CN106518166A - Carbon/carbon composite material anti-oxidation coating layer and heat treatment method - Google Patents
Carbon/carbon composite material anti-oxidation coating layer and heat treatment method Download PDFInfo
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- CN106518166A CN106518166A CN201610844409.0A CN201610844409A CN106518166A CN 106518166 A CN106518166 A CN 106518166A CN 201610844409 A CN201610844409 A CN 201610844409A CN 106518166 A CN106518166 A CN 106518166A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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Abstract
The invention discloses a carbon/carbon composite material anti-oxidation coating layer and a heat treatment method, and is characterized in that the anti-oxidation coating layer comprises the following components by the weight percentage: 1-10% of SiO2, 5-20% of TiO2, 30-50% of TiB2, 10-30% of SiC, 10-30% of B4C, 1-10% of B, and 1-5% of OP-4. Phosphoric acid is added into the components according to the ratio of 0.5-1.5 ml/g, then the components are stirred evenly, and the anti-oxidation coating layer is obtained; the anti-oxidation coating layer is brushed on the surface of a carbon/carbon composite material, then is placed in a vacuum or protective atmosphere and is subjected to heat treatment, the treatment temperature is 600 DEG C-900 DEG C, heat preservation is carried out for 1-4 h, and the heat treatment is completed; the coating layer composition ratio improves the fracture toughness of the coating layer, the antioxidant capacity of the coating layer is improved, the obtained coating layer has the advantages of easy construction, low production cost, compact coating layer structure, good water solubility, and good oxidation resistance and thermal shock resistance abilities.
Description
Technical field
Patent of the present invention is related to carbon/carbon composite material oxidation-proof coating technical field, more particularly to a kind of charcoal/charcoal composite wood
Material compact structure, the inoxidzable coating of resistance to good water solubility, and the heat treatment method of the carbon/carbon composite.
Background technology
In recent years, the research of carbon/carbon composite and application were just received more and more attention.Carbon/carbon composite is
It is made up of Carbon fibe and carbon matrix, with density is low, corrosion-resistant, the good characteristic such as high intensity, high-moduluss, electrical and thermal conductivity be good.
Because of its mechanical property good at high temperature, carbon/carbon composite has been widely used in Aeronautics and Astronautics field, and such as rocket is sent out
A kind of thermal protection system on the space vehicles device such as motivation, nose cone and leading edge of a wing, it is considered to be high temperature of great application prospect
Structural material.However, research shows, in the oxidizing atmosphere higher than 723K, because significantly oxidation reaction causes charcoal/charcoal to be combined
The mechanical property of material is decreased obviously, so as to limit its application at high temperature.
In decades, people have carried out substantial amounts of research to carbon/carbon composite, develop many anti-oxidation technologies, its
Middle inoxidzable coating technology is one of topmost method.
A kind of carbon/carbon composite material oxidation-proof based on phosphate is described in China Patent Publication No. CN1544536A
Coating, wherein silicon 10%-15%, boron 10%-15%, phosphate 60%-70%, aluminium oxide 5%-10%, its recipe ratio are simpler
It is single, and low temperature and high-temp antioxidizing effect are not too preferable.
What another kind of research was more is SiC coatings, and Jing is frequently with chemical vapor deposition (CVD) method.At high temperature, due to
SiC and O2 reacts the SiO2 thin film to form densification, thus has good protection effect.But this kind of high temperature coating is due to the coefficient of expansion
Cause to crack under low temperature with the difference of the carbon/carbon composite coefficient of expansion, thus be not suitable for prolonged application in middle low temperature ring
Border, is not suitable for aircraft carbon-carbon composites brake disc.
In order to improve the performance of inoxidzable coating, it is anti-that many patents carry out prolonged oxidation by the way of composite coating
Shield, based on phosphate, outer layer is that, containing borosilicate, such heatproof increases, and the time is also extended to usual bottom.But should
The class PROCESS FOR TREATMENT cycle is long.In this type coating, many raw materials are toxic, and workmen and environment are adversely affected.
Describing one kind in China Patent Publication No. CN1415669A has prepreg solution (boric acid, phosphoric acid and distilled water) and coating
The compound inoxidzable coating of (900# high-temperature agglomerants and SiC, boron and boride, silica flour, alchlor powder, distilled water), wherein
Boric acid needs to dissolve in a heated state, or dissolves in ethanol, and binding agent and diluent are generally toxic.Chinese patent is public
The number of opening CN100410212C, a kind of carbon/carbon composite material oxidation-proof coating is also a kind of composite coating, and main component is Al
(OH) 3, Zn3 (PO4) 2 4H2O, Na2B4O7 10H2O, SiO2, B etc., the carbon/carbon composite obtained after processing twice
Inoxidzable coating, has preferable antioxidant effect, and the feature of environmental protection is good.This kind of composite coating is divided into bottom and outer layer, and bottom is by Al
(OH) clear solution that 3, Zn3 (PO4), 2 4H2O, and H3PO4 are formed, after brushing in charcoal/charcoal material surface, in nitrogen or
Obtain primer coating under vacuum condition after 500-900 DEG C of high-temperature process, then by Na2B4O7 10H2O, SiO2, B and the third three
The coating of alcohol composition is coated in above carbon/carbon composite primer coating, and is dried through 200 DEG C and formed.The coating is needed
Brush twice, heat treatment twice, with reference to bottom is low temperature resistant and the characteristics of outer layer high temperature resistance, plays good antioxidant effect.
But while also causing long the production cycle, improve production cost.
A kind of with short production cycle, low production cost, and low temperature is described in China Patent Publication No. CNIO2492318A
And high-temp antioxidizing effect is good, nontoxic carbon/carbon composite material oxidation-proof agent and heat treatment method.Antioxidant coating is by weight
Percentage ratio is：25-35%SiO2,15-25%TiO2,8-20%SiC, 10-20%B4C, 5-15%NaAlO2,5-15%Al
(OH) 3,1-3% hexadecyltrimethylammonium chlorides composition, wherein Al (OH) 3 are dissolved in H3PO4 with the ratio of 7mL/g,
NaAlO2 is dissolved in the water with the ratio of 4mL/g, and hexadecyltrimethylammonium chloride is dissolved in the water with the ratio of 5mL/g, will
During SiO2, TiO2, SiC, B4C powder adds the phosphoric acid solution dissolved with Al (OH) 3, the body of dilution, water and phosphoric acid solution is added water
Product is than being 20-100:100, stir, be subsequently adding NaAlO2 solution and be sufficiently stirred for, be eventually adding cetyl trimethyl chlorine
Change aqueous ammonium, be sufficiently stirred for forming its uniform mixed preparing.Its process for preparation is complicated, is not easy to operation.Chinese patent is public
A kind of preparation method of quick anti-oxidation process is described in the number of opening CN 101805207.Mainly include 30-50%SiC, 1-
10%Al (OH) 3,15-35%Si02,5-40% Kaolin, Al (OH) 3 is dissolved in H3PO4 with 5-15ml/g ratios, and
Mixed with other compositions after dilute again, obtained coating is directly brushed in charcoal material surface, Jing baking oven low-temperature solids
Can use after change.But which is kept for 15 hours in 700 DEG C of air, oxidative mass loss is less than 1.0%.Only it is adapted to short-term fast
The anti-oxidation process of speed, it is impossible to meet the antioxidation requirement of braking disk with composite carbon/carbon material life-time service.
The content of the invention
For the problems of the prior art, the invention aims to a kind of with short production cycle, low production cost is provided, can
The antioxidant effect for arriving is played very much for a long time, and construction is simple, it is easy to the carbon/carbon composite material oxidation-proof coating of popularization and heat treatment side
Method.
In order to achieve the above object, the technical scheme is that：
A kind of carbon/carbon composite material oxidation-proof coating, it is characterised in that：The inoxidzable coating is by following percentage by weight
Into being grouped into：1-10%SiO2,5-20%TiO2,30-50%TiB2,10-30%SiC, 10-30%B4C, 1-10%B, 1-
5%OP-4；Stir after phosphoric acid is added with the ratio of 0.5-1.5ml/g in the component, obtain the inoxidzable coating.
Patent of the present invention provides a kind of carbon/carbon composite heat treatment method simultaneously, it is characterised in that：By 1-10%
SiO2,5-20%TiO2,30-50%TiB2,10-30%SiC, 10-30%B4C, 1-10%B, 1-5%OP-4 percentage by weight
Phosphoric acid is added than the ratio after mixing according to 0.5-1.5ml/g, is stirred, is obtained the inoxidzable coating, it is then that this is anti-oxidation
Coating brushing is on carbon/carbon composite surface, and is put into heat treated in vacuum or protective atmosphere, treatment temperature be 600 DEG C-
900 DEG C, 1-4 hours are incubated, heat treatment is completed.
Further, the inoxidzable coating by following percentage by weight into being grouped into：5%SiO2,10%TiO2,40%
TiB2,20%SiC, 15%B4C, 5%B, 5%OP-4；In the component add stirring after phosphoric acid equal with the ratio of 1.0ml/g
It is even, obtain the inoxidzable coating.
Further, by 5%SiO2,10%TiO2,40%TiB2,20%SiC, 15%B4C, 5%B, 5%OP-4 by weight
Phosphoric acid is added according to the ratio of 1.0ml/g after amount percentage ratio mixing, is stirred, is obtained the inoxidzable coating, then by the oxygen
Change coating brushing on carbon/carbon composite surface, and be put into heat treated in vacuum or protective atmosphere, treatment temperature is 750 DEG C,
Insulation 2 hours, completes heat treatment.
Compared with prior art, the composition of the carbon/carbon composite material oxidation-proof coating that the present invention is provided is unusual, oxygen
Change effect is significant, the TiB2 powder in the present invention is a kind of industrial ceramics raw material, have the dual of structural ceramicss and function ceramics concurrently
Purposes, with the characteristic more excellent than general industry ceramic material, such as wear-resistant, acid and alkali-resistance, the property under the atmosphere of high-temperature oxydation
Matter is still sufficiently stable, and thermal shock resistance is excellent.This characteristic of the present invention using TiB2 powder, should by a certain amount of TiB2 powder
Use in the inoxidzable coating of carbon/carbon composite, play good high temperature resistant, antioxidation, corrosion resistant feature.
The antioxidizing paint that the present invention is adopted adds the antioxidant composition such as a certain amount of TiO2, SiC, B4C based on TiB2,
It is wear-resistant using TiB2, acid and alkali-resistance, antioxidation, thermal shock resistance advantage, the fracture toughness of raising coating, and the addition of B4C
The growth of TiB2 crystal grain can be suppressed, further improve the fracture toughness of coating, improve the oxidation resistance of coating.The present invention is made
Standby inoxidzable coating is not only prepared simply, is adopted and is once brushed, a heat treatment, it is easy to construct, low production cost, and is applied
Rotating fields are fine and close, and resistance to good water solubility has good antioxidation and thermal shock resistance.In 700 DEG C of air, aoxidize within 30 hours, it is weightless
Rate is close to zero.Which is particularly suited for the anti-oxidation process of braking disk with composite carbon/carbon material.
Specific embodiment
The present invention is further described with reference to embodiment.
Embodiment one：
The preparation of inoxidzable coating, work progress, anti-oxidation experiment are as follows:
1：By 5%SiO2,10%TiO2,40%TiB2,20%SiC, 15%B4C, 5%B, 5%OP-4 percentage by weight
Phosphoric acid is added than the ratio after mixing according to 1.0ml/g, is stirred, is obtained the inoxidzable coating；
2：By the inoxidzable coating brushing on the surface of carbon/carbon composite sample (10mm × 10mm × 15mm), and
The lower heat treated of nitrogen protection, is heated to 750 DEG C of temperature, is incubated 2 hours, completes heat treatment.
3：The carbon/carbon composite sample with inoxidzable coating that step 2 is obtained in 700 DEG C of Muffle furnaces, air
In the case of, to test 30 hours, oxidation weight loss result is not more than 0.01%.Meanwhile, the sample that step 2 is obtained is placed in tap water
Immersion more than 24 hours, coating can be intact.
Embodiment two
The preparation of inoxidzable coating, work progress, anti-oxidation experiment are as follows:
1：By 10%SiO2,20%TiO2,30%TiB2,19%SiC, 10%B4C, 10%B, 1%OP-4 by weight hundred
Divide and phosphoric acid is added than the ratio after mixing according to 0.5ml/g, stir, obtain the inoxidzable coating；
2：By the inoxidzable coating brushing on the surface of carbon/carbon composite sample (10mm × 10mm × 15mm), and
The lower heat treated of nitrogen protection, is heated to 600 DEG C of temperature, is incubated 4 hours, completes heat treatment.
3：The carbon/carbon composite sample with inoxidzable coating that step 2 is obtained in 700 DEG C of Muffle furnaces, air
In the case of, to test 30 hours, oxidation weight loss result is not more than 0.01%.Meanwhile, the sample that step 2 is obtained is placed in tap water
Immersion more than 24 hours, coating can be intact.
Embodiment three
The preparation of inoxidzable coating, work progress, anti-oxidation experiment are as follows:
1：By 1%SiO2,5%TiO2,50%TiB2,10%SiC, 30%B4C, 1%B, 3%OP-4 by weight percentage
Ratio after mixing according to 1.5ml/g adds phosphoric acid, stirs, obtains the inoxidzable coating；
2：By the inoxidzable coating brushing on the surface of carbon/carbon composite sample (10mm × 10mm × 15mm), and
The lower heat treated of nitrogen protection, is heated to 900 DEG C of temperature, is incubated 1 hour, completes heat treatment.
3：The carbon/carbon composite sample with inoxidzable coating that step 2 is obtained in 700 DEG C of Muffle furnaces, air
In the case of, to test 30 hours, oxidation weight loss result is not more than 0.01%.Meanwhile, the sample that step 2 is obtained is placed in tap water
Immersion more than 24 hours, coating can be intact.
Example IV：
The preparation of inoxidzable coating, work progress, anti-oxidation experiment are as follows:
1：By 3%SiO2,8%TiO2,45%TiB2,15%SiC, 20%B4C, 6%B, 3%OP-4 by weight percentage
Ratio after mixing according to 1.2ml/g adds phosphoric acid, stirs, obtains the inoxidzable coating；
2：By the inoxidzable coating brushing on the surface of carbon/carbon composite sample (10mm × 10mm × 15mm), and
The lower heat treated of nitrogen protection, is heated to 650 DEG C of temperature, is incubated 3 hours, completes heat treatment.
3：The carbon/carbon composite sample with inoxidzable coating that step 2 is obtained in 700 DEG C of Muffle furnaces, air
In the case of, to test 30 hours, oxidation weight loss result is not more than 0.01%.Meanwhile, the sample that step 2 is obtained is placed in tap water
Immersion more than 24 hours, coating can be intact.
It is understood that above with respect to the specific descriptions of the present invention, being merely to illustrate the present invention and being not limited to this
Technical scheme described by inventive embodiments, it will be understood by those within the art that, still the present invention can be carried out
Modification or equivalent, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (4)
1. a kind of carbon/carbon composite material oxidation-proof coating, it is characterised in that：The inoxidzable coating by following percentage by weight into
It is grouped into：1-10%SiO2,5-20%TiO2,30-50%TiB2,10-30%SiC, 10-30%B4C, 1-10%B, 1-5%
OP-4；Stir after phosphoric acid is added with the ratio of 0.5-1.5ml/g in the component, obtain the inoxidzable coating.
2. a kind of carbon/carbon composite heat treatment method, it is characterised in that：By 1-10%SiO2,5-20%TiO2,30-50%
TiB2,10-30%SiC, 10-30%B4C, 1-10%B, 1-5%OP-4 mix by weight percentage after according to 0.5-1.5ml/g
Ratio add phosphoric acid, stir, obtain the inoxidzable coating, then by the inoxidzable coating brushing in carbon/carbon composite
Surface, and heat treated in vacuum or protective atmosphere is put into, treatment temperature is 600 DEG C -900 DEG C, is incubated 1-4 hours, completes heat
Process.
3. a kind of carbon/carbon composite material oxidation-proof coating according to claim 1, it is characterised in that：The inoxidzable coating
By following percentage by weight into being grouped into：5%SiO2,10%TiO2,40%TiB2,20%SiC, 15%B4C, 5%B, 5%
OP-4；Stir after phosphoric acid is added with the ratio of 1.0ml/g in the component, obtain the inoxidzable coating.
4. a kind of carbon/carbon composite heat treatment method according to claim 2, it is characterised in that：By 5%SiO2,
10%TiO2,40%TiB2,20%SiC, 15%B4C, 5%B, 5%OP-4 mix by weight percentage after according to 1.0ml/g's
Ratio adds phosphoric acid, stirs, obtains the inoxidzable coating, then by the inoxidzable coating brushing in carbon/carbon composite table
Face, and heat treated in vacuum or protective atmosphere is put into, treatment temperature is 750 DEG C, is incubated 2 hours, completes heat treatment.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110452019A (en) * | 2019-09-02 | 2019-11-15 | 广东省材料与加工研究所 | A kind of anti-oxidant maceration extract of graphite jig, preparation method and application |
| CN112341166A (en) * | 2020-12-04 | 2021-02-09 | 淄博昊祥模具科技有限公司 | Ceramic hand mold coating suitable for nitrile rubber glove production and preparation method thereof |
| CN113089047A (en) * | 2021-04-12 | 2021-07-09 | 四川九洲电器集团有限责任公司 | Aluminum alloy component and preparation method and application thereof |
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| CN103936465A (en) * | 2014-03-27 | 2014-07-23 | 中南大学 | Anti-oxidation coating of carbon/carbon composite material and preparation method of anti-oxidation coating |
| CN104973886A (en) * | 2014-04-10 | 2015-10-14 | 梅西耶-布加蒂-道提公司 | Protecting parts made of carbon-containing composite material from oxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110452019A (en) * | 2019-09-02 | 2019-11-15 | 广东省材料与加工研究所 | A kind of anti-oxidant maceration extract of graphite jig, preparation method and application |
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| CN113089047A (en) * | 2021-04-12 | 2021-07-09 | 四川九洲电器集团有限责任公司 | Aluminum alloy component and preparation method and application thereof |
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