CN114907103A - Mixing process for preparing interlaminar particle reinforced oxide ceramic matrix composite material - Google Patents
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Abstract
A mixing process for preparing an interlaminar particle reinforced oxide ceramic matrix composite relates to the preparation of ceramic matrix composites. Preparing interlayer particle slurry: dispersing the interlayer particles into a dispersing agent, and performing ball milling to obtain particle slurry; removing glue from oxide fiber cloth: cutting the fiber cloth, and performing heat treatment to finish the degumming process; slurry impregnation and fiber cloth lamination: laying fiber cloth, dipping the particle slurry on the fiber cloth, drying, and laminating the fiber cloth containing the slurry to obtain a prefabricated body containing interlayer particles; sol impregnation: taking the oxide sol to carry out vacuum impregnation on the preform, taking out and drying to obtain a rough blank, and placing the rough blank in a drying box for gelation; the sol heat treatment is inorganic: placing the rough blank in a high-temperature environment for inorganic preparation; repeating the impregnation-gel-heat treatment process: until a dense interlaminar particle reinforced oxide ceramic matrix composite is obtained. The closed pore rate of the prepared oxide ceramic matrix composite can be reduced, and the density and the structural uniformity of the oxide ceramic matrix composite are improved.
Description
Technical Field
The invention relates to the field of ceramic matrix composite material preparation, in particular to a mixing process for preparing an interlaminar particle reinforced oxide ceramic matrix composite material.
Background
Compared with a non-oxide fiber reinforced composite material, the continuous oxide fiber reinforced oxide matrix composite material (oxide/oxide composite material) has the advantages of oxidation resistance, high-temperature stability and low preparation cost, can be used in a high-temperature oxidation environment for a long time, and is mainly applied to high-temperature hot end structural members such as aerospace engines and the like. The oxide fiber may be classified into quartz fiber, alumina fiber and other oxide fiber according to the composition of the oxide fiber. The prior oxide matrix mainly comprises alumina, silicon oxide, mullite and other oxides, the matrix in the ceramic matrix composite mainly plays a role in transferring load, the matrix is firstly cracked when the composite is loaded, and the shear strength and the compression strength of the composite are mostly dependent on the matrix.
The preparation process of the current oxide/oxide composite material matrix mainly comprises a slurry method and a sol-gel method. The slurry method is to fill oxide powder into an oxide fiber prefabricated part by using the oxide powder as a raw material in a dipping or brushing mode, and then to perform pressureless or hot-pressing sintering to obtain the composite material. The slurry method has the advantages of simple process and short period, and is suitable for preparing the two-dimensional composite material. However, the high-temperature environment of hot-pressing sintering can damage oxide fibers, and meanwhile, if the slurry impregnation effect is poor, the density of the composite material is low, and the interlaminar shear strength of the composite material is poor. The sol-gel method uses a liquid precursor as a raw material, and finishes the densification of the composite material through a plurality of dipping-gel-heat treatment processes. The sol-gel method has lower preparation temperature, can reduce the thermal damage to the oxide fiber, has lower cost and is suitable for industrial production. However, the sol-gel method has low ceramic yield and needs a plurality of dipping-gel-heat treatment processes to realize the densification of the composite material.
In summary, the slurry method and the sol-gel method are more common methods for preparing the oxide ceramic matrix composite material, and have respective advantages and disadvantages. Therefore, in order to prepare the oxide ceramic matrix composite material with excellent performance, a new preparation system needs to be developed. Therefore, the invention provides a mixing process of the interlayer particle reinforced oxide ceramic matrix composite, which combines a slurry method and a sol-gel method, introduces interlayer particles, improves the compactness and the performance of the oxide ceramic matrix composite and simplifies the preparation process.
Disclosure of Invention
The invention aims to provide a mixing process for preparing an interlaminar particle reinforced oxide ceramic-based composite material, which can improve the compactness and the performance of the oxide ceramic-based composite material and simplify the preparation process aiming at the defects in the prior art.
The preparation method comprises the steps of firstly preparing interlayer particle slurry, alternately laminating the interlayer particle slurry and oxide fiber cloth to prepare an oxide fiber preform containing interlayer particles, and then repeating the processes of dipping, gelling and heat treatment of oxide sol to obtain the compact interlayer particle reinforced oxide ceramic matrix composite.
The invention comprises the following steps:
1) preparing interlayer particle slurry: dispersing the interlayer particles into a dispersing agent, and performing ball milling to obtain particle slurry;
2) removing glue from oxide fiber cloth: cutting the fiber cloth, and performing heat treatment to finish the degumming process;
3) slurry impregnation and fiber cloth lamination: laying fiber cloth, dipping the particle slurry on the fiber cloth, drying, and laminating and pressurizing the fiber cloth containing the slurry to obtain a prefabricated body containing interlayer particles;
4) sol impregnation-gel: taking the oxide sol to carry out vacuum impregnation on the prefabricated body, taking out the prefabricated body and drying to obtain a rough blank, and placing the rough blank in a drying box for gelation;
5) the sol heat treatment is inorganic: placing the rough blank in a high-temperature environment for heat treatment and inorganic preparation;
6) repeating the impregnation-gel-heat treatment process: repeating the impregnation-gel-heat treatment process until a dense interlaminar particle reinforced oxide ceramic matrix composite is obtained.
In the step 1), the interlayer particles can be any one or more of different ceramic particles, preferably any one or a mixture of alumina, yttria, zirconia and silica, the particle diameter is 200-400 μm, the particle diameter is uniform, and the solid fraction of the particle slurry is 50-60%.
In the step 2), the photoresist removing temperature is 600-700 ℃, and the photoresist removing time is 1-2 hours.
In step 3), the impregnation may employ any one of a vacuum impregnation method or an electrophoresis impregnation method;
the vacuum infiltration method comprises the steps of laying a layer of fiber cloth in a glass dryer, adding particle slurry, sealing, vacuumizing for 40-60 min, ultrasonically oscillating for 15-20 min, repeating for 2-3 times, taking out and drying;
the electrophoresis infiltration method comprises the steps of connecting fiber cloth with a direct current power supply cathode, placing the fiber cloth in particle slurry, connecting the interior of a container with a direct current power supply anode, switching on a power supply, infiltrating for 40-60 min, and drying;
the lamination pressurization conditions are as follows: applying a constant pressure of 20-40 MPa, and maintaining the pressure for 20-40 min.
In step 4), the oxide sol is preferably an alumina sol; the vacuum impregnation time can be 6-8 h; the drying time is 2-4 h, and the drying temperature is 200-250 ℃.
In the step 5), the heat treatment temperature is 800-1000 ℃, and the heat treatment time is 1-2 h.
In the step 6), repeating the dipping-gelling-heat treatment process until the weight of the oxide ceramic matrix composite material is increased by less than 1-2%.
The invention provides a mixing process for preparing an interlayer particle reinforced oxide ceramic matrix composite, and provides a preparation idea of a novel oxide ceramic matrix composite based on an interlayer particle reinforcing technology. The invention obtains the interlaminar particle reinforced oxide ceramic matrix composite material by preparing interlaminar particle slurry, removing glue from oxide fiber cloth, impregnating the slurry, laminating fiber cloth and repeatedly impregnating sol, gelling and carrying out heat treatment, and the invention at least comprises the following advantages:
1) the invention combines the advantages of the slurry method and the sol-gel method, and the preparation process is simple.
2) The invention fills the air holes in the fiber preform by the interlayer particles, reduces the times of dipping, gelling and heat treatment, reduces the preparation time and improves the production efficiency.
3) The invention can realize the preparation of the high-density oxide ceramic matrix composite, reduce the air hole defect in the composite and improve the performance of the composite.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Figure 2 is a sample prepared in example 1.
FIG. 3 is a photomicrograph of the stretched sample of example 1 after tensile failure.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description will be given to the specific implementation, structure, features and effects of the mixed process for preparing an inter-layer particle reinforced oxide ceramic matrix composite material according to the present invention in combination with the preferred embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The invention combines a slurry method and a sol-gel method, firstly prepares interlayer particle slurry, alternately laminates the interlayer particle slurry and oxide fiber cloth to prepare an oxide fiber preform containing interlayer particles, and then repeats the processes of dipping, gelling and heat treatment of oxide sol to obtain the compact interlayer particle reinforced oxide ceramic matrix composite material.
Example 1:
referring to fig. 1, the preparation method of this example is as follows:
(1) preparing interlayer particle slurry: silicon oxide particles (diameter: 250 μm) were dispersed in deionized water, and after ball milling, stable particle slurry was obtained with a solid fraction of 50%.
(2) Removing glue from the alumina fiber cloth: cutting the fiber cloth, and performing heat treatment at 600 ℃ in the air for 1h to finish the degumming process;
(3) slurry impregnation and fiber cloth lamination: laying out fiber cloth, dipping the particle slurry on the fiber cloth by using an electrophoretic deposition method, wherein the impregnation time is 40min, taking out, drying, laminating and pressurizing (20MPa) to obtain a preform containing interlayer particles.
(4) Sol impregnation-gel: and (3) taking the alumina sol to carry out vacuum impregnation on the preform for 6h, taking out and drying to obtain a rough blank, and placing the rough blank in a drying oven for gelation at 200 ℃, wherein the gelation time is 2 h.
(5) The sol heat treatment is inorganic: placing the rough blank in 1000 ℃ for heat treatment inorganic preparation, wherein the heat treatment is 1 h;
(6) repeating the impregnation-gel-heat treatment process: and repeating the processes of dipping, gelling and heat treatment until the weight of the composite material is increased by less than 1 percent, thus obtaining the compact interlaminar particle reinforced oxide ceramic matrix composite material.
Through detection, the density of the alumina ceramic matrix composite material obtained in the embodiment is 2.69g/cm 3 The porosity was 26% and the tensile strength was 287 MPa. See figure 2 for samples prepared in example 1. A macroscopic photograph of the stretched sample of example 1 after tensile failure is shown in fig. 3.
Example 2:
(1) preparing interlayer particle slurry: zirconium oxide particles (diameter: 230 μm) were dispersed in deionized water and ball milled to obtain a stable slurry of particles with a solid fraction of 55%.
(2) Removing glue from the alumina fiber cloth: cutting the fiber cloth, and performing heat treatment at 650 ℃ in the air for 1.5h to finish the degumming process;
(3) slurry impregnation and fiber cloth lamination: laying fiber cloth, dipping the particle slurry on the fiber cloth by an electrophoretic deposition method for 50min, taking out, drying, laminating and pressurizing (30MPa) to obtain a preform containing interlayer particles.
(4) Sol impregnation-gel: and (3) taking the alumina sol to carry out vacuum impregnation on the preform for 7h, taking out and drying to obtain a rough blank, and placing the rough blank in a drying oven for gelation at 220 ℃ for 3 h.
(5) The sol heat treatment is inorganic: placing the rough blank in 900 ℃ for heat treatment and inorganic preparation, wherein the heat treatment is 1.5 h;
(6) repeating the dipping-gel-heat treatment process: and repeating the processes of dipping, gelling and heat treatment until the weight of the composite material is increased by less than 1 percent, thus obtaining the compact interlaminar particle reinforced oxide ceramic matrix composite material.
Through detection, the density of the alumina ceramic matrix composite material obtained in the embodiment is 2.84, the porosity is 21%, and the bending strength is 298 MPa.
Example 3:
(1) preparing interlayer particle slurry: alumina particles (diameter: 250 μm) were dispersed in deionized water, and after ball milling, stable particle slurry was obtained with a solid fraction of 60% of the particle slurry.
(2) Removing glue from the alumina fiber cloth: the cut fiber cloth is subjected to heat treatment in the air at 700 ℃, the heat treatment time is 2 hours, and the degumming process is completed;
(3) slurry impregnation and fiber cloth lamination: laying out fiber cloth, dipping the particle slurry on the fiber cloth by using an electrophoretic deposition method, wherein the dipping time is 60min, taking out, drying, laminating and pressurizing (40MPa) to obtain a prefabricated body containing interlayer particles.
(4) Sol impregnation-gel: and (3) taking the alumina sol to carry out vacuum impregnation on the preform for 8h, taking out and drying to obtain a rough blank, and placing the rough blank in a drying oven for gelation at 250 ℃, wherein the gelation time is 3 h.
(5) Performing sol heat treatment to mineralize: placing the rough blank in 800 ℃ for heat treatment inorganic preparation, wherein the heat treatment time is 2 h;
(6) repeating the impregnation-gel-heat treatment process: and repeating the processes of dipping, gelling and heat treatment until the weight of the composite material is increased by less than 1 percent, thus obtaining the compact interlaminar particle reinforced oxide ceramic matrix composite material.
The density of the alumina ceramic matrix composite material obtained in the embodiment is detected to be 3.42g/cm 3 The porosity was 17%, and the bending strength was 367 MPa.
The invention combines two technologies of fiber reinforcement and particle reinforcement to prepare interlayer particle reinforced oxidationThe preparation method of the ceramic matrix composite material comprises the steps of firstly preparing interlayer particle slurry, impregnating the particle slurry on fiber cloth by using an electrophoretic deposition method or a vacuum impregnation method, and then repeating the processes of sol impregnation-gel-heat treatment until a compact oxide ceramic matrix composite material is obtained. The density of the oxide ceramic matrix composite material prepared by the invention is 2.69-3.42 g/cm 3 The porosity is 17-26%, and the bending strength is 287-367 MPa. The relative properties are shown in Table 1, in comparison with an alumina ceramic matrix composite without interlayer particles (comparative example).
TABLE 1 relevant parameters of oxide ceramic matrix composites
In conclusion, the method can combine the advantages of a slurry method and a sol-gel method, introduce interlayer particles, improve the density and performance of the composite material, reduce the cycle times of the dipping-gel-heat treatment process and improve the preparation efficiency.
It should be noted that although embodiments of the present invention have been shown and described, it would be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents. The foregoing is illustrative of some, but not all, embodiments of the invention and is not to be construed as limiting the invention in any way. Any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention, and all other embodiments obtained without inventive labor are still within the scope of the technical solution of the present invention.
Claims (10)
1. A mixing process for preparing an interlaminar particle reinforced oxide ceramic matrix composite is characterized by comprising the following steps:
1) preparing interlayer particle slurry: dispersing the interlayer particles into a dispersing agent, and performing ball milling to obtain particle slurry;
2) removing glue from oxide fiber cloth: cutting the fiber cloth, and performing heat treatment to finish the degumming process;
3) slurry impregnation and fiber cloth lamination: laying fiber cloth, dipping the particle slurry on the fiber cloth, drying, and laminating and pressurizing the fiber cloth containing the slurry to obtain a prefabricated body containing interlayer particles;
4) sol impregnation-gel: taking the oxide sol to carry out vacuum impregnation on the prefabricated body, taking out the prefabricated body and drying to obtain a rough blank, and placing the rough blank in a drying box for gelation;
5) the sol heat treatment is inorganic: placing the rough blank in a high-temperature environment for heat treatment and inorganic preparation;
6) repeating the impregnation-gel-heat treatment process: repeating the impregnation-gel-heat treatment process until a dense interlaminar particle reinforced oxide ceramic matrix composite is obtained.
2. The mixing process for preparing an interlaminar particle reinforced oxide ceramic matrix composite material according to claim 1, wherein in step 1), the interlaminar particles are any one or a combination of several different ceramic particles, preferably any one or a mixture of alumina, yttria, zirconia and silica, the particle diameter is 200-400 μm, the particle diameter is uniform, and the solid fraction of the particle slurry is 50-60%.
3. The mixing process for preparing an interlaminar particle reinforced oxide ceramic matrix composite material according to claim 1, wherein in the step 2), the temperature for removing the photoresist is 600-700 ℃, and the time for removing the photoresist is 1-2 h.
4. The hybrid process for preparing an interlaminar particle reinforced oxide ceramic matrix composite according to claim 1, wherein in step 3), the impregnation is performed by any one of vacuum infiltration or electrophoresis infiltration.
5. The mixing process for preparing an interlaminar particle reinforced oxide ceramic matrix composite according to claim 4, wherein the vacuum infiltration method comprises the steps of laying a layer of fiber cloth in a glass dryer, adding the particle slurry, sealing and vacuumizing for 40-60 min, then ultrasonically oscillating for 15-20 min, repeating for 2-3 times, taking out and drying;
the electrophoresis infiltration method comprises the steps of connecting a fiber cloth with a direct current power supply cathode, placing the fiber cloth in a particle slurry, connecting the interior of a container with a direct current power supply anode, switching on a power supply, infiltrating for 40-60 min, and drying.
6. The hybrid process for preparing an interlaminar particle reinforced oxide ceramic matrix composite according to claim 1, wherein in step 3), the stack is pressurized under the following conditions: applying a constant pressure of 20-40 MPa, and maintaining the pressure for 20-40 min.
7. The hybrid process for preparing an interlaminar particle reinforced oxide ceramic matrix composite according to claim 1, wherein in step 4), the oxide sol is an alumina sol; the vacuum impregnation time can be 6-8 h; the drying time is 2-4 h, and the drying temperature is 200-250 ℃.
8. The mixing process for preparing an interlaminar particle reinforced oxide ceramic matrix composite material according to claim 1, wherein in the step 5), the temperature of the heat treatment is 800-1000 ℃ and the time of the heat treatment is 1-2 h.
9. The hybrid process for preparing an interlaminar particle reinforced oxide ceramic matrix composite according to claim 1, wherein in step 6), the dipping-gelling-heat treatment process is repeated until the oxide ceramic matrix composite has gained less than 1% to 2% weight.
10. The interlaminar particle reinforced oxide ceramic matrix composite prepared by the mixing process according to any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116082048A (en) * | 2022-12-22 | 2023-05-09 | 上海榕融新材料技术有限公司 | Alumina continuous fiber reinforced modified ceramic matrix composite sealing ring and preparation method thereof |
| CN116082048B (en) * | 2022-12-22 | 2023-10-27 | 上海榕融新材料技术有限公司 | Alumina continuous fiber reinforced modified ceramic matrix composite sealing ring and preparation method thereof |
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