CN114920573A - Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material - Google Patents

Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material Download PDF

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CN114920573A
CN114920573A CN202210628302.8A CN202210628302A CN114920573A CN 114920573 A CN114920573 A CN 114920573A CN 202210628302 A CN202210628302 A CN 202210628302A CN 114920573 A CN114920573 A CN 114920573A
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carbon fiber
hard carbon
asphalt
thermal insulation
coating process
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陈晓庆
么伟
陈钢
金成琦
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Jilin Lianke Special Graphite Material Co ltd
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    • C04B35/71Ceramic products containing macroscopic reinforcing agents
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    • C04B35/524Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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Abstract

The invention relates to a one-time coating process sintering method for a pitch-based hard carbon fiber thermal insulation material, which belongs to the technical field of thermal insulation materials and comprises the following steps: preparing a substrate, preparing a pretreatment material, using the pretreatment material, preparing a coating material, and using the coating material. The method optimizes the coating process, reduces 10% of cost on the basis of the original process, enlarges 30% of capacity, has the following states of secondary coating and primary coating products, has basically similar coating effect, and does not influence the coating effect after optimizing the coating process; the problems of low utilization rate of the high-temperature furnace, low capacity and high cost in the hard carbon fiber heat-insulating material are solved, and the market demand on the hard carbon fiber heat-insulating material is met.

Description

Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material
Technical Field
The invention relates to the technical field of heat insulation materials, in particular to a one-time coating process sintering method for a pitch-based hard carbon fiber heat insulation material.
Background
The hard carbon fiber thermal insulation material is a main consumable material for producing and manufacturing monocrystalline silicon in the photovoltaic industry, and has the characteristics of small density, small heat conductivity coefficient, high carbon content and the like.
The sintering furnace used for manufacturing the hard carbon fibers is a cuboid vacuum sintering furnace with fixed size, the charging amount of products in the vacuum sintering furnace is reduced along with the increase of the size of manufactured products, the productivity is reduced, the cost is increased, and new cost requirements of customers cannot be met if the traditional process is used.
The surface of a hard carbon fiber product is very easy to be corroded in a single crystal furnace, so that the production process mainly comprises two coating processes, the functions of the coating processes are respectively used for filling a substrate and polishing and encrypting, carbonization treatment is needed after the two coatings, the process occupies the largest proportion of a high-temperature furnace in the production process, the performance of the hard carbon fiber heat-insulating material is not influenced, and the production cost is reduced.
Disclosure of Invention
The invention aims to provide a one-time coating process sintering method for an asphalt-based hard carbon fiber thermal insulation material, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a one-time coating process sintering method for an asphalt-based hard carbon fiber thermal insulation material comprises the following steps:
preparing a matrix: processing a carbon fiber soft felt, then winding the carbon fiber soft felt on a forming die, sequentially performing curing treatment and carbonization treatment to obtain a hard carbon fiber heat-insulating material blank, and mechanically processing the hard carbon fiber heat-insulating material blank to obtain a matrix workpiece;
preparing a pretreatment material;
using a pretreatment charge: uniformly brushing the pretreatment material on the surface of a substrate workpiece, curing, and leveling;
preparing a coating material;
using a coating material: and uniformly coating the coating material on the surface of the leveled substrate workpiece, then polishing, and then performing post-curing treatment and post-carbonization treatment.
As a further technical scheme of the invention, when the matrix is prepared, the carbon fiber soft felt is an asphalt-based soft felt, the filament diameter of the asphalt-based soft felt is 12-18 mu m, and the density is 0.125g/cm 3 And treating by dipping or spraying an adhesive.
As a further technical scheme of the invention, when the matrix is prepared, the curing treatment is carried out for 6-9h at 160-180 ℃; the carbonization treatment is carried out at 1600-2000 ℃ for 14-20 h.
As a further technical scheme of the invention, the pretreatment material comprises the following raw materials in parts by weight: 80-90 parts of epoxy resin, 8-9 parts of curing agent, 1-3 parts of fiber and 3-5 parts of graphite filler; the preparation method comprises mixing the raw materials, and stirring under vacuum.
As a further technical scheme of the invention, the epoxy resin is a water-based epoxy resin with the model number of CYDW-125; the curing agent is CYDHD-2321; the fiber is asphalt-based short fiber, and the length of the fiber is one or more of 0.5mm, 0.8mm, 1mm and 1.5 mm; the graphite filler is at least one of spherical graphite powder or graphene with a flaky structure; the vacuum stirring is carried out at a vacuum degree of-1 MPa at 3000r/min for 10-15 min.
As a still further technical scheme of the invention, when the pretreatment material is used, the coating amount of the pretreatment material is 0.15-0.4kg, more preferably 0.25kg, per 1kg of the base workpiece; the curing treatment is carried out at 80-140 ℃ for 2-5 h.
As a further technical scheme of the invention, the coating material comprises the following raw materials in parts by weight: 15-40 parts of phenolic resin, 35-55 parts of solvent, 8-15 parts of graphite filler, 5-10 parts of fiber, 0.5-1 part of suspending agent and 0.5-1 part of surface leveling auxiliary agent; the preparation method comprises mixing the raw materials, and stirring with high speed shearing emulsifying machine.
As a further technical solution of the present invention, the phenolic resin is EXP 0371; the solvent is ethanol; the fiber is asphalt-based short fiber, and the length of the fiber is one or more of 0.5mm, 0.8mm, 1mm and 1.5 mm; the graphite filler is at least one of spherical graphite powder or graphene with a flaky structure; the suspending agent is carbon black; the surface leveling auxiliary agent is modified polyacrylic acid.
As a still further technical scheme of the invention, the post-curing treatment is treatment at 160-180 ℃ for 4-6 h.
As a further technical scheme of the invention, the post-carbonization treatment is carried out at 1600-2200 ℃ for 14-20 h.
Compared with the prior art, the invention has the beneficial effects that: the coating process is optimized, the cost is reduced by 10% on the basis of the original process, the productivity is expanded by 30%, the secondary coating and the primary coating are in the following states, the coating effect is basically similar, and the coating effect is not influenced after the coating process is optimized; the problems of low utilization rate of the high-temperature furnace, low capacity and high cost in the hard carbon fiber heat-insulating material are solved, and the market demand on the hard carbon fiber heat-insulating material is met.
Drawings
FIG. 1 is a graph showing the coating densification of the primary coating in example 1;
fig. 2 is a graph showing the coating denseness test of the conventional secondary coating in comparative example 1.
Detailed Description
Example 1
A one-time coating process sintering method for a pitch-based hard carbon fiber thermal insulation material is characterized by comprising the following steps:
preparing a matrix: impregnating or spraying epoxy resin adhesive on asphalt-based soft felt (the diameter of asphalt-based filament is 12 mu m, and the density is 0.125 g/cm) 3 ) Treating, winding on a forming mould, and sequentially curing at 160 deg.C and carbonizingRegulating for 9 h; the carbonization treatment is carried out for 20 hours at 1600 ℃ to obtain a hard carbon fiber heat-insulating material blank, and the hard carbon fiber heat-insulating material blank is mechanically processed to obtain a matrix workpiece;
preparing a pretreatment material: weighing 80kg of waterborne epoxy resin with the model number of CYDW-125, 1kg of curing agent CYDHD-23218 kg of asphalt-based short fiber (the length is 0.5mm) and 3kg of spherical graphite powder; mixing the above raw materials, and stirring at 3000r/min for 10min under vacuum degree of-1 MPa;
using a pretreatment material: uniformly brushing the pretreatment material on the surface of a substrate workpiece, treating at 80 ℃ for 5 hours, and then polishing and flattening the surface of the product by using an electric polisher;
preparing a coating material: weighing 15kg of phenolic resin with the model number of EXP0371, 35kg of ethanol, 8kg of spherical graphite powder, 5kg of asphalt-based short fiber (with the length of 0.8mm), 0.5kg of carbon black and 0.5kg of modified polyacrylic acid; mixing the above raw materials, and processing with high speed shearing emulsifying machine at 8500rpm for 30min to obtain the final product;
using a coating material: and uniformly brushing the coating material on the surface of the leveled substrate workpiece, polishing and leveling the surface of the product by using an electric polisher, treating at 160 ℃ for 6 hours, and treating at 1600 ℃ for 20 hours.
Example 2
A one-time coating process sintering method for an asphalt-based hard carbon fiber thermal insulation material is characterized by comprising the following steps:
preparing a matrix: impregnating or spraying phenolic resin adhesive on asphalt-based soft felt (the diameter of asphalt-based filament is 15 mu m, and the density is 0.125 g/cm) 3 ) Treating, winding the obtained product on a forming die, and sequentially carrying out curing treatment and carbonization treatment, wherein the curing treatment is treatment at 180 ℃ for 8 hours; the carbonization treatment is carried out for 17 hours at 1800 ℃ to obtain a hard carbon fiber heat-insulating material blank, and the hard carbon fiber heat-insulating material blank is mechanically processed to obtain a matrix workpiece;
preparing a pretreatment material: weighing 85kg of waterborne epoxy resin with the model number of CYDW-125, 2kg of curing agent CYDHD-23218.5 kg of asphalt-based short fibers (two of which the lengths are 0.5mm and 1.5mm are mixed according to the mass ratio of 1: 1) and 4kg of sheet-structure graphene; mixing the above raw materials, and stirring at 3000r/min for 13min under vacuum degree of-1 MPa;
using a pretreatment charge: uniformly brushing the pretreatment material on the surface of a substrate workpiece, treating at 110 ℃ for 3.5h, and then polishing and flattening the surface of the product by using an electric polisher;
preparing a coating material: weighing 30kg of phenolic resin with the model of EXP0371, 45kg of ethanol, 12kg of graphene with a sheet structure, 8kg of asphalt-based short fibers (three of which the lengths are 0.5mm, 0.8mm and 1.5mm are mixed according to the mass ratio of 1:1: 2), 0.8kg of carbon black and 0.7kg of modified polyacrylic acid; mixing the above raw materials, and processing with high speed shearing emulsifying machine at 12000rpm for 25min to obtain the final product;
using a coating material: and uniformly brushing the coating material on the surface of the flattened base workpiece, then using an electric sander to polish and flatten the surface of the product, treating at 170 ℃ for 5 hours, and then treating at 1900 ℃ for 17 hours.
Example 3
A one-time coating process sintering method for a pitch-based hard carbon fiber thermal insulation material is characterized by comprising the following steps:
preparing a matrix: impregnating or spraying epoxy resin adhesive on asphalt-based soft felt (the diameter of asphalt-based filament is 18 mu m, and the density is 0.125 g/cm) 3 ) Treating, winding the obtained product on a forming die, and sequentially carrying out curing treatment and carbonization treatment, wherein the curing treatment is treatment at 180 ℃ for 6 hours; the carbonization treatment is carried out for 14 hours at 2000 ℃, so as to obtain a hard carbon fiber heat-insulating material blank, and the hard carbon fiber heat-insulating material blank is mechanically processed, so as to obtain a matrix workpiece;
preparing a pretreatment material: weighing 90kg of waterborne epoxy resin with the model number of CYDW-125, 90kg of curing agent CYDHD-23219 kg, 3kg of asphalt-based short fiber (obtained by mixing four materials with the lengths of 0.5mm, 0.8mm, 1mm and 1.5mm according to the weight ratio of 1:1:1: 1), 2.5kg of spherical graphite powder and 2.5kg of graphene with a sheet structure; mixing the above raw materials, and stirring at 3000r/min for 15min under vacuum degree of-1 MPa;
using a pretreatment charge: uniformly coating the pretreatment material on the surface of a substrate workpiece, treating for 2 hours at 140 ℃, and then polishing and flattening the surface of the product by using an electric polisher;
preparing a coating material: weighing 40kg of phenolic resin with the model number of EXP0371, 55kg of ethanol, 10kg of spherical graphite powder, 5kg of graphene with a sheet structure, 10kg of asphalt-based short fibers (four types of fibers with the lengths of 0.5mm, 0.8mm, 1mm and 1.5mm are mixed according to the weight ratio of 1:1:1: 1), 1kg of carbon black and 1kg of modified polyacrylic acid; mixing the above raw materials, and processing at 15000rpm for 20min by high speed shearing emulsifying machine to obtain the final product;
using a coating material: and uniformly coating the coating material on the surface of the leveled substrate workpiece, then polishing and leveling the surface of the product by using an electric polisher, treating at 180 ℃ for 4h, and treating at 2200 ℃ for 14 h.
Comparative example 1
The hard carbon fiber thermal insulation material prepared by the existing two-time coating process is taken as a comparative example 1, and the specific preparation method comprises the following steps:
preparing a matrix: impregnating or spraying epoxy resin adhesive on asphalt-based soft felt (the diameter of asphalt-based filament is 12 mu m, and the density is 0.125 g/cm) 3 ) Treating, winding the obtained product on a forming die, and sequentially carrying out curing treatment and carbonization treatment, wherein the curing treatment is treatment at 160 ℃ for 9 hours; the carbonization treatment is carried out for 20 hours at 1600 ℃ to obtain a hard carbon fiber heat-insulating material blank, and the hard carbon fiber heat-insulating material blank is mechanically processed to obtain a matrix workpiece;
sequentially carrying out conventional primary coating and secondary coating on a machined part; carrying out post-curing treatment and post-carbonization treatment in sequence after the conventional primary coating and the conventional secondary coating;
the primary coating comprises the following raw materials by weight: 3.5kg of phenolic resin, 1kg of 500-mesh graphite powder, 0.75kg of 1000-mesh sic powder and 6kg of ethanol, and the raw materials are mixed during preparation and stirred for 30min under the condition of 20000 rpm;
primary coating: uniformly brushing the primary coating on the surface of a substrate workpiece, treating for 6 hours at 160 ℃, and then treating for 18 hours at 1600 ℃;
the secondary coating comprises the following raw materials by weight: 3kg of phenolic resin, 0.8kg of graphite powder with 300 meshes, 0.75kg of sic powder with 500 meshes, 0.5kg of short fiber with 1mm and 5kg of ethanol, and the raw materials are mixed during preparation and stirred for 30min under the condition of 20000 rpm;
secondary coating material: and uniformly brushing the secondary coating material on the leveled surface of the substrate machined part, polishing and leveling the surface of the product by using an electric polisher, treating for 6 hours at 160 ℃, and treating for 20 hours at 1600 ℃.
Examples of the experiments
And (3) detecting the compactness of the coating: the coatings used in example 1 and comparative example 1 were tested for coating densification and the results are shown in detail in fig. 1 and 2, where it can be seen that the densification was substantially similar for both processes.
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 one-time coating process sintering method for a pitch-based hard carbon fiber thermal insulation material is characterized by comprising the following steps:
preparing a matrix: processing a carbon fiber soft felt, then winding the carbon fiber soft felt on a forming die, sequentially carrying out curing treatment and carbonization treatment to obtain a hard carbon fiber heat-insulating material blank, and mechanically processing the hard carbon fiber heat-insulating material blank to obtain a matrix machined part;
preparing a pretreatment material;
using a pretreatment material: uniformly brushing the pretreatment material on the surface of a substrate workpiece, curing, and leveling;
preparing a coating material;
using a coating material: and uniformly coating the coating material on the surface of the leveled substrate workpiece, then polishing, and then performing post-curing treatment and post-carbonization treatment.
2. The sintering method of one-step coating process for asphalt-based hard carbon fiber thermal insulation material according to claim 1, wherein during the preparation of the matrix, the carbon fiber soft felt is asphalt-based soft felt, the filament diameter of the asphalt-based soft felt is 12-18 μm, and the density is 0.125g/cm 3 And treating by dipping or spraying an adhesive.
3. The pitch-based hard carbon fiber thermal insulation material one-time coating process sintering method as claimed in claim 2, wherein the curing treatment is treatment at 160-180 ℃ for 6-9h during the preparation of the matrix; the carbonization treatment is carried out for 14-20h at 1600-2000 ℃.
4. The pitch-based hard carbon fiber thermal insulation material one-time coating process sintering method as claimed in claim 1, wherein the pretreatment material comprises the following raw materials in parts by weight: 80-90 parts of epoxy resin, 8-9 parts of curing agent, 1-3 parts of fiber and 3-5 parts of graphite filler; the preparation method comprises mixing the raw materials, and stirring under vacuum.
5. The primary coating process sintering method of the asphalt-based hard carbon fiber thermal insulation material as claimed in claim 4, wherein the epoxy resin is a water-based epoxy resin with a model number of CYDW-125; the model of the curing agent is CYDHD-2321; the fiber is asphalt-based short fiber, and the length of the fiber is one or more of 0.5mm, 0.8mm, 1mm and 1.5 mm; the graphite filler is at least one of spherical graphite powder or graphene with a sheet structure; the vacuum stirring is carried out at 3000r/min for 10-15min under the vacuum degree of-1 MPa.
6. The pitch-based hard carbon fiber thermal insulation material one-coating process sintering method as claimed in claim 1, wherein the application amount of the pretreatment material is 0.15-0.4kg, more preferably 0.25kg, per 1kg of the substrate workpiece when the pretreatment material is used; the curing treatment is carried out at 80-140 ℃ for 2-5 h.
7. The sintering method of the primary coating process of the asphalt-based hard carbon fiber thermal insulation material as claimed in claim 1, wherein the coating material comprises the following raw materials in parts by weight: 15-40 parts of phenolic resin, 35-55 parts of solvent, 8-15 parts of graphite filler, 5-10 parts of fiber, 0.5-1 part of suspending agent and 0.5-1 part of surface leveling auxiliary agent; the preparation method comprises mixing the raw materials, and stirring with a high-speed shearing emulsifying machine.
8. The primary coating process sintering method of the asphalt-based hard carbon fiber thermal insulation material as claimed in claim 7, wherein the type of the phenolic resin is EXP 0371; the solvent is ethanol; the fiber is asphalt-based short fiber, and the length of the fiber is one or more of 0.5mm, 0.8mm, 1mm and 1.5 mm; the graphite filler is at least one of spherical graphite powder or graphene with a sheet structure; the suspending agent is carbon black; the surface leveling auxiliary agent is modified polyacrylic acid; the high-speed shearing emulsifying machine is used for treating for 20-30min at 8500-15000 rpm.
9. The sintering method of asphalt-based hard carbon fiber thermal insulation material with one-step coating process as claimed in claim 1, wherein the post-curing treatment is treatment at 160-180 ℃ for 4-6 h.
10. The sintering method of the primary coating process of the asphalt-based hard carbon fiber thermal insulation material as claimed in claim 1, wherein the post-carbonization treatment is carried out at 1600-.
CN202210628302.8A 2022-06-06 2022-06-06 Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material Pending CN114920573A (en)

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Application publication date: 20220819