CN114133248A - Method for improving conversion rate of precursor ceramic - Google Patents
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- CN114133248A CN114133248A CN202111581341.9A CN202111581341A CN114133248A CN 114133248 A CN114133248 A CN 114133248A CN 202111581341 A CN202111581341 A CN 202111581341A CN 114133248 A CN114133248 A CN 114133248A
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- 239000002243 precursor Substances 0.000 title claims abstract description 39
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 16
- 239000012700 ceramic precursor Substances 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 35
- 238000005470 impregnation Methods 0.000 claims abstract description 31
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000007873 sieving Methods 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 229920003257 polycarbosilane Polymers 0.000 claims description 66
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 45
- 238000002360 preparation method Methods 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 8
- 239000011153 ceramic matrix composite Substances 0.000 claims description 7
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims 2
- 238000007654 immersion Methods 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 24
- 238000000227 grinding Methods 0.000 description 24
- 239000011521 glass Substances 0.000 description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- 238000004321 preservation Methods 0.000 description 11
- 238000003892 spreading Methods 0.000 description 11
- 230000007480 spreading Effects 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000004132 cross linking Methods 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
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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Abstract
The invention discloses a method for improving the conversion rate of precursor ceramics and impregnation liquid, which comprises the following steps: firstly, crushing a ceramic precursor, ball-milling the crushed ceramic precursor, drying and sieving the crushed ceramic precursor for later use; secondly, preserving the heat of the treated ceramic precursor powder in the air for 1-10h at the temperature of 100 ℃ and 300 ℃; dissolving the ceramic precursor powder in solvent to prepare ceramic precursor soaking liquid, wherein the solvent contains 10-80 wt%. The invention can improve the density of the SiC ceramic body and the ceramic conversion rate of the precursor.
Description
Technical Field
The invention relates to the field of ceramic matrix composite material preparation, in particular to a method for improving the conversion rate of precursor ceramic.
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 the first 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 soaking the fiber preform with liquid ceramic precursor, crosslinking and curing the liquid ceramic precursor, pyrolyzing to obtain ceramic matrix, and repeating the soaking, curing and pyrolyzing steps to obtain the final ceramic matrix composite.
In the PIP process, the ceramic precursor releases small molecules from organic polymers to inorganic ceramics to form pores, the volume of the ceramic precursor shrinks and cracks are generated, so that the compactness of the ceramics is influenced, the yield of the ceramics is reduced, the preparation period is prolonged, and the manufacturing cost is increased.
Disclosure of Invention
Based on the problems, the invention provides a method for improving the ceramic conversion rate of a precursor, which can improve the compactness of a SiC ceramic body and the ceramic conversion rate of the precursor.
A method for increasing the conversion rate of precursor ceramics, comprising the following steps:
firstly, crushing a ceramic precursor, ball-milling the crushed ceramic precursor, drying and sieving the crushed ceramic precursor for later use;
secondly, preserving the heat of the treated ceramic precursor powder in the air for 1-10h at the temperature of 100 ℃ and 300 ℃;
dissolving the ceramic precursor powder in solvent to prepare ceramic precursor soaking liquid, wherein the solvent contains 10-80 wt%.
In one or more specific embodiments of the present application, in the above-mentioned (i), the ball milling time is 3-6 h, and the rotation speed is 300-600 revolutions per second.
In one or more specific embodiments herein, the ceramic precursor is a polycarbosilane precursor.
In one or more specific embodiments herein, the solvent is one or more of xylene, cyclohexane, divinylbenzene.
The invention also provides a preparation method of the impregnation liquid.
A preparation method of an impregnation liquid comprises the following steps:
firstly, crushing a ceramic precursor, ball-milling the crushed ceramic precursor, drying and sieving the crushed ceramic precursor for later use;
secondly, preserving the heat of the treated ceramic precursor powder in the air for 1-10h at the temperature of 100 ℃ and 300 ℃;
dissolving the ceramic precursor powder in solvent to prepare ceramic precursor soaking liquid, wherein the solvent contains 10-80 wt%.
In one or more specific embodiments of the present application, in the above-mentioned (i), the ball milling time is 3-6 h, and the rotation speed is 300-600 revolutions per second.
In one or more specific embodiments herein, the ceramic precursor is a polycarbosilane precursor.
In one or more specific embodiments herein, the solvent is one or more of xylene, cyclohexane, divinylbenzene.
The invention also provides the impregnation liquid.
The impregnation liquid is prepared by the preparation method of the impregnation liquid.
The invention also provides a ceramic matrix composite.
The ceramic matrix composite material is prepared from the impregnation liquid.
The principle and the beneficial effects of the invention are as follows:
according to the preparation method, the ceramic precursor is subjected to preoxidation treatment, the prepared impregnation liquid is cured and pyrolyzed to obtain a compact SiC ceramic body, and the ceramic conversion rate of the precursor is greatly increased.
Drawings
FIG. 1 is a graph of the morphology of a pyrolyzed ceramic body according to examples 1-9 of the present application.
FIG. 2 is a graph of the morphology of a pyrolyzed ceramic body in comparative example 1 of the present application;
Detailed Description
The invention will be further explained with reference to the drawings.
A method for increasing the conversion rate of precursor ceramics, comprising the following steps:
firstly, a certain amount of ceramic precursor is taken for crushing, and the crushed ceramic precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and ball milling is carried out for 3-6 hours at the rotating speed of 300-600 revolutions per second. Then drying and sieving for standby.
Secondly, heating the oven to 100 ℃ and 300 ℃, spreading the ball-milled ceramic precursor powder in a glass culture dish, and putting the glass culture dish in the air of the oven for heat preservation for 1-10 hours.
Dissolving the ceramic precursor powder in solvent to prepare ceramic precursor soaking liquid, wherein the solvent contains 10-80 wt%.
Based on the method for improving the conversion rate of the precursor ceramic, the application also provides a preparation method of the impregnation liquid.
A preparation method of an impregnation liquid comprises the following steps:
firstly, a certain amount of ceramic precursor is taken for crushing, and the crushed ceramic precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and ball milling is carried out for 3-6 hours at the rotating speed of 300-600 revolutions per second. Then drying and sieving for standby.
Secondly, heating the oven to 100 ℃ and 300 ℃, spreading the ball-milled ceramic precursor powder in a glass culture dish, and putting the glass culture dish in the air of the oven for heat preservation for 1-10 hours.
Dissolving the ceramic precursor powder in solvent to prepare ceramic precursor soaking liquid, wherein the solvent contains 10-80 wt%.
The ceramic-based composite material is prepared from the ceramic precursor impregnation liquid.
Example 1:
firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Heating the oven to 160 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 2 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 2:
firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 160 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 4 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 3:
firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 160 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 6 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 4:
firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 180 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 2 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 5:
firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 180 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 4 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 6
Firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 180 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 6 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 7
Firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 200 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 2 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 8
Firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 200 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 4 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 9
Firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Secondly, heating the oven to 200 ℃, spreading 10g of the ball-milled PCS powder in a glass culture dish, and putting the glass culture dish in the oven for heat preservation for 6 hours.
Dissolving the PCS powder treated by the second step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Comparative example 1
Firstly, a certain amount of Polycarbosilane (PCS) precursor is taken to be crushed, and the crushed polycarbosilane precursor is mixed with a proper amount of grinding medium absolute ethyl alcohol and zirconia grinding balls, and the mixture is subjected to ball milling for 3 hours at the rotating speed of 600 revolutions per second. Then drying and sieving by a 100-mesh sieve for later use.
Dissolving PCS powder of the first step in dimethylbenzene to prepare PCS impregnation liquid, wherein the dimethylbenzene is 50 wt%.
Example 10
10ml of PCS impregnating solution of examples 1-9 and comparative example 1 are respectively taken, and the PCS impregnating solution is respectively kept at 1.5MPa and 300 ℃ for 8 hours until the impregnating solution is completely solidified and weighed.
And secondly, pyrolyzing the cured impregnation liquid at 1200 ℃ in a nitrogen atmosphere, weighing and calculating the ceramic yield after pyrolysis, wherein the cured weight, the cracked weight and the ceramic yield are shown in the following table 1.
TABLE 1
Examples 1-9 the pyrolyzed ceramic bodies are shown in FIG. 1, and comparative example 1 the pyrolyzed ceramic bodies are shown in FIG. 2.
As can be seen from table 1 and fig. 1-2 above, a compact SiC ceramic body can be obtained after the impregnation liquid prepared from the PCS powder subjected to the pre-oxidation treatment is cured and pyrolyzed, the ceramic yield is directly correlated with the treatment temperature and the treatment time, and the impregnation liquid prepared from the powder not subjected to the pre-oxidation treatment is cured and pyrolyzed and then foamed, so that the obtained SiC ceramic body is porous and the ceramic yield is low.
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. A method for increasing the conversion rate of precursor ceramics, comprising the following steps:
firstly, crushing a ceramic precursor, ball-milling the crushed ceramic precursor, drying and sieving the crushed ceramic precursor for later use;
secondly, preserving the heat of the treated ceramic precursor powder in the air for 1-10h at the temperature of 100 ℃ and 300 ℃;
dissolving the ceramic precursor powder in solvent to prepare ceramic precursor soaking liquid, wherein the solvent contains 10-80 wt%.
2. The method for improving the conversion rate of the precursor ceramic according to claim 1, wherein in the step (i), the ball milling time is 3-6 h, and the rotation speed is 300-600 revolutions per second.
3. A method of increasing the conversion of a precursor ceramic according to any of claims 1 to 2 wherein the ceramic precursor is a polycarbosilane precursor.
4. A method for improving conversion of a precursor ceramic as claimed in any one of claims 1 to 3 wherein said solvent is one or more of xylene, cyclohexane and divinylbenzene.
5. A preparation method of an impregnation liquid comprises the following steps:
firstly, crushing a ceramic precursor, ball-milling the crushed ceramic precursor, drying and sieving the crushed ceramic precursor for later use;
secondly, preserving the heat of the treated ceramic precursor powder in the air for 1-10h at the temperature of 100 ℃ and 300 ℃;
dissolving the ceramic precursor powder in solvent to prepare ceramic precursor soaking liquid, wherein the solvent contains 10-80 wt%.
6. The method for preparing the impregnation liquid according to claim 5, wherein in the first step, the ball milling time is 3-6 hours, and the rotation speed is 300-600 revolutions per second.
7. The method of preparing an immersion liquid according to any one of claims 5 to 6, wherein the ceramic precursor is a polycarbosilane precursor.
8. A process for the preparation of the impregnation fluid according to any one of claims 5 to 7, characterized in that: the solvent is one or more of dimethylbenzene, cyclohexane and divinylbenzene.
9. An impregnation fluid prepared by the method of any one of claims 5 to 8.
10. A ceramic matrix composite prepared from the impregnation solution of claim 9.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110922191A (en) * | 2019-12-20 | 2020-03-27 | 厦门大学 | Silicon carbide polymer precursor ceramic defect healing method |
| CN111848196A (en) * | 2020-07-24 | 2020-10-30 | 北京航空航天大学 | Preparation method of in-situ silicon carbide nanowire toughened silicon carbide ceramic |
| CN113354434A (en) * | 2021-07-06 | 2021-09-07 | 成都成维精密机械制造有限公司 | Ceramic slurry for low-porosity ceramic matrix composite material, prepreg and manufacturing method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110922191A (en) * | 2019-12-20 | 2020-03-27 | 厦门大学 | Silicon carbide polymer precursor ceramic defect healing method |
| CN111848196A (en) * | 2020-07-24 | 2020-10-30 | 北京航空航天大学 | Preparation method of in-situ silicon carbide nanowire toughened silicon carbide ceramic |
| CN113354434A (en) * | 2021-07-06 | 2021-09-07 | 成都成维精密机械制造有限公司 | Ceramic slurry for low-porosity ceramic matrix composite material, prepreg and manufacturing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 范华: "聚碳硅烷交联-成型-热解合成三维碳化硅陶瓷", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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Application publication date: 20220304 |