CN115058131A - Preparation method of coating for reducing red zone at bottom of ingot - Google Patents
Preparation method of coating for reducing red zone at bottom of ingot Download PDFInfo
- Publication number
- CN115058131A CN115058131A CN202210774913.3A CN202210774913A CN115058131A CN 115058131 A CN115058131 A CN 115058131A CN 202210774913 A CN202210774913 A CN 202210774913A CN 115058131 A CN115058131 A CN 115058131A
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- Prior art keywords
- purity
- coating
- zirconium silicate
- crucible
- binder
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Links
- 238000000576 coating method Methods 0.000 title claims abstract description 27
- 239000011248 coating agent Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000010453 quartz Substances 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011230 binding agent Substances 0.000 claims abstract description 15
- 238000005266 casting Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000002378 acidificating effect Effects 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 4
- 230000001680 brushing effect Effects 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000004033 plastic Substances 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims abstract description 4
- 239000007921 spray Substances 0.000 claims abstract description 4
- 238000005507 spraying Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical group CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- JBSLOWBPDRZSMB-FPLPWBNLSA-N dibutyl (z)-but-2-enedioate Chemical compound CCCCOC(=O)\C=C/C(=O)OCCCC JBSLOWBPDRZSMB-FPLPWBNLSA-N 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- -1 acrylic ester Chemical class 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 230000006872 improvement Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C09D7/63—Additives non-macromolecular organic
-
- 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
- C09D7/65—Additives macromolecular
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/002—Crucibles or containers for supporting the melt
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a preparation method of a coating for reducing the red zone at the bottom of an ingot, which comprises the following steps: the method comprises the following steps: the crucible body is manufactured by gel casting, and is cleaned after being qualified after being sintered; step two: cleaning and drying the body, then manufacturing a compact high-purity quartz layer, ball-milling compact high-purity quartz layer slurry which is high-purity quartz particles, adding silica sol and a binder, brushing the silica sol and the binder on the bottom of a crucible, and drying the mixture for later use; step three: preparing high-purity zirconium silicate coating solution, which comprises the following raw materials: zirconium silicate, an acidic dispersant, a binder, deionized water and absolute ethyl alcohol; step four: and (3) isolating the four sides of the crucible manufactured in the second step by using plastic plates, weighing 300g of the solution in the third step, uniformly spraying the solution on the bottom of the crucible by using a high-pressure pneumatic spray gun, and drying to finish the manufacturing of the coating. The invention has the following advantages: the high-purity zirconium silicate high-purity coating is prepared on the bottom high-purity quartz layer, and then the silicon nitride layer is coated on the high-purity zirconium silicate high-purity coating, so that the bottom red area can be effectively reduced.
Description
Technical Field
The invention relates to the technical field of ingot casting coatings, in particular to a preparation method of a coating for reducing a red zone at the bottom of an ingot.
Background
The prior ingot casting technology comprises two processes of ingot casting single crystal and ingot casting polycrystal, wherein the two processes are both manufactured by using a square crucible and using an ingot casting furnace for directional solidification, the cost is reduced due to the single crystal pulling technology, the ingot casting production mode is more and more competitive, in order to reduce the product percent of pass of ingot casting silicon ingots and reduce the bottom red zone as the focus of attention of ingot manufacturers, various patents exist at present based on the purpose of the bottom red zone, the coating scheme of the existing patents mainly comprises a quartz structure layer and a silicon nitride composite layer, the dense barrier effect of the quartz layer is mainly applied to reduce the red zone, impurities can still be transferred between the quartz layers due to the loose characteristic of the silicon nitride layer, the improvement effect to the red removal of bottom is very poor, and the difference is with current coating technique, and this patent can effectual reduction bottom red district through introducing the zirconium silicate coating, and especially the application effect in the ingot casting single crystal is showing.
Disclosure of Invention
The invention aims to solve the technical problem that the improvement effect of the red zone is poor, and provides a preparation method of a coating with a better effect for reducing the red zone at the bottom of an ingot.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a preparation method of a coating for reducing the red zone at the bottom of an ingot comprises the following steps:
the method comprises the following steps: the crucible body is manufactured by gel casting, and is cleaned after being qualified after being sintered;
step two: cleaning and drying the body, then manufacturing a compact high-purity quartz layer, ball-milling compact high-purity quartz layer slurry which is high-purity quartz particles, adding silica sol and a binder, brushing the silica sol and the binder on the bottom of a crucible, and drying the mixture for later use;
step three: preparing high-purity zirconium silicate coating solution, which comprises the following raw materials: zirconium silicate, an acidic dispersant, a binder, deionized water and absolute ethyl alcohol;
step four: and (3) isolating the four sides of the crucible manufactured in the second step by using plastic plates, weighing 300g of the solution in the third step, uniformly spraying the solution on the bottom of the crucible by using a high-pressure pneumatic spray gun, and drying to finish the manufacturing of the coating.
Preferably, the ratio of the zirconium silicate to the acidic dispersant to the binder to the deionized water to the absolute ethyl alcohol is as follows: zirconium silicate: acid dispersant: adhesive: deionized water: anhydrous ethanol ═ 10: 0.5:2:5:5.
Preferably, the purity of the zirconium silicate is more than 99.9 percent, and the particle size is 0.1-1.2 um.
Preferably, the acidic dispersant is lactic acid, dibutyl maleate and acrylate according to the weight ratio of 2: mixing at a ratio of 0.5: 0.1.
Preferably, the binding agent is PVA and PVP which are mixed according to the ratio of 1:2 of the aqueous solution.
The invention has the following advantages: the high-purity zirconium silicate coating is applied to the ingot casting coating for the first time, so that the red zone at the bottom can be effectively reduced, and the application effect of the coating on ingot casting single crystals is particularly obvious; after the scheme is tried, the red area at the bottom is reduced to 25-35mm from 50-60 mm, and the yield of cast ingots is improved by about 4%.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1, the present application relates to a method for preparing a coating for reducing the red zone at the bottom of an ingot, comprising the steps of:
1. the crucible body is manufactured by gel casting, and is cleaned after being qualified after being sintered;
2. cleaning and drying the body, then manufacturing a compact high-purity quartz layer, ball-milling compact high-purity quartz layer slurry which is high-purity quartz particles, adding silica sol and a binder, brushing the silica sol and the binder on the bottom of a crucible, and drying the mixture for later use;
3. preparing high-purity zirconium silicate coating solution, wherein the purity of zirconium silicate is more than 99.9%, the particle size is 0.1-1.2um, and the acidic dispersing agent is lactic acid, dibutyl maleate and acrylic ester according to the ratio of 2: mixing at a ratio of 0.5:0.1, wherein the binder is PVA and PVP, and mixing according to a ratio of 1: 2; the coating solution is zirconium silicate: dispersing agent: adhesive: deionized water: anhydrous ethanol ═ 10: 0.5:2:5:5, stirring for 24 hours in a high-speed stirrer for later use after the preparation is finished;
4. and (3) isolating the four sides of the crucible manufactured in the step (2) by using plastic plates, weighing 300g of the solution, uniformly spraying the solution on the bottom of the crucible by using a high-pressure pneumatic spray gun, and drying to finish the manufacturing of the coating.
According to the invention, the high-purity zirconium silicate coating is prepared on the bottom high-purity quartz layer and then coated with the silicon nitride layer, so that the red zone at the bottom can be effectively reduced, and the application effect in ingot casting of single crystals is particularly obvious; after practical trial, the bottom red area is reduced to 25-35mm from 50-60 mm, and the yield of cast ingots is improved by about 4%.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (5)
1. A preparation method of a coating for reducing the red zone at the bottom of an ingot comprises the following steps:
the method comprises the following steps: the crucible body is manufactured by gel casting, and is cleaned after being qualified after being sintered;
step two: cleaning and drying the body, then manufacturing a compact high-purity quartz layer, ball-milling compact high-purity quartz layer slurry which is high-purity quartz particles, adding silica sol and a binder, brushing the silica sol and the binder on the bottom of a crucible, and drying the mixture for later use;
step three: preparing high-purity zirconium silicate coating solution, which comprises the following raw materials: zirconium silicate, an acidic dispersant, a binder, deionized water and absolute ethyl alcohol;
step four: and (3) isolating the four sides of the crucible manufactured in the second step by using plastic plates, weighing 300g of the solution in the third step, uniformly spraying the solution on the bottom of the crucible by using a high-pressure pneumatic spray gun, and drying to finish the manufacturing of the coating.
2. The method of claim 1, wherein: the ratio of the zirconium silicate to the acidic dispersant to the binder to the deionized water to the absolute ethyl alcohol is as follows: zirconium silicate: acid dispersant: adhesive: deionized water: anhydrous ethanol ═ 10: 0.5:2:5:5.
3. The method of claim 1, wherein: the purity of the zirconium silicate is more than 99.9 percent, and the particle size is 0.1-1.2 um.
4. The method of claim 1, wherein: the acidic dispersing agent is lactic acid, dibutyl maleate and acrylic ester according to the proportion of 2: mixing at a ratio of 0.5: 0.1.
5. The method of claim 1, wherein: the adhesive is prepared by mixing PVA and PVP according to the ratio of 1: 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210774913.3A CN115058131A (en) | 2022-07-01 | 2022-07-01 | Preparation method of coating for reducing red zone at bottom of ingot |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210774913.3A CN115058131A (en) | 2022-07-01 | 2022-07-01 | Preparation method of coating for reducing red zone at bottom of ingot |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115058131A true CN115058131A (en) | 2022-09-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210774913.3A Pending CN115058131A (en) | 2022-07-01 | 2022-07-01 | Preparation method of coating for reducing red zone at bottom of ingot |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115058131A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1721583A (en) * | 2005-05-24 | 2006-01-18 | 西北工业大学 | Process for preparing silicon carbide crystal whisker |
| US20140182511A1 (en) * | 2012-12-28 | 2014-07-03 | Sunedison, Inc. | Protective coating to prevent reaction between graphite susceptor and quartz crucible |
| CN104185696A (en) * | 2012-01-31 | 2014-12-03 | 原子能及能源替代委员会 | Crucible for solidifying silicon ingot |
| CN107739209A (en) * | 2011-08-05 | 2018-02-27 | 科卢斯博知识产权有限公司 | Crucible material |
| CN108588823A (en) * | 2018-04-19 | 2018-09-28 | 常熟华融太阳能新型材料有限公司 | A kind of preparation method of the quartzy coating of efficient barrier impurity diffusion |
| CN110952136A (en) * | 2019-12-23 | 2020-04-03 | 苏州纳迪微电子有限公司 | Polycrystalline silicon ingot casting quartz crucible composite coating and preparation method and application thereof |
| CN111570220A (en) * | 2020-05-29 | 2020-08-25 | 徐州协鑫太阳能材料有限公司 | Preparation method of bottom high-purity spray-free coating for ingot single crystal |
| CN111589678A (en) * | 2020-05-29 | 2020-08-28 | 徐州协鑫太阳能材料有限公司 | Preparation method of compact quartz crucible high-purity coating |
| CN112144115A (en) * | 2020-09-21 | 2020-12-29 | 无锡市尚领石英科技有限公司 | Quartz crucible with long service life and low deformation rate and preparation method thereof |
-
2022
- 2022-07-01 CN CN202210774913.3A patent/CN115058131A/en active Pending
Patent Citations (9)
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Application publication date: 20220916 |
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