CN103274760A - 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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- CN103274760A CN103274760A CN2013101837822A CN201310183782A CN103274760A CN 103274760 A CN103274760 A CN 103274760A CN 2013101837822 A CN2013101837822 A CN 2013101837822A CN 201310183782 A CN201310183782 A CN 201310183782A CN 103274760 A CN103274760 A CN 103274760A
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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, relate in particular to a kind of antioxidizing paint and application thereof of carbon/carbon composite.
Background technology
Carbon/carbon composite is higher than 370 ℃ oxidizing reaction just takes place when temperature, and temperature significantly oxidation above 450 ℃ causes the rapid deterioration of physics, chemistry and mechanical property of material.And the moment of aircraft normal landing brake, the brake flange surface temperature is up to more than 1000 ℃, and body holds temperature and reaches 600 ℃～800 ℃, and overload and scram body hold temperature can reach 800 ℃～1000 ℃.Therefore, must become the gordian technique that guarantees brake safety for heavy duties such as aircraft braking with carbon/carbon composite brake flange (calling the charcoal dish in the following text) high-temp antioxidizing.
For many years, external aircraft charcoal dish mainly uses phosphoric acid salt and silicate two big class inoxidzable coatings.The composition of phosphate coating is simpler, is solvent with water how; The composition of silicate coating is complicated, uses organic binder bond more, more than two type coatings all have oxidation-protective effect preferably.Introduced a kind of by rare earth chloride modification borosilicate, boron, boride, SiC, CeS in the China Patent No. 9011058.6
2And the aircraft charcoal dish inoxidzable coating of resol composition.Introduced a kind of inoxidzable coating and coating process thereof for aircraft charcoal dish among the Chinese patent publication number CN1415669A, coating is to be made of presoak (boric acid, phosphoric acid and distilled water) and coating (silicon carbide, boron and boride, silica flour etc.).More than two patented technologies all improved the resistance of oxidation of charcoal dish to some extent, but the preparation of its coating and coating process are complicated, its high-temperature oxidation resistance also need improve.Introduced a kind of carbon/carbon composite material oxidation-proof coating based on phosphoric acid salt among the Chinese patent publication number CN1544536A, wherein silicon 10%～15%, boron 10%～15%, phosphoric acid salt 60%～70%, aluminum oxide 5%～10%, though it is fairly simple to fill a prescription, low temperature and high-temp antioxidizing effect are not too desirable.
In addition, Chinese patent publication number CN100410212C, a kind of carbon/carbon composite material oxidation-proof coating is a kind of compound coating, main component is Al (OH)
3, Zn
3(PO
4)
24H
2O, Na
2B
4O
710H
2O, SiO
2, B etc. through the carbon/carbon composite material oxidation-proof coating that obtains after twice processing, have antioxidant effect preferably, and the feature of environmental protection is good.This class compound coating need brush twice, thermal treatment twice, and the production cycle is long, has improved production cost.
Summary of the invention
The technical problem to be solved in the present invention provides 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 is stronger, and preparation, coating process are simpler.The technical scheme that adopts is as follows:
A kind of antioxidizing paint of 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 above-mentioned granularity of used powder of respectively forming is all less than 45 μ m(microns), to guarantee fully, evenly to mix.
The preparation method of the antioxidizing paint of described carbon/carbon composite comprises the steps:
(1), with Zn
3(PO
4)
2Be dissolved in phosphoric acid;
(2), will be through H
2O(water) MoSi after the dilution
2, B, B
2O
3, Al
2O
3, SiO
2Mixed solution is poured H into
3PO
4In (phosphoric acid);
(3), mix, make liquid antioxidizing paint.
A kind of preparation method of inoxidzable coating of carbon/carbon composite is characterized in that comprising the steps:
(1), the above-mentioned antioxidizing paint of employing is coated with the formation inoxidzable coating on the carbon/carbon composite surface;
(2), under nitrogen protection, the carbon/carbon composite that is coated with inoxidzable coating is placed under 800 ℃～1000 ℃ the environment and is incubated 2～3 hours;
(3), under nitrogen protection, the carbon/carbon composite that will be coated with inoxidzable coating after the cooling takes out.
As preferred version of the present invention, in the described step (3), the carbon/carbon composite that is coated with inoxidzable coating is cooling to taking-up below 200 ℃.
Inoxidzable coating of the present invention compared with prior art has following advantage:
(1) owing to adopted phosphoric acid salt as basic coating; the penetrating power of its solution is strong; the envelope effect is filled out on the carbon/carbon composite surface, make by the surface and inwardly form continuous, the fine and close protective film that can stop the oxygen molecule scattering and permeating than the carbon/carbon composite surface in the dark scope.
(2) because B
2O
3Begin to soften at 209 ℃, 720 ℃ of fusions, so can make the coating crack self-healing, this also is with B in the prior art
2O
3Reason as the carbon/carbon composite material oxidation-proof coating important component.Core technology of the present invention is at B
2O
3Introduce MoSi in the components such as (boron oxides)
2(molybdenum silicide); when temperature reached more than 700 ℃, its oxidising process was slowly carried out by the logarithmic curve rule, generate that to be glass borosilicate protective membrane finer and close, airtight; be attached on the carbon/carbon composite surface more stablely, and the more high protective membrane of temperature forms more thoroughly.Because the operative temperature of this symbiosis borosilicate can reach more than 1000 ℃, 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 ℃～1000 ℃, and subject range is quite wide, all has good resistance of oxidation under basic, normal, high temperature.
(4) coating preparation of the present invention and coating process are simple, are applicable to the inoxidzable coating of multiple configuration charcoal dish.
Embodiment
Embodiment one
With Zn
3(PO
4)
2Be dissolved in H
3PO
4(phosphoric acid); Again will be through H
2O(water) MoSi after the dilution
2, B, B
2O
3, Al
2O
3, SiO
2Mixed solution is poured in the phosphoric acid solution, more than each composition be 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; Mix then, make liquid antioxidizing paint.The antioxidizing paint of liquid state is coated on 5 carbon/carbon composite specimen surfaces (specimen size: length * wide * height=10mm * 8mm * 6mm, down with), under nitrogen protection, be heated to 800 ℃ again, be incubated 2 hours, cool to 200 ℃ of samplings with the furnace.Heating was carried out sample in 10 hours in 800 ℃ air ambient, and its average oxidative mass loss is 1.14%.
Embodiment two
With Zn
3(PO
4)
2Be dissolved in H
3PO
4(phosphoric acid); Again will be through H
2O(water) MoSi after the dilution
2, B, B
2O
3, Al
2O
3, SiO
2Mixed solution is poured in the phosphoric acid solution, more than each composition be 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; Mix then, make liquid antioxidizing paint.The antioxidizing paint of liquid state is coated on 5 carbon/carbon composite specimen surfaces, under nitrogen protection, is heated to 900 ℃ again, be incubated 3 hours, cool to 200 ℃ of samplings with the furnace.Heating was carried out sample in 5 hours in 900 ℃ air ambient, and its average oxidative mass loss is 1.38%.
Embodiment three
With Zn
3(PO
4)
2Be dissolved in H
3PO
4(phosphoric acid); Again will be through H
2O(water) MoSi after the dilution
2, B, B
2O
3, Al
2O
3, SiO
2Mixed solution is poured in the phosphoric acid solution, more than each composition be 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; Mix then, make liquid antioxidizing paint.The antioxidizing paint of liquid state is coated on 5 carbon/carbon composite specimen surfaces, under nitrogen protection, is heated to 1000 ℃ again, be incubated 2.5 hours, cool to 200 ℃ of samplings with the furnace.Heating was carried out sample in 3 hours in 1000 ℃ air ambient, and its average oxidative mass loss is 1.92%.
By Chinese national military standard GJB 4193-2001 " military aircraft brake flange general specification " " 3.13 anti-oxidation performance " regulation, " the anti-oxidation performance of charcoal dish should meet special technology condition regulation.General oxidative mass loss should be less than 10% ".As seen, all much smaller than 10% of " military aircraft brake flange general specification " defined, high-temperature oxidation resistance is stronger for the oxidative mass loss of the various embodiments described above.
In addition; need to prove, the specific embodiment described in this specification sheets, its each several part titles etc. can be different; allly conceive equivalence or the simple change that described structure, feature and principle are done according to patent of the present invention, be included in the protection domain of patent of the present invention.Those skilled in the art can make various modifications or replenish or adopt similar mode to substitute described specific embodiment; only otherwise depart from structure of the present invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.
Claims (4)
1. the antioxidizing paint of a 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.
2. the preparation method of antioxidizing paint as claimed in claim 1 is characterized in that comprising the steps:
(1), with Zn
3(PO
4)
2Be dissolved in phosphoric acid;
(2), will be through H
2O(water) MoSi after the dilution
2, B, B
2O
3, Al
2O
3, SiO
2Mixed solution is poured H into
3PO
4In;
(3), mix, make liquid antioxidizing paint.
3. the preparation method of the inoxidzable coating of a carbon/carbon composite is characterized in that comprising the steps:
(1), employing antioxidizing paint as claimed in claim 1 is coated with the formation inoxidzable coating on the carbon/carbon composite surface;
(2), under nitrogen protection, the carbon/carbon composite that is coated with inoxidzable coating is placed under 800 ℃～1000 ℃ the environment and is incubated 2～3 hours;
(3), under nitrogen protection, the carbon/carbon composite that will be coated with inoxidzable coating after the cooling takes out.
4. the preparation method of inoxidzable coating as claimed in claim 3 is characterized in that: in the described step (3), the carbon/carbon composite that is coated with inoxidzable coating takes out cooling to below 200 ℃.
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 |
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|---|---|---|---|
| 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 true CN103274760A (en) | 2013-09-04 |
| CN103274760B CN103274760B (en) | 2015-02-11 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111935A (en) * | 2015-09-02 | 2015-12-02 | 航天材料及工艺研究所 | High-temperature-resistant and high-radiation-resistant thermal control coating and preparation method thereof |
| CN108178663A (en) * | 2018-01-26 | 2018-06-19 | 河南省化工研究所有限责任公司 | A kind of preparation method of superhigh temperature oxidation-resistant graphite mold |
| US10087101B2 (en) | 2015-03-27 | 2018-10-02 | Goodrich Corporation | Formulations for oxidation protection of composite articles |
| US10377675B2 (en) | 2016-05-31 | 2019-08-13 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10465285B2 (en) | 2016-05-31 | 2019-11-05 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10508206B2 (en) | 2016-06-27 | 2019-12-17 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10526253B2 (en) | 2016-12-15 | 2020-01-07 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10767059B2 (en) | 2016-08-11 | 2020-09-08 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11046619B2 (en) | 2018-08-13 | 2021-06-29 | Goodrich Corporation | High temperature oxidation protection for composites |
| CN113666758A (en) * | 2021-09-03 | 2021-11-19 | 江苏锦耐新材料科技有限公司 | Antioxidant coating for magnesia carbon brick and preparation method thereof |
| US11634213B2 (en) | 2018-11-14 | 2023-04-25 | Goodrich Corporation | High temperature oxidation protection for composites |
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| 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 |
| CN105111935A (en) * | 2015-09-02 | 2015-12-02 | 航天材料及工艺研究所 | High-temperature-resistant and high-radiation-resistant thermal control coating and preparation method thereof |
| US10941486B2 (en) | 2016-05-31 | 2021-03-09 | Goodrich Corporation | High temperature oxidation protection for composites |
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| US11325868B2 (en) | 2016-05-31 | 2022-05-10 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10377675B2 (en) | 2016-05-31 | 2019-08-13 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11001533B2 (en) | 2016-05-31 | 2021-05-11 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10508206B2 (en) | 2016-06-27 | 2019-12-17 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11168222B2 (en) | 2016-06-27 | 2021-11-09 | Goodrich Corporation | High temperature oxidation protection for composites |
| US10767059B2 (en) | 2016-08-11 | 2020-09-08 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11091402B2 (en) | 2016-12-15 | 2021-08-17 | Goodrich Coporation | High temperature oxidation protection for composites |
| US10526253B2 (en) | 2016-12-15 | 2020-01-07 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11505507B2 (en) | 2016-12-15 | 2022-11-22 | Goodrich Corporation | High temperature oxidation protection for composites |
| CN108178663A (en) * | 2018-01-26 | 2018-06-19 | 河南省化工研究所有限责任公司 | A kind of preparation method of superhigh temperature oxidation-resistant graphite mold |
| US11046619B2 (en) | 2018-08-13 | 2021-06-29 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11453619B2 (en) | 2018-08-13 | 2022-09-27 | Goodrich Corporation | High temperature oxidation protection for composites |
| US11634213B2 (en) | 2018-11-14 | 2023-04-25 | Goodrich Corporation | High temperature oxidation protection for composites |
| CN113666758A (en) * | 2021-09-03 | 2021-11-19 | 江苏锦耐新材料科技有限公司 | Antioxidant coating for magnesia carbon brick and preparation method thereof |
| 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 |
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| CN103274760B (en) | 2015-02-11 |
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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. |