CN114685177B - High-strength carbon graphite material and preparation method and application thereof - Google Patents
High-strength carbon graphite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-strength carbon graphite composite material, a preparation method and application thereof, wherein the high-strength carbon graphite composite material can be used for manufacturing structural members for furnaces and comprises the following components in parts by mass: 25-35 parts of silicon composite powder, 15-25 parts of graphite powder, 40-50 parts of carbon fiber powder, 20-30 parts of phenolic resin and 1 part of silane coupling agent. The composite material has excellent performance, particularly obtains performance parameters similar to those of isostatic pressing graphite and carbon/carbon composite materials in the aspects of thermal, electrical and mechanical properties, and has good application prospect and application effect when being used for manufacturing structural members for furnaces; the preparation method of the invention can realize uniform pore size distribution in the composite material, improve the impregnation efficiency and the impregnation effect, simplify the production flow and reduce the production cost.
Description
Technical Field
The invention relates to the field of carbon materials, in particular to a modified carbon fiber, a modified carbon graphite material and a preparation method thereof.
Background
With the rapid growth of the global new energy market, the carbon-based materials in the photovoltaic industry and the industries upstream of the photovoltaic industry are developed vigorously. On one hand, a large amount of carbon micro powder is inevitably generated when manufacturing and processing the carbon-based products for the photovoltaic thermal field and the heat preservation; for the micro powder of the carbon/carbon composite material, secondary efficient utilization is difficult, most of the micro powder is treated in a landfill mode, and the harmfulness of the micro powder to the environment is difficult to evaluate. On the other hand, a large amount of harmful non-carbon micro powder exists on the surface of the material after heat preservation and heating service, the material can cause environmental damage and pollution during solid waste treatment, and more seriously, the non-carbon micro powder is easy to cause human body health; similarly, a large amount of fiber powder is generated during the production of carbon fiber woven materials, and this type of material also has a problem of difficulty in effective utilization and handling.
Most of the existing research reports are concentrated in the preparation and performance research fields of furnace carbon graphite materials and carbon/carbon composite material structural members, and the research reports of preparing high-performance furnace structural members by secondary utilization of solid waste materials are fresh in documents. Meanwhile, the carbon graphite material prepared by the existing process needs to be subjected to processes such as kneading, grinding, molding, multiple dipping and roasting, graphitization and the like. The process is complicated, the control difficulty of the process is high, and after the sample is roasted, because open pores and closed pores are randomly distributed, the impregnation efficiency is difficult to guarantee in the impregnation process, and the target impregnation effect (porosity and density) can be achieved by multiple times of impregnation and roasting, so that the problem that how to simplify the process and improve the impregnation efficiency needs to be solved urgently is solved.
Disclosure of Invention
The invention provides a high-strength carbon graphite material and a preparation method and application thereof, and aims to solve the technical problems that the existing carbon fiber waste is difficult to treat, the existing carbon graphite material preparation process is complex, and the impregnation effect is poor.
In order to solve the technical problem, the invention adopts the following technical scheme:
a high-strength carbon graphite composite material comprises the following components in parts by mass:
20-35 parts of silicon composite powder, 15-25 parts of graphite powder, 30-50 parts of carbon fiber powder and 20-30 parts of phenolic resin. The design idea of the technical scheme is that the carbon fiber powder is used as a main aggregate, a phenolic resin binder with high carbon residue during high-temperature treatment is used as a continuous phase, and then inorganic antioxidant silicon composite powder is used for designing a formula, the silicon composite powder plays a role in particle reinforcement to inhibit the generation and expansion of cracks and disperse stress concentration of a structural member when the structural member is stressed, a reinforcing steel bar-like structure is constructed in the composite material by using the carbon fiber powder, the effect of pulling the graphite powder and the silicon composite powder is achieved, the mechanical strength of the composite material is further improved, a channel is provided for CVD densification by using a gap formed around the carbon fiber, the densification efficiency is improved, the electric conduction and heat conduction performance of the composite material are enhanced by using the graphite powder, and finally the carbon composite material with thermal, electrical and mechanical properties close to those of isostatic pressure graphite is obtained.
As a further optimization of the technical scheme, the carbon fiber powder is carbon micro powder generated by manufacturing a carbon fiber woven body, processing a photovoltaic thermal field or a heat-insulating carbon-based product. The optimal scheme utilizes a large amount of carbon micro powder generated in the process of manufacturing and processing the photovoltaic thermal field and the heat-insulating carbon-based product, finds a new way of sustainable development for efficient solid waste treatment of carbon fiber product using enterprises, carbon graphite material processing enterprises and graphite material using enterprises, and simultaneously reduces the cost of the high-strength carbon graphite composite material.
As a further preferable aspect of the above technical solution, the high-strength carbon graphite composite material further includes 0.1 parts by mass of a silane coupling agent. The purpose of adding the coupling agent is to ensure that the bonding strength of the silicon composite powder, the graphite powder and the phenolic resin is higher.
Based on the same technical concept, the invention also provides a preparation method of the high-strength carbon graphite composite material, which comprises the following steps:
(1) Uniformly mixing the silicon composite powder and graphite powder, and kneading for a set time to obtain a mixed material A;
(2) Adding carbon fiber powder into the mixed material A, and kneading for a set time to obtain a mixed material B;
(3) Adding phenolic resin into the mixed material B, and kneading for a set time to obtain a mixed paste;
(4) Compression molding and curing the mixed paste to obtain an intermediate product; and sequentially carrying out roasting, dipping, graphitization and purification processes on the intermediate product to obtain the high-strength carbon graphite composite material.
This technical scheme's design thinking lies in, through the aforesaid thoughtlessly hold between the fingers and the solidification, flooding, graphitization and purification technology, each component homodisperse, make the hole that forms between carbon fibre and other powder and the hole that the phenolic resin inflation formed in the curing process can evenly distributed, the effect of equal hole has been realized, follow-up impregnation technology's effect and efficiency have been promoted greatly, make this technical scheme's high-strength carbon graphite combined material only need through once flooding, compare in prior art's many times flooding and calcination technology, the flow has been simplified, and the production cost is reduced.
As a further preferable mode of the above-mentioned means, 1 part by mass of a silane coupling agent is further added before kneading in the step (1).
As a further preferable mode of the above-described embodiment, the kneading time in the step (1) is 20min, the kneading time in the step (2) is 30min, and the kneading time in the step (3) is 30min. The mixing time can ensure the uniform mixing of materials in each step, the unreasonable mixing and kneading time can cause adverse effects, the mixing and kneading time is short, the mixing and kneading between powder and between powder and a binder are not uniform, and the particle size of the powder is reduced and agglomeration is caused due to overlong mixing and kneading time.
As a further preferred mode of the above-mentioned means, the molding density of the mixed paste molding by press molding in the step (4) is 1.40g/cm 3 -1.45g/cm 3 . The material in the density range has the best mechanical strength and heat conducting property.
As a further preferred aspect of the above-mentioned technical means, in the step (4), the curing temperature profile of the mixed paste after press molding is: heating to 60-70 ℃ after 30-40 min at normal temperature, preserving heat for 60-70 min, then heating to 100-110 ℃ after 70-80 min, preserving heat for 60-70 min, then heating to 200-210 ℃ after 120-160 min, preserving heat for 120-160 min, and then naturally cooling to room temperature. The curing temperature curve can fully cure the phenolic resin in the composite material, improve the mechanical strength of the composite material and facilitate the later-stage impregnation.
As a further preferable mode of the above technical solution, in the impregnation process of the intermediate product in the step (4), phenolic resin is used as an impregnant, and the impregnation pressure is 5MPa to 7MPa. The impregnation process under the above working conditions can improve the density of the composite material.
As a further preferable mode of the above technical solution, in the process for graphitizing the intermediate product in the step (4), the graphitization temperature is 1800 ℃ to 2400 ℃. The graphitization process within the temperature range can ensure that the carbonized phenolic resin is graphitized smoothly and fully, and improve the resistivity and the heat conductivity coefficient of the composite material.
As a further preferable mode of the above technical means, the process of purifying the intermediate product in the step (4) is performed under freon atmosphere, and the purification temperature is 2600 ℃ to 2800 ℃. The purification process within the temperature range can reduce the impurity content of the material and meet the use requirement.
Based on the same technical concept, the invention also provides application of the high-strength carbon graphite composite material, which is used for preparing structural members for furnaces.
Compared with the prior art, the invention has the advantages that:
(1) The composite material has excellent performance, particularly obtains performance parameters similar to those of isostatic pressing graphite and carbon/carbon composite materials in the aspects of thermal, electrical and mechanical properties, and has good application prospect and application effect when being used for manufacturing structural members for furnaces;
(2) The preparation method of the invention can realize uniform pore size distribution in the composite material, improve the impregnation efficiency and the impregnation effect, simplify the production flow and reduce the production cost.
Drawings
Fig. 1 is an electron micrograph of the high strength carbon graphite composite material of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
the morphology structure of the high-strength carbon graphite composite material of the embodiment is shown in fig. 1, and the high-strength carbon graphite composite material comprises the following components in parts by mass:
20 parts of silicon composite powder, 20 parts of graphite powder, 40 parts of carbon fiber powder, 20 parts of phenolic resin and 0.1 part of silane coupling agent; wherein, the carbon fiber powder is carbon micro powder waste products generated by manufacturing and processing the photovoltaic thermal field. The silicon composite powder is mainly from a silicon carbide layer formed on the surface when the silicon single crystal is pulled, and leftover bits when silicon ingots are processed.
The high-strength carbon graphite composite material of the embodiment is prepared by the following method:
(1) 200g of silicon composite powder and 200g of graphite powder are dry-mixed in a kneading pot for 30min, and then 100g of silane coupling agent with the concentration of 1wt% is added for kneading for 20min, so that a mixed material A is obtained.
(2) Adding 400g of carbon fiber powder into the mixed material A, kneading for 30min, then adding 200g of phenolic resin, and kneading for 20min to obtain a mixed paste;
(3) The mixed paste is subjected to compression molding (the molding density is 1.40-1.45 g/cm) 3 ) The molded sample was cured (curing temperature profile: heating to 60-70 ℃ for 30-40 min at normal temperature, preserving heat for 60-70 min, heating to 100-110 ℃ for 70-80 min, preserving heat for 60-70 min, heating to 200-210 ℃ for 120-160 min, and cooling to room temperature along with the furnace. The density after curing was 1.32g/cm 3 ～1.36g/cm 3 ) And roasting the intermediate product, and sequentially impregnating (an impregnant is phenolic resin and the impregnation pressure is 5 MPa), roasting and graphitizing (the graphitization temperature is 2600-3000 ℃) after roasting, so as to obtain the high-strength carbon graphite composite material of the embodiment.
The high-strength carbon graphite composite material of the present example was subjected to performance testing, and the static physical indexes are shown in table 1 (the following data are sampled in random directions during testing):
table 1 physical parameters of the high strength carbon graphite composite material of example 1
Note: /, denotes the resistivity of the two vertical direction sampling tests.
Example 2:
the high-strength carbon graphite composite material comprises the following components in parts by mass:
20 parts of silicon composite powder, 25 parts of graphite powder, 35 parts of carbon fiber powder, 20 parts of phenolic resin and 0.1 part of silane coupling agent; wherein the carbon fiber powder is carbon micro powder waste products generated in the manufacturing and processing of the photovoltaic thermal field.
The high-strength carbon graphite composite material of the embodiment is prepared by the following method:
(1) 200g of silicon composite powder and 250g of graphite powder are dry-mixed in a kneading pot for 30min, and then 100g of silane coupling agent with the concentration of 1wt% is added for kneading for 20min, so that a mixed material A is obtained.
(2) Adding 350g of carbon fiber powder into the mixed material A, kneading for 30min, then adding 200g of phenolic resin, and kneading for 20min to obtain a mixed paste;
(3) The mixed paste is subjected to compression molding (the molding density is between 1.40 and 1.45 g/cm) 3 ) The molded sample was cured (curing temperature curve: heating to 60-70 ℃ after 30-40 min at normal temperature, preserving heat for 60-70 min, heating to 100-110 ℃ after 70-80 min, preserving heat for 60-70 min, heating to 200-210 ℃ after 120-160 min, preserving heat for 120-160 min, and cooling to room temperature along with the furnace. The density after curing was 1.32g/cm 3 ～1.36g/cm 3 ) And roasting the intermediate product, and sequentially impregnating (an impregnant is phenolic resin and the impregnation pressure is 5 MPa), roasting and graphitizing (the graphitization temperature is 2600-3000 ℃) after roasting, so as to obtain the high-strength carbon graphite composite material of the embodiment.
The high-strength carbon graphite composite material of the present example was subjected to performance testing, and the static physical indexes are shown in table 2 (the following data are sampled in random directions during testing):
table 2 physical parameters of the high strength carbon graphite composite material of example 2
Note: /. Represents the resistivity of two vertical direction sampling tests.
Example 3:
the high-strength carbon graphite composite material comprises the following components in parts by mass:
25 parts of silicon composite powder, 20 parts of graphite powder, 35 parts of carbon fiber powder, 20 parts of phenolic resin and 0.1 part of silane coupling agent; wherein, the carbon fiber powder is carbon micro powder waste products generated by manufacturing and processing the photovoltaic thermal field.
The high-strength carbon graphite composite material of the embodiment is prepared by the following method:
(1) And (2) dry-mixing 200g of silicon composite powder and 250g of graphite powder in a kneading pot for 30min, and then adding 100g of silane coupling agent with the concentration of 1wt% for kneading for 20min to obtain a mixed material A.
(2) Adding 35 parts of carbon fiber powder into the mixed material A, kneading for 30min, then adding 200g of phenolic resin, and kneading for 20min to obtain a mixed paste;
(3) The mixed paste is subjected to compression molding (the molding density is between 1.40 and 1.45 g/cm) 3 ) The molded sample was cured (curing temperature curve: heating to 60-70 ℃ after 30-40 min at normal temperature, preserving heat for 60-70 min, heating to 100-110 ℃ after 70-80 min, preserving heat for 60-70 min, heating to 200-210 ℃ after 120-160 min, preserving heat for 120-160 min, and cooling to room temperature along with the furnace. The density after curing was 1.32g/cm 3 ～1.36g/cm 3 ) And roasting the intermediate product, and sequentially impregnating (an impregnating agent is phenolic resin and the impregnation pressure is 5 MPa), roasting and graphitizing (the graphitizing temperature is 2600-3000 ℃) after roasting to obtain the high-strength carbon graphite composite material of the embodiment.
The high-strength carbon graphite composite material of the present example was subjected to performance testing, and the static physical indexes are shown in table 3 (the following data are sampled in random directions during testing):
table 3 physical parameters of the high strength carbon graphite composite material of example 3
Note: /. Represents the resistivity of two vertical direction sampling tests.
Example 4:
the high-strength carbon graphite composite material comprises the following components in parts by mass:
25 parts of silicon composite powder, 25 parts of graphite powder, 30 parts of carbon fiber powder, 20 parts of phenolic resin and 0.1 part of silane coupling agent; wherein the carbon fiber powder is carbon micro powder waste products generated in the manufacturing and processing of the photovoltaic thermal field.
The high-strength carbon graphite composite material of the embodiment is prepared by the following method:
(1) And (2) dry-mixing 250g of silicon composite powder and 250g of graphite powder in a kneading pot for 30min, and then adding 100g of silane coupling agent with the concentration of 1wt% for kneading for 20min to obtain a mixed material A.
(2) Adding 300g of carbon fiber powder into the evidence section of the mixed material A, kneading for 30min, and then adding 200g of phenolic resin, kneading for 20min to obtain a mixed paste;
(3) The mixed paste is subjected to compression molding (the molding density is 1.40-1.45 g/cm) 3 ) The molded sample was cured (curing temperature profile: heating to 60-70 ℃ after 30-40 min at normal temperature, preserving heat for 60-70 min, heating to 100-110 ℃ after 70-80 min, preserving heat for 60-70 min, heating to 200-210 ℃ after 120-160 min, preserving heat for 120-160 min, and cooling to room temperature along with the furnace. The density after curing was 1.32g/cm 3 ～1.36g/cm 3 ) And roasting the intermediate product, and sequentially impregnating (an impregnating agent is phenolic resin and the impregnation pressure is 5 MPa), roasting and graphitizing (the graphitizing temperature is 2600-3000 ℃) after roasting to obtain the high-strength carbon graphite composite material of the embodiment.
The high-strength carbon graphite composite material of the present example was subjected to performance testing, and the static physical indexes are shown in table 4 (the following data are sampled in random directions during testing):
table 4 physical parameters of the high strength carbon graphite composite material of example 4
Note: /, denotes the resistivity of the two vertical direction sampling tests.
The above description is only a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above-described examples. It will be apparent to those skilled in the art that various modifications and variations can be made without departing from the spirit of the invention.
Claims (8)
1. The high-strength carbon graphite composite material is characterized by comprising the following components in parts by mass:
20 to 35 parts of silicon composite powder, 15 to 25 parts of graphite powder, 30 to 50 parts of carbon fiber powder and 20 to 30 parts of phenolic resin; the carbon fiber powder is carbon micro powder waste products generated by manufacturing carbon fiber woven bodies and processing photovoltaic thermal fields or heat-insulating carbon-based products; the silicon composite powder is derived from a silicon carbide layer formed on the surface when pulling the Czochralski silicon, and a leftover material when processing the silicon ingot.
2. A method for preparing the high-strength carbon graphite composite material according to claim 1, comprising the steps of:
(1) Uniformly mixing the silicon composite powder and graphite powder, and kneading for 10-20min to obtain a mixed material A;
(2) Adding carbon fiber powder into the mixed material A, and kneading for 30 to 40min to obtain a mixed material B;
(3) Adding phenolic resin into the mixed material B, and kneading for 30-40min to obtain a mixed paste;
(4) Compression molding and curing the mixed paste to obtain an intermediate product; and sequentially carrying out roasting, dipping, graphitization and purification processes on the intermediate product to obtain the high-strength carbon graphite composite material.
3. The method for producing a high-strength carbon graphite composite material according to claim 2, wherein the molding density of the mixed paste in the step (4) is 1.40g/cm by press molding 3 ~1.45g/cm 3 。
4. The method for preparing the high-strength carbon graphite composite material according to claim 2, wherein the curing temperature profile of the mixed paste in step (4) after compression molding is as follows: heating to 60-70 ℃ in 30min to 40min at normal temperature, preserving heat for 60min-70min, heating to 100-110 ℃ in 70min-80min, preserving heat for 60min-70min, heating to 200-210 ℃ in 120min-160min, preserving heat for 120min-160min, and naturally cooling to room temperature.
5. The preparation method of the high-strength carbon graphite composite material as claimed in claim 2, wherein the impregnation process of the intermediate product in the step (4) adopts phenolic resin as an impregnant, and the impregnation pressure is 5MPa to 7MPa.
6. The method for preparing the high-strength carbon graphite composite material according to claim 2, wherein in the graphitization process of the intermediate product in the step (4), the graphitization temperature is 1800-2400 ℃.
7. The preparation method of the high-strength carbon graphite composite material as claimed in claim 2, wherein the purification process of the intermediate product in the step (4) is performed under a freon atmosphere, and the purification temperature is 2600 ℃ to 2800 ℃.
8. Use of the high strength carbon graphite composite material according to claim 1 or produced by the method of any one of claims 2 to 7 for the production of structural components for furnaces.
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| CN102515800A (en) * | 2011-12-20 | 2012-06-27 | 叶乐 | Microporous graphite silicon carbide brick |
| CN109020596A (en) * | 2018-09-25 | 2018-12-18 | 湖南科嘉新材料有限公司 | A kind of carbon-carbon composite and preparation method thereof and the application in electrolytic manganese dioxide production |
| CN113497241A (en) * | 2020-03-18 | 2021-10-12 | 广州汽车集团股份有限公司 | Carbon/carbon composite material, fuel cell bipolar plate, fuel cell and preparation method |
| CN113979751A (en) * | 2021-09-28 | 2022-01-28 | 大同新成新材料股份有限公司 | Graphene-carbon graphite composite isostatic pressing material and preparation method thereof |
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| US6878331B2 (en) * | 2002-12-03 | 2005-04-12 | Ucar Carbon Company Inc. | Manufacture of carbon composites by hot pressing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515800A (en) * | 2011-12-20 | 2012-06-27 | 叶乐 | Microporous graphite silicon carbide brick |
| CN109020596A (en) * | 2018-09-25 | 2018-12-18 | 湖南科嘉新材料有限公司 | A kind of carbon-carbon composite and preparation method thereof and the application in electrolytic manganese dioxide production |
| CN113497241A (en) * | 2020-03-18 | 2021-10-12 | 广州汽车集团股份有限公司 | Carbon/carbon composite material, fuel cell bipolar plate, fuel cell and preparation method |
| CN113979751A (en) * | 2021-09-28 | 2022-01-28 | 大同新成新材料股份有限公司 | Graphene-carbon graphite composite isostatic pressing material and preparation method thereof |
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