CN111875399B - Preparation method of multi-element toughened silicon carbide ceramic matrix composite - Google Patents
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Abstract
The invention belongs to the technical field of ceramic matrix composite preparation, and particularly relates to a preparation method of a multi-element toughened silicon carbide ceramic matrix composite. The method is based on a reaction infiltration process, metal Ti powder or TiC powder is mixed into matrix slurry for preparing the silicon carbide ceramic matrix composite, the metal Ti powder or TiC powder and fibers are prepared into prepreg, the prepreg and the fiber are subjected to curing and carbonization processes to obtain a porous body, then Si-B alloy is melted and infiltrated into the porous body at high temperature, and Ti or TiC reacts with C, B to generate Ti in situ in a SiC matrix3SiC2And TiB2Toughening phase to obtain the multi-element toughened fiber reinforced silicon carbide ceramic matrix composite. The method utilizes Ti3SiC2Layered structure of grains themselves, combined with TiB2The columnar structure of the crystal grains and the synergistic effect of the two toughening mechanisms further improve the toughness of the ceramic matrix composite material.
Description
Technical Field
The invention belongs to the technical field of ceramic matrix composite preparation, and particularly relates to a preparation method of a multi-element toughened silicon carbide ceramic matrix composite.
Background
The fiber reinforced silicon carbide ceramic matrix composite has a series of excellent characteristics of high specific strength, high specific modulus, high temperature resistance, ablation resistance and the like, and has wide application prospects in the fields of aviation, aerospace and the like. For certain specific application parts, materials with special functional characteristics are required, such as rotating parts of aircraft engines and the like, and composite materials with higher toughness are required. Because the SiC matrix has the characteristic of high brittleness, the defects such as cracks and the like are not weakened or deflected when the SiC matrix bears load. Therefore, from the perspective of material design, the toughening of the composite material is expected to be realized by modifying the SiC matrix.
A new ternary transition metal compound MAX phase (M: transition metal element; a: main group element; X is C or N; and N is 1 to 3) has attracted attention because of taking into consideration the characteristics of a metal material and a ceramic material. Due to its unique layered structure, when bearing load, the crack will be hindered from propagating to the layer interface and be deflected or passivated, which can effectively weaken the stress concentration at the crack tip, but the mechanical property of the MAX phase is poor, which will limit its application as a structural material alone, and therefore it is often used in combination with other structural ceramics. Representative of the MAX phase is Ti3SiC2The composite material is used as a toughening phase and is compounded with SiC, so that the toughness of the SiC is expected to be increased. At present, researches show that the adoption of a multi-component toughening phase can obtain a remarkable toughening effect. TiB2The grains are columnar, and the grains with larger length-diameter ratio can toughen the material. While TiB2With Ti3SiC2Have similar thermal expansion coefficients, thereby simultaneously introducing Ti into the SiC matrix3SiC2And TiB2The two toughening phases and the two toughening mechanisms act synergistically to ensure that the toughness of the ceramic matrix composite is remarkableAnd (4) improving.
Various means have been used to improve the toughness of silicon carbide. Application Nos. CN201810193507.1 and CN200910129807.4 Using ternary layered Ti3SiC2The toughening effect of the toughened silicon carbide ceramic matrix composite is limited because the toughening mechanism is single. The application numbers CN201710948861.6 and CN201610110058.0 and the like all utilize SiC whisker to toughen the silicon carbide ceramic matrix composite, and the SiC whisker is introduced into a silicon carbide matrix by adopting a pure mechanical mixing method, so that on one hand, the mechanical mixing has great influence on the material performance; on the other hand, the degree of densification of the composite material is difficult due to the bridging effect between the whiskers. The latter adopts an in-situ growth method to synthesize whiskers in a SiC matrix, and the whisker growth is relatively uncontrollable. In addition, the aim of toughening is achieved by introducing nano particles or carbon nano tubes into SiC, the methods adopt a mechanical mixing method to introduce a toughening phase, and in addition, the dispersion stability of the nano particles is poor.
Disclosure of Invention
The invention provides a preparation method of a multi-element toughened silicon carbide ceramic matrix composite. Aims at utilizing the reaction infiltration process to generate Ti in situ in the SiC matrix3SiC2And TiB2Two toughening phases, thereby obtaining a high-toughness matrix and realizing the toughening of the ceramic matrix composite.
The technical solution of the invention comprises the following steps:
step 1: mixing metal Ti powder or TiC powder, a powder dispersing agent, an organic solvent and high carbon residue resin, and performing ball milling for more than 12 hours to prepare mixed slurry;
and 2, step: coating the mixed slurry prepared in the step 1 on a fiber fabric containing an interface layer, and removing an organic solvent by utilizing reduced pressure evaporation to prepare a prepreg;
and 3, step 3: placing the prepreg obtained in the step 2 in a mould, and curing and molding by using a hot press, wherein the curing temperature is set to be 150-300 ℃, the pressure is set to be 0.2-12 MPa, and the time is set to be 1-5 h, so as to obtain a prefabricated body;
and 4, step 4: carbonizing the prefabricated body obtained in the step (3) at 800-1200 ℃ in an inert atmosphere for 30-120 min to obtain a porous body;
and 5: and (3) infiltrating the Si-B alloy into the porous body under the vacuum condition, wherein the infiltration temperature is 1400-1600 ℃, and the reaction time is 5-40 min, so as to obtain the fiber/SiC-Ti 3SiC2-TiB2 composite material.
The slurry comprises metal Ti powder or TiC powder, a powder dispersing agent, an organic solvent, phenolic resin and derivatives thereof in parts by mass: 10-50: 0.2-1: 50-200: 50 to 100.
The organic solvent is one or a mixture of ethanol, methanol, isopropanol, acetone, toluene, xylene, butyl acetate and ethyl acetate.
The fiber fabric is one of SiC fiber fabric and C fiber fabric.
The mass ratio of the Si powder to the B powder is 10-50: 1.
the mass ratio of the Si-B alloy to the porous body is 1-5: 1.
The grain diameter of the metal Ti powder or TiC powder is 0.5-5 mu m, and the purity is not less than 99.9%.
The purity of the silicon powder is not less than 99.9%.
The purity of the boron powder is not less than 99.9%.
The high carbon residue resin is one of phenolic resin and derivatives thereof, furan resin and derivatives thereof.
The invention has the advantages and beneficial effects that:
firstly, Ti3SiC2 and TiB2 are introduced into a SiC matrix by using an in-situ generation method, so that the compatibility of the matrix and a toughening body is good, the interface bonding strength is high, the mechanical property of the obtained material is higher than that of the obtained material by other introduction modes, and meanwhile, the process is simple and the cost is lower; TiB2, Ti3SiC2 and SiC have matched thermal expansion coefficients, so Ti3SiC2 and TiB2 are ideal SiC toughening phases; when bearing load, when the crack extends to the layer interface of the Ti3SiC2 phase, the crack deflects or passivates, the stress concentration of the crack tip can be effectively weakened, the TiB2 crystal grain generated in situ presents columnar crystal with certain length-diameter ratio, and the material toughening is effectively realized mainly by means of the mechanisms of pulling, bridging and crack deflection and the synergistic action of the toughening mechanisms; and fourthly, adding boron powder into the silicon powder, so that the corrosion of silicon to fibers can be reduced.
Detailed Description
The preparation method of the multi-element toughened silicon carbide ceramic matrix composite is described by combining the following specific examples:
example 1:
step 1: mixing 20g of metal Ti powder (the particle size is 0.5 mu m, the purity is 99.9 percent), 0.4g of powder dispersing agent, 150g of absolute ethyl alcohol and 50g of phenolic resin, and performing ball milling for 12 hours to prepare mixed slurry;
step 2: coating the mixed slurry prepared in the step 1 on a SiC fiber fabric containing an interface layer, and removing absolute ethyl alcohol by reduced pressure evaporation to prepare a prepreg;
and step 3: placing the prepreg obtained in the step 2 in a mould, and curing and molding by using a hot press, wherein the curing temperature is set to be 220 ℃, the pressure is set to be 0.2MPa, and the time is set to be 5 hours, so that a prefabricated body is obtained;
and 4, step 4: carbonizing the preform obtained in the step (3) at 1000 ℃ in an inert atmosphere for 60min to obtain a porous body;
and 5: infiltrating Si (99.99%) and B (99.99%) alloy powder with a mass ratio of 50:1 into the porous body under vacuum conditions, wherein the mass ratio of the Si-B alloy to the porous body is 5: 1. the infiltration temperature is 1400 ℃, and the reaction time is 20min, thereby obtaining the SiCf/SiC-Ti3SiC2-TiB2 composite material.
Example 2:
step 1: mixing 35g of TiC (particle size of 1 mu m and purity of 99.9%), 0.7g of powder dispersing agent, 180g of mixture of isopropanol and butyl acetate (mass ratio of 1:2) and 80g of furan resin, and performing ball milling for 24 hours to prepare mixed slurry;
step 2: coating the mixed slurry prepared in the step 1 on a C fiber fabric containing an interface layer, and removing a mixture of isopropanol and butyl acetate by reduced pressure evaporation to prepare a prepreg;
and step 3: placing the prepreg obtained in the step 2 in a mould, and curing and molding by using a hot press, wherein the curing temperature is set to be 150 ℃, the pressure is set to be 0.5MPa, and the time is set to be 2.5 hours, so that a prefabricated body is obtained;
and 4, step 4: carbonizing the prefabricated body obtained in the step (3) at 800 ℃ in an inert atmosphere for 120min to obtain a porous body;
and 5: under the vacuum condition, Si (99.99%) and B (99.99%) alloy powder with the mass ratio of 30:1 are infiltrated into the porous body, wherein the mass ratio of the Si-B alloy to the porous body is 2.5: 1. the infiltration temperature is 1600 ℃, and the reaction time is 10min, thereby obtaining the Cf/SiC-Ti3SiC2-TiB2 composite material.
Example 3:
step 1: mixing 50g of TiC (particle size 5 mu m, purity 99.9%), 1g of powder dispersing agent, 200g of dimethylbenzene and 100g of phenolic resin derivative, and performing ball milling for 30 hours to prepare mixed slurry;
step 2: coating the mixed slurry prepared in the step 1 on a SiC fiber fabric containing an interface layer, and removing xylene by reduced pressure evaporation to prepare a prepreg;
and 3, step 3: placing the prepreg obtained in the step 2 in a mould, and curing and molding by using a hot press, wherein the curing temperature is set to be 300 ℃, the pressure is set to be 12MPa, and the time is set to be 1h, so that a prefabricated body is obtained;
and 4, step 4: carbonizing the preform obtained in the step (3) at 1200 ℃ in an inert atmosphere for 30min to obtain a porous body;
and 5: infiltrating Si (99.9%) and B (99.9%) alloy powder with the mass ratio of 10:1 into the porous body under the vacuum condition, wherein the mass ratio of the Si-B alloy to the porous body is 3: 1. the infiltration temperature is 1420 ℃, and the reaction time is 40min, thereby obtaining the SiCf/SiC-Ti3SiC2-TiB2 composite material.
Claims (7)
1. The preparation method of the multi-element toughened silicon carbide ceramic matrix composite is characterized by comprising the following steps:
step 1: mixing metal Ti powder or TiC powder, a powder dispersing agent, an organic solvent and high carbon residue resin, and ball-milling for more than 12 hours to prepare mixed slurry, wherein the mass part ratio of the metal Ti powder or TiC powder, the powder dispersing agent, the organic solvent and the high carbon residue resin in the mixed slurry is as follows: 10-50: 0.2-1: 50-200: 50-100 parts;
step 2: coating the mixed slurry prepared in the step 1 on a fiber fabric containing an interface layer, and removing an organic solvent by reduced pressure evaporation to prepare a prepreg;
and step 3: placing the prepreg obtained in the step 2 in a mould, and curing and molding by using a hot press, wherein the curing temperature is set to be 150-300 ℃, the pressure is set to be 0.2-12 MPa, and the time is set to be 1-5 h, so that a prefabricated body is obtained;
and 4, step 4: carbonizing the prefabricated body obtained in the step (3) at 800-1200 ℃ in an inert atmosphere for 30-120 min to obtain a porous body;
and 5: and (5) placing the porous body obtained in the step (4) under Si and B powder, wherein the mass ratio of the Si to the B powder is 10-50: 1; under the conditions of vacuum and infiltration temperature of 1400-1600 ℃, the Si and B powder are melted to form Si-B alloy, and the mass ratio of the Si-B alloy to the porous body is 1-5: 1; permeating into the porous body, reacting for 5-40 min to obtain the fiber/SiC-Ti3SiC2-TiB2A composite material.
2. The method for preparing the multi-component toughened silicon carbide ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the organic solvent is one or a mixture of ethanol, methanol, isopropanol, acetone, toluene, xylene, butyl acetate and ethyl acetate.
3. The method for preparing the multi-component toughened silicon carbide ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the fiber fabric is one of SiC fiber fabric and C fiber fabric.
4. The method for preparing the multi-component toughened silicon carbide ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the grain diameter of the metal Ti powder or TiC powder is 0.5-5 mu m, and the purity is not less than 99.9%.
5. The method for preparing the multi-component toughened silicon carbide ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the purity of the silicon powder is not less than 99.9%.
6. The method for preparing the multi-component toughened silicon carbide ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the purity of the boron powder is not less than 99.9%.
7. The method for preparing the multi-component toughened silicon carbide ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the high carbon residue resin is one of phenolic resin and derivatives thereof, and furan resin and derivatives thereof.
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| CN113943160B (en) * | 2021-10-15 | 2022-08-09 | 中国航发北京航空材料研究院 | Preparation method of silicon carbide ceramic matrix composite with self-repairing function |
| CN114278692B (en) * | 2022-01-05 | 2022-10-04 | 中国人民解放军63963部队 | Disc brake friction pair for heavy-duty vehicle and manufacturing method thereof |
| CN114538943A (en) * | 2022-03-04 | 2022-05-27 | 南京航空航天大学 | Selective laser sintering dual-phase toughened SiC ceramic and preparation method thereof |
| CN116496097A (en) * | 2023-03-24 | 2023-07-28 | 西北工业大学 | Multi-element silicon carbide ceramic matrix composite material and preparation method thereof |
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