CN111018540A - High-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering - Google Patents

High-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering Download PDF

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CN111018540A
CN111018540A CN202010034774.1A CN202010034774A CN111018540A CN 111018540 A CN111018540 A CN 111018540A CN 202010034774 A CN202010034774 A CN 202010034774A CN 111018540 A CN111018540 A CN 111018540A
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sintering
boron nitride
powder
composite material
ceramic composite
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徐淑波
孙化鑫
孙海波
张世超
王瀚林
刘建营
孙星
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Shandong Jianzhu University
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Abstract

A high-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering belongs to the technical field of ceramic preparation. The invention is obtained by the following method. High-purity hexagonal boron nitride (h-BN) powder is taken as a raw material, titanium carbide whiskers, silicon carbide whiskers and a small amount of sintering aid B are added2O3Stirring under the ultrasonic environment, then adding chromium and graphene, and stirring under the ultrasonic condition. Putting the raw materials into a ball milling tank, adding zirconia grinding balls (the material ball ratio is 1:10) by taking absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 20 h, drying for 12 h in a drying box, and finally grinding and sieving the mixture to obtain uniform composite powder. At a lower sintering temperature (1300-1500℃)DEG C) preparing the boron nitride ceramic composite material by a hot-pressing sintering method. In a lower sintering temperature range, the density and the bending strength of the boron nitride ceramic composite material can be obviously improved by increasing the sintering temperature and the sintering pressure, but the increase range of the fracture toughness is smaller.

Description

High-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering
Technical Field
The invention relates to the technical field of ceramic preparation, in particular to a boron nitride ceramic composite material which is suitable for h-BN and other substances with a layered crystal structure similar to hexagonal graphite, and is difficult to densify in the sintering process due to the fact that the substances are combined by strong covalent bonds in the layers and the diffusion coefficient is low.
Background
The h-BN ceramic has been widely applied to the fields of chemical industry, metallurgy, photoelectricity, semiconductor electronics, aerospace, atomic energy and the like due to high thermal conductivity, low dielectric constant, good high-temperature electrical insulation performance, small thermal expansion coefficient, good heat resistance, easy processing and the like, but because the h-BN has a layered crystal structure similar to hexagonal graphite, the densification of the boron nitride ceramic composite material in the layer is difficult due to very strong covalent bond combination and low diffusion coefficient, and the flaky boron nitride crystal grains are easy to form a mutually cross-stacked 'card house' layered structure, more pores which are difficult to fill are generated among the crystal grains, and the larger the crystal grains are, the situation is more serious, the density of the prepared boron nitride ceramic composite material is reduced finally, so the h-BN ceramic material with high densification degree is required to be obtained, it is necessary to add appropriate additives, control the size of the grains and select an appropriate sintering method.
Therefore, based on the above purpose, the method for preparing a high-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering provided by the invention can solve the above problems by adding titanium carbide whiskers, silicon carbide whiskers, and mixing chromium and graphene under an ultrasonic condition, so that more atoms in the composite material are activated, diffusion is accelerated, the density is increased, the porosity is reduced, and grain boundary bonding is firmer, so that the fracture toughness and the bending strength are both improved, h-BN ceramic with higher density can be prepared, and the method has very important industrial application value.
Disclosure of Invention
The invention aims to provide the following technical scheme: aiming at the difficulty in densification caused by the structure of the material, the invention provides the method for sintering the boron nitride ceramic composite material by low-temperature hot pressing.
The technical scheme of the invention is as follows: the invention relates to a method for preparing a high-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering and a preparation process of powder.
The invention relates to a ceramic sintering method suitable for low-temperature hot pressing and preparation of powder, wherein high-purity hexagonal boron nitride (h-BN) powder is used as a raw material, titanium carbide whiskers, silicon carbide whiskers and a small amount of sintering aid B2O3 are added, stirring is carried out in an ultrasonic environment, then chromium and graphene are added, stirring is carried out under the ultrasonic condition, the raw material is placed into a ball milling tank, absolute ethyl alcohol is used as a ball milling medium, zirconium oxide grinding balls (the ball-ball ratio is 1:10) are added, drying is carried out in a drying box for 12 h after ball milling for 20 h, and finally, the mixture is ground and sieved to obtain uniform composite powder.
The invention relates to a method for sintering low-temperature hot-pressed ceramics.
The first step is as follows: selecting boron nitride fine powder with purity more than 99wt.% and average particle size of about 1 μm, and adding sintering aid B2O3The purity is more than 98%, and the addition amount is 10 wt.%.
The second step is that: adding titanium carbide whiskers and silicon carbide whiskers to enable the content of the titanium carbide whiskers and the silicon carbide whiskers to be 7% -12% in boron nitride powder, adding 5% of chromium and 0.2% of graphene, and mixing to form uniform composite powder.
The third step: putting the mixed powder into a ball milling tank, adding zirconia grinding balls (the material ball ratio is 1:10) by taking absolute ethyl alcohol as a ball milling medium, and carrying out ball milling for 20 hours.
The fourth step: and drying the ball-milled raw materials in a drying oven for 12 hours, and finally grinding and sieving the mixture to obtain uniform composite powder.
The fifth step: and putting the obtained uniform composite powder into a sintering furnace, continuously filling nitrogen for protection in the sintering process, and ensuring that the sintering temperature is changed under a fixed sintering pressure in the sintering process, wherein the temperature range is 1300-1500 ℃, and on the other hand, the fixed sintering temperature changes the sintering pressure in the range of 20-30 MPa, so that the optimal sintering scheme is obtained.
Compared with the prior art, the invention has the following advantages.
(1) The h-BN ceramic with higher density can be prepared by adopting low-temperature hot-pressing sintering, and the densification of the h-BN ceramic can be obviously promoted by increasing the sintering temperature and the sintering pressure.
(2) The boron nitride ceramic composite material with uniform and fine grains can be obtained by hot-pressing sintering at low temperature, the grain size is slightly increased along with the increase of the sintering temperature, and the fine flaky grains are beneficial to the movement and rearrangement of the grains and can promote the sintering densification of the boron nitride ceramic composite material.
(3) The ultrasonic wave is used in the stirring process, so that the components of the powder are distributed more uniformly and more fully in the sintering process.
(4) The titanium carbide whisker, the silicon carbide whisker, the chromium and the graphene are added, so that the fracture resistance and the bending resistance of the ceramic can be further improved, the ceramic is corrosion-resistant, and the sintering densification of the boron nitride ceramic composite material can be promoted.
Detailed Description
The following is a description of preferred embodiments of the present invention.
Mixing high-purity hexagonal boron nitride fine powder (purity is more than 99wt.%, and average particle size is about 1 μm) with sintering aid B2O3Mixing with the addition of 10wt.%, adding titanium carbide whisker and silicon carbide whisker to make the content of the titanium carbide whisker and the silicon carbide whisker in the boron nitride powder be 7-12%, stirring for 30min under the ultrasonic condition after mixing, adding chromium 5%,0.2% of graphene, stirring for 30min under the ultrasonic condition again to obtain mixed powder, putting the mixed powder into a ball milling tank, adding zirconia grinding balls (the material-ball ratio is 1:10) by taking absolute ethyl alcohol as a ball milling medium, carrying out ball milling for 20 h, drying the ball-milled raw materials in a drying box for 12 h, finally grinding and sieving the mixture to obtain uniform composite powder, putting the obtained uniform composite powder into a sintering furnace, continuously filling nitrogen for protection in the sintering process, ensuring that the temperature is 1450 ℃ and the pressure is 30MPa in the sintering process, and preparing the h-BN ceramic composite material with the relative density of about 96% under the sintering condition.

Claims (7)

1. A high-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering is characterized in that high-purity hexagonal boron nitride (h-BN) powder is used as a raw material, titanium carbide whiskers, silicon carbide whiskers and a small amount of sintering aid B are added2O3Stirring under an ultrasonic environment, adding chromium and graphene, stirring under an ultrasonic condition, putting raw materials into a ball milling tank, taking absolute ethyl alcohol as a ball milling medium, adding zirconia grinding balls (the material ball ratio is 1:10), drying in a drying oven for 12 hours after ball milling for 20 hours, finally grinding and sieving mixed powder to obtain uniform composite powder, putting the composite powder into a sintering furnace for sintering, filling nitrogen for protection in the sintering process, and setting the heat preservation time at the highest sintering temperature to be 1 hour;
(a) in the whole preparation process, the purity of the boron nitride fine powder is more than 99wt.%, and the average grain diameter is about 1 mu m2O3The purity of the powder is more than 98%, and the addition amount is 10 wt.%;
(b) the content of the titanium carbide whisker and the silicon carbide whisker in the boron nitride powder is 7-12%, 5% of chromium and 0.2% of graphene are added, and the titanium carbide whisker and the silicon carbide whisker are mixed to form uniform composite powder;
(c) and nitrogen is filled in the sintering process for protection, the sintering temperature is guaranteed to be changed under the fixed sintering pressure, the temperature range is 1300-1500 ℃, and on the other hand, the fixed sintering temperature changes the sintering pressure, and the range is 20-30 MPa.
2. According to claim 1: the titanium carbide whisker and the silicon carbide whisker have higher strength and elastic modulus.
3. According to claim 1: the raw materials are added and stirred twice in an ultrasonic environment, the sound flow effect of ultrasonic waves can be utilized, so that the components of the powder are more uniform and are more sufficient in the sintering process, and the stirring time is 20-50 min.
4. According to claim 1: the chromium has high strength, good toughness and corrosion resistance, and can further improve the hardness and the fracture resistance of the ceramic.
5. According to claim 1: the graphene has extremely high strength and good toughness, can improve the bending resistance of the material, and prolongs the service life.
6. According to claim 1: when absolute ethyl alcohol is used as a dispersing medium, the mixed powder is more uniformly dispersed, the titanium carbide whiskers and the silicon carbide whiskers can be prevented from agglomerating and winding, and the sintering densification of the boron nitride ceramic composite material is promoted.
7. According to claim 1: the boron nitride ceramic composite material with uniform and fine grains can be obtained by hot-pressing sintering at low temperature, the grain size is slightly increased along with the increase of the sintering temperature, and fine flaky particles are favorable for the movement of the particles and can promote the sintering densification of the boron nitride ceramic composite material.
CN202010034774.1A 2020-01-14 2020-01-14 High-strength boron nitride ceramic composite material based on low-temperature hot-pressing sintering Pending CN111018540A (en)

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CN111848179A (en) * 2020-08-04 2020-10-30 山东理工大学 Preparation method of high-strength boron nitride ceramic capable of being used in ultrahigh-temperature environment
CN112296889A (en) * 2020-11-06 2021-02-02 河南科恩超硬材料技术有限公司 Thinned porous ceramic composite bonding agent for SIC wafer, diamond tool bit, grinding wheel and manufacturing method of grinding wheel
CN113278893A (en) * 2021-05-31 2021-08-20 山东建筑大学 Steel composition for shield machine cutter under complex spring domain condition and preparation
CN113683431A (en) * 2021-06-23 2021-11-23 重庆科技学院 Aluminum borate whisker reinforced and toughened nonmetal-based composite material and preparation method thereof
CN113929430A (en) * 2021-10-26 2022-01-14 清华大学深圳国际研究生院 Preparation method of pure or composite hexagonal boron nitride densified macroscopic body

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CN105198443A (en) * 2015-10-21 2015-12-30 哈尔滨工业大学 Transition phase assisted low-temperature sintering method of boron nitride multi-phase ceramic
CN105908041A (en) * 2016-04-27 2016-08-31 富耐克超硬材料股份有限公司 High-tenacity polycrystalline composite material, high-tenacity polycrystalline blade and preparation method of high-tenacity polycrystalline blade
CN109574677A (en) * 2017-09-28 2019-04-05 河南海纳德新材料有限公司 A kind of bonding agent, polycrystalline cubic boron nitride composite material and preparation method

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Publication number Priority date Publication date Assignee Title
CN102173792A (en) * 2011-02-23 2011-09-07 哈尔滨工业大学 Ceramic composite material for thin-strip casting side sealing plate and preparation method thereof
CN105198443A (en) * 2015-10-21 2015-12-30 哈尔滨工业大学 Transition phase assisted low-temperature sintering method of boron nitride multi-phase ceramic
CN105908041A (en) * 2016-04-27 2016-08-31 富耐克超硬材料股份有限公司 High-tenacity polycrystalline composite material, high-tenacity polycrystalline blade and preparation method of high-tenacity polycrystalline blade
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848179A (en) * 2020-08-04 2020-10-30 山东理工大学 Preparation method of high-strength boron nitride ceramic capable of being used in ultrahigh-temperature environment
CN111848179B (en) * 2020-08-04 2022-12-02 山东理工大学 Preparation method of high-strength boron nitride ceramic capable of being used in ultrahigh-temperature environment
CN112296889A (en) * 2020-11-06 2021-02-02 河南科恩超硬材料技术有限公司 Thinned porous ceramic composite bonding agent for SIC wafer, diamond tool bit, grinding wheel and manufacturing method of grinding wheel
CN112296889B (en) * 2020-11-06 2021-11-09 河南科恩超硬材料技术有限公司 Thinned porous ceramic composite bonding agent for SIC wafer, diamond tool bit, grinding wheel and manufacturing method of grinding wheel
CN113278893A (en) * 2021-05-31 2021-08-20 山东建筑大学 Steel composition for shield machine cutter under complex spring domain condition and preparation
CN113683431A (en) * 2021-06-23 2021-11-23 重庆科技学院 Aluminum borate whisker reinforced and toughened nonmetal-based composite material and preparation method thereof
CN113929430A (en) * 2021-10-26 2022-01-14 清华大学深圳国际研究生院 Preparation method of pure or composite hexagonal boron nitride densified macroscopic body

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Application publication date: 20200417