CN106277823A - A kind of grain size distribution improves the method for silicon nitride coating compactness - Google Patents

A kind of grain size distribution improves the method for silicon nitride coating compactness Download PDF

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Publication number
CN106277823A
CN106277823A CN201610736037.XA CN201610736037A CN106277823A CN 106277823 A CN106277823 A CN 106277823A CN 201610736037 A CN201610736037 A CN 201610736037A CN 106277823 A CN106277823 A CN 106277823A
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Prior art keywords
silicon nitride
grain size
size distribution
compactness
improves
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颜记朋
刘久明
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Hebei Corefra Silicon Nitride Material Co Ltd
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Hebei Corefra Silicon Nitride Material Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B28/00Production of homogeneous polycrystalline material with defined structure
    • C30B28/04Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

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  • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Composite Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention belongs to field of new, it is provided that a kind of grain size distribution improves the method for silicon nitride coating compactness, including: (1), by varigrained beta-silicon nitride powder two or three, carries out mixing according to a certain percentage to realize grain size distribution;(2) silicon nitride powder, Ludox and water grain size distribution obtained, mixes by a certain percentage, is stirred until homogeneous, and sprays silica crucible print, prepares silica crucible print, does sweep test, the compactness of observation coating.The silica crucible print observed, the compactness of coating is significantly improved, and space, crackle significantly reduce, and polycrystalline silicon ingot casting coating quality is greatly improved.This method is simple to operate, enforcement is effective, and the coating compactness of preparation is good, can reduce the amount of waste of polycrystal silicon ingot, effectively save cost, it is adaptable to large-scale industrial production.

Description

A kind of grain size distribution improves the method for silicon nitride coating compactness
Technical field
The invention belongs to field of new, more particularly, it relates to a kind of grain size distribution improves silicon nitride coating compactness Method.
Background technology
At present, in the polycrystalline silicon ingot casting production process of photovoltaic industry, silicon material experiences fusing, crystal life in silica crucible Long, annealing cooling, finally casts polycrystal silicon ingot.In melting sources, crystal growing process, silicon melt and silica crucible are long-time Contact, can produce stiction.Owing to silicon is different from the thermal coefficient of expansion of silicon dioxide, if silicon melt and silica crucible wall knot Close closely, be likely to when crystal cools down cause crystalline silicon or silica crucible to rupture;Meanwhile, silicon melt and crucible connect for a long time Touching, silicon can react with silicon dioxide, causes the corrosion of silica crucible, makes the oxygen concentration in polysilicon raise, and then impact The performance of polysilicon chip.In order to avoid silicon melt contacts with the direct of silica crucible, solve viscid problem, reduce polysilicon simultaneously Oxygen in ingot, carbon impurity content, in polycrystalline silicon ingot casting production process commonly used utilize silicon nitride powder as coating, therefore, nitrogen The compactness of SiClx coating directly affects the effect of the ingot casting demoulding.
But along with the development of polycrystalline silicon ingot casting technology in photovoltaic industry, silica crucible filler quantitative change is big, the high temperature melt time Elongated, silicon nitride coating prescription is improved further, silicon nitride coating compactness directly reflects coating quality, and compactness is not Well just cannot meet the polycrystalline silicon ingot casting rigors to coating quality, the quality problems such as viscous powder, viscous pot can be caused aborning. Therefore, how to improve the compactness of silicon nitride coating, thus meet the requirement of polycrystalline silicon ingot casting coating, be this area scientific research personnel Need badly and solve the technical problem that.
Summary of the invention
Present invention is directed at the problem that silicon nitride coating compactness is bad, propose a kind of grain size distribution and improve silicon nitride painting The method of layer compactness, improves the compactness of silicon nitride coating, and then improves the quality of silicon nitride coating.
In order to achieve the above object, the present invention provides following technical scheme:
A kind of grain size distribution improves the method for silicon nitride coating compactness, including:
(1) by varigrained silicon nitride powder two or three, mixing is carried out according to a certain percentage to realize grain size distribution;
(2) silicon nitride powder, Ludox and water grain size distribution obtained, mixes by a certain percentage, is stirred until homogeneous, to quartz earthenware Crucible print sprays, and prepares silica crucible print, does sweep test, the compactness of observation coating.
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, and the purity of described silicon nitride powder is (99~100) %.
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, the different grains of described silicon nitride powder Degree is respectively D50 (0.5~1.5), D50 (1.5~2.5), D50 (2.5~3.6).
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, the α phase content of described silicon nitride powder For (10~100) %.
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, and the ratio of two kinds of powder body proportionings is (1~6): 1.
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, the ratio of described three kinds of powder body proportionings Example is (1~6): (1~6): 1.
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, described powder body be mixed into be dry mixed or Wet mixing.
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, and described water is deionized water or super Pure water.
Preferably, above-mentioned grain size distribution improves in the method for silicon nitride coating compactness, described beta-silicon nitride powder, Ludox The ratio mixed with water is (1~3): 1:(5~10).
Detailed description of the invention
Below in conjunction with embodiment, the detailed description of the invention of the present invention is described further.
Embodiment 1
A kind of grain size distribution improves the method for silicon nitride coating compactness, and its method is as follows:
(1) by D50 1.0,3.0 3 kinds of varigrained silicon nitride powders of D50 2.0, D50, mix according to the ratio of 5:3:2 Close, realize grain size distribution;
(2) silicon nitride powder that grain size distribution obtains is weighed 8g, add 3ml Ludox and 30ml ultra-pure water, by the ratio of 8:3:30 Example mixes, and is stirred until homogeneous, sprays silica crucible print, prepares silica crucible print, do sweep test, observe painting Layer void significantly reduces, there is not crackle, and the compactness of coating has the biggest lifting.
Embodiment 2
A kind of grain size distribution improves the method for silicon nitride coating compactness, and its method is as follows:
(1) by D50 1.0,3.0 3 kinds of varigrained silicon nitride powders of D50 2.0, D50, mix according to the ratio of 2:2:1 Close, realize grain size distribution;
(2) silicon nitride powder that grain size distribution obtains is weighed 8g, add 3ml Ludox and 30ml ultra-pure water, by the ratio of 8:3:30 Example mixes, and is stirred until homogeneous, sprays silica crucible print, prepares silica crucible print, do sweep test, observe painting Layer void significantly reduces, there is not crackle, and the compactness of coating has the biggest lifting.
Embodiment 3
A kind of grain size distribution improves the method for silicon nitride coating compactness, and its method is as follows:
(1) by D50 1.0,3.0 two kinds of varigrained silicon nitride powders of D50, mix according to the ratio of 5:3, realize Grain size distribution;
(2) silicon nitride powder that grain size distribution obtains is weighed 8g, add 3ml Ludox and 30ml ultra-pure water, by the ratio of 8:3:30 Example mixes, and is stirred until homogeneous, sprays silica crucible print, prepares silica crucible print, do sweep test, observe painting Layer void significantly reduces, there is not crackle, and the compactness of coating has the biggest lifting.
Embodiment 4
A kind of grain size distribution improves the method for silicon nitride coating compactness, and its method is as follows:
(1) by D50 1.0,3.0 two kinds of varigrained silicon nitride powders of D50, mix according to the ratio of 7:3, realize grain Degree grating;
(2) silicon nitride powder that grain size distribution obtains is weighed 8g, add 3ml Ludox and 30ml ultra-pure water, by the ratio of 8:3:30 Example mixes, and is stirred until homogeneous, sprays silica crucible print, prepares silica crucible print, do sweep test, observe painting Layer void significantly reduces, there is not crackle, and the compactness of coating has the biggest lifting.
To the disclosed embodiments in described above, it is to make those skilled in the art be capable of or using this Bright.Obviously, above-mentioned described embodiment is only a part of fact Example of the present invention rather than whole embodiments.To ability For the technical staff in territory, these embodiments above-mentioned are made multiple amendment more will be easy to do, as defined herein General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one The widest scope caused.Based on embodiments of the invention, those skilled in the art are institute under not making creative work premise The every other embodiment obtained, broadly falls into the scope of protection of the invention.

Claims (10)

1. the method that a grain size distribution improves silicon nitride coating compactness, it is characterised in that including: (1) is by varigrained In beta-silicon nitride powder two or three, carry out mixing according to a certain percentage to realize grain size distribution;(2) grain size distribution is obtained Silicon nitride powder, Ludox and water, mix by a certain percentage, is stirred until homogeneous, and sprays silica crucible print, preparation quartz Crucible print, does sweep test, the compactness of observation coating.
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described The purity of beta-silicon nitride powder is (99~100) %.
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described The different grain size of silicon nitride powder is respectively D50 (0.5~1.5), D50 (1.5~2.5), D50 (2.5~3.6).
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described The α phase content of beta-silicon nitride powder is (10~100) %.
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described The ratio of two kinds of powder body proportionings is (1~6): 1.
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described The ratio of three kinds of powder body proportionings is (1~6): (1~6): 1.
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described Powder body is mixed into dry or wet mixing.
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described Water is deionized water or ultra-pure water.
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that described The ratio that beta-silicon nitride powder, Ludox mix with water is (1~3): 1:(5~10).
Grain size distribution the most according to claim 1 improves in the method for silicon nitride coating compactness, it is characterised in that institute The grain size distribution stated is not only limited to the improvement of silicon nitride powder compactness, is equally applicable to the improvement of other powder body compactness.
CN201610736037.XA 2016-08-26 2016-08-26 A kind of grain size distribution improves the method for silicon nitride coating compactness Pending CN106277823A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107573101A (en) * 2017-09-13 2018-01-12 扬州荣德新能源科技有限公司 A kind of crucible and preparation method thereof
CN107619303A (en) * 2017-09-11 2018-01-23 江西中昱新材料科技有限公司 A kind of polycrystalline crucible and preparation method thereof
CN108069731A (en) * 2017-12-15 2018-05-25 江苏润弛太阳能材料科技有限公司 A kind of casting polysilicon exempts to spray crucible silicon nitride coating and preparation method thereof
CN108585535A (en) * 2018-03-31 2018-09-28 无锡舜阳新能源科技股份有限公司 High-purity production technology for exempting to spray crucible
CN108911520A (en) * 2018-08-02 2018-11-30 晶科能源有限公司 A kind of production method of silicon nitride coating
CN111349967A (en) * 2018-12-20 2020-06-30 比亚迪股份有限公司 Efficient crucible and preparation method thereof
CN114437619A (en) * 2022-04-04 2022-05-06 河北大唐国际王滩发电有限责任公司 Silicon carbide wear-resistant paint for repairing and protecting overcurrent component
CN115745641A (en) * 2022-11-16 2023-03-07 航天特种材料及工艺技术研究所 Preparation method of inorganic coating on surface of quartz fiber/quartz composite material

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107619303A (en) * 2017-09-11 2018-01-23 江西中昱新材料科技有限公司 A kind of polycrystalline crucible and preparation method thereof
CN107573101A (en) * 2017-09-13 2018-01-12 扬州荣德新能源科技有限公司 A kind of crucible and preparation method thereof
CN107573101B (en) * 2017-09-13 2020-12-01 扬州荣德新能源科技有限公司 Crucible and preparation method thereof
CN108069731A (en) * 2017-12-15 2018-05-25 江苏润弛太阳能材料科技有限公司 A kind of casting polysilicon exempts to spray crucible silicon nitride coating and preparation method thereof
CN108585535A (en) * 2018-03-31 2018-09-28 无锡舜阳新能源科技股份有限公司 High-purity production technology for exempting to spray crucible
CN108585535B (en) * 2018-03-31 2021-03-19 无锡舜阳新能源科技股份有限公司 Production process of high-purity spraying-free crucible
CN108911520A (en) * 2018-08-02 2018-11-30 晶科能源有限公司 A kind of production method of silicon nitride coating
CN111349967A (en) * 2018-12-20 2020-06-30 比亚迪股份有限公司 Efficient crucible and preparation method thereof
CN114437619A (en) * 2022-04-04 2022-05-06 河北大唐国际王滩发电有限责任公司 Silicon carbide wear-resistant paint for repairing and protecting overcurrent component
CN114437619B (en) * 2022-04-04 2022-06-21 河北大唐国际王滩发电有限责任公司 Silicon carbide wear-resistant paint for repairing and protecting overcurrent component
CN115745641A (en) * 2022-11-16 2023-03-07 航天特种材料及工艺技术研究所 Preparation method of inorganic coating on surface of quartz fiber/quartz composite material
CN115745641B (en) * 2022-11-16 2024-02-13 航天特种材料及工艺技术研究所 Preparation method of inorganic coating on surface of quartz fiber/quartz composite material

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