CN102432345A - Carbon/carbon composite material silicon-based composite coating capable of resisting high-temperature oxidation for long time, and its preparation method and use - Google Patents
Carbon/carbon composite material silicon-based composite coating capable of resisting high-temperature oxidation for long time, and its preparation method and use Download PDFInfo
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- CN102432345A CN102432345A CN2011102836705A CN201110283670A CN102432345A CN 102432345 A CN102432345 A CN 102432345A CN 2011102836705 A CN2011102836705 A CN 2011102836705A CN 201110283670 A CN201110283670 A CN 201110283670A CN 102432345 A CN102432345 A CN 102432345A
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Abstract
The invention discloses a carbon/carbon composite material silicon-based composite coating capable of resisting high-temperature oxidation for a long time, and its preparation method and use. The carbon/carbon composite material silicon-based composite coating capable of resisting high-temperature oxidation for a long time is characterized in that composite coatings of a SiC connection layer combined with a carbon/carbon composite material matrix and a MoSi2-Si2N2O-CrSi2 ceramic layer are coated on a carbon/carbon composite material surface inside and out, wherein the SiC connection layer has a function of connecting the carbon/carbon composite material matrix and the MoSi2-Si2N2O-CrSi2 ceramic layer has a function of sealing and oxygen blocking. The carbon/carbon composite material silicon-based composite coating capable of resisting high-temperature oxidation for a long time can firmly combine with the carbon/carbon composite material matrix, does not produce penetrating cracks, can resist high-temperature oxidation for a long time, and can be completely utilized for preparation of an aeroengine afterburner material.
Description
Technical field
The present invention relates to a kind of surface treatment of carbon/carbon composite, relate in particular to a kind of novel aeroengine thrust augmentation combustion chamber and substitute superalloy with long-time high-temperature antioxidant silicon base composite coating in carbon/carbon composite surface and methods for making and using same thereof.
Background technology
Carbon/carbon composite is the new type high temperature material of carbon fiber reinforced carbon matrix body, and this material light specific gravity, theoretical density are 2.2g/cm
3Have high-strength modulus, little, the anti-ablation of thermal expansivity, antifatigue, unreactiveness, dimensional stability height; Particularly intensity raises and series of advantages such as rising and high-fracture toughness, low creep with temperature under the high temperature; Be ideal thermal structure and ablation resistant material, be widely used in aerospace field.At present, countries in the world are all with the preferred material of anti-oxidant carbon/carbon composite as the nose cone and the leading edge of space shuttle.Carbon/carbon composite has the heat-stable characteristics of light weight, thereby also is thrust-weight ratio greater than the important equivalent material of 10 aircraft engine hot-end component alloy material.
But be prone to oxidized when carbon/carbon composite uses in the high temperature aerobic environment.Under aerobic conditions, the initial oxidation temperature of carbon/carbon composite is 370 ℃; When being higher than 500 ℃, the rapid oxidation of carbon/carbon composite meeting, and catastrophic explosion takes place.Alloy material is adopted in tradition aeroengine combustor buring chamber more, and the temperature out of combustion chamber has reached 1000 ℃-1500 ℃, if can replace alloy material with carbon/carbon composite, and the weight of mover can alleviate greatly, and then improves the thrust-weight ratio of aircraft.Therefore, the coating carbon/carbon composite of developing a kind of novel long-time high-temperature oxidation resistant replaces high temperature alloy, makes on its after-burner that can be applied in aircraft engine to have great significance.
At the anti-oxidant composite ceramic coat of carbon/carbon composite surface-coated is effective measure.Simultaneously, in order to improve constantly or improve the barrier propterty of ORC, the structure design of coating is progressively developed to the compound coating system by the single coating system, and the silicon based ceramic coating is the most deep ORC system of studying at present.In the silicon based ceramic, the thermal expansivity of SiC and carbon base body are comparatively approaching, and good chemical compatibility is arranged.Adopt entrapping method to prepare the SiC internal layer and have coating and matrix bond is good and cost is low advantage.And the MoSi in the skin
2High temperature toughness and excellent high-temperature oxidation resistance with metal, more than 800 ℃, MoSi
2Surface energy generation one deck is fine and close, continuous, the SiO of self-healing
2Film can stop the entering of oxygen.Cr and Si reaction generate CrSi
2Generate SiO with oxygen reaction with extremely low oxygen permeability
2And Cr
2O
3, and the Cr that is generated
2O
3Can improve SiO
2The high-temperature stability of glass, this compound glass layer not only can stop the intrusion of oxygen effectively but also has high-temperature stability preferably.In addition, under 1100～1500 ℃, Si
3N
4Oxidation rate than little 2～3 one magnitude of SiC, mainly be because Si
3N
4When oxidation, generated and compared SiO
2Si with lower oxygen diffusion rate
2N
2O is with SiO
2Film is compared Si
2N
2The O film has netted more closely coating, thereby to anti-oxidant important effect is arranged.
Goal of the invention
The object of the invention be exactly to the carbon/carbon composite surface ceramic coat because of physics and chemistry match and do not cause being prone to the situation of defectives such as crackle, design and prepare a kind of brand-new firm with matrix bond, the SiC/MoSi of no through-wall crack
2-Si
2N
2O-CrSi
2(from inside to outside) the silicon based ceramic compound coating of long-time resistance to high temperature oxidation, and methods for making and using same.
The objective of the invention is to realize through following manner:
The preparation method of the long-time high-temperature antioxidant silicon base composite coating of a kind of carbon/carbon composite,
Be on the carbon/carbon composite surface, to prepare articulamentum and ceramic coating from inside to outside successively; Described articulamentum is the SiC layer of entrapping method preparation, and described ceramic coating is the MoSi of spread coating and gas-phase reaction method preparation
2-Si
2N
2O-CrSi
2Ceramic layer.
It is with Si powder, Al that described entrapping method prepares articulamentum
2O
3Powder, C powder, the SiC powder is a raw material, and with the carbon/carbon composite embedding, high-temperature calcination gets final product after the milling mixing, and the articulamentum thickness that makes is about 100 μ m-200 μ m.
Concrete steps are following:
According to the quality proportioning be: Si 40-75%, Al
2O
32-13%, C 8-20%, SiC 10-38% take by weighing Si powder, Al
2O
3Powder, C powder, the SiC powder adds dispersion agent, and the dry back of taking-up is for use behind the abundant mixing of ball milling; At last, carbon/carbon composite is placed plumbago crucible, and it is buried fully with the powder of mixing, after crucible is put into High Temperature Furnaces Heating Apparatus, at 1700 ℃-2000 ℃ following insulation 1.5-3h.
Described Si powder, SiC powder, C powder, Al
2O
3All preferred mistake 325 orders of powder.
Described spread coating and gas-phase reaction method prepare MoSi
2-Si
2N
2O-CrSi
2Ceramic layer is at first to take by weighing MoSi
2Powder, Cr powder, Si powder, C powder and acceleration of sintering agent Al
2O
3Mix, selecting deionized water for use is solvent, and Z 150PH is a sticker; The preparation slurry is cleaning up on the also dry good carbon/carbon composite that has the SiC articulamentum drying with the slurry brushing for preparing; Repeating to brush drying process at least 3 times, is with the sample after brushing and drying, under nitrogen atmosphere at last; High temperature sintering is introduced N in the sintering process
2And SiO, utilize gas-phase reaction method to prepare Si
2N
2O, the ceramic layer thickness for preparing are about 100 μ-150 μ m.
Concrete steps are following:
By weight being MoSi
2: Cr: Si: C: Al
2O
3=20-50: 6-20: 30-50: 3-11: 2-10 mixes, and selecting deionized water for use is solvent, and Z 150PH is a sticker, and solid phase mixing powder and sticker proportioning are 1-3g: 20-30ml; The Z 150PH mass concentration is 2～5%; The preparation slurry; The slurry brushing for preparing is being cleaned up on the also dry good carbon/carbon composite that has the SiC articulamentum; Drying repeats to brush dry 3-4 time, is at last the sample after brushing and drying is put into vacuum carbon pipe sintering oven; Under nitrogen atmosphere, 1200 ℃-1600 ℃ insulation 15～80min; Introduce N in the sintering process
2And SiO, utilize gas-phase reaction method to prepare Si
2N
2O.
Described MoSi
2Powder, Cr powder, Si powder, all preferred mistake 325 orders of C powder.
The specific configuration process of described slurry is: in absolute ethyl alcohol, clean beaker with ultrasonic cleaner, magnetic stirring apparatus is subsequent use; Dry beaker and solid material; Take by weighing various raw material powders according to the proportioning that configures and pour in the beaker, on magnetic stirring apparatus, stir 4h at least, mix until powder.
Silica-based compound coating of the present invention is applied to preparation preparation aeroengine thrust augmentation combustor material.
Method of the present invention can prepare the anti-oxidant function compound coating of the C/C matrix material of chemical vapor infiltration and/or liquid impregnation prepared.
The advantage and the positively effect of invention
Compared with prior art, advantage of the present invention and positively effect are embodied in:
(1) entrapping method prepares the effect of SiC articulamentum.Because oxide ceramic coating has higher thermal expansivity and the problem bad with the chemical compatibility of carbon base body, causes supercoat to lose efficacy fast easily.And the thermal expansivity of SiC and carbon base body is comparatively approaching and chemical compatibility is better.Utilize SiC as internal layer, can alleviate the thermal expansion mismatch between top coating and the matrix effectively.In addition, utilizing entrapping method to prepare binder couse, to have technology simple, practices thrift the advantage of cost.The most important thing is that this method can prepare the C-SiC coating with finite concentration gradient, can alleviate the mismatch degree of CTE between coating and the carbon/carbon composite greatly, make the coating sample have excellent thermal shock resistance.
(2) spread coating and gas-phase reaction method prepare MoSi
2-Si
2N
2O-CrSi
2The effect of ceramic coating.The advantage of spread coating be method simply, easily and fast, cost is low, can be easy to prepare the coating system MoSi of design in advance
2And CrSi
2Can be easy to obtain the Si that coating designs in advance through gas-phase reaction method
2N
2The O composition.And these compositions and SiC layer have good chemistry and physical compatibility, and their oxide compound has very excellent resistance oxygen function.
(3) it is firm to have utilized the major advantage of above three kinds of methods to prepare with matrix bond, and no through-wall crack and interlayer crackle have superior thermal shock resistance, can satisfy carbon/carbon composite and under well-oxygenated environment, use for a long time.And above method is easy to apply the surface treatment at large-scale carbon/carbon composite.
Description of drawings
Fig. 1 (a) is the compound coating sectional view for cross section, surface topography and the EDS line sweep result of compound coating of the present invention, is respectively MoSi from left to right
2-Si
2N
2O-CrSi
2Ceramic layer, embedding SiC articulamentum, matrix of carbon/carbon composite materials; (b) be corresponding power spectrum line sweep result, wherein top coating is MoSi
2-Si
2N
2O-CrSi
2Ceramic layer; (c) be MoSi
2-Si
2N
2O-CrSi
2The surface microscopic topographic of layer;
Fig. 2 is MoSi
2-Si
2N
2O-CrSi
2The microscopic appearance of ceramic layer after 1500 ℃ of oxidations;
Fig. 3 is the isothermal oxidation curve of coating sample of the present invention under 1500 ℃, and the coating sample is through 108h, and 1500 ℃ of oxidative mass loss are 1.37%.
Embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1
At first the C/C matrix material is cut into the block sample of 20 * 20 * 5mm, with after the 400# sand papering chamfering with the fine grinding of 800# sand paper, again with down subsequent use behind baking 1～2h after the alcohol wash in 120 ℃;
What then carry out is that embedding treatment prepares the SiC articulamentum:
With Si powder, SiC powder, C powder, Al
2O
3Powder is the mixed powder of feedstock production embedding.The powder quality proportioning is: 50%Si-12%Al
2O
3-18%C-20%SiC.Take by weighing Si powder (crossing 325 orders), the Al of aforementioned proportion
2O
3Powder (cross 325 orders), C powder (crossing 325 orders), SiC powder (crossing 325 orders) is a dispersion agent with ethanol, is placed in the planetary ball mill fully that to take out dry back behind the mixing for use.At last, the C/C matrix material is placed plumbago crucible, and it is buried fully with the powder of mixing, after crucible is put into High Temperature Furnaces Heating Apparatus, from room temperature to 1100 ℃, need 50min; Need 1.5h from 1100 ℃-1800 ℃; 1800 ℃ of insulation 2.5h, argon shield.Be cooling subsequently, need 1h from 1800 ℃ to 1200 ℃.Last furnace cooling.
After the SiC binder couse prepares, in ultrasonic washing instrument, wash the powder that sticks on the coating, and place 100 ℃ of thorough dryings of baking oven to sample with alcohol.
Then be that spread coating and gas-phase reaction method prepare MoSi
2-Si
2N
2O-CrSi
2Outer
At first take by weighing MoSi
2Powder (crossing 325 orders), Cr powder (crossing 325 orders), Si powder (crossing 325 orders), C powder (crossing 325 orders) and a small amount of acceleration of sintering agent (Al
2O
3) the preparation mixed powder, its weight ratio is MoSi
2: Cr: Si: C: Al
2O
3=25: 6: 50: 11: 8.Selecting deionized water for use is solvent, and Z 150PH (PVA) is a sticker, and wherein agglomerant concentration is 2～3%.During the preparation slurry, solid phase mixing powder and sticker proportioning are 1g: 20ml.The specific configuration process of slurry is: in absolute ethyl alcohol, clean beaker with ultrasonic cleaner, the relevant articles for use of experiment such as magnetic stirring apparatus 1.; 2. drying experiment articles for use and test required solid material; 3. take by weighing various powder according to the proportioning that configures and pour in the glass cylinder,, mix until powder stirring more than the 4h on the magnetic stirring apparatus.Then be the coating of precoated layer, the slurry for preparing brushed cleaning up also dry good having on the internally coated carbon/carbon composite of SiC, and insert the baking oven inner drying or the seasoning of 80 ℃ of temperature.In order to obtain certain coat-thickness, repeat this process 3-4 time, then coated precoated layer sample is put into 80 ℃ the dry 12h of loft drier.Be that the sample after brushing and drying is put into vacuum carbon pipe sintering oven at last, under nitrogen atmosphere, 1450 ℃ of insulation 45min.Introduce N in the sintering process
2And SiO, utilize gas-phase reaction method to prepare Si
2N
2O.SiO is through in sintering oven, placing Si powder and SiO
2The reaction of the mixed powder of powder produces, and both mass ratioes are Si: SiO
2=1: 1.Concrete heating process is: from room temperature to 1450 ℃, need 140 minutes, argon shield in the temperature-rise period feeds N in the insulating process
2Gas, insulation is furnace cooling later.
Be anti-oxidant test at last, the compound coating sample is through 108h, anti-oxidant test in 1500 ℃ of air, and coating is kept perfectly, and does not occur coming off, and falls the piece phenomenon, and its oxidative mass loss is merely 1.37%.
Embodiment 2
Adopt 45%Si-10%Al
2O
3-10%C-35%SiC investment prepares the SiC articulamentum; Adopt MoSi
2: Cr: Si: C: Al
2O
3=46: 16: 30: 5: 3 powder proportionings prepare ceramic outer coating, and all the other steps are the same.The coating sample that makes is through 108h, anti-oxidant test in 1500 ℃ of air, and coating is kept perfectly, and does not occur coming off, and its oxidative mass loss is merely 1.05%.
Embodiment 3
Adopt 70%Si-4%Al
2O
3-12%C-14%SiC investment prepares the SiC articulamentum; Adopt MoSi
2: Cr: Si: C: Al
2O
3=35: 10: 45: 6: 4 powder proportionings prepare ceramic outer coating, and all the other steps are the same.The coating sample that makes is through 108h, anti-oxidant test in 1500 ℃ of air, and coating is kept perfectly, and does not occur coming off, and its oxidative mass loss is merely 2.15%.
Claims (10)
1. the preparation method of the long-time high-temperature antioxidant silicon base composite coating of carbon/carbon composite is characterized in that,
Be on the carbon/carbon composite surface, to prepare articulamentum and ceramic coating from inside to outside successively; Described articulamentum is the SiC layer of entrapping method preparation, and described ceramic coating is the MoSi of spread coating and gas-phase reaction method preparation
2-Si
2N
2O-CrSi
2Ceramic layer.
2. preparation method according to claim 1 is characterized in that, it is with Si powder, Al that described entrapping method prepares articulamentum
2O
3Powder, C powder, the SiC powder is a raw material, with the carbon/carbon composite embedding, high-temperature calcination gets final product after the milling mixing.
3. preparation method according to claim 2 is characterized in that, the concrete steps that described entrapping method prepares articulamentum are following:
According to the quality proportioning be: Si 40-75%, Al
2O
32-13%, C 8-20%, SiC 10-38% take by weighing Si powder, Al
2O
3Powder, C powder, the SiC powder adds dispersion agent, and the dry back of taking-up is for use behind the abundant mixing of ball milling; At last, carbon/carbon composite is placed plumbago crucible, and it is buried fully with the powder of mixing, after crucible is put into High Temperature Furnaces Heating Apparatus, at 1700 ℃-2000 ℃ following insulation 1.5-3h.
4. preparation method according to claim 3 is characterized in that, described Si powder, SiC powder, C powder, Al
2O
3Powder is all crossed 325 orders.
5. preparation method according to claim 1 is characterized in that described spread coating and gas-phase reaction method prepare MoSi
2-Si
2N
2O-CrSi
2Ceramic layer is at first to take by weighing MoSi
2Powder, Cr powder, Si powder, C powder and acceleration of sintering agent Al
2O
3Mix, selecting deionized water for use is solvent, and Z 150PH is a sticker; The preparation slurry is cleaning up on the also dry good carbon/carbon composite that has the SiC articulamentum drying with the slurry brushing for preparing; Repeating to brush drying process at least 3 times, is with the sample after brushing and drying, under nitrogen atmosphere at last; High temperature sintering is introduced N in the sintering process
2And SiO, utilize gas-phase reaction method to prepare Si
2N
2O.
6. preparation method according to claim 5 is characterized in that, described spread coating and gas-phase reaction method prepare MoSi
2-Si
2N
2O-CrSi
2The concrete steps of ceramic layer are following:
By weight being MoSi
2: Cr: Si: C: Al
2O
3=20-50: 6-20: 30-50: 3-11: 2-10 mixes, and selecting deionized water for use is solvent, and Z 150PH is a sticker, and solid phase mixing powder and sticker proportioning are 1-3g: 20-30ml; The Z 150PH mass concentration is 2～5%; The preparation slurry; The slurry brushing for preparing is being cleaned up on the also dry good carbon/carbon composite that has the SiC articulamentum; Drying repeats to brush dry 3-4 time, is at last the sample after brushing and drying is put into vacuum carbon pipe sintering oven; Under nitrogen atmosphere, 1200 ℃-1600 ℃ insulation 15～80min; Introduce N in the sintering process
2And SiO, utilize gas-phase reaction method to prepare Si
2N
2O.
7. preparation method according to claim 6 is characterized in that, described MoSi
2Powder, Cr powder, Si powder, C powder are all crossed 325 orders.
8. preparation method according to claim 6 is characterized in that, the specific configuration process of described slurry is: in absolute ethyl alcohol, clean beaker with ultrasonic cleaner, magnetic stirring apparatus is subsequent use; Dry beaker and solid material; Take by weighing various raw material powders according to the proportioning that configures and pour in the beaker, on magnetic stirring apparatus, stir 4h at least, mix until powder.
9. the long-time high-temperature antioxidant silicon base composite coating of carbon/carbon composite is characterized in that, is the silica-based compound coating that is prepared from any described method of claim 1-8.
10. the application method of the described silica-based compound coating of claim 9 is characterized in that, is applied to prepare the aeroengine thrust augmentation combustor material.
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| CN105036801A (en) * | 2015-07-17 | 2015-11-11 | 常州大学 | Carbon/carbon composite material surface high temperature oxidation resistant coating and preparation method thereof |
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