CN108794033B - Self-toughening fiber monolithic structure ceramic and preparation method thereof - Google Patents
Self-toughening fiber monolithic structure ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a self-toughened fiber monolithic structure ceramic, which consists of ceramic fiber cell bodies and relatively thin interface separation layers among the cell bodies, wherein the ceramic fiber cell bodies and the interface separation layers are arranged in a one-dimensional orientation mode, the interface separation layers and the fiber cell bodies are made of the same ceramic materials, and the grain size of the interface separation layer ceramic is larger than that of the fiber cell bodies. The invention also discloses a preparation method of the monolithic structure ceramic. The interface separation layer with larger crystal grains can induce the deflection, the bifurcation and the transverse expansion of cracks, and simultaneously can avoid the oxidation of the interface layer in a high-temperature environment or the stripping caused by thermal mismatch, thereby improving the reliability of the material in long-term service in the high-temperature environment.
Description
Technical Field
The invention relates to a self-toughening fiber monolithic structure ceramic and a preparation method thereof, belonging to the field of structural materials, in particular to the field of bionic structural materials.
Background
The ceramic material has excellent characteristics which are not possessed by a plurality of metal materials and high polymer materials, such as high melting point, high hardness, wear resistance, oxidation resistance, light weight, high strength and the like, and has wide application prospect as a structural material in a high-temperature environment. But the intrinsic brittleness of ceramic materials severely reduces the reliability and stability of the materials. Researchers in this field have made many years of effort to develop various ceramic toughening methods, such as phase change toughening, whisker toughening, particle dispersion toughening, biomimetic structure toughening, and the like.
In the last 80 th century, Coblenz et al (U.S. Patent 4772524[ P ]]) A fiber monolithic structure is provided by simulating a bamboo-wood structure, fibrous cell bodies are arranged according to a certain mode, and relatively thin cell interfaces are separated and integrated into a block body. The special structure can make the crack deflect and increase when the material is brokenReproduction, transverse propagation and the like, and further passivates cracks, thereby improving the fracture toughness and the fracture work of the material. Baskaran and Wang Chang' an et al (J. Am. center. Soc., 1993, 76(9): 2209-3N4/BN、Al2O3/Ni、TZP/Al2O3、Ce-TZP/Ce-TZP-Al2O3And the like, which shows that the structure can obviously improve the fracture resistance and the thermal shock resistance of the ceramic material.
However, the fiber monolithic structure ceramic is in service in a high-temperature environment for a long time, and the problem that a heterogeneous interface separation layer is oxidized or an interface layer falls off due to thermal mismatch of a fiber cell body and the interface separation layer exists, so that the long-term service reliability of a component under a high-temperature condition is influenced.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a self-toughening fiber monolithic structure ceramic with long-term high-temperature resistance and oxidation resistance and a preparation method thereof.
A self-toughened monolithic structural ceramic comprising ceramic fibre cells arranged in a one-dimensional orientation and a relatively thin interfacial separation layer between the cells, as shown in figure 1, characterised in that the interfacial separation layer and the fibre cells are of the same ceramic material to form a single component monolithic structural ceramic, and in that the grain size of the interfacial separation layer ceramic is greater than the grain size of the fibre cells, the single component monolithic structural ceramic being formed by the difference in grain size. The whole material is composed of the same ceramic with a single component, so that the material has excellent oxidation resistance under high temperature, and can avoid the problem of poor reliability caused by thermal mismatch, thereby realizing stable and reliable service under a high temperature environment for a long time.
The component of the above-mentioned fibrous monolithic structural ceramic may be Al2O3、SiC、Si3N4And ZrO2And the like.
The difference of the sizes of the ceramic grains of the fibrocyte body and the interface separation layer is the key for forming the self-toughening fiber monolithic structure, and the larger the difference is, the more beneficial the interface is to play the effect of inducing crack propagation. Thus, the grain size of the interfacial separator ceramic material is preferably more than an order of magnitude larger than the grain size of the celluloid ceramic.
In another preferred embodiment of the present invention, the diameter of the fibroid is 100 to 1200 μm, and the thickness of the interfacial separation layer is 10 to 50 μm.
The invention also provides a preparation method of the self-toughening fiber monolithic structure ceramic, which comprises the following steps:
1) preparation of ceramic cellule: the fine-grained ceramic powder is added into PVA (polyvinyl alcohol) (polymerization degree 1750 +/-50) aqueous solution to form ceramic slurry, wherein the PVA is used as an adhesive. And then, forming a ceramic fiber cell body by extruding the uniformly mixed ceramic slurry, controlling the diameter of the obtained fiber cell body through the inner diameter of an extrusion opening, and airing the extruded fiber cell body for the next operation.
2) Preparing an interfacial separation layer: dispersing coarse-grain ceramic powder with the same phase as that in the step 1) in a PVA aqueous solution to obtain interface separation layer slurry, wherein the mass ratio of the ceramic powder to the PVA is 99: 1. And then, attaching an interface separation layer of the same phase on the surface of the ceramic fiber cell body by a dipping method. The thickness of the interfacial separation layer can be controlled by the solids content of the slurry and the number of dips.
3) And (3) forming of a blank body: and arranging the dried ceramic fiber cells containing the interface separation layer in a steel mold according to one-dimensional orientation, then pressurizing to 180-250 MPa for molding, maintaining the pressure for 3-10 min, and demolding to obtain a blank of the ceramic with the self-toughening fiber monolithic structure.
4) Glue discharging and sintering: and (3) carrying out glue discharging on the obtained blank in a vacuum furnace at 500 ℃ for 1 h, sintering for 5-10 min by adopting SPS (spark plasma sintering), wherein the pressure is 25-30 MPa, and cooling and demoulding to obtain the self-toughening fiber monolithic structural ceramic. The sintering temperature is determined by the selected ceramic densification temperature.
In the step 1), the mass concentration of the PVA aqueous solution is preferably 2%, and the mass fraction of the solid phase content of the slurry is preferably 50%.
The size of the ceramic crystal grain in the step 2) is more than one order of magnitude larger than that of the ceramic crystal grain in the step 1), and the size of the ceramic crystal grain in the step 1) is less than 500 nm.
The invention has the advantages that:
the cellula body and the interface separation layer in the self-toughening fiber monolithic structure ceramic adopt the same ceramic material, and the difference is only the difference of the grain sizes. Therefore, the interface can induce the transverse propagation of cracks, and simultaneously, the interface layer can be prevented from being oxidized in a high-temperature environment or being stripped due to thermal mismatch, so that the service reliability of the material in the high-temperature environment is improved.
Drawings
FIG. 1 is a schematic representation of a self-toughening fiber monolithic structural ceramic according to the present invention.
FIG. 2 is a photomicrograph of inventive example 1.
FIG. 3 is a photomicrograph of a partial magnification of the interphase layer and the fibroplasts of example 1 of the present invention.
In the figure: 1. a ceramic cellulose cell body; 2. a ceramic interfacial separation layer.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
Example 1
Mixing nano Al2O3Adding the powder (80-200 nm) into a PVA aqueous solution with the mass concentration of 2% to form Al2O3The slurry comprises PVA (polyvinyl alcohol) serving as an adhesive, and the mass fraction of the solid phase content of the slurry is 50%. Then evenly mixing Al2O3Extruding the paste to obtain Al with the diameter of 800 mu m2O3The fibrous cell body. Mixing micron Al2O3Powder (1-3 μm) powderDispersing in water, adding PVA as binder, and adding nano Al2O3The cellucosomes are dipped in Al2O3Micron Al adhered to the surface of the cellule2O3An interfacial layer. The green body of the material is obtained through one-dimensional directional arrangement and dry pressing molding, and the molding pressure is 180 MPa. After the binder is removed, sintering is carried out for 5 min at 1250 ℃ by adopting an SPS sintering method, the pressure is 25 MPa, and the Al with the self-toughening fiber monolithic structure is successfully prepared2O3A ceramic.
Although the grains grow in the sintering process of the ceramic, the grain size difference after sintering can be realized by controlling the initial grain size of the powder, thereby forming a pre-designed fiber monolithic structure. Prepared self-toughening fiber monolithic structure Al2O3The microstructure of the ceramic in a cross section perpendicular to the axial direction of the fiber is shown in FIG. 2. Further, a photograph of a microstructure of the interfacial separation layer and the fibrocyte body partially enlarged is shown in FIG. 3. The fracture toughness of the material can reach 8.0 MPa.m1/2Is single phase Al2O3More than twice of the total amount of the antioxidant, has excellent antioxidant performance for a long time in a high-temperature aerobic environment, and greatly improves the reliability of high-temperature service.
Example 2
Based on the same design thought and preparation method, SiC and Si are respectively used3N4And ZrO2Different kinds of self-toughening fiber monolithic structural ceramics with different structural parameters are successfully prepared for raw materials. The self-toughened monolithic structural ceramic is prepared by selecting fibrocyte bodies with diameters of 100 μm, 300 μm, 500 μm and 1200 μm and interfacial separation layers with thicknesses of 10 μm, 30 μm and 50 μm. Because the ceramic interface separation layer and the fibrocyte body with the self-toughening fiber monolithic structure are both the same ceramic materials, the crack resistance of the material is improved by utilizing the coarse crystal interface separation layer to induce cracks to deflect, proliferate, transversely expand and the like, and the fracture toughness can reach 10 MPa.m1/2The above. The problem that the interface layer falls off due to oxidation of the heterogeneous interface separation layer or thermal mismatch of a cellula body and the interface separation layer can be solved, so that the service reliability of the material under a high-temperature condition is improved. At 1000 ℃ with an oxygen ringAfter the material is subjected to ambient heat treatment for 5 hours, the interface layer of the material has no cracking phenomenon, and the retention rate of the fracture toughness can reach more than 90%.
Claims (5)
1. A self-toughened monolithic ceramic structure consisting of ceramic fibre cell bodies arranged in a one-dimensional orientation and a relatively thin interfacial separation layer between the cell bodies, characterised in that the interfacial separation layer and the fibre cell bodies are of the same ceramic material and the grain size of the interfacial separation layer ceramic is greater than the grain size of the fibre cell bodies;
the preparation method comprises the following steps:
1) preparation of ceramic cellule: adding fine-grain ceramic powder into a PVA aqueous solution to form ceramic slurry, and then extruding the uniformly mixed ceramic slurry to form a ceramic cellule body; the polymerization degree of the PVA is 1750 +/-50; the concentration of the PVA aqueous solution is 2%, and the mass fraction of the solid phase content of the slurry is 50%;
2) preparing an interfacial separation layer: dispersing coarse-grain ceramic powder with the same phase as that in the step 1) in PVA aqueous solution to obtain interface separation layer slurry, and attaching an interface separation layer with the same phase to the surface of the ceramic fiber cell body by a dipping method; the mass ratio of the ceramic powder to the PVA is 99: 1;
3) and (3) forming of a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer in a steel mold according to one-dimensional orientation, then performing pressure forming, pressure maintaining and demolding to obtain a blank body of the ceramic with the self-toughening fiber monolithic structure; the pressurizing pressure is 180-250 MPa, and the pressure is maintained for 3-10 min;
4) glue discharging and sintering: removing glue from the obtained blank, sintering by adopting SPS, cooling and demoulding to obtain the self-toughening fiber monolithic structure ceramic; the conditions of rubber discharge are as follows: 500 ℃ for 1 h; the sintering conditions are as follows: 5-10 min, 25-30 Mpa.
2. The self-toughened fibrous monolithic structural ceramic of claim 1 wherein said cellules and interfacial separation layer are both Al2O3、SiC、Si 3N4 And ZrO2One kind of (1).
3. The self-toughened fibrous monolithic structural ceramic of claim 1 wherein said interfacial separation layer ceramic has a grain size more than an order of magnitude larger than the grain size of the fibrous cellular ceramic.
4. The self-toughened fibrous monolithic structural ceramic of claim 1 wherein the diameter of said cell bodies is from 100 to 1200 μm and the thickness of the interfacial separation layer is from 10 to 50 μm.
5. The self-toughened fibrous monolithic structural ceramic of claim 1 wherein the ceramic grain size in step 2) is more than one order of magnitude larger than the ceramic grain size in step 1), and wherein the ceramic grain size in step 1) is less than 500 nm.
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| CN113896553B (en) * | 2021-09-30 | 2022-11-11 | 中国人民解放军国防科技大学 | Fiber monolithic structure ultrahigh-temperature ceramic composite material and preparation method thereof |
| CN114644529A (en) * | 2022-04-25 | 2022-06-21 | 中国人民解放军陆军装甲兵学院 | Preparation process of honeycomb-shaped fiber interlayer modern ceramic |
| CN114853482B (en) * | 2022-05-11 | 2023-06-06 | 西安交通大学 | High-toughness silicon nitride nanowire/silicon nitride layered ceramic and preparation method thereof |
| CN115160004B (en) * | 2022-05-30 | 2023-04-07 | 中国人民解放军陆军装甲兵学院 | Preparation method of self-toughening fiber structure ceramic |
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| CN1232805A (en) * | 1999-05-28 | 1999-10-27 | 清华大学 | Preparation of silicon nitride-based composite material with superhigh tenacity |
| US6887569B1 (en) * | 1999-10-20 | 2005-05-03 | The Board Of Trustees Of The University | High temperature tolerant ceramic composites having porous interphases |
| WO2001053059A1 (en) * | 2000-01-21 | 2001-07-26 | The University Of Chicago | Method for fabricating ceramic composites, fibrous ceramic monoliths |
| CN107838428A (en) * | 2017-11-08 | 2018-03-27 | 吉林大学 | A kind of composite polycrystal-diamond with biomimetic features and preparation method thereof |
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