CN110981490A - CNT toughening of B4C-SiC laminated composite ceramic and preparation method thereof - Google Patents
CNT toughening of B4C-SiC laminated composite ceramic and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 85
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 81
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 81
- 239000002153 silicon-carbon composite material Substances 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005011 phenolic resin Substances 0.000 claims abstract description 9
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- 239000011858 nanopowder Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 230000003247 decreasing effect Effects 0.000 claims abstract description 4
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011863 silicon-based powder Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000002620 silicon nanotube Substances 0.000 abstract 1
- 229910021430 silicon nanotube Inorganic materials 0.000 abstract 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 6
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- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
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- 238000005245 sintering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- 238000000280 densification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- 238000009210 therapy by ultrasound Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
CNT (carbon nanotube) toughening B4A C-SiC layered composite ceramic and a preparation method thereof belong to the technical field of composite material preparation. The CNT toughens B4The preparation method of the C-SiC layered composite ceramic comprises the following steps: s1, designing CNT, PVP and H according to a layered structure2Mixing O uniformly in different proportions to prepare CNT dispersion liquids with different proportions; s2, configuring CNT-B with different mixture ratio based on the step S14C-Si composite pastes, each composite paste comprising the same weight of B4C, nano powder, simple substance silicon and phenolic resin; s3, mixing the materials in different proportionsCNT-B of (A)4Respectively spraying and granulating the C-Si composite slurry to obtain CNT-B with different proportions4C-Si composite dry powder; s4, gradually increasing or decreasing the weight ratio of CNT, and laying CNT-B with different proportions in a mould in a layered manner4C-Si composite dry powder, compacting, forming and firing to obtain CNT toughened B4C-SiC laminated composite ceramic. The invention improves the toughness of the prepared laminated composite ceramic by adding simple substance silicon and CNT and adopting the laminated structure design.
Description
Technical Field
The invention relates to a technology in the field of composite material preparation, in particular to CNT (carbon nanotube) toughened B4C-SiC laminated composite ceramic and a preparation method thereof.
Background
B4The C has physical and mechanical properties such as low density and high strength, and is widely applied to the fields of aviation, military equipment and the like. However B4C is brittle in itself and therefore needs to be improved by additives, reaction sintering B4The C-SiC material is an ideal composite ceramic material. But currently used B4The C raw material is limited by the preparation process and often contains a certain amount of free carbon, and the existence of the free carbon can cause reaction sintering B4The compactness and hardness of the C-SiC composite ceramic material are reduced.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a CNT (carbon nanotube) toughened B4The C-SiC laminated composite ceramic is prepared by adding simple substance silicon and B4And free carbon in the raw material C reacts, so that the compactness of the composite ceramic is improved, the hardness of the composite ceramic is enhanced, and the toughness of the composite ceramic is improved by adopting a laminated structure and adding CNT.
The invention relates to a CNT toughened B4The preparation method of the C-SiC layered composite ceramic comprises the following steps:
s1, designing CNT, PVP (polyvinyl pyrrolidone) and H according to a layered structure2Mixing O uniformly in different proportions, and preparing CNT dispersion liquids with different proportions;
s2, configuring CNT-B with different mixture ratio based on the step S14C-Si composite pastes, each composite paste comprising the same weight of B4C, nano powder, elemental silicon with the same weight and phenolic resin with the same weight;
s3, mixing CNT-B with different proportions4Respectively spraying and granulating the C-Si composite slurry to obtain CNT-B with different proportions4C-Si composite dry powder;
s4, gradually increasing or decreasing the weight ratio of CNT, and laying CNT-B with different proportions in a mould in a layered manner4C-Si composite dry powder is pressed into a blank for forming; under vacuum condition, heatingFiring at 1850-2100 ℃ to obtain CNT toughened B4C-SiC laminated composite ceramic.
Preferably, the CNT-B4CNT and B in C-Si composite slurry4The mixing ratio of C to Si is 8-15: 10-50: 1 to 10, CNT-B4The weight proportion of the phenolic resin in the C-Si composite slurry is 1-10%.
The invention relates to a CNT toughened B4The C-SiC laminated composite ceramic is prepared by the method.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) mixing CNT-B with different proportions4The C-Si composite dry powder is laid in a mould in a layered mode, and a pressed blank is formed and fired to obtain a layered structure material, so that the toughness of the ceramic product is enhanced, and the problem that the toughness and hardness of the conventional ceramic product are difficult to improve simultaneously is solved;
2) by adding elemental silicon with B4Free carbon in C reacts to generate SiC, so that the compactness and hardness of the ceramic are improved;
3) adding CNT to improve the toughness of the composite ceramic, preparing CNT into dispersion, and B4C. The affinity of Si is improved.
Drawings
FIG. 1 CNT toughening B prepared in example 14XRD pattern of C-SiC laminated composite ceramic;
FIG. 2 CNT toughening B prepared in example 14SEM photograph of C-SiC layered composite ceramic.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The embodiment of the invention relates to CNT (carbon nanotube) toughened B4The preparation method of the C-SiC layered composite ceramic comprises the following steps:
s1, mixing CNT, PVP and H according to the design of a laminated structure (at least 3 layers)2Mixing O uniformly in different proportions to prepare CNT dispersion liquids with different proportions;
s2, configuring differently based on the step S1Formulated CNT-B4C-Si composite pastes, each composite paste comprising the same weight of B4C, nano powder, elemental silicon with the same weight and phenolic resin with the same weight;
s3, mixing CNT-B with different proportions4Respectively spraying and granulating the C-Si composite slurry to obtain CNT-B with different proportions4C-Si composite dry powder;
s4, gradually increasing or decreasing the weight ratio of CNT, and laying CNT-B with different proportions in a mould in a layered manner4C-Si composite dry powder is pressed into a blank for forming; under the vacuum condition, the temperature is raised to 1850-4C-SiC laminated composite ceramic.
Preferably, the CNT-B4CNT and B in C-Si composite slurry4The mixing ratio of C to Si is 8-15: 10-50: 1 to 10, CNT-B4The weight proportion of the phenolic resin in the C-Si composite slurry is 1-10%.
Preferably, the CNT dispersion comprises CNT, PVP and H2The mixing ratio of O is 1-50: 1: 100 to 500.
Preferably, the CNT is a whisker multi-wall carbon nanotube, the length of the CNT is 5-20 μm, and the diameter of the CNT is 50-200 nm.
Preferably, B is4The grain size of the C nano powder is 100-500 nm.
Preferably, the elemental silicon is silicon powder.
Example 1
This example relates to a CNT toughened B4The preparation method of the C-SiC layered composite ceramic comprises the following steps:
s1, preparing CNT dispersion-1, CNT dispersion-2 and CNT dispersion-3 respectively;
mixing CNT, PVP and H2Mixing O uniformly, performing ultrasonic treatment, and stirring uniformly to obtain CNT dispersion liquid-1, CNT dispersion liquid-2 and CNT dispersion liquid-3; CNT in CNT dispersion-1, CNT dispersion-2, and CNT dispersion-3: PVP: h2The weight ratio of O is 1: 1: 200. 10: 1: 200. 20: 1: 200 of a carrier;
s2 based on CNT Dispersion-1, CNT Dispersion-2 and CNT Dispersion-3 with CNT-B4C-Si composite paste-1, CNT-B4C-Si composite paste-2, CNT-B4C-Si composite slurry-3;
each CNT-B4The C-Si composite slurry comprises B45.0kg of C nano powder, 0.2kg of silicon powder, 0.45kg of phenolic resin and 5.0kg of B4Mixing the C nano powder with 10.0kg of water, adding 0.2kg of silicon powder and 2.0kg of CNT dispersion liquid, sanding for 30min, adding 0.45kg of phenolic resin, and uniformly stirring;
s3 CNT toughening B4Firing the C-SiC laminated composite ceramic;
mixing CNT-B4C-Si composite paste-1, CNT-B4C-Si composite paste-2, CNT-B4Spray-drying C-Si composite slurry-3 respectively to obtain CNT-B4C-Si composite dry powder-1, CNT-B4C-Si composite dry powder-2, CNT-B4C-Si composite dry powder-3; then adding CNT-B4C-Si composite dry powder-1, CNT-B4C-Si composite dry powder-2, CNT-B4C-Si composite dry powder-3 is sequentially laid in a mould in a layered manner, and pressed into a blank for forming; heating to 2000 deg.C at a rate of 5-20 deg.C/min under vacuum condition, and firing at 2000 deg.C to obtain CNT toughened B4C-SiC laminated composite ceramic.
CNT toughening B prepared in this example by scanning Electron microscope and X-ray diffractometer4And carrying out structural characterization on the C-SiC layered composite ceramic to obtain an XRD (X-ray diffraction) spectrum shown in figure 1 and an SEM (scanning Electron microscope) pattern shown in figure 2. As can be seen from the XRD pattern of FIG. 1, CNT toughened B4The C-SiC laminated composite ceramic consists of C, B4C. SiC is composed of three phases, and no other phases or substances are found. As can be seen from the SEM image of FIG. 2, CNT toughening B4The C-SiC laminated composite ceramic has good densification and uniform dispersion of CNT. CNT toughening B measured by Archimedes method4The density of the C-SiC layered composite ceramic was 98.22% of the theoretical value.
It is to be emphasized that: the above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (7)
1. CNT (carbon nanotube) toughening B4The preparation method of the C-SiC layered composite ceramic is characterized by comprising the following steps of:
s1, designing CNT, PVP and H according to a layered structure2Mixing O uniformly in different proportions to prepare CNT dispersion liquids with different proportions;
s2, configuring CNT-B with different mixture ratio based on the step S14C-Si composite pastes, each composite paste comprising the same weight of B4C, nano powder, elemental silicon with the same weight and phenolic resin with the same weight;
s3, mixing CNT-B with different proportions4Respectively spraying and granulating the C-Si composite slurry to obtain CNT-B with different proportions4C-Si composite dry powder;
s4, gradually increasing or decreasing the weight ratio of CNT, and laying CNT-B with different proportions in a mould in a layered manner4C-Si composite dry powder is pressed into a blank for forming; heating to 1850-4C-SiC laminated composite ceramic.
2. CNT toughened B according to claim 14The preparation method of the C-SiC layered composite ceramic is characterized in that CNT, PVP and H in the CNT dispersion liquid2The mixing ratio of O is 1-50: 1: 100 to 500.
3. CNT toughened B according to claim 24The preparation method of the C-SiC layered composite ceramic is characterized in that the CNT toughens the B4The C-SiC laminated composite ceramic is designed with three layers, correspondingly, CNT dispersions with three proportions are adopted, namely CNT dispersion-1, CNT dispersion-2 and CNT dispersion-3, wherein the CNT dispersions in the CNT dispersion-1, the CNT dispersion-2 and the CNT dispersion-3 comprise CNT: PVP: h2The weight ratio of O is 1: 1: 200. 10: 1: 200. 20: 1: 200.
4. CNT toughened B according to claim 34Preparation method of C-SiC laminated composite ceramicCharacterized in that the CNT-B4CNT and B in C-Si composite slurry4The mixing ratio of C to simple substance silicon is 8-15: 10-50: 1 to 10, CNT-B4The weight proportion of the phenolic resin in the C-Si composite slurry is 1-10%.
5. CNT toughened B according to claim 44The preparation method of the C-SiC layered composite ceramic is characterized in that the simple substance silicon is silicon powder.
6. CNT toughened B according to claim 14The preparation method of the C-SiC layered composite ceramic is characterized in that the heating rate is 5-20 ℃/min.
7. CNT (carbon nanotube) toughening B4C-SiC layered composite ceramics, characterized in that it is obtained by the process according to any one of claims 1 to 6.
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| CN113773086A (en) * | 2021-09-01 | 2021-12-10 | 河北工业职业技术学院 | Polycrystal B4C-SiC double-layer composite material and preparation method thereof |
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Application publication date: 20200410 |