CN114773079A - Preparation method of hard carbon fiber thermal insulation material with graphene efficient erosion-resistant layer - Google Patents
Preparation method of hard carbon fiber thermal insulation material with graphene efficient erosion-resistant layer Download PDFInfo
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Abstract
The invention relates to a preparation method of a hard carbon fiber thermal insulation material with a graphene efficient erosion-resistant layer, belonging to the technical field of thermal insulation materials and comprising the following steps: uniformly spraying the binder to the surface of the carbon fiber needled felt; winding the treated carbon fiber needled felt fibers on a forming die for forming; sequentially carrying out curing treatment and carbonization treatment on the molded product to obtain a hard carbon fiber heat-insulating material blank; mechanically processing the blank of the hard carbon fiber heat-insulating material to obtain a processed piece; and carrying out coating treatment on the workpiece. The product prepared by the invention solves the problem that the product can not be directly used in a single crystal furnace, can improve the surface compactness and the anti-corrosion capability of the product, increases the variety of hard carbon fiber products, can replace the carbon/graphite material in the existing single crystal furnace, improves the product competitiveness, and improves the total service life by 2-3 times compared with the hard cylindrical heat-insulating material of the traditional coating.
Description
Technical Field
The invention relates to the technical field of heat-insulating materials, in particular to a preparation method of a hard carbon fiber heat-insulating material with a graphene efficient erosion-resistant layer.
Background
The hard carbon fiber felt is one of advanced thermal structure materials which can be used in high-temperature environment, has the characteristics of low density, high stability, ablation resistance, corrosion resistance, excellent high-temperature mechanical property and the like, and has a large number of micropores in the interior to ensure that the hard carbon fiber felt has outstanding high-temperature heat-insulating property, so the hard carbon fiber felt is widely applied to heat-insulating materials of aerospace, aviation and high-temperature industrial furnaces. However, some high-temperature industrial equipment (such as a metal heat treatment furnace and a single crystal growth furnace) has large environmental temperature change of a thermal field, the temperature is increased and decreased at 0-1800 ℃, the thermal shock strength of a product is large, inert gas is mostly adopted for gas cooling, particulate matters in the thermal field are mixed in the gas to form high-speed particle flow, the surface of a furnace lining material is eroded, and meanwhile, silicon vapor erodes the surface of the material. If the heat insulation material is used alone, the service life of the material is seriously shortened.
Aiming at the problem that the low-density hard carbon fiber felt is poor in oxidation and erosion resistance, in order to improve the thermal shock resistance and the silicon vapor corrosion resistance of the low-density hard carbon fiber felt, the optimal choice is to improve the compactness of the surface of the low-density hard carbon fiber felt and prepare a gas erosion resistant protective layer. Graphene, one of ideal candidate materials for the gas erosion resistant coating, has excellent properties such as high melting point, high thermal stability, large flake structure, good physicochemical compatibility with a hard carbon fiber felt, approximate linear expansion coefficient and the like, and is paid much attention as a high-temperature oxidation resistant coating, but the graphene coating can also improve the thermal shock resistance of a matrix besides protecting the matrix from being oxidized.
At present, most of hard carbon fiber felt surface coatings are graphite powder or graphite emulsion and resin, and the coatings are finished by manual coating, the graphite powder is granular, graphite powder with different granularities is accumulated on the surface of a product and is linked with a residual carbon skeleton after the resin is heated to form a protective layer, so that the surface of the existing coating is not high in compactness, in recent years, the photovoltaic industry is continuously developed, the cost control of monocrystalline silicon is more and more strict, the requirement on auxiliary material cost is correspondingly reduced, the idea of canceling a carbon-carbon heat-insulating cylinder is provided for reducing the cost, the hard carbon fiber heat-insulating material is directly used, and under the protection of a carbon-carbon inner cylinder in a monocrystalline furnace, a heater is directly faced to the monocrystalline furnace, the corrosion of silicon steam and the purging of inert protective gas are realized, the existing coatings cannot bear the complex environment, the coatings are quickly corroded by the environment in the furnace, the surfaces of the products are cracked, and are pulverized and cannot be used.
Disclosure of Invention
The invention aims to provide a preparation method of a hard carbon fiber heat-insulating material with a graphene efficient erosion-resistant layer, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a hard carbon fiber heat-insulating material with a graphene efficient erosion-resistant layer comprises the following steps:
uniformly spraying the binder onto the surface of the carbon fiber needled felt;
winding the treated carbon fiber needled felt fibers on a forming die for forming;
sequentially carrying out curing treatment and carbonization treatment on the molded product to obtain a hard carbon fiber heat-insulating material blank;
mechanically processing the blank of the hard carbon fiber heat-insulating material to obtain a processed piece;
and carrying out coating treatment on the workpiece.
As a further technical scheme of the invention, the coating treatment comprises a primary coating, a secondary coating and a seal coating which are sequentially carried out, and the primary coating and the secondary coating are respectively and sequentially subjected to post-curing treatment and post-carbonization treatment; the primary coating comprises the following raw materials in percentage by weight: 20-40 parts of phenolic resin, 10-20 parts of graphite powder, 40-70 parts of ethanol and 0.5-2 parts of carbon black, and the raw materials are mixed during preparation and stirred for 20-40min under the conditions of 15000-25000 rpm.
As a further technical scheme of the invention, the secondary coating comprises the following raw materials in percentage by weight: 15-35 parts of phenolic resin, 5-10 parts of graphite powder, 5-10 parts of graphene, 5-10 parts of short fibers, 45-60 parts of ethanol and 0.5-2 parts of carbon black, wherein the raw materials are mixed during preparation and stirred for 20-40min under the condition of 15000-25000 rpm.
As a still further technical scheme of the invention, the seal coat comprises the following raw materials in percentage by weight: 1-5 parts of phenolic resin, 3-10 parts of graphene, 0.5-1 part of surface film-forming aid, 0.5-1 part of leveling aid, 0.5-1 part of antioxidant aid and 72-90 parts of ethanol, and the raw materials are mixed during preparation and stirred for 20-40min under the condition of 15000-25000 rpm.
As a further technical scheme of the invention, the carbon fiber needled felt is polypropylene-based needled felt or asphalt-based needled felt.
As a further technical scheme of the present invention, the binder is an epoxy resin adhesive or a phenolic resin adhesive.
As a further technical scheme of the invention, the curing treatment temperature is 160-180 ℃, and the curing treatment time is 6-9 h.
As a further technical scheme of the invention, the carbonization treatment temperature is 1600-2000 ℃, and the carbonization treatment time is 14-20 h.
As a further technical scheme of the invention, the post-curing treatment temperature is 160-180 ℃, and the post-curing treatment time is 4-6 h.
As a further technical scheme of the invention, the post-carbonization treatment temperature is 1600-2200 ℃, and the post-carbonization treatment time is 14-20 h.
Compared with the prior art, the invention has the beneficial effects that: the prepared product solves the problem that the product can not be directly used in a single crystal furnace, can improve the surface compactness and the anti-corrosion capability of the product, increases the variety of hard carbon fiber products, can replace the carbon/graphite material in the existing single crystal furnace, improves the product competitiveness, and improves the overall service life by 2-3 times compared with the hard cylindrical heat-insulating material of the traditional coating.
Drawings
FIG. 1 is a graph of the densification of the coating of example 1;
FIG. 2 is a graph showing the densification of the coating in comparative example 1.
Detailed Description
Example 1
A preparation method of a hard carbon fiber thermal insulation material with a graphene efficient erosion-resistant layer comprises the following steps:
uniformly spraying an epoxy resin adhesive to the surface of the polypropylene-based needled felt;
winding the polypropylene-based needled felt on a forming die for forming;
sequentially carrying out curing treatment and carbonization treatment on the molded product, wherein the curing treatment is carried out for 9 hours at 160 ℃, and the carbonization treatment is carried out for 20 hours at 1600 ℃ to obtain a hard carbon fiber heat-insulating material blank;
machining the hard carbon fiber heat-insulating material blank to obtain a machined part;
sequentially carrying out primary coating, secondary coating and seal coating on the machined part, and sequentially carrying out post-curing treatment and post-carbonization treatment on the primary coating and the secondary coating;
the primary coating comprises the following raw materials by weight: 2kg of phenolic resin, 1kg of graphite powder, 4kg of ethanol and 0.05kg of carbon black, wherein the raw materials are mixed during preparation and stirred for 40min under the condition of 15000 rpm;
the secondary coating comprises the following raw materials by weight: 1.5kg of phenolic resin, 0.5kg of graphite powder, 0.5kg of graphene, 0.5kg of short fiber, 4.5kg of ethanol and 0.05kg of carbon black, wherein the raw materials are mixed and stirred for 40min at the speed of 15000 rpm;
the seal coat comprises the following raw materials by weight: 0.1kg of phenolic resin, 0.3kg of graphene, 0.05kg of surface film-forming aid, 0.05kg of leveling aid, 0.05kg of antioxidant aid and 7.2kg of ethanol, wherein the raw materials are mixed and stirred for 40min at the speed of 15000rpm during preparation;
the post-curing treatment is carried out at 160 ℃ for 6h, and the post-carbonizing treatment is carried out at 1600 ℃ for 20 h.
Example 2
A preparation method of a hard carbon fiber heat-insulating material with a graphene efficient erosion-resistant layer comprises the following steps:
uniformly spraying the phenolic resin adhesive to the surface of the asphalt-based needled felt;
winding the asphalt-based needled felt on a forming die for forming;
sequentially carrying out curing treatment and carbonization treatment on the molded product, wherein the curing treatment is carried out for 7 hours at 170 ℃, and the carbonization treatment is carried out for 17 hours at 1800 ℃ to obtain a hard carbon fiber heat-insulating material blank;
machining the hard carbon fiber heat-insulating material blank to obtain a machined part;
sequentially carrying out primary coating, secondary coating and seal coating on the machined part, and sequentially carrying out post-curing treatment and post-carbonization treatment on the primary coating and the secondary coating;
the primary coating comprises the following raw materials by weight: 3kg of phenolic resin, 1.5kg of graphite powder, 5.5kg of ethanol and 0.1kg of carbon black, wherein the raw materials are mixed during preparation and stirred for 30min at 20000 rpm;
the secondary coating comprises the following raw materials by weight: 2.5kg of phenolic resin, 0.75kg of graphite powder, 0.75kg of graphene, 0.75kg of short fiber, 5kg of ethanol and 0.1kg of carbon black, wherein the raw materials are mixed and stirred for 30min at 20000rpm during preparation;
the seal coat comprises the following raw materials by weight: 0.25kg of phenolic resin, 0.6kg of graphene, 0.075kg of surface film-forming additive, 0.075kg of leveling additive, 0.075kg of antioxidant additive and 8.5kg of ethanol, wherein the raw materials are mixed and stirred for 30min at 20000rpm during preparation;
the post-curing treatment was carried out at 170 ℃ for 5 hours, and the post-carbonization treatment was carried out at 1900 ℃ for 17 hours.
Example 3
A preparation method of a hard carbon fiber heat-insulating material with a graphene efficient erosion-resistant layer comprises the following steps:
uniformly spraying an epoxy resin adhesive to the surface of the asphalt-based needled felt;
winding the asphalt-based needled felt on a forming die for forming;
sequentially carrying out curing treatment and carbonization treatment on the molded product, wherein the curing treatment is carried out for 6 hours at 180 ℃, and the carbonization treatment is carried out for 14 hours at 2000 ℃, so as to obtain a hard carbon fiber heat-insulating material blank;
mechanically processing the blank of the hard carbon fiber heat-insulating material to obtain a processed piece;
sequentially carrying out primary coating, secondary coating and seal coating on the machined part, and sequentially carrying out post-curing treatment and post-carbonization treatment on the primary coating and the secondary coating;
the primary coating comprises the following raw materials by weight: 4kg of phenolic resin, 2kg of graphite powder, 7kg of ethanol and 0.2kg of carbon black, wherein the raw materials are mixed during preparation and stirred for 20min at 25000 rpm;
the secondary coating comprises the following raw materials by weight: 3.5kg of phenolic resin, 1kg of graphite powder, 1kg of graphene, 1kg of short fibers, 6kg of ethanol and 0.2kg of carbon black, wherein the raw materials are mixed and stirred at 25000rpm for 20 during preparation;
the seal coat comprises the following raw materials by weight: 0.5kg of phenolic resin, 1kg of graphene, 0.1kg of surface film-forming aid, 0.1kg of leveling aid, 0.1kg of antioxidant aid and 9kg of ethanol, wherein the raw materials are mixed and stirred for 20min at 25000 rpm;
the post-curing treatment is carried out at 180 ℃ for 4h, and the post-carbonizing treatment is carried out at 2200 ℃ for 14 h.
Comparative example 1
The asphalt-based needled felt thermal insulation material prepared by using conventional graphite powder as a coating is a comparative example 1.
Examples of the experiments
And (3) detecting the compactness of the coating: the coatings of example 1 and comparative example 1 were tested, and referring to fig. 1 and 2, it can be seen that the density of the coating of example 1 of the present invention is significantly improved.
Detection of extreme conditions: after the products prepared in the example 1 and the comparative example 1 are heated to 1000 ℃ in a muffle furnace, the products are taken out and quickly put into cold water for quenching, and the product is pulverized after the coating of the product is oxidized for a plurality of times; multiple groups were tested and the average was rounded, the results are shown in table 1 below.
TABLE 1 extreme conditions Experimental data
| Type of product | Number of stoves |
| Example 1 | 20 |
| Comparative example 1 | 7 |
As can be seen from Table 1, the product prepared in example 1 of the invention has longer lasting time, good oxidation resistance and thermal shock resistance, and the total service life is improved by 2-3 times compared with that of the hard cylindrical thermal insulation material with the conventional coating.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A preparation method of a hard carbon fiber heat-insulating material with a graphene efficient erosion-resistant layer is characterized by comprising the following steps:
uniformly spraying the binder to the surface of the carbon fiber needled felt;
winding the treated carbon fiber needled felt fibers on a forming die for forming;
sequentially carrying out curing treatment and carbonization treatment on the molded product to obtain a hard carbon fiber heat-insulating material blank;
machining the hard carbon fiber heat-insulating material blank to obtain a machined part;
and carrying out coating treatment on the workpiece.
2. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer according to claim 1, wherein the coating treatment comprises a primary coating, a secondary coating and a seal coating which are sequentially carried out, and the primary coating and the secondary coating are sequentially subjected to post-curing treatment and post-carbonizing treatment; the primary coating comprises the following raw materials in parts by weight: 20-40 parts of phenolic resin, 10-20 parts of graphite powder, 40-70 parts of ethanol and 0.5-2 parts of carbon black, and the raw materials are mixed during preparation and stirred for 20-40min under the conditions of 15000-25000 rpm.
3. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer according to claim 2, wherein the secondary coating comprises the following raw materials in percentage by weight: 15-35 parts of phenolic resin, 5-10 parts of graphite powder, 5-10 parts of graphene, 5-10 parts of short fibers, 45-60 parts of ethanol and 0.5-2 parts of carbon black, wherein the raw materials are mixed during preparation and stirred for 20-40min under the condition of 15000-25000 rpm.
4. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer according to claim 2, wherein the seal coating comprises the following raw materials in percentage by weight: 1-5 parts of phenolic resin, 3-10 parts of graphene, 0.5-1 part of surface film-forming assistant, 0.5-1 part of leveling assistant, 0.5-1 part of antioxidant assistant and 72-90 parts of ethanol, and the raw materials are mixed during preparation and stirred for 20-40min under the condition of 15000-25000 rpm.
5. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer according to claim 1, wherein the carbon fiber needled felt is polypropylene-based needled felt or asphalt-based needled felt.
6. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer according to claim 1, wherein the binder is an epoxy resin adhesive or a phenolic resin adhesive.
7. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer as claimed in claim 1, wherein the curing temperature is 160-180 ℃, and the curing time is 6-9 h.
8. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer as claimed in claim 1, wherein the carbonization temperature is 1600-2000 ℃, and the carbonization time is 14-20 h.
9. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer as claimed in claim 1, wherein the post-curing treatment temperature is 160-180 ℃, and the post-curing treatment time is 4-6 h.
10. The preparation method of the hard carbon fiber thermal insulation material with the graphene high-efficiency erosion-resistant layer as claimed in claim 1, wherein the post-carbonization treatment temperature is 1600-2200 ℃, and the post-carbonization treatment time is 14-20 h.
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| US5389400A (en) * | 1993-04-07 | 1995-02-14 | Applied Sciences, Inc. | Method for making a diamond/carbon/carbon composite useful as an integral dielectric heat sink |
| CN105110809A (en) * | 2015-08-18 | 2015-12-02 | 河南泛锐复合材料研究院有限公司 | Preparation method for graphene-modified high thermal conductivity three-dimensional carbon/carbon composite material |
| US20180100047A1 (en) * | 2016-10-11 | 2018-04-12 | Palo Alto Research Center Incorporated | Low volatility, high efficiency gas barrier coating for cryo-compressed hydrogen tanks |
| CN108947557A (en) * | 2018-09-25 | 2018-12-07 | 航天特种材料及工艺技术研究所 | A kind of carbon/carbon compound material and preparation method thereof |
| JP2020070197A (en) * | 2018-10-29 | 2020-05-07 | 国立大学法人名古屋大学 | Carbon composite material manufacturing method, composition, heat dissipation component, conductive component, and mobile component |
| CN111362713A (en) * | 2020-03-17 | 2020-07-03 | 吉林联科特种石墨材料有限公司 | Preparation method of asphalt-based carbon fiber felt heat-insulation cylinder |
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- 2022-05-10 CN CN202210505015.8A patent/CN114773079B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5389400A (en) * | 1993-04-07 | 1995-02-14 | Applied Sciences, Inc. | Method for making a diamond/carbon/carbon composite useful as an integral dielectric heat sink |
| CN105110809A (en) * | 2015-08-18 | 2015-12-02 | 河南泛锐复合材料研究院有限公司 | Preparation method for graphene-modified high thermal conductivity three-dimensional carbon/carbon composite material |
| US20180100047A1 (en) * | 2016-10-11 | 2018-04-12 | Palo Alto Research Center Incorporated | Low volatility, high efficiency gas barrier coating for cryo-compressed hydrogen tanks |
| CN108947557A (en) * | 2018-09-25 | 2018-12-07 | 航天特种材料及工艺技术研究所 | A kind of carbon/carbon compound material and preparation method thereof |
| JP2020070197A (en) * | 2018-10-29 | 2020-05-07 | 国立大学法人名古屋大学 | Carbon composite material manufacturing method, composition, heat dissipation component, conductive component, and mobile component |
| CN111362713A (en) * | 2020-03-17 | 2020-07-03 | 吉林联科特种石墨材料有限公司 | Preparation method of asphalt-based carbon fiber felt heat-insulation cylinder |
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