CN108033803B - Three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material and preparation method thereof - Google Patents
Three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) stabilizing the alumina-zirconia composite sol; (2) dipping: vacuum dipping the three-dimensional silicon carbide fiber prefabricated part in the alumina-zirconia composite sol; (3) drying the impregnated three-dimensional silicon carbide fiber prefabricated member; (4) heat treatment; (5) and (4) repeating the dipping-drying-heat treatment processes in the steps (2) to (4) until the weight of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is increased by less than 1% compared with the weight of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate in the last dipping-drying-heat treatment process, so as to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material. The three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared by the invention has the advantages of high temperature resistance, oxidation resistance, excellent mechanical property and the like.
Description
Technical Field
The invention belongs to the technical field of high-temperature-resistant fiber-reinforced ceramic matrix composite materials and preparation thereof, and particularly relates to a three-dimensional silicon carbide fiber-reinforced alumina-zirconia composite material and a preparation method thereof.
Background
The alumina-zirconia composite ceramic has the advantages of high temperature resistance, oxidation resistance, creep resistance, corrosion resistance and the like of alumina and zirconia, is an excellent high-temperature-resistant ceramic material, and is widely researched as a thermal barrier and protective coating, an aeroengine turbine blade and the like. As the monomer ceramic, the fracture toughness of the alumina-zirconia complex phase ceramic is low, and is 4-5 MPa.m in most cases1/2. The low fracture toughness makes the monomer alumina-zirconia complex phase ceramic difficult to be used as a structural material for practical application, and particularly in the occasions with large mechanical load impact and thermal shock, toughening treatment is required.
The introduction of fibers in ceramic matrices has proven to be the most effective toughening method capable of significantly improving fracture toughness. The silicon carbide fiber has high temperature resistance, oxidation resistance, high tensile strength and high modulus, is more and more emphasized as a reinforcing phase of a high-performance ceramic matrix composite material, and is particularly applied to occasions with long service life and oxidation resistance. Therefore, if the silicon carbide fiber and the alumina-zirconia complex phase ceramic can be compounded together, and the advantages of the silicon carbide fiber and the alumina-zirconia complex phase ceramic are combined, the fiber reinforced alumina-zirconia complex phase ceramic composite material with high temperature resistance, oxidation resistance, high strength and high toughness is expected to be obtained theoretically.
The fiber preform reinforced composite material can be divided into one-dimensional, two-dimensional and three-dimensional preform reinforced composite materials according to the arrangement mode of fibers in the composite material, namely the structural form of the fiber preform. The one-dimensional composite material is prepared by winding fiber bundles into non-woven cloth through slurry prepared from ceramic matrix powder (the slurry contains a binder for adhering the ceramic powder to fibers), then laying the non-woven cloth in different directions and different angles, or directly winding the non-woven cloth into a required shape in different directions and different angles, and then sintering at high temperature and under no pressure or under hot pressure. The two-dimensional composite material is obtained by adhering a ceramic matrix on the surface of fiber cloth in a manner of coating, dip-coating and the like with slurry prepared from ceramic matrix powder, laminating the fiber cloth, and then sintering at high temperature and under no pressure or under hot pressure. The three-dimensional composite material is obtained by firstly manufacturing fibers into a three-dimensional prefabricated part and then introducing a ceramic matrix into the prefabricated part by means of a gas phase method, a liquid phase method and the like. In comparison, the three-dimensional composite material has better integrity (the in-plane and interlayer performance of the one-dimensional and two-dimensional composite materials is weaker), and the designability of the fiber content and the arrangement directionality is strong, so that the three-dimensional composite material is more suitable for preparing components with complex shapes.
However, densification of three-dimensional composites is difficult to handle in one-dimensional and two-dimensional composite manufacturing processes due to the different preform structures. For the structural features of three-dimensional preforms, two densification methods are currently commonly used: firstly, heating a prefabricated member to a required temperature, introducing gaseous raw materials, diffusing the raw materials into the prefabricated member, reacting and depositing under the action of high temperature to obtain a ceramic matrix, gradually filling pores in the prefabricated member with the ceramic matrix along with the prolonging of deposition time, and continuously increasing the density, namely a gas phase method; secondly, after the prefabricated member is soaked in the liquid raw material, the prefabricated member is dried to remove the solvent, then the prefabricated member is subjected to heat treatment at high temperature to obtain a ceramic matrix, the soaking, drying and heat treatment are repeated for a plurality of periods, the pores in the prefabricated member are gradually filled with the ceramic matrix, the density is continuously increased, and the method is called as a liquid phase method. In contrast, the liquid phase method has low requirements on equipment, is insensitive to a temperature field and a chemical field in the equipment during compounding, and has more obvious advantages in the preparation of complex shapes and batch components. And for the fiber reinforced alumina-zirconia composite ceramic material, the existing gaseous raw materials suitable for depositing alumina and zirconia are too few, the deposition characteristics are not ideal enough, and the liquid raw materials are easy to obtain and have reliable performance.
For the liquid phase method, how to rapidly prepare the three-dimensional fiber preform reinforced alumina-zirconia composite ceramic material with high density and high mechanical property is a key problem to be solved, and the related key technical points comprise liquid raw material properties, an impregnation process and a heat treatment process. At present, no research report on the preparation of the three-dimensional silicon carbide fiber preform reinforced alumina-zirconia composite ceramic material by a liquid phase method is found.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material with high temperature resistance, oxidation resistance and excellent mechanical property and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material comprises the following steps:
(1) preparing alumina-zirconia composite sol: mixing Al2O3Sol and ZrO2Mixing the sol, and adding a stabilizer to obtain an alumina-zirconia composite sol;
(2) dipping: placing the three-dimensional silicon carbide fiber prefabricated part into a container, vacuumizing, sucking the alumina-zirconia composite sol obtained in the step (1), and performing vacuum impregnation to fill the alumina-zirconia composite sol into the three-dimensional silicon carbide fiber prefabricated part;
(3) and (3) drying: taking out the three-dimensional silicon carbide fiber prefabricated part and drying to remove the solvent and the stabilizing agent in the alumina-zirconia composite sol;
(4) and (3) heat treatment: carrying out heat treatment under the protection of inert atmosphere to obtain a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate;
(5) and (4) repeating the dipping-drying-heat treatment processes in the steps (2) to (4) until the weight of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is increased by less than 1% compared with the weight of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate in the last dipping-drying-heat treatment process, so as to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material.
In the above preparation method of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, preferably, in the step (1), the stabilizer includes HNO3HCl or H2SO4One or more of (a).
In the preparation method of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, the addition amount of the stabilizer is preferably 20-30% of the mass of the alumina sol.
Preferably, in the step (1), the solid content of the alumina-zirconia composite sol is 20wt% -40 wt%, the molar ratio of alumina to zirconia is 95/5-5/95, and the size of the colloidal particles of the composite sol is less than or equal to 30 nm.
In the preparation method of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, preferably, in the step (3), the drying temperature is 350-750 ℃, and the drying time is 1-6 h.
In the above method for preparing the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, preferably, in the step (2), the vacuum impregnation process conditions are as follows: the vacuum degree is less than or equal to 500Pa, and the dipping time is 4-8 h.
In the above method for preparing a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, preferably, in the step (2), after vacuum impregnation, air pressure-assisted impregnation is further performed under a set pressure, so that the alumina-zirconia composite sol is further filled in the three-dimensional silicon carbide fiber preform, and the process conditions of the air pressure-assisted impregnation are as follows: the set pressure is 2MPa to 10MPa, and the dipping time is 2h to 6 h.
In the above preparation method of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, preferably, in the step (4), the heat treatment process includes: under the protection of inert atmosphere, heating to 1100-1500 ℃ at the speed of 10-20 ℃/min, and keeping the temperature for 0.5-2 h.
Preferably, the preparation method of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material further comprises a pretreatment step of a three-dimensional silicon carbide fiber preform before the step (2), specifically: and (3) placing the three-dimensional silicon carbide fiber prefabricated part in vacuum or inert atmosphere, heating to 600-1200 ℃ at the speed of 5-15 ℃/min, and preserving heat for 1-4 h.
Preferably, the three-dimensional silicon carbide fiber preform is one or more of a three-dimensional silicon carbide fiber preform obtained by laminating and sewing silicon carbide fiber cloth, a three-dimensional silicon carbide fiber preform obtained by alternately laminating and needling silicon carbide fiber cloth and a mesh, a three-dimensional silicon carbide fiber preform with a three-dimensional five-way woven structure, a three-dimensional silicon carbide fiber preform with a two-dimensional semi-woven structure and a three-dimensional silicon carbide fiber preform with a three-dimensional four-way woven structure; the volume fraction of the silicon carbide fiber in the three-dimensional silicon carbide fiber prefabricated part is 20-55%.
As a general inventive concept, the invention further provides a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared by the preparation method, which comprises a three-dimensional silicon carbide fiber prefabricated part and alumina-zirconia composite ceramic, wherein the alumina-zirconia composite ceramic contains 5-95% of zirconia by mole, the alumina-zirconia composite ceramic is uniformly filled in pores of the three-dimensional silicon carbide fiber prefabricated part, and the porosity of the three-dimensional silicon carbide fiber prefabricated part reinforced alumina-zirconia composite ceramic material is 9-15%. .
Compared with the prior art, the invention has the advantages that:
1. the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material is prepared by a liquid phase method by taking the alumina-zirconia composite sol as a liquid raw material, the sol with high solid content and nanoscale can enable alumina-zirconia particles to be rapidly and uniformly filled into gaps in a prefabricated part, and compared with a technical route starting from a solution, the densification efficiency is high; compared with the technical route using slurry prepared from ceramic powder as a raw material, the alumina-zirconia particles have good distribution uniformity, the temperature for generating the alumina-zirconia composite ceramic is low, and the damage to fibers is small.
In the process of preparing the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, acid liquor is introduced into liquid raw material alumina-zirconia composite sol as a stabilizer, so that the problem of poor compatibility caused by obviously different hydrolysis speeds of the alumina sol and the zirconia sol is solved, the stable alumina-zirconia composite sol is obtained, and reliable raw material guarantee is provided for the preparation of the composite material. The applicant finds that, in the process of preparing the alumina-zirconia composite sol, the alumina sol and the zirconia sol are mixed and then precipitated, the precipitation destroys the monodispersion state of nano-sized colloidal particles in the sol, and the obtained particles are in a large-size aggregation state, cannot be impregnated into pores of a fiber preform, and cannot be used as a raw material of a technical route of impregnation-drying-heat treatment. In the former stage, attempts have been made to stabilize the alumina-zirconia composite sol by dilution, addition of chelating agent, etc. (the principle is to increase steric hindrance and reduce collision probability of colloidal particles), but firstly, the stabilizing effect is not ideal, and secondly, the solid content of the composite sol is reduced to a certain extent, thereby reducing the preparation efficiency of the composite material. In order to better stabilize the alumina-zirconia composite sol, the applicant carries out deep theoretical research and practical exploration on the reason of precipitation generated after the alumina sol and the zirconia sol are mixed, and the research result shows that: the alumina sol is alkaline and the zirconia sol is acidic, so when the alumina sol and the zirconia sol are mixed, the pH value is mismatched, the sol is unstable, and precipitation occurs. According to the invention, the reverse thinking is realized, and according to the hydrolysis mechanism in the synthesis process of the alumina sol and the zirconia sol, the hydrolyzed colloidal particles are partially peptized by adding the acid solution, so that the collision instability probability is reduced, and meanwhile, the pH values of the alumina sol and the zirconia sol are adjusted to the same level, so that the stability of the composite sol is obviously improved, and the solid content and the composite efficiency of the composite sol are not reduced. In addition, the viscosity of the composite sol can be reduced to a certain extent by adding the acid liquor, so that the impregnation into the fiber preform is facilitated.
The acid solution is preferably strong acid, the stabilizing effect of the strong acid on the alumina-zirconia composite sol is better than that of the weak acid, and the stabilizing effect of the nitric acid on the alumina-zirconia composite sol is optimal.
2. Because the alumina-zirconia composite sol contains the stabilizer, the stabilizer can remain in the gel in the form of acid radicals, and if the stabilizer cannot be removed completely at a lower temperature, the reaction and sintering of alumina and zirconia at a high temperature can be influenced, and simultaneously, silicon carbide fibers can be damaged. The invention chooses to remove it in the drying stage by raising the drying temperature (350-750 deg.C), in which temperature range the acid radicals will be decomposed, e.g. nitrate radicals can be decomposed to NOxAnd O2And the silicon carbide fiber is removed completely, so that the reaction and sintering shrinkage of alumina and zirconia cannot be influenced due to gas volatilization at high temperature, and the silicon carbide fiber cannot be obviously damaged.
3. Preferably, in the sol used in the invention, the alumina-zirconia is in an amorphous state and in a nanoscale, and the surface energy is very high, so that the sol has high sintering activity and provides a high-quality raw material guarantee for high-temperature heat treatment of the composite material.
4. Preferably, in the dipping stage, a mode of vacuum dipping and then air pressure auxiliary dipping is adopted, air in the gaps in the prefabricated part is firstly removed by vacuum pumping, a space is provided for the infiltration of the sol, and the sol is alumina-zirconia composite colloidal particles with nano-sized single particles uniformly dispersed and has good stability, so the sol can quickly and uniformly enter the gaps of the prefabricated part; then, the sol is promoted to further permeate into the interior of the prefabricated member through the action of external air pressure, enters some complex pore spaces of the pore channels, and even can destroy some closed pores to open pores, so that the impregnation efficiency and the filling degree are improved.
5. Preferably, on the basis of selecting the amorphous alumina-zirconia composite sol with small and stable particle size as the matrix raw material of the composite material, the heat treatment temperature is set to 1100-1500 ℃ through the research on the sintering shrinkage behavior of the alumina-zirconia, and in the temperature range, the alumina-zirconia can be converted into the alumina-zirconia composite ceramic, higher matrix density can be obtained (the capacity of the matrix for bearing load and transmitting load is improved), and finally the three-dimensional silicon carbide fiber preform reinforced alumina-zirconia composite ceramic material with excellent comprehensive performance is obtained.
In a word, the invention starts from the aspects of liquid raw material characteristics, dipping process, drying process and heat treatment temperature, obviously improves the compactness of the three-dimensional silicon carbide fiber prefabricated part reinforced alumina-zirconia complex phase ceramic composite material, not only enhances the bearing capacity of the matrix, but also enhances the load transfer capacity of the matrix, so that the prepared three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material has excellent mechanical property, high temperature resistance and oxidation resistance.
6. The three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared by the invention combines the advantages of the silicon carbide fiber, the alumina-zirconia composite ceramic and the three-dimensional prefabricated part for the first time, and the high-temperature-resistant and oxidation-resistant three-dimensional silicon carbide fiber prefabricated part reinforced alumina-zirconia composite ceramic composite material with excellent mechanical property is obtained. The mechanical property of the three-dimensional silicon carbide fiber prefabricated part is utilized to provide excellent mechanical property, particularly high fracture toughness, and the brittleness of the monomer alumina-zirconia composite ceramic is overcome; the excellent oxidation resistance of the composite material is provided by utilizing the excellent oxidation resistance of the alumina-zirconia complex phase ceramic and the silicon carbide fiber; the high temperature resistance of the composite material is provided by utilizing the high temperature resistance of the silicon carbide fiber and the high melting point of the alumina-zirconia complex phase ceramic. In addition, the porosity of the composite material is lower (9-15%), namely the content and the density of the alumina-zirconia are high, so that the composite material has excellent mechanical property, high temperature resistance and oxidation resistance.
Drawings
FIG. 1 is a photomicrograph of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite prepared in example 1 of the present invention.
Fig. 2 is a microscopic structural view of a three-dimensional silicon carbide fiber-reinforced alumina-zirconia composite material prepared in example 1 of the present invention.
FIG. 3 shows an alumina-zirconia composite sol (Al) as a base material according to the present invention2O3And ZrO2In a molar ratio of 1: 0.3) XRD pattern of the gel powder obtained by drying.
FIG. 4 shows an alumina-zirconia composite sol (Al) as a base material of the present invention2O3And ZrO2In a molar ratio of 1: 0.3) the linear shrinkage after heat treatment at different temperatures after pressing the dried gel powder into blocks.
FIG. 5 shows an alumina-zirconia composite sol (Al) as a base material according to the present invention2O3And ZrO2In a molar ratio of 1: 0.3) XRD patterns of the dried gel powder after heat treatment at different temperatures.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
Example 1:
the invention relates to a preparation method of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, which comprises the following specific process steps:
(1) selecting sol: selecting alumina-zirconia composite sol with solid phase content of 40wt% as a raw material of an alumina-zirconia composite ceramic matrix, wherein the molar ratio of alumina to zirconia is 1: 0.3, and adding HNO into the alumina-zirconia composite sol3As stabilizer, HNO3The amount added was 30% by weight of the alumina sol.
(2) Pre-treating a prefabricated part: selecting a three-dimensional silicon carbide fiber prefabricated part obtained by alternately laminating and needling silicon carbide fiber cloth and a net blank as a reinforcing phase, wherein the volume fraction of fibers in the three-dimensional silicon carbide fiber prefabricated part is 24%. And (3) placing the selected three-dimensional silicon carbide fiber prefabricated member in vacuum, heating to 600 ℃ at the speed of 5 ℃/min, preserving heat for 4 hours, and then cooling along with a furnace to finish the pretreatment of the prefabricated member.
(3) Vacuum impregnation: and (2) placing the pretreated three-dimensional silicon carbide fiber prefabricated part into a vacuum tank, vacuumizing until the vacuum degree reaches 500Pa, sucking the alumina-zirconia composite sol in the step (1) to enable the alumina-zirconia composite sol to submerge the three-dimensional silicon carbide fiber prefabricated part, and soaking for 8 hours.
(4) Air pressure assisted impregnation: and (4) moving the prefabricated member (still soaked in the sol) to a pressure kettle, inflating to 2MPa, carrying out air pressure assisted impregnation, and keeping for 6 hours.
(5) And (3) drying: the three-dimensional silicon carbide fiber preform was taken out of the sol and dried at 400 ℃ for 6h in an inert atmosphere.
(6) And (3) heat treatment: and (3) heating the dried three-dimensional silicon carbide fiber prefabricated part to 1100 ℃ at the speed of 10 ℃/min under the protection of high-purity inert gas, preserving heat for 2 hours, and then cooling along with a furnace to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate.
(7) The process is repeated: and (4) repeating the steps (3) to (6) for 30 times, detecting, and after the last treatment, obtaining the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material after the weight gain of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is 0.87% compared with the weight gain of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate after the last treatment, and finishing the composite process.
Fig. 1 is a macroscopic photograph of the three-dimensional silicon carbide fiber-reinforced alumina-zirconia composite material prepared in this example. Through detection, the porosity of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material obtained in the embodiment is 14.7%, the bending strength is 135.3MPa, and the fracture toughness is 7.9 MPa-m1/2. After heat treatment for 1h in 1500 ℃ high-temperature inert atmosphere, the strength retention rate is 97.2%; after static air oxidation at 1500 ℃ for 0.5h, the strength retention rate is 98.4%.
FIG. 2 shows the three-dimensional silicon carbide fiber reinforced alumina-alumina prepared in this exampleThe microstructure of the zirconium composite material can be seen, the composition of the zirconium composite material comprises a three-dimensional silicon carbide fiber prefabricated part and alumina-zirconia complex phase ceramic, wherein the alumina-zirconia complex phase ceramic is used as a matrix, the three-dimensional silicon carbide fiber prefabricated part is used as a reinforcing phase, and alumina-zirconia complex phase ceramic particles are sintered to form blocks and are uniformly filled in the fiber bundle, namely gaps among single fibers. In the alumina-zirconia complex phase ceramic matrix, Al2O3And ZrO2The molar ratio of (A) to (B) is 1: 0.3.
Example 2:
the invention relates to a preparation method of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, which comprises the following specific process steps:
(1) selecting sol: selecting an alumina-zirconia composite sol with the solid phase content of 30wt% as a raw material of an alumina-zirconia composite ceramic matrix, wherein the molar ratio of alumina to zirconia is 95: 5, and adding HNO into the alumina-zirconia composite sol3As stabilizer, HNO3Is added in an amount of 25% by weight of the alumina sol.
(2) Pre-treating a prefabricated part: selecting a three-dimensional silicon carbide fiber prefabricated part obtained by laminating and sewing silicon carbide fiber cloth as a reinforcing phase, wherein the volume fraction of fibers in the three-dimensional silicon carbide fiber prefabricated part is 46%. And (3) placing the selected three-dimensional silicon carbide fiber prefabricated member in vacuum, heating to 1000 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours, and then cooling along with a furnace to finish the pretreatment of the prefabricated member.
(3) Vacuum impregnation: and (2) placing the pretreated three-dimensional silicon carbide fiber prefabricated part into a vacuum tank, vacuumizing until the vacuum degree reaches 300Pa, sucking the alumina-zirconia composite sol in the step (1) to enable the alumina-zirconia composite sol to submerge the three-dimensional silicon carbide fiber prefabricated part, and soaking for 6 hours.
(4) Air pressure assisted impregnation: and (4) moving the prefabricated member (still soaked in the sol) to a pressure kettle, inflating to 4MPa, carrying out air pressure assisted impregnation, and keeping for 4 h.
(5) And (3) drying: and taking the three-dimensional silicon carbide fiber prefabricated member out of the sol, and drying the three-dimensional silicon carbide fiber prefabricated member for 2 hours at 500 ℃ in an inert atmosphere.
(6) And (3) heat treatment: and (3) heating the dried three-dimensional silicon carbide fiber prefabricated part to 1400 ℃ at the speed of 15 ℃/min under the protection of high-purity inert gas, preserving heat for 1h, and then cooling along with a furnace to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate.
(7) The process is repeated: and (4) repeating the steps (3) to (6) for 26 times, detecting, and after the last treatment, the weight gain ratio of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is 0.92% compared with the weight gain ratio after the last treatment, and obtaining the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material after the completion of the composite process.
Through detection, the porosity of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material obtained in the embodiment is 11.1%, the bending strength is 228.0MPa, and the fracture toughness is 12.4 MPa-m1/2. After heat treatment for 1h in 1500 ℃ high-temperature inert atmosphere, the strength retention rate is 96.6 percent; after static air oxidation at 1500 ℃ for 0.5h, the strength retention rate is 97.3%. The composite material comprises a three-dimensional silicon carbide fiber prefabricated part and alumina-zirconia composite ceramic, wherein the alumina-zirconia composite ceramic is used as a matrix, and Al is used as2O3The molar ratio of the ceramic to the zirconia ceramic is 95: 5, the three-dimensional silicon carbide fiber prefabricated part is a reinforcing phase, and the alumina-zirconia complex phase ceramic is uniformly filled in the gaps of the three-dimensional silicon carbide fiber prefabricated part.
Example 3:
the invention relates to a preparation method of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, which comprises the following specific process steps:
(1) selecting sol: selecting alumina-zirconia composite sol with the solid phase content of 35wt% as a raw material of an alumina-zirconia composite ceramic matrix, wherein the molar ratio of alumina to zirconia is 5: 95, and adding HNO into the alumina-zirconia composite sol3As stabilizer, HNO3The amount added was 20% by weight of the alumina sol.
(2) Pre-treating a prefabricated part: the three-dimensional silicon carbide fiber prefabricated part with a three-dimensional four-way weaving structure is selected as a reinforcing phase, and the volume fraction of fibers in the three-dimensional silicon carbide fiber prefabricated part is 51%. And (3) placing the selected three-dimensional silicon carbide fiber prefabricated member in a high-purity argon atmosphere, heating to 1200 ℃ at the speed of 15 ℃/min, preserving heat for 1h, and then cooling along with a furnace to finish the pretreatment of the prefabricated member.
(3) Vacuum impregnation: and (2) placing the pretreated three-dimensional silicon carbide fiber prefabricated part into a vacuum tank, vacuumizing until the vacuum degree reaches 100Pa, sucking the alumina-zirconia composite sol in the step (1) to enable the alumina-zirconia composite sol to submerge the three-dimensional silicon carbide fiber prefabricated part, and soaking for 4 hours.
(4) Air pressure assisted impregnation: and (4) moving the prefabricated member (still soaked in the sol) to a pressure kettle, inflating to 8MPa, carrying out air pressure assisted impregnation, and keeping for 6 hours.
(5) And (3) drying: the three-dimensional silicon carbide fiber preform was taken out of the sol and dried at 400 ℃ for 4h in an inert atmosphere.
(6) And (3) heat treatment: and (3) heating the dried three-dimensional silicon carbide fiber prefabricated part to 1500 ℃ at the speed of 15 ℃/min under the protection of high-purity inert gas, preserving the heat for 0.5h, and then cooling along with a furnace to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate.
(7) The process is repeated: and (4) repeating the steps (3) to (6) for 28 times, detecting, and after the last treatment, the weight gain ratio of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is 0.80% compared with the weight gain ratio after the last treatment, and obtaining the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material after the completion of the composite process.
Through detection, the porosity of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared in the embodiment is 13.5%, the bending strength is 260.7MPa, and the fracture toughness is 11.5 MPa-m1/2. After heat treatment for 1h in 1500 ℃ high-temperature inert atmosphere, the strength retention rate is 95.0 percent; after static air oxidation at 1500 ℃ for 0.5h, the strength retention rate is 96.3%. The composite material comprises a three-dimensional silicon carbide fiber prefabricated part and alumina-zirconia composite ceramic, wherein the alumina-zirconia composite ceramic is used as a matrix, the molar ratio of the alumina ceramic to the zirconia ceramic is 5: 95, and the three-dimensional silicon carbide fiberThe prefabricated member is a reinforcing phase, and the alumina-zirconia complex phase ceramic is uniformly filled in the gaps of the three-dimensional silicon carbide fiber prefabricated member.
Example 4:
the invention relates to a preparation method of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, which comprises the following specific process steps:
(1) selecting sol: selecting an alumina-zirconia composite sol with the solid phase content of 20wt% as a raw material of an alumina-zirconia composite ceramic matrix, wherein the molar ratio of alumina to zirconia is 1: 3, and adding HNO into the alumina-zirconia composite sol3As stabilizer, HNO3The amount added was 20% by weight of the alumina sol.
(2) Pre-treating a prefabricated part: the three-dimensional silicon carbide fiber prefabricated part with the two-dimensional semi-woven structure is selected as a reinforcing phase, and the volume fraction of fibers in the three-dimensional silicon carbide fiber prefabricated part is 43%. And (3) placing the selected three-dimensional silicon carbide fiber prefabricated member in vacuum, heating to 800 ℃ at the speed of 10 ℃/min, preserving heat for 3 hours, and then cooling along with a furnace to finish the pretreatment of the prefabricated member.
(3) Vacuum impregnation: and (2) placing the pretreated three-dimensional silicon carbide fiber prefabricated part into a vacuum tank, vacuumizing until the vacuum degree reaches 200Pa, sucking the alumina-zirconia composite sol in the step (1) to enable the alumina-zirconia composite sol to submerge the three-dimensional silicon carbide fiber prefabricated part, and soaking for 8 hours.
(4) Air pressure assisted impregnation: and (4) moving the prefabricated member (still soaked in the sol) to a pressure kettle, inflating to 10MPa, carrying out air pressure assisted impregnation, and keeping for 2 h.
(5) And (3) drying: and taking the three-dimensional silicon carbide fiber prefabricated member out of the sol, and drying the three-dimensional silicon carbide fiber prefabricated member for 1h at 700 ℃ in an inert atmosphere.
(6) And (3) heat treatment: and (3) heating the dried three-dimensional silicon carbide fiber prefabricated part to 1200 ℃ at the speed of 10 ℃/min under the protection of high-purity inert gas, preserving the heat for 1.5h, and then cooling along with the furnace to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate.
(7) The process is repeated: and (4) repeating the steps (3) to (6) for 25 times, detecting, and after the last treatment, the weight gain ratio of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is 0.96% compared with the weight gain ratio after the last treatment, and obtaining the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material after the completion of the composite process.
Through detection, the porosity of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared in the embodiment is 12.8%, the bending strength is 289.1MPa, and the fracture toughness is 12.8 MPa-m1/2. After heat treatment for 1h in 1500 ℃ high-temperature inert atmosphere, the strength retention rate is 96.8%; after being oxidized by static air at 1500 ℃ for 0.5h, the strength retention rate is 98.5 percent. The composite ceramic comprises a three-dimensional silicon carbide fiber prefabricated part and alumina-zirconia composite ceramic, wherein the alumina-zirconia composite ceramic is used as a matrix, the molar ratio of alumina to zirconia is 1: 3, the three-dimensional silicon carbide fiber prefabricated part is used as a reinforcing phase, and the alumina-zirconia composite ceramic is uniformly filled in gaps of the three-dimensional silicon carbide fiber prefabricated part.
Example 5:
the invention relates to a preparation method of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material, which comprises the following specific process steps:
(1) selecting sol: selecting an alumina-zirconia composite sol with the solid phase content of 30wt% as a raw material of an alumina-zirconia composite ceramic matrix, wherein the molar ratio of alumina to zirconia is 1: 1, and adding HNO into the alumina-zirconia composite sol3As stabilizer, HNO3The amount added was 25% by weight of the alumina sol.
(2) Pre-treating a prefabricated part: selecting a three-dimensional silicon carbide fiber prefabricated part with a three-dimensional five-direction woven structure as a reinforcing phase, wherein the volume fraction of fibers in the three-dimensional silicon carbide fiber prefabricated part is 50%. And (3) placing the selected three-dimensional silicon carbide fiber prefabricated member in a high-purity argon atmosphere, heating to 1000 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours, and then cooling along with a furnace to finish the pretreatment of the prefabricated member.
(3) Vacuum impregnation: and (2) placing the pretreated three-dimensional silicon carbide fiber prefabricated part into a vacuum tank, vacuumizing until the vacuum degree reaches 400Pa, sucking the alumina-zirconia composite sol in the step (1) to enable the alumina-zirconia composite sol to submerge the three-dimensional silicon carbide fiber prefabricated part, and soaking for 6 hours.
(4) Air pressure assisted impregnation: and (4) moving the prefabricated member (still soaked in the sol) to a pressure kettle, inflating to 6MPa, carrying out air pressure assisted impregnation, and keeping for 4 hours.
(5) And (3) drying: the three-dimensional silicon carbide fiber preform was taken out of the sol and dried at 600 ℃ for 3 hours in an inert atmosphere.
(6) And (3) heat treatment: and (3) heating the dried three-dimensional silicon carbide fiber prefabricated part to 1300 ℃ at the speed of 20 ℃/min under the protection of high-purity inert gas, preserving the heat for 1h, and then cooling along with a furnace to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate.
(7) The process is repeated: and (4) repeating the steps (3) to (6) for 24 times, detecting, and after the last treatment, the weight gain ratio of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is 0.77% compared with the weight gain ratio after the last treatment, and obtaining the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material after the completion of the composite process.
Through detection, the porosity of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared in the embodiment is 9.9%, the bending strength is 321.4MPa, and the fracture toughness is 13.7 MPa-m1/2. After heat treatment for 1h in 1500 ℃ high-temperature inert atmosphere, the strength retention rate is 97.7%; after being oxidized by static air at 1500 ℃ for 0.5h, the strength retention rate is 98.5 percent. The composite material comprises a three-dimensional silicon carbide fiber prefabricated part and alumina-zirconia composite ceramic, wherein the alumina-zirconia composite ceramic is used as a matrix, the molar ratio of the alumina ceramic to the zirconia ceramic is 1: 1, the three-dimensional silicon carbide fiber prefabricated part is used as a reinforcing phase, and the alumina-zirconia composite ceramic is uniformly filled in gaps of the three-dimensional silicon carbide fiber prefabricated part.
From examples 1 to 5, it can be seen that the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared by the preparation method of the invention has low porosity, high mechanical properties and excellent high temperature oxidation resistance.
In conclusion, the invention provides a novel material system of the three-dimensional silicon carbide fiber prefabricated part reinforced alumina-zirconia complex phase ceramic composite material by combining the advantages of the silicon carbide fiber, the alumina-zirconia complex phase ceramic and the three-dimensional prefabricated part based on the characteristics, the research current situation and the existing problems of the alumina-zirconia complex phase ceramic, and forms a preparation method capable of obtaining excellent performance.
In the preparation method, HNO is firstly added3The stable alumina-zirconia composite sol is obtained as an additive, the reliable raw material guarantee is provided for the preparation of the composite material, then the alumina-zirconia composite sol with the solid phase content of 20-40 wt% (the particle size of the colloid is less than or equal to 30 nm) is adopted as a matrix raw material, and the preparation method can prepare the alumina-zirconia composite sol with the porosity of about 10 percent, the bending strength of 321.4MPa and the fracture toughness of 13.7 MPa.m within a limited period (25 periods)1/2The three-dimensional five-way silicon carbide fiber reinforced alumina-zirconia composite ceramic material. While there is no fully corresponding other method for making a three-dimensional five-way silicon carbide fiber reinforced alumina-zirconia composite ceramic composite that is comparable, it is comparable to similar prior art: firstly, AlCl is adopted in the prior art3·6H2O or Al (NO)3)3·9H2Sol prepared from O inorganic salt is used as a matrix raw material, and a three-dimensional four-way carbon fiber reinforced alumina composite material is prepared through 13 periods of 'dipping-drying-1260 ℃ heat treatment', and the following continuous compounding process is found that the density is not increased, the porosity is about 30%, and the bending strength is only 100 MPa-150 MPa; secondly, preparing Y from organic salt containing Si and organic salt solution containing Y2SiO5The coating needs to remove a large amount of solvent and additive, the preparation efficiency is very low, and a typical parameter is that the thickness is 2 mu m after 20 times of dip-coating heat treatment. Thus, by comparison, it can be seen that the use of a high solid content alumina-zirconia composite sol as the starting material for the alumina-zirconia composite ceramic matrix has a self-evident advantage in terms of production efficiency compared to the technical route starting from solutions of organic or inorganic salts.
In addition, the microstructure of the three-dimensional silicon carbide fiber prefabricated part reinforced alumina-zirconia complex phase ceramic composite material is observed by adopting a scanning electron microscope, as shown in figure 2, the alumina-zirconia complex phase ceramic particles are sintered into blocks and are uniformly filled in the fiber bundle, namely gaps among single fibers, so that the problem of uneven distribution of slurry raw materials is avoided. Therefore, the alumina-zirconia composite sol adopted by the invention not only maintains the advantages of uniform filling of inorganic salt or organic salt solution raw materials and high-efficiency impregnation of slurry raw materials, but also overcomes the defects of low densification efficiency of inorganic salt or organic salt solution raw materials and nonuniform filling of slurry raw materials.
Then, the invention adopts a mode of vacuum impregnation firstly and then air pressure auxiliary impregnation, firstly, the air in the gap in the prefabrication is removed by vacuum pumping, and a space is provided for the infiltration of the sol; then, the sol is promoted to further permeate into the interior of the prefabricated member through the action of external air pressure, enters some complex pore spaces of the pore channels, and even can destroy some closed pores to open pores, so that the impregnation efficiency and the filling degree are improved.
Finally, in the sol used by the invention, the alumina-zirconia is in an amorphous state and is in a nano-scale state, and the surface energy of the sol is very high, so that the sol has high sintering activity. On the basis, through research on sintering shrinkage behavior of the alumina-zirconia, the heat treatment temperature is set to be 1100-1500 ℃, and in the temperature range, the alumina-zirconia is converted into the alumina-zirconia composite ceramic, higher density of a matrix can be obtained (the capacity of bearing load and transmitting load of the matrix is improved), reaction between the matrix and silicon carbide fibers cannot be caused (a chemically strong bonding interface is prevented from being formed and the mechanical property of the silicon carbide fibers is prevented from being damaged), and finally the three-dimensional silicon carbide fiber prefabricated member reinforced alumina-zirconia composite ceramic material with excellent comprehensive performance is obtained.
Carrying out XRD detection on gel powder obtained after drying the alumina-zirconia sol:
the phase composition of gel powder (the molar ratio of alumina to zirconia is 1: 0.3) is analyzed by an X-ray diffractometer of D8 Advance type under the test conditions of CuK α rays, tube current of 40mA, tube voltage of 40KV, 2 theta = 10-60 degrees and scanning speed of 4 DEG/min.
The detection result is shown in FIG. 3, which shows that: the chromatogram presents the peak characteristics of 'steamed bread', no sharp alumina or zirconia characteristic diffraction peak is presented, the alumina-zirconia gel powder dried at 700 ℃ is in a typical amorphous state, and the amorphous state has high surface energy and can promote sintering densification.
After gel powder obtained by drying the alumina-zirconia sol is pressed into blocks, the linear shrinkage condition of the gel powder after heat treatment at different temperatures is detected:
the dried alumina-zirconia gel powder (molar ratio of alumina to zirconia 1: 0.3) was placed in a 40mm diameter metal mold and pressed on a press at 100MPa into 40mm diameter and 5mm thick round pieces. And (3) putting the round block into a heat treatment furnace, carrying out heat treatment for 1 hour at different temperatures, measuring the change rate of the diameter and the thickness before and after the heat treatment, and measuring 5 points to obtain an average value as a final result.
The detection result is shown in fig. 4, and it can be seen from the figure that: after heat treatment at 1100-1500 ℃, the linear shrinkage rate is gradually increased along with the temperature rise within the range of 12-24%, wherein, when the temperature is increased from 1300 ℃ to 1400 ℃, the change of the linear shrinkage rate is very small, and the linear shrinkage rate is obviously increased from 1400 ℃ to 1500 ℃, which shows that the alumina-zirconia has better sintering activity. As can be inferred from FIG. 4, when the temperature is lower than 1100 ℃, the linear shrinkage rate after heat treatment is obviously reduced, which is not favorable for sintering densification, and the lower limit of the heat treatment temperature is selected to be 1100 ℃ in the invention; when the temperature exceeds 1500 ℃, the sintering line shrinkage rate may further increase to promote densification, but the possibility of carbothermic reduction reaction between the silicon carbide fiber and the zirconia is high, so the upper limit of the heat treatment temperature is selected to be 1500 ℃ in the invention.
Carrying out XRD detection on the alumina-zirconia gel powder after heat treatment at different temperatures:
and (2) carrying out heat treatment on the dried alumina-zirconia gel powder (the molar ratio of alumina to zirconia is 1: 0.3) at different temperatures for 1h, and then analyzing the phase composition of the powder by using a D8 advanced X-ray diffractometer under the test conditions of CuK α rays, tube current of 40mA, tube voltage of 40KV, 2 theta = 10-60 degrees and scanning speed of 4 DEG/min.
The detection result is shown in fig. 5, and it can be seen from the figure that: an alumina-zirconia composite ceramic phase is generated at 1100 ℃, an alumina phase appears at 1200 ℃, and the crystallization degree of the two phases is obviously increased along with the temperature rise. It is presumed that below 1100 ℃ it is likely to take an amorphous state, so that the lower limit of the heat treatment temperature of the present invention is 1100 ℃; the crystallization degree of the two phases is very high at 1500 ℃, and the upper limit of the heat treatment temperature of the invention is 1500 ℃ considering that the possibility of carbothermic reduction reaction between the silicon carbide fiber and the zirconia is very high after the temperature exceeds 1500 ℃.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (8)
1. A preparation method of a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material comprises the following steps:
(1) preparing alumina-zirconia composite sol: mixing Al2O3Sol and ZrO2Mixing the sol, adding a stabilizer which is HNO3HCl or H2SO4The adding amount of the stabilizer is 20-30% of the mass of the alumina sol, so as to obtain alumina-zirconia composite sol;
(2) dipping: placing the three-dimensional silicon carbide fiber prefabricated part into a container, vacuumizing, sucking the alumina-zirconia composite sol obtained in the step (1), and performing vacuum impregnation to fill the alumina-zirconia composite sol into the three-dimensional silicon carbide fiber prefabricated part;
(3) and (3) drying: taking out the three-dimensional silicon carbide fiber prefabricated part and drying to remove the solvent and the stabilizing agent in the alumina-zirconia composite sol;
(4) and (3) heat treatment: carrying out heat treatment under the protection of inert atmosphere to obtain a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate;
(5) and (4) repeating the dipping-drying-heat treatment processes in the steps (2) to (4) until the weight of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate is increased by less than 1% compared with the weight of the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material intermediate in the last dipping-drying-heat treatment process, so as to obtain the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material.
2. The method for preparing the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material according to claim 1, wherein in the step (1), the solid content in the alumina-zirconia composite sol is 20wt% to 40wt%, the molar ratio of alumina to zirconia is 95/5 to 5/95, and the size of the colloidal particles of the composite sol is less than or equal to 30 nm.
3. The method for preparing the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material according to claim 1 or 2, wherein in the step (3), the drying temperature is 350 ℃ to 750 ℃ and the drying time is 1h to 6 h.
4. The method for preparing the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material according to claim 3, wherein the vacuum impregnation in the step (2) is performed under the following process conditions: the vacuum degree is less than or equal to 500Pa, and the dipping time is 4-8 h.
5. The method for preparing the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material according to claim 4, wherein the step (2) further comprises performing air pressure assisted impregnation under a set pressure after vacuum impregnation, so that the alumina-zirconia composite sol is further filled in the three-dimensional silicon carbide fiber preform, wherein the process conditions of the air pressure assisted impregnation are as follows: the set pressure is 2MPa to 10MPa, and the dipping time is 2h to 6 h.
6. The method for preparing the three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material according to claim 4 or 5, wherein the heat treatment in the step (4) comprises the following steps: under the protection of inert atmosphere, heating to 1100-1500 ℃ at the speed of 10-20 ℃/min, and keeping the temperature for 0.5-2 h.
7. The method for preparing a three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material according to claim 6, wherein the three-dimensional silicon carbide fiber preform is one or more of a three-dimensional silicon carbide fiber preform obtained by sewing silicon carbide fiber cloth in a laminated manner, a three-dimensional silicon carbide fiber preform obtained by alternately laminating silicon carbide fiber cloth and a mesh fabric and needling, a three-dimensional silicon carbide fiber preform with a three-dimensional five-way woven structure, a three-dimensional silicon carbide fiber preform with a two-dimensional half-woven structure, and a three-dimensional silicon carbide fiber preform with a three-dimensional four-way woven structure; the volume fraction of the silicon carbide fiber in the three-dimensional silicon carbide fiber prefabricated part is 20-55%.
8. The three-dimensional silicon carbide fiber reinforced alumina-zirconia composite material prepared by the preparation method of any one of claims 1 to 7, which comprises a three-dimensional silicon carbide fiber preform and an alumina-zirconia composite ceramic, wherein the alumina-zirconia composite ceramic contains 5 to 95 mol% of zirconia, the alumina-zirconia composite ceramic is uniformly filled in pores of the three-dimensional silicon carbide fiber preform, and the porosity of the three-dimensional silicon carbide fiber preform reinforced alumina-zirconia composite ceramic composite material is 9 to 15%.
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