CN111892405A - Preparation method for preparing ceramic matrix composite material by interface-layer-free process - Google Patents
Preparation method for preparing ceramic matrix composite material by interface-layer-free process Download PDFInfo
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Abstract
The invention relates to a preparation method for preparing a ceramic matrix composite by a non-interface layer process, which is characterized in that boron nitride powder is introduced into a ceramic matrix composite substrate, and because the boron nitride has good lubricating effect, a weak interface is generated between a fiber and the substrate interface, so that the toughening effect is achieved, and the ceramic matrix composite is prepared by the following three traditional systems: the fibers, interface layer and matrix become a two-system: fibers and a matrix. On one hand, the invention avoids the process flow of an interface layer in the preparation process of the composite material, thereby avoiding the need of a chemical vapor deposition high-temperature furnace in the preparation process and avoiding the waste generated in the deposition process; on the other hand, the traditional precursor impregnation cracking process is accompanied by large-volume shrinkage, and the densification can be realized only by multiple impregnation cracking processes, and the shrinkage of slurry in the cracking process can be reduced by adding the boron nitride powder into the precursor, so that the circulation efficiency is greatly improved, and the cycle efficiency is reduced to 4 times from the original 8-10 times.
Description
Technical Field
The invention relates to a preparation method for preparing a ceramic matrix composite by a non-interface layer process, belonging to the technical field of composite preparation.
Background
The ceramic matrix composite has the advantages of high temperature resistance, oxidation resistance, low density and the like, and is widely applied in the field of aerospace. Commonly used methods for preparing ceramic matrix composites include precursor dip cracking (PIP), chemical vapor deposition, melt siliconizing, and others. Traditional ceramic matrix composites consist of three parts: the fiber comprises fibers, an interface layer and a matrix, wherein the interface layer is a layer structure material of the fiber surface, the thickness of the interface layer is usually less than 1 μm, and the interface layer can play a role of deflecting cracks generated in the matrix. Typically, the interfacial layer type is pyrolytic carbon or boron nitride, which plays a decisive role in the fracture behavior of the composite, composites without or with an unreasonable design of the interfacial layer are typically brittle fractures, while a reasonably designed interfacial layer will cause the composite to exhibit ductile fractures. The preparation of the interface layer usually adopts a chemical vapor deposition method, the process needs high-temperature deposition equipment, the requirement on the deposition equipment is higher because of more byproducts and tail gas, and the post-treatment process contains waste gas, waste oil and waste water.
The PIP process is one of the ceramic matrix composite material preparation processes which are researched more and developed rapidly in recent years. The process takes a polymer liquid phase precursor (or solution) as a impregnant, and obtains a densified composite material through multi-cycle crosslinking curing and high-temperature cracking. Because the cracking process is usually accompanied with gas evolution and volume shrinkage, a plurality of pores are generated in the matrix after cracking, and a plurality of dipping-cracking processes are generally needed to achieve a more ideal densification effect. The PIP process has the advantages that: the single-phase or multi-phase ceramic with controllable components and structures can be prepared by designing precursor components; the cracking temperature is low, and the damage to the fiber in the heat treatment process is small; the method can realize near net shape forming, reduce later processing cost and prepare large components with complex shapes. The disadvantages are that: the cracking process of the polymer precursor is accompanied by large volume shrinkage, and the process can cause certain damage to fibers; the single-cycle ceramic has low yield, needs to be subjected to multi-cycle impregnation cracking treatment, and has a long manufacturing period.
Disclosure of Invention
The invention provides a preparation method for preparing a ceramic matrix composite material by an interface-layer-free process, aiming at solving the problems in the prior art, and aiming at the ceramic matrix composite material prepared by a precursor impregnation cracking process, the method reduces the cost and shortens the preparation period.
The purpose of the invention is realized by the following technical scheme:
the preparation method for preparing the ceramic matrix composite by the interface layer-free process aims at a precursor impregnation cracking process and is characterized in that: adding boron nitride powder into a polymer liquid phase precursor as an impregnant, fully and uniformly mixing, and after prepreg preparation, resin curing and high-temperature cracking are completed, densifying the ceramic matrix composite material by using the impregnant in a repeated vacuum impregnation process to finally obtain the ceramic matrix composite material without an interface layer.
In one implementation, the polymer liquid phase precursor is a liquid polycarbosilane precursor, and the mixture of the precursor and the boron nitride powder comprises the following chemical raw materials in parts by mass: 100 parts of polycarbosilane and 50-130 parts of boron nitride powder.
Further, a curing agent is added into the mixture of the precursor and the boron nitride powder, and the mass part of the curing agent is 0.2-0.5 part compared with that of the polycarbosilane.
In one implementation, the mixture of the precursor and the boron nitride powder is ball milled and mixed thoroughly for 2 hours.
In one implementation, the fibers used in the prepreg preparation are carbon fibers, silicon carbide fibers, or a mixture of the two.
In one implementation, the process parameters for curing the resin are: the curing temperature is 100-300 ℃, the curing time is 2-5 h, and the mold needs to be vacuumized in the whole process in the curing process, so that the influence of air on resin curing is avoided.
In one implementation, the pyrolysis is to place the cured composite material in a high temperature furnace for pyrolysis, wherein the pyrolysis temperature is 800-1200 ℃, and the heat preservation time is 0.2-2 h.
In one implementation, the vacuum impregnation is to put the cracked porous body into polycarbosilane for impregnation, wherein the impregnation vacuum degree is less than-0.085 MPa, and the impregnation time is 1-3 h.
In one implementation, the preparation method for preparing the ceramic matrix composite material by the interface layer-free process comprises the following steps:
step one, removing a sizing agent on the surface of a fiber: a muffle furnace is adopted for heat preservation for 1 hour at the temperature of 400-700 ℃, and a sizing agent on the surface of the fiber is removed;
step two, slurry preparation: uniformly mixing a liquid polycarbosilane precursor with boron nitride powder, and carrying out ball milling for 2 hours, wherein the weight of the polycarbosilane is 100 parts, the weight of the curing agent is 0.2-0.5 part, and the weight of the boron nitride powder is 50-130 parts;
step three, prepreg preparation: coating the slurry obtained in the second step on the surface of the fiber to prepare a prepreg;
step four, curing resin: putting the prepreg prepared in the third step into a mold for resin curing, wherein the curing temperature is 100-300 ℃, the curing time is 2-5 hours, and the mold needs to be vacuumized in the whole curing process, so that the influence of air on resin curing is avoided;
step five, pyrolysis: the cured composite material is placed in a high-temperature furnace for cracking, the cracking temperature is 800-1200 ℃, and the heat preservation time is 0.2-2 h;
step six, vacuum impregnation: dipping the cracked porous body in polycarbosilane, wherein the dipping vacuum degree is less than-0.085 MPa, and the dipping time is 1-3 h;
and seventhly, repeating the fifth step and the sixth step for four times until the cracking weight gain rate of the sample piece is less than 1%, thus obtaining the ceramic matrix composite material prepared by the interface layer-free process.
The technical scheme of the invention is characterized in that boron nitride powder is introduced into a ceramic matrix composite substrate, and the boron nitride has good lubricating effect, so that a weak interface is generated between a fiber and the substrate interface, the toughening effect is achieved, and the ceramic matrix composite material is prepared by the following three traditional systems: the fibers, interface layer and matrix become a two-system: fibers and a matrix. On one hand, the invention avoids the process flow of an interface layer in the preparation process of the composite material, thereby avoiding the need of a chemical vapor deposition high-temperature furnace in the preparation process and avoiding the waste generated in the deposition process; on the other hand, the traditional precursor impregnation cracking process is accompanied by large-volume shrinkage, and the densification can be realized only by multiple impregnation cracking processes, and the shrinkage of slurry in the cracking process can be reduced by adding the boron nitride powder into the precursor, so that the circulation efficiency is greatly improved, and the cycle efficiency is reduced to 4 times from the original 8-10 times.
The technical scheme of the invention has the advantages that:
1. the traditional precursor impregnation cracking process needs to prepare a pyrolytic carbon or boron nitride interface layer, and weak connection between fibers and a matrix is realized through the interface layer, so that the toughening effect is achieved. The invention subverts the traditional thought, realizes weak connection between the fiber and the matrix by introducing boron nitride into the matrix, and has the toughening effect. The process for preparing the composite material does not need interface layer deposition equipment, so that the equipment investment cost can be effectively reduced, and waste generated in the deposition process can be avoided;
2. according to the invention, because the boron nitride powder with lower price is added into the matrix, the consumption of the precursor can be saved, and the price of the precursor in the current market is 5000-; in addition, due to the addition of the boron nitride powder, the cycle time of the impregnation cracking can be reduced to 4 times from 8 to 10 times, the manufacturing period is effectively shortened, the loss generated by a high-temperature furnace in the impregnation cracking process can be reduced, and the corresponding production cost is reduced.
Detailed Description
The technical scheme of the invention is further detailed by combining the specific embodiments as follows:
example 1
The preparation method for preparing the ceramic matrix composite material by the interface layer-free process comprises the following steps:
(1) arranging 4 pieces of carbon fibers with the diameter of 200 multiplied by 200mm in a muffle furnace, preserving the heat for 1 hour at the temperature of 400 ℃, and removing sizing agent on the surface of the carbon fibers;
(2) putting 200g of liquid polycarbosilane precursor, 0.8g of curing agent and 140g of boron nitride powder into a ball ink tank for uniform mixing, and carrying out ball milling for 2 hours;
(3) coating the slurry obtained in the step (2) on the surface of the carbon fiber to prepare a prepreg;
(4) cutting the prepreg prepared in the step (3) into a size of 100 multiplied by 100mm, putting the prepreg into a mould of 100 multiplied by 100mm for resin curing, wherein the curing temperature is 150 ℃, the curing time is 2 hours, and the mould is vacuumized in the whole curing process;
(5) and (4) pyrolysis. Putting the cured composite material into a high-temperature furnace for cracking, wherein the cracking temperature is 1000 ℃, and the heat preservation time is 1 h;
(6) and (4) vacuum impregnation. Dipping the cracked porous body in liquid polycarbosilane, wherein the dipping vacuum degree is less than-0.085 MPa, and the dipping time is 1 h;
(7) repeating the steps (5) and (6) for four times until the cracking weight gain rate of the sample piece is less than 1%, thus preparing the interface layer-free carbon fiber reinforced ceramic matrix composite material.
Example 2
The preparation method for preparing the ceramic matrix composite material by the interface layer-free process comprises the following steps:
(1) arranging 4 pieces of silicon carbide fibers with the diameter of 200 multiplied by 200mm in a muffle furnace, preserving the heat for 1 hour at the temperature of 600 ℃, and removing a sizing agent on the surface of the carbon fibers;
(2) putting 200g of liquid polycarbosilane precursor, 0.8g of curing agent and 160g of boron nitride powder into a ball ink tank for uniform mixing, and carrying out ball milling for 2 hours;
(3) coating the slurry obtained in the step (2) on the surface of the silicon carbide fiber to prepare a prepreg;
(4) cutting the prepreg prepared in the step (3) into a size of 100 multiplied by 100mm, putting the prepreg into a mould of 100 multiplied by 100mm for resin curing, wherein the curing temperature is 150 ℃, the curing time is 2 hours, and the mould is vacuumized in the whole curing process;
(5) and (4) pyrolysis. Putting the cured composite material into a high-temperature furnace for cracking, wherein the cracking temperature is 1000 ℃, and the heat preservation time is 1 h;
(6) and (4) vacuum impregnation. Dipping the cracked porous body in liquid polycarbosilane, wherein the dipping vacuum degree is less than-0.085 MPa, and the dipping time is 1 h;
(7) repeating the steps (5) and (6) for four times until the cracking weight gain rate of the sample piece is less than 1 percent, thus preparing the interface layer-free silicon carbide fiber reinforced ceramic matrix composite.
Example 3
The preparation method for preparing the ceramic matrix composite material by the interface layer-free process comprises the following steps:
(1) placing 2 pieces of carbon fiber cloth with the thickness of 200 x 200mm and 2 pieces of silicon carbide fiber with the thickness of 200 x 200mm in a muffle furnace, preserving the heat for 1 hour at the temperature of 400 ℃, and removing a sizing agent on the surface of the fiber;
(2) putting 200g of liquid polycarbosilane precursor, 1g of curing agent and 160g of boron nitride powder into a ball ink tank for uniform mixing, and carrying out ball milling for 2 hours;
(3) coating the slurry obtained in the step (2) on the surfaces of carbon fibers and silicon carbide fibers to prepare a prepreg;
(4) cutting the prepreg prepared in the step (3) into a size of 100 multiplied by 100mm, putting the prepreg into a mould of 100 multiplied by 100mm for resin curing, wherein the curing temperature is 160 ℃, the curing time is 3 hours, and the mould is vacuumized in the whole curing process;
(5) and (4) pyrolysis. Putting the cured composite material into a high-temperature furnace for cracking, wherein the cracking temperature is 1100 ℃, and the heat preservation time is 1 h;
(6) and (4) vacuum impregnation. Dipping the cracked porous body in liquid polycarbosilane, wherein the dipping vacuum degree is less than-0.085 MPa, and the dipping time is 2 h;
(7) repeating the steps (5) and (6) for four times until the cracking weight gain rate of the sample piece is less than 1 percent, thus preparing the interface layer-free fiber reinforced ceramic matrix composite material.
Claims (9)
1. A preparation method for preparing ceramic matrix composite material by using a non-interface layer process aims at a precursor impregnation cracking process, and is characterized in that: adding boron nitride powder into a polymer liquid phase precursor as an impregnant, fully and uniformly mixing, and after prepreg preparation, resin curing and high-temperature cracking are completed, densifying the ceramic matrix composite material by using the impregnant in a repeated vacuum impregnation process to finally obtain the ceramic matrix composite material without an interface layer.
2. The method for preparing a ceramic matrix composite material according to the interface layer-free process of claim 1, wherein: the polymer liquid phase precursor is a liquid polycarbosilane precursor, and the mixture of the precursor and the boron nitride powder comprises the following chemical raw materials in parts by mass: 100 parts of polycarbosilane and 50-130 parts of boron nitride powder.
3. The method for preparing a ceramic matrix composite material according to the interface layer-free process of claim 2, wherein: and adding a curing agent into the mixture of the precursor and the boron nitride powder, wherein the mass part of the curing agent is 0.2-0.5 part compared with that of the polycarbosilane.
4. The method for preparing a ceramic matrix composite according to claim 1, 2 or 3, wherein: and fully mixing the precursor and the boron nitride powder by ball milling for 2 hours.
5. The method for preparing a ceramic matrix composite material according to the interface layer-free process of claim 1, wherein: the fibers adopted for preparing the prepreg are carbon fibers, silicon carbide fibers or a mixture of the carbon fibers and the silicon carbide fibers.
6. The method for preparing a ceramic matrix composite material according to the interface layer-free process of claim 1, wherein: the technological parameters of resin curing are as follows: the curing temperature is 100-300 ℃, the curing time is 2-5 h, and the mold needs to be vacuumized in the whole process in the curing process, so that the influence of air on resin curing is avoided.
7. The method for preparing a ceramic matrix composite material according to the interface layer-free process of claim 1, wherein: and the high-temperature cracking is to crack the cured composite material in a high-temperature furnace, wherein the cracking temperature is 800-1200 ℃, and the heat preservation time is 0.2-2 h.
8. The method for preparing a ceramic matrix composite material according to the interface layer-free process of claim 1, wherein: and in the vacuum impregnation, the cracked porous body is placed in polycarbosilane for impregnation, the impregnation vacuum degree is less than-0.085 MPa, and the impregnation time is 1-3 h.
9. The method for preparing a ceramic matrix composite material according to the interface layer-free process of claim 1, wherein: the method comprises the following steps:
step one, removing a sizing agent on the surface of a fiber: a muffle furnace is adopted for heat preservation for 1 hour at the temperature of 400-700 ℃, and a sizing agent on the surface of the fiber is removed;
step two, slurry preparation: uniformly mixing a liquid polycarbosilane precursor with boron nitride powder, and carrying out ball milling for 2 hours, wherein the weight of the polycarbosilane is 100 parts, the weight of the curing agent is 0.2-0.5 part, and the weight of the boron nitride powder is 50-130 parts;
step three, prepreg preparation: coating the slurry obtained in the second step on the surface of the fiber to prepare a prepreg;
step four, curing resin: putting the prepreg prepared in the third step into a mold for resin curing, wherein the curing temperature is 100-300 ℃, the curing time is 2-5 hours, and the mold needs to be vacuumized in the whole curing process, so that the influence of air on resin curing is avoided;
step five, pyrolysis: the cured composite material is placed in a high-temperature furnace for cracking, the cracking temperature is 800-1200 ℃, and the heat preservation time is 0.2-2 h;
step six, vacuum impregnation: dipping the cracked porous body in polycarbosilane, wherein the dipping vacuum degree is less than-0.085 MPa, and the dipping time is 1-3 h;
and seventhly, repeating the fifth step and the sixth step for four times until the cracking weight gain rate of the sample piece is less than 1%, thus obtaining the ceramic matrix composite material prepared by the interface layer-free process.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113896555A (en) * | 2021-10-26 | 2022-01-07 | 厦门大学 | Particle-reinforced fiber woven composite material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093066A (en) * | 2010-12-24 | 2011-06-15 | 中国人民解放军国防科学技术大学 | High temperature resistant broadband wave-transparent ceramic matrix composite and preparation method thereof |
| CN105474791B (en) * | 2012-12-14 | 2015-02-18 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of silicon carbide fiber reinforced ceramic matric composite |
| CN105254320A (en) * | 2015-11-13 | 2016-01-20 | 中航复合材料有限责任公司 | Preparation method of continuous oxide fiber reinforced oxide ceramic based composite |
| CN106699209A (en) * | 2016-12-26 | 2017-05-24 | 中航复合材料有限责任公司 | Preparation method of continuous alumina fiber-reinforced aluminum oxide ceramic matrix composite material |
| CN110317073A (en) * | 2019-07-09 | 2019-10-11 | 中国航发北京航空材料研究院 | A kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites |
| US10703025B1 (en) * | 2016-12-23 | 2020-07-07 | Hrl Laboratories, Llc | Methods and formulations for joining preceramic polymers in the fabrication of ceramic assemblies |
-
2020
- 2020-07-08 CN CN202010654421.1A patent/CN111892405A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093066A (en) * | 2010-12-24 | 2011-06-15 | 中国人民解放军国防科学技术大学 | High temperature resistant broadband wave-transparent ceramic matrix composite and preparation method thereof |
| CN105474791B (en) * | 2012-12-14 | 2015-02-18 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of silicon carbide fiber reinforced ceramic matric composite |
| CN105254320A (en) * | 2015-11-13 | 2016-01-20 | 中航复合材料有限责任公司 | Preparation method of continuous oxide fiber reinforced oxide ceramic based composite |
| US10703025B1 (en) * | 2016-12-23 | 2020-07-07 | Hrl Laboratories, Llc | Methods and formulations for joining preceramic polymers in the fabrication of ceramic assemblies |
| CN106699209A (en) * | 2016-12-26 | 2017-05-24 | 中航复合材料有限责任公司 | Preparation method of continuous alumina fiber-reinforced aluminum oxide ceramic matrix composite material |
| CN110317073A (en) * | 2019-07-09 | 2019-10-11 | 中国航发北京航空材料研究院 | A kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113896555A (en) * | 2021-10-26 | 2022-01-07 | 厦门大学 | Particle-reinforced fiber woven composite material and preparation method thereof |
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