CN114477781A - Preparation process of composite ceramic coating release agent - Google Patents

Preparation process of composite ceramic coating release agent Download PDF

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CN114477781A
CN114477781A CN202011144468.XA CN202011144468A CN114477781A CN 114477781 A CN114477781 A CN 114477781A CN 202011144468 A CN202011144468 A CN 202011144468A CN 114477781 A CN114477781 A CN 114477781A
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powder
coating
beta
release agent
crucible
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贺刚
邓书香
杨增朝
李江涛
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Technical Institute of Physics and Chemistry of CAS
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Technical Institute of Physics and Chemistry of CAS
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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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • 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
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/29—Mixtures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/112—Deposition methods from solutions or suspensions by spraying

Abstract

The invention discloses a composite ceramic coating release agent for silicon ingot release in a preparation process of solar-grade polycrystalline silicon, which is prepared from silicon oxynitride, beta silicon nitride, polyvinyl alcohol and water as raw materials. Si2N2Thermal and mechanical properties of O and Si3N4The material is similar, but the oxidation resistance, the thermal shock resistance and the chemical stability of the material are all superior to those of Si3N4A material. Si melt to Si2N2The O material has the super-hydrophobic characteristic, and the O material do not have chemical reaction, so that the condition that the quality of the Si cast ingot is reduced due to adhesion and impurity diffusion can be effectively reduced, and the aim of improving the first-grade yield of the polycrystalline Si is fulfilled; and beta-Si3N4Free energy is lower than that of alpha phase, preparation difficulty is low, and the same amount of Si is prepared3N4Powder, the cost of the alpha phase being that of the beta phase3 to 5 times, so that beta-Si is used3N4The preparation cost of the base coating can be effectively controlled. In summary, Si2N2O/β‑Si3N4The composite ceramic coating has thermodynamic performance and wetting performance superior to those of the traditional Si3N4And the demolding coating has low cost.

Description

Preparation process of composite ceramic coating release agent
Technical Field
The invention relates to the field of preparation of photovoltaic silicon ingots, in particular to improvement of a release agent.
Background
Solar energy has become the most concerned domestic and foreign research hotspot in the field of new energy as a clean energy. At present, the mainstream solar cell technology in the industry mostly adopts a polycrystalline Si wafer as a photoelectric conversion material, and the quality of the polycrystalline Si wafer has a decisive influence on the performance, the service life and the cost of a cell module. Si materials for solar cells are mainly produced by a directional solidification process. The process flow has extremely strict requirements on containing the crucible, and the crucible is required to simultaneously meet the requirements of high temperature resistance, no pollution or little pollution, good high temperature deformation resistance, small thermal expansion coefficient and good thermal shock stability; high volume density and high breaking and compression strength. In view of the above considerations, quartz crucibles are the best choice, but there are also some problems. First, due to the high activity of molten Si, the quartz crucible reacts chemically with liquid Si (l) + SiO)2(s) ═ SiO (g)) to cause the adhesion of the silicon ingot to the crucible, and the mismatching of the thermal expansion coefficients of the silicon ingot and the quartz crucible in the cooling process causes uneven stress on the silicon ingot, thus causing the cracking of the cast ingot and the generation of dislocation; secondly, elements such as O, B, P, Al and Fe in the quartz crucible can diffuse into the silicon ingot through the joint, and the photoelectric conversion efficiency of the polysilicon material is affected. Therefore, in the demolding process of polycrystalline silicon, in order to smoothly demold the silicon ingot from the crucible, a barrier coating is generally prepared on the inner wall of the crucible. The coating functions as follows: (1) impurities in the crucible are prevented from diffusing into the silicon melt, and the pollution of the silicon ingot is reduced; (2) smooth demoulding of the silicon ingot is ensured, and the risk of crucible adhesion is reduced.
Originally, considering that the coating material is used as a separation layer to reduce adhesion of the silicon melt and the quartz crucible, inorganic salts of some metal elements were used as the coating material. Originally CaCl was used by Ravishirikar et al2As a coating material, the silicon ingot can be successfully separated from the crucible, so that the silicon ingot is prevented from cracking; thereafter, considering that the melting temperature of polysilicon is high (about 1550 ℃), the coating material is required to have the characteristics of high temperature resistance and good high-temperature chemical stability, BN and SiO are adopted2And ceramic powder such as SiC and the like as coating materials. However, the inorganic salt coating materials of the above metals introduce impurities into the Si meltThe material elements such as Ca, Sr, C and the like greatly reduce the photoelectric conversion efficiency of the polycrystalline silicon, and the B element is difficult to remove in the process of purifying the polycrystalline silicon by a metallurgy method. At present, the coating material commonly used in the industry is alpha-Si3N4. This is because Si3N4 is a strongly covalent bond compound, through which impurities do not easily pass, and has good high temperature resistance and chemical stability. However, the existing problems are that after the preparation and smelting of polycrystalline silicon are carried out by gradually enlarging the technical routes of G5, G6 and G7 to obtain the central silicon side as much as possible and the photoelectric conversion efficiency as high as possible, the yield of the central silicon side prepared by the G7 process is only 51%, and the photoelectric conversion efficiency is less than 20%. The cause of this is, α -Si3N4A layer of SiO2 is present on the surface of the release agent particles, and the hot Si melt reacts with SiO2 at high temperature to form Si (l) + SiO2(s) ═ SiO (g) on SiO2The contact antenna of the alpha-Si3N4. Si melt to Si3N4 after depletion is 45 degrees, so when the oxide film is removed, the Si melt can well wet Si3N4, and then the Si melt can permeate in the porous coating, even contact the crucible and react. Therefore, the mold release is difficult after cooling, and the yield of the central silicon is reduced.
In conclusion, it is very important to develop a coating material that does not react with polycrystalline Si and is not wet to improve the quality of Si ingots.
Disclosure of Invention
The invention provides a Si-based alloy2N2O and Si3N4The composite ceramic coating release agent has no reaction and wetting with Si melt, so that the first-grade product rate of Si cast ingots is greatly improved, and the industrial cost is controlled.
The invention adopts the following technical scheme:
a preparation process of a composite ceramic coating release agent comprises the following steps:
(1) single photo layered Si2N2Preparing O ceramic powder: with Si and SiO2As raw material, using NH4Cl powder is used as additive, and combustion synthesis method is adopted in nitrogen atmosphere to prepare single-phase Si2N2O ceramic powder having a particle diameter D50 is between 0.5 and 2 μm;
(2) preparing compound slurry: reacting beta-Si3N4Powder and the above Si2N2Mixing O powder in a weight ratio of 1:1-1:3, putting the mixture into a container to obtain mixed powder, and adding a polyvinyl alcohol solution to ensure that the mass fraction of the mixed powder in the solution is 10-16%; then ball milling and mixing are carried out for 3-5 minutes to obtain compound slurry;
(3) spray coating of a compound coating: spraying the compound slurry on the inner surface of the preheated quartz crucible, and drying to obtain a compound coating;
(4) sintering and heat preservation: placing the crucible with the compound coating into a muffle furnace, and preserving the heat for 2 hours at 800 ℃ to obtain Si on the inner surface of the crucible2N2O/β-Si3N4A composite ceramic coating release agent.
Preferably, the beta-Si is3N4The average particle diameter D50 of the powder is between 0.5 and 2 mu m;
preferably, the mass concentration of the polyvinyl alcohol solution is 5%;
preferably, the nitrogen pressure in the combustion synthesis reaction in the step (1) is 1-5 MPa;
preferably, the preheating temperature of the quartz crucible in the step (3) is 90 ℃; the porosity of the preferred quartz crucible is 15-17%;
preferably, the drying in step (3) is preferably carried out at 120 ℃ for 2 to 4 hours.
Preferably, beta-Si3N4Powder and the above Si2N2O powder is prepared according to the weight ratio of 1: 2; the mass fractions of the mixed powder in the solution are 12%, 14% and 15%.
Preferably, the contact angle of the composite ceramic coating release agent and the polycrystalline silicon melt is more than 90 degrees.
The invention has the beneficial effects that:
Si2N2thermal and mechanical properties of O and Si3N4The material is similar, but the oxidation resistance, the thermal shock resistance and the chemical stability of the material are all superior to those of Si3N4A material. Si melt to Si2N2The O material has super-hydrophobic property, and the O material do not have chemical reaction, so that the condition of quality reduction caused by adhesion and impurity diffusion of Si ingots can be effectively reduced, and the aim of improving the first-grade yield of the polycrystalline Si is fulfilled. And beta-Si3N4The free energy is lower than that of alpha phase, and the preparation difficulty is far lower than that of metastable alpha-Si with higher free energy3N4Powder, preparation of same amount of Si3N4The powder has an alpha phase cost 3 to 5 times that of a beta phase, and beta-Si is used therefor3N4The preparation cost of the base coating can be effectively controlled; and beta-Si3N4The oxide film on the particle surface is thinner than alpha-Si3N4On the surface of the particles, reduction of Si melt and SiO in the coating2The reaction of the oxide layer reduces the permeation and improves the anti-seepage effect of the coating.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings.
Fig. 1, (a) XRD pattern of commonly used α -Si3N4 material; (b) the micro-morphology of the common alpha-Si 3N4 material; (c) si for the present coating2N2An XRD spectrum of the O material; (d) si used2N2The micro-morphology of the O material; (e) beta-Si for the coating3N4An XRD pattern of the material; (d) beta-Si used3N4Microscopic morphology of the material;
FIG. 2 shows a device for testing the contact angle between a composite ceramic coating release agent and polycrystalline silicon;
FIG. 3 is a wetting curve of a polycrystalline silicon melt on a quartz substrate of a composite ceramic coating release agent;
FIG. 4A high temperature process of Si melt coating with Si2N2O/Si3N4And (3) a shape change diagram of the composite ceramic coating release agent on the quartz substrate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the embodiments described are only some representative embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
The invention adopts a combustion synthesis method to prepare single-phase Si2N2O powder of Si and SiO2As raw material, using NH4Cl powder is used as an additive, is synthesized in a nitrogen atmosphere of 1-5MPa, and can be obtained by adopting a conventional preparation process, specifically referring to CN 201910089374.8.
Example 1
Taking single-phase Si with D50 ═ 1.7 mu m2N2O powder, single-phase beta-Si with D50 ═ 1.4 mu m3N4Powder, PVA solution with the mass fraction of 5 percent, counting by weight parts, and mixing 5 parts of beta-Si3N4Powder, 5 parts of Si2N2The powder O was put into a polyethylene container, and 90 parts of PVA solution was added thereto.
Putting silicon nitride balls into a container containing the mixed powder and the polyvinyl alcohol solution, tightly covering, and placing the container in a planetary ball mill for ball milling for 3 minutes to make the mixture uniform to obtain the compound slurry. The slurry was spray-coated on the inner surface of a quartz crucible preheated to 90 ℃ and having a porosity of 15%, a bottom surface of 100mm, square shape, and a depth of 100 mm. And (3) putting the crucible coated with the compound coating into a drying oven, and drying for 2 hours at 120 ℃. Putting the dried crucible into a muffle furnace, preserving the heat for 2 hours at 800 ℃, and obtaining Si on the inner surface of the crucible2N2O/β-Si3N4A composite ceramic coating release agent.
For the convenience of testing, Si-coated films were obtained by the same method as described above2N2O/Si3N4A quartz substrate coated with a composite ceramic coating release agent is prepared by placing polycrystalline Si having a size of 4mm × 4mm × 4mm on a substrate coated with Si2N2O/Si3N4The sample is placed on an alumina porcelain boat as shown in figure 2, and is put into a high-temperature contact angle tester, and the temperature system imitates the temperature system used in the process of preparing the monocrystalline silicon wafer by the current Czochralski method. Heating to 1000 deg.C at a rate of 10 deg.C/min, heating to 1480 deg.C at a rate of 2.5 deg.C/min, maintaining for 1h, cooling to 1000 deg.C at a rate of 2.5 deg.C/min, and naturally cooling to room temperatureAnd (4) warming. In the processes of heating, heat preservation and temperature reduction, a Pt-Rh thermocouple is used for monitoring the temperature of the sample in real time, and an image processing system is used for monitoring the shape change of the sample in situ. It can be seen that the contact angle of the polysilicon to the coating is always greater than 90 deg., and that no movement of the silicon particles/droplets occurs throughout the experiment. The above phenomena illustrate that Si and Si2N2O/Si3N4The composite ceramic coating release agent is non-wetting and non-reactive, so that the phenomenon that the Si melt reacts with the release agent to cause the Si melt to lose efficacy, finally contacts a crucible and reduces the quality of an Si ingot is avoided. FIG. 3 is a graph quantifying the contact angle throughout the sessile drop experiment, and it can be seen that after the Si particles are completely melted, the Si and Si are completely melted2N2O/Si3N4The contact angle of the composite ceramic coating release agent firstly floats up and down at 120 degrees, and finally is stabilized at 120 degrees until solidification. As can be seen from the inset, the Si particles did not make intimate contact with the substrate (upon impact) after the sessile drop experiment, and the coating remained porous after the experiment. In summary, the poly Si and Si2N2O/Si3N4The composite ceramic coating release agent is not wetted, and the coating is not decomposed and failed within one hour of heat preservation time. So Si2N2O/Si3N4The composite ceramic coating release agent coating can be used as a novel release agent in the preparation of solar-grade polycrystalline silicon ingots, and the effect is far better than that of alpha-Si3N4And (4) coating a release agent.
Example 2
Si for demolding silicon ingots2N2O/β-Si3N4The preparation method of the composite coating comprises the following steps:
taking single-phase Si with D50 ═ 1.2 mu m2N2O powder, single-phase beta-Si of 2 μm D50 ═ m3N4Powder, PVA solution with the mass fraction of 5 percent, counting by weight parts, and mixing 5 parts of beta-Si3N4Powder, 10 parts of Si2N2The powder O was put into a polyethylene container, and 85 parts of PVA solution was added thereto.
Putting silicon nitride balls into a container containing mixed powder and polyvinyl alcohol solution, tightly covering, and placingAnd ball-milling the mixture in a planetary ball mill for 5 minutes to ensure that the mixture is uniform to obtain the compound slurry. The slurry was spray-coated on the inner surface of a quartz crucible preheated to 90 ℃ and having a porosity of 15%, a bottom surface of 100mm, square shape, and a depth of 100 mm. And (3) putting the crucible coated with the compound coating into a drying oven, and drying for 3 hours at 120 ℃. Putting the dried crucible into a muffle furnace, and preserving the heat for 2 hours at 800 ℃ to obtain the Si-coated crucible2N2O/β-Si3N4A crucible for compounding a release agent.
The coating has good demoulding effect in the process of preparing the polycrystalline silicon ingot by the Czochralski method, only slight adhesion occurs, and the effect is far better than that of using alpha-Si3N4And (4) coating a release agent.
Example 3
Si for demolding silicon ingots2N2O/β-Si3N4The preparation method of the composite coating comprises the following steps:
taking single-phase Si with D50 ═ 1.4 mu m2N2O powder, D50 ═ 1.6 μm single-phase beta-Si3N4Powder, PVA solution with the mass fraction of 5 percent, 4 parts of beta-Si by weight3N4Powder, 8 parts of Si2N2The powder O was put into a polyethylene container, and 88 parts of PVA solution was added thereto.
Putting silicon nitride balls into a container containing the mixed powder and the polyvinyl alcohol solution, tightly covering, and placing the container in a planetary ball mill for ball milling for 4 minutes to make the mixture uniform to obtain the compound slurry. The slurry was spray-coated on the inner surface of a quartz crucible preheated to 90 ℃ and having a porosity of 15%, a bottom surface of 100mm, square shape, and a depth of 100 mm. And (3) putting the crucible coated with the compound coating into a drying oven, and drying for 5 hours at 120 ℃. Putting the dried crucible into a muffle furnace, and preserving the heat for 2 hours at 800 ℃ to obtain the Si-coated crucible2N2O/β-Si3N4A crucible for compounding a release agent.
The coating has good demoulding effect in the process of preparing the polycrystalline silicon ingot by the Czochralski method, only slight adhesion occurs, and the effect is far better than that of using alpha-Si3N4And (4) coating a release agent.
Example 4
Si for demolding silicon ingots2N2O/β-Si3N4The preparation method of the composite coating comprises the following steps:
taking single-phase Si with D50 ═ 2 mu m2N2O powder, single-phase beta-Si with D50 ═ 1.8 mu m3N4Powder, PVA solution with the mass fraction of 5 percent, 4 parts of beta-Si by weight3N4Powder, 12 parts of Si2N2The powder O was put into a polyethylene container, and 84 parts of PVA solution was added thereto.
Putting silicon nitride balls into a container containing the mixed powder and the polyvinyl alcohol solution, tightly covering, and placing the container in a planetary ball mill for ball milling for 5 minutes to make the mixture uniform to obtain the compound slurry. The slurry was spray-coated on the inner surface of a quartz crucible preheated to 90 ℃ and having a porosity of 15%, a bottom surface of 100mm, square shape, and a depth of 100 mm. And (3) putting the crucible coated with the compound coating into a drying oven, and drying for 4 hours at 120 ℃. Putting the dried crucible into a muffle furnace, and preserving the heat for 2 hours at 800 ℃ to obtain the Si-coated crucible2N2O/β-Si3N4A crucible for compounding a release agent.
The coating has good demoulding effect in the process of preparing the polycrystalline silicon ingot by the Czochralski method, only slight adhesion occurs, and the effect is far better than that of using alpha-Si3N4And (4) coating a release agent.
Example 5
Si for demolding silicon ingots2N2O/β-Si3N4The preparation method of the composite coating comprises the following steps:
taking single-phase Si with D50 ═ 0.5 mu m2N2O powder, single-phase beta-Si with D50 ═ 0.5 mu m3N4Powder, PVA solution with the mass fraction of 5 percent, 7 parts of beta-Si by weight3N4Powder, 7 parts of Si2N2The powder O was put into a polyethylene container, and 86 parts of PVA solution was added thereto.
Putting silicon nitride balls into a container containing the mixed powder and the polyvinyl alcohol solution, tightly covering, and placing the container in a planetary ball mill for ball milling for 5 minutes to make the mixture uniform to obtain the compound slurry. Spray coating the slurryPreheating to 90 deg.C, wherein the inner surface of the quartz crucible has porosity of 15%, bottom surface of 100mm, square shape and depth of 100 mm. And (3) putting the crucible coated with the compound coating into a drying oven, and drying for 2 hours at 120 ℃. Putting the dried crucible into a muffle furnace, and preserving the heat for 2 hours at 800 ℃ to obtain the Si-coated crucible2N2O/β-Si3N4A crucible for compounding a release agent.
The coating has good demoulding effect in the process of preparing the polycrystalline silicon ingot by the Czochralski method, only slight adhesion occurs, and the effect is far better than that of using alpha-Si3N4And (4) coating a release agent.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. A preparation process of a composite ceramic coating release agent is characterized by comprising the following steps:
(1) single photo layered Si2N2Preparing O ceramic powder: with Si and SiO2As raw material, using NH4Cl powder is used as additive, and combustion synthesis method is adopted in nitrogen atmosphere to prepare single-phase Si2N2O ceramic powder, Si2N2The grain diameter D50 of the O ceramic powder is between 0.5 and 2 mu m;
(2) preparing compound slurry: reacting beta-Si3N4Powder and the above Si2N2Mixing O powder in a weight ratio of 1:1-1:3, putting the mixture into a container to obtain mixed powder, and adding a polyvinyl alcohol solution, wherein the mass fraction of the mixed powder in the solution is 10% -16%; then ball milling and mixing are carried out for 3-5 minutes to obtain compound slurry;
(3) spray coating of a compound coating: spraying the compound slurry on the inner surface of the preheated quartz crucible, and drying to obtain a compound coating;
(4) sintering and heat preservation: placing the crucible with the compound coating into a muffle furnace, and preserving the heat for 2 hours at 800 ℃ to obtain Si on the inner surface of the crucible2N2O/β-Si3N4A composite ceramic coating release agent.
2. The process of claim 1, wherein the beta-Si is present in a form selected from the group consisting of3N4The average particle diameter D50 of the powder is between 0.5 and 2 μm.
3. The process according to claim 1 or 2, wherein the polyvinyl alcohol solution has a mass concentration of 5%.
4. A production process according to claims 1 to 3, wherein the nitrogen pressure in the combustion synthesis reaction in step (1) is between 1 and 5MPa, preferably 1 MPa.
5. The production process according to claims 1 to 3, wherein the preheating temperature of the quartz crucible in the step (3) is 90 ℃; more preferably, the quartz crucible has a porosity of 15 to 17%.
6. A process according to claims 1 to 3, wherein drying in step (3) is preferably carried out at 120 ℃ for 2 to 4 hours.
7. The process of claims 1-3, wherein β -Si3N4Powder and the above Si2N2O powder is prepared according to the weight ratio of 1: 2; the mass fractions of the mixed powder in the solution are 12%, 14% and 15%.
8. The process of claims 1-7, wherein the composite ceramic coating release agent has a contact angle with the molten polysilicon of greater than 90 °.
CN202011144468.XA 2020-10-23 2020-10-23 Preparation process of composite ceramic coating release agent Pending CN114477781A (en)

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CN107916451A (en) * 2017-12-15 2018-04-17 江苏润弛太阳能材料科技有限公司 One kind casting polysilicon exempts to spray crucible
CN109750351A (en) * 2018-05-31 2019-05-14 河北高富氮化硅材料有限公司 A kind of efficient Si of polycrystalline silicon ingot casting3N4Powder
CN109056059A (en) * 2018-08-11 2018-12-21 周浪 A kind of crystalline silicon ingot casting crucible inside coating material
CN109704782A (en) * 2019-01-30 2019-05-03 中国科学院理化技术研究所 A kind of Si for photovoltaic production of polysilicon2N2The preparation method of O ceramic powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116851630A (en) * 2023-08-15 2023-10-10 上海勘测设计研究院有限公司 Slurry for casting and demolding as well as preparation method and application thereof
CN116851630B (en) * 2023-08-15 2024-04-05 上海勘测设计研究院有限公司 Slurry for casting and demolding as well as preparation method and application thereof

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