CN114133251A - Impregnation slurry and preparation method thereof - Google Patents
Impregnation slurry and preparation method thereof Download PDFInfo
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- CN114133251A CN114133251A CN202111581355.0A CN202111581355A CN114133251A CN 114133251 A CN114133251 A CN 114133251A CN 202111581355 A CN202111581355 A CN 202111581355A CN 114133251 A CN114133251 A CN 114133251A
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- 239000002002 slurry Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005470 impregnation Methods 0.000 title claims description 22
- 238000007613 slurry method Methods 0.000 title description 2
- 239000000919 ceramic Substances 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 63
- 239000012700 ceramic precursor Substances 0.000 claims abstract description 43
- 238000007598 dipping method Methods 0.000 claims abstract description 24
- 238000002679 ablation Methods 0.000 claims abstract description 22
- 239000011153 ceramic matrix composite Substances 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims description 49
- 238000000227 grinding Methods 0.000 claims description 22
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 11
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 5
- 229910003862 HfB2 Inorganic materials 0.000 claims description 5
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005336 cracking Methods 0.000 claims description 5
- 238000001723 curing Methods 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 8
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 238000009991 scouring Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 239000000835 fiber Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000012216 screening Methods 0.000 description 8
- 229910052726 zirconium Inorganic materials 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 6
- 229920003257 polycarbosilane Polymers 0.000 description 6
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011226 reinforced ceramic Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a dipping slurry and a preparation method thereof, wherein the dipping slurry comprises the following components: 5-20 wt% of ceramic powder; 80-95 wt% of a ceramic precursor solution; wherein the ceramic powder is ceramic powder containing an ablation resistant component. The dipping slurry is prepared by introducing ceramic powder containing an anti-ablation component into a ceramic precursor solution, so that the anti-ablation capacity of the composite material is fundamentally improved, and the oxidation resistance and the scouring resistance of the ceramic matrix composite material are improved.
Description
Technical Field
The invention relates to the field of preparation of ceramic matrix composites, in particular to impregnation slurry and a preparation method thereof.
Background
The ceramic matrix composite material has wide application potential in the fields of aerospace, nuclear fission and nuclear fusion, the continuous fiber toughened ceramic matrix composite material is a current research hotspot, and the preparation method mainly comprises the following steps: polymer Impregnation and Pyrolysis (PIP), Chemical Vapor Infiltration (CVI), nano-impregnation and Transient eutectic phase (Nan o-impregnated and Transient eutectid, NITE), and Reaction Infiltration (RI).
The PIP process comprises the steps of dipping a fiber prefabricated member (dipping) by using a liquid ceramic precursor, crosslinking and curing the liquid ceramic precursor (curing), then carrying out pyrolysis (cracking) to convert the liquid ceramic precursor into a ceramic matrix, and then repeating the dipping-curing-cracking process to finally prepare the ceramic matrix composite.
In the PIP process, a ceramic precursor is one of the keys of the whole PIP process, pores and cracks inevitably exist in the ceramic matrix composite material prepared by the PIP process from the existing ceramic precursor, and the pores and the cracks become channels for oxygen to enter the composite material in a high-temperature oxidation environment, so that the integral oxidation resistance of the composite material in the high-temperature thermal oxidation environment is weakened, and the application of the fiber reinforced ceramic matrix composite material in a high thrust-weight ratio aeroengine is restricted.
The modification of the fiber reinforced ceramic matrix composite material is mainly carried out from four aspects of fibers, an interface phase, a matrix and a surface coating. At present, the research is more about the modification of fiber, interface phase and surface coating, the modification report on the matrix is less, and the means for successfully introducing an ablation-resistant component into the fiber-reinforced ceramic matrix composite material is lacked.
Disclosure of Invention
The invention discloses a dipping slurry, which is prepared by introducing an anti-ablation component into a precursor solution, so that the anti-ablation capacity of a composite material is fundamentally improved, and the oxidation resistance and the scouring resistance of the prepared ceramic matrix composite material are improved.
An impregnation slurry, comprising:
80-95 wt% of ceramic powder;
5-20 wt% of a ceramic precursor solution;
wherein the ceramic powder is ceramic powder containing an ablation resistant component.
In one or more specific embodiments of the present application, the ceramic precursor solution is a solution in which a ceramic precursor is dissolved in a solvent.
In one or more specific embodiments herein, the solvent is one or more of xylene, cyclohexane, divinyl benzene, and the like organic solvents.
In one or more specific embodiments of the present application, the ceramic powder containing an ablation-resistant component is Si3N4、SiC、ZrB2、ZrC、HfC、HfB2BN and B4One or more of C powder.
The invention also provides a preparation method of the dipping slurry.
A preparation method of impregnation slurry comprises the following steps:
pretreatment: ceramic powder Si containing anti-ablation component3N4、SiC、ZrB2、ZrC、HfC、HfB2BN and B4Performing wet ball milling on one or more components in the C powder;
secondly, the ceramic precursor is crushed and then slowly dissolved in one or more organic solvents such as dimethylbenzene, cyclohexane, divinyl benzene base and the like to form ceramic precursor solution;
and thirdly, mixing and ball-milling the ceramic precursor solution obtained in the second step, the ceramic powder pretreated in the first step and a ceramic dispersant to obtain the dipping slurry.
In one or more specific embodiments of the present application, in the above-mentioned (i), the ball milling rotation speed is 400 to 600r/min, and the milling time is 4 to 8 hours.
2. In one or more specific embodiments of the present application, in the pretreatment of the first step, after wet ball milling, powder obtained after wet ball milling is put into a drying oven to dry and mix the uniformly mixed powder for 4-8 hours at 100-120 ℃; and then collecting the dried mixed powder, grinding the powder in an agate mortar for 1-2 h, and then sieving the powder by a 100-mesh sieve.
In one or more specific embodiments of the present application, the third step includes 80 to 95 wt% of the ceramic precursor solution, 5 to 20 wt% of the pretreated ceramic powder, and the amount of the ceramic dispersant is 2 to 6 permillage of the pretreated ceramic powder.
In one or more specific embodiments of the present application, the ball milling rotation speed is 200 to 400r/min, and the time is 0.5 to 1 h.
The ceramic matrix composite is prepared by dipping, curing and cracking dipping slurry and a prefabricated member, wherein the dipping slurry is prepared from the dipping slurry.
The invention principle and the beneficial effects are as follows:
in the preparation of the dipping slurry, the ablation-resistant ceramic powder is ground and mixed uniformly by a first wet ball milling; the ceramic precursor is prepared into a precursor solution with certain viscosity through solvents with different proportions, wherein the precursor is crushed and the dissolution of the precursor is accelerated by a water bath heating environment, so that the efficiency is improved; introducing the ceramic superfine powder into the precursor solution by secondary ball milling and keeping the ceramic superfine powder in a uniform state; the slurry was maintained in a uniform steady state for a long period of time by the rotation of the tank mill.
The inventor successfully introduces the ablation-resistant component into the ceramic precursor by the preparation method of the dipping slurry, and the dipping slurry is the dipping slurry for the application, wherein the ablation-resistant component is introduced into the base material, the consumption rate of the ablation-resistant component is lower than that of carbon with the same volume in the ablation process or the ablation-resistant component plays a role in inhibiting the integral ablation of the material, the ablation resistance of the composite material is fundamentally improved, and the oxidation resistance and the scouring resistance of the ceramic matrix composite material are finally improved.
Detailed Description
The present invention will be further explained below.
A preparation method of impregnation slurry comprises the following steps:
firstly, ceramic powder Si of anti-ablation component3N4、SiC、ZrB2、ZrC、HfC、HfB2BN and B4One or more components in C are poured into the alumina ball mill slowly in turnAdding distilled water into a tank, and adding zirconium balls as a ball milling medium, wherein the mass ratio of raw materials (ceramic powder containing an anti-ablation component), grinding balls and water is 2-4: 5-9: 2-4; placing the ball milling tank in a planetary ball mill, grinding for 4-8 h at the rotating speed of 400-600 r/min, screening out ball milling media, and placing the ball milling media in a drying oven to dry and mix the uniformly mixed powder for 4-8 h at the temperature of 100-120 ℃; collecting the dried mixed powder, grinding the powder in an agate mortar for 1-2 h, and then sieving the powder through a 100-mesh sieve to obtain uniformly mixed ceramic powder;
secondly, crushing the ceramic precursor, and slowly dissolving the ceramic precursor into one or more organic solvents such as dimethylbenzene, cyclohexane, divinyl benzene base and the like at the dissolving temperature of 20-40 ℃ in a water bath manner to form a ceramic precursor solution;
putting the ceramic precursor solution obtained in the step II and the uniformly mixed ceramic powder obtained in the step I into an alumina ball-milling tank in sequence, wherein 80-95 wt% of the ceramic precursor solution and 5-20 wt% of the uniformly mixed ceramic powder are mixed; adding a ceramic dispersing agent which is 2-6 per mill of the specific gravity of the uniformly mixed ceramic powder, and putting zirconium balls as ball milling media, wherein the mass ratio of the raw materials (the ceramic precursor solution, the uniformly mixed ceramic powder and the ceramic dispersing agent) to the grinding balls is 1: 2-4; placing the ball milling tank in a planetary ball mill, grinding for 0.5-1 h at the rotating speed of 200-400 r/min, and screening out a ball milling medium to obtain impregnation slurry;
and fourthly, after the impregnating slurry is filled into a sealing tank and sealed, the tank mill frame is placed on the tank mill frame to continuously rotate at the rotating speed of 100-200 r/min until the tank mill frame is taken down before use, the tank mill frame is continuously put back to rotate after use, a little solvent volatilizes in use, and organic solvent can be supplemented according to the requirement of an impregnating process to adjust the viscosity.
Example 1
Firstly, ZrB2Slowly pouring the ceramic powder into an alumina ball-milling tank, adding distilled water, and adding zirconium balls as ball-milling media, wherein the raw material (ZrB)2Ceramic powder), grinding balls and water in a mass ratio of 3:8: 2; placing the ball milling tank in a planetary ball mill, grinding for 6h at the rotating speed of 600r/min, screening out ball milling media, and placing the ball milling media in a drying oven to dry and mix the uniformly mixed powder for 8h at 110 ℃; collecting the dried mixed powderGrinding in an agate mortar for 1h, and sieving with a 100-mesh sieve to obtain ZrB2Ultrafine ceramic powder;
secondly, crushing polycarbosilane, and slowly dissolving the polycarbosilane into dimethylbenzene, wherein the dissolving temperature is 40 ℃, and the heating mode is water bath, so that a ceramic precursor solution (the viscosity is 120mPa & s) is formed;
thirdly, the ceramic precursor solution in the second step and ZrB in the first step2Sequentially filling the superfine ceramic powder into an alumina ball-milling tank, wherein 95 wt% of the ceramic precursor solution and 5 wt% of the uniformly mixed ceramic powder are mixed; adding a ceramic dispersing agent which is 4 per mill of the specific gravity of the uniformly mixed ceramic powder, and putting zirconium balls as ball milling media, wherein the mass ratio of the raw materials (ceramic precursor solution, the uniformly mixed ceramic powder and the ceramic dispersing agent) to the grinding balls is 1: 2; placing the ball milling tank in a planetary ball mill, grinding for 0.5h at the rotating speed of 300r/min, and screening out a ball milling medium to obtain dipping slurry;
and fourthly, after the impregnating slurry in the third step is filled into a sealing tank and sealed, the tank mill frame is placed on the tank mill frame to rotate continuously at the rotating speed of 150r/min until the tank mill frame is taken down before use, the tank mill frame is continuously placed back to rotate after use, the solvent volatilizes in use, and the organic solvent can be supplemented according to the impregnating requirement to adjust the viscosity.
Example 2
Pouring ZrC ceramic powder slowly into an alumina ball-milling tank, adding distilled water, and putting zirconium balls as ball-milling media, wherein the mass ratio of raw materials (ZrC ceramic powder), grinding balls and water is 3:8: 2; placing the ball milling tank in a planetary ball mill, grinding for 6h at the rotating speed of 600r/min, screening out ball milling media, and placing the ball milling media in a drying oven to dry and mix the uniformly mixed powder for 8h at 110 ℃; collecting the dried mixed powder in an agate mortar, grinding for 1h, and then sieving with a 100-mesh sieve to obtain ZrC superfine ceramic powder;
secondly, crushing polycarbosilane, and slowly dissolving the polycarbosilane into dimethylbenzene, wherein the dissolving temperature is 40 ℃, and the heating mode is water bath, so that a ceramic precursor solution (the viscosity is 120mPa & s) is formed;
thirdly, sequentially filling the ceramic precursor solution obtained in the second step and the ZrC superfine ceramic powder obtained in the first step into an alumina ball milling tank, wherein 95 wt% of the ceramic precursor solution and 5 wt% of the ceramic powder are obtained; adding a ceramic dispersant with the ceramic powder specific gravity of 4 per mill, and adding zirconium balls as ball milling media, wherein the mass ratio of the raw materials (ceramic precursor solution, uniformly mixed ceramic powder and ceramic dispersant) to the grinding balls is 1: 2; placing the ball milling tank in a planetary ball mill, grinding for 0.5h at the rotating speed of 300r/min, and screening out a ball milling medium to obtain dipping slurry;
and fourthly, after the impregnating slurry in the third step is filled into a sealing tank and sealed, the tank mill frame is placed on the tank mill frame to rotate continuously at the rotating speed of 150r/min until the tank mill frame is taken down before use, the tank mill frame is continuously placed back to rotate after use, the solvent volatilizes in use, and the organic solvent can be supplemented according to the impregnating requirement to adjust the viscosity.
Example 3
Firstly, ZrB2Slowly pouring ceramic powder and ZrC ceramic powder into an alumina ball-milling tank according to the mass ratio of 1:1, adding distilled water, and putting zirconium balls as ball-milling media, wherein the raw material (ZrB)2Ceramic powder and ZrC ceramic powder), grinding balls and water in a mass ratio of 3:8: 2; placing the ball milling tank in a planetary ball mill, grinding for 8h at the rotating speed of 600r/min, screening out ball milling media, and placing the ball milling media in a drying oven to dry and mix the uniformly mixed powder for 8h at 110 ℃; collecting the dried mixed powder in an agate mortar, grinding for 2h, and then sieving with a 100-mesh sieve to obtain uniformly mixed superfine ceramic powder;
secondly, crushing polycarbosilane, and slowly dissolving the polycarbosilane into dimethylbenzene, wherein the dissolving temperature is 40 ℃, and the heating mode is water bath, so that a ceramic precursor solution (the viscosity is 120mPa & s) is formed;
thirdly, sequentially filling the ceramic precursor solution obtained in the second step and the uniformly mixed superfine ceramic powder obtained in the first step into an alumina ball milling tank, wherein 90 wt% of the ceramic precursor solution and 10 wt% of the uniformly mixed ceramic powder are mixed; adding ceramic dispersing agent which is 5 per mill of the specific gravity of the uniformly mixed ceramic powder, and putting zirconium balls as ball milling media, wherein the mass ratio of the raw materials (ceramic precursor solution, the uniformly mixed ceramic powder and the ceramic dispersing agent) to the grinding balls is 1: 3; placing the ball milling tank in a planetary ball mill, grinding for 1h at the rotating speed of 200r/min, and screening out a ball milling medium to obtain dipping slurry;
and fourthly, after the impregnating slurry in the third step is filled into a sealing tank and sealed, the tank mill frame is placed on the tank mill frame to rotate continuously at the rotating speed of 150r/min until the tank mill frame is taken down before use, the tank mill frame is continuously placed back to rotate after use, the solvent volatilizes in use, and the organic solvent can be supplemented according to the impregnating requirement to adjust the viscosity.
Example 4
The impregnation slurries prepared in examples 1 to 3 were used to prepare ceramic matrix composites using the PIP process.
A method for preparing a ceramic matrix composite material by a PIP process comprises the following steps:
first, a fiber preform was impregnated in the impregnation slurry prepared in examples 1 to 3.
② the dipped fiber is pre-cured in a curing tank at 300 ℃.
Thirdly, cracking the solidified prefabricated member at 1200 ℃ in the nitrogen atmosphere.
Fourthly, densification: and (c) repeating the step (I) and the step (III).
Obtaining the ceramic matrix composite.
The prepared ceramic matrix composite material is subjected to oxidation resistance and anti-scouring capacity tests, and the results are shown in the following table 1.
Example 5
The ceramic matrix composite material prepared by the ceramic precursor solution of example 1 by the PIP process was subjected to oxidation resistance and erosion resistance tests, and the results are shown in table 1 below. Example 5 compared to example 4, the experimental conditions were the same except that example 4 was the impregnation slurry and example 5 was the ceramic precursor solution.
TABLE 1
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An impregnation slurry, characterized in that the impregnation slurry comprises:
5-20 wt% of ceramic powder of an ablation resistant component;
80-95 wt% of ceramic precursor solution.
2. The impregnation slurry according to claim 1, wherein the ceramic precursor solution is a solution in which a ceramic precursor is dissolved in a solvent.
3. The impregnation slurry according to claim 1, wherein the solvent is one or more of organic solvents such as xylene, cyclohexane, divinyl benzene and the like.
4. The impregnation slurry of any one of claims 1 to 3, wherein the ablation-resistant component ceramic powder is Si3N4、SiC、ZrB2、ZrC、HfC、HfB2BN and B4One or more of C powder.
5. A preparation method of impregnation slurry comprises the following steps:
pretreatment: ceramic powder Si containing anti-ablation component3N4、SiC、ZrB2、ZrC、HfC、HfB2BN and B4Performing wet ball milling on one or more components in the C powder;
secondly, the ceramic precursor is crushed and then slowly dissolved in one or more organic solvents such as dimethylbenzene, cyclohexane, divinyl benzene base and the like to form ceramic precursor solution;
and thirdly, mixing and ball-milling the ceramic precursor solution obtained in the second step, the ceramic powder pretreated in the first step and a ceramic dispersant to obtain the dipping slurry.
6. The preparation method of the impregnation slurry according to claim 5, wherein in the step (i), the ball milling rotation speed is 400-600 r/min, and the grinding time is 4-8 h.
7. The preparation method of the impregnation slurry according to any one of claims 5 to 6, characterized in that in the pretreatment of the first step, after wet ball milling, powder subjected to wet ball milling is put into a drying oven to dry and mix the uniformly mixed powder for 4 to 8 hours at 100 to 120 ℃; and then collecting the dried mixed powder, grinding the powder in an agate mortar for 1-2 h, and then sieving the powder by a 100-mesh sieve.
8. The preparation method of the impregnation slurry according to any one of claims 5 to 7, wherein the third step is to mix 80 to 95 wt% of the ceramic precursor solution and 5 to 20 wt% of the pretreated ceramic powder, and the amount of the ceramic dispersant is 2 to 6 per mill of the pretreated ceramic powder.
9. The preparation method of the impregnation slurry according to claim 5, wherein the ball milling rotation speed is 200 to 400r/min, and the time is 0.5 to 1 hour.
10. The ceramic matrix composite is prepared by dipping, curing and cracking dipping slurry and a prefabricated member, and is characterized in that: the dipping slurry is prepared from the dipping slurry of any one of claims 1 to 4.
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