CN107324847B - For CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material - Google Patents
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- CN107324847B CN107324847B CN201710495947.8A CN201710495947A CN107324847B CN 107324847 B CN107324847 B CN 107324847B CN 201710495947 A CN201710495947 A CN 201710495947A CN 107324847 B CN107324847 B CN 107324847B
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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
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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
- C04B41/5062—Borides, Nitrides or Silicides
- C04B41/507—Borides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to one kind to be used for CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material, belongs to special cermacis coating technology field.The coating is by ZrB2、SiC、B2O3It is made with acidic silicasol, preparation method is by ZrB2、SiC、B2O3It is mixed with acidic silicasol, is subsequently placed in ball grinder and carries out ball milling, obtain slurry, be sprayed at Cf/ SiC ceramic matrix composite material component surface, is heated up and is kept the temperature under argon atmosphere after drying, and C of the surface with anti-deposition antioxidant coating is obtainedf/ SiC ceramic matrix composite material.Coating of the invention uses ZrB2/SiC/B2O3Material system has good anti-deposition antioxygenic property, while having short preparation period, feature at low cost.
Description
Technical field
The present invention relates to one kind to be used for CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material, belongs to special cermacis coating skill
Art field.
Background technique
The development of aerospace and national defence new and high technology puts forward new requirements high-temperature structural material, military power, the world
The material of the metal and metal alloy that have not adapted to new demand can be all substituted in urgent searching.Advanced Ceramic Matrix Composites Fabricated
(CMCs) it is used as a kind of novel High-tech Material, there are the excellent properties such as high temperature resistant, antiscour, anticorrosive, high-strength light.It is external
The research of CMCs is concentrated mainly on the advanced countries such as the U.S., France, Germany and Japan, has developed Cf/SiC、SiC/SiC、C/
Al2O3、 C/Si3N4Etc. a variety of systems, wherein Cf/ SiC has been proved the CMCs material of most application prospect by beauty, moral, Fa Dengguo
Material. Cf/ SiC is also to study the most deep, the most commonly used a kind of ceramic matric composite of development and application so far.Currently, and Cf/
The various aspects such as the relevant raw material of SiC composite material, microstructure design, preparation process, characterization of structure and properties and failure mechanism
Basic research have become the hot spot of current composite material disciplinary study.
Cf/ SiC ceramic matrix composite material combines the plurality of advantages of carbon fiber and silicon carbide ceramics.Currently, Cf/ SiC ceramic matrix composite material exists
The fields such as strategic arms, space technology, energy technology, chemical industry, transportation industries have broad application prospects.The U.S., France, day
This grade developed country is successfully by Cf/ SiC ceramic matrix composite material is applied to the fields such as space propulsion system and aerospace craft thermal protection.
Cf/ SiC ceramic matrix composite material has enough intensity at high temperature, and has good antioxygenic property and thermal shock resistance, because
And it is extremely suitable as space propulsion system material.Cf/ SiC ceramic matrix composite material, which is applied to space propulsion system, can mitigate 30-
50% weight, and allow operating temperature higher, to improve the specific impulse of propulsion system.Developed country starts to visit in the eighties
Rope uses Cf/ SiC ceramic matrix composite material prepares the thrust chamber of satellite attitude control, rail control liquid-propellant rocket engine instead of niobium alloy, in recent years
It has carried out ground run successively, and has entered the practical stage.Use CfCombustion can be greatly lowered in/SiC ceramic matrix composite material thrust chamber
Room-nozzle structure quality is burnt, and largely saves propellant, rushes matter ratio to improve, increase the payload of satellite and is extended
The working life in space.Attach great importance to development always with C in the U.S.f/ SiC is the ceramic matric composite thrust chamber of representative.
Hyper-Therm HTC Inc. successfully develops C under the support of USAF Phillips Laboratoryf/ SiC ceramic
Based composites motor power room.Europe C is successfully developed using ICVI technique with SEP companyf/ SiC ceramic matrix composite material jet pipe,
And complete high-altitude ignition test run twice.Japanese Yamaguchi, Muarata etc. describe Japanese C in U.S. Patentf/SiC
Development work in terms of composite thrust room.They prepare C using CVI combination PIP techniquef/ SiC ceramic matrix composite material thrust
Room, and carried out engine ignition test.
The National University of Defense technology uses the C of PIP technique preparationf/ SiC ceramic matrix composite material thrust chamber successfully passed chamber pressure in 2005
The liquid-propellant rocket engine heat run of 3MPa, fuel gas temperature up to 3000K are examined, and the product steady operation time reaches 520s, are obtained
The historical breakthrough of the domestic high chamber pressure thrust chamber development work of composite material, properties of product are reached advanced world standards, and herein
On the basis of, carry out the C of different applying working conditionsfThe development of/SiC ceramic matrix composite material thrust chamber, realized at present small lot production with
Using.
China all mentions to further increase the combat radius of fighter plane and the efficiency of missile armament in multiple guided missile models
The scheme using solid rocket ramjet is gone out.For the requirement for adapting to New Generation Missile technology, solid-rocket punching press is started
Propellant used in machine will develop to energetic direction, and addition metal fuel is a current important development side of high-energy propellant
To.Fuel-rich propellant contains more metallic particles, can not abundant point due to anoxic and low temperature in gas generator
Fire burning, therefore, the fuel-rich combustion gas containing a large amount of metallic particles are to blend to complete burning with air in afterburning chamber, without
The metallic particles of burning, a small amount of metal oxide can form " sedimentary " in combustor surface, to influence the abundant of combustion gas
Burning, causes the efficiency of combustion of engine to reduce, it is therefore prevented that fuel-rich propellant deposition is a key technology, due to combustion
It is high-temperature oxygen-enriched for burning the environment in room, and has solids to wash away, and therefore, engine material it is also desirable to have high temperature resistant, resistance to burning
Erosion, anti-thermal shock, the performance of antiscour.Currently, being deposited in venturi and jet pipe position there are solids from the point of view of ground experiment
Problem be easy to cause blocking even engine shorting-out, is not able to satisfy the requirement of solid rocket ramjet.
Therefore a kind of high temperature resistant, anti-oxidant, antisiludging new structural material or coating are developed, is to meet solid-rocket punching
The demand of hydraulic motor, and then meet the most effective approach of needs of national New Generation Missile development.
Summary of the invention
To overcome the problems of the prior art, the object of the present invention is to provide one kind to be used for Cf/ SiC ceramic matrix composite material it is anti-settling
Product antioxidant coating, have the characteristics that preparation process simply, low manufacture cost.
It is of the present invention to be used for CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material is by ZrB2、SiC、B2O3And acidity
Silica solution is made, in which:
ZrB2、SiC、B2O3Volume ratio be 8-12:2-4:1-2, it is preferable that ZrB2、SiC、B2O3Volume ratio be 8:2:
1, it is highly preferred that ZrB2、SiC、B2O3Volume ratio be 8:3:1.
The quality and ZrB of acidic silicasol2, SiC and B2O3The ratio between gross mass of three is 2-3:1；
The preparation method of the coating the following steps are included:
A, by the ZrB of proportional quantity2, SiC and B2O3It mixes, acidic silicasol is then added, stirs evenly and is placed on ball grinder
Middle carry out ball milling, obtains slurry；Wherein, ZrB2、SiC、B2O3It is commercial product with acidic silicasol；
B, by Cf/ SiC ceramic matrix composite material component, which is placed in distilled water, to be cleaned by ultrasonic, spare after baking oven is dried；
C, slurry obtained in step a is sprayed at Cf/ SiC ceramic matrix composite material component surface, after drying under argon atmosphere
It is heated up and is kept the temperature, obtain C of the surface with anti-deposition antioxidant coatingf/ SiC ceramic matrix composite material.
Wherein it is preferred to which technical solution is as follows:
Ball-milling Time is 12-16h；
Coating layer thickness is 100-200 μm；
Heating rate is 5-10 DEG C/min, and warming temperature is 800-900 DEG C.
Soaking time is 1-1.5h.
In the present invention:
B2O3With very low fusing point (450 DEG C), high vapour pressure and low oxygen diffusion rate, while ZrB2At 1000 DEG C
Start oxidation and generates B2O3And ZrO2, in the 1100-1200 DEG C of continuous glassivation in part formed below, can play very
Good oxidation protection effect；1200 DEG C of beginning SiC start oxidation and generate SiO2, and and B2O3、ZrO2In conjunction with generate Pyrex and
ZrSiO4, ZrSiO4Equilibrium temperature be 1949K, be higher than this liquid-phase conversion of this temperature be cristobalite-four directions ZrO2New liquid
Phase, this new liquid phase can also play a protective role to 2400K, the ZrO generated in whole process2The nail stake that network structure is played
Effect can prevent the mechanical denuding of liquid glass layer well again, this is also the antioxidation mechanism of the coating.And the coating is anti-
Deposition characteristics are mostly derived from both sides reason, in oxygen-depleted zone due to the unburned complete metal such as metallic iron, aluminium, magnesium and non-gold
The ZrB of category2/SiC/B2O3There is the infiltration angle angles for being greater than 100 °, it is difficult to adhere to；In oxygen-rich area composite material surface shape
At oxidation liquid film, metal oxide is difficult to adhere under airflow scouring.Therefore, ZrB2/SiC/B2O3Material system has good
Anti- deposition and antioxygenic property.
Beneficial effects of the present invention are as follows:
Coating of the invention uses ZrB2/SiC/B2O3Material system can generate collaboration antiopxidant effect and lotus under high temperature
Leaf hydrophobic effect has good anti-deposition antioxygenic property, while having short preparation period, feature at low cost.
Detailed description of the invention
Fig. 1 is the SEM photograph for the coating that embodiment 1 obtains.
Specific embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
(1) commercially available ZrB is taken2Powder, SiC powder, B2O3Powder, according to ZrB2:SiC:B2O3The volume ratio of=8:2:1 is mixed to get
Powder A；
(2) commercial acid silica solution is taken, is mixed in mass ratio for the ratio of 2:1 with powder A, ball in ball grinder is then placed in
16h is ground, slurry B is obtained；
(3) by Cf/ SiC ceramic matrix composite material component, which is placed in, to be cleaned by ultrasonic in distilled water and is dried for standby in an oven；
(4) spraying process is used, slurry B is sprayed on Cf/ SiC ceramic matrix composite material surface, control coating layer thickness are 100 μm,
800 DEG C are warming up to according to the system that heating rate is 5 DEG C/min under an argon atmosphere after drying, 1h is kept the temperature, obtains surface and have
The C of anti-deposition antioxidant coatingf/ SiC ceramic matrix composite material component.
Through engines ground test run experimental test, the solids deposition of jet pipe is 0.001mm/s, is had good anti-
Deposition properties.
Embodiment 2
(1) commercially available ZrB is taken2Powder, SiC powder, B2O3Powder, according to ZrB2:SiC:B2O3The volume ratio of=8:3:1 is mixed to get
Powder A；
(2) commercial acid silica solution is taken, is mixed in mass ratio for the ratio of 2:1 with powder A, ball in ball grinder is then placed in
16h is ground, slurry B is obtained；
(3) by Cf/ SiC ceramic matrix composite material component, which is placed in, to be cleaned by ultrasonic in distilled water and is dried for standby in an oven；
(4) spraying process is used, slurry B is sprayed on Cf/ SiC ceramic matrix composite material surface, control coating layer thickness are 150 μm,
800 DEG C are warming up to according to the system that heating rate is 5 DEG C/min under an argon atmosphere after drying, 1h is kept the temperature, obtains surface and have
The C of anti-deposition antioxidant coatingf/ SiC ceramic matrix composite material component.
Embodiment 3
(1) commercially available ZrB is taken2Powder, SiC powder, B2O3Powder, according to ZrB2:SiC:B2O3The volume ratio of=8:2:1 is mixed to get
Powder A；
(2) commercial acid silica solution is taken, is mixed in mass ratio for the ratio of 2:1 with powder A, ball in ball grinder is then placed in
16h is ground, slurry B is obtained；
(3) by Cf/ SiC ceramic matrix composite material component, which is placed in, to be cleaned by ultrasonic in distilled water and is dried for standby in an oven；
(4) spraying process is used, slurry B is sprayed on Cf/ SiC ceramic matrix composite material surface, control coating layer thickness are 100 μm,
900 DEG C are warming up to according to the system that heating rate is 5 DEG C/min under an argon atmosphere after drying, 1h is kept the temperature, obtains surface and have
The C of anti-deposition antioxidant coatingf/ SiC ceramic matrix composite material component.
Embodiment 4
(1) commercially available ZrB is taken2Powder, SiC powder, B2O3Powder, according to ZrB2:SiC:B2O3The volume ratio of=8:3:1 is mixed to get
Powder A；
(2) commercial acid silica solution is taken, is mixed in mass ratio for the ratio of 2:1 with powder A, ball in ball grinder is then placed in
16h is ground, slurry B is obtained；
(3) by Cf/ SiC ceramic matrix composite material component, which is placed in, to be cleaned by ultrasonic in distilled water and is dried for standby in an oven；
(4) spraying process is used, slurry B is sprayed on Cf/ SiC ceramic matrix composite material surface, control coating layer thickness are 200 μm,
900 DEG C are warming up to according to the system that heating rate is 5 DEG C/min under an argon atmosphere after drying, 1h is kept the temperature, obtains surface and have
The C of anti-deposition antioxidant coatingf/ SiC ceramic matrix composite material component.
Embodiment 5
(1) commercially available ZrB is taken2Powder, SiC powder, B2O3Powder, according to ZrB2:SiC:B2O3The volume ratio of=8:2:1 is mixed to get
Powder A；
(2) commercial acid silica solution is taken, is mixed in mass ratio for the ratio of 2:1 with powder A, ball in ball grinder is then placed in
16h is ground, slurry B is obtained；
(3) by Cf/ SiC ceramic matrix composite material component, which is placed in, to be cleaned by ultrasonic in distilled water and is dried for standby in an oven；
(4) spraying process is used, slurry B is sprayed on Cf/ SiC ceramic matrix composite material surface, control coating layer thickness are 200 μm,
800 DEG C are warming up to according to the system that heating rate is 5 DEG C/min under an argon atmosphere after drying, 1.5h is kept the temperature, obtains surface band
There is the C of anti-deposition antioxidant coatingf/ SiC ceramic matrix composite material component.
Claims (4)
1. one kind is used for CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material, it is characterised in that:
(1) coating is by ZrB2、SiC、B2O3It is made with acidic silicasol, wherein ZrB2、SiC、B2O3Volume ratio be 8-
12:2-4:1-2, the quality and ZrB of acidic silicasol2, SiC and B2O3The ratio between gross mass of three is 2-3:1；
(2) preparation method the following steps are included:
A, by the ZrB of proportional quantity2, SiC and B2O3Mix, acidic silicasol is then added, stir evenly be placed in ball grinder into
Row ball milling, obtains slurry；
B, by Cf/ SiC ceramic matrix composite material component, which is placed in distilled water, to be cleaned by ultrasonic, spare after baking oven is dried；
C, slurry obtained in step a is sprayed at Cf/ SiC ceramic matrix composite material component surface, is risen under argon atmosphere after drying
Temperature is simultaneously kept the temperature, and obtains C of the surface with anti-deposition antioxidant coatingf/ SiC ceramic matrix composite material；
Wherein:
Coating layer thickness is 100-200 μm；
Heating rate is 5-10 DEG C/min, and warming temperature is 800-900 DEG C；
Soaking time is 1-1.5h.
2. according to claim 1 be used for CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material, it is characterised in that: ZrB2、
SiC、B2O3Volume ratio be 8:2:1.
3. according to claim 1 be used for CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material, it is characterised in that: ZrB2、
SiC、B2O3Volume ratio be 8:3:1.
4. according to claim 1 be used for CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material, it is characterised in that: ball milling
Time is 12-16h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710495947.8A CN107324847B (en) | 2017-06-26 | 2017-06-26 | For CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710495947.8A CN107324847B (en) | 2017-06-26 | 2017-06-26 | For CfThe anti-deposition antioxidant coating of/SiC ceramic matrix composite material |
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| CN107324847B true CN107324847B (en) | 2019-05-21 |
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| CN109987971A (en) * | 2019-05-09 | 2019-07-09 | 中国科学院金属研究所 | Ceramic Matrix Composites Reinforced by Carbon Fibers surface high temperature long-time antioxidant coating and preparation method thereof |
| CN110028338A (en) * | 2019-05-22 | 2019-07-19 | 山东理工大学 | A kind of ZrB2-SiC-B2O3-SiO2-Zr(H3PO4)2The preparation method of coating |
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| CN101182191B (en) * | 2007-11-15 | 2012-07-04 | 复旦大学 | Method for preparing rear-earth modified zirconium diboride/aluminum oxide composite powder |
| CN102659452B (en) * | 2012-05-31 | 2014-01-01 | 西北有色金属研究院 | Carbon/carbon composite ultra-high-temperature oxidation-resistant coating layer and preparation method thereof |
| CN102674893B (en) * | 2012-05-31 | 2014-03-19 | 西北有色金属研究院 | Ultrahigh-temperature antioxidant coating for carbon/carbon composite material and preparation method of ultrahigh-temperature antioxidant coating |
| CN102674892B (en) * | 2012-05-31 | 2014-03-19 | 西北有色金属研究院 | Carbon/carbon composite ultrahigh temperature anti-oxidation coating and preparation process thereof |
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