CN101898906B - Preparation method of SiO2-mullite-Al2O3 gradient outer coating for carbon/carbon composite material - Google Patents

Preparation method of SiO2-mullite-Al2O3 gradient outer coating for carbon/carbon composite material Download PDF

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CN101898906B
CN101898906B CN201010198954XA CN201010198954A CN101898906B CN 101898906 B CN101898906 B CN 101898906B CN 201010198954X A CN201010198954X A CN 201010198954XA CN 201010198954 A CN201010198954 A CN 201010198954A CN 101898906 B CN101898906 B CN 101898906B
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黄剑锋
杨强
曹丽云
吴建鹏
曾燮榕
李贺军
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a preparation method of a SiO2-mullite-Al2O3 gradient outer coating for a carbon/carbon composite material, comprising the following steps of: uniformly mixing tetraethoxysilane, absolute alcohol and distilled water to form six mixed solutions, stirring the obtained six solutions by using a magnetic stirrer at normal temperature after respectively regulating the pH values of the six mixed solutions to 2-4, and then dissolving Al(NO3)3.9H2O with the distilled water to obtain six Al(NO3)3 solutions; respectively adding five Al(NO3)3 solutions in the five mixed solutions to finally obtain seven solutions, and respectively lifting a composite material in the seven solution once and then drying to obtain a sample; and carrying out heat insulation on the sample for 2-4h at 1000-1200 DEG C, and then cooling to the room temperature along with a furnace to obtain the carbon/carbon composite material SiO2-mullite-Al2O3 gradient outer coating. The preparation method has the advantages of simple preparation process, convenient operation, easy obtainment of raw materials, short preparation period and low cost. The prepared SiO2-mullite-Al2O3 gradient outer coating has favorable antioxidation and can protect the C/C composite material 135 h in static air of 1500 DEG C, and the oxidation weight loss is only 1.2%.

Description

Carbon/carbon compound material SiO 2-mullite-Al 2O 3The preparation method of gradient top coating
Technical field
The invention belongs to carbon/carbon compound material top coating technical field, be specifically related to a kind of carbon/carbon compound material SiO 2-mullite-Al 2O 3The preparation method of gradient top coating.
Background technology
Carbon/carbon (C/C) matrix material is an advanced composite material hot research fields in the world at present; It has a series of advantage; Low like thermal expansivity, density is low, anti-ablation, corrosion-resistant, stable friction factor, the heat-conductivity conducting performance is good and characteristics such as HS, high-modulus; The characteristic that particularly goes up not down with temperature rising mechanical property makes it become one of preferred material of high-temperature structural material, is widely used in field of aerospace; Especially the nose cone cap and the leading edge of a wing of space shuttle, and the brake facing of ultra sonic etc.As a kind of high-temperature structural material; Its fatal shortcoming is oxidative attack, and promptly under air atmosphere, 450 ℃ just begin oxidation; High temperature is basic has down brought into play not its excellent mechanical property, thereby has limited it as the widespread use of high-temperature refractory under oxidizing atmosphere.Have research to point out that the oxidative mass loss of C/C matrix material is at 1% o'clock, intensity approximately loses 10%.Therefore, the anti-oxidation C/C matrix material key in application that becomes.
At present, the oxidation protection of C/C matrix material is mainly taked following two kinds of different measures: the one, when preparation C/C matrix material, in matrix, add oxidation retarder, i.e. C/C matrix modification method in advance.Its main purpose is to make that C/C matrix itself can antioxidant; The 2nd, prepare the coating of high temperature oxidation resisting at the C/C composite material surface, i.e. ORC method, its essence is that high temperature oxidation resisting coating isolation from oxygen and C/C matrix reach anti-oxidation purpose.Research shows that coating technology is to solve C/C matrix material problem of oxidation valid approach.But single coating is difficult to effectively protect carbon/carbon compound material to avoid oxidation for a long time.At present, coating system is to compound coating system development, mainly with the SiC stupalith that has the good physical chemical compatibility with the C/C matrix as undercoat, have the top coating of good thermal stability, consistency and resistance oxygen ability then in its surface-coated.
Have a variety ofly as the material of top coating, the coating system of the C/C matrix material of having developed mainly contains glass coating [Zhang Weigang, Cheng Huiming, Shen Zuhong; Deng the influence [J] of .TiC, novel charcoal material, 1998,13 (1): 13-18 to C-SiC-B4C matrix material oxidation behavior], metallic coating [Worrell; Wayne L, Lee K N.High temperature alloys, United States Patent; 6127047,2000.], ceramic coating [once mediate banyan, Zheng Changqing; The anti-oxidation research [J] of the .C/C of Li He army matrix material MoSi2 coating. matrix material journal, 1997,14 (3): 37-40] and compound coating [Huang J F; Zeng X R, Li H J, et al.Mullite-Al2O3-SiC oxidation protective coating for carbon/carbon composites [J] .Carbon; 2003,41 (14): 2825-2829.], and compound coating comprises gradient cladding and bilayer and laminated coating etc.
The preparation method of C/C matrix material ORC has a lot, mainly contains entrapping method [Huang J F, LiH J; Zeng X R; Li H J, et al.Influence of the preparing temperature on phase, microstructure and anti-oxidation property of SiC coating for C/C composites [J] .Carbon; 2004; 42 (8-9): 1517-1521.], chemical vapor deposition (CVD) [Cheng L F, Xu YD, Zhang L T; Et al.Preparation of An Oxidation Protection Coating for C/C Composites by Low Pressure Chemical Vapor Deposition [J] .Carbon; 2000, (38): 1493-1498.], molten slurry method [Joshi A.Coating with Particulate Ddispersions for High Temperature Oxidation Protection of Carbon and C/C composites [J] .Composites (Part A), 1997; 28 (2): 181-189], flame plating and plasma spraying method [Cheng Laifei; Zhang Litong. liquid phase method prepares the anti-oxygen of C/C and ends the liquid spreading research [J] of coating. aviation journal, 1996,17 (4): 508-510] etc.These methods or high to equipment requirements, equipment and instrument are relatively more expensive; Preparation technology is relatively harsher, and preparation condition is more extreme; Perhaps complex process, preparation cycle is long, and is repeatable poor.
Summary of the invention
The technical problem that the present invention will solve is: shortcoming and deficiency to prior art exists disclose the carbon/carbon compound material SiO that a kind of technology is simple, preparation cost is low 2-mullite-Al 2O 3The preparation method of gradient top coating, prepared carbon/carbon compound material SiO 2-mullite-Al 2O 3Gradient top coating thickness is even, compact structure, combines closely between the inside and outside coating, and has good materialization consistency.
For achieving the above object, the technical scheme that the present invention adopts is:
1) getting 5ml tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water respectively mixes and processes 6 parts of mixing solutionss; The pH value that in 6 parts of mixing solutionss, adds hydrochloric acid conditioning solution more respectively is 2-4; Stir 1h down with magnetic stirring apparatus normal temperature, make the abundant prehydrolysis of tetraethoxy get 6 parts of solution and count 1#, 2#, 3#, 4#, 5# and 6# solution respectively;
2) Si successively set by step 1): the Al mol ratio is to get analytically pure Al (NO in 3: 1,3: 2,3: 3,2: 3,1: 3 3) 39H 2O obtains 5 parts of Al (NO with the dissolved in distilled water normal temperature magnetic agitation 30-60min of 10-20ml respectively 3) 3Solution is counted 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution respectively, gets the analytically pure Al (NO of 25.00g-26.50g again 3) 39H 2O gets Al (NO with the dissolved in distilled water normal temperature magnetic agitation 30-60min of 10-20ml 3) 3Solution is counted 7# solution;
3) 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution are joined respectively process 5 parts of gradient solutions in 2#, 3#, 4#, 5# and the 6# solution and count 2-2#, 3-2#, 4-2#, 5-2# and 6-2# respectively; With 1#, 2-2#, 3-2#, 4-2#, 5-2#, 6-2# and 7# solution difference normal temperature magnetic agitation 2-4h, in this process, use ammoniacal liquor to regulate its pH value and be 4.5-5.5 again;
4) 7 parts of good ageing of solution 24-48h of reaction; And then place the C/C matrix material that prepares undercoat SiC 1# colloidal sol to lift once; In humidity is 60 ℃ of baking ovens of 60%-80%, dry then, take out the back and in 2-2# colloidal sol, carries out lifting the second time, in humidity is 60 ℃ of baking ovens of 60%-80%, dry then; By that analogy, up to 7 parts of colloidal sols all lift accomplish and dry sample;
5) sample is put into alumina crucible, place retort furnace, it is 5 ℃/min that temperature rise rate is set, and is warming up to 1000-1200 ℃ from room temperature, and insulation 2-4h cools to room temperature then with the furnace and makes carbon/carbon compound material SiO 2-mullite-Al 2O 3The gradient top coating.
SiO in the tetraethoxy of the present invention 2Content more than or equal to 28%.
The pH=10.7 of said ammoniacal liquor.
Top coating of the present invention outwards is according to SiO from the lining 2: Al 2O 3Getting different ratios prepares.SiO 2-mullite-Al 2O 3Gradient cladding uses as the C/C-SiC top coating and has the following advantages: (1) SiO 2Has the function of the defective of packing undercoat SiC at high temperature, like crackle, space etc.And the mullite of outside, aluminum oxide have higher thermostability and antioxidant property, and fusing point can effectively improve the oxidation-resistance of C/C matrix material greater than 1800 ℃.(2) SiO 2-mullite-Al 2O 3The thermal expansivity of gradient cladding and SiC are very approaching, and matching is fine, and are gradient claddings, have eliminated elevated temperature heat stress.This method not only greatly reduces preparation cost, and preparation condition is gentle, technology is simple, preparation cycle is short, and the coating even compact of preparing.The SiO that this method makes 2-mullite-Al 2O 3Gradient cladding uniform in thickness surface flawless.Preparation technology is simple, and is easy to operate, and raw material is easy to get, and preparation cycle is short, and cost is low.The SiO of preparation 2-mullite-Al 2O 3Gradient cladding has good antioxidant property, can be at 1500 ℃ of still airs protection C/C matrix material 135h, and oxidation weight loss only 1.2%.
Description of drawings
The SiO of Fig. 1 embodiment of the invention 1 preparation 2-mullite-Al 2O 3Gradient cladding surface (XRD) collection of illustrative plates, wherein X-coordinate is diffraction angle 2 θ, unit is °; Ordinate zou is a diffraction peak intensity, and unit is a.u;
The SiO of Fig. 2 embodiment of the invention 1 preparation 2-mullite-Al 2O 3ESEM (SEM) photo on gradient cladding surface;
The SiO of Fig. 3 embodiment of the invention 1 preparation 2-mullite-Al 2O 3Section surface sweeping Electronic Speculum (SEM) photo of the SiC-C/C sample of gradient cladding protection.
Embodiment
Embodiment 1:1) gets 5ml SiO respectively 2Content mix more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water and process 6 parts of mixing solutionss; The pH value that in 6 parts of mixing solutionss, adds hydrochloric acid conditioning solution more respectively is 2; Stir 60min down with magnetic stirring apparatus normal temperature, make the abundant prehydrolysis of tetraethoxy get 6 parts of solution and count 1#, 2#, 3#, 4#, 5# and 6# solution respectively;
2) Si successively set by step 1): the Al mol ratio is to get analytically pure Al (NO in 3: 1,3: 2,3: 3,2: 3,1: 3 3) 39H 2O uses the dissolved in distilled water of 10ml respectively, and normal temperature magnetic agitation 30min obtains 5 parts of Al (NO 3) 3Solution is counted 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution respectively, gets the analytically pure Al (NO of 25.00g again 3) 39H 2O is with the dissolved in distilled water of 10ml, and normal temperature magnetic agitation 30min gets Al (NO 3) 3Solution is counted 7# solution;
3) 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution are joined respectively process 5 parts of gradient solutions in 2#, 3#, 4#, 5# and the 6# solution and count 2-2#, 3-2#, 4-2#, 5-2# and 6-2# respectively; With 1#, 2-2#, 3-2#, 4-2#, 5-2# and 6-2# and 7# solution difference normal temperature magnetic agitation 2h, in this process, using ammoniacal liquor to regulate its pH value is 5.5 again;
4) 7 parts of good ageing of solution 24h of reaction; And then place the C/C matrix material that prepares undercoat SiC 1# colloidal sol to lift once; In humidity is 60 ℃ of baking ovens of 60%, dry then, take out the back and in 2-2# colloidal sol, carries out lifting the second time, in humidity is 60 ℃ of baking ovens of 60%, dry then; By that analogy, up to 7 parts of colloidal sols all lift accomplish and dry sample;
5) sample is put into alumina crucible, place retort furnace, it is 5 ℃/min that temperature rise rate is set, and is warming up to 1000 ℃ from room temperature, and insulation 4h cools to room temperature then with the furnace and makes carbon/carbon compound material SiO 2-mullite-Al 2O 3The gradient top coating.
Can know coating by the mullite phase by Fig. 1 combined standard card, silicon-dioxide constitutes with aluminum oxide mutually mutually, relatively meets the thing phase composite of coating, and SiO is described 2-mullite-Al 2O 3Gradient cladding successfully prepares.
As can be seen from Figure 2, coatingsurface is made up of many tiny particulate state crystal grain, and particle is tightly packed, and coating is dense and even.
As can be seen from Figure 3, prepared SiO 2-mullite-Al 2O 3The gradient cladding coat-thickness is greatly about about 37.7 μ m.Whole coat-thickness is even and fine and close, combines between the inside and outside coating closely, does not have phenomenons such as ftractureing and peels off, and this has explained to have good materialization consistency between gradient cladding and the SiC undercoat, and this preparation technology's meliority also has been described simultaneously.
Embodiment 2:
1) gets 5ml SiO respectively 2Content mix more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water and process 6 parts of mixing solutionss; The pH value that in 6 parts of mixing solutionss, adds hydrochloric acid conditioning solution more respectively is 3; Stir 60min down with magnetic stirring apparatus normal temperature, make the abundant prehydrolysis of tetraethoxy get 6 parts of solution and count 1#, 2#, 3#, 4#, 5# and 6# solution respectively;
2) Si successively set by step 1): the Al mol ratio is to get analytically pure Al (NO in 3: 1,3: 2,3: 3,2: 3,1: 3 3) 39H 2O uses the dissolved in distilled water of 13ml respectively, and normal temperature magnetic agitation 30min obtains 5 parts of Al (NO 3) 3Solution is counted 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution respectively, gets the analytically pure Al (NO of 25.50g again 3) 39H 2O is with the dissolved in distilled water of 13ml, and normal temperature magnetic agitation 30min gets Al (NO 3) 3Solution is counted 7# solution;
3) 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution are joined respectively process 5 parts of gradient solutions in 2#, 3#, 4#, 5# and the 6# solution and count 2-2#, 3-2#, 4-2#, 5-2# and 6-2# respectively; With 2h after 1#, 2-2#, 3-2#, 4-2#, 5-2# and 6-2# and the 7# solution difference normal temperature magnetic agitation, in this process, using ammoniacal liquor to regulate its pH value is 5 again;
4) 7 parts of good ageing of solution 36h of reaction; And then place the C/C matrix material that prepares undercoat SiC 1# colloidal sol to lift once; In humidity is 60 ℃ of baking ovens of 80%, dry then, take out the back and in 2-2# colloidal sol, carries out lifting the second time, in humidity is 60 ℃ of baking ovens of 80%, dry then; By that analogy, up to 7 parts of colloidal sols all lift accomplish and dry sample;
5) sample is put into alumina crucible, place retort furnace, it is 5 ℃/min that temperature rise rate is set, and is warming up to 1200 ℃ from room temperature, and insulation 2h cools to room temperature then with the furnace and makes carbon/carbon compound material SiO 2-mullite-Al 2O 3The gradient top coating.
Embodiment 3:
1) gets 5ml SiO respectively 2Content mix more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water and process 6 parts of mixing solutionss; The pH value that in 6 parts of mixing solutionss, adds hydrochloric acid conditioning solution more respectively is 4; Stir 60min down with magnetic stirring apparatus normal temperature, make the abundant prehydrolysis of tetraethoxy get 6 parts of solution and count 1#, 2#, 3#, 4#, 5# and 6# solution respectively;
2) Si successively set by step 1): the Al mol ratio is to get analytically pure Al (NO in 3: 1,3: 2,3: 3,2: 3,1: 3 3) 39H 2O uses the dissolved in distilled water of 17ml respectively, and normal temperature magnetic agitation 30min obtains 5 parts of Al (NO 3) 3Solution is counted 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution respectively, gets the analytically pure Al (NO of 26.00g again 3) 39H 2O is with the dissolved in distilled water of 17ml, and normal temperature magnetic agitation 30min gets Al (NO 3) 3Solution is counted 7# solution;
3) 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution are joined respectively process 5 parts of gradient solutions in 2#, 3#, 4#, 5# and the 6# solution and count 2-2#, 3-2#, 4-2#, 5-2# and 6-2# respectively; With 1#, 2-2#, 3-2#, 4-2#, 5-2# and 6-2# and 7# solution difference normal temperature magnetic agitation 2h, in this process, using ammoniacal liquor to regulate its pH value is 4.5 again;
4) 7 parts of good ageing of solution 42h of reaction; And then place the C/C matrix material that prepares undercoat SiC 1# colloidal sol to lift once; In humidity is 60 ℃ of baking ovens of 70%, dry then, take out the back and in 2-2# colloidal sol, carries out lifting the second time, in humidity is 60 ℃ of baking ovens of 70%, dry then; By that analogy, up to 7 parts of colloidal sols all lift accomplish and dry sample;
5) sample is put into alumina crucible, place retort furnace, it is 5 ℃/min that temperature rise rate is set, and is warming up to 1080 ℃ from room temperature, and insulation 3h cools to room temperature then with the furnace and makes carbon/carbon compound material SiO 2-mullite-Al 2O 3The gradient top coating.
Embodiment 4:1) gets 5ml SiO respectively 2Content mix more than or equal to 28% tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water and process 6 parts of mixing solutionss; The pH value that in 6 parts of mixing solutionss, adds hydrochloric acid conditioning solution more respectively is 3; Stir 60min down with magnetic stirring apparatus normal temperature, make the abundant prehydrolysis of tetraethoxy get 6 parts of solution and count 1#, 2#, 3#, 4#, 5# and 6# solution respectively;
2) Si successively set by step 1): the Al mol ratio is to get analytically pure Al (NO in 3: 1,3: 2,3: 3,2: 3,1: 3 3) 39H 2O uses the dissolved in distilled water of 20ml respectively, and normal temperature magnetic agitation 30min obtains 5 parts of Al (NO 3) 3Solution is counted 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution respectively, gets the analytically pure Al (NO of 26.50g again 3) 39H 2O is with the dissolved in distilled water of 20ml, and normal temperature magnetic agitation 30min gets Al (NO 3) 3Solution is counted 7# solution;
3) 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution are joined respectively process 5 parts of gradient solutions in 2#, 3#, 4#, 5# and the 6# solution and count 2-2#, 3-2#, 4-2#, 5-2# and 6-2# respectively; With 1#, 2-2#, 3-2#, 4-2#, 5-2# and 6-2# and 7# solution difference normal temperature magnetic agitation 3h, in this process, using ammoniacal liquor to regulate its pH value is 5 again;
4) 7 parts of good ageing of solution 48h of reaction; And then place the C/C matrix material that prepares undercoat SiC 1# colloidal sol to lift once; In humidity is 60 ℃ of baking ovens of 65%, dry then, take out the back and in 2-2# colloidal sol, carries out lifting the second time, in humidity is 60 ℃ of baking ovens of 65%, dry then; By that analogy, up to 7 parts of colloidal sols all lift accomplish and dry sample;
5) sample is put into alumina crucible, place retort furnace, it is 5 ℃/min that temperature rise rate is set, and is warming up to 1140 ℃ from room temperature, and insulation 3h cools to room temperature then with the furnace and makes carbon/carbon compound material SiO 2-mullite-Al 2O 3The gradient top coating.

Claims (3)

1. carbon/carbon compound material SiO 2-mullite-Al 2O 3The preparation method of gradient top coating is characterized in that may further comprise the steps:
1) getting 5ml tetraethoxy, 20ml absolute ethyl alcohol and 10ml zero(ppm) water respectively mixes and processes 6 parts of mixing solutionss; The pH value that in 6 parts of mixing solutionss, adds hydrochloric acid conditioning solution more respectively is 2-4, makes the abundant prehydrolysis of tetraethoxy get 6 parts of solution with stirring 1h under the magnetic stirring apparatus normal temperature and counts 1#, 2#, 3#, 4#, 5# and 6# solution respectively;
2) Si successively set by step 1): the Al mol ratio is to get analytically pure Al (NO in 3: 1,3: 2,3: 3,2: 3,1: 3 3) 39H 2After O used the dissolved in distilled water of 10-20ml respectively, normal temperature magnetic agitation 30-60min obtained 5 parts of Al (NO 3) 3Solution is counted 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution respectively, gets the analytically pure Al (NO of 25.00g-26.50g again 3) 39H 2O gets Al (NO with the dissolved in distilled water normal temperature magnetic agitation 30-60min of 10-20ml 3) 3Solution is counted 7# solution;
3) 2-1#, 3-1#, 4-1#, 5-1# and 6-1# solution are joined respectively process 5 parts of gradient solutions in 2#, 3#, 4#, 5# and the 6# solution and count 2-2#, 3-2#, 4-2#, 5-2# and 6-2# respectively; With 1#, 2-2#, 3-2#, 4-2#, 5-2#, 6-2# and 7# solution difference normal temperature magnetic agitation 2-4h, in this process, use ammoniacal liquor to regulate its pH value and be 4.5-5.5 again;
4) 7 parts of good ageing of solution 24-48h of reaction; And then place the C/C matrix material that prepares undercoat SiC 1# colloidal sol to lift once; In humidity is 60 ℃ of baking ovens of 60%-80%, dry then, take out the back and in 2-2# colloidal sol, carries out lifting the second time, in humidity is 60 ℃ of baking ovens of 60%-80%, dry then; By that analogy, up to 7 parts of colloidal sols all lift accomplish and dry sample;
5) sample is put into alumina crucible, place retort furnace, it is 5 ℃/min that temperature rise rate is set, and is warming up to 1000-1200 ℃ from room temperature, and insulation 2-4h cools to room temperature then with the furnace and makes carbon/carbon compound material SiO 2-mullite-Al 2O 3The gradient top coating.
2. carbon/carbon compound material SiO according to claim 1 2-mullite-Al 2O 3The preparation method of gradient top coating is characterized in that: SiO in the said tetraethoxy 2Content more than or equal to 28%.
3. carbon/carbon compound material SiO according to claim 1 2-mullite-Al 2O 3The preparation method of gradient top coating is characterized in that: the pH=10.7 of said ammoniacal liquor.
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CN102992816B (en) * 2012-10-12 2014-04-16 陕西科技大学 Method for preparing carbon/carbon composite material SiC-MoSi2-C-AlPO4 composite gradient external coating
CN103044075B (en) * 2013-01-08 2014-04-16 陕西科技大学 Method for preparing carbon/carbon composite MoSi2-ZrSiO4-SiC gradient complex outer coating
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CN106336248A (en) * 2016-08-22 2017-01-18 陕西科技大学 Preparation method of carbon/carbon composite mullite coating
CN106348786A (en) * 2016-08-22 2017-01-25 陕西科技大学 Preparation method of carbon/carbon composite material mullite coating
US10526253B2 (en) 2016-12-15 2020-01-07 Goodrich Corporation High temperature oxidation protection for composites
US11046619B2 (en) 2018-08-13 2021-06-29 Goodrich Corporation High temperature oxidation protection for composites
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4249913A (en) * 1979-05-21 1981-02-10 United Technologies Corporation Alumina coated silicon carbide abrasive
CN1793017A (en) * 2005-11-22 2006-06-28 武汉理工大学 Mullite whisker-mullite composite coating and preparation process thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4249913A (en) * 1979-05-21 1981-02-10 United Technologies Corporation Alumina coated silicon carbide abrasive
CN1793017A (en) * 2005-11-22 2006-06-28 武汉理工大学 Mullite whisker-mullite composite coating and preparation process thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Huang Jian-Feng et al..Mullite-Al2O3-SiC oxidation protective coating for carbon/carbon composites.《Carbon》.2003,第41卷2825–2829. *
黄剑锋等.国内碳/碳复合材料高温抗氧化涂层研究新进展.《航空材料学报》.2007,第27卷(第2期),74-78. *

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