CN116023163A - High-performance ceramic matrix composite material with bionic heterostructure and preparation method thereof - Google Patents
High-performance ceramic matrix composite material with bionic heterostructure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-performance ceramic matrix composite material with a bionic heterostructure, which comprises the steps of firstly mixing inorganic micro/nano sheets, inorganic sintering auxiliary agents and organic matter solution according to a certain proportion to form a series of dispersion slurry, preparing the slurry into a series of mother-of-pearl layered structure composite films with different inorganic component types or contents through a specific solution casting method, sequentially arranging and laminating the prepared films according to design requirements, sintering to prepare a porous ceramic frame, and finally pouring resin and curing after interface pretreatment to obtain the high-performance ceramic matrix composite material with the bionic heterostructure. The method can efficiently realize the simple preparation of the high-performance ceramic matrix composite material with the large-size bionic heterostructure. The method has universality and economy, and can assemble various inorganic nano/micron sheets into the high-performance ceramic matrix composite material with the bionic heterostructure.
Description
Technical Field
The invention relates to the technical field of composite structural materials, in particular to a high-performance ceramic matrix composite material with a bionic heterostructure and a preparation method thereof.
Background
The rapid development in the engineering field places increasing demands on the materials of construction. In order to meet the application requirements of complex working conditions, novel structural materials with a variety of combinations of good mechanical properties (such as low density, high strength, stiffness, hardness and toughness) are highly desirable, but these mechanical properties are often mutually exclusive and difficult to integrate into a single material. The natural biological material shows the characteristic of excellent combination of various mechanical properties by virtue of the unique multi-scale micro-nano structure and interface design. The natural biological material is connected with the multilevel heterogeneous layers by using gradient interfaces, and the heterogeneous layers with different mechanical characteristics are combined into a single biological structure material with a complex and fine structure, so that the organic combination of various mutual exclusion mechanical properties is realized. By simulating the biological structure, especially the layered structure of shell and mother-of-pearl, researchers have developed various methods to create a series of ceramic-based bionic structural materials with high mechanical properties.
However, the biomimetic structure which can be realized at present is still single, and is far from a complex fine structure (such as a heterostructure with a gradient interface) of a biological structural material, so that the performance of the realized material cannot reach an ideal level. The development and application of bionic structural materials are greatly hindered by the contradiction between the imitation of the fine biological structure and the macro preparation of the materials.
Disclosure of Invention
1. Technical problem to be solved
The invention aims to solve the problems that the bionic structure is still single and the complex fine structure of the biological structure material is far away in the prior art, and provides a high-performance ceramic matrix composite material with a bionic heterostructure and a preparation method thereof.
2. Technical proposal
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of a high-performance ceramic matrix composite material with a bionic heterostructure comprises the following steps:
step 1: mixing inorganic micron/nano sheet, inorganic sintering aid and organic matter solution in certain proportion to prepare a series of dispersion slurry with different component types or component contents;
step 2: preparing a series of mother-of-pearl layer-like structure composite films with different inorganic component types or contents from the dispersion slurry prepared in the step 1 by a specific solution casting method;
step 3: the different composite films prepared in the step 2 are arranged and laminated in sequence according to the design requirement, and then sintered to obtain a three-dimensional continuous heterostructure porous ceramic frame;
step 4: performing interface pretreatment on the porous ceramic frame obtained in the step 3, and grafting a silane coupling agent;
step 5: and (3) filling the pretreated porous ceramic frame obtained in the step (4) with a resin prepolymer for compaction, and curing to obtain the ceramic matrix composite material with the bionic heterostructure.
Preferably, in the step 1, the inorganic nano/micro sheet in the slurry is one or more of natural mineral clay sheets, boron nitride, flake glass powder and alumina micro/nano sheets with the concentration of 10-100mg/mL, wherein the natural mineral clay sheets are one or more of mica, kaolin, bentonite and montmorillonite.
Preferably, in the step 1, the inorganic sintering aid in the slurry is one or more of silicon dioxide, kaolin, titanium dioxide and aluminum oxide, and the concentration is 1-10mg/mL.
Preferably, in the step 1, the solvent in the organic solution is one or more of water, ethanol, methanol, acetone, acetic acid, hydrochloric acid, methyl formate and ethyl acetate.
Preferably, in the step 1, the organic matter in the slurry is one or more of chitosan, sodium alginate, polyvinyl alcohol, sodium carboxymethyl cellulose, lignocellulose nanofiber and bacterial cellulose nanofiber, and the concentration is 1-40mg/mL.
Preferably, the solution film casting method in the step 2 comprises one of casting, vacuum filtration, natural evaporation drying, brush coating auxiliary evaporation drying and spray coating auxiliary evaporation drying, wherein the temperature is 20-100 ℃.
Preferably, the composite film in the step 2 has a layered stacked structure imitating mother-of-pearl, and the thickness of the film is 5-500 mu m.
Preferably, the laminated composite film in the step 3 can be composite films with different component types or component contents, the arrangement sequence of the different films can be freely selected according to the requirement, the lamination pressure is 0-20MPa, and the temperature is 20-200 ℃; the sintering step temperature is 600-1600 ℃, the sintering time is 0.1-5h, and the sintering pressure is 0-100MPa.
Preferably, the interface pretreatment process of the porous ceramic frame in the step 4 comprises soaking the piranha washing liquid and grafting the silane coupling agent, wherein the soaking time of the piranha washing liquid is 0.5-2h, the concentration of the silane coupling agent is 0.1-5wt%, the reaction time is 1-5h, and the reaction temperature is 20-100 ℃.
Preferably, the resin prepolymer in the step 5 is one or more of epoxy resin, acrylic resin, cyanate resin and phenolic resin, and the method for pouring the resin prepolymer is one of a vacuum auxiliary pouring method, a hot pressing bag pouring method and an isostatic pressing method.
The invention also provides a high-performance ceramic matrix composite material with a bionic heterostructure, which is prepared by the preparation method, and the ceramic matrix composite material has the thickness of 2-200mm, has a layered stacking structure imitating mother-of-pearl, and has different component types or component contents in different areas in the thickness direction.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) According to the method, the simple preparation of the high-performance ceramic matrix composite material with the large-size bionic heterostructure can be efficiently realized. The method has universality and economy, and can assemble various inorganic nano/micron sheets into the high-performance ceramic matrix composite material with the bionic heterostructure.
(2) According to the method, the effects of adjusting different heterostructures and gradient interfaces are achieved by adjusting the types, the number and the stacking arrangement sequence of the stacked films, and the prepared bionic heterostructure ceramic matrix composite can achieve the effect of combining various mutually exclusive mechanical properties into a whole.
Drawings
FIG. 1 is a photograph of a high performance ceramic matrix composite of a biomimetic heterostructure according to the present invention;
FIG. 2 is a cross-sectional scanning electron micrograph of a high performance ceramic matrix composite of a biomimetic heterostructure in accordance with the present invention;
FIG. 3 is a cross-sectional scanning electron micrograph of a gradient structure ceramic framework of the present invention prior to resin infusion;
fig. 4 is a cross-sectional scanning electron microscope photograph of the alternate density structure ceramic frame of the present invention before resin impregnation.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Example 1:
a preparation method of a high-performance ceramic matrix composite material with a bionic heterostructure comprises the following steps:
step 1: inorganic micron/nanometer sheets, inorganic sintering auxiliary agent and organic matter solution are mixed according to a certain proportion to prepare a series of dispersion liquid slurry with different components or component contents, wherein the inorganic nanometer/nanometer sheets in the slurry are one or more of natural mineral clay sheets, boron nitride, flaky glass powder and aluminum oxide micro/nanometer sheets with the concentration of 10-100mg/mL, and the natural mineral clay sheets are one or more of mica, kaolin, bentonite and montmorillonite;
the inorganic sintering aid in the slurry is one or more of silicon dioxide, kaolin, titanium dioxide and aluminum oxide, the concentration is 1-10mg/mL, the organic matters in the slurry are one or more of chitosan, sodium alginate, polyvinyl alcohol, sodium carboxymethyl cellulose, lignocellulose nanofiber and bacterial cellulose nanofiber, and the concentration is 1-40mg/mL;
the solvent in the organic matter solution is one or more of water, ethanol, methanol, acetone, acetic acid, hydrochloric acid, methyl formate and ethyl acetate;
step 2: preparing a series of mother-of-pearl imitated layered structure composite films with different inorganic component types or contents from the dispersion slurry prepared in the step 1 by a specific solution casting method, wherein the solution casting method comprises one of casting molding, vacuum suction filtration, natural evaporation drying, brush coating auxiliary evaporation drying and spray coating auxiliary evaporation drying, the temperature is 20-100 ℃, the composite film has a mother-of-pearl imitated layered stacking structure, and the film thickness is 5-500 mu m;
step 3: the different composite films prepared in the step 2 are arranged and laminated according to the design requirement, and then sintered to obtain a three-dimensional continuous heterostructure porous ceramic frame, wherein the laminated composite films can be composite films with different component types or component contents, the arrangement order of the different films can be freely selected according to the requirement, the lamination pressure is 0-20MPa, and the temperature is 20-200 ℃; the sintering step temperature is 600-1600 ℃, the sintering time is 0.1-5h, and the sintering pressure is 0-100MPa;
step 4: carrying out interface pretreatment on the porous ceramic frame obtained in the step 3, grafting a silane coupling agent, wherein the interface pretreatment process of the porous ceramic frame comprises soaking the piranha lotion for 0.5-2h and grafting the silane coupling agent, the concentration of the silane coupling agent is 0.1-5wt%, the reaction time is 1-5h, and the reaction temperature is 20-100 ℃;
step 5: and (3) filling the pretreated porous ceramic frame obtained in the step (4) with a resin prepolymer, compacting, and curing to obtain the ceramic matrix composite material with the bionic heterostructure, wherein the resin prepolymer is one or more of epoxy resin, acrylic resin, cyanate resin and phenolic resin, and the method for pouring the resin prepolymer is one of a vacuum auxiliary pouring method, a hot pressing bag pouring method and an isostatic pressing method.
The invention also provides a high-performance ceramic matrix composite material with a bionic heterostructure, which is prepared by the preparation method, and the ceramic matrix composite material has the thickness of 2-200mm, has a layered stacking structure imitating mother-of-pearl, and has different component types or component contents in different areas in the thickness direction.
According to the method, the simple preparation of the high-performance ceramic matrix composite material with the large-size bionic heterostructure can be efficiently realized. The method has universality and economy, and can assemble various inorganic nano/micron sheets into the high-performance ceramic matrix composite material with the bionic heterostructure.
According to the method, the effects of adjusting different heterostructures and gradient interfaces are achieved by adjusting the types, the number and the stacking arrangement sequence of the stacked films, and the prepared bionic heterostructure ceramic matrix composite can achieve the effect of combining various mutually exclusive mechanical properties into a whole.
Example 2:
it has the implementation content of the above embodiments, where reference may be made to the foregoing description for specific implementation of the above embodiments, and the details of the embodiments herein are not repeated; in the embodiment of the present application, however, the difference from the above embodiment is that:
in this example, 9g of alumina micro-flakes and 1g of kaolin powder were dispersed in 400mL of bacterial cellulose nanofiber dispersion (1.25 mg/mL) and mixed by ultrasonication to obtain a mixed dispersion, wherein the mass ratio of kaolin to alumina was 1:9. the dispersion slurry was dried by self-evaporation to prepare a composite film (thickness about 100 μm) having a mother-of-pearl layered structure. And laminating and hot-pressing the obtained mother-of-pearl film at 60 ℃ under 10MPa for 4 hours.
In this example, the stacked blocks were sintered in a muffle furnace at 1600 ℃ for 3 hours to obtain a porous ceramic frame having a layered stacked structure. The porous ceramic frame obtained was soaked in the piranha lotion for half an hour, washed with water, and then treated with 1wt% of 3-trimethoxy propyl methacrylate at 60℃for 2 hours. And (3) pouring the obtained porous ceramic frame with polymethacrylic resin by using a vacuum auxiliary pouring method, and curing to obtain the homogeneous mother-of-pearl imitated layered structure ceramic matrix composite material, as shown in figure 1. The observation by using a scanning electron microscope shows that the homogeneous ceramic matrix composite material has a typical mother-of-pearl layer-like stacking structure, and is shown in figure 2.
Example 3:
it has the implementation content of the above embodiments, where reference may be made to the foregoing description for specific implementation of the above embodiments, and the details of the embodiments herein are not repeated; in the embodiment of the present application, however, the difference from the above embodiment is that:
in this example, alumina micro-flakes (9 g,8g,7 g) and kaolin powder (1 g,2g,3 g) of a certain mass were respectively dispersed in 400mL of bacterial cellulose nanofiber dispersion (1.25 mg/mL), and mixed by ultrasonic crushing to obtain a mixed dispersion, wherein the mass ratio of kaolin to alumina was 1:9,2:8,3:7 kinds of the materials. The dispersion slurry was dried by self-evaporation to prepare three composite films (thickness: about 100 μm) having a mother-of-pearl layered structure. Laminating a certain number of three mother-of-pearl imitation films, wherein the sequence of lamination is as follows from top to bottom: pure alumina flakes (thickness 0.2mm, n=1), kaolin: alumina = 3: film of 7 (n=3), kaolin: alumina = 2: film of 8 (n=3), kaolin: alumina = 1:9 (n=48), then hot-pressing at 60 ℃ under 10MPa for 4 hours.
In this example, the stacked blocks were sintered in a muffle furnace at 1600 ℃ for 3 hours to obtain a porous ceramic frame. The porous ceramic frame obtained was soaked in the piranha lotion for half an hour, washed with water, and treated with 1wt% of 3-trimethoxy propyl methacrylate at 60℃for 2 hours. And (3) pouring the polymethacrylic resin into the porous ceramic frame by using a vacuum auxiliary pouring method, and curing to obtain the final product. Observation by a scanning electron microscope shows that the ceramic frame has a typical gradient structure and a layered stacking structure imitating mother-of-pearl, and is shown in figure 3.
In the embodiment, tests on mechanical properties and the like show that the bionic ceramic matrix composite material realizes various mutually exclusive mechanical properties at the same time, and has low density (about 2.8 g/cm) 3 3.9g/cm lower than commercial alumina ceramics 3 ) High strength (bending strength of about 300MPa, comparable to commercial alumina ceramics), high toughness (bending fracture toughness of about 6.4MPa m) 1/2 3.7MPa m higher than commercial alumina ceramics 1/2 ) And a high surface hardness (about 1144kgf mm -2 Comparable to commercial alumina ceramics).
Example 4:
it has the implementation content of the above embodiments, where reference may be made to the foregoing description for specific implementation of the above embodiments, and the details of the embodiments herein are not repeated; in the embodiment of the present application, however, the difference from the above embodiment is that:
in this example, alumina micro-flakes (9 g,7 g) of a certain mass and kaolin powder (1 g,3 g) of a certain mass were respectively dispersed in 400mL of bacterial cellulose nanofiber dispersion (1.25 mg/mL), and mixed by an ultrasonic disruption method to obtain a mixed dispersion, wherein the mass ratio of kaolin to alumina was 1:9,3: 7. The dispersion slurry was dried by self-evaporation to prepare two kinds of composite films (thickness: about 100 μm) having a mother-of-pearl layered structure.
In this example, a certain number of two mother-of-pearl films were alternately laminated, and then hot-pressed at 60℃under 10MPa for 4 hours. And (3) placing the laminated blocks into a muffle furnace for sintering at 1400 ℃ for 3 hours to obtain the porous ceramic frame. Observation by a scanning electron microscope shows that the ceramic frame has a typical alternate dense and thin layered packing structure, as shown in fig. 4.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (11)
1. The preparation method of the high-performance ceramic matrix composite material with the bionic heterostructure is characterized by comprising the following steps of:
step 1: mixing inorganic micron/nano sheet, inorganic sintering aid and organic matter solution in certain proportion to prepare a series of dispersion slurry with different component types or component contents;
step 2: preparing a series of mother-of-pearl layer-like structure composite films with different inorganic component types or contents from the dispersion slurry prepared in the step 1 by a specific solution casting method;
step 3: the different composite films prepared in the step 2 are arranged and laminated in sequence according to the design requirement, and then sintered to obtain a three-dimensional continuous heterostructure porous ceramic frame;
step 4: performing interface pretreatment on the porous ceramic frame obtained in the step 3, and grafting a silane coupling agent;
step 5: and (3) filling the pretreated porous ceramic frame obtained in the step (4) with a resin prepolymer for compaction, and curing to obtain the ceramic matrix composite material with the bionic heterostructure.
2. The method for preparing the high-performance ceramic matrix composite with the bionic heterostructure according to claim 1, wherein in the step 1, the inorganic nano/micro sheets in the slurry are one or more of natural mineral clay sheets, boron nitride, sheet glass powder and alumina micro/nano sheets with various components, and the concentration is 10-100mg/mL, wherein the natural mineral clay sheets are one or more of mica, kaolin, bentonite and montmorillonite.
3. The method for preparing the high-performance ceramic matrix composite with the bionic heterostructure according to claim 1, wherein in the step 1, the inorganic sintering aid in the slurry is one or more of silicon dioxide, kaolin, titanium dioxide and aluminum oxide, and the concentration is 1-10mg/mL.
4. The method for preparing the layered nano-pore structured light high-strength heat-insulating ceramic according to claim 1, wherein in the step 1, the solvent in the organic solution is one or more of water, ethanol, methanol, acetone, acetic acid, hydrochloric acid, methyl formate and ethyl acetate.
5. The method for preparing the high-performance ceramic matrix composite with the bionic heterostructure according to claim 1, wherein in the step 1, the organic matters in the slurry are one or more of chitosan, sodium alginate, polyvinyl alcohol, sodium carboxymethyl cellulose, lignocellulose nanofibers and bacterial cellulose nanofibers, and the concentration is 1-40mg/mL.
6. The method for preparing the high-performance ceramic matrix composite with the bionic heterostructure according to claim 1, wherein the solution casting method in the step 2 comprises one of casting molding, vacuum filtration, natural evaporation drying, brush coating auxiliary evaporation drying and spraying auxiliary evaporation drying, and the temperature is 20-100 ℃.
7. The method for preparing the high-performance ceramic matrix composite with the bionic heterostructure according to claim 1, wherein the composite film in the step 2 has a layered stacking structure imitating mother-of-pearl, and the thickness of the film is 5-500 μm.
8. The preparation method of the high-performance ceramic matrix composite material with the bionic heterostructure according to claim 1, wherein the laminated composite films in the step 3 can be composite films with different component types or component contents, the arrangement order of the different films can be freely selected according to requirements, the lamination pressure is 0-20MPa, and the temperature is 20-200 ℃; the sintering step temperature is 600-1600 ℃, the sintering time is 0.1-5h, and the sintering pressure is 0-100MPa.
9. The method for preparing the high-performance ceramic matrix composite with the bionic heterostructure according to claim 1, wherein the interface pretreatment process of the porous ceramic frame in the step 4 comprises soaking the piranha lotion and grafting a silane coupling agent, wherein the soaking time of the piranha lotion is 0.5-2h, the concentration of the silane coupling agent is 0.1-5wt%, the reaction time is 1-5h, and the reaction temperature is 20-100 ℃.
10. The method for preparing the high-performance ceramic matrix composite with the bionic heterostructure according to claim 1, wherein the resin prepolymer in the step 5 is one or more of epoxy resin, acrylic resin, cyanate resin and phenolic resin, and the method for pouring the resin prepolymer is one of a vacuum auxiliary pouring method, a hot pressing bag pouring method and an isostatic pressing method.
11. A high performance ceramic matrix composite of biomimetic heterostructure, characterized in that it is produced by the method of any one of the above claims 1-10, and the ceramic matrix composite has a thickness of 2-200mm, has a layered stacking structure imitating mother of pearl, and different regions in the thickness direction have different component types or component contents.
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