CN115180966A - Continuous carbon fiber toughened ZrB 2 Preparation method of/SiOC ceramic matrix composite material - Google Patents
Continuous carbon fiber toughened ZrB 2 Preparation method of/SiOC ceramic matrix composite material Download PDFInfo
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Abstract
The invention relates to the technical field of high-temperature structural ceramic materials, and discloses continuous carbon fiber toughened ZrB 2 The preparation method of the/SiOC ceramic matrix composite material comprises the step of mixing ZrB 2 Injecting the SiOC ceramic precursor slurry into a continuous carbon fiber woven body, placing the continuous carbon fiber woven body in an SiOC ceramic precursor solution for vacuum impregnation and drying, and cracking the continuous carbon fiber woven body to obtain the continuous carbon fiber toughened ZrB 2 The composite material is subjected to the operation for multiple times to obtain the continuous carbon fiber toughened ZrB with required density 2 The SiOC ceramic matrix composite material. The invention adopts powder and ceramic firstlyThe mode that the carbon fiber woven body is introduced into the driving body together changes the traditional way that ceramic powder is directly compounded with carbon fiber, and ZrB can be introduced to the maximum degree by adopting a slurry injection mode 2 Ceramic powder and SiOC ceramic, and the SiOC ceramic can be further introduced through vacuum impregnation, so that the density of the composite material is improved.
Description
Technical Field
The invention relates to the technical field of high-temperature structural ceramic materials, in particular to continuous carbon fiber toughened ZrB 2 A method for preparing a SiOC ceramic matrix composite material.
Background
ZrB 2 The ultrahigh-temperature ceramic has excellent ultrahigh-temperature comprehensive performance, has very great application prospect in the field of aerospace, and can be used in ZrB 2 The introduction of silicon-containing compounds into the superhigh temperature ceramic can effectively improve the high temperature oxidation resistance of the material, for example, zrB is adopted as a relatively mature system at present 2 the/SiC superhigh temperature ceramic composite material. However, zrB 2 The engineering application of the material is limited due to the intrinsic brittleness problem of the ultrahigh-temperature ceramic. The continuous carbon fiber toughened ultrahigh-temperature ceramic can effectively improve the fracture toughness and the thermal shock resistance, but the ultrahigh-temperature ceramic powder is difficult to effectively compound with a continuous carbon fiber woven body, so that the material obtains higher density. Therefore, the continuous carbon fiber toughened ZrB with controllable density needs to be searched 2 A method for preparing a ceramic matrix composite material. The SiOC ceramic is widely applied to high-temperature structural ceramic as an antioxidant component, and can be obtained by a precursor conversion method, so that the SiOC ceramic has great advantages in the density control of the continuous carbon fiber toughened ceramic matrix composite.
Disclosure of Invention
Aiming at the prior continuous carbon fiber toughening ZrB proposed in the background technology 2 The invention provides a continuous carbon fiber toughened ZrB, which is difficult to solve in the preparation process of a superhigh temperature ceramic composite material 2 The preparation method of the/SiOC ceramic matrix composite material can solve the problem of ZrB 2 The problem provided in the background technology is solved by the advantage of the difficult problem that the basic ultra-high temperature ceramic and continuous carbon fiber woven body are difficult to effectively compound.
The invention provides the following technical scheme: continuous carbon fiberDimensional toughening ZrB 2 The preparation method of the/SiOC ceramic matrix composite material comprises the following steps:
step one, configuring an SiOC ceramic precursor:
preparing a solution according to a mass ratio of methyltrimethoxysilane to dimethyldimethoxysilane = 5;
adding deionized water into the solution, and mixing the deionized water according to the mass ratio of (methyltrimethoxysilane + dimethyldimethoxysilane) = 1;
adding absolute ethanol into the solution, wherein the mass of the absolute ethanol is 10 percent of the total mass of (water + methyltrimethoxysilane + dimethyldimethoxysilane);
adding nitric acid into the solution in a magnetic stirrer while stirring, wherein the amount of the nitric acid added is about 1-2 ml per 100g of the solution, and the stirring time is 20-30 min, so as to obtain an SiOC ceramic precursor solution;
step two, taking the SiOC ceramic precursor solution prepared in the step one, and adding ZrB 2 Magnetically stirring the ceramic powder to obtain ZrB 2 A SiOC ceramic precursor slurry;
step three, using an injector to convert the ZrB in the step two 2 Injecting the SiOC ceramic precursor slurry into the continuous carbon fiber woven body until the slurry can not be injected, injecting ZrB into the continuous carbon fiber woven body 2 Placing the continuous carbon fiber woven body of the SiOC ceramic precursor slurry in an oven for drying;
step four, placing the dried continuous carbon fiber woven body in the SiOC ceramic precursor solution prepared in the step one for vacuum impregnation, and then placing the continuous carbon fiber woven body subjected to vacuum impregnation in an oven for drying;
step five, putting the continuous carbon fiber braid dried in the step four into a tube furnace for cracking to obtain continuous carbon fiber toughened ZrB 2 The cracking atmosphere is flowing argon protection;
step six, toughening ZrB of the continuous carbon fiber obtained in the step five 2 Continuous carbon fiber woven by taking SiOC ceramic matrix composite material as step threeWeaving the body, repeating the processes from the first step to the fifth step for 3-5 times to obtain the continuous carbon fiber toughened ZrB with required density 2 a/SiOC ceramic matrix composite material.
Preferably, the ZrB in the second step 2 The solid content of the ceramic powder is ZrB 2 30-50% by mass of/SiOC ceramic precursor slurry, zrB 2 The average grain diameter of the ceramic powder is 50 nm-2 μm, and the magnetic stirring time is 30-60 min.
Preferably, the temperature of the oven in the third step is controlled to be 80-100 ℃, and the drying time is 24-48 h.
Preferably, the vacuum impregnation time in the fourth step is 40-60 min, the temperature of an oven for drying after vacuum impregnation is controlled to be 80-100 ℃, and the drying time is 24-48 h.
Preferably, in the fifth step, the flow rate of the argon gas is 30-60 ml/min, the cracking temperature is 1400-1500 ℃, and the heat preservation time is 30-60 min.
The invention has the following beneficial effects: the method adopts a mode of introducing the powder and the ceramic precursor into the continuous carbon fiber braided body together, changes the traditional way of directly compounding the ceramic powder and the carbon fiber, and can introduce ZrB to the maximum extent by adopting a slurry injection mode in the third step 2 Ceramic powder and SiOC ceramic, and the vacuum impregnation in the fourth step further introduces the SiOC ceramic, thereby improving the density of the composite material.
Drawings
FIG. 1 is a scanning electron microscope image of the microstructure of a woven body of raw carbon fibers in example 1;
FIG. 2 shows ZrB toughened by continuous carbon fibers obtained in example 1 2 A scanning electron microscope image of the microstructure of the/SiOC ceramic matrix composite material;
FIG. 3 is ZrB toughened by continuous carbon fibers obtained in example 3 2 A scanning electron microscope image of the microstructure of the/SiOC ceramic matrix composite material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1:
step one, configuring an SiOC ceramic precursor: weighing and mixing 100g of methyltrimethoxysilane solution and 20g of dimethyldimethoxysilane solution, and then adding 24g of deionized water and 14.4g of absolute ethyl alcohol; and (3) adding 3ml of nitric acid into the solution in a magnetic stirrer while stirring, and stirring for 30min to obtain the SiOC ceramic precursor solution.
Step two, adding 100g of ZrB into the SiOC ceramic precursor solution prepared in the step one 2 Ceramic powder is magnetically stirred, wherein ZrB 2 The average grain diameter of the ceramic powder is 2 mu m, the magnetic stirring time is 60min, and ZrB is obtained 2 A SiOC ceramic precursor slurry.
Step three, using an injector to convert the ZrB in the step two 2 Injecting the SiOC ceramic precursor slurry into the continuous carbon fiber woven body until the slurry can not be injected; then injecting ZrB 2 The continuous carbon fiber woven body of the SiOC ceramic precursor slurry is placed in an oven to be dried, wherein the drying temperature is 80 ℃, and the drying time is 24 hours.
Step four, placing the dried continuous carbon fiber woven body into the SiOC ceramic precursor solution prepared in the step one for vacuum impregnation, wherein the vacuum impregnation time is 60min; and then placing the continuous carbon fiber woven body after vacuum impregnation into an oven for drying, wherein the drying temperature is 80 ℃, and the drying time is 24 hours.
Step five, putting the continuous carbon fiber woven body dried in the step four into a tubular furnace for cracking, wherein the cracking atmosphere is flow argon protection, the flow rate of argon is 30ml/min, the cracking temperature is 1400 ℃, and the heat preservation time is 30min, so as to obtain the continuous carbon fiber toughened ZrB 2 The SiOC ceramic matrix composite material.
Step six, repeating the process from the step one to the step five for 3 times to obtain the continuous carbon fiber toughened ZrB with required density 2 a/SiOC ceramic matrix composite material.
Example 2:
step one, configuring an SiOC ceramic precursor: weighing and mixing 200g of methyltrimethoxysilane solution and 40g of dimethyldimethoxysilane solution, and then adding 24g of deionized water and 28.8g of absolute ethyl alcohol; and (3) adding 6ml of nitric acid into the solution in a magnetic stirrer while stirring, and stirring for 30min to obtain the SiOC ceramic precursor solution.
Step two, adding 180g of ZrB into the SiOC ceramic precursor solution prepared in the step one 2 Ceramic powder is magnetically stirred, wherein ZrB 2 The average grain diameter of the ceramic powder is 1 mu m, the magnetic stirring time is 60min, and ZrB is obtained 2 A SiOC ceramic precursor slurry.
Step three, using an injector to convert the ZrB in the step two 2 Injecting the SiOC ceramic precursor slurry into the continuous carbon fiber woven body until the slurry can not be injected; then injecting ZrB 2 The continuous carbon fiber woven body of the SiOC ceramic precursor slurry is placed in an oven to be dried, wherein the drying temperature is 100 ℃, and the drying time is 48 hours.
Step four, placing the dried continuous carbon fiber woven body into the SiOC ceramic precursor solution prepared in the step one for vacuum impregnation, wherein the vacuum impregnation time is 60min; and then placing the continuous carbon fiber woven body after vacuum impregnation into an oven for drying, wherein the drying temperature is 100 ℃, and the drying time is 48h.
Step five, placing the continuous carbon fiber woven body dried in the step four into a tubular furnace for cracking, wherein the cracking atmosphere is flowing argon protection, the flow rate of argon is 60ml/min, the cracking temperature is 1500 ℃, and the heat preservation time is 60min, so as to obtain the continuous carbon fiber toughened ZrB 2 a/SiOC ceramic matrix composite material.
Step six, repeating the process from the step one to the step five for 4 times to obtain the continuous carbon fiber toughened ZrB with required density 2 The SiOC ceramic matrix composite material.
Example 3:
step one, configuring an SiOC ceramic precursor: weighing and mixing 100g of methyltrimethoxysilane solution and 20g of dimethyldimethoxysilane solution, and then adding 24g of deionized water and 14.4g of absolute ethyl alcohol; and (3) adding 3ml of nitric acid into the solution in a magnetic stirrer while stirring, and stirring for 30min to obtain the SiOC ceramic precursor solution.
Step two, 140g of ZrB is added into the SiOC ceramic precursor solution prepared in the step one 2 Ceramic powder is magnetically stirred, wherein ZrB 2 The average grain diameter of the ceramic powder is 50nm, the magnetic stirring time is 60min, and ZrB is obtained 2 A SiOC ceramic precursor slurry.
Step three, using an injector to convert the ZrB in the step two 2 Injecting the SiOC ceramic precursor slurry into the continuous carbon fiber woven body until the slurry cannot be injected; then injecting ZrB 2 And putting the continuous carbon fiber woven body of the SiOC ceramic precursor slurry into an oven for drying, wherein the drying temperature is 80 ℃, and the drying time is 48 hours.
Step four, placing the dried continuous carbon fiber woven body into the SiOC ceramic precursor solution prepared in the step one for vacuum impregnation, wherein the vacuum impregnation time is 40min; and then placing the continuous carbon fiber woven body after vacuum impregnation into an oven for drying, wherein the drying temperature is 80 ℃, and the drying time is 24 hours.
Step five, placing the continuous carbon fiber woven body dried in the step four into a tubular furnace for cracking, wherein the cracking atmosphere is flowing argon protection, the flow rate of argon is 50ml/min, the cracking temperature is 1400 ℃, and the heat preservation time is 60min, so as to obtain the continuous carbon fiber toughened ZrB 2 a/SiOC ceramic matrix composite material.
Step six, repeating the process from the step one to the step five for 5 times to obtain the continuous carbon fiber toughened ZrB with required density 2 The SiOC ceramic matrix composite material.
Referring to the attached drawings 1 to 3, wherein fig. 1 is a scanning electron microscope image of the microstructure of the original carbon fiber braid, and fig. 2 and 3 are continuous carbon fiber toughened ZrB obtained in example 1 and 3, respectively 2 The microstructure scanning electron microscope picture of the/SiOC ceramic matrix composite material can be known through comparison by the method of the inventionThe ceramic phase can be effectively and uniformly introduced into the continuous carbon fiber woven body, and the composite material has higher density.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. Continuous carbon fiber toughened ZrB 2 The preparation method of the/SiOC ceramic matrix composite material is characterized by comprising the following steps:
step one, configuring an SiOC ceramic precursor:
preparing a solution according to a mass ratio of methyltrimethoxysilane to dimethyldimethoxysilane = 5;
adding deionized water into the solution, and mixing the deionized water according to the mass ratio of (methyltrimethoxysilane + dimethyldimethoxysilane) = 1;
adding absolute ethyl alcohol into the solution, wherein the mass of the absolute ethyl alcohol is 10% of the total mass of (water + methyltrimethoxysilane + dimethyldimethoxysilane);
adding nitric acid into the solution in a magnetic stirrer while stirring, wherein the amount of the nitric acid added is about 1-2 ml per 100g of the solution, and the stirring time is 20-30 min, so as to obtain an SiOC ceramic precursor solution;
step two, taking the SiOC ceramic precursor solution prepared in the step one, and adding ZrB 2 Ceramic powder is magnetically stirred to obtain ZrB 2 A SiOC ceramic precursor slurry;
step three, using an injector to subject the ZrB in the step two 2 Injecting the SiOC ceramic precursor slurry into the continuous carbon fiber woven body until the slurry can not be injected, injecting ZrB 2 Placing the continuous carbon fiber woven body of the SiOC ceramic precursor slurry in an oven for drying;
step four, placing the dried continuous carbon fiber woven body in the SiOC ceramic precursor solution prepared in the step one for vacuum impregnation, and then placing the continuous carbon fiber woven body subjected to vacuum impregnation in an oven for drying;
step five, putting the continuous carbon fiber braid dried in the step four into a tube furnace for cracking to obtain continuous carbon fiber toughened ZrB 2 The cracking atmosphere is flowing argon protection;
step six, toughening ZrB of the continuous carbon fiber obtained in the step five 2 Taking the SiOC ceramic matrix composite material as a continuous carbon fiber woven body in the third step, repeating the process from the first step to the fifth step for 3-5 times to obtain the continuous carbon fiber toughened ZrB with required density 2 The SiOC ceramic matrix composite material.
2. The continuous carbon fiber toughened ZrB of claim 1 2 The preparation method of the/SiOC ceramic matrix composite material is characterized by comprising the following steps: zrB in the second step 2 The solid content of the ceramic powder is ZrB 2 30-50% by mass of/SiOC ceramic precursor slurry, zrB 2 The average grain diameter of the ceramic powder is 50 nm-2 μm, and the magnetic stirring time is 30-60 min.
3. The continuous carbon fiber toughened ZrB of claim 1 2 The preparation method of the/SiOC ceramic matrix composite material is characterized in that: step three the temperature of the oven is controlled to be 80 toDrying time is 24-48 h at 100 ℃.
4. The continuous carbon fiber toughened ZrB of claim 1 2 The preparation method of the/SiOC ceramic matrix composite material is characterized by comprising the following steps: the vacuum impregnation time in the fourth step is 40-60 min, the temperature of an oven for drying after vacuum impregnation is controlled at 80-100 ℃, and the drying time is 24-48 h.
5. The continuous carbon fiber toughened ZrB of claim 1 2 The preparation method of the/SiOC ceramic matrix composite material is characterized in that: in the fifth step, the flow rate of the argon gas is 30-60 ml/min, the cracking temperature is 1400-1500 ℃, and the heat preservation time is 30-60 min.
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| 彭飞: "高温 Cf/SiOC-ZrB2复合材料的制备与性能研究", 《中国优秀硕士学位论⽂文全⽂文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115745584A (en) * | 2022-11-14 | 2023-03-07 | 马鞍山利尔开元新材料有限公司 | Sliding plate brick and preparation method thereof |
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| CN115180966B (en) | 2023-04-21 |
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