CN106747530B - Boron nitride nanosheet reinforced ceramic matrix composite and preparation method thereof - Google Patents
Boron nitride nanosheet reinforced ceramic matrix composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a boron nitride nanosheet reinforced ceramic matrix composite and a preparation method thereof. Firstly, respectively filling the boron nitride nanosheets and the ceramic powder into a container, and obtaining uniformly dispersed suspension by high-speed stirring and ultrasonic processing. After the pH values of the two suspensions are adjusted to be within a certain range, dropwise adding the boron nitride nanosheet suspension into the ceramic powder suspension, standing, precipitating, filtering, and drying to obtain mixed powder. And then placing the mixed powder in a graphite mold, carrying out hot-pressing sintering in a multifunctional sintering furnace, keeping the temperature for a period of time, and stopping heating to naturally cool the mixed powder to room temperature in the furnace to obtain a finished product. The method has the advantages of simple preparation method, good product performance, lower cost and easy realization of large-scale production, and the obtained boron nitride nanosheet reinforced ceramic matrix composite has good effects of excellent mechanical properties and excellent high-temperature stability.
Description
Technical Field
The invention relates to a preparation method of an inorganic non-metallic material, in particular to a boron nitride nanosheet reinforced ceramic matrix composite and a preparation method thereof.
Background
The ceramic material is unique in the field of materials by virtue of excellent properties, and the ceramic material has higher strength and elastic modulus, but the application of the ceramic material is severely limited by poor toughness, so that the problem of reinforcement and toughening of the ceramic material is solved above all. The boron nitride nanosheet has good high-temperature stability and chemical stability, high thermal conductivity, excellent dielectric property and good mechanical property, and has extremely high application potential in the aspect of ceramic toughening.
Typical ceramic material toughening methods include: phase change toughening, whisker and particle toughening, fiber toughening, nanowire and nanotube toughening and the like. But the effects of phase change, whisker and particle toughening are not particularly ideal; the operation process of fiber toughening is complex, the operation is not easy, and the compactness of the product is poor. At present, carbon nanotubes and graphene are used for toughening, and although the mechanical properties of ceramic materials can be greatly improved, the application of the carbon nanotubes and graphene is limited by the defects that the carbon nanotubes and graphene are easily oxidized at high temperature and easily react with matrix materials at high temperature. Compared with the prior art, the boron nitride material has excellent high-temperature stability, and the oxidation temperature can reach more than 800 ℃.
200910015758.1 discloses a boron nitride nanotube reinforced silicon nitride ceramic and a preparation method thereof, the boron nitride nanotube, silicon nitride powder and sintering aid are mixed by ball milling and then placed in a graphite die and a sintering furnace for sintering to obtain the boron nitride nanotube reinforced silicon nitride ceramic. 200910014220.9 discloses a method for preparing boron nitride nanotube reinforced alumina ceramics, which comprises ball-milling and mixing boron nitride nanotubes and alumina, and sintering in a graphite mold and a multifunctional sintering furnace to obtain boron nitride nanotube reinforced alumina ceramics. 201010196170.3 discloses a method for preparing boron nitride nanotube reinforced silicon dioxide ceramics, which comprises ball-milling and mixing boron nitride nanotube and nano-level powder and micron-level powder of silicon dioxide, placing in a multifunctional sintering furnace, and sintering in protective atmosphere to obtain the boron nitride nanotube reinforced silicon dioxide ceramics. 201010277828.3 discloses a preparation method of boron nitride nanotube reinforced and toughened zirconia ceramics, which comprises ball-milling and mixing boron nitride nanotubes and zirconia powder, sieving, pre-sintering in a muffle furnace, and sintering in a multifunctional sintering furnace to obtain boron nitride nanotube reinforced and toughened zirconia ceramics.
The boron nitride nanotube has good mechanical property, is an excellent ceramic toughening body, has been applied to the strengthening and toughening of ceramic materials, and can greatly improve the mechanical property of the ceramic materials. However, boron nitride nanotubes also have certain disadvantages in reinforcing ceramic materials: firstly, the boron nitride nanotube belongs to a one-dimensional nanostructure, and has a less obvious effect on the aspect of inhibiting crack propagation; secondly, the difficulty of large-scale synthesis of boron nitride nanotubes also limits their application in the preparation of composite materials.
In summary, in the prior art, an effective solution is not provided for the problems that the high-temperature stability of the ceramic matrix composite material reinforced by the carbon nanotubes and the graphene is poor, the boron nitride nanotubes are difficult to synthesize in a large scale, the effect of inhibiting crack propagation is not obvious when the ceramic material is reinforced, and the like.
Disclosure of Invention
In order to overcome the defects of the prior art that the high-temperature stability of the ceramic matrix composite reinforced by the carbon nano tube and the graphene is poor, the boron nitride nano tube is difficult to synthesize in a large scale, the effect of inhibiting crack propagation is not obvious when the ceramic material is reinforced, and the like, the invention provides the boron nitride nano sheet reinforced ceramic matrix composite and the preparation method thereof.
The boron nitride nanosheet reinforced ceramic matrix composite provided by the invention takes the boron nitride nanosheet as a reinforcing phase and the ceramic as a matrix.
Preferably, the ceramic matrix used in the present invention is magnesia ceramic, alumina ceramic, zirconia ceramic, silica ceramic, fused silica ceramic, mullite ceramic, silicon nitride ceramic, aluminum nitride ceramic, silicon oxynitride ceramic, silicon carbide ceramic, boron carbide ceramic, zirconium boride ceramic, or titanium boride ceramic.
Preferably, the ceramic substrate used in the present invention is fused silica ceramic. The fused quartz ceramic has poor mechanical properties, and the application of the fused quartz ceramic in the fields of aerospace, metallurgy and the like is severely limited.
Preferably, the mass fraction of the boron nitride nanosheet is 0.1-10.0 wt%,
preferably, the mass fraction of the boron nitride nanosheet is 0.5 wt% to 2.0 wt%.
The preparation method of the boron nitride nanosheet reinforced ceramic matrix composite material provided by the invention comprises the following steps:
(1) weighing a proper amount of boron nitride nanosheets and ceramic powder;
(2) respectively filling the boron nitride nanosheets and the ceramic powder into a glass container, adding a certain amount of distilled water, and then stirring at a high speed in cooperation with ultrasonic treatment to obtain a uniformly dispersed suspension;
(3) adjusting the pH value of the suspension obtained in the step (2) to a certain range;
(4) dropwise adding the boron nitride nanosheet suspension into the ceramic powder suspension, and stirring the ceramic powder suspension at a high speed while dropwise adding until the two are fully mixed to obtain a mixed solution;
(5) sealing, standing and precipitating the mixed solution obtained in the step (4), performing vacuum filtration to remove supernatant, and drying to obtain mixed powder;
(6) and (5) placing the mixed powder in the step (5) in a graphite mold, carrying out hot-pressing sintering in a protective atmosphere, and cooling to obtain the boron nitride nanosheet reinforced ceramic matrix composite.
Preferably, the reinforcing phase of the preparation method is a boron nitride nanosheet, the boron nitride nanosheet can be obtained by stripping hexagonal boron nitride powder, the preparation process is high in production efficiency, and the technical effect of large-scale synthesis can be realized more easily.
Preferably, the mass fraction of the boron nitride nanosheet added in the step (1) is 0.1-10.0 wt%,
preferably, the mass fraction of the boron nitride nanosheet added in the step (1) is 0.5 wt% to 2.0 wt%.
Preferably, the time of the high-speed stirring and ultrasonic treatment in the step (2) is 1-10 hours, so that the boron nitride nanosheets are distributed in the ceramic matrix more uniformly.
Preferably, the power of the ultrasonic cleaning instrument used for ultrasonic treatment in the step (2) is 40w, and the power is set to meet the requirement of uniform dispersion of the boron nitride nanosheets in the suspension, so that the damage to the structure of the nanosheets due to overhigh power is avoided.
Preferably, hydrochloric acid or an ammonia solution with a certain concentration can be used for adjusting the pH value of the suspension in the step (3), and the adjustment range of the pH value is changed according to the change of the types of the ceramic matrix.
Preferably, the time for sealing, standing and precipitating the mixed solution in the step (5) is 24-48 hours.
Preferably, in the step (5), the drying process parameters are that the drying temperature is 100 +/-5 ℃, the drying time is 24-48 hours, and then the product is sieved by a 200-mesh sieve.
Preferably, the hot-pressing sintering process in the step (6) is as follows: and (3) placing the mixed powder into a graphite mold, placing the mold into a multifunctional hot-pressing sintering furnace, heating to 1200-1900 ℃ at a heating rate of 19-21 ℃/min under a protective atmosphere, sintering under 25-30 Mpa, keeping the temperature for 1-1.5 hours, and stopping heating to naturally cool to room temperature in the furnace to obtain a finished product.
Preferably, the graphite mold in the step (6) has a diameter of 30 to 42 mm.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the boron nitride nanosheet is used as the reinforcing phase, so that a larger bonding area can be formed with the ceramic matrix, the interface bonding force is increased, the stress transfer efficiency from the matrix to the boron nitride nanosheet is improved, and the mechanical property of the material is improved. In addition, the cracks can be deflected on the plane, and the crack propagation can be even prevented on the three-dimensional space, so that the toughness of the ceramic material is further improved.
(2) The boron nitride nanosheet reinforced ceramic matrix composite material prepared by the invention has good high-temperature stability.
(3) The reinforcing phase selected by the preparation method is the boron nitride nanosheet, and the boron nitride nanosheet can be obtained by stripping hexagonal boron nitride powder, so that large-scale synthesis can be realized more easily.
(4) The equipment used by the invention is simple and has good safety, the preparation process is stable, the operation and treatment are simple, the production efficiency is high, the product performance is good, and the bending strength of the obtained product boron nitride nanosheet enhanced fused quartz ceramic reaches 100.8MPa and is improved by 53 percent compared with pure fused quartz ceramic.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is a scanning electron microscope topography of the mixed powder;
FIG. 2 is an X-ray diffraction pattern of a boron nitride nanosheet enhanced sample;
FIG. 3 is a scanning electron microscope topography of a boron nitride nanosheet enhanced sample;
fig. 4 is a bending strength curve of a boron nitride nanosheet reinforced sample.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide a preferred description of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings.
The surface morphology of the mixed powder in example 1 was tested using a scanning electron microscope, and the specific test results are shown in fig. 1. FIG. 1 is a scanning electron microscope topography of the mixed powder in example 1, and it can be seen from FIG. 1 that the boron nitride nanosheets are relatively uniformly dispersed in the powder, no significant agglomeration occurs, and the structure of the nanosheets is not destroyed.
The crystal phase of the composite material of example 1 was measured by X-ray and the specific test results are shown in FIG. 2. FIG. 2 is an X-ray diffraction diagram of the boron nitride nanosheet-enhanced fused silica ceramic prepared in example 1. The product is shown in fig. 2 as being predominantly amorphous with minimal crystallization, indicating that the sintered fused silica-based composite remains predominantly amorphous. Meanwhile, as the mass fraction of the added boron nitride nanosheets is small, no diffraction peak of hexagonal boron nitride appears in fig. 2.
The fracture morphology of the composite material of example 1 was tested by a scanning electron microscope, and the specific test results are shown in fig. 3. FIG. 3 is a fracture morphology diagram of the boron nitride nanosheet-reinforced fused silica ceramic prepared in example 1. The fracture morphology graph shows that the boron nitride nanosheets are relatively uniformly distributed in the fused quartz matrix. In the process of material fracture, the pulling-out of the boron nitride nanosheets and the bridging at the fracture can consume the energy of crack propagation, so that the performance of the material is effectively improved.
Fig. 4 is a curve showing the change in bending strength of the boron nitride nanosheet-reinforced fused silica ceramic. As can be seen from fig. 4, the mechanical properties of the composite material are improved compared to pure fused silica ceramic. The sample with the boron nitride nanosheet content of 0.5 wt% achieves the highest bending strength value of 100.8MPa, which is 53% higher than that of pure fused quartz ceramic. When the content of the nanosheets is greater than 0.5 wt%, the flexural strength of the composite material gradually decreases as the content of the nanosheets increases.
Example 1:
boron nitride nanosheets are used as a reinforcing phase, and the fused quartz-based composite material is prepared by adopting hot-pressing sintering.
1) A step of; respectively putting 0.06g of boron nitride nanosheet and 11.94g of fused quartz powder into a glass container by using a balance scale, adding 1000mL of distilled water into the container, and performing high-speed stirring and ultrasonic treatment for 8 hours to obtain uniformly dispersed suspension;
2) a step of; adjusting the pH values of the two suspensions to 3 by adopting a hydrochloric acid diluted solution (1M), dropwise adding the boron nitride nanosheet suspension into the fused silica suspension, and stirring the fused silica suspension at a high speed while dropwise adding so as to fully mix the two suspensions;
3) a step of; then sealing, standing and precipitating the obtained mixed solution for 24 hours, removing supernatant through vacuum filtration, and drying for 24 hours to obtain mixed powder;
4) a step of; placing the mixed powder in a graphite mold, placing the graphite mold in a multifunctional sintering furnace, heating to 1300 ℃ at the speed of 20 ℃/min, pressurizing to 30Mpa for sintering, and preserving heat for 1 hour to naturally cool the mixed powder to room temperature in the furnace;
5) a step of; and grinding and cutting the sintered ceramic block to obtain a finished product.
Example 2:
boron nitride nanosheets are used as a reinforcing phase, and the fused quartz-based composite material is prepared by adopting hot-pressing sintering.
1) A step of; respectively putting 0.12g of boron nitride nanosheet and 11.88g of fused quartz powder into a glass container by using a balance scale, adding 800mL of distilled water into the container, and performing high-speed stirring and ultrasonic treatment for 10 hours to obtain uniformly dispersed suspension;
2) a step of; adjusting the pH values of the two suspensions to 3 by adopting a hydrochloric acid diluted solution (1M), dropwise adding the boron nitride nanosheet suspension into the fused silica suspension, and stirring the fused silica suspension at a high speed while dropwise adding so as to fully mix the two suspensions;
3) a step of; sealing, standing and precipitating the obtained mixed solution for 24 hours, removing supernatant liquid through vacuum filtration, and drying for 24 hours to obtain mixed powder;
4) a step of; and placing the mixed powder into a graphite mold, placing the graphite mold into a multifunctional sintering furnace, heating to 1300 ℃ at the speed of 20 ℃/min, pressurizing to 30Mpa for sintering, and preserving heat for 1 hour to naturally cool the mixed powder to room temperature in the furnace.
5) And grinding and cutting the sintered ceramic block to obtain a finished product.
Example 3:
boron nitride nanosheets are used as a reinforcing phase, and the fused quartz-based composite material is prepared by adopting hot-pressing sintering.
1) A step of; respectively putting 0.18g of boron nitride nanosheet and 11.82g of fused quartz powder into a glass container by using a balance scale, adding 700mL of distilled water into the container, and performing high-speed stirring and ultrasonic treatment for 8 hours to obtain uniformly dispersed suspension;
2) a step of; then, regulating the pH values of the two suspensions to 3.5 by adopting a hydrochloric acid diluted solution (2M), dropwise adding the boron nitride nanosheet suspension into the fused quartz suspension, and stirring the fused quartz suspension at a high speed while dropwise adding so as to fully mix the two suspensions;
3) a step of; then sealing, standing and precipitating the obtained mixed solution for 40 hours, removing supernatant liquid through vacuum filtration, and drying for 34 hours to obtain mixed powder;
4) a step of; and placing the mixed powder into a graphite mold, placing the graphite mold into a multifunctional sintering furnace, heating to 1200 ℃ at a speed of 20 ℃/min, pressurizing to 30Mpa for sintering, and preserving heat for 2 hours to naturally cool the mixed powder to room temperature in the furnace.
5) A step of; and grinding and cutting the sintered ceramic block to obtain a finished product.
Example 4:
boron nitride nanosheets are used as a reinforcing phase, and the fused quartz-based composite material is prepared by adopting hot-pressing sintering.
1) A step of; respectively putting 0.24g of boron nitride nanosheet and 11.76g of fused quartz powder into a glass container by using a balance scale, adding 1000mL of distilled water into the container, and performing high-speed stirring and ultrasonic treatment for 8 hours to obtain uniformly dispersed suspension;
2) a step of; then, regulating the pH values of the two suspensions to 3 by adopting a hydrochloric acid diluted solution (1M), dropwise adding the boron nitride nanosheet suspension into the fused quartz suspension, and stirring the fused quartz suspension at a high speed while dropwise adding so as to fully mix the two suspensions;
3) a step of; then sealing, standing and precipitating the obtained mixed solution for 24 hours, removing supernatant liquid through vacuum filtration, and drying for 48 hours to obtain mixed powder;
4) a step of; placing the mixed powder in a graphite mold, placing the graphite mold in a multifunctional sintering furnace, heating to 1350 ℃ at the speed of 20 ℃/min, sintering under the pressure of 30Mpa, and preserving heat for 1 hour to naturally cool the mixed powder to room temperature in the furnace;
5) a step of; and grinding and cutting the sintered ceramic block to obtain a finished product.
Example 5:
the boron nitride nanosheet is used as a reinforcing phase, and the alumina-based ceramic composite material is prepared by adopting hot-pressing sintering.
1) A step of; weighing 0.085g of boron nitride nanosheet and 16.915g of alumina powder by using a balance, respectively putting into a glass container, adding 800mL of distilled water into the container, and performing high-speed stirring and ultrasonic treatment for 10 hours to obtain uniformly dispersed suspension;
2) a step of; then, adjusting the pH values of the two suspensions to 6 by adopting a hydrochloric acid diluted solution (1M) and an ammonia water diluted solution (1M), dropwise adding the boron nitride nanosheet suspension into the alumina suspension, and stirring the alumina suspension at a high speed while dropwise adding so as to fully mix the two suspensions;
3) a step of; then sealing, standing and precipitating the obtained mixed solution for 24 hours, removing supernatant through vacuum filtration, and drying for 24 hours to obtain mixed powder;
4) a step of; placing the mixed powder in a graphite mold, placing the graphite mold in a multifunctional sintering furnace, heating to 1500 ℃ at a speed of 20 ℃/min, sintering under a pressure of 30Mpa, and preserving heat for 1 hour to naturally cool the mixed powder to room temperature in the furnace;
5) a step of; and grinding and cutting the sintered ceramic block to obtain a finished product.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (4)
1. A boron nitride nanosheet reinforced ceramic matrix composite is characterized in that the boron nitride nanosheet is used as a reinforcing phase, and ceramic is used as a matrix;
the preparation method of the boron nitride nanosheet reinforced ceramic matrix composite material comprises the following steps:
(1) weighing a proper amount of boron nitride nanosheets and ceramic powder;
(2) respectively filling the boron nitride nanosheets and the ceramic powder into a glass container, adding a certain amount of distilled water, then stirring at a high speed and performing ultrasonic treatment to obtain uniformly dispersed suspension, and respectively adjusting the pH value of the uniformly dispersed suspension;
(3) dropwise adding the boron nitride nanosheet suspension into the ceramic powder suspension, and stirring the ceramic powder suspension at a high speed while dropwise adding until the two are fully mixed to obtain a mixed solution;
(4) sealing, standing and precipitating the mixed solution obtained in the step (3), performing vacuum filtration to remove supernatant, and drying to obtain mixed powder;
(5) placing the mixed powder in the step (4) in a graphite mold, carrying out hot-pressing sintering in a protective atmosphere, and cooling to obtain the boron nitride nanosheet reinforced ceramic matrix composite;
selecting a boron nitride nanosheet as a reinforcing phase of the preparation method in the step (1), wherein the boron nitride nanosheet is obtained by stripping hexagonal boron nitride powder;
the hot-pressing sintering process in the step (5) comprises the following steps: placing the mixed powder into a graphite mold, placing the mold into a multifunctional hot-pressing sintering furnace, heating to 1200-1900 ℃ at a heating rate of 19-21 ℃/min under a protective atmosphere, sintering under 25-30 MPa, keeping the temperature for 1-1.5 hours, and stopping heating to naturally cool the mixed powder to room temperature in the furnace to obtain a finished product, wherein the diameter of the graphite mold is 30-42 mm;
the ceramic matrix is fused quartz ceramic;
the mass fraction of the boron nitride nanosheet is 0.1-10.0 wt%.
2. The boron nitride nanosheet-reinforced ceramic matrix composite of claim 1, wherein the boron nitride nanosheet has a mass fraction of 0.5 wt% to 2.0 wt%.
3. The boron nitride nanosheet-reinforced ceramic matrix composite material according to claim 1, wherein the time for the high-speed stirring and ultrasonic treatment in step (2) is 1-10 hours, the power of an ultrasonic cleaning instrument for ultrasonic treatment is 40w, and the pH value of the suspension is adjusted by using hydrochloric acid or an ammonia water solution with a certain concentration.
4. The boron nitride nanosheet-reinforced ceramic matrix composite of claim 1, wherein the mixed solution in step (4) is sealed, left to stand and precipitated for 24 to 48 hours; the drying process parameters are that the drying temperature is 100 +/-5 ℃, and the drying time is 24-48 hours.
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| CN103044014B (en) * | 2013-01-17 | 2014-03-12 | 山东大学 | Preparation method of graphene-nanosheet-reinforced alumina ceramic |
| CN106082147B (en) * | 2016-05-31 | 2018-06-05 | 山东大学 | The method that a kind of liquid phase chemical stripping of stabilization prepares boron nitride nanosheet |
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