture of silicon nitride powder, ultrapure water and silica sol, and the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol is =2.5-3:8-10: 1;
the coating of the slurry B is prepared by spraying the slurry B, the slurry B is a mixture of silicon nitride powder, ultrapure water, silica sol and mixed powder alpha, the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol to the mixed powder alpha is 2.5-3:8-10:1:0.3-0.5, and the mixed powder alpha is prepared by mixing 200-mesh and 300-mesh silicon powder and silicon dioxide powder.
In this example, the mixed powder α contains 1 to 10% by mass of the silica powder as a whole.
In this example, the silicon powder and silica powder purity is greater than 99.99%.
Example 2
The embodiment provides a spraying process and application of a crucible bottom coating for full-melting efficient polycrystalline growth in embodiment 1, and the spraying process specifically comprises the following steps:
(1) preparing slurry A and slurry B, namely taking a measuring cup, sequentially adding 540g of ultrapure water and 60g of silica sol, stirring, adding 150g of silicon nitride powder during stirring, stirring for 20-30 minutes, filtering to obtain slurry A of the coating of the slurry A, taking another measuring cup, sequentially adding 360g of ultrapure water and 40g of silica sol, stirring, adding 100g of silicon nitride powder during stirring, stirring for 20-30 minutes, filtering, and adding 16g of silicon powder with 200 meshes and 0.8g of silicon dioxide powder to obtain slurry B of the coating of the slurry B for later use;
(2) setting the atomizing pressure of the spray gun to be 4.0kgf/cm and the mist pressure to be 4.2 kgf/cm;
(3) setting a spraying starting point and a spraying finishing point on a crucible edge line, wherein the interval between every two guns is 8-11cm, selecting six temperature measuring points on the surface of the crucible, wherein one temperature measuring point is arranged on each of the four side walls of the crucible, the temperature of the two temperature measuring points at the bottom of the crucible reaches 60-90 ℃, and spraying the bottom of the crucible by using the slurry A prepared in the step (1);
(4) adding the slurry B when the slurry A is left at 200-;
(5) and (3) charging in a crucible for forming a coating, casting ingots, operating an ingot casting program according to a full-melting process, discharging the ingots when the surface temperature of the ingots is reduced to 40 ℃, and checking the bottoms of the ingots, wherein the area proportion of the boughs with the diameter of 3-5mm is 100%.
The crucible sprayed with the coating is applied to ingot casting, the area proportion of the crystal flower at the bottom of the ingot with the diameter of 3-5mm is increased by 6%, and the silicon wafer batch verification conversion efficiency is improved by 0.02%; the red area of the ingot is reduced by 1.6mm, the corresponding black edge of the silicon wafer is reduced by 10%, and the larger the size of the silicon wafer is, the more the corresponding black edge is reduced.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (6)
1. The crucible bottom coating for the full-melting high-efficiency polycrystalline growth is characterized in that the coating covers the bottom surface of a crucible and comprises a slurry A coating and a slurry B coating, wherein:
the coating of the slurry A is prepared by spraying the slurry A, the slurry A is a mixture of silicon nitride powder, ultrapure water and silica sol, and the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol is =2.5-3:8-10: 1;
the coating of the slurry B is prepared by spraying the slurry B, the slurry B is a mixture of silicon nitride powder, ultrapure water, silica sol and mixed powder alpha, the mass ratio of the silicon nitride powder to the ultrapure water to the silica sol to the mixed powder alpha is 2.5-3:8-10:1:0.3-0.5, and the mixed powder alpha is prepared by mixing 200-mesh 300-mesh silicon powder and silicon dioxide powder.
2. The crucible bottom coating for all-molten high-efficiency polycrystalline growth according to claim 1, wherein: the mixed powder alpha contains 1-10% of silicon dioxide powder by mass ratio.
3. The crucible bottom coating for all-molten high-efficiency polycrystalline growth according to claim 1, wherein: the purity of the silicon powder and the silicon dioxide powder is more than 99.99 percent.
4. The spray coating process of the crucible bottom coating for the all-molten high-efficiency polycrystalline growth according to claim 1, characterized in that: the method specifically comprises the following steps:
(1) setting spray gun atomization pressure to 4-4.5kgf/cm, and setting mist pressure to 4-4.5 kgf/cm;
(2) the spraying starting point and the spraying finishing point are arranged on the edge line of the crucible, the interval of each gun is 8-11cm, six temperature measuring points are selected on the surface of the crucible, one temperature measuring point is arranged on each of the four side walls of the crucible, the temperature of the two temperature measuring points at the bottom of the crucible reaches 60-90 ℃, and the bottom of the crucible is sprayed by using the slurry A;
(3) adding the slurry B when the slurry A is left at 200-.
5. The spray coating process of the crucible bottom coating for the all-molten high-efficiency polycrystalline growth according to claim 4, characterized in that: slurry A and slurry B used in the spraying process are calculated according to the mass ratio: slurry B =1-1.4: 1-0.6.
6. The use of a bottom coating for a crucible for all-molten high efficiency polycrystalline growth according to claim 1, wherein: charging materials into a crucible for forming a coating, casting ingots, reducing the surface temperature of the ingot to below 50 ℃ after discharging, and discharging the ingot.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010342019.XA CN111518422A (en) | 2020-04-27 | 2020-04-27 | Crucible bottom coating for full-melting efficient polycrystalline growth and spraying process and application thereof |
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| CN202010342019.XA CN111518422A (en) | 2020-04-27 | 2020-04-27 | Crucible bottom coating for full-melting efficient polycrystalline growth and spraying process and application thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924295A (en) * | 2014-03-01 | 2014-07-16 | 浙江晶盛机电股份有限公司 | Polysilicon ingot furnace and method for monitoring polycrystalline ingot seed height at multiple temperature measuring points |
| CN104047048A (en) * | 2014-06-17 | 2014-09-17 | 徐州工业职业技术学院 | Novel ingot casting crucible and manufacturing method thereof |
| CN106637401A (en) * | 2016-11-01 | 2017-05-10 | 河北正雍新材料科技有限公司 | Preparation method for crucible coating used for low-oxygen-content polycrystalline silicon cast ingot |
| CN107417301A (en) * | 2017-08-18 | 2017-12-01 | 晶科能源有限公司 | A kind of silicon nitride coating preparation method of quartz crucible for casting polycrystalline silicon ingot |
| CN107876362A (en) * | 2017-11-10 | 2018-04-06 | 江苏协鑫硅材料科技发展有限公司 | The automatic spraying process and crucible of large scale crucible for casting ingots coating |
| CN108262237A (en) * | 2018-01-23 | 2018-07-10 | 镇江环太硅科技有限公司 | A kind of efficient G7 crucible coating layers preparation method |
-
2020
- 2020-04-27 CN CN202010342019.XA patent/CN111518422A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924295A (en) * | 2014-03-01 | 2014-07-16 | 浙江晶盛机电股份有限公司 | Polysilicon ingot furnace and method for monitoring polycrystalline ingot seed height at multiple temperature measuring points |
| CN104047048A (en) * | 2014-06-17 | 2014-09-17 | 徐州工业职业技术学院 | Novel ingot casting crucible and manufacturing method thereof |
| CN106637401A (en) * | 2016-11-01 | 2017-05-10 | 河北正雍新材料科技有限公司 | Preparation method for crucible coating used for low-oxygen-content polycrystalline silicon cast ingot |
| CN107417301A (en) * | 2017-08-18 | 2017-12-01 | 晶科能源有限公司 | A kind of silicon nitride coating preparation method of quartz crucible for casting polycrystalline silicon ingot |
| CN107876362A (en) * | 2017-11-10 | 2018-04-06 | 江苏协鑫硅材料科技发展有限公司 | The automatic spraying process and crucible of large scale crucible for casting ingots coating |
| CN108262237A (en) * | 2018-01-23 | 2018-07-10 | 镇江环太硅科技有限公司 | A kind of efficient G7 crucible coating layers preparation method |
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Effective date of registration: 20201217 Address after: No. 198 Guangming Road, Zhongzhong Economic Development Zone, Zhenjiang City, Jiangsu Province Applicant after: Jiangsu Meike Solar Energy Technology Co.,Ltd. Address before: 212200 new materials Industrial Park, Youfang Town, Yangzhong City, Zhenjiang City, Jiangsu Province Applicant before: ZHENJIANG HUANTAI SILICON TECHNOLOGY Co.,Ltd. |
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Address after: No. 198 Guangming Road, Zhongzhong Economic Development Zone, Zhenjiang City, Jiangsu Province Applicant after: Jiangsu Meike Solar Energy Technology Co.,Ltd. Address before: No. 198 Guangming Road, Zhongzhong Economic Development Zone, Zhenjiang City, Jiangsu Province Applicant before: Jiangsu Meike Solar Energy Technology Co.,Ltd. |
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