CN103274760B - Anti-oxidative coating of charcoal/charcoal composite material and application of anti-oxidative coating - Google Patents
Anti-oxidative coating of charcoal/charcoal composite material and application of anti-oxidative coating Download PDFInfo
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- CN103274760B CN103274760B CN201310183782.2A CN201310183782A CN103274760B CN 103274760 B CN103274760 B CN 103274760B CN 201310183782 A CN201310183782 A CN 201310183782A CN 103274760 B CN103274760 B CN 103274760B
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Abstract
The invention relates to an anti-oxidative coating of a charcoal/charcoal composite material and an application of the anti-oxidative coating. The anti-oxidative coating of the charcoal/charcoal composite material is characterized by comprising the components in percentage by weight: 10-15% of MoSi2, 5-10% of B, 10-15% of B2O3, 10-15% of SiO2, 5-10% of Al2O3, 10-15% of Zn3(PO4)2, 15-20% of H3PO4 and15-20% of H2O. The core technology of the invention is as follows: components such as boride are introduced into molybdenum silicide. When temperature is over 700 DEG C, a symbiotic glass borosilicate anti-oxidative film is compact, airtight and self-healing and is stable to adhere to the surface of the charcoal/charcoal composite material. The higher the temperature is, the more thorough the protective film is formed. The anti-oxidative coating is suitable for long-time work at 400-1000 DEG C. The preparation and coating processes of the anti-oxidative coating are simpler, so that the anti-oxidative coating is suitable for anti-oxidative coatings of various forms of charcoal discs.
Description
Technical field
The present invention relates to a kind of coating, particularly relate to a kind of antioxidizing paint and application thereof of carbon/carbon composite.
Background technology
Carbon/carbon composite is worked as temperature and just oxidizing reaction is occurred higher than 370 DEG C, and temperature will significantly be oxidized more than 450 DEG C, causes the physics of material, chemistry and mechanical property sharply deteriorated.And the moment of aircraft normal landing brake, brake flange surface temperature is up to more than 1000 DEG C, and volume temperature reaches 600 DEG C ~ 800 DEG C, and overload and scram volume temperature can reach 800 DEG C ~ 1000 DEG C.Therefore, the gordian technique ensureing braking safe must be become for heavily loaded braking braking disk with composite carbon/carbon material (calling charcoal dish in the following text) high-temp antioxidizings such as aircrafts.
For many years, external aircraft charcoal dish mainly uses phosphoric acid salt and the large class inoxidzable coating of silicate two.The composition of phosphate coating is comparatively simple, is solvent mainly with water; The composition of silicate coating is more complicated, uses organic binder bond more, and above two type coatings all have good oxidation-protective effect.Describe a kind of by Modified by Rare Earth Chloride borosilicate, boron, boride, SiC, CeS in China Patent No. 9011058.6
2and the aircraft charcoal dish inoxidzable coating of resol composition.Describe a kind of inoxidzable coating for aircraft charcoal dish and coating process thereof in China Patent Publication No. CN1415669A, coating is made up of presoak (boric acid, phosphoric acid and distilled water) and coating (silicon carbide, boron and boride, silica flour etc.).Above two patented technologies improve the resistance of oxidation of charcoal dish all to some extent, but the preparation of its coating and coating process more complicated, its high-temperature oxidation resistance also need improve.A kind of carbon/carbon composite material oxidation-proof coating based on phosphoric acid salt is described in China Patent Publication No. CN1544536A, wherein silicon 10% ~ 15%, boron 10% ~ 15%, phosphoric acid salt 60% ~ 70%, aluminum oxide 5% ~ 10%, although this formula is fairly simple, low temperature and high-temp antioxidizing effect are not too desirable.
In addition, China Patent Publication No. CN100410212C, a kind of carbon/carbon composite material oxidation-proof coating is a kind of compound coating, and main component is Al (OH)
3, Zn
3(PO
4)
24H
2o, Na
2b
4o
710H
2o, SiO
2, B etc., the carbon/carbon composite material oxidation-proof coating obtained after twice process, has good antioxidant effect, and the feature of environmental protection is good.This kind of compound coating needs brushing twice, thermal treatment twice, and the production cycle is long, improves production cost.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of antioxidizing paint of carbon/carbon composite, and adopt this antioxidizing paint to prepare the method for the inoxidzable coating of carbon/carbon composite, the high-temperature oxidation resistance of the inoxidzable coating of this carbon/carbon composite more by force, and is prepared, coating process is simpler.The technical scheme adopted is as follows:
An antioxidizing paint for carbon/carbon composite, is characterized in that each composition of described antioxidizing paint is by weight percentage: 10 ~ 15%MoSi
2, 5 ~ 10%B, 10 ~ 15%B
2o
3, 5 ~ 10%SiO
2, 5 ~ 10%Al
2o
3, 10 ~ 15%Zn
3(PO
4)
2, 15 ~ 20%H
3pO
4, 15 ~ 20%H
2o.
The granularity of the powder used by above-mentioned each composition is all less than 45 μm (microns), to guarantee abundant, Homogeneous phase mixing.
The preparation method of the antioxidizing paint of described carbon/carbon composite comprises the steps:
(1), by Zn
3(PO
4)
2be dissolved in phosphoric acid;
(2), will through H
2o(water) dilution after MoSi
2, B, B
2o
3, Al
2o
3, SiO
2h poured into by mixed solution
3pO
4in (phosphoric acid);
(3), be uniformly mixed, make liquid antioxidizing paint.
A preparation method for the inoxidzable coating of carbon/carbon composite, is characterized in that comprising the steps:
(1), adopt above-mentioned antioxidizing paint to be coated with on carbon/carbon composite surface, form inoxidzable coating;
(2) 2 ~ 3 hours are incubated under, under nitrogen protection, the carbon/carbon composite being coated with inoxidzable coating being placed on the environment of 800 DEG C ~ 1000 DEG C;
(3), under nitrogen protection, after cooling, the carbon/carbon composite being coated with inoxidzable coating is taken out.
As preferred version of the present invention, in described step (3), the carbon/carbon composite being coated with inoxidzable coating is cooling to less than 200 DEG C taking-ups.
Compared with prior art, tool has the following advantages inoxidzable coating of the present invention:
(1) owing to have employed phosphoric acid salt as base coating; the penetrating power of its solution is strong; envelope effect is filled out to carbon/carbon composite surface, makes to form continuous, the fine and close protective film that can stop oxygen molecule scattering and permeating by the carbon/carbon composite surface in surface inwardly darker scope.
(2) due to B
2o
3start to soften at 209 DEG C, 720 DEG C of meltings, so can make coating crack self-healing, this is also by B in prior art
2o
3as the reason of carbon/carbon composite material oxidation-proof coating important component.Core technology of the present invention is at B
2o
3moSi is introduced in components such as (boron oxides)
2(molybdenum silicide); when temperature reaches more than 700 DEG C, its oxidising process is slowly carried out by logarithmic curve rule, generate in glass borosilicate protective membrane finer and close, airtight; be attached on carbon/carbon composite more stable on the surface, and the higher protective membrane of temperature forms more thorough.Because the operative temperature of this symbiosis borosilicate can reach more than 1000 DEG C, so inoxidzable coating of the present invention can improve the high-temperature oxidation resistance of carbon/carbon composite by a relatively large margin.
(3) working temperature of the inoxidzable coating of carbon/carbon composite of the present invention is 400 DEG C ~ 1000 DEG C, and subject range is quite wide, under basic, normal, high temperature, all have excellent resistance of oxidation.
(4) coating preparation of the present invention and coating process simply, are applicable to the inoxidzable coating of multiple configuration charcoal dish.
Embodiment
Embodiment one
By Zn
3(PO
4)
2be dissolved in H
3pO
4(phosphoric acid); Again will through H
2o(water) dilution after MoSi
2, B, B
2o
3, Al
2o
3, SiO
2mixed solution is poured in phosphoric acid solution, and above each composition is by weight percentage: 10%MoSi
2, 10%B, 10%B
2o
3, 10%SiO
2, 10%Al
2o
3, 15%Zn
3(PO
4)
2, 15%H
3pO
4, 20%H
2o; Then be uniformly mixed, make liquid antioxidizing paint.The antioxidizing paint of liquid state is coated on (specimen size: length × wide × height=10mm × 8mm × 6mm, lower same) on 5 carbon/carbon composite specimen surfaces, then is heated to 800 DEG C under nitrogen protection, be incubated 2 hours, cool to 200 DEG C of samplings with the furnace.In the air ambient of 800 DEG C, heating carries out sample in 10 hours, and its average oxidation rate of weight loss is 1.14%.
Embodiment two
By Zn
3(PO
4)
2be dissolved in H
3pO
4(phosphoric acid); Again will through H
2o(water) dilution after MoSi
2, B, B
2o
3, Al
2o
3, SiO
2mixed solution is poured in phosphoric acid solution, and above each composition is by weight percentage: 15%MoSi
2, 5%B, 15%B
2o
3, 5%SiO
2, 10%Al
2o
3, 15%Zn
3(PO
4)
2, 15%H
3pO
4, 20%H
2o; Then be uniformly mixed, make liquid antioxidizing paint.The antioxidizing paint of liquid state is coated on 5 carbon/carbon composite specimen surfaces, then is heated to 900 DEG C under nitrogen protection, be incubated 3 hours, cool to 200 DEG C of samplings with the furnace.In the air ambient of 900 DEG C, heating carries out sample in 5 hours, and its average oxidation rate of weight loss is 1.38%.
Embodiment three
By Zn
3(PO
4)
2be dissolved in H
3pO
4(phosphoric acid); Again will through H
2o(water) dilution after MoSi
2, B, B
2o
3, Al
2o
3, SiO
2mixed solution is poured in phosphoric acid solution, and above each composition is by weight percentage: 15%MoSi
2, 5%B, 15%B
2o
3, 10%SiO
2, 10%Al
2o
3, 10%Zn
3(PO
4)
2, 20%H
3pO
4, 15%H
2o; Then be uniformly mixed, make liquid antioxidizing paint.The antioxidizing paint of liquid state is coated on 5 carbon/carbon composite specimen surfaces, then is heated to 1000 DEG C under nitrogen protection, be incubated 2.5 hours, cool to 200 DEG C of samplings with the furnace.In the air ambient of 1000 DEG C, heating carries out sample in 3 hours, and its average oxidation rate of weight loss is 1.92%.
By Chinese national military standard GJB 4193-2001 " military aircraft brake flange general specification " " 3.13 oxidation proof properties " regulation, " charcoal dish oxidation proof properties should meet special technology condition regulation.General oxidative mass loss should be less than 10% ".Visible, the oxidative mass loss of the various embodiments described above is all much smaller than 10% of " military aircraft brake flange general specification " defined, and high-temperature oxidation resistance is stronger.
In addition; it should be noted that, the specific embodiment described in this specification sheets, its each several part title etc. can be different; all equivalences of doing according to structure, feature and the principle described in inventional idea of the present invention or simple change, be included in the protection domain of patent of the present invention.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
Claims (4)
1. an antioxidizing paint for carbon/carbon composite, is characterized in that each composition of described antioxidizing paint is by weight percentage: 10 ~ 15%MoSi
2, 5 ~ 10%B, 10 ~ 15%B
2o
3, 5 ~ 10%SiO
2, 5 ~ 10%Al
2o
3, 10 ~ 15%Zn
3(PO
4)
2, 15 ~ 20%H
3pO
4, 15 ~ 20%H
2o, the granularity of the powder used by each composition is all less than 45 μm.
2. the preparation method of antioxidizing paint as claimed in claim 1, is characterized in that comprising the steps:
(1), by Zn
3(PO
4)
2be dissolved in phosphoric acid;
(2), will through H
2o(water) dilution after MoSi
2, B, B
2o
3, Al
2o
3, SiO
2h poured into by mixed solution
3pO
4in;
(3), be uniformly mixed, make liquid antioxidizing paint.
3. a preparation method for the inoxidzable coating of carbon/carbon composite, is characterized in that comprising the steps:
(1), adopt antioxidizing paint as claimed in claim 1 to be coated with on carbon/carbon composite surface, form inoxidzable coating;
(2) 2 ~ 3 hours are incubated under, under nitrogen protection, the carbon/carbon composite being coated with inoxidzable coating being placed on the environment of 800 DEG C ~ 1000 DEG C;
(3), under nitrogen protection, after cooling, the carbon/carbon composite being coated with inoxidzable coating is taken out.
4. the preparation method of inoxidzable coating as claimed in claim 3, it is characterized in that: in described step (3), the carbon/carbon composite being coated with inoxidzable coating is cooling to less than 200 DEG C taking-ups.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310183782.2A CN103274760B (en) | 2013-05-17 | 2013-05-17 | Anti-oxidative coating of charcoal/charcoal composite material and application of anti-oxidative coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310183782.2A CN103274760B (en) | 2013-05-17 | 2013-05-17 | Anti-oxidative coating of charcoal/charcoal composite material and application of anti-oxidative coating |
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| CN103274760A CN103274760A (en) | 2013-09-04 |
| CN103274760B true CN103274760B (en) | 2015-02-11 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10087101B2 (en) | 2015-03-27 | 2018-10-02 | Goodrich Corporation | Formulations for oxidation protection of composite articles |
| CN105111935B (en) * | 2015-09-02 | 2017-08-29 | 航天材料及工艺研究所 | A kind of high temperature resistant height radiation thermal control coating and preparation method thereof |
| US10465285B2 (en) | 2016-05-31 | 2019-11-05 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10377675B2 (en) | 2016-05-31 | 2019-08-13 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10508206B2 (en) | 2016-06-27 | 2019-12-17 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10767059B2 (en) | 2016-08-11 | 2020-09-08 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10526253B2 (en) | 2016-12-15 | 2020-01-07 | Goodrich Corporation | High temperature oxidation protection for composites |
| CN108178663B (en) * | 2018-01-26 | 2020-09-22 | 河南省化工研究所有限责任公司 | Preparation method of ultrahigh-temperature antioxidant graphite mold |
| US11046619B2 (en) | 2018-08-13 | 2021-06-29 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11634213B2 (en) | 2018-11-14 | 2023-04-25 | Goodrich Corporation | High temperature oxidation protection for composites |
| CN113666758B (en) * | 2021-09-03 | 2023-02-17 | 江苏锦耐新材料科技有限公司 | Antioxidant coating for magnesia carbon brick and preparation method thereof |
| US12065380B2 (en) | 2021-11-16 | 2024-08-20 | Goodrich Corporation | High temperature oxidation protection for carbon-carbon composites |
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| CN101153123A (en) * | 2007-09-11 | 2008-04-02 | 西安超码科技有限公司 | Anti-oxidization coating for airplane carbon/carbon brake disc and method of producing the same |
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| CN101153123A (en) * | 2007-09-11 | 2008-04-02 | 西安超码科技有限公司 | Anti-oxidization coating for airplane carbon/carbon brake disc and method of producing the same |
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Address after: 515000 Guangdong city of Shantou province university road gold Shengping Industrial Zone West Patentee after: Guangdong Northwest Airlines Polytron Technologies Inc Address before: University of Jinping District 515000 in Guangdong province Shantou city circle road Shengping Industrial Zone West Patentee before: Shantou Northwest Aviation Articles Co., Ltd. |