CN115387131B - Hard carbon fiber felt composite coating and preparation method thereof - Google Patents

Hard carbon fiber felt composite coating and preparation method thereof Download PDF

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Publication number
CN115387131B
CN115387131B CN202210852078.0A CN202210852078A CN115387131B CN 115387131 B CN115387131 B CN 115387131B CN 202210852078 A CN202210852078 A CN 202210852078A CN 115387131 B CN115387131 B CN 115387131B
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graphite powder
carbon fiber
coating material
fiber felt
hard carbon
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CN115387131A (en
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陈荣华
路良
陈新华
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Jiangsu Mige New Material Co ltd
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Jiangsu Mige New Material Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06CFINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00Heating or cooling textile fabrics
    • D06C7/04Carbonising or oxidising
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0011Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0063Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2201/00Chemical constitution of the fibres, threads or yarns
    • D06N2201/08Inorganic fibres
    • D06N2201/087Carbon fibres
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention relates to a hard carbon fiber felt composite coating and a preparation method thereof, which belong to the technical field of carbon fibers, wherein after ethylene glycol and phenolic resin are mixed according to a proportion, graphite powder, colloidal graphite powder and carbon black are sequentially added according to a proportion, and the mixture is uniformly stirred to be used as a primary coating material; mixing glycol, phenolic resin, colloidal graphite powder, graphite powder and short fiber in proportion, and stirring uniformly to obtain the secondary coating material. Compared with the conventional coating, the service life of the hard carbon fiber felt composite coating is 2-3 times that of the conventional coating, the strength of the hard carbon fiber felt composite coating is ensured by short fiber introduction, coarse and fine graphite powder selection and carbon black skeleton reinforcement, the problems of slag and ash falling of the product are solved, and the overflow of impurities in the product is blocked.

Description

Hard carbon fiber felt composite coating and preparation method thereof
Technical Field
The invention belongs to the technical field of carbon fibers, and particularly relates to a hard carbon fiber felt composite coating and a preparation method thereof.
Background
The carbon fiber is used as a fibrous material and has the characteristics of low density, high strength, high modulus, ablation resistance and corrosion resistance, and simultaneously has higher braiding performance; the high-performance carbon fiber is mostly used in the field of aerospace, national defense, military and semiconductor high-end equipment manufacturing industry; the general type carbon fiber is widely applied to the fields of environmental protection, sports, civil industry and photovoltaic semiconductor heat insulation due to the characteristics of higher specific strength, specific modulus, low density, high temperature resistance and the like.
The development of the fields of photovoltaics, wind energy, hydrogen energy and the like is greatly promoted along with the rapid schedule of the new policy adjustment carbon neutralization concept in the country; in the photovoltaic and semiconductor fields, the product preparation process not only requires the furnace body environment to have extremely high cleanliness, but also requires the furnace body heat insulation layer to have high temperature resistance and excellent heat insulation performance; the carbon fiber and the composite material thereof have extremely high purity and good heat insulation performance.
The hard carbon fiber felt is widely used in special thermal fields, especially photovoltaic single crystal and polycrystal thermal fields, due to its excellent high temperature resistance and heat preservation characteristics and high purity. The only disadvantage of the hard carbon fiber felt is that the surface ash and slag are removed due to corrosion of the furnace atmosphere in the long-time use process, so that the product pollution is caused, and the product strength and the service life are greatly reduced; the excellent surface coating not only can prevent the dust, slag and impurities from falling off the hard felt, but also can greatly prolong the service life of the hard felt.
Based on the above, a hard carbon fiber felt composite coating and a preparation method thereof are provided.
Disclosure of Invention
The invention aims to solve the problems that the existing carbon fiber felt surface coating is easy to remove ash and slag, or SiC and Si are deposited on the surface 3 N 4 The method is characterized in that the method solves the problems of low production efficiency and the like caused by long treatment time, and provides a hard carbon fiber felt composite coating and a preparation method thereof.
The invention realizes the above purpose through the following technical scheme:
a preparation method of a hard carbon fiber felt composite coating comprises the following steps:
(1) Mixing ethylene glycol, phenolic resin, graphite powder, colloidal graphite powder and carbon black, and uniformly stirring to obtain a primary coating material; uniformly brushing a primary coating material on the surface of the carbon fiber felt, and performing high-temperature carbonization heat treatment to form a densified matrix on the surface of the carbon fiber felt to obtain a primary coating;
(2) Mixing ethylene glycol, phenolic resin, colloidal graphite powder, graphite powder and short fibers in proportion, and uniformly stirring to obtain a secondary coating material; and (3) polishing and polishing the surface of the primary coating, uniformly brushing a secondary coating material on the surface of the primary coating, and performing high-temperature carbonization and graphitization heat treatment again to form a densification protective film on the surface, thereby obtaining the hard carbon fiber felt composite coating.
Further, the primary coating material in the step (1) comprises the following components in percentage by mass: (2-10): (0.5-1): (0.5-1): (0.05-0.5).
Further, the graphite powder used in the primary coating material comprises graphite powder with the particle size below 200um and graphite powder with the particle size above 200um, and the mass ratio of the graphite powder with the two particle sizes is (0.5-1): (0.5-1).
Further, the secondary coating material in the step (2) comprises the following components in percentage by mass (0.5-1): (0.2-0.7): (3-4): (4-5): (0.5-1).
Further, the particle size of graphite powder used in the secondary coating material is smaller than 200um, and the length of the short fiber is 0.1-5mm.
Further, the stirring in the step (1) or (2) is carried out under vacuum, the vacuum degree is 2000-8000pa, the stirring speed is 10-80r/min, and the stirring time is 10-60min.
Further, the high-temperature carbonization temperature of the primary coating material is 1400-1600 ℃ and the heat treatment time is 2-4h.
Further, the high-temperature carbonization graphitization temperature of the secondary coating material is 2000-2350 ℃ and the heat treatment time is 2-4h.
The invention also provides a hard carbon fiber felt composite coating prepared by the preparation method.
The principle of the invention is as follows: the forming process of the composite coating mainly comprises the steps of adhering a layer of carbon fiber short filaments on the surface of a composite material by taking resin as an adhesive, reinforcing the primary coating by carbon black, taking graphite powder, carbon black and phenolic resin as a matrix, and obtaining primary coverage after high temperature, wherein the phenolic resin has better cohesiveness on the carbon fiber composite material to ensure that the carbon black and the graphite powder cannot fall off; the secondary coating material can effectively ensure the bonding effect through the graphite powder and the short fibers under the bonding of the phenolic resin, and simultaneously, the carbon fibers can be used as a framework to effectively improve the surface adhesion force and the surface strength, so that the surface hardness of the composite material is further improved, and the ash falling phenomenon is prevented.
The invention has the beneficial effects that:
1. compared with the conventional coating, the service life of the composite coating is 2-3 times that of the conventional coating, the strength of the composite coating is ensured by short fiber introduction and coarse and fine graphite powder selection and carbon black skeleton reinforcement, the problems of slag and ash falling of the product are solved, and the overflow of impurities in the product is blocked.
2. The invention has the advantages of simple preparation process and normal temperature operation compared with the deposition coating while achieving the same effect; the preparation time is short, and the preparation process is controllable; the energy consumption is reduced by 80-120% compared with the deposition method.
Drawings
FIG. 1 is a flow chart of the preparation of a hard carbon fiber mat composite coating of the present invention;
FIG. 2 is an electron microscope image of the hard carbon fiber mat composite coating (right) and conventional coating in example 2 of the present invention.
Detailed Description
The following detailed description of the present application is provided to illustrate the present application and should not be construed as limiting the scope of the present application, since numerous insubstantial modifications and adaptations of the present application will be apparent to those skilled in the art from the foregoing disclosure.
1. Material
The methods used in the present invention are conventional methods known to those skilled in the art unless otherwise indicated, and the materials such as reagents used, if otherwise indicated, are commercially available products.
2. Detailed description of the preferred embodiments
2.1 example 1
A. Preparing a primary coating material, and preparing ethylene glycol: phenolic resin: graphite powder: colloidal graphite powder: carbon black was prepared as follows: 5:0.6:0.6: sequentially adding 0.1 parts by mass of the components into a stirring container; stirring for 30min at a stirring speed of 30r/min and a vacuum degree of 3000pa to obtain a homogeneous phase coating material; uniformly coating the surface of the hard carbon fiber felt; carbonizing at high temperature under vacuum environment at 1600 ℃ for 3 hours, and polishing to obtain a primary treated blank;
B. preparing a secondary coating material, namely preparing ethylene glycol: phenolic resin: colloidal graphite powder: graphite powder: staple fiber was prepared at 0.8:0.4:3.2:4.3: sequentially adding the materials with the mass portion ratio of 0.6 into a stirring container, stirring for 30min at the stirring speed of 30r/min and the vacuum degree of 3000pa to obtain a homogeneous phase coating material; uniformly coating the surface of the primary treated blank, carbonizing and graphitizing at high temperature in a vacuum environment, wherein the treatment temperature is 2200 ℃ and the service life of the secondary coating finished product is 2 times that of the conventional primary coating, and the overall energy consumption and the time cost are saved by 85 percent compared with those of a deposition method.
Note that: the conventional coating method is to coat a layer of silicon carbide series liquid material on the surface of the carbon fiber without high temperature heat treatment.
2.2 example 2
A. Preparing a primary coating material, and preparing ethylene glycol: phenolic resin: graphite powder: colloidal graphite powder: carbon black was prepared according to 7.8:5.2:0.65:0.65: sequentially adding 0.12 parts by mass of the components into a stirring container; stirring for 30min at a stirring speed of 30r/min and a vacuum degree of 3000pa to obtain a homogeneous phase coating material; uniformly coating the surface of the hard carbon fiber felt; carbonizing at high temperature under vacuum environment at 1600 ℃ for 3 hours, and polishing to obtain a primary treated blank;
B. preparing a secondary coating material, namely preparing ethylene glycol: phenolic resin: colloidal graphite powder: graphite powder: staple fiber was prepared at 0.75:0.35:3.2:4.4: sequentially adding the components in a mass portion ratio of 0.5 into a stirring container, and stirring for 30min at a stirring speed of 30r/min and a vacuum degree of 3000pa to obtain a homogeneous phase coating material; uniformly coating the surface of the primary treated blank, carbonizing and graphitizing at high temperature in a vacuum environment, wherein the treatment temperature is 2200 ℃ and the service life of the secondary coating finished product is 2.2 times that of the conventional primary coating, and the overall energy consumption and the time cost are saved by 85 percent compared with those of a deposition method.
Note that: the conventional coating method is to coat a layer of silica sol series liquid material on the surface of the carbon fiber without high temperature heat treatment.
2.3 example 3
A. Preparing a primary coating material, and preparing ethylene glycol: phenolic resin: graphite powder: colloidal graphite powder: carbon black was prepared according to 6:6:0.7:0.8: sequentially adding 0.08 mass portion ratio into a stirring container; stirring for 30mi < n >, stirring speed 30r/min and vacuum degree 3000pa to obtain homogeneous phase coating material; uniformly coating the surface of the hard carbon fiber felt; carbonizing at high temperature under vacuum environment at 1600 ℃ for 3 hours, and polishing to obtain a primary treated blank;
B. preparing a secondary coating material, namely preparing ethylene glycol: phenolic resin: colloidal graphite powder: graphite powder: staple fiber was prepared at 0.7:0.6:3.4:4.4: sequentially adding the components in a mass portion ratio of 0.5 into a stirring container, and stirring for 30min at a stirring speed of 30r/min and a vacuum degree of 3000pa to obtain a homogeneous phase coating material; uniformly coating the surface of the primary treated blank, carbonizing and graphitizing at high temperature in a vacuum environment, wherein the treatment temperature is 2200 ℃ and the service life of the secondary coating finished product is 2.2 times that of the conventional primary coating, and the overall energy consumption and the time cost are saved by 85 percent compared with those of a deposition method.
Note that: the conventional coating method is to coat a layer of silicon carbide series liquid material on the surface of the carbon fiber without high temperature heat treatment.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.

Claims (3)

1. The preparation method of the hard carbon fiber felt composite coating is characterized by comprising the following steps of:
(1) Mixing ethylene glycol, phenolic resin, graphite powder, colloidal graphite powder and carbon black, and uniformly stirring to obtain a primary coating material; uniformly brushing a primary coating material on the surface of the carbon fiber felt, and performing high-temperature carbonization heat treatment to form a densified matrix on the surface of the carbon fiber felt to obtain a primary coating;
the primary coating material in the step (1) comprises the following components in percentage by mass: (2-10): (0.5-1): (0.5-1): (0.05-0.5); the graphite powder used in the primary coating material comprises graphite powder with the particle size below 200um and graphite powder with the particle size above 200um, and the mass ratio of the graphite powder with the two particle sizes is (0.5-1): (0.5-1); the high-temperature carbonization temperature of the primary coating material is 1400-1600 ℃ and the heat treatment time is 2-4h;
(2) Mixing ethylene glycol, phenolic resin, colloidal graphite powder, graphite powder and short fibers, and uniformly stirring to obtain a secondary coating material; polishing and polishing the surface of the primary coating, uniformly brushing a secondary coating material on the surface of the primary coating, and forming a densification protective film on the surface through high-temperature carbonization graphitization heat treatment again to obtain a hard carbon fiber felt composite coating;
the secondary coating material in the step (2) comprises the following components in percentage by mass (0.5-1): (0.2-0.7): (3-4): (4-5): (0.5-1); the particle size of graphite powder used in the secondary coating material is smaller than 200um, and the length of the short fiber is 0.1-5mm; the high-temperature carbonization graphitization temperature of the secondary coating material is 2000-2350 ℃ and the heat treatment time is 2-4h.
2. The method for preparing the hard carbon fiber felt composite coating according to claim 1, wherein stirring in the step (1) or (2) is performed under vacuum, wherein the vacuum degree is 2000-8000pa, the stirring speed is 10-80r/min, and the stirring time is 10-60min.
3. A hard carbon fiber mat composite coating, characterized in that the composite coating is made by the preparation method of any one of claims 1-2.
CN202210852078.0A 2022-07-20 2022-07-20 Hard carbon fiber felt composite coating and preparation method thereof Active CN115387131B (en)

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CN115387131B true CN115387131B (en) 2023-07-25

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Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009048422A1 (en) * 2009-10-06 2011-04-07 Sgl Carbon Se Composite of carbon fiber soft felt and carbon fiber hard felt
CN103568385B (en) * 2013-10-18 2015-04-22 四川创越炭材料有限公司 Heat-preservation hard composite carbon fiber felt and preparation method thereof
CN109824380B (en) * 2019-03-28 2021-09-14 山东众途复合材料有限公司 Preparation method of carbon fiber thermal insulation material coated with antioxidant impact-resistant coating
CN111996813A (en) * 2020-08-27 2020-11-27 佛山市石金科技有限公司 Coating of hard felt and preparation method thereof
CN112376267A (en) * 2020-10-19 2021-02-19 安徽弘昌新材料有限公司 Preparation method of cured carbon felt
CN113636853B (en) * 2021-08-30 2022-08-19 江西宁新新材料股份有限公司 Carbon fiber composite brake pad and preparation method thereof

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