CN114436668A - Preparation method of C/C crucible side inlaid with ceramic lining - Google Patents
Preparation method of C/C crucible side inlaid with ceramic lining Download PDFInfo
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Abstract
The invention discloses a preparation method of a C/C crucible edge inlaid with a ceramic lining. The method comprises the following steps: preparing colloidal ceramic modifying liquid of glass fiber cloth; soaking the glass fiber cloth in the colloidal ceramic modifying solution, taking out the glass fiber cloth, and drying to obtain modified prepreg cloth; winding the modified prepreg cloth on a winding machine to form a cylindrical body with a multi-layer structure; putting the cylindrical body into a curing furnace and heating to obtain a primary cured cylindrical body; preparing a carbon fiber pre-impregnation liquid, and taking out the carbon fiber cloth after the carbon fiber cloth is impregnated in the pre-impregnation liquid to obtain the carbon fiber pre-impregnation cloth; coating the outer surface of the primary cured cylindrical body with an adhesive, and winding a plurality of layers of carbon fiber prepreg cloth by a winding machine to obtain a composite cylindrical body; putting the composite cylindrical body into a curing furnace and heating to obtain a primary cured composite cylindrical body; and (3) placing the primarily cured composite cylindrical body into a high-temperature furnace, heating to 1500-1800 ℃, preserving the heat for 4 hours, cooling to 150-250 ℃ along with the furnace, and discharging to obtain the C/C crucible edge inlaid with the ceramic lining.
Description
The technical field is as follows:
the invention relates to preparation of a high-temperature-resistant and corrosion-resistant material structural member, in particular to a preparation method of a crucible edge used in a monocrystalline silicon drawing furnace.
Background art:
with the implementation of new energy solar photovoltaic power generation guidelines in China, the photovoltaic power generation material single (poly) crystal silicon preparation industry is rapidly developed, and the demand of C/C thermal field structural members required to be used in the furnace is greatly increased. Particularly, the demand of a C/C material crucible side used by a monocrystalline silicon drawing furnace is greatly increased, the production process of monocrystalline silicon comprises the steps of putting silicon material into a quartz crucible, heating to 1500-1700 ℃ to melt the silicon material, drawing monocrystalline silicon in a molten state, and as the quartz crucible begins to soften at 1500 ℃, in order to prevent the quartz crucible from softening and deforming at high temperature to cause cracking of the crucible, the C/C material crucible side is inevitably sleeved on the outer surface of the quartz crucible, and the crucible side not only can bear the weight and material weight of the quartz crucible, the acting force generated by deformation of the quartz crucible and expansion of silicon liquid, but also is required to have high thermal conductivity and ensure the stability of a thermal field. In order to further reduce the cost of the production of the monocrystalline silicon, a production process of continuously adding a silicon material and continuously pulling is adopted, the pulling time is prolonged to 240-300 hours from 30-40 hours, so that the service life of the existing C/C material crucible side is rapidly shortened, the service life is shortened to 2-3 months at most, and the service life is shortened mainly because the C/C material crucible side is tightly attached to a quartz crucible, the C/C material crucible side reacts with silicon dioxide at high temperature to form a decarburization phenomenon, so that the C/C material crucible side is thinned, the strength is reduced to cause fracture and failure, and the quartz crucible is desilicated while the crucible side is decarburized, so that the service life of the quartz crucible is also seriously influenced. Therefore, how to effectively solve the corrosion resistance and oxidation resistance of the crucible edge made of the C/C material and improve the service life has important significance and economic value.
The invention content is as follows:
the invention aims to disclose a preparation method of a C/C material crucible side with high temperature resistance, corrosion resistance and high strength and a ceramic lining.
The technical solution for realizing the invention is as follows: the preparation method of the C/C crucible side inlaid with the ceramic lining comprises the following steps: a. preparing colloidal ceramic modifying liquid of glass fiber cloth; b. soaking glass fiber cloth in the colloidal ceramic modifying solution, taking out, and drying at 90-110 ℃ to obtain glass fiber cloth modified prepreg cloth; c. winding the modified prepreg cloth obtained in the step b on a cylindrical mold of a winding machine to obtain a cylindrical body with a multilayer structure; d. c, placing the cylindrical body with the cylindrical mold obtained in the step c into a curing furnace, and heating to obtain a primary cured cylindrical body; e. preparing a carbon fiber pre-impregnation liquid, and taking out the carbon fiber cloth after the carbon fiber cloth is impregnated in the pre-impregnation liquid to obtain the carbon fiber pre-impregnation cloth; f. d, coating an adhesive on the outer surface of the primarily cured cylindrical body obtained in the step d, and winding a plurality of layers of the carbon fiber prepreg cloth by a winding machine to obtain a composite cylindrical body; g. putting the product obtained in the step f into a curing furnace, and heating to obtain a primary cured composite cylindrical body; h. g, removing the product obtained in the step gPlacing the mould into a high-temperature furnace in nitrogen (N)2) Heating to 1500-1800 ℃ under protection, preserving heat for 4 hours, cooling to 150-250 ℃ along with the furnace, discharging, and obtaining the C/C crucible edge inlaid with the ceramic lining.
The colloidal ceramic modifying solution comprises the following components in percentage by weight:
the carbon fiber pre-impregnation liquid comprises the following components in percentage by weight:
the curing steps of the step d and the step g are as follows: the cylindrical body or the composite cylindrical body with the mold is placed in a curing furnace, the curing furnace is vacuumized to-0.098 MPa, the pressure is maintained for 2 hours, the pressure rise rate is less than 50Pa/h, then the curing furnace is pressurized by an air compressor, the pressurizing medium is air, the pressurizing speed is 0.08 MPa/min, the pressure is maintained after the pressurizing is carried out to 2.0MPa, meanwhile, the curing furnace is heated in the inner cavity of the mold, the heating rate is 2-7 ℃/h, and the curing furnace is heated to 180-200 ℃ for 2 hours.
And h, arranging an anti-deformation bracket which symmetrically supports the inner wall surface of the composite cylindrical body in the cured composite cylindrical body.
The adhesive in the step f comprises the following components in percentage by weight:
the content of the preliminarily solidified colloidal ceramic modifying liquid contained in the preliminarily solidified cylindrical body obtained in the step d is 40-60% of the weight of the preliminarily solidified cylindrical body in percentage by weight.
And d, winding 20-30 layers of the modified prepreg cloth in the step c on the die, wherein the number of winding layers of the carbon fiber prepreg cloth in the step f is 25-30.
According to the technical scheme disclosed by the invention, the glass fiber cloth modified prepreg cloth is sintered and vitrified at high temperature to form a ceramic structure consisting of various high-melting-point and corrosion-resistant compounds, and the ceramic structure has high mechanical property and corrosion resistance; the carbon fiber prepreg cloth forms a structure which takes C/C materials as main materials and contains a small amount of ceramic components after being fired at high temperature; when the ceramic lining-inlaid C/C crucible side is used, the ceramic lining-inlaid C/C crucible side is in direct contact with the outer wall surface of a quartz crucible, namely the structure of a ceramic component does not react with the quartz crucible, and the structure mainly made of a C/C material is prevented from being in direct contact with the quartz crucible, so that the decarburization of the crucible side is prevented, the desilication of the quartz crucible is prevented, the ceramic lining-inlaid C/C crucible side also has good structural strength and heat conduction performance, the transition of density and the transition of a crystal structure are ensured, the occurrence of thermal stress is avoided, besides the good performance, the preparation cost and the raw material cost are greatly reduced, and the final service life can be prolonged by more than one time.
The specific implementation mode is as follows:
the following detailed description of the present invention will be given in detail, and it should be noted that the description of the embodiments of the present invention is made for the purpose of facilitating a comprehensive understanding of the technical spirit of the present invention, and should not be construed as limiting the scope of the claims of the present invention.
The technical solution of the specific embodiment of the invention is as follows: the preparation method of the C/C crucible side inlaid with the ceramic lining comprises the following steps: a. preparing colloidal ceramic modifying liquid of glass fiber cloth; b. soaking glass fiber cloth in the colloidal ceramic modifying solution, taking out, and drying at 90-110 ℃ to obtain glass fiber cloth modified prepreg cloth; c. winding the modified prepreg cloth obtained in the step b on a cylindrical mold of a winding machine to obtain a cylindrical body with a multilayer structure; d. c, placing the cylindrical body with the cylindrical mold obtained in the step c into a curing furnace, and heating to obtain a primary cured cylindrical body; e. preparing a carbon fiber pre-impregnation liquid, and taking out the carbon fiber cloth after the carbon fiber cloth is impregnated in the pre-impregnation liquid to obtain the carbon fiber pre-impregnation cloth; f. d, coating an adhesive on the outer surface of the primarily cured cylindrical body obtained in the step d, and winding a plurality of layers of the carbon fiber prepreg cloth by a winding machine to obtain a composite cylindrical body; g. putting the product obtained in the step f into a curing furnace, and heating to obtain a primary cured composite cylindrical body; h. and g, demoulding the product obtained in the step g, putting the demoulded product into a high-temperature furnace, heating to 1500-1800 ℃ under the protection of nitrogen (N2), preserving heat for 4 hours, cooling to 150-250 ℃ along with the furnace, and discharging to obtain the C/C crucible edge inlaid with the ceramic lining.
In the above method for preparing a crucible side inlaid with a ceramic lining C/C, the colloidal ceramic modifying solution in step a is formed by mixing a plurality of components, and is in a colloidal state with a certain rheological property, wherein the "ceramic" refers to that the colloidal ceramic modifying solution becomes a ceramic material after subsequent high-temperature firing, and does not mean that the colloidal ceramic modifying solution has ceramic properties or is a ceramic material; in the step b, the glass fiber cloth is dipped in the colloidal ceramic modifying solution and then taken out, the colloidal ceramic modifying solution is attached to the two surfaces and the inside of the glass fiber cloth, and the glass fiber cloth is baked and dried at the temperature of 90-110 ℃, wherein the baking and drying can volatilize part of volatile matters in the colloidal ceramic modifying solution, so as to obtain the modified prepreg cloth of the glass fiber cloth; in the step c, the modified prepreg is wound on a cylindrical die of a winding machine, a plurality of layers of cylindrical bodies of the modified prepreg are arranged on the cylindrical die, the die is hollow and cylindrical, and the section of the cylindrical die is circular, elliptical or rectangular as required; step d, placing the cylindrical body with the cylindrical mold into a curing furnace, heating to further volatilize part of volatile matters in the cylindrical body, and further fusing or mutually permeating all the components to obtain a primary cured cylindrical body; e, after preparing the carbon fiber pre-impregnation liquid, impregnating the carbon fiber cloth in the pre-impregnation liquid, and taking out the carbon fiber cloth, wherein the pre-impregnation liquid is attached to the two surfaces and the inside of the carbon fiber cloth to obtain the carbon fiber pre-impregnation cloth, and the pre-impregnation liquid is formed by mixing a plurality of components, has certain rheological property, and is convenient for the pre-impregnation liquid to permeate into the inside of the carbon fiber cloth and coat the carbon fiber yarns of the carbon fiber cloth; in the step f, coating an adhesive on the outer surface of the primary curing cylindrical body obtained in the step d, and winding a plurality of layers of the carbon fiber prepreg cloth on the outer surface of the primary curing cylindrical body by a winding machine to obtain a composite cylindrical body; in the winding process of the modified prepreg cloth of the glass fiber cloth and the carbon fiber prepreg cloth, the winding machines are respectively provided with a certain balance weight to ensure that the modified prepreg cloth and the carbon fiber prepreg cloth have certain tension, so that a cylindrical body and a composite cylindrical body obtained by winding are more compact; putting the product obtained in the step f into a curing furnace, and heating to obtain a primary cured composite cylindrical body; after the high-temperature firing in the step h, the components in the composite cylinder body are subjected to high-temperature reaction, the colloidal ceramic modified liquid reacts with the surfaces of the fiber yarns of the glass fiber cloth while reacting, the carbon fiber pre-immersion liquid reacts with the surfaces of the carbon fiber yarns of the carbon fiber cloth while reacting, the reaction is quite complex, can be different due to the change of the formula, the proportion, the component granularity and the high-temperature firing temperature, is not completely predicted theoretically, and still belongs to the field of experimental science substantially, and the applicant can obtain the technical scheme step by step after repeated large amount of tests and detections, and can obtain the corrosion-resistant, high-temperature-resistant and high-strength C/C crucible side on the basis of a simpler process compared with the prior art.
The colloidal ceramic modifying solution comprises the following components in percentage by weight: 30-40% of phenolic resin, 30-40% of alcohol, 10-20% of mullite powder, 5-10% of carbon fiber powder, 10-20% of silicon powder, 5-10% of silicon carbide powder, 4-8% of zirconia powder and 5-15% of short carbon fiber. Uniformly mixing all the components of the colloidal ceramic modifying solution to obtain the colloidal ceramic modifying solution with certain rheological property, wherein in the primary curing step d, the phenolic resin and the alcohol can be partially volatilized; in the high-temperature firing step h, the components are subjected to complex chemical reaction to obtain a ceramic material layer, the glass fiber cloth is clamped by the ceramic material layers on the two surfaces, and the components and the fiber yarns of the glass fiber cloth are subjected to interface reaction to realize firm connection of the ceramic material layer and the glass fiber cloth.
The carbon fiber pre-impregnation liquid comprises the following components in percentage by weight: 30-50% of phenolic resin, 30-50% of alcohol, 5-10% of carbon fiber powder, 5-10% of silicon powder and 5-20% of graphite powder. And in the preliminary curing step g, the phenolic resin and the alcohol can be partially volatilized, and in the high-temperature firing step h, the components react to obtain the C/C material.
In order to improve the density and the structural strength of the cylindrical body and the composite cylindrical body, primary curing is carried out in the step d and the step g, and the curing steps of the two steps are as follows: the cylindrical body or the composite cylindrical body with the mold is placed in a curing furnace, the mold can support the cylindrical body or the composite cylindrical body to avoid deformation, the curing furnace is vacuumized to-0.098 MPa, the pressure is maintained for 2 hours, the pressure rise rate is less than 50Pa/h, then an air compressor is used for pressurizing, the pressurizing medium is air, the pressurizing rate is 0.08 MPa/min, the pressure is maintained after the pressure is increased to 2.0MPa, meanwhile, the mold is heated in an inner cavity, the temperature rise rate is 2-7 ℃/h, and the temperature is increased to 180-200 ℃ and is kept for 2 hours. In the curing process, the inner surface of the cylindrical body, which is contacted with the mold, is heated firstly by heating the inner cavity of the mold, so that the inner surface of the cylindrical body or the composite cylindrical body is heated, the inner surface of the cylindrical body or the composite cylindrical body undergoes a primary reaction, and volatile matters generate bubbles.
In the step h of high-temperature firing, the composite cylindrical body is easy to deform at high temperature, so in the step h, an anti-deformation support which symmetrically supports the inner wall surface of the composite cylindrical body is arranged in the cured composite cylindrical body, and the anti-deformation support is a multi-point support frame, or a plurality of vertical strip-shaped supports, or a plurality of horizontal annular supports.
The adhesive comprises the following components in percentage by weight: 30-50% of phenolic resin, 30-50% of alcohol, 5-10% of carbon fiber powder, 5-10% of silicon nitride powder, 5-10% of silicon powder and 5-20% of graphite powder. The adhesive bonds the primary curing cylinder body and the multi-layer carbon fiber prepreg cloth, and in the high-temperature firing process, the adhesive reacts with the surfaces of the primary curing cylinder body and the multi-layer carbon fiber prepreg cloth respectively to form a transition layer.
The content of the preliminarily cured colloidal ceramic modifying liquid contained in the preliminarily cured cylindrical body obtained in the step d is 40-60% of the weight of the preliminarily cured cylindrical body in percentage by weight, so that the preliminarily cured cylindrical body can be ensured to have enough ceramic components after being fired at high temperature, and the corrosion resistance of the invention is ensured.
In order to improve the comprehensive performance of the invention, the modified prepreg cloth in the step c is wound on the die by 20-30 layers, and the number of the wound layers of the carbon fiber prepreg cloth in the step f is 25-30.
Claims (8)
1. The preparation method of the C/C crucible side inlaid with the ceramic lining is characterized by comprising the following steps
a. Preparing colloidal ceramic modifying liquid of glass fiber cloth;
b. soaking glass fiber cloth in the colloidal ceramic modifying solution, taking out, and drying at 90-110 ℃ to obtain glass fiber cloth modified prepreg cloth;
c. winding the modified prepreg cloth obtained in the step b on a cylindrical mold of a winding machine to obtain a cylindrical body with a multilayer structure;
d. c, placing the cylindrical body with the cylindrical mold obtained in the step c into a curing furnace, and heating to obtain a primary cured cylindrical body;
e. preparing a carbon fiber pre-impregnation liquid, and taking out the carbon fiber cloth after the carbon fiber cloth is impregnated in the pre-impregnation liquid to obtain the carbon fiber pre-impregnation cloth;
f. d, coating an adhesive on the outer surface of the primarily cured cylindrical body obtained in the step d, and winding a plurality of layers of the carbon fiber prepreg cloth by a winding machine to obtain a composite cylindrical body;
g. putting the product obtained in the step f into a curing furnace, and heating to obtain a primary cured composite cylindrical body;
h. g, demoulding the product obtained in the step g, putting the demoulded product into a high-temperature furnace, and introducing nitrogen (N)2) Heating to 1500-1800 ℃ under protection, preserving heat for 4 hours, cooling to 150-250 ℃ along with the furnace, discharging, and obtaining the C/C crucible edge inlaid with the ceramic lining.
2. The method for preparing a C/C crucible side inlaid with a ceramic lining according to claim 1, wherein the colloidal ceramic modifying solution comprises the following components in percentage by weight:
3. the method for preparing a C/C crucible side inlaid with a ceramic lining according to claim 1, wherein the carbon fiber pre-impregnation liquid comprises the following components in percentage by weight:
4. the method for preparing a C/C crucible side inlaid with a ceramic lining according to claim 1, 2 or 3, wherein the curing steps of the step d and the step g are as follows: the cylindrical body or the composite cylindrical body with the mold is placed in a curing furnace, the curing furnace is vacuumized to-0.098 MPa, the pressure is maintained for 2 hours, the pressure rise rate is less than 50Pa/h, then the curing furnace is pressurized by an air compressor, the pressurizing medium is air, the pressurizing speed is 0.08 MPa/min, the pressure is maintained after the pressurizing is carried out to 2.0MPa, meanwhile, the curing furnace is heated in the inner cavity of the mold, the heating rate is 2-7 ℃/h, and the curing furnace is heated to 180-200 ℃ for 2 hours.
5. The method for preparing a C/C crucible edge with a ceramic lining as claimed in claim 4, wherein in the step h, a deformation-preventing support is provided in the cured composite cylindrical body for symmetrically supporting the inner wall surface of the composite cylindrical body.
6. The method for preparing a C/C crucible side inlaid with a ceramic lining according to claim 5, wherein the adhesive in the step f comprises the following components in percentage by weight:
7. the method for preparing a ceramic lining-inlaid C/C crucible edge as claimed in claim 6, wherein the primary cured tubular body obtained in step d contains the primary cured colloidal ceramic modifying solution in an amount of 40-60% by weight based on the weight of the primary cured tubular body.
8. The method for preparing a C/C crucible side with a ceramic lining according to claim 7, wherein the modified prepreg cloth in the step C is wound on a mold for 20-30 layers, and the number of the wound layers of the carbon fiber prepreg cloth in the step f is 25-30 layers.
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| CN102936148A (en) * | 2012-12-05 | 2013-02-20 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material for high-temperature furnace |
| CN106191987A (en) * | 2014-10-24 | 2016-12-07 | 罗万前 | A kind of crucible for growing single-crystal silicon and preparation method thereof |
| CN111039685A (en) * | 2019-11-22 | 2020-04-21 | 烟台凯泊复合材料科技有限公司 | Large integral thin-wall carbon/ceramic composite material gas limiting cylinder and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936148A (en) * | 2012-12-05 | 2013-02-20 | 湖南博云新材料股份有限公司 | Preparation method of carbon/carbon composite material for high-temperature furnace |
| CN106191987A (en) * | 2014-10-24 | 2016-12-07 | 罗万前 | A kind of crucible for growing single-crystal silicon and preparation method thereof |
| CN111039685A (en) * | 2019-11-22 | 2020-04-21 | 烟台凯泊复合材料科技有限公司 | Large integral thin-wall carbon/ceramic composite material gas limiting cylinder and preparation method thereof |
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