CN115160004B - Preparation method of self-toughening fiber structure ceramic - Google Patents

Preparation method of self-toughening fiber structure ceramic Download PDF

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Publication number
CN115160004B
CN115160004B CN202210602254.5A CN202210602254A CN115160004B CN 115160004 B CN115160004 B CN 115160004B CN 202210602254 A CN202210602254 A CN 202210602254A CN 115160004 B CN115160004 B CN 115160004B
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ceramic
adhesive
self
separation layer
aqueous solution
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CN115160004A (en
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唐修检
吴秀鹏
刘谦
徐舟毅
谢凤宽
张永东
何小冰
汪志军
刘金松
胡贵林
蒋坤鹏
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Academy of Armored Forces of PLA
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Abstract

The invention belongs to the technical field of ceramic materials, and discloses a preparation method of self-toughening fiber structure ceramic. The method comprises the following steps: (1) preparation of ceramic cellula: adding nano fine-grain ceramic powder and an adhesive into an aqueous solution to form ceramic slurry, and extruding to form a ceramic fiber cell body; (2) preparation of an interfacial separation layer: dispersing micron fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain slurry of an interface separation layer, immersing the slurry into a ceramic fiber cell body, attaching the interface separation layer, and drying; (3) forming a blank; and (4) removing the glue and sintering. The method has simple process, the fracture toughness of the obtained ceramic is further improved, the bending strength and the thermal conductivity are also higher, and the method can be applied to a wider range.

Description

Preparation method of self-toughening fiber structure ceramic
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a preparation method of self-toughening fiber structure ceramic.
Background
The engineering ceramic has the advantages of corrosion resistance, high temperature resistance, wear resistance, low density and the like, and has wide application prospects in the fields of aerospace, national defense and military industry, engineering machinery and the like. However, the engineering ceramics have poor reliability and damage resistance due to the characteristics of large brittleness and low toughness. Improving the toughness of engineering ceramics is always a focus and hot spot of attention of scientific researchers and engineering technicians. Inspired by the characteristics of uneven distribution, loose inner layer and compact outer layer of natural bamboo wood, research and development personnel imagine to start from a bionic concept, design novel ceramic based on a bionic structure, change the single structure of the ceramic through the fine combination of simple components and complex structure, and improve the toughness of the ceramic, thereby improving the brittle nature of the ceramic material to a great extent.
For example, the prior art CN108794033A discloses a self-toughened monolithic ceramic structure, which is composed of ceramic fiber cells arranged in a one-dimensional orientation manner and a relatively thin interfacial separation layer between the cells, wherein the interfacial separation layer and the fiber cells are made of the same ceramic material, and the grain size of the interfacial separation layer ceramic is larger than that of the fiber cells. However, the invention uses the interaction of different structural units to make cracks deflect repeatedly in different structural layers, thereby consuming a large amount of fracture energy, only improving the possibility of long-term service of the material, and having limited improvement on the material performance, and the material has low bending strength and thermal conductivity, so that the application field is limited.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provides a preparation method of self-toughening fiber structure ceramic, the method has simple process, the fracture toughness of the obtained ceramic is further improved, the bending strength and the thermal conductivity are higher, and the application range is wider.
To achieve the object of the present invention, the method for preparing the self-toughening fiber structure ceramic of the present invention comprises the following steps:
(1) Preparation of ceramic cellule: adding nano fine-grain ceramic powder and an adhesive into an aqueous solution to form ceramic slurry, and forming a ceramic fiber cell body by an extrusion method;
(2) Preparing an interfacial separation layer: dispersing micron fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separation layer slurry, immersing the ceramic cellulums obtained in the step (1) in the interface separation layer slurry, attaching an interface separation layer, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer in the steel mould according to one-dimensional orientation, then carrying out pressure forming, and carrying out pressure maintaining demoulding to obtain a blank body of the self-toughening fiber structure ceramic;
(4) Glue discharging and sintering: and (3) performing heat preservation and glue discharge on the obtained blank in a nitrogen environment at 480-600 ℃, then performing heat preservation at 450-550 ℃ to remove the remaining carbide, sintering for 5-10min by adopting a discharge plasma sintering method under the pressure of 25-30MPa, and cooling and demolding.
Further, in some embodiments of the present invention, the ceramic powder in the step (1) and the step (2) is Al 2 O 3 、SiC、Y 2 O 3 、AlN、Si 3 N 4 And ZrO 2 Preferably Al 2 O 3 。
Further, in some embodiments of the present invention, the size of the fine crystalline ceramic powder in the step (1) is 50 to 250nm.
Further, in some embodiments of the present invention, the adhesive in step (1) and step (2) comprises two or more of polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica, and polyvinyl alcohol.
Preferably, in some embodiments of the present invention, the adhesive in step (1) and step (2) comprises polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica and polyvinyl alcohol, and the mass ratio of the polyurethane resin to the polyborosilazane resin is 30-40:30-40:5-10:3-7:40-60.
Further, in some embodiments of the present invention, after the adhesive is added into the aqueous solution in the step (1), the mass concentration of the adhesive in the aqueous solution is 0.8-1.5%.
Further, in some embodiments of the present invention, the slurry solid content in the step (1) is 40-60%.
Further, in some embodiments of the present invention, the diameter of the ceramic fiber cell body in the step (1) is 800 to 1000 μm.
Further, in some embodiments of the present invention, the size of the fine crystalline ceramic powder in the step (2) is 0.5 to 5 μm.
Further, in some embodiments of the present invention, in the step (2), the mass ratio of the fine-crystalline ceramic powder, the polyethylene glycol and the adhesive is 95-98:0.5-1.5:1-3.
Further, in some embodiments of the present invention, the thickness of the interfacial separation layer in step (2) is 5 to 60 μm, which is controlled by the solid content of the slurry of the separation layer in step (2) and the number of times the ceramic cellulose bodies are immersed in the slurry of the interfacial separation layer.
Further, in some embodiments of the present invention, in the step (3), the pressure-maintaining molding is performed, and the pressure-maintaining demolding is performed at 150-300Mpa, and the pressure-maintaining is performed for 2-13min.
Compared with the prior art, the invention has the following advantages:
(1) According to the invention, two or more of polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica and polyvinyl alcohol are used as adhesives, and micron fine-grained ceramic powder is dispersed in aqueous solution of polyethylene glycol and adhesives, so that the bending strength and the thermal conductivity of the obtained self-toughened fiber structure ceramic are improved, and a certain effect on improving the fracture toughness is achieved.
(2) The self-toughened fiber structure ceramic obtained by the invention can be arranged in a honeycomb manner, relatively thin interface layers are added at intervals of each cell body, and the grain size of the interface partition layer is larger than that of the fiber cell body, so that a block structural material is combined. Meanwhile, the cell body is the structural characteristic of dense outside and sparse inside, the characteristics of dense outside and gradual loosening of the inner layer are met, the combination of multiple layers of fiber cell bodies, and the structure has multiple layers while alternating soft and hard, so that a structure mechanism of soft and hard intersection and multilayer toughening is formed.
(3) The self-toughening fiber structure ceramic can form a ceramic structure with relatively single components through the difference of grain sizes, so that the interface has excellent oxidation resistance under a high-temperature condition while playing a role of inducing transverse crack propagation, and the problem that the interface layer is stripped due to thermal mismatch can be avoided, thereby realizing stable service in a high-temperature environment for a long time.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of 8230comprises" excludes any non-specified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of 8230title" appears in a clause of the subject matter of the claims and not immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "either" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
The indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates only the singular.
Furthermore, the description below of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. In addition, the technical features according to the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
Self-toughening fiber structure Al 2 O 3 A method of making a ceramic comprising the steps of:
(1) Preparation of ceramic cellule: nano Al with the size of 50-250nm 2 O 3 Adding the fine-grained ceramic powder and the adhesive into an aqueous solution to form ceramic slurry, wherein the solid content of the slurry is 50%, and forming ceramic fiber cells by an extrusion method, wherein the diameter of the ceramic fiber cells is 800-1000 mu m;
(2) Preparing an interfacial separation layer: mixing micrometer Al with size of 0.5-5 μm 2 O 3 Dispersing fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separation layer slurry, immersing the ceramic fiber cell body obtained in the step (1) in the obtained interface separation layer slurry, attaching an interface separation layer, wherein the thickness of the interface separation layer is 10 micrometers, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer obtained in the step (2) in a steel mould according to one-dimensional orientation, then carrying out pressure forming under the condition of 200Mpa, and carrying out pressure maintaining for 7min and demoulding to obtain a blank body of the self-toughened fiber structure ceramic;
(4) Glue discharging and sintering: and (3) insulating and discharging the obtained blank at 550 ℃ in a nitrogen environment, then insulating at 520 ℃ in air to remove the remaining carbide, sintering for 6min by adopting spark plasma sintering at the pressure of 25MPa, cooling and demolding.
The adhesive comprises polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica and polyvinyl alcohol, wherein the mass ratio of the polyurethane resin to the polyborosilazane resin to the aluminum borate nanowhiskers to the fumed silica to the polyvinyl alcohol is 35:35:8:5:50; the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 1.0%.
The mass ratio of the fine-grained ceramic powder, the polyethylene glycol and the adhesive in the step (2) is 97:1:2.
example 2
Self-toughening fiber structure Al 2 O 3 A method of making a ceramic comprising the steps of:
(1) Preparation of ceramic cellule: mixing nano Al with the size of 50-250nm 2 O 3 Adding fine-grain ceramic powder and an adhesive into an aqueous solution to form ceramic slurry, wherein the solid content of the slurry is 60%, and forming ceramic cellules by an extrusion method, wherein the diameter of the ceramic cellules is 800-1000 mu m;
(2) Preparing an interfacial separation layer: mixing micrometer Al with size of 0.5-5 μm 2 O 3 Dispersing fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separating layer slurry, immersing the ceramic cellules obtained in the step (1) in the interface separating layer slurry, attaching an interface separating layer, wherein the thickness of the interface separating layer is 50 microns, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer obtained in the step (2) in a steel mould according to one-dimensional orientation, then carrying out pressure forming under the condition of 200Mpa, keeping the pressure for 10min, and demoulding to obtain a blank body of the self-toughening fiber structure ceramic;
(4) Glue discharging and sintering: and (3) performing heat preservation and glue discharge on the obtained blank at 560 ℃ in a nitrogen environment, then performing heat preservation at 490 ℃ in air to remove the remaining carbide, sintering for 6min by adopting spark plasma sintering at the pressure of 25MPa, and cooling and demolding.
The adhesive comprises polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica and polyvinyl alcohol, wherein the mass ratio of the polyurethane resin to the polyborosilazane resin to the aluminum borate nanowhiskers to the fumed silica to the polyvinyl alcohol is 40:30:5:3:60; the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 1.5%.
The mass ratio of the fine-grained ceramic powder, the polyethylene glycol and the adhesive in the step (2) is 98:0.5:1.5.
example 3
Self-toughening fiber structure Al 2 O 3 A method of making a ceramic comprising the steps of:
(1) Preparation of ceramic cellule: mixing nano Al with the size of 50-250nm 2 O 3 Adding fine-grain ceramic powder and an adhesive into an aqueous solution to form ceramic slurry, wherein the solid content of the slurry is 40%, and forming ceramic cellules by an extrusion method, wherein the diameter of the ceramic cellules is 800-1000 microns;
(2) Preparing an interfacial separation layer: mixing micrometer Al with size of 0.5-5 μm 2 O 3 Dispersing fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separation layer slurry, immersing the ceramic fiber cell body obtained in the step (1) in the obtained interface separation layer slurry, attaching an interface separation layer, wherein the thickness of the interface separation layer is 30 micrometers, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer obtained in the step (2) in a steel mould according to one-dimensional orientation, then carrying out pressure forming under the condition of 200Mpa, keeping the pressure for 8min, and demoulding to obtain a blank body of the self-toughening fiber structure ceramic;
(4) Glue discharging and sintering: and (3) performing heat preservation and glue discharge on the obtained blank at 530 ℃ in a nitrogen environment, then performing heat preservation at 510 ℃ in air to remove the remaining carbide, sintering for 6min by adopting spark plasma sintering at the pressure of 25MPa, cooling and demolding.
The adhesive comprises polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica and polyvinyl alcohol, wherein the mass ratio of the polyurethane resin to the polyborosilazane resin to the aluminum borate nanowhiskers to the fumed silica to the polyvinyl alcohol is 30:40:10:7:40; the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 0.8%.
The mass ratio of the fine-grained ceramic powder, the polyethylene glycol and the adhesive in the step (2) is 97:0.5:2.5.
example 4
Self-toughening fiber structure Al 2 O 3 A method of making a ceramic comprising the steps of:
(1) Preparation of ceramic cellule: mixing nano Al with the size of 50-250nm 2 O 3 Adding fine-grain ceramic powder and an adhesive into an aqueous solution to form ceramic slurry, wherein the solid content of the slurry is 50%, and forming ceramic cellules by an extrusion method, wherein the diameter of the ceramic cellules is 800-1000 microns;
(2) Preparing an interfacial separation layer: mixing micrometer Al with size of 0.5-5 μm 2 O 3 Dispersing fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separating layer slurry, immersing the ceramic cellules obtained in the step (1) in the interface separating layer slurry, attaching an interface separating layer, wherein the thickness of the interface separating layer is 10 microns, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer obtained in the step (2) in a steel mould according to one-dimensional orientation, then carrying out pressure forming under the condition of 200Mpa, and carrying out pressure maintaining for 7min and demoulding to obtain a blank body of the self-toughening fiber structure ceramic;
(4) Glue discharging and sintering: and (3) insulating and discharging the obtained blank at 550 ℃ in a nitrogen environment, then insulating at 520 ℃ in air to remove the remaining carbide, sintering for 6min by adopting spark plasma sintering at the pressure of 25MPa, cooling and demolding.
The adhesive comprises polyurethane resin, fumed silica and polyvinyl alcohol, wherein the mass ratio of the polyurethane resin to the fumed silica to the polyvinyl alcohol is 35:5:50; the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 1.0%.
The mass ratio of the fine-grained ceramic powder, the polyethylene glycol and the adhesive in the step (2) is 97:1:2.
example 5
Self-toughening fiber structure Al 2 O 3 A method of making a ceramic comprising the steps of:
(1) Preparation of ceramic cellule: nano Al with the size of 50-250nm 2 O 3 Adding the fine-grained ceramic powder and the adhesive into an aqueous solution to form ceramic slurry, wherein the solid content of the slurry is 50%, and forming ceramic fiber cells by an extrusion method, wherein the diameter of the ceramic fiber cells is 800-1000 mu m;
(2) Preparing an interfacial separation layer: mixing micrometer Al with size of 0.5-5 μm 2 O 3 Dispersing fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separating layer slurry, immersing the ceramic cellules obtained in the step (1) in the interface separating layer slurry, attaching an interface separating layer, wherein the thickness of the interface separating layer is 10 microns, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer obtained in the step (2) in a steel mould according to one-dimensional orientation, then carrying out pressure forming under the condition of 200Mpa, and carrying out pressure maintaining for 7min and demoulding to obtain a blank body of the self-toughening fiber structure ceramic;
(4) And (3) glue discharging and sintering: and (3) insulating and discharging the obtained blank at 550 ℃ in a nitrogen environment, then insulating at 520 ℃ in air to remove the remaining carbide, sintering for 6min by adopting spark plasma sintering at the pressure of 25MPa, cooling and demolding.
The adhesive comprises polyurethane resin, polyborosilazane resin and polyvinyl alcohol, wherein the mass ratio of the polyurethane resin to the polyborosilazane resin to the polyvinyl alcohol is 35:35:50; the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 1.0%.
The mass ratio of the fine-grained ceramic powder, the polyethylene glycol and the adhesive in the step (2) is 97:1:2.
example 6
Self-toughening fiber structure Al 2 O 3 A method of making a ceramic comprising the steps of:
(1) Preparation of ceramic cellule: will be provided withNano Al with size of 50-250nm 2 O 3 Adding the fine-grained ceramic powder and the adhesive into an aqueous solution to form ceramic slurry, wherein the solid content of the slurry is 50%, and forming ceramic fiber cells by an extrusion method, wherein the diameter of the ceramic fiber cells is 800-1000 mu m;
(2) Preparing an interfacial separation layer: mixing micrometer Al with size of 0.5-5 μm 2 O 3 Dispersing fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separating layer slurry, immersing the ceramic cellules obtained in the step (1) in the interface separating layer slurry, attaching an interface separating layer, wherein the thickness of the interface separating layer is 10 microns, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer obtained in the step (2) in a steel mould according to one-dimensional orientation, then carrying out pressure forming under the condition of 200Mpa, and carrying out pressure maintaining for 7min and demoulding to obtain a blank body of the self-toughened fiber structure ceramic;
(4) Glue discharging and sintering: and (3) insulating the obtained blank at 550 ℃ in a nitrogen environment, removing the binder, then insulating at 520 ℃ in air to remove the remaining carbide, sintering for 6min by adopting spark plasma sintering at the pressure of 25MPa, cooling and demolding.
The adhesive comprises aluminum borate nano crystal whiskers, fumed silica and polyvinyl alcohol, wherein the mass ratio of the polyurethane resin to the polyborosilazane resin to the aluminum borate nano crystal whiskers to the fumed silica to the polyvinyl alcohol is 8:5:50; the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 1.0%.
The mass ratio of the fine-grained ceramic powder, the polyethylene glycol and the adhesive in the step (2) is 97:1:2.
comparative example 1
Self-toughening fiber structure Al 2 O 3 A method of making a ceramic comprising the steps of:
(1) Preparation of ceramic cellule: nano Al with the size of 50-250nm 2 O 3 Adding fine-grain ceramic powder and adhesive into an aqueous solution to form ceramic slurry, wherein the solid content of the slurry is 50%, and forming ceramic cellules and ceramic fibers by an extrusion methodThe diameter of the vitamin body is 800-1000 μm;
(2) Preparing an interfacial separation layer: mixing micrometer Al with size of 0.5-5 μm 2 O 3 Soaking the ceramic cellules obtained in the step (1) into the interface separating layer slurry, attaching an interface separating layer, wherein the thickness of the interface separating layer is 10 microns, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer obtained in the step (2) in a steel mould according to one-dimensional orientation, then carrying out pressure forming under the condition of 200Mpa, and carrying out pressure maintaining for 7min and demoulding to obtain a blank body of the self-toughening fiber structure ceramic;
(4) Glue discharging and sintering: and (3) insulating and discharging the obtained blank at 550 ℃ in a nitrogen environment, then insulating at 520 ℃ in air to remove the remaining carbide, sintering for 6min by adopting spark plasma sintering at the pressure of 25MPa, cooling and demolding.
The adhesive comprises polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica and polyvinyl alcohol, wherein the mass ratio of the polyurethane resin to the polyborosilazane resin to the aluminum borate nanowhiskers to the fumed silica to the polyvinyl alcohol is 35:35:8:5:50; the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 1.0%.
The mass ratio of the fine-grain ceramic powder to the adhesive in the step (2) is 97:2.
comparative example 2
This comparative example refers to example 1 of the prior art CN108794033A for the preparation of a self-toughening fiber structure ceramic.
Effects of the embodiment
The flexural strength, fracture toughness and thermal conductivity of the toughened fiber structural ceramics obtained from the above examples and comparative examples were tested.
The bending strength is measured by a three-point bending resistance test method, the fracture toughness is measured by an indentation crack direct measurement method, a laser thermal conductivity meter is used for testing the thermal diffusion coefficient in the thermal conductivity test, and the thermal conductivity lambda = the thermal diffusion coefficient alpha x density rho x specific heat c.
The test results are shown in the following table.
Figure BDA0003669847880000111
Figure BDA0003669847880000121
It can be seen from the above examples and comparative examples that one or more of polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica, and polyvinyl alcohol are used as the adhesive in the present invention, and the micro fine-grained ceramic powder is dispersed in the aqueous solution of polyethylene glycol and the adhesive, which is beneficial to improving the bending strength and the thermal conductivity of the obtained self-toughened fiber structure ceramic, and has a certain effect on improving the fracture toughness.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.

Claims (11)

1. A preparation method of self-toughening fiber structure ceramics is characterized by comprising the following steps:
(1) Preparation of ceramic cellule: adding nano fine-grain ceramic powder and an adhesive into an aqueous solution to form ceramic slurry, and forming a ceramic cellula body by an extrusion method;
(2) Preparing an interfacial separation layer: dispersing micron fine-grained ceramic powder in aqueous solution of polyethylene glycol and an adhesive to obtain interface separation layer slurry, immersing the ceramic cellulums obtained in the step (1) in the interface separation layer slurry, attaching an interface separation layer, and drying;
(3) Forming a blank body: arranging the dried ceramic fiber cell bodies containing the interface separation layer in the steel mould according to one-dimensional orientation, then carrying out pressure forming, and carrying out pressure maintaining demoulding to obtain a blank body of the self-toughening fiber structure ceramic;
(4) Glue discharging and sintering: keeping the obtained blank at 480-600 ℃ in a nitrogen environment, discharging glue, keeping the temperature at 450-550 ℃ in the air to remove the remaining carbide, sintering for 5-10min by adopting a discharge plasma sintering method, keeping the pressure at 25-30MPa, cooling and demolding;
the adhesive in the step (1) and the step (2) comprises polyurethane resin, polyborosilazane resin, aluminum borate nanowhiskers, fumed silica and polyvinyl alcohol, and the mass ratio of the polyurethane resin to the polyborosilazane resin is 30-40:30-40:5-10:3-7:40-60.
2. The method of claim 1, wherein the ceramic powder in step (1) and step (2) is Al 2 O 3 、SiC、Y 2 O 3 、AlN 、Si 3 N 4 And ZrO 2 One or more of (a).
3. The method of claim 1, wherein the ceramic powder in step (1) and step (2) is Al 2 O 3 。
4. The method of making a self-toughening fiber structural ceramic of claim 1 wherein the fine crystalline ceramic powder of step (1) has a size of 50 to 250nm.
5. The method for preparing self-toughening fiber structural ceramics according to claim 1, wherein the mass concentration of the adhesive in the aqueous solution after the adhesive is added into the aqueous solution in the step (1) is 0.8-1.5%.
6. The method of making a self-toughening fiber structural ceramic of claim 1 wherein the slurry solids content in step (1) is 40-60%.
7. The method of claim 1, wherein the diameter of the ceramic fiber cell body in step (1) is 800-1000 μm.
8. The method of making a self-toughening fiber structural ceramic of claim 1 wherein the fine crystalline ceramic powder of step (2) has a size of 0.5 to 5 μm.
9. The method for preparing the self-toughening fiber structure ceramic according to claim 1, wherein the mass ratio of the fine-grained ceramic powder, the polyethylene glycol and the adhesive in the step (2) is 95-98:0.5-1.5:1-3.
10. The method of claim 1, wherein the interfacial separation layer in step (2) has a thickness of 5-60 μm.
11. The method for preparing self-toughening fiber structural ceramics according to claim 1, wherein the step (3) is pressure forming, and the pressure maintaining demolding is carried out at 150-300MPa for 2-13min.
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