CN112430116A - Preparation method of carbon/carbon composite material PECVD bearing frame - Google Patents
Preparation method of carbon/carbon composite material PECVD bearing frame Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5248—Carbon, e.g. graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
Abstract
The invention discloses a preparation method of a carbon/carbon composite material PECVD bearing frame, which comprises the following steps: 1) forming a prefabricated body, namely layering the carbon cloth and the net tire on a flat needle machine, and performing a needle punching process to prepare a prefabricated body plate; 2) curing in a vacuum pressure state by using an RTM (resin transfer molding) process; 3) carbonizing the resin plate; 4) liquid phase impregnation densification; 5) performing high-temperature graphitization treatment; 6) and (4) machining and forming. Compared with the prior art, the carbon/carbon composite material bearing frame used by the invention is a 2.5D structure prefabricated plate obtained by needling the prefabricated body, and the method has the advantages that the interlayer bonding force of the prefabricated body is enhanced, and the layering problem is better avoided; secondly, the RTM process and the liquid phase impregnation densification process greatly shorten the production period and the cost of the product.
Description
Technical Field
The invention relates to the technical field of solar photovoltaics, in particular to a preparation method of a carbon/carbon composite material PECVD bearing frame.
Background
With the continuous development of new energy in recent years, the photovoltaic solar power generation industry is regarded as a key development project in many countries, solar cell module systems are paid more and more attention, and a film needs to be coated on a silicon wafer in the production of silicon cells, so that the reflection of light is reduced, and the utilization rate of the light is improved. Currently, the most widely used coating process is a Plasma Enhanced Chemical Vapor Deposition (PECVD) process. The process is to make the gas containing film component atoms form plasma locally by means of microwave or radio frequency, and the plasma is very chemically active and can easily react to deposit the desired film on the substrate. In view of the complex process environment of PECVD, commonly used PECVD boats or boat plates are mainly made of graphite. However, the graphite boat has high operation difficulty and low strength, so that the use and replacement frequency is high and the cost is high.
The method for solving the problems in the market at present is to improve the plate preparation process, improve the density and increase the strength, and although some problems are solved, the problems of low strength and easy damage are not solved fundamentally, so that the replacement frequency and the cost of the bearing frame are greatly increased.
In the carbon-carbon composite material, the performance of the PECVD bearing frame prepared by the carbon cloth lamination post-mould pressing impregnation carbonization process and the deposition, impregnation and carbonization process after the flat plate needling can meet the use requirements of the carbon cloth lamination post-mould pressing impregnation carbonization process. However, the production cycle based on this process is long and costly, and these problems have been difficult to solve for a while. Based on the above, the scheme designs a preparation method of the carbon/carbon composite material PECVD bearing frame, so as to solve the problems.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a carbon/carbon composite material PECVD bearing frame to solve the problems.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a carbon/carbon composite material PECVD bearing frame is characterized by comprising the following steps: the method comprises the following steps:
1) forming a prefabricated body, namely layering the carbon cloth and the net tire on a flat needle machine, and performing a needle punching process to prepare a prefabricated body plate;
2) curing in a vacuum pressure state by using an RTM (resin transfer molding) process;
3) carbonizing the resin plate;
4) liquid phase impregnation densification;
5) performing high-temperature graphitization treatment;
6) and (4) machining and forming.
Preferably, in the step 1), an automatic flat needle machine is adopted to perform Z-direction needling on the layered carbon cloth and the net tire to prepare the 2.5D prefabricated plate.
Preferably, the density of the needled preform plate is 0.8-1.1 g/m, the thickness of the preform plate is 5-20 mm, the length is 1000-2000 mm, and the width is 500-1500 mm.
Preferably, the plate in step 2) is subjected to vacuum resin introduction and hot-pressing curing process, the carbon/carbon prefabricated plate is obtained through resin impregnation, temperature rise and pressure curing, and the carbon/carbon plate is completely filled with the resin, so that the porosity of the plate is 1% -5%.
Preferably, the resin is one of an ammonia phenolic resin or a furan resin.
Preferably, the RTM process temperature in the step 2) is 120-200 ℃, and the pressurizing pressure is 0.8-1.5 MPa.
Preferably, in the step 3), the cured carbon/carbon plate is placed by a tool and then is hung into a carbonization furnace, carbonization treatment is carried out according to the carbonization curve of furan and ammonia phenolic aldehyde, the carbonization temperature is 800-950 ℃, and the temperature is naturally reduced to room temperature after the process is finished.
Preferably, in the step 4), the carbonized carbon/carbon plate is subjected to liquid-phase impregnation densification so that the plate density is not less than 1.4g/m for carrying out thin film cultivation.
Preferably, in the step 5), the carbon/carbon plate meeting the density requirement and a tool are subjected to high-temperature graphitization treatment at 2000-2500 ℃.
The preparation method of the carbon/carbon composite material PECVD bearing frame comprises the following steps: the method comprises the steps of preform forming, curing in a RTM process vacuum pressure state, resin plate carbonization, liquid phase impregnation densification, high temperature graphitization treatment and machine processing forming. Compared with the prior art, the carbon/carbon composite material bearing frame used by the invention is a 2.5D structure prefabricated plate obtained by needling the prefabricated body, and the method has the advantages that the interlayer bonding force of the prefabricated body is enhanced, and the layering problem is better avoided; secondly, the RTM process and the liquid phase impregnation densification process greatly shorten the production period and the cost of the product.
Drawings
Fig. 1 is a schematic structural diagram of a carrying frame according to the present invention.
Detailed Description
In order to further understand and appreciate the structural features and advantages of the present invention, preferred embodiments are described in detail below with reference to the accompanying drawings:
example 1
A preparation method of a carbon/carbon composite material PECVD bearing frame comprises the following steps:
1) preparing and forming the prefabricated body, namely alternately layering carbon cloth woven by 12k fibers and 80g/m carbon cloth by adopting an automatic flat needle machine, and needling the carbon cloth and the net tire into a 2.5D flat prefabricated body with Z-direction fibers by utilizing flat needle punching, wherein the density of the flat prefabricated body is 1.2g/cm through thin film needle punching, and the size of the flat plate is 1200mm 800mm 550 mm;
2) the RTM process is cured under a vacuum pressure state, the prefabricated flat plate is subjected to hot-pressing curing by utilizing the modes of resin internal vacuum introduction and external pressurization and temperature rise, a resin agent is furan resin and a 1% p-toluenesulfonic acid curing agent, the temperature is raised to 150 ℃, and the pressure is raised to 1MPa, so that the resin is completely cured and filled into the pores of the flat plate;
3) carbonizing a flat plate, designing a tool by using a graphite plate, putting the solidified flat plate between two graphite plate tools, heating and carbonizing according to a carbonization curve process of furan resin, wherein the carbonization temperature is 950 ℃, and then naturally cooling the flat plate to room temperature in a furnace;
4) liquid phase impregnation, namely putting the flat plates into a vacuum pressure impregnation furnace, impregnating the flat plates with furan resin, padding a carbon felt block between each flat plate to ensure that impregnation liquid between the flat plates is completely infiltrated, sucking the impregnation liquid into the furnace with the flat plates by utilizing vacuum pressure difference, pressurizing to 2MPa, returning redundant impregnation liquid after maintaining pressure for 3 hours, heating the furnace to 180 ℃ for densification, and carrying out thin-wall forging on the plates to ensure that the density of the plates reaches 1.6 g/cm;
5) high-temperature graphitization purification, namely performing high-temperature graphitization treatment by using a flat plate of a graphite tool used in carbonization, wherein the treatment temperature is 2000 ℃;
6) and machining the bearing frame into the precise size of the required bearing frame according to requirements.
Example 2
A preparation method of a carbon/carbon composite material PECVD bearing frame comprises the following steps:
1) preparing and forming the prefabricated body, namely alternately layering carbon cloth woven by 12k fibers and carbon cloth of 70g/m by adopting an automatic flat needle machine, and needling the carbon cloth and the net tire into the 2.5D flat prefabricated body with Z-direction fibers by utilizing flat needle punching. The density of the slab preform was 1.0g/cm for thin-wall labor, the slab size was 1300mm 1200mm 550 mm;
2) the RTM process is cured under a vacuum pressure state, the prefabricated body flat plate is subjected to hot-pressing curing by utilizing the modes of resin internal vacuum introduction and external pressurization and temperature rise, a resin agent is ammonia phenolic resin, the temperature is raised to 140 ℃, and the pressure is raised to 1MPa, so that the resin is completely cured and filled into the flat plate pores;
3) carbonizing a flat plate, designing a tool by using a graphite plate, putting the solidified flat plate between two graphite plate tools, heating and carbonizing according to a carbonization curve process of phenolic resin, wherein the carbonization temperature is 900 ℃, and then naturally cooling the flat plate to room temperature in a furnace;
4) liquid phase impregnation, namely putting the flat plates into a vacuum pressure impregnation furnace, impregnating the flat plates with furan resin, padding a carbon felt block between each flat plate to ensure that impregnation liquid between the flat plates is completely infiltrated, sucking the impregnation liquid into the furnace with the flat plates by utilizing vacuum pressure difference, pressurizing to 2MPa, returning redundant impregnation liquid after maintaining pressure for 3 hours, heating the furnace to 180 ℃ for densification, and carrying out thin-wall forging on the plates to ensure that the density of the plates reaches 1.55 g/cm;
5) high-temperature graphitization purification, namely performing high-temperature graphitization treatment by using a flat plate of a graphite tool used in carbonization, wherein the treatment temperature is 2050 ℃;
6) and machining the bearing frame into the precise size of the required bearing frame according to requirements.
Example 3
A preparation method of a carbon/carbon composite material PECVD bearing frame comprises the following steps:
1) preparing and forming the prefabricated body, namely alternately layering carbon cloth woven by 12k fibers and carbon cloth of 50g/m by adopting an automatic flat needle machine, and needling the carbon cloth and the net tire into the 2.5D flat prefabricated body with Z-direction fibers by utilizing flat needle punching. The density of the slab preform was 1.10g/cm for thin-wall labor, the slab size was 2000mm 1500mm 600 mm;
2) the RTM process is cured under a vacuum pressure state, the prefabricated body flat plate is subjected to hot-pressing curing by utilizing the modes of resin internal vacuum introduction and external pressurization and temperature rise, the ratio of a resin agent to furan-ammonia phenolic resin is 1:1, the temperature is raised to 180 ℃, and the pressure is raised to 1MPa, so that the resin is completely cured and filled into the flat plate pores;
3) carbonizing a flat plate, designing a tool by using a graphite plate, putting the solidified flat plate between two graphite plate tools, heating and carbonizing according to a carbonization curve process of furan and phenolic resin, wherein the carbonization temperature is 920 ℃, and then naturally cooling the flat plate to room temperature in a furnace;
4) liquid phase impregnation, namely putting the flat plates into a vacuum pressure impregnation furnace, impregnating the flat plates with furan resin, padding a carbon felt block between each flat plate to ensure that impregnation liquid between the flat plates is completely infiltrated, sucking the impregnation liquid into the furnace with the flat plates by utilizing vacuum pressure difference, pressurizing to 2MPa, returning redundant impregnation liquid after maintaining pressure for 3 hours, heating the furnace to 180 ℃ for densification, and carrying out thin-wall forging on the plates to ensure that the density of the plates reaches 1.6 g/cm;
5) high-temperature graphitization purification, namely performing high-temperature graphitization treatment by using a flat plate of a graphite tool used in carbonization, wherein the treatment temperature is 2100 ℃;
6) and machining the bearing frame into the precise size of the required bearing frame according to requirements.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A preparation method of a carbon/carbon composite material PECVD bearing frame is characterized by comprising the following steps: the method comprises the following steps:
1) forming a prefabricated body, namely layering the carbon cloth and the net tire on a flat needle machine, and performing a needle punching process to prepare a prefabricated body plate;
2) curing in a vacuum pressure state by using an RTM (resin transfer molding) process;
3) carbonizing the resin plate;
4) liquid phase impregnation densification;
5) performing high-temperature graphitization treatment;
6) and (4) machining and forming.
2. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 1, is characterized in that: and in the step 1), Z-direction needling is carried out on the layered carbon cloth and the net tire by adopting an automatic flat needle machine, so as to prepare the 2.5D prefabricated plate.
3. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 1, is characterized in that: the density of the needled prefabricated plate is 0.8-1.1 g/m, the thickness of the prefabricated plate is 5-20 mm, the length of the prefabricated plate is 1000-2000 mm, and the width of the prefabricated plate is 500-1500 mm.
4. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 1, is characterized in that: and (3) performing vacuum resin introduction and hot-pressing curing on the plate in the step 2), impregnating the plate with resin, heating, pressurizing and curing to obtain a carbon/carbon prefabricated plate, and completely filling the carbon/carbon plate with the resin to ensure that the porosity of the plate is 1-5%.
5. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 4, is characterized in that: the resin is one of ammonia phenolic resin or furan resin.
6. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 1, is characterized in that: the RTM process temperature in the step 2) is 120-200 ℃, and the pressurizing pressure is 0.8-1.5 MPa.
7. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 1, is characterized in that: and 3) placing the cured carbon/carbon plate by using a tool, then hoisting the cured carbon/carbon plate into a carbonization furnace, carrying out carbonization treatment according to the carbonization curve of furan and ammonia phenolic aldehyde, wherein the carbonization temperature is 800-950 ℃, and naturally cooling to room temperature after the process is finished.
8. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 1, is characterized in that: and in the step 4), carrying out liquid-phase impregnation densification on the carbonized carbon/carbon plate so as to enable the density of the plate to be more than or equal to 1.4g/m for carrying out thin film strip production.
9. The method for preparing the carbon/carbon composite PECVD carrying frame according to the claim 1, is characterized in that: and in the step 5), a carbon/carbon plate meeting the density requirement is added with a tool to perform high-temperature graphitization treatment, wherein the treatment temperature is 2000-2500 ℃.
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Cited By (2)
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| CN113135766A (en) * | 2021-04-29 | 2021-07-20 | 上海骐杰碳素材料有限公司 | Carbon or carbon ceramic plate prefabricated body, product and preparation method thereof |
| CN113845369A (en) * | 2021-10-29 | 2021-12-28 | 西安美兰德新材料有限责任公司 | Production process of plate for carbon spliced heat-insulation cylinder |
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Application publication date: 20210302 |