CN116041090B - Carbon/carbon composite material with silicon nitride ceramic coating and preparation method and application thereof - Google Patents
Carbon/carbon composite material with silicon nitride ceramic coating and preparation method and application thereof Download PDFInfo
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- CN116041090B CN116041090B CN202310040988.3A CN202310040988A CN116041090B CN 116041090 B CN116041090 B CN 116041090B CN 202310040988 A CN202310040988 A CN 202310040988A CN 116041090 B CN116041090 B CN 116041090B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 211
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 211
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 100
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000002131 composite material Substances 0.000 title claims abstract description 97
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 55
- 238000000576 coating method Methods 0.000 claims abstract description 55
- 239000002994 raw material Substances 0.000 claims abstract description 51
- 239000011159 matrix material Substances 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 36
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 58
- 239000005011 phenolic resin Substances 0.000 claims description 58
- 229920001568 phenolic resin Polymers 0.000 claims description 58
- 239000011812 mixed powder Substances 0.000 claims description 41
- 239000000725 suspension Substances 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 33
- 238000009826 distribution Methods 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 244000137852 Petrea volubilis Species 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 239000012298 atmosphere Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 230000035939 shock Effects 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 238000000197 pyrolysis Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 229910010271 silicon carbide Inorganic materials 0.000 description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 13
- 238000004140 cleaning Methods 0.000 description 11
- 238000005498 polishing Methods 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000002679 ablation Methods 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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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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- 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
- C04B41/5066—Silicon nitride
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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)
- Ceramic Products (AREA)
Abstract
The invention relates to a preparation method and application of a carbon/carbon composite material with a silicon nitride ceramic coating. The carbon/carbon composite material with the silicon nitride ceramic coating comprises a carbon/carbon composite material matrix and Si coated on the matrix 3 N 4 A ceramic coating; the silicon nitride ceramic coating comprises the following raw material components in percentage by mass: alpha-Si 3 N 4 50～90％；Al 2 O 3 4～6％；Y 2 O 3 4 to 6 percent; si 0-40%. The silicon nitride ceramic layer is prepared by adopting a coating-pyrolysis and in-situ growth process, and the preparation method comprises the following steps: preparing slurry according to the design components, coating the slurry on the surface of a carbon/carbon composite material matrix, drying, solidifying and placing the carbon/carbon composite material matrix in embedding materials to fire at 1400-1600 ℃ for about 60-180 minutes to obtain a finished product. The invention has simple process, convenient operation, controllable coating thickness, firm and even combination with the matrix, and good thermal shock resistance and oxidation resistance.
Description
Technical Field
The invention belongs to the technical field of surfaces, and particularly relates to a preparation method and application of a carbon/carbon composite material with a silicon nitride ceramic coating.
Background
Carbon fiber reinforced carbon composite materials (carbon/carbon) are considered as one of the important thermal protection materials of high-speed aircrafts due to the characteristics of low density, high specific strength, low thermal expansion coefficient, excellent thermal shock resistance, oxidation resistance, ablation resistance, high-temperature abrasion resistance and the like. However, the carbon/carbon is extremely susceptible to oxidation and ablation in an aerobic environment, which results in gradual material failure, greatly limiting the application of the carbon/carbon composite material, and the preparation of an anti-oxidation coating is considered to be the most effective and direct means for improving the oxidation and ablation performance of the carbon/carbon composite material.
SiC is widely used in matrix modification or oxidation-resistant coating of carbon/carbon composite materials because of its good physicochemical compatibility with carbon/carbon matrix, and has good binding force. However, the difference in thermal expansion coefficient between SiC and carbon/carbon composite materials is large (carbon/carbon is 1 to 2×10 ～6 K, siC 4.5X10 ～6 And K), thermal stress cracks are easy to generate in the high-temperature cyclic use process, so that the oxidation resistance time of SiC is short, and the thermal shock resistance and the ablation capacity cannot meet the requirements. Our previous patentLi [ ZL201710452631.0 ]]The double-layer protection system is provided, wherein the inner layer is a SiC coating, the outer layer is a glass ceramic composite coating, the self-healing effect of the outer layer is used for blocking the entry of oxygen, the defect of the SiC coating is overcome, and the antioxidation time of a sample at 1200 ℃ is greatly improved to 650h. However, considering the complex and severe use environment of carbon, the oxidation temperature resistance, ablation resistance, thermal shock resistance and other performances of the carbon are required to be improved so as to meet the use requirements. In addition, earlier patent [202210401021.9 ]]The HfC-TaC-B4C-SiC (HTBS) high-entropy ceramic material for replacing the SiC coating is excellent in oxidation resistance, thermal shock resistance and ablation resistance, but the binding force of the coating/substrate is still to be improved.
Because SiC ceramics have a good bond with carbon/carbon composites and a large difference in thermal expansion coefficients from the matrix, it is highly desirable to develop new ceramic coatings with a small thermal expansion coefficient and good bond with carbon/carbon.
Disclosure of Invention
Aiming at the problems, the invention provides a carbon/carbon composite material with a silicon nitride ceramic coating, and a preparation method and application thereof. Thermal expansion coefficient of silicon nitride (3.39X10) ～6 and/K) is smaller than silicon carbide, so that the thermal stress between the silicon carbide and the carbon/carbon matrix can be reduced, and the generation of cracks is reduced. Meanwhile, silicon nitride is used as an intermediate layer instead of silicon carbide, and can be densely combined with the matrix and the outer glass ceramic layer, so that the protective performance in the use environment is improved.
In order to achieve the above purpose, the technical scheme of the invention is as follows: a carbon/carbon composite material with a silicon nitride ceramic coating comprises a carbon/carbon composite material matrix and a silicon nitride ceramic coating; the silicon nitride ceramic coating comprises the following raw material components in percentage by mass:
α-Si 3 N 4 50 to 90%, preferably 50 to 60%;
si 0-40%, preferably 30-40%;
Al 2 O 3 3 to 10%, preferably 4 to 6%;
Y 2 O 3 3 to 10%, preferably 4 to 6%.
As a further preferable scheme, the carbon/carbon composite material of the silicon nitride ceramic coating comprises the following raw material components in percentage by mass:
α-Si 3 N 4 90％、Si0％、Al 2 O 3 4％、Y 2 O 3 6％；
or (b)
α-Si 3 N 4 80％、Si10％、Al 2 O 3 4％、Y 2 O 3 6％；
Or (b)
α-Si 3 N 4 70％、Si20％、Al 2 O 3 4％、Y 2 O 3 6％；
Or (b)
α-Si 3 N 4 60％、Si30％、Al 2 O 3 4％、Y 2 O 3 6％；
Or (b)
α-Si 3 N 4 50％、Si40％、Al 2 O 3 4％、Y 2 O 3 6％。
The invention relates to a carbon/carbon composite material with a silicon nitride ceramic coating, wherein the thickness of the silicon nitride ceramic coating is 50-300 microns.
The invention relates to a carbon/carbon composite material with a silicon nitride ceramic coating, wherein the coating contains beta-phase silicon nitride, and the beta-phase silicon nitride is gradually generated in the sintering process. The beta phase silicon nitride content of the coating is about 60-90% (i.e., beta phase silicon nitride is about 60-90% of the total silicon nitride, preferably 65-75%).
The invention relates to a preparation method of a carbon/carbon composite material with a silicon nitride ceramic coating, which is characterized by comprising the following steps:
step 1
Coating an S-SN phenolic resin suspension on a carbon/carbon composite material matrix with a clean and dry surface, then drying at room temperature, and then curing for 1-3 hours at 150-200 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material;
in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:1.8 to 2.5, preferably 1:1.9 to 2.1, more preferably 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after all the raw material powders are taken according to the design components, uniformly mixing to obtain mixed powder, and then mixing the mixed powder with a phenolic resin solution according to the mass ratio of 1:1.8 to 2.5, preferably 1:1.9 to 2.1, more preferably 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass:
α-Si 3 N 4 50 to 90%, preferably 50 to 60%;
si 0-40%, preferably 30-40%;
Al 2 O 3 3 to 10%, preferably 4 to 6%;
Y 2 O 3 3 to 10%, preferably 4 to 6%.
Step 2
Embedding the obtained S-SN precoat sample into embedding materials, and preserving heat for 1-3 hours at 1400-1600 ℃ under a protective atmosphere; cooling to obtain a product with Si 3 N 4 A ceramic coated carbon/carbon composite; the embedding material comprises the following components in percentage by mass;
α-Si 3 N 4 50 to 90%, preferably 50 to 60%;
si 0-40%, preferably 30-40%;
Al 2 O 3 3 to 10%, preferably 4 to 6%;
Y 2 O 3 3 to 10%, preferably 4 to 6%.
The invention relates to a preparation method of a carbon/carbon composite material with a silicon nitride ceramic coating,
in the step 1, a carbon/carbon composite material matrix is polished by sand paper, the edge part is chamfered, and the carbon/carbon composite material matrix is ultrasonically cleaned by absolute ethyl alcohol and dried for standby;
the protective atmosphere in the step 2 is a nitrogen atmosphere.
Preferably, in the step 2, the temperature is kept at 1480-1550 ℃ for 2-3 hours under a protective atmosphere. Further preferably, the temperature is kept at 1490-1520 ℃ for 2-3 hours.
Preferably, according to the preparation method of the carbon/carbon composite material with the silicon nitride ceramic coating, the mixed powder in the step 1 and the embedding material in the step 2 have the same proportion.
The invention relates to a preparation method of a carbon/carbon composite material with a silicon nitride ceramic coating, wherein the particle size distribution of each raw material in mixed powder is 1-10 microns, preferably 1-3 microns.
The invention relates to a preparation method of a carbon/carbon composite material with a silicon nitride ceramic coating, wherein the grain size distribution of each raw material of an embedding material is 1-10 microns, preferably 1-3 microns.
The carbon/carbon composite material with the silicon nitride ceramic coating can effectively protect a carbon/carbon matrix. The beta-phase silicon nitride ceramic coating is gradually generated in the sintering process, is well combined with the carbon/carbon composite material matrix, has no obvious cracks, and has obviously improved fracture toughness and thermal shock resistance.
The invention relates to an application of a carbon/carbon composite material with a silicon nitride ceramic coating, which comprises the steps of using the carbon/carbon composite material with the silicon nitride ceramic coating in medium and low temperature environments; the medium-low temperature environment is an oxygen-containing environment with the temperature of 1200-1500 ℃.
Compared with the prior art, the invention has the following advantages:
1) The prepared silicon nitride coating is well combined with the matrix, a compact silicon nitride layer is arranged at a position close to the matrix, the prepared silicon nitride coating is mainly a beta-phase silicon nitride ceramic coating, the phase has a self-toughening effect, and the silicon nitride coating is endowed with more excellent fracture toughness;
2) The thermal expansion coefficient of beta-phase silicon nitride is 3.39X10 ～6 K is less than 4.5X10 of SiC ～6 The thermal stress between the substrate and the substrate can be reduced, and the generation of cracks is reduced;
3) The coating has strong adaptability to the shape of the matrix, has no special requirement on the shape of the carbon/carbon matrix, has simple preparation process and convenient operation, and can realize large-area industrialized production without shape limitation.
Drawings
Fig. 1 is an XRD pattern of the silicon nitride coated layers prepared in examples 1 to 5.
FIGS. 2 (a) - (b) are surface and cross-sectional scanning electron microscope topography views of the silicon nitride coated surface prepared in example 1.
FIGS. 3 (a) - (b) are surface and cross-sectional scanning electron microscope topography views of the silicon nitride coated surface prepared in example 5.
Fig. 4 is an XRD pattern of the silicon nitride-coated layers prepared in examples 5 to 7.
FIG. 5 is a cross-sectional scanning electron microscope topography of the silicon nitride coated layers prepared in comparative example 3 and comparative example 4; wherein (a) is a profile of a surface scanning electron microscope with a silicon nitride coating prepared in comparative example 3, and (b) is a profile of a cross-section scanning electron microscope with a silicon nitride coating prepared in comparative example 4.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples.
Example 1
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 90％；Al 2 O 3 4％；Y 2 O 3 6％。
Embedding the obtained S-SN precoat sample into an embedding material (the particle size distribution of each raw material in the embedding material is 1-3 microns), and preserving heat for 2h at 1500 ℃ under the protection of nitrogen; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 90％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; from XRD patterns it can be seen that alpha-Si is present in the coating at the same time 3 N 4 And beta-Si 3 N 4 ，β-Si 3 N 4 The main part (the content of beta phase silicon nitride in the coating is about 70%, the beta phase silicon nitride accounts for 70% of the total silicon nitride), but Si 3 N 4 The degree of crystallization of (2) is not good enough.
Detecting the surface and the interface of the sample by using a scanning electron microscope to obtain a scanning electron microscope image, namely obtaining the image 2; as can be seen from FIG. 2, the silicon-free coating has poor crystal growth effect, and the portion close to the C/C matrix does not form a dense layer, and cannot form good bonding with the matrix.
Example 2
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2 mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by massThe components are as follows: alpha-Si 3 N 4 80％；Si 10％；Al 2 O 3 4％；Y 2 O 3 6％。
Embedding the obtained S-SN precoat sample into an embedding material (the particle size distribution of each raw material in the embedding material is 1-3 microns), and preserving heat for 2h at 1500 ℃ under the protection of nitrogen; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 80％；Si 10％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
The sample was detected using an X-ray diffractometer to obtain an XRD diffractogram. As can be seen from XRD patterns, when the silicon content is 10%, the crystallinity of the crystal is good, and the beta-Si 3 N 4 The content increased (the content of beta-phase silicon nitride in the coating was about 80%, i.e., the beta-phase silicon nitride accounted for 80% of the total silicon nitride).
Example 3
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 70％；Si 20％；Al 2 O 3 4％；Y 2 O 3 6％。
Embedding the obtained S-SN precoat sampleIn the embedding material (the grain size distribution of each raw material in the embedding material is 1-3 microns), preserving heat for 2h at 1500 ℃ under the protection of nitrogen; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 70％；Si 20％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
The sample was examined using an X-ray diffractometer to obtain an XRD diffractogram with a content of beta-phase silicon nitride in the coating of about 60%, i.e. 60% of the total silicon nitride.
Example 4
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 60％；Si 30％；Al 2 O 3 4％；Y 2 O 3 6％。
Embedding the obtained S-SN precoat sample into an embedding material (the particle size distribution of each raw material in the embedding material is 1-3 microns), and preserving heat for 2h at 1500 ℃ under the protection of nitrogen; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 60％；Si 30％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; as can be seen from XRD patterns, the silicon content is 30%, and the coating is beta-Si 3 N 4 The content is significantly increased compared with examples 2 and 3 (the content of beta-phase silicon nitride in the coating is about 90%, the beta-phase silicon nitride accounts for 90% of the total silicon nitride), beta-Si 3 N 4 The increase of the content is beneficial to the improvement of the properties such as fracture toughness and the like of the coating.
Example 5
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
Embedding the obtained S-SN precoat sample into an embedding material (the particle size distribution of each raw material in the embedding material is 1-3 microns), and preserving heat for 2h at 1500 ℃ under the protection of nitrogen; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; the content of beta-phase silicon nitride in the coating is about 70%, i.e. the beta-phase silicon nitride accounts for 70% of the total silicon nitride;
detecting the surface and the interface of the sample by using a scanning electron microscope to obtain a scanning electron microscope image, namely obtaining the image 3; as can be seen from FIG. 3, as the silicon content increases, a compact layer of about 20 μm exists at the joint of the coating and the substrate, the bonding force of the coating and the substrate is obviously improved, and the bonding strength of the coating is 5.88MPa. It can also be seen from fig. 3 that a complete, crack-free silicon nitride coating is obtained.
The performance of the product obtained in this example was most excellent during the whole experimental exploration.
Example 6
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
Embedding the obtained S-SN precoat sample into an embedding material (the particle size distribution of each raw material in the embedding material is 1-3 microns), and preserving heat for 2h at 1400 ℃ under the protection of nitrogen; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; compared with example 5, beta-Si in the coating 3 N 4 The content is reduced (the content of beta-phase silicon nitride in the coating is about 60%, i.e. the beta-phase silicon nitride accounts for the total amount of silicon nitride), and the temperature is a main factor affecting the beta-phase content.
Example 7
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
Embedding the obtained S-SN precoat sample into an embedding material (the particle size distribution of each raw material in the embedding material is 1-3 microns), and preserving heat for 2 hours at 1600 ℃ under the nitrogen atmosphere; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
Using X-ray diffractionDetecting the sample by using an ejector to obtain an XRD diffraction pattern; compared with example 5, the coating surface is beta-Si 3 N 4 The content was increased (the content of beta-phase silicon nitride in the coating was about 80%, i.e., the beta-phase silicon nitride accounted for 80% of the total silicon nitride), but the inside of the coating was mainly SiC. The sintering temperature is too high to form a complete coating.
In the foregoing, the protection scope of the present invention is not limited to the simple changes and equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the technical scope of the present invention disclosed in the present invention, and all fall within the protection scope of the present invention.
Comparative example 1
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
The obtained S-SN precoat sample is subjected to heat preservation for 2 hours at 1600 ℃ under the protection of nitrogen; cooling to obtain the carbon/carbon composite material with silicon nitride ceramic coating
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; and detecting the surface and the interface of the sample by using a scanning electron microscope to obtain a scanning electron microscope image. The coating was found to have poor sinter compactness and a small amount of SiC coating was generated on the surface.
Comparative example 2
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
The obtained S-SN precoat sample is subjected to heat preservation for 2 hours at 1500 ℃ under the protection atmosphere of nitrogen; cooling to obtain the carbon/carbon composite material with silicon nitride ceramic coating
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; and detecting the surface and the interface of the sample by using a scanning electron microscope to obtain a scanning electron microscope image. The silicon nitride coating was found to have a number of cracks.
Comparative example 3
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
coating the S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean and dry surface, drying at room temperature, and curing for 3 hours at 160 ℃ in a box-type furnace to form an S-SN precoat on the surface of the carbon/carbon composite material; in the S-SN phenolic resin suspension, the mass ratio of the S-SN powder to the phenolic resin is 1:2;
the S-SN phenolic resin solution is prepared by the following scheme;
after the raw material powders are taken according to the design components, the raw material powders are uniformly mixed to obtain mixed powder (the particle size distribution of the raw materials is 1-3 microns), and then the mixed powder and the phenolic resin solution are mixed according to the mass ratio of 1:2, mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
The obtained S-SN precoat sample is subjected to heat preservation for 2 hours at 1400 ℃ under the protection atmosphere of nitrogen; and cooling to obtain the carbon/carbon composite material with the silicon nitride ceramic coating.
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; the surface and interface of the sample were examined using a scanning electron microscope to obtain a scanning electron microscope image (see fig. 5 a). The coating was found to develop a number of cracks.
Comparative example 4
Polishing the carbon/carbon composite material matrix by sand paper, chamfering the edge part, ultrasonically cleaning by using absolute ethyl alcohol and drying for later use;
placing the carbon/carbon composite material matrix with clean and dry surface into embedding materials (the grain size distribution of each raw material in the embedding materials is 1-3 microns), and preserving heat for 2 hours at 1600 ℃ under the protection of nitrogen; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material comprises the following components in percentage by mass; alpha-Si 3 N 4 50％；Si 40％；Al 2 O 3 4％；Y 2 O 3 6％。
Experimental results
Detecting the sample by using an X-ray diffractometer to obtain an XRD diffraction pattern; scanning electron microscopy was used to detect the surface and interface of the sample to obtain a scanning electron micrograph (see figure 5 b). It was found that the surface of the carbon/carbon matrix embedded alone was not capable of growing a complete silicon nitride coating.
Claims (10)
1. A carbon/carbon composite material with a silicon nitride ceramic coating, characterized by: the carbon/carbon composite material with the silicon nitride ceramic coating comprises a carbon/carbon composite material matrix and a silicon nitride ceramic coating, wherein the silicon nitride ceramic coating is uniformly coated on the carbon/carbon composite material matrix, the coating contains beta-phase silicon nitride, and the beta-phase silicon nitride is gradually generated in the sintering process; the content of beta-phase silicon nitride in the coating is 60-90%;
the carbon/carbon composite material with the silicon nitride ceramic coating is prepared by the following steps:
step 1
Coating an S-SN phenolic resin suspension on a carbon/carbon composite material substrate with a clean surface, then drying at room temperature, and then curing for 1-3 hours at 150-200 ℃ in a box furnace to form an S-SN precoat on the surface of the carbon/carbon composite material;
the S-SN phenolic resin suspension is prepared by the following scheme;
after all the raw material powders are taken according to the design components, uniformly mixing to obtain mixed powder, and then mixing the mixed powder with a phenolic resin solution according to the mass ratio of 1: 1.8-2.5, and mixing to obtain slurry suspension, wherein the mixed powder comprises the following components in percentage by mass: alpha-Si 3 N 4 50~90%；Si0~40%；Al 2 O 3 4~6%；Y 2 O 3 4~6%，
Step 2
Embedding the obtained S-SN precoat sample into an embedding material, and preserving heat for 2-3 hours at 1480-1550 ℃ under a protective atmosphere; cooling to obtain a carbon/carbon composite material with a silicon nitride ceramic coating; the embedding material consists of the following components in percentage by mass; alpha-Si 3 N 4 50~90%；Si0~40%；Al 2 O 3 4~6%；Y 2 O 3 4-6%; the protective atmosphere in the step 2 is nitrogen atmosphere;
the mixed powder in the step 1 and the embedding material in the step 2 have the same proportion.
2. Root of Chinese characterA silicon nitride ceramic coated carbon/carbon composite material according to claim 1, wherein; the silicon nitride ceramic coating comprises the following raw material components in percentage by mass: alpha-Si 3 N 4 50~60%；Si 30~40%；Al 2 O 3 4~6%；Y 2 O 3 4~6%。
3. A silicon nitride ceramic coated carbon/carbon composite material according to claim 1, wherein; the silicon nitride ceramic coating comprises the following raw material components in percentage by mass:
α-Si 3 N 4 90%、Si0%、Al 2 O 3 4%、Y 2 O 3 6%；
or (b)
α-Si 3 N 4 80%、Si10%、Al 2 O 3 4%、Y 2 O 3 6%；
Or (b)
α-Si 3 N 4 70%、Si20%、Al 2 O 3 4%、Y 2 O 3 6%；
Or (b)
α-Si 3 N 4 60%、Si30%、Al 2 O 3 4%、Y 2 O 3 6%；
Or (b)
α-Si 3 N 4 50%、Si40%、Al 2 O 3 4%、Y 2 O 3 6%。
4. A silicon nitride ceramic coated carbon/carbon composite material according to claim 1, wherein: the thickness of the silicon nitride ceramic coating is 50-300 microns.
5. A silicon nitride ceramic coated carbon/carbon composite material according to claim 1, wherein: in the step 1, the carbon/carbon composite material matrix is polished by sand paper, the edge part is chamfered, and the carbon/carbon composite material matrix is ultrasonically cleaned by absolute ethyl alcohol and dried for standby.
6. A silicon nitride ceramic coated carbon/carbon composite material according to claim 1, wherein: the particle size distribution of each raw material in the mixed powder is 1-10 microns.
7. A silicon nitride ceramic coated carbon/carbon composite material according to claim 6, wherein: the particle size distribution of each raw material in the mixed powder is 1-3 microns.
8. A silicon nitride ceramic coated carbon/carbon composite material according to claim 1, wherein: the particle size distribution of each raw material of the embedding material is 1-10 microns.
9. A silicon nitride ceramic coated carbon/carbon composite material according to claim 1, wherein: the particle size distribution of each raw material of the embedding material is 1-3 microns.
10. Use of a carbon/carbon composite material with a silicon nitride ceramic coating according to any one of claims 1 to 5, characterized in that: the application comprises the use of the carbon/carbon composite material with the silicon nitride ceramic coating in medium and low temperature environments; the medium-low temperature environment is an oxygen-containing environment with the temperature of 1200-1500 ℃.
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