CN115231923A - Structure function integrated ceramic matrix composite and preparation method thereof - Google Patents
Structure function integrated ceramic matrix composite and preparation method thereof Download PDFInfo
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- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 76
- 238000000034 method Methods 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 63
- 239000002002 slurry Substances 0.000 claims abstract description 43
- 230000008595 infiltration Effects 0.000 claims abstract description 33
- 238000001764 infiltration Methods 0.000 claims abstract description 33
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 238000004227 thermal cracking Methods 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 18
- 239000004917 carbon fiber Substances 0.000 claims abstract description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011302 mesophase pitch Substances 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 239000004744 fabric Substances 0.000 claims abstract description 15
- 238000000465 moulding Methods 0.000 claims abstract description 15
- 239000004831 Hot glue Substances 0.000 claims abstract description 11
- XTYUEDCPRIMJNG-UHFFFAOYSA-N copper zirconium Chemical compound [Cu].[Zr] XTYUEDCPRIMJNG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 10
- 238000013329 compounding Methods 0.000 claims abstract description 8
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- 239000000758 substrate Substances 0.000 claims abstract description 4
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
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- 239000000126 substance Substances 0.000 claims description 10
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- 238000002679 ablation Methods 0.000 abstract description 4
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- 229910026551 ZrC Inorganic materials 0.000 description 8
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 8
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- XABJJJZIQNZSIM-UHFFFAOYSA-N azane;phenol Chemical compound [NH4+].[O-]C1=CC=CC=C1 XABJJJZIQNZSIM-UHFFFAOYSA-N 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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Abstract
The invention discloses a structure-function integrated ceramic matrix composite and a preparation method thereof, relating to the technical field of composite materials, wherein ceramic powder and mesophase asphalt solution are mixed to prepare slurry; compounding the slurry and the high-thermal-conductivity carbon fiber cloth by adopting a hot melt adhesive membrane method to obtain a prepreg; stacking prepreg layers and preparing a molding flat plate; carrying out thermal cracking on the mould pressing flat plate to obtain a carbon/carbon blank; processing the carbon/carbon blank to obtain the carbon/carbon blank with a carbon interface layer and a carbon substrate; covering the zirconium-copper alloy powder on a carbon/carbon blank, and preparing the ceramic matrix composite by adopting a reaction infiltration method; the ceramic-based composite material is brushed, dried and treated at high temperature by adopting the mixed slurry of the ceramic powder and the mesophase pitch to obtain a ceramic coating, so that the structure-function integrated ceramic-based composite material is obtained, and the material has high-temperature resistance and ablation resistance.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a structure function integrated ceramic matrix composite material and a preparation method thereof.
Background
The ceramic matrix composite with the integrated structure and function has a series of excellent performances such as high heat conduction, high temperature resistance and ablation resistance, and has a wide application prospect in the field of aerospace. The preparation process of the ultrahigh-temperature ceramic is generally a precursor impregnation-pyrolysis method and a slurry method. The structure-function integrated ceramic matrix composite prepared by the precursor impregnation-cracking method has excellent mechanical and ablation resistance, but the preparation period is relatively long, and the risk of grain growth exists in the internal ceramic in multiple high-temperature cracking processes. The slurry method is to prepare slurry with a certain proportion by adopting ultrahigh-temperature ceramic powder, resin or ceramic precursor solution and the like, and then prepare the structure-function integrated ceramic matrix composite by adopting a dipping or hot pressing process. Due to the fact that the density of the ultrahigh-temperature ceramic powder is high, the phenomena of closed pores, crusting and the like which influence the dipping effect are easily formed in the dipping process, and the material density is low, so that the performance of the material is influenced.
In recent years, ultra-high temperature ceramic powder is adopted to prepare slurry liquid, then a painting process is adopted to paint carbon cloth, then a mould pressing process is adopted to prepare a composite material flat plate, and the flat plate is subjected to reaction infiltration after cracking to obtain the ceramic matrix composite with integrated structure and function. The process has the advantages of small grain size, controllable addition amount and short preparation period in the ultrahigh-temperature ceramic matrix.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a structure function integrated ceramic matrix composite and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a structure-function integrated ceramic matrix composite comprises the following steps:
1) Mixing the ceramic powder and the mesophase pitch solution to prepare slurry;
2) Compounding the slurry and the high-thermal-conductivity carbon fiber cloth by adopting a hot melt adhesive membrane method to obtain a prepreg;
3) Laying and stacking prepreg layers and preparing a molding flat plate; carrying out thermal cracking on the mould pressing flat plate to obtain a carbon/carbon blank;
4) Processing the carbon/carbon blank to obtain a carbon/carbon blank with a carbon interface layer and a carbon matrix;
5) Covering the zirconium-copper alloy powder on a carbon/carbon blank, and preparing the ceramic matrix composite by adopting a reaction infiltration method;
6) The ceramic powder and the mesophase pitch are mixed with the slurry, and the ceramic coating is obtained after the ceramic matrix composite is brushed, dried and treated at high temperature, so that the structure and function integrated ceramic matrix composite is obtained.
Preferably, the mesophase pitch solution in step 1) is selected from any one or more of coal pitch and petroleum pitch, preferably petroleum mesophase pitch; the ceramic powder is selected from superhigh temperature ceramic including HfC and HfB 2 、ZrC、ZrB 2 、TaC、TaB 2 And the like.
Preferably, the mass ratio of the ceramic powder in the slurry in the step 1) is 20-50%.
Preferably, the thermal conductivity of the carbon fiber cloth in the high-thermal-conductivity carbon fiber cloth in the step 2) is more than or equal to 650W/m.K, and the slurry accounts for 40-70% of the mass percentage of the prepreg.
Preferably, when the molding flat plate is prepared in the step 3), the fiber volume fraction of the molding flat plate is 30-50% through ply numerical control molding;
preferably, the molded flat plate is prepared by a molding process, and the molding process conditions include: the pressurizing temperature is 100-150 ℃, the pressure range is 8-22 MPa, the curing temperature is 260-300 ℃, and the heat preservation time is 3-5 h.
Preferably, the thermal cracking in step 3) is performed under an inert atmosphere, and the process conditions of the thermal cracking are as follows: the heating rate is 0.5-2 ℃/min, and the thermal cracking temperature is 600-1000 ℃.
Preferably, the carbon fiber preform is processed in step 4) by using a chemical vapor infiltration process, wherein the process conditions of the chemical vapor infiltration process include: the deposition temperature is 900-1150 ℃; the furnace pressure is controlled to be 2-10 kPa.
Preferably, the density of the carbon/carbon blank after deposition in step 4) is 1.4 to 1.8g/cm 3 。
Preferably, in the step 5), the molar fraction of the zirconium powder in the zirconium-copper alloy powder is 50-70%, the mass ratio of the alloy powder to the carbon/carbon matrix is (2-5): 1, the infiltration temperature is 1000-1200 ℃, and the heat preservation time is 0.5-2 h.
Preferably, the drying temperature in the step 6) is 100-150 ℃, and the drying time is 2-4 h; the high-temperature treatment temperature is 600-1000 ℃, and the treatment time is 2-4 h; the thickness of the coating ranges from 10 to 20 mu m.
A structure function integrated ceramic matrix composite is prepared by the method.
Compared with the prior art, the invention has the following advantages:
(1) The high-heat-conductivity C/C green body is prepared by adopting the ultrahigh-temperature ceramic powder prepreg, the adding amount of the ultrahigh-temperature ceramic powder is controllable, the period and the cost are reduced, and the high-temperature resistance and ablation resistance of the material are improved;
(2) The invention adopts zirconium-copper alloy to carry out reaction infiltration on the pitch fiber prefabricated blank. In reactive infiltration, it is generally desirable that the metal melt infiltrates to react with the carbon matrix in the body, rather than with the carbon fibers. According to the zirconium-copper binary phase diagram, the melting point of zirconium is about 1855 ℃, if zirconium is completely melted and permeates into a C/C blank to react independently, the temperature needs to reach at least 1900 ℃, zirconium is taken as an active metal element and can rapidly react with a carbon matrix and asphalt fibers at the temperature of above 1900 ℃, the asphalt fibers are damaged, the performance of the composite material is further reduced, and the material preparation is difficult to succeed. The invention innovatively introduces elements with high thermal conductivity of a second phase and low melting point, so that the reaction infiltration temperature can be reduced, the cost and the preparation period are reduced, the pitch-based carbon fiber is protected, the thermal conductivity of the composite material can be further improved, and the thermal management efficiency is improved. According to the phaseAs shown, the melting point of copper is about 1085 ℃ and the thermal conductivity is about 400W/mK. Binary compounds of zirconium and copper, e.g. CuZr, having a melting point of about 935℃, cuZr 2 The melting point of the copper is about 1002 ℃, which shows that the reaction infiltration temperature can be obviously reduced to 1000-1200 ℃ by adding a certain proportion of copper, and the CuZr generated at high temperature 2 And various melts such as Cu and the like can permeate into the C/C blank body and react with the carbon matrix, so that the process window is widened, the corrosion of the infiltration process on the carbon fiber is effectively reduced, and the comprehensive performance of the composite material is improved. Through research, the molar fraction of zirconium in the zirconium-copper alloy powder is 50% -70%, if the content of zirconium is too high, the melting temperature is rapidly increased, the reaction infiltration difficulty is increased, and if the content of zirconium is too low, the content of ultrahigh-temperature zirconium carbide generated after the reaction infiltration is lower, the reaction is insufficient, and the porosity is higher; the mass ratio of the alloy powder to the C/C blank is 2-5, if the ratio of the alloy powder is too high, powder is wasted, the composite material is difficult to take out after reaction infiltration, and if the ratio is too low, incomplete reaction is caused, and the performance of the composite material is reduced.
Drawings
FIG. 1 shows a scanning electron micrograph of a fracture of a composite material obtained in example 1 of the present invention after bending.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a preparation method of a structure-function integrated ceramic matrix composite, which comprises the following steps:
(1) Mixing the ceramic powder and the mesophase pitch solution to prepare slurry;
in some preferred embodimentsThe mesophase pitch solution is selected from any one or more of coal pitch and petroleum pitch, and is preferably petroleum mesophase pitch; the ceramic powder is selected from ultra-high temperature ceramic including HfC and HfB 2 、ZrC、ZrB 2 、TaC、TaB 2 And the like.
The concentration of the slurry (i.e., the mass percentage of the ceramic powder in the slurry) is preferably 20% to 50% in the present invention, and may be any value (inclusive) within this range, for example, 20%, 25%, 30%, 35%, 40%, 45%, 50%. The powder adding proportion is too high, the viscosity of the ceramic powder slurry is too high, and the ceramic powder slurry is not suitable for preparing a glue film; meanwhile, because the content of the powder is higher, the bonding between flat plate layers after mould pressing is poorer, and the layering is easy. The proportion addition is too low to achieve the ceramic powder addition expectations. It can be seen that the maximum addition amount of the ceramic powder in the technical scheme of the invention can reach 50%.
(2) Compounding the slurry and the high-thermal-conductivity carbon fiber cloth by adopting a hot melt adhesive membrane method to obtain a prepreg;
the invention adopts a hot melt adhesive film method for compounding to prepare the prepreg. The hot melt adhesive film method specifically comprises the following steps: firstly, preparing the sizing agent into a glue film, then compounding the glue film on the surface of the carbon cloth, heating and pressurizing to melt the glue film, and immersing the carbon cloth. The process conditions of the hot melt adhesive film method are not specifically limited, and the method belongs to the conventional technology, and the prior technical scheme can be referred. However, the content of the slurry in the prepreg to be produced is limited in the present invention, and is preferably 40 to 70% (mass percentage content), and may be any value (inclusive) within this range, for example, 40%, 45%, 50%, 55%, 60%, 65%, 70%.
(3) Laying and stacking prepreg layers and preparing a molding flat plate; carrying out thermal cracking on the mould pressing flat plate to obtain a carbon/carbon blank;
in preparing the molding plate, the fiber volume fraction of the molding plate may be 30% to 55%, for example, 30%, 35%, 40%, 45%, 50%, 55% by ply numerical control molding.
The invention preferably adopts a mould pressing process to prepare the mould pressing flat plate, and the process conditions of the mould pressing process are as follows:
the pressurization temperature is 100 to 150 ℃, for example, 100 ℃, 110 ℃, 120 ℃,130 ℃, 140 ℃,150 ℃;
the pressure range is 8 to 22MPa, for example, 8MPa, 12MPa, 16MPa, 20MPa, 22MPa;
the curing temperature is 260 to 300 ℃, for example, 260 ℃, 280 ℃ and 300 ℃;
the holding time is 3 to 5 hours, for example, 3 hours, 4 hours, or 5 hours.
For the thermal cracking process, the present invention preferably performs the thermal cracking under an inert atmosphere (preferably nitrogen or argon) under the following process conditions:
the heating rate is 0.5-2 deg.C/min, preferably 1 deg.C/min to avoid deformation and cracking of the product, and the thermal cracking temperature is 600-1000 deg.C (such as 600 deg.C, 700 deg.C, 800 deg.C, 900 deg.C, 1000 deg.C).
(4) Processing the carbon/carbon blank to obtain a carbon/carbon blank with a carbon interface layer and a matrix;
in this step, the present invention preferably uses a chemical vapor infiltration process to treat the carbon/carbon blank, wherein the process conditions of the chemical vapor infiltration process are as follows:
the deposition temperature is 900 to 1150 ℃, for example, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃;
the furnace pressure is controlled to be 2 to 10kPa, and may be, for example, 2kPa, 3kPa, 4kPa, 5kPa, 6kPa, 7kPa, 8kPa, 9kPa, or 10kPa.
The density of the carbon/carbon blank after deposition is 1.4-1.8 g/cm 3 For example, it may be 1.4g/cm 3 、1.5g/cm 3 、1.6g/cm 3 、1.7g/cm 3 、1.8g/cm 3 .
(5) Covering a carbon/carbon matrix with zirconium-copper alloy powder, and obtaining the structure-function integrated ceramic matrix composite by adopting a reaction infiltration method.
The reactive infiltration can be referred to the prior art, for example, by using a graphite crucible as a reaction vessel and performing a high-temperature treatment using a high-temperature furnace. Preferably, however, the reactive infiltration treatment is performed such that the molar fraction of zirconium powder in the zirconium-copper alloy powder is 50% to 70% (for example, 50%, 55%, 60%, 65%, 70% is acceptable), and the mass ratio of the alloy powder to the C/C compact is 2 to 5:1 (for example, 2, 3, 4 or 5), a infiltration temperature of 1000 to 1200 ℃ (for example, 1000 ℃, 1050 ℃, 1100 ℃ or 1200 ℃), and a holding time of 0.5 to 2 hours (for example, 0.5 hour, 1 hour, 1.5 hours or 2 hours).
(6) The ceramic coating is obtained by brushing, drying and high-temperature treatment of mixed slurry of ceramic powder and mesophase pitch, and the ceramic matrix composite with the structure and function integrated is finally obtained. The drying temperature is 100-150 ℃ (100 ℃, 110 ℃, 120 ℃,130 ℃, 140 ℃ and 150 ℃), and the drying time is 2-4 h (2 h, 3h and 4 h); the high-temperature treatment temperature is 600-1000 ℃ (600 ℃, 800 ℃ and 1000 ℃), and the treatment time is 2-4 h (2 h, 3h and 4 h); the thickness of the prepared coating ranges from 10 to 20 mu m.
In the preparation method provided by the present invention, the detailed description of the present invention is not given to the known techniques of those skilled in the art.
The invention also provides a structure function integrated ceramic matrix composite material prepared by the preparation method provided by the invention.
The following are examples of the present invention.
Example 1
In this embodiment, a structure-function integrated ceramic matrix composite is prepared by the method provided by the invention:
(1) Preparing slurry: the intermediate phase asphalt solution is blended with the ultra-high temperature ceramic powder HfC powder to prepare the slurry, wherein the ultra-high temperature ceramic powder HfC powder accounts for 45% of the mass of the slurry.
(2) Preparing a prepreg: the intermediate phase asphalt slurry is adopted, a hot melt adhesive membrane method is adopted, and the intermediate phase asphalt slurry and the high-thermal-conductivity carbon cloth are compounded to prepare the ultrahigh-temperature ceramic powder prepreg, wherein the mass content of the slurry is 60%.
(3) Preparing a low-density carbon/carbon blank: the composite material is prepared by adopting a die pressing process, wherein the volume fraction of the flat fiber is controlled to be 45% by the ply number, the pressurizing temperature is controlled to be 120 ℃, the pressure is 10MPa, the curing temperature is 280 ℃, and the heat preservation time is 3 hours.
And carrying out thermal cracking on the mould pressing flat plate, wherein the thermal cracking is carried out in a nitrogen atmosphere, the heating rate is 1 ℃/min, and the thermal cracking treatment temperature is 800 ℃.
(4) Preparing a carbon interface layer and a matrix: preparing an interface layer and a carbon part matrix by chemical vapor infiltration, wherein the deposition temperature is 1100 ℃, the furnace pressure is controlled to be 5kPa, and the density of a blank body after deposition is 1.6g/cm 3 。
(5) And (3) reaction infiltration: placing the carbon fiber blank in a graphite crucible, covering with alloy powder of which the molar fraction is 65% of zirconium and 35% of copper, wherein the mass ratio of the alloy powder to the blank is 3.
(6) And (2) brushing the slurry obtained in the step (1), drying at 130 ℃ for 4h and performing high-temperature treatment at 600 ℃ for 3h to obtain the ceramic matrix composite with integrated structure and function.
Through detection, the porosity of the structure-function integrated ceramic matrix composite is 2.7%, the bending strength is 285MPa, and the in-plane thermal conductivity is 287W/m.K.
Example 2
In this embodiment, a structure-function integrated ceramic matrix composite is prepared by the method provided by the invention:
(1) Preparing slurry: the slurry is prepared by blending mesophase pitch solution and ultrahigh-temperature ceramic powder ZrC powder, wherein the mass percent of the ultrahigh-temperature ceramic powder ZrC powder in the slurry is 50%.
(2) Preparing a prepreg: the intermediate phase asphalt slurry is adopted, a hot melt adhesive membrane method is adopted, and the intermediate phase asphalt slurry and the high-thermal-conductivity carbon cloth are compounded to prepare the ultrahigh-temperature ceramic powder prepreg, wherein the mass content of the slurry is 70%.
(3) Preparing a low-density carbon/carbon blank: the preparation method is characterized in that the preparation method adopts a die pressing process, the volume fraction of the flat fiber is 30% through the ply number, the pressurizing temperature is controlled to be 100 ℃, the pressure is 8MPa, the curing temperature is 260 ℃, and the heat preservation time is 4h.
And carrying out thermal cracking on the mould pressing flat plate, wherein the thermal cracking is carried out in a nitrogen atmosphere, the heating rate is 0.5 ℃/min, and the thermal cracking treatment temperature is 600 ℃.
(4) Preparing a carbon interface layer and a matrix: preparing an interface layer and a carbon part matrix by adopting chemical vapor infiltration, wherein the deposition temperature is 900 ℃, the furnace pressure is controlled to be 2kPa, and the density of a blank body after deposition is 1.4g/cm 3 。
(5) And (3) reaction infiltration: placing the carbon fiber blank in a graphite crucible, covering by using alloy powder with the molar fraction of 50% zirconium and 50% copper, wherein the mass ratio of the alloy powder to the blank is 2.
(6) And (3) brushing the slurry obtained in the step (1), drying at 100 ℃ for 3h and performing high-temperature treatment at 800 ℃ for 2h to obtain the structure-function integrated ceramic matrix composite.
The porosity of the composite material is 3.5%, the bending strength is 267MPa, and the in-plane thermal conductivity is 274W/m.K.
Example 3
In this embodiment, a ceramic matrix composite with integrated structure and function is prepared by the method provided by the present invention:
(1) Preparing slurry: the intermediate phase asphalt solution is blended with the ultra-high temperature ceramic powder HfC and ZrC to prepare the slurry, wherein the ultra-high temperature ceramic powder HfC and ZrC accounts for 20% of the mass of the slurry.
(2) Preparing a prepreg: the ultrahigh-temperature ceramic powder prepreg is prepared by compounding mesophase asphalt slurry and high-thermal-conductivity carbon cloth by adopting a hot melt adhesive membrane method, wherein the mass content of the slurry is 40%.
(3) Preparing a low-density carbon/carbon blank: the composite material is prepared by adopting a die pressing process, the volume fraction of the flat fiber is controlled to be 50% by the ply number, the pressurizing temperature is controlled to be 150 ℃, the pressure is 22MPa, the curing temperature is 300 ℃, and the heat preservation time is 5 hours.
And carrying out thermal cracking on the mould pressing flat plate, wherein the thermal cracking is carried out in a nitrogen atmosphere, the heating rate is 2 ℃/min, and the thermal cracking treatment temperature is 1000 ℃.
(4) Preparation of carbonInterface layer and base body: preparing an interface layer and a carbon part matrix by adopting chemical vapor infiltration, wherein the deposition temperature is 1150 ℃, the furnace pressure is controlled to be 10kPa, and the density of a blank body after deposition is 1.8g/cm 3 。
(5) Reaction infiltration: placing the carbon fiber blank in a graphite crucible, covering with alloy powder of 70% of zirconium and 30% of copper in molar fraction, wherein the mass ratio of the alloy powder to the blank is 5.
(6) And (3) brushing the slurry obtained in the step (1), drying at 150 ℃ for 2h and treating at 1000 ℃ for 4h to obtain the structure-function integrated ceramic matrix composite.
The porosity of the composite material was 3.7%, the bending strength was 261MPa, and the in-plane thermal conductivity was 259W/m.K.
Example 4
Example 4 is essentially the same as example 1, except that:
example 4 when the low-density carbon/carbon green body is prepared in step (3), a mold pressing process is adopted to prepare the low-density carbon/carbon green body, the volume fraction of the flat fiber is controlled to be 40% by the ply number, the pressurization temperature is controlled to be 100 ℃, the pressure is 15MPa, the curing temperature is 260 ℃, and the heat preservation time is 4 hours.
The porosity of the composite material is 3.0%, the bending strength is 280MPa, and the in-plane thermal conductivity is 277W/m.K.
Example 5
Example 5 is essentially the same as example 1, except that:
example 5 in the step (4) of preparing the carbon interface layer and the carbon substrate, chemical vapor infiltration was used to prepare the interface layer and the carbon substrate, the deposition temperature was 1050 ℃, the furnace pressure was controlled at 7kPa, and the density of the green body after deposition was 1.4g/cm 3 。
The porosity of the composite material is 4.1%, the bending strength is 207MPa, and the in-plane thermal conductivity is 213W/m.K.
Example 6
Example 6 is essentially the same as example 1, except that:
example 6 when the reaction infiltration is performed in the step (5), a carbon fiber blank is placed in a graphite crucible, and is covered with an alloy powder of 50% zirconium and 50% copper by mole, the mass ratio of the alloy powder to the blank is 4.
The porosity of the composite material is 4.5%, the bending strength is 195MPa, and the in-plane thermal conductivity is 235W/m.K.
The test performance of the composite material product prepared in example 1 of examples 1 to 6 is the best, because the inventor finally finds the best parameter combination through multiple experimental comparisons and deep analysis of the test structure, and the best composite material can be prepared by using the parameter combination.
Comparative example 1
Comparative example 1 was conducted in substantially the same manner as in example 1 except that:
comparative example 1 when the prepreg was prepared in step (1), an ammonia phenol solution was used to prepare a slurry by blending with the ultrahigh-temperature ceramic powder ZrC powder. When the prepreg is prepared in the step (2), a hot melt adhesive membrane method is adopted to prepare the ultrahigh-temperature ceramic powder prepreg by compounding with polyacrylonitrile-based carbon cloth, wherein the mass content of the slurry is 50%.
The porosity of the composite material is 3.0%, the bending strength is 243MPa, and the in-plane thermal conductivity is 32W/m.K.
As can be seen from the test results of the composite products prepared in comparative example 1 and comparative example 1, the thermal conductivity of the product in example 1 is much higher than that in comparative example 1, because the mesophase pitch solution and the mesophase pitch slurry are used in example 1, which can effectively improve the thermal conductivity of the composite product.
Comparative example 2
Comparative example 2 was conducted in substantially the same manner as in example 1 except that:
comparative example 2 when the reaction infiltration is performed in the step (5), the carbon fiber blank is placed in a graphite crucible, only single zirconium powder is used for covering, the graphite crucible is placed in a high-temperature furnace, the temperature is raised to 1900 ℃, and the temperature is maintained for 2 hours, so that the ceramic matrix composite is obtained.
The porosity of the composite material is 11.3%, the bending strength is 92MPa, and the in-plane thermal conductivity is 112W/m.K.
As can be seen from the results of comparing the composite products prepared in example 1 and comparative example 2, the flexural strength and thermal conductivity of the product prepared in example 1 are much higher than those of the product prepared in comparative example 2, because the zirconium-copper alloy is adopted in example 1, which can effectively improve the overall performance of the composite product.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a structure-function integrated ceramic matrix composite is characterized by comprising the following steps:
1) Mixing ceramic powder and a mesophase pitch solution to prepare slurry;
2) Compounding the slurry and the high-thermal-conductivity carbon fiber cloth by adopting a hot melt adhesive membrane method to obtain a prepreg;
3) Stacking prepreg layers and preparing a molding flat plate; carrying out thermal cracking on the mould pressing flat plate to obtain a carbon/carbon blank;
4) Processing the carbon/carbon blank to obtain the carbon/carbon blank with a carbon interface layer and a carbon substrate;
5) Covering the zirconium-copper alloy powder on a carbon/carbon blank, and preparing the ceramic matrix composite by adopting a reaction infiltration method;
6) The ceramic powder and the mesophase pitch mixed slurry are adopted to brush, dry and treat the ceramic matrix composite at high temperature to obtain a ceramic coating, and the structure-function integrated ceramic matrix composite is obtained.
2. The method of claim 1, wherein the mesophase pitch solution in step 1) is selected from any one or more of coal pitch, petroleum pitch, preferably petroleum mesophase pitch; the ceramic powder is selected from superhigh temperature ceramic including HfC and HfB 2 、ZrC、ZrB 2 、TaC、TaB 2 And the like; the mass percentage of the ceramic powder in the slurry is 20-50%.
3. The method as claimed in claim 1, wherein the thermal conductivity of the carbon fiber cloth in the high thermal conductivity carbon fiber cloth in the step 2) is more than or equal to 650W/m.K, and the slurry accounts for 40-70% of the mass percent of the prepreg.
4. The method of claim 1, wherein in the step 3) of preparing the molding plate, the fiber volume fraction of the molding plate is 30% to 50% by ply number molding; preparing a mould pressing flat plate by adopting a mould pressing process, wherein the conditions of the mould pressing process comprise: the pressurizing temperature is 100-150 ℃, the pressure range is 8-22 MPa, the curing temperature is 260-300 ℃, and the heat preservation time is 3-5 h.
5. The method of claim 1, wherein the thermal cracking in step 3) is performed under an inert atmosphere, and the thermal cracking process conditions are as follows: the heating rate is 0.5-2 ℃/min, and the thermal cracking temperature is 600-1000 ℃.
6. The method according to claim 1, wherein the carbon fiber preform is treated in the step 4) by a chemical vapor infiltration process, wherein the process conditions of the chemical vapor infiltration process include: the deposition temperature is 900-1150 ℃; the furnace pressure is controlled to be 2-10 kPa.
7. The method of claim 1, wherein the density of the carbon/carbon body after deposition in step 4) is from 1.4 to 1.8g/cm 3 。
8. The method according to claim 1, wherein the molar fraction of zirconium powder in the zirconium-copper alloy powder in the step 5) is 50 to 70%, the mass ratio of the alloy powder to the carbon/carbon matrix is (2 to 5): 1, the infiltration temperature is 1000 to 1200 ℃, and the holding time is 0.5 to 2 hours.
9. The method of claim 1, wherein the drying temperature in step 6) is 100-150 ℃ and the drying time is 2-4 h; the high-temperature treatment temperature is 600-1000 ℃, and the treatment time is 2-4 h; the thickness of the coating ranges from 10 to 20 μm.
10. A structurally-functionally-integrated ceramic matrix composite, characterized in that it is obtained by a process according to any one of claims 1 to 9.
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Application publication date: 20221025 |