CN114292112A - High-toughness ceramic material with bionic clay brick structure and preparation method thereof - Google Patents
High-toughness ceramic material with bionic clay brick structure and preparation method thereof Download PDFInfo
- Publication number
- CN114292112A CN114292112A CN202210022626.7A CN202210022626A CN114292112A CN 114292112 A CN114292112 A CN 114292112A CN 202210022626 A CN202210022626 A CN 202210022626A CN 114292112 A CN114292112 A CN 114292112A
- Authority
- CN
- China
- Prior art keywords
- bionic
- brick structure
- ceramic
- toughness
- clay brick
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 27
- 239000011664 nicotinic acid Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011449 brick Substances 0.000 title claims abstract description 20
- 239000004927 clay Substances 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 claims abstract description 49
- 239000011454 mudbrick Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000000725 suspension Substances 0.000 claims abstract description 27
- 239000004005 microsphere Substances 0.000 claims abstract description 26
- 238000007598 dipping method Methods 0.000 claims abstract description 3
- 239000002131 composite material Substances 0.000 claims description 26
- 239000012071 phase Substances 0.000 claims description 22
- 238000005245 sintering Methods 0.000 claims description 22
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 19
- 239000011325 microbead Substances 0.000 claims description 18
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 16
- 238000007731 hot pressing Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000005452 bending Methods 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 6
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000007790 solid phase Substances 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- 229920002873 Polyethylenimine Polymers 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011153 ceramic matrix composite Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001513 hot isostatic pressing Methods 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000002490 spark plasma sintering Methods 0.000 claims description 2
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 239000000243 solution Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000003592 biomimetic effect Effects 0.000 description 2
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000707 layer-by-layer assembly Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Ceramic Products (AREA)
Abstract
The invention provides a preparation method of a high-strength and high-toughness ceramic material with a bionic clay brick structure. The method takes spherical ceramic microspheres as bricks, and the wrapped second phase as mud which is piled up under the action of pressure to form a compact mud-brick structure. The mud-brick structure causes the cracks to deflect along the interface of two phases, and the fracture function is improved, thereby improving the fracture toughness of the ceramic material and obtaining the structural ceramic with high mechanical property. The preparation process is simple and environment-friendly, raw materials are easy to obtain, disordered complex industrial equipment and pretreatment processes are adopted, the method for directly dipping after stable suspension is prepared is simple and easy to implement, the second phase is flexible to select, the requirement of multi-element compounding is met, and the structural design and functional regulation and control of the interface layer are facilitated.
Description
Technical Field
The invention relates to the technical field of structural ceramic materials, in particular to a novel method for preparing a high-toughness ceramic material with a bionic clay brick structure based on ceramic microspheres.
Background
Brittle fracture is one of the key problems faced by structural ceramic materials in the application process, and how to improve the fracture toughness of the structural ceramic materials is always the research focus in the field. The preparation of the composite ceramic material through component and structure design is an effective means for improving the fracture toughness of the structural ceramic. According to the difference of distribution form and toughening principle of the second phase of the composite ceramic in the matrix material, three main toughening methods of particle dispersion toughening, whisker/fiber toughening and lamellar structure toughening can be divided. The laminated structure toughening is inspired by the 'mud-brick' structure of shells and mother-of-pearl in nature, and the 'mud-brick' laminated structure ceramic similar to a natural biological structure is constructed by multi-component layer-by-layer assembly. When stressed, the cracks deflect between layers, and more energy is consumed, so that the aim of toughening is fulfilled, and the comprehensive performance of the structural ceramic material is improved.
The early method for constructing the bionic mud-brick structure mainly comprises a tape casting method, an extrusion molding method and the like which are combined with hot-pressing sintering, but the laminated structure of the composite ceramic constructed by the methods has larger scale, the average layer thickness reaches 0.1-2mm, the requirement of structural design on smaller scale is difficult to meet, and the strength of the material is sacrificed to a certain extent. In recent years, researchers have used an ice template-freeze drying method to prepare composite ceramics with a mud-brick structure, which has smaller layer size and finer structure, as in patent application 201710570994.4. The ice template-freeze drying method utilizes the phenomenon of preferential orientation of partial solvent crystals during growth, forms a porous blank with lamellar pores by sublimation after crystallization, and then structures the layered composite ceramic with a similar mud-brick structure by presintering the blank and impregnating a second phase, thereby achieving the purpose of toughening. The thickness of the mud-brick structure constructed by the method is generally 1-10 mu m, and the fine regulation and control of the structure on the micrometer scale are realized. In addition, researchers have developed biomimetic mineralization methods to construct and regulate micron-scale and nanoscale "mud-brick" structures. The biomimetic mineralization method imitates the phenomenon that shells and other organisms control the formation of inorganic matters by using proteins, and the organic system is used for regulating and controlling the crystallization of the inorganic matters to construct a compound with two different crystal forms, so that a mud-brick structure is constructed to realize the improvement of the mechanical properties of the composite material. However, the two methods have the disadvantages of complex process and high cost, and the prepared composite material has small size and is difficult to meet the requirement of large-scale industrial production.
The invention provides a new method for constructing a bionic mud-brick structure, and also provides a new method for strengthening and toughening a ceramic matrix composite. According to the invention, the ceramic microspheres are impregnated by using the second phase suspension, the uniform impregnation of the microspheres is realized by controlling the mass ratio of the microspheres to the suspension, and the ceramic microspheres are further pressed, sintered and molded. The spherical ceramic microspheres are used as bricks, and the wrapped second phase is used as mud which is piled up under the action of pressure to form a compact mud-brick structure. The mud-brick structure causes the cracks to deflect along the interface of two phases, and the fracture function is improved, thereby improving the fracture toughness of the ceramic material and obtaining the structural ceramic with high mechanical property.
Disclosure of Invention
The invention aims to construct a mud-brick structure by a simple and convenient method with strong operability, prepare high-toughness composite ceramic, realize the toughening of structural ceramic materials, overcome the defects of complex process, high cost, poor interface regulation and control performance and the like in the preparation process of the traditional bionic layered ceramic materials, construct the mud-brick structure composite ceramic by the simple and convenient method with strong operability and realize the toughening of the structural ceramic materials.
Aiming at the problems, the invention provides a preparation method of a high-strength and high-toughness ceramic material with a bionic clay brick structure.
The preparation method specifically comprises the following steps:
a first step of preparing a second phase suspension;
secondly, uniformly dispersing the ceramic microspheres in a second-phase suspension;
thirdly, drying to obtain a ceramic microbead blank with a second phase uniformly coated on the surface;
and fourthly, pressurizing and sintering to obtain the high-strength and high-toughness ceramic matrix composite material with a bionic mud-brick structure.
Wherein the liquid phase in the second phase suspension in the first step is deionized water or absolute ethyl alcohol, the solid phase is any one or more of yttrium-stabilized zirconia powder, nickel oxide powder, silicon carbide powder, boron nitride powder, carbon nano tubes and graphene, and the solid phase content is preferably 1-40 wt%.
Wherein, a dispersant is added in the second phase suspension, and the dispersant can be ammonium citrate, Sodium Tripolyphosphate (STPP), polyvinylpyrrolidone (PVP) and ammonium polyacrylate (PAA-NH)4) One of tetramethylammonium hydroxide (TMAOH), Polyethyleneimine (PEI) and polyvinyl alcohol (PVA), and the addition amount of the dispersant is 0.1-0.5 wt%.
In the first step, the solid phase, the liquid phase and the dispersing agent are mixed together in proportion and stirred uniformly to obtain a second phase suspension.
The ceramic microspheres in the second step can be hollow or solid microspheres, the particle size of the microspheres is preferably 10-200 μm, and the ceramic microspheres are made of any one or a combination of silicon nitride, silicon carbide, zirconium oxide, aluminum oxide and silicon dioxide.
Wherein, the ceramic micro-bead can be a ceramic micro-bead blank or a ceramic micro-bead pre-sintered at the temperature of 600-1900 ℃.
In the second step, the mass ratio of the ceramic microspheres to the second phase suspension is controlled to be 1:1 so as to ensure uniform impregnation of the microspheres.
Wherein the fourth step of sintering by pressure is hot-pressing sintering, spark plasma sintering or hot isostatic pressing sintering.
Wherein the sintering pressure of the pressure sintering is 5-50 MPa. The sintering temperature is 500-2000 ℃ and the heat preservation time is 0.5-6 h.
Wherein, the bending strength of the prepared high-strength and high-toughness ceramic matrix composite material with a bionic mud-brick structure is more than 600MPa, and the fracture toughness is 7.20 MPa.m1/2Above, the density is more than 90.0 percent,
the invention has the advantages of
The preparation process of the high-toughness ceramic material with the bionic clay brick structure provided by the invention is simple and environment-friendly, and the ceramic microspheres are industrially produced at present, and have easily available raw materials, disordered complex industrial equipment and a pretreatment process. The method for directly dipping after preparing the stable suspension is simple and easy, the second phase is flexible to select, the requirement of multi-element compounding is met, the structural design and the functional regulation and control of an interface layer are convenient to carry out, and the mud-brick structure high-toughness composite ceramic prepared by the method can meet the application requirements of multiple fields and the requirement of industrial production.
Drawings
FIG. 1 is a process flow chart of a preparation method of a high-strength and high-toughness ceramic material with a bionic clay brick structure provided by the invention;
FIG. 2 shows ZrO produced in example 1 of a field emission scanning electron microscope2/Si3N4The structural appearance of the composite ceramic mud brick is shown schematically;
FIG. 3 shows ZrO of example 1 under an optical microscope2/Si3N4The shape of the vertical surface of the composite ceramic mud brick structure and the c axis;
FIG. 4 shows ZrO of example 1 under an optical microscope2/Si3N4The shape of the parallel surface of the composite ceramic mud brick structure and the c axis.
Detailed Description
To better illustrate the present invention, the main contents of the present invention will be further described below with reference to specific examples and drawings, which do not limit the scope of the present invention.
Example 1
S1, presintering 32.4g of silicon nitride hollow microspheres (the particle size is 80-120 mu m) at 1550 ℃ under 0.8MPa in nitrogen atmosphere, and preserving heat for 0.5 h; s2, configuring 36mL PAA-NH with mass fraction of 0.4 wt%4Solution 3.6g of yttrium-stabilized zirconia powder with an average particle size of about 500nm was added to the PAA-NH-containing solution4The aqueous dispersion of (1) is subjected to pH adjustment with concentrated aqueous ammonia to a pH of 10.0 to stably disperse the suspension; s3, pouring 32.4g of silicon nitride cenospheres into the zirconia suspension for multiple times, and continuously shaking by hands until the silicon nitride cenospheres and the zirconia suspension are uniformly mixed. S4, placing the impregnated silicon nitride hollow microspheres in a drying box for drying, then placing the dried silicon nitride hollow microspheres in a hot-pressing die, and prepressing under the pressure of 5 MPa; and S5, hot-pressing and sintering the pre-pressed sample at 1750 ℃ under the nitrogen atmosphere and under the pressure of 30MPa, and keeping the temperature for 2h to obtain the zirconia/silicon nitride composite ceramic with the mud-brick structure.
The zirconia/silicon nitride composite ceramic with the mud-brick structure prepared by the preparation method has the bending strength of 950MPa and the fracture toughness of 8.35 MPa.m1/2The compactness is 90.3%.
Example 2
The method for constructing the mud-brick structure toughened silicon nitride ceramic by using the hollow microspheres comprises the following steps:
s1, pre-burning 39.2g of silicon nitride hollow microspheres (the particle size is about 40-80 μm) at 1600 ℃ in a nitrogen atmosphere at 0.4MPa, and preserving heat for 0.5 h; s2, dispersing 0.8g of graphene oxide in 200mL of isopropanol, and performing ultrasonic oscillation for 40min to uniformly disperse the graphene oxide; and S3, adding the beads subjected to the pre-sintering treatment in the S1 into the graphene oxide dispersion liquid, and continuously stirring. Heating the mixed suspension to 130 ℃ to evaporate the solvent; s4, placing the graphene oxide/silicon nitride hollow microspheres in a hot-pressing mold, and pre-pressing under 10 MPa; and S5, hot-pressing and sintering the pre-pressed sample at 1750 ℃ under the nitrogen atmosphere and under the pressure of 50MPa, and keeping the temperature for 2h to obtain the graphene oxide/silicon nitride composite ceramic with the mud-brick structure.
Prepared by the above methodThe 'mud-brick' structure graphene oxide/silicon nitride composite ceramic prepared by the method has the bending strength of 873MPa and the fracture toughness of 9.03 MPa.m1/2The compactness is 99.0%.
Example 3
The method for constructing the mud-brick structure toughened alumina ceramic by using the solid microspheres comprises the following steps:
s1, presintering 32g of alumina solid microspheres (the particle size is 120-; s2, configuring 36mL PAA-NH with mass fraction of 0.4 wt%4Solution 3.6g of yttrium-stabilized zirconia powder with an average particle size of about 500nm was added to the PAA-NH-containing solution4Adjusting the pH value of the suspension to 10.0 by using strong ammonia water, and stirring for 30min to stably disperse the suspension; s3, pouring 32.4g of alumina solid microspheres into the zirconia suspension for multiple times, and continuously shaking by hands until the two are uniformly mixed. S4, placing the impregnated alumina solid microbeads in a drying box for drying, then placing the dried alumina solid microbeads in a hot-pressing die, and prepressing the dried alumina solid microbeads under the pressure of 5 MPa; and S5, hot-pressing and sintering the pre-pressed sample at 1550 ℃, in an argon atmosphere and under a pressure of 50MPa, and keeping the temperature for 2h to obtain the zirconia/alumina composite ceramic with the mud-brick structure.
The zirconia/alumina composite ceramic with the mud-brick structure prepared by the preparation method has the bending strength of 600MPa and the fracture toughness of 7.23 MPa.m1/2The density is 99.6%.
Example 4
S1, preparing 36mL of 0.5 wt% PVA solution, adding 4g of nickel oxide into the PVA solution, ultrasonically oscillating for 20min, and then continuously stirring until nickel oxide particles are uniformly dispersed; s2, pouring 32.4g of alumina cenospheres into the zirconia suspension for multiple times, and continuously shaking by hands until the two are uniformly mixed. S3, placing the impregnated alumina solid microbeads in a drying box for drying, then placing the dried alumina solid microbeads in a hot-pressing die, and prepressing the dried alumina solid microbeads under the pressure of 5 MPa; and S5, hot-pressing and sintering the pre-pressed sample at 1550 ℃, in an argon atmosphere and under a pressure of 30MPa, and keeping the temperature for 1.5h to obtain the nickel oxide/aluminum oxide composite ceramic with the mud-brick structure.
The nickel oxide/alumina composite ceramic with the mud-brick structure prepared by the preparation method has the bending strength of 670MPa and the fracture toughness of 7.30 MPa-m1/2The density is 99.4%.
Example 5
S1, preparing 36mL of tetramethylammonium hydroxide solution with the mass fraction of 0.4 wt%, adding 3.6g of hexagonal boron nitride powder into an aqueous solution containing a tetramethylammonium hydroxide dispersing agent, adjusting the pH value of a suspension to 10.0 by using concentrated ammonia water, and stirring for 30min to stably disperse the suspension; s2, adding silicon nitride solid microbeads to the boron nitride suspension for multiple times, wherein the diameter of each microbead is 50-150 mu m, and oscillating the microbeads with hands without stopping until the mixture is in a slurry state, so that the microbeads can be completely soaked in the dispersion liquid, and the microbeads and the dispersion liquid cannot be layered due to over dilution; s3, putting the obtained mixture into an oven for drying, then putting the mixture into a hot-pressing die, and prepressing under the pressure of 5 MPa; s4, hot-pressing and sintering the pre-pressed sample at 1750 ℃ under the nitrogen atmosphere and under the pressure of 30MPa, and keeping the temperature for 2h to obtain the BN/Si with the mud-brick structure3N4Composite ceramics.
The zirconia/silicon nitride composite ceramic with the mud-brick structure prepared by the preparation method has the bending strength of 850MPa and the fracture toughness of 9.62 MPa.m1/2The compactness is 90.6%.
All of the above mentioned intellectual property rights are not intended to be restrictive to other forms of implementing the new and/or new products. Those skilled in the art will take advantage of this important information, and the foregoing will be modified to achieve similar performance. However, all modifications or alterations are based on the new products of the invention and belong to the reserved rights.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a high-toughness ceramic material with a bionic clay brick structure is characterized by comprising the following steps: and uniformly dipping the ceramic microspheres by the second-phase suspension, and performing pressure sintering to realize fine controllable construction of a two-phase or multi-phase composite structure, thereby preparing the high-toughness ceramic-based composite material with a bionic 'mud-brick' structure.
2. The preparation method of the high-strength and high-toughness ceramic material with the bionic clay brick structure as claimed in claim 1, is characterized in that:
a first step of preparing a second phase suspension;
secondly, uniformly dispersing the ceramic microspheres in a second-phase suspension;
thirdly, drying to obtain a ceramic microbead blank with a second phase uniformly coated on the surface;
and fourthly, pressurizing and sintering to obtain the high-strength and high-toughness ceramic matrix composite material with a bionic mud-brick structure.
3. The method for preparing the high-toughness ceramic material with the bionic clay brick structure as claimed in claim 2, wherein the ceramic beads can be ceramic bead blanks or ceramic beads which are respectively pre-sintered at 600-1900 ℃.
4. The preparation method of the high-strength and toughness ceramic material with the bionic clay brick structure as claimed in claim 2, wherein the ceramic beads can be hollow or solid beads, the particle size of the beads is 10-200 μm, and the ceramic beads are made of any one or a combination of silicon nitride, silicon carbide, zirconium oxide, aluminum oxide and silicon dioxide.
5. The preparation method of the high-strength and high-toughness ceramic material with the bionic clay brick structure according to claim 2, wherein a liquid phase in the second-phase suspension is deionized water or absolute ethyl alcohol, a solid phase is any one or more of yttrium-stabilized zirconia powder, nickel oxide powder, silicon carbide powder, boron nitride powder, carbon nano-tubes and graphene, and the content of the solid phase is 1-40 wt%.
6. The method for preparing high-toughness ceramic material with bionic clay brick structure according to claim 2, wherein the dispersant in the second phase suspension can be ammonium citrate, Sodium Tripolyphosphate (STPP), polyvinylpyrrolidone (PVP), ammonium polyacrylate (PAA-NH)4) One of tetramethylammonium hydroxide (TMAOH), Polyethyleneimine (PEI) and polyvinyl alcohol (PVA), and the addition amount of the dispersant is 0.1-0.5 wt%.
7. The preparation method of the high-toughness ceramic material with the bionic clay brick structure according to claim 2, wherein the mass ratio of the microbeads to the second-phase suspension liquid is controlled to be 1:1 so as to ensure the uniform impregnation of the microbeads.
8. The method for preparing the high-strength and high-toughness ceramic material with the bionic clay brick structure according to claim 2, wherein the pressure sintering is hot-pressing sintering, spark plasma sintering or hot isostatic pressing sintering.
9. The preparation method of the high-strength and high-toughness ceramic material with the bionic clay brick structure as claimed in claim 2, wherein the sintering pressure of the pressure sintering is 5-50MPa, the sintering temperature is 500-2000 ℃, and the heat preservation time is 0.5-3 h.
10. The high-toughness ceramic-based composite material with the bionic clay brick structure, which is prepared by adopting the preparation method of the high-toughness ceramic material with the bionic clay brick structure of any one of claims 1 to 9, has the bending strength of more than 600MPa and the fracture toughness of 7.20 MPa-m1/2The density is more than 90.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210022626.7A CN114292112A (en) | 2022-01-10 | 2022-01-10 | High-toughness ceramic material with bionic clay brick structure and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210022626.7A CN114292112A (en) | 2022-01-10 | 2022-01-10 | High-toughness ceramic material with bionic clay brick structure and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114292112A true CN114292112A (en) | 2022-04-08 |
Family
ID=80975073
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210022626.7A Pending CN114292112A (en) | 2022-01-10 | 2022-01-10 | High-toughness ceramic material with bionic clay brick structure and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114292112A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241515A (en) * | 2010-05-14 | 2011-11-16 | 河北勇龙邦大新材料有限公司 | Ceramic with light weight, high strength and high toughness and preparation method thereof |
| CN108249929A (en) * | 2018-01-22 | 2018-07-06 | 哈尔滨工业大学 | A kind of preparation method of the brick of multiple dimensioned toughening-mud structure superhigh temperature ceramic material |
| CN111777427A (en) * | 2020-06-24 | 2020-10-16 | 清华大学 | Preparation method of nacre-like layered high-strength super-tough ceramic |
| CN113004050A (en) * | 2021-05-10 | 2021-06-22 | 山东大学苏州研究院 | Double-toughened shell-structure-imitated composite ceramic material and preparation method thereof |
| US20210214280A1 (en) * | 2019-01-29 | 2021-07-15 | Qilu University Of Technology | Nickel-coated hexagonal boron nitride nanosheet composite powder, preparation and high performance composite ceramic cutting tool material |
-
2022
- 2022-01-10 CN CN202210022626.7A patent/CN114292112A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241515A (en) * | 2010-05-14 | 2011-11-16 | 河北勇龙邦大新材料有限公司 | Ceramic with light weight, high strength and high toughness and preparation method thereof |
| CN108249929A (en) * | 2018-01-22 | 2018-07-06 | 哈尔滨工业大学 | A kind of preparation method of the brick of multiple dimensioned toughening-mud structure superhigh temperature ceramic material |
| US20210214280A1 (en) * | 2019-01-29 | 2021-07-15 | Qilu University Of Technology | Nickel-coated hexagonal boron nitride nanosheet composite powder, preparation and high performance composite ceramic cutting tool material |
| CN111777427A (en) * | 2020-06-24 | 2020-10-16 | 清华大学 | Preparation method of nacre-like layered high-strength super-tough ceramic |
| CN113004050A (en) * | 2021-05-10 | 2021-06-22 | 山东大学苏州研究院 | Double-toughened shell-structure-imitated composite ceramic material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| RYAN P. WILKERSON ET AL.: "A Novel Approach to Developing Biomimetic ("Nacre-Like") Metal-Compliant-Phase (Nickel–Alumina) Ceramics through Coextrusion", 《ADV. MATER.》 * |
| 孙娜等: "贝壳珍珠层及其仿生材料的研究进", 《高等学校化学学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111777427B (en) | Preparation method of nacre-like layered high-strength super-tough ceramic | |
| Franks et al. | Colloidal processing: enabling complex shaped ceramics with unique multiscale structures | |
| CN108706978B (en) | Method for preparing silicon carbide ceramic matrix composite by combining spray granulation with 3DP and CVI | |
| CN109987941B (en) | High-entropy ceramic composite material with oxidation resistance and preparation method and application thereof | |
| CN107686366B (en) | Preparation method of nano-wire and whisker synergistic toughened ceramic matrix composite material | |
| Sun et al. | 3D printing of porous SiC ceramics added with SiO2 hollow microspheres | |
| CN102241515A (en) | Ceramic with light weight, high strength and high toughness and preparation method thereof | |
| CN106633652A (en) | Preparation method of bicontinuous-phase alumina/epoxy resin composite material | |
| CN102517469B (en) | Method for preparing porous material | |
| CN112125653A (en) | Graphene ceramic composite material prepared based on 3D printing and preparation method thereof | |
| CN106167413A (en) | A kind of toughness reinforcing 90 aluminium oxide ceramics of On In-situ Synthesis of Mullite Whisker and preparation method | |
| CN112110677A (en) | Rigid nano heat-insulating material based on hot-pressing bonding mechanism and preparation method thereof | |
| CN108129151A (en) | A kind of graphene/carbon SiClx nano composite structure layered ceramic and preparation method thereof | |
| CN109320257B (en) | Preparation method of high-strength high-porosity porous silicon nitride ceramic | |
| CN1944018A (en) | Method for preparing strong magnetic-weak magnetic gradient material formed by slip casting in pulse magnetic field | |
| CN113800837B (en) | Continuous carbon fiber reinforced phosphate group geopolymer composite material and preparation method thereof | |
| CN110483081A (en) | A kind of high-temperature resistant nano heat-barrier material and preparation method thereof | |
| CN100429176C (en) | Process for preparing nano complex phase ceramic material by in-situ reaction | |
| CN110669975A (en) | High-strength ceramic material | |
| CN113831101A (en) | Chopped carbon fiber reinforced phosphate group geopolymer composite material and preparation method thereof | |
| CN117567165A (en) | Continuous fiber reinforced ceramic matrix composite material and preparation method thereof | |
| CN116375504B (en) | Compact high-temperature oxidation-resistant coating on surface of carbon-based or ceramic-based composite material and preparation method thereof | |
| CN114292112A (en) | High-toughness ceramic material with bionic clay brick structure and preparation method thereof | |
| CN108117381A (en) | A kind of inertia composite calcining-endure plate and preparation method thereof | |
| CN113831102B (en) | Continuous basalt fiber reinforced phosphate group geopolymer composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220408 |
|
| RJ01 | Rejection of invention patent application after publication |