CN104276835A - Preparation method of carbon/carbon composite thermal insulation material containing anti-oxidization coating - Google Patents
Preparation method of carbon/carbon composite thermal insulation material containing anti-oxidization coating Download PDFInfo
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- CN104276835A CN104276835A CN201410435822.2A CN201410435822A CN104276835A CN 104276835 A CN104276835 A CN 104276835A CN 201410435822 A CN201410435822 A CN 201410435822A CN 104276835 A CN104276835 A CN 104276835A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Abstract
The invention relates to a preparation method of a carbon/carbon composite thermal insulation material containing an anti-oxidization coating. The method mainly comprises the following steps: mixing soluble thermosetting phenolic resin with ethanol evenly to form an impregnant; spraying the impregnant on the surface of a carbonization felt, and then carrying out hot press molding; mixing SiC powder, thermosetting resin and ethanol evenly at a certain ratio, coating the surface of a hot press plate, putting the hot press plate into a graphitization furnace and graphitizing; and cooling to form the carbon/carbon composite thermal insulation material with a ceramic-coated surface. According to the preparation method, the problem that the carbon/carbon composite thermal insulation material is easily oxidized in the use procedure or the production process is solved, and the service life of the carbon/carbon composite thermal insulation material is greatly prolonged. In addition, the preparation method is synchronous with the preparation process of the carbon/carbon composite thermal insulation material, and is simple and feasible.
Description
Technical field
The invention belongs to carbon/carbon composite heat-insulated material technical field; relate in particular to carbon/carbon compound heat-insulation formed material that a kind of surface-coated has inoxidzable coating; be directly be used in the High Temperature Furnaces Heating Apparatus of vacuum and protection of inert gas, be especially used in polycrystalline silicon ingot or purifying furnace and monocrystal silicon straight pull furnace.
Background technology
Carbon/carbon composite heat-insulated material is a kind of novel high-performance structure, there is the features such as high-strength and high-modulus, heat insulation excellence and low density, be used widely in aerospace, communication optical fiber, new forms of energy, high-performance ceramic manufacture, field of crystal growth, especially the development of new forms of energy photovoltaic industry, the lagging material of polycrystalline ingot furnace and thermal field of single crystal furnace is extensively concerned again becomes a focus.Current carbon/carbon compound heat-insulation formed material be inner, top layer density is homogeneous, top layer does not have densification, makes heat-proof quality, powder amount and work-ing life all undesirable.Graphite paper or carbon cloth are pasted in the many employings of existing surface treatment method, although can solve the problem of easy dry linting, all do not play good improvement result for the carbon volatilization under hot conditions and oxidation.
Summary of the invention
Main purpose of the present invention is the preparation method of the carbon/carbon compound insulating material providing a kind of surface-coated to have inoxidzable coating, and the method is simple.The invention is characterized in and adopt SiC to be the matrix of inoxidzable coating, can not pollution be produced for silicon wafer production process, avoid the existence of source of pollution, improve quality and the production efficiency of product.
The present invention's felt used is Polyacrylonitrile carbon fiber felt, and inoxidzable coating is SiC, and for reaching above-mentioned purpose, the face of the present invention proposes is coated with the preparation method of the carbon/carbon compound insulating material of inoxidzable coating, and the step mainly comprised is as follows:
(1) heat-reactive phenolic resin and alcohol are mixed with the ratio of 1:1, for subsequent use as colloid.
(2) in colloid and Polyacrylonitrile carbon fiber felt with the ratio of 3:1, by colloid even application on felt; During spraying colloid, by the two sides being sprayed on felt of colloid aliquot; Felt after spraying is good dries naturally in ventilation, for subsequent use.
(3) by the thermofixation sizing in thermocompressor of felt in step (2), hard felt is become for subsequent use.
(4) SiC, resol and the alcohol ratio in 1:0.5:0.5 mixed, be coated on hot-forming carbon fiber felt surface, the thickness of coating is no more than 1mm.
(5) coated carbon fiber felt is put into graphitizing furnace and carry out high temperature process, graphitization temperature is 2400 DEG C, obtains carbon/carbon compound insulating material that final surface has antioxidation coating.
(6) in step (5), graphitizing furnace is homemade nonstandard stove, and temperature can reach 2000 more and spend.
Current carbon/carbon compound insulating material is all that the post-treatment method adopted carrys out surface treatment, such as paste graphite paper or carbon cloth etc., although can reduce the powder amount of lagging material like this, the problem easily oxidized for lagging material does not well solve, but the present invention well solves this problem.The preparation method of the carbon/carbon lagging material containing inoxidzable coating that the present invention proposes, not only can solve the problem of oxidation of lagging material preparation process, but also lagging material problem of oxidation in use can be solved, simultaneously to stoping the problem of dry linting in lagging material use procedure also to serve certain effect, be conducive to the work-ing life increasing lagging material, production process can not be increased, be synchronized with the preparation process of carbon/carbon lagging material, and pollution can not be produced to fabricated product, improve production of articles efficiency, reduce production of articles cost.
Accompanying drawing explanation
Accompanying drawing 1 total technological process figure
Accompanying drawing 2 is containing inoxidzable coating lagging material schematic diagram
Nomenclature
In accompanying drawing 2:
1-SiC coating
2-carbon/carbon lagging material sheet material.
Embodiment
The embodiment of the present invention proposes a kind of method that good preparation contains the carbon/carbon lagging material of inoxidzable coating, which increases the use properties of lagging material, mainly comprise for:
(1) cut out: some pieces, the soft felt of polyacrylonitrile carbon fiber cutting out desired size, as the idiosome preparing lagging material.
(2) glue: by solubility heat-reactive phenolic resin and content be 99% analytical pure alcohol be the ratio of 1:1 according to weight ratio, mixing and stirring, for subsequent use.
(3) spraying dipping: carry out spraying dipping than the ratio for 1:3 according to felt and gel weight.By colloid in (2) with the two sides of the method for the mechanical spraying formula proportionally even spraying of equivalent every sheet felt in (1), be then placed in ventilation, alcohol is volatilized naturally.
(4) hot-forming: to complete separate-type paper at mold bottom, evenly completed by the felt lamination in (3), separate-type paper is also completed in top, and mould pressurizing intensification is carried out hot-forming.Technique time hot-forming is: pressure 0.625Kg/cm2, goes straight up to for 0 ~ 90 DEG C, and 90 ~ 140 DEG C heat up with 30 DEG C/h, and 140 DEG C of insulation 1h, go straight up to for 140 ~ 165 DEG C, and 165 DEG C of insulation 3h, Temperature fall is come out of the stove to room temperature.
(5) apply: SiC, resol and the alcohol ratio in 1:0.5:0.5 mixed, be coated on hot-forming carbon fiber felt surface, the thickness of coating is no more than 1mm.
(6) high temperature sintering: under nitrogen/other protection of inert gas, under 10 ~ 8000Pa pressure, be warmed up to 400 DEG C with 75 DEG C/h, then 25 DEG C/h is warmed up to 500 DEG C, 500 DEG C of insulations 2 hours, this sinks carbon process for liquid phase.Then be graphitizing process, main process is, is warmed up to 600 DEG C from 500 DEG C with 25 DEG C/h, be warmed up to 750 DEG C with 30 DEG C/h, 750 DEG C of constant temperature 2 hours, be then warmed up to 950 DEG C with 40 DEG C/h, 50 DEG C/h is warmed up to 1200 DEG C, 55 DEG C/h is warmed up to 1500 DEG C, and 60 DEG C/h is warmed up to 1800 DEG C, and 70 DEG C/h is warmed up to 2000 DEG C, 75 DEG C/h is warmed up to 2200 DEG C, 80 DEG C/h is warmed up to 2400 DEG C, and 2400 DEG C of insulations, after 3 hours, are come out of the stove after last Temperature fall to room temperature.
Claims (6)
1., containing a preparation method for the carbon/carbon compound insulating material of inoxidzable coating, its feature comprises the following steps:
A certain proportion of resin, alcohol are mixed, as colloid;
By a certain percentage colloid is sprayed on carbon fiber felt surface, dries;
By felt laying in (2), put into press, impose a condition lower hot-forming;
SiC powder, resin and alcohol are mixed by a certain percentage, is coated in the surface of hot-forming hard felt;
Felt hard in (4) is put into high temperature graphitization stove and carries out graphitization processing, obtain the carbon/carbon compound insulating material of surface coverage pottery.
2. according to claim 1, resin is heat-reactive phenolic resin, and alcohol is industrial spirit, and the ratio of resin and alcohol is 1:1(weight ratio).
3., according to claim 1, during spraying, the ratio of felt and glue is 1:3(weight ratio), the two sides being sprayed on felt of glue equivalent, under room temperature, ventilation is dried naturally.
4. according to claim 1, technique time hot-forming is: go straight up to for 0 ~ 90 DEG C, and 90 ~ 140 DEG C heat up with 30 DEG C/h, and 140 DEG C of insulation 1h, go straight up to for 140 ~ 165 DEG C, and 165 DEG C of insulation 3h, Temperature fall is come out of the stove to room temperature.
5. according to claim 1, SiC, resol and alcohol mix in the ratio of 1:0.5:0.5, and the thickness of coating is not more than 1mm.
6. according to claim 1, graphitizing process mainly under 10 ~ 8000Pa pressure, 400 DEG C are warmed up to 75 DEG C/h, then 500 DEG C are warmed up to 25 DEG C/h, 500 DEG C are incubated 2 hours, finally reach 2400 DEG C with the temperature rise rate of 25 ~ 100 DEG C/h, 2400 DEG C of insulations stop after 1 hour heating up, and come out of the stove after Temperature fall to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410435822.2A CN104276835A (en) | 2014-09-01 | 2014-09-01 | Preparation method of carbon/carbon composite thermal insulation material containing anti-oxidization coating |
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| CN201410435822.2A CN104276835A (en) | 2014-09-01 | 2014-09-01 | Preparation method of carbon/carbon composite thermal insulation material containing anti-oxidization coating |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106116626A (en) * | 2016-06-27 | 2016-11-16 | 朗铂新材料科技（上海）有限公司 | A kind of preparation method of oxidation resistant carbon carbon composite heat-insulated material |
| CN109505132A (en) * | 2018-12-29 | 2019-03-22 | 湖南九华碳素高科有限公司 | It is a kind of for making the dipping method of carbon fiber hard composite felt |
| CN109824380A (en) * | 2019-03-28 | 2019-05-31 | 山东众途复合材料有限公司 | A kind of preparation method of the carbon fiber thermal insulating material coated with anti-oxidant shock resistance coating |
| CN114907145A (en) * | 2022-06-10 | 2022-08-16 | 辽宁奥亿达新材料有限公司 | Silicon carbide coating adhesive on surface of carbon fiber composite material and preparation and use method thereof |
| CN115028466A (en) * | 2022-06-21 | 2022-09-09 | 上海鼎炘实业有限公司 | Carbon fiber composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948327A (en) * | 2010-08-17 | 2011-01-19 | 西安超码科技有限公司 | Method for preparing work hardening insulation quilt for high temperature furnace |
-
2014
- 2014-09-01 CN CN201410435822.2A patent/CN104276835A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948327A (en) * | 2010-08-17 | 2011-01-19 | 西安超码科技有限公司 | Method for preparing work hardening insulation quilt for high temperature furnace |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106116626A (en) * | 2016-06-27 | 2016-11-16 | 朗铂新材料科技（上海）有限公司 | A kind of preparation method of oxidation resistant carbon carbon composite heat-insulated material |
| CN109505132A (en) * | 2018-12-29 | 2019-03-22 | 湖南九华碳素高科有限公司 | It is a kind of for making the dipping method of carbon fiber hard composite felt |
| CN109824380A (en) * | 2019-03-28 | 2019-05-31 | 山东众途复合材料有限公司 | A kind of preparation method of the carbon fiber thermal insulating material coated with anti-oxidant shock resistance coating |
| 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 |
| CN114907145A (en) * | 2022-06-10 | 2022-08-16 | 辽宁奥亿达新材料有限公司 | Silicon carbide coating adhesive on surface of carbon fiber composite material and preparation and use method thereof |
| CN114907145B (en) * | 2022-06-10 | 2023-03-31 | 辽宁奥亿达新材料有限公司 | Carbon fiber composite material surface silicon carbide coating adhesive and preparation and use method thereof |
| CN115028466A (en) * | 2022-06-21 | 2022-09-09 | 上海鼎炘实业有限公司 | Carbon fiber composite material and preparation method thereof |
| CN115028466B (en) * | 2022-06-21 | 2023-04-18 | 上海鼎炘实业有限公司 | Carbon fiber composite material and preparation method thereof |
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Application publication date: 20150114 |