CN108794033A - A kind of self toughening fibrous monolithic ceramic structural ceramics and preparation method thereof - Google Patents

A kind of self toughening fibrous monolithic ceramic structural ceramics and preparation method thereof Download PDF

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CN108794033A
CN108794033A CN201810686037.2A CN201810686037A CN108794033A CN 108794033 A CN108794033 A CN 108794033A CN 201810686037 A CN201810686037 A CN 201810686037A CN 108794033 A CN108794033 A CN 108794033A
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ceramic
cell space
separate layer
ceramics
interface separate
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CN108794033B (en
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张永胜
苏云峰
宋俊杰
樊恒中
胡丽天
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

The present invention discloses a kind of self toughening fibrous monolithic ceramic structural ceramics, the material is made of interface separate layer relatively thin between the ceramic fibre cell space and cell space arranged by one-dimensional oriented approach, its median surface separate layer and fiber cell space are ceramic material of the same race, and the crystallite dimension of interface separate layer ceramics is more than the crystallite dimension of fiber cell space.The invention also discloses the preparation methods of monolithic structure ceramics.The larger interface separate layer of crystal grain of the present invention play induction crackle deflect, bifurcated and it is extending transversely while, it also can avoid boundary layer oxidation occurs under high temperature environment or removes caused by thermal mismatching, to improve the reliability of material long service under high temperature environment.

Description

A kind of self toughening fibrous monolithic ceramic structural ceramics and preparation method thereof
Technical field
The present invention relates to a kind of self toughening fibrous monolithic ceramic structural ceramics and preparation method thereof, belong to structural material field, special It is not bionic structure material field.
Background technology
Ceramic material has many metal materials and the height such as high-melting-point, high rigidity, wear-resistant, anti-oxidant and high-strength light Excellent specific property not available for molecular material, is with a wide range of applications as structural material under high temperature environment.But it makes pottery The intrinsic brittleness problems of ceramic material, seriously reduce the reliability and stability of material.Area research personnel are by for many years Effort has developed the method for toughening of a variety of ceramics, and e.g., transformation toughening, crystal whisker toughened, yttria stabilizator and biomimetic features increase It is tough etc..
The eighties in last century, Coblenz et al.（U.S. Patent 4772524[P]）It is proposed by imitating bamboo-wood structure Fibrous monolithic ceramic structure, fibrous cell space arrange by certain way, have relatively thin born of the same parents interface to separate and assemble one Block.Crackle deflects, is proliferated, is extending transversely etc. when this special structure can be such that material is broken, and then makes crack blunting, To improve the fracture toughness and work to break of material.Baskaran and Tsinghua University Wang Chang'an et al.（J. Am. Ceram. Soc., 1993, 76(9): 2209-2216；《High-performance multiphase composite》Publishing house of Tsinghua University, pp: 285-351, 2008）The preparation method and fracture behaviour for having extensively studied multiple system fibrous monolithic ceramic structural ceramics, are related to SiC/C, Si3N4/ BN、Al2O3/Ni、TZP/Al2O3、Ce-TZP/Ce-TZP-Al2O3Etc. systems, show that the structure is remarkably improved ceramic material Break resistance and thermal shock resistance.
However be on active service under high temperature environment for a long time, there are heterogeneous boundary separate layers to aoxidize for this kind of fibrous monolithic ceramic structural ceramics Or fiber cell space and interface separate layer the problem of because of thermal mismatching boundary layer being fallen off, to affect component under the high temperature conditions The reliability of long service.
Invention content
In order to overcome drawbacks described above, the technical problem to be solved in the present invention is to provide one kind having long-term fire-resistant oxidation resistant Self toughening fibrous monolithic ceramic structural ceramics of performance and preparation method thereof.
A kind of self toughening fibrous monolithic ceramic structural ceramics, the ceramics by the ceramic fibre cell space arranged by one-dimensional oriented approach and Relatively thin interface separate layer composition between cell space, as shown in Figure 1, which is characterized in that interface separate layer and fiber cell space are same Kind ceramic material, forms the fibrous monolithic ceramic structural ceramics of single component, and the crystallite dimension of interface separate layer ceramics is greater than fibre The crystallite dimension of Weiberg process body forms the fibrous monolithic ceramic structural ceramics of single component by the difference of crystallite dimension.Due to entire material Material be all made of the ceramics of the same race of one-component, therefore under the high temperature conditions have excellent antioxygenic property, can avoid because The problem of poor reliability that thermal mismatching causes, to realize reliable and stable military service in a high temperauture environment for a long time.
The ingredient of above-mentioned fibrous monolithic ceramic structural ceramics can be Al2O3、SiC、Si3N4And ZrO2Equal ceramic materials.
The difference of fiber cell space and interface separate layer ceramic crystalline grain size is the key that form self toughening fibrous monolithic ceramic structure, Difference is bigger, is more beneficial to the effect that induction crack propagation is played at interface.Therefore, the crystal grain of median surface separate layer ceramic material Size is more preferably greater than more than fiber cell space ceramic crystalline grain size an order of magnitude.
As another preferred embodiment of the present invention, wherein a diameter of 100 ~ 1200 μm of fiber cell space, interface separate layer Thickness is 10 ~ 50 μm.
The present invention also provides the preparation methods of self toughening fibrous monolithic ceramic structural ceramics as described above, include the following steps：
1）The preparation of ceramic fibre cell space：Superfine ceramics powder is added to PVA（Polyvinyl alcohol）（The degree of polymerization 1750 ± 50）It is water-soluble Ceramic slurry is formed in liquid, wherein PVA is as adhesive.Then uniformly mixed ceramic slurry is formed by the method extruded Ceramic fibre cell space, and the diameter of fiber cell space obtained by being controlled as the internal diameter of extrusion, after the fiber cell space of extrusion dries It can be used for operating in next step.
2）The preparation of interface separate layer：Using with step 1）The coarse-grain ceramic powder of phase jljl phase is dispersed in PVA aqueous solutions, Interface separate layer slurry is obtained, the wherein mass ratio of ceramic powder and PVA is 99:1.Ceramic fibre cell space is passed through into the side that dips again Method adheres to the interface separate layer of phase jljl phase on ceramic fibre cell space surface.By slurry solid concentration and number control can be dipped The thickness of interface separate layer.
3）The molding of green body：Ceramic fibre cell space containing interface separate layer after drying is pressed into one-dimensional orientation in steel mold Arrangement, 180 ~ 250 MPa moldings of then pressurizeing, 3 ~ 10 min of pressurize obtain self toughening fibrous monolithic ceramic structural ceramics after demoulding Green body.
4）Dumping and sintering：After gained green body in a vacuum furnace 500 DEG C of 1 h of dumping, using SPS（Plasma discharging is burnt Knot）5-10 min are sintered, pressure is 25 ~ 30 MPa, and prepared self toughening fibrous monolithic ceramic structural ceramics is obtained after cooling and demolding.It burns Junction temperature is determined by selected ceramic densifying temperature.
The step 1）In the mass concentrations of preferably PVA aqueous solutions be 2%, slurry solid concentration mass fraction is 50%.
The step 2）Middle ceramic crystalline grain size ratio step 1）More than middle ceramic crystalline grain size is order of magnitude greater, and step 1）Ceramic crystalline grain size is less than 500 nm.
It is an advantage of the invention that：
Fiber cell space and interface separate layer use ceramic material of the same race in self toughening fibrous monolithic ceramic structural ceramics of the present invention, Difference is only that crystallite dimension is different.Therefore interface is played while inducing crackle extending transversely, also can avoid boundary layer in high temperature Oxidation occurs under environment or is removed caused by thermal mismatching, to improve the reliability that material is on active service under high temperature environment.
Description of the drawings
The schematic diagram of Fig. 1 self toughening fibrous monolithic ceramic structural ceramics of the present invention.
The microphoto of Fig. 2 embodiment of the present invention 1.
The microphoto of Fig. 3 embodiment of the present invention 1 interface separate layer and fiber cell space partial enlargement.
In figure：1, ceramic fibre cell space；2, ceramic interface separate layer.
Specific implementation mode
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment Only a part of the embodiment of the invention, rather than whole embodiments.Based on the embodiments of the present invention, ordinary skill The every other embodiment that personnel obtain without making creative work, shall fall within the protection scope of the present invention.
Embodiment 1
By nanometer Al2O3Powder（80~200 nm）It is added in the PVA aqueous solutions that mass concentration is 2% and forms Al2O3Slurry, wherein PVA As adhesive, the solid concentration mass fraction of slurry is 50%.Then by uniformly mixed Al2O3Method of the slurry by extruding Squeeze out a diameter of 800 μm of Al2O3Fiber cell space.By micron Al2O3Powder（1~3 μm）Powder is dispersed in water, and PVA works are added For binder, then by nanometer Al2O3Fiber cell space is by the method dipped in Al2O3Micron Al is adhered on fiber cell space surface2O3Boundary Face layer.By one-dimensional oriented alignment, it is dry-pressing formed obtain the green body of the material, briquetting pressure is 180 MPa.It is used after dumping The method of SPS sintering is sintered 5 min at 1250 DEG C, and pressure is 25 MPa, is successfully prepared self toughening fibrous monolithic ceramic structure Al2O3Ceramics.
Although having the phenomenon that crystal grain is grown up during ceramic post sintering, burning can be realized by controlling powder initial particle The difference of crystallite dimension after knot, to form the fibrous monolithic ceramic structure being pre-designed.Prepared self toughening fibrous monolithic ceramic structure Al2O3Ceramics are as shown in Figure 2 perpendicular to the microscopic appearance of fiber axial cross section.Further, interface separate layer and fiber cell space part The microsctructural photograph of amplification is as shown in Figure 3.The material fracture toughness is up to 8.0 MPam1/2, it is single-phase Al2O3Twice with On, there is excellent antioxygenic property for a long time under high temperature aerobic environment, greatly improve the reliability of high-temperature service.
Embodiment 2
Based on same mentality of designing and preparation method, respectively with SiC, Si3N4And ZrO2It is successfully prepared variety classes for raw material The self toughening fibrous monolithic ceramic structural ceramics of Different structural parameters.Select a diameter of 100 μm, 300 μm, 500 μm and 1200 μ The fiber cell space of m, thickness are that 10 μm, 30 μm and 50 μm of interface separate layer prepares self toughening fibrous monolithic ceramic structural ceramics.By It is ceramic material of the same race in this kind of self toughening fibrous monolithic ceramic structural ceramics interface separate layer and fiber cell space, utilizes coarse-grain interface Separate layer realize induction crackle deflect, be proliferated and it is extending transversely etc. improve the break resistance of material, fracture is tough Property is up to 10 MPam1/2More than.Heterogeneous boundary separate layer oxidation or fiber cell space and interface separate layer can also be solved because of heat The problem of mismatch makes boundary layer fall off, to improve the service reliability of material under the high temperature conditions.It is aerobic at 1000 DEG C After environment is heat-treated 5h, material interface layer is without cracking phenomena, and the conservation rate of fracture toughness is up to 90% or more.

Claims (10)

1. a kind of self toughening fibrous monolithic ceramic structural ceramics, the ceramics are by the ceramic fibre cell space arranged by one-dimensional oriented approach and born of the same parents Relatively thin interface separate layer composition between body, it is characterised in that the interface separate layer and fiber cell space are ceramic material of the same race Material, and the crystallite dimension of interface separate layer ceramics is more than the crystallite dimension of fiber cell space.
2. self toughening fibrous monolithic ceramic structural ceramics as described in claim 1, it is characterised in that the fiber cell space and interface point Interlayer is Al2O3、SiC、Si3N4And ZrO2In one kind.
3. self toughening fibrous monolithic ceramic structural ceramics as described in claim 1, it is characterised in that the interface separate layer ceramics Crystallite dimension is greater than fiber cell space ceramic crystalline grain size an order of magnitude or more.
4. self toughening fibrous monolithic ceramic structural ceramics as described in claim 1, it is characterised in that the fiber cell space it is a diameter of 100 ~ 1200 μm, the thickness of interface separate layer is 10 ~ 50 μm.
5. a kind of method preparing Claims 1-4 any one of them self toughening fibrous monolithic ceramic structural ceramics, including following step Suddenly：
1）The preparation of ceramic fibre cell space：Superfine ceramics powder is added in PVA aqueous solutions and forms ceramic slurry, it then will mixing Uniform ceramic slurry forms ceramic fibre cell space by the method extruded；
2）The preparation of interface separate layer：Using with step 1）The coarse-grain ceramic powder of phase jljl phase is dispersed in PVA aqueous solutions, is obtained Interface separate layer slurry, then ceramic fibre cell space is adhered into phase jljl phase by the method dipped on ceramic fibre cell space surface Interface separate layer；
3）The molding of green body：Ceramic fibre cell space containing interface separate layer after drying is arranged in steel mold by one-dimensional orientation Then cloth is press-formed, pressurize, and the green body of self toughening fibrous monolithic ceramic structural ceramics is obtained after demoulding；
4）Dumping and sintering：It by gained green body dumping, is sintered using SPS, the self toughening fibrous monolithic ceramic is obtained after cooling and demolding Structural ceramics.
6. method as claimed in claim 5, it is characterised in that the degree of polymerization of the PVA is 1750 ± 50.
7. method as claimed in claim 5, it is characterised in that the step 1）A concentration of the 2% of middle PVA aqueous solutions, slurry is solid Phase content mass fraction is 50%；Step 2）Described in ceramic powder and PVA mass ratioes be 99:1.
8. method as claimed in claim 5, it is characterised in that the step 2）Middle ceramic crystalline grain size ratio step 1）Middle ceramics More than crystallite dimension is order of magnitude greater, and step 1）Ceramic crystalline grain size is less than 500 nm.
9. method as claimed in claim 5, it is characterised in that step 3）Described in the pressure pressurizeed be 180 ~ 250 MPa, protect Press 3 ~ 10 min.
10. method as claimed in claim 5, it is characterised in that step 4）Described in dumping condition：500 DEG C, 1 h；It is described The condition of sintering：5-10 min, 25 ~ 30 Mpa.
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CN111825448A (en) * 2020-06-18 2020-10-27 日照鼎源新材料有限公司 Method for preparing straight-through-hole zirconia ceramic with compact hole wall by wet spinning dipping method
CN111848138A (en) * 2020-06-18 2020-10-30 日照鼎源新材料有限公司 Wet spinning-dipping process for preparing straight-through hole alumina ceramic with compact hole wall
CN111848208A (en) * 2020-06-18 2020-10-30 日照鼎源新材料有限公司 Wet spinning coextrusion preparation of straight-through hole zirconia ceramic with compact hole wall
CN111848158A (en) * 2020-06-18 2020-10-30 日照鼎源新材料有限公司 Method for preparing straight-through-hole zirconia ceramic with compact hole wall by wet spinning coextrusion
CN111875407A (en) * 2020-06-18 2020-11-03 日照鼎源新材料有限公司 Wet spinning coextrusion preparation of straight-through hole alumina ceramic with compact hole wall
CN111892406A (en) * 2020-06-18 2020-11-06 山东理工大学 Preparation of weak interface fiber monolithic zirconium boride ultra-high temperature ceramic by wet spinning-dipping method
CN111892407A (en) * 2020-06-18 2020-11-06 山东理工大学 Wet spinning-dipping method for preparing double-interface fiber monolithic zirconium boride composite material
CN112898038A (en) * 2021-03-22 2021-06-04 河海大学 Preparation method of silicon nitride-based fiber monolithic ceramic wave-transmitting material
CN113149688A (en) * 2020-01-23 2021-07-23 上海交通大学 Composite ceramic with honeycomb fiber structure and preparation method thereof
CN113511913A (en) * 2021-04-27 2021-10-19 中国科学院兰州化学物理研究所 Bionic fiber monolithic structure boron nitride high-temperature self-lubricating material and preparation method thereof
CN113896553A (en) * 2021-09-30 2022-01-07 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
CN114853482A (en) * 2022-05-11 2022-08-05 西安交通大学 High-toughness silicon nitride nanowire/silicon nitride layered ceramic and preparation method thereof
CN115160004A (en) * 2022-05-30 2022-10-11 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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CN113149688A (en) * 2020-01-23 2021-07-23 上海交通大学 Composite ceramic with honeycomb fiber structure and preparation method thereof
CN111825448B (en) * 2020-06-18 2022-06-17 日照鼎源新材料有限公司 Method for preparing straight-through-hole zirconia ceramic with compact hole wall by wet spinning dipping method
CN111848138B (en) * 2020-06-18 2022-06-17 日照鼎源新材料有限公司 Wet spinning-dipping process for preparing straight-through hole alumina ceramic with compact hole wall
CN111892406B (en) * 2020-06-18 2022-06-07 山东理工大学 Preparation of weak interface fiber monolithic zirconium boride ultra-high temperature ceramic by wet spinning-dipping method
CN111875407A (en) * 2020-06-18 2020-11-03 日照鼎源新材料有限公司 Wet spinning coextrusion preparation of straight-through hole alumina ceramic with compact hole wall
CN111892406A (en) * 2020-06-18 2020-11-06 山东理工大学 Preparation of weak interface fiber monolithic zirconium boride ultra-high temperature ceramic by wet spinning-dipping method
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CN111848208A (en) * 2020-06-18 2020-10-30 日照鼎源新材料有限公司 Wet spinning coextrusion preparation of straight-through hole zirconia ceramic with compact hole wall
CN111848138A (en) * 2020-06-18 2020-10-30 日照鼎源新材料有限公司 Wet spinning-dipping process for preparing straight-through hole alumina ceramic with compact hole wall
CN111892407B (en) * 2020-06-18 2022-06-07 山东理工大学 Wet spinning-dipping method for preparing double-interface fiber monolithic zirconium boride composite material
CN111848158B (en) * 2020-06-18 2022-10-04 日照鼎源新材料有限公司 Method for preparing straight-through-hole zirconia ceramic with compact hole wall by wet spinning coextrusion
CN111825448A (en) * 2020-06-18 2020-10-27 日照鼎源新材料有限公司 Method for preparing straight-through-hole zirconia ceramic with compact hole wall by wet spinning dipping method
CN111848158A (en) * 2020-06-18 2020-10-30 日照鼎源新材料有限公司 Method for preparing straight-through-hole zirconia ceramic with compact hole wall by wet spinning coextrusion
CN112898038A (en) * 2021-03-22 2021-06-04 河海大学 Preparation method of silicon nitride-based fiber monolithic ceramic wave-transmitting material
CN112898038B (en) * 2021-03-22 2022-06-10 河海大学 Preparation method of silicon nitride-based fiber monolithic ceramic wave-transmitting material
CN113511913A (en) * 2021-04-27 2021-10-19 中国科学院兰州化学物理研究所 Bionic fiber monolithic structure boron nitride high-temperature self-lubricating material and preparation method thereof
CN113511913B (en) * 2021-04-27 2022-09-23 中国科学院兰州化学物理研究所 Bionic fiber monolithic structure boron nitride high-temperature self-lubricating material and preparation method thereof
CN113896553A (en) * 2021-09-30 2022-01-07 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
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
CN114853482A (en) * 2022-05-11 2022-08-05 西安交通大学 High-toughness silicon nitride nanowire/silicon nitride layered ceramic and preparation method thereof
CN115160004A (en) * 2022-05-30 2022-10-11 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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