CN104261852A - Preparation method of carbon-carbon composite heat-barrier material - Google Patents

Preparation method of carbon-carbon composite heat-barrier material Download PDF

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Publication number
CN104261852A
CN104261852A CN201410435821.8A CN201410435821A CN104261852A CN 104261852 A CN104261852 A CN 104261852A CN 201410435821 A CN201410435821 A CN 201410435821A CN 104261852 A CN104261852 A CN 104261852A
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CN
China
Prior art keywords
carbon
composite heat
preparation
insulated material
carbon composite
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Pending
Application number
CN201410435821.8A
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Chinese (zh)
Inventor
陈茂斌
唐波
吴新锋
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SHANGHAI DINGXIN INDUSTRIAL Co Ltd
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SHANGHAI DINGXIN INDUSTRIAL Co Ltd
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Priority to CN201410435821.8A priority Critical patent/CN104261852A/en
Publication of CN104261852A publication Critical patent/CN104261852A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248Carbon, e.g. graphite

Abstract

The invention discloses a preparation method of a carbon-carbon composite heat-barrier material. The carbon-carbon composite heat-barrier material is composed of carbon fiber felt and a phenol formaldehyde resin. The method is characterized in that the carbon fiber felt treated with a highly oxidative liquid can obviously enhance the interface binding force between the carbon fibers and phenol formaldehyde resin and enhances the mechanical properties of the heat-barrier material while keeping lower volume density. The carbon-carbon composite heat-barrier material is simple in production technique; and the volume density is 0.16-0.18 g/cm<3>. When the volume density is 0.160g/cm<3>, the mechanical properties are as follows: the compression strength can reach 0.73 MPa (face direction) and 0.4 MPa (two-side direction), and the bending strength can reach 3.52 MPa (face direction) and 1.86 MPa (two-side direction).

Description

A kind of preparation method of carbon carbon composite heat-insulated material
Technical field
The present invention relates to high temperature thermal field field of material technology, be specifically related to a kind of preparation method of carbon carbon composite heat-insulated material, the carbon carbon composite heat-insulated material of preparation can be applied in metal heat treatmet, the sintering of fine ceramics, the generation of various crystallization, optical fiber production, the fields such as the silicon substrate used in solar power system, the sintering of single crystal silicon semiconductor.
Background technology
Carbon fiber is a kind of strongthener grown up after the 1950's, it has high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, conduction and the excellent properties such as thermal expansivity is little, and its matrix material has been widely used in the field such as aerospace, sports equipment.
High-performance carbon fibre composite heat-insulated material, this is a kind of novel high-temperature flame-proof lagging material, and it is by greying and the thermostable heat-isolating material with density gradient obtained again after the anisotropic high-temperature resistant carbon fiber heat insulation felt of a kind of fiber orientation and resol compound.Have lightweight, intensity is high, wear-resistant, high temperature resistant, the characteristic that high connductivity etc. are excellent, mainly be used in high-temperature vacuum equipment, in metal heat treatmet, the sintering of fine ceramics, the generation of various crystallization, optical fiber production, the fields such as the silicon substrate used in solar power system, the sintering of single crystal silicon semiconductor are widely used.
The performance of carbon-fibre composite depends on the performance of body material and the combination degree etc. of fiber and body material.Research shows, carbon fiber before without surface treatment, little (the general < 1m of its specific surface area active 2/ g), surface energy is low, and surface presentation goes out lyophobicity.Fiber strength is exactly chemically reactive in order to fortifying fibre surface and physical activity, thus the combination increased between itself and matrix or bonding.At present, in fiber-reinforced resin matrix compound material, to Fiber strength with the close-burning research of reinforced composite, mainly contain the methods such as air oxidation process, liquid phase oxidation, plasma oxidation method and electrochemical oxidation process.
Summary of the invention
The object of the invention is, by carrying out surface treatment to carbon fiber, to improve carbon fiber and resin-bonded property, the density of lagging material can be made to be reduced to 0.16g/cm 3while, keep higher ultimate compression strength (20-30 MPa), and production technique is simple.The technical solution used in the present invention is as described below:
Carbon fiber flexible felt is put into the treating pond filling Strong oxdiative liquid, soak 30-120 minute, take out and carry out washing and drying; After resol and ethanol are mixed in proportion, enter in carbon fiber flexible felt by glue-spraying machine compound, press curing at 200 DEG C, greying at 2000 DEG C, carbon carbon composite heat-insulated material.
Carbon fiber flexible felt of the present invention is the nonwoven that carbon fiber weaving becomes, and thickness is 5-15mm, volume density 0.1g/cm 3.
Strong oxdiative liquid of the present invention is the one in nitric acid, acid potassium bichromate, clorox.
Resin of the present invention is resol, and viscosity is 800-1500mPas, solid content >=65%, and carbon yield >=35%, as PFn-5300M.
Condition of cure of the present invention is, solidifying pressure is 20 tons, and temperature is 200 DEG C.
Greying condition of the present invention is, temperature is 2000 DEG C.
Embodiment
Provide preferred embodiment of the present invention below, these embodiments unrestricted content of the present invention.
embodiment 1
Get carbon fiber flexible felt 10 pieces, long 1550mm, wide 1550mm, thick 5mm, put into the treating pond filling concentrated nitric acid, the concentration of concentrated nitric acid is 65%, processes 60 minutes, takes out use water and rinses, dry in an oven; Get resol 20kg, dehydrated alcohol 20kg, stirs; Every layer of carbon fiber flexible felt sprays into the resol ethanolic soln that 4kg configures, and after drying, successively stacks, suppresses in press, fixed high 47mm, pressure 20 tons, and temperature 200 DEG C, is incubated 2 hours; Taking-up gained solidification felt is put into High Temperature Furnaces Heating Apparatus and is carried out greying, temperature 2000 DEG C, 72 hours time, obtains carbon carbon composite heat-insulated material, volume density 0.160g/cm 3, ultimate compression strength 0.73MPa (direction, face), direction, 0.4MPa(both sides), flexural strength is 3.52MPa (direction, face), direction, 1.86MPa(both sides).
embodiment 2
Get carbon fiber flexible felt 10 pieces, long 1550mm, wide 1550mm, thick 5mm, put into the treating pond filling clorox, the concentration of clorox is 70%, processes 60 minutes, takes out use water and rinses, dry in an oven; Get resol 20kg, dehydrated alcohol 20kg, stirs; Every layer of carbon fiber flexible felt sprays into the resol ethanolic soln that 4kg configures, and after drying, successively stacks, suppresses in press, fixed high 47mm, pressure 20 tons, and temperature 200 DEG C, is incubated 2 hours; Taking-up gained solidification felt is put into High Temperature Furnaces Heating Apparatus and is carried out greying, temperature 2000 DEG C, 72 hours time, obtains carbon carbon composite heat-insulated material, volume density 0.165g/cm 3, ultimate compression strength 0.75MPa (direction, face), direction, 0.42MPa(both sides), flexural strength is 3.6MPa (direction, face), direction, 1.87MPa(both sides).
embodiment 3
Get carbon fiber flexible felt 10 pieces, long 1550mm, wide 1550mm, thick 5mm, put into the treating pond filling acid potassium bichromate, the concentration of potassium bichromate is 50%, processes 60 minutes, takes out use water and rinses, dry in an oven; Get resol 20kg, dehydrated alcohol 20kg, stirs; Every layer of carbon fiber flexible felt sprays into the resol ethanolic soln that 4kg configures, and after drying, successively stacks, suppresses in press, fixed high 47mm, pressure 20 tons, and temperature 200 DEG C, is incubated 2 hours; Taking-up gained solidification felt is put into High Temperature Furnaces Heating Apparatus and is carried out greying, temperature 2000 DEG C, 72 hours time, obtains carbon carbon composite heat-insulated material, volume density 0.177g/cm 3, ultimate compression strength 0.78MPa (direction, face), direction, 0.45MPa(both sides), flexural strength is 3.8MPa (direction, face), direction, 1.95MPa(both sides).

Claims (7)

1. a preparation method for carbon carbon composite heat-insulated material, is characterized in that carbon carbon composite heat-insulated material adopts carbon fiber flexible felt to bond with resin after the process of Strong oxdiative liquid again, obtains carbon carbon composite heat-insulated material after overcuring and greying.
2. the preparation method of carbon carbon composite heat-insulated material according to claim 1, is characterized in that, carbon fiber flexible felt is the nonwoven that carbon fiber weaving becomes, and thickness is 5-15mm, volume density 0.1g/cm3.
3. the preparation method of carbon carbon composite heat-insulated material according to claim 1, is characterized in that, Strong oxdiative liquid is the one in nitric acid, acid potassium bichromate, clorox.
4. the preparation method of carbon carbon composite heat-insulated material according to claim 1, is characterized in that, resin is resol, and viscosity is 800-1500mPas, solid content >=65%, and carbon yield >=35%, as PFn-5300M.
5. the preparation method of carbon carbon composite heat-insulated material according to claim 1, is characterized in that, solidifying pressure is 20 tons, and temperature is 200 DEG C.
6. the preparation method of carbon carbon composite heat-insulated material according to claim 1, is characterized in that, graphitization temperature is 2000 DEG C.
7. the preparation method of carbon carbon composite heat-insulated material according to claim 1, is characterized by, above-mentioned carbon fiber flexible felt is put into the treating pond filling Strong oxdiative liquid, soaks 30-120 minute, takes out and carries out washing and drying; After resol and ethanol are mixed in proportion, enter in carbon fiber flexible felt by glue-spraying machine compound, press curing at 200 DEG C, greying at 2000 DEG C, carbon carbon composite heat-insulated material, material can become the device of different shape through Vehicle Processing.
CN201410435821.8A 2014-09-01 2014-09-01 Preparation method of carbon-carbon composite heat-barrier material Pending CN104261852A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108203307A (en) * 2016-12-20 2018-06-26 甘肃康博丝特新材料有限责任公司 A kind of preparation method of carbon/carbon compound heat-insulation sheet forming
CN111424421A (en) * 2020-05-08 2020-07-17 杭州幄肯新材料科技有限公司 Carbon fiber composite felt and method for enhancing heat conduction and electric conduction performance of polymer composite material
CN112481817A (en) * 2020-11-27 2021-03-12 中宝(西安)科技集团有限公司 Carbon fiber heat insulation material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002255664A (en) * 2001-03-05 2002-09-11 Tokai Carbon Co Ltd C/c composite material and production method therefor
CN101880174A (en) * 2010-05-28 2010-11-10 上海麦戈士科贸有限公司 Carbon/carbon composite density gradient thermal-insulation material
CN102531658A (en) * 2010-12-17 2012-07-04 湖南海鑫新材料股份有限公司 Preparation method of hard composite carbon fiber heat insulation material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002255664A (en) * 2001-03-05 2002-09-11 Tokai Carbon Co Ltd C/c composite material and production method therefor
CN101880174A (en) * 2010-05-28 2010-11-10 上海麦戈士科贸有限公司 Carbon/carbon composite density gradient thermal-insulation material
CN102531658A (en) * 2010-12-17 2012-07-04 湖南海鑫新材料股份有限公司 Preparation method of hard composite carbon fiber heat insulation material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李劲 等: "碳纤维单丝带对酚醛树脂基复合材料力学性能的增强作用", 《复合材料学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108203307A (en) * 2016-12-20 2018-06-26 甘肃康博丝特新材料有限责任公司 A kind of preparation method of carbon/carbon compound heat-insulation sheet forming
CN111424421A (en) * 2020-05-08 2020-07-17 杭州幄肯新材料科技有限公司 Carbon fiber composite felt and method for enhancing heat conduction and electric conduction performance of polymer composite material
CN111424421B (en) * 2020-05-08 2022-07-22 杭州幄肯新材料科技有限公司 Carbon fiber composite felt and method for enhancing heat conduction and electric conduction performance of polymer composite material
CN112481817A (en) * 2020-11-27 2021-03-12 中宝(西安)科技集团有限公司 Carbon fiber heat insulation material and preparation method thereof

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Application publication date: 20150107