CN110395988B - High-strength boron nitride ceramic and preparation method thereof - Google Patents
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Abstract
The invention relates to a high-strength boron nitride ceramic and a preparation method thereof, wherein the preparation method comprises the following steps: A) charging: weighing a certain mass of single-particle-size nano cubic boron nitride powder, prepressing and forming, and putting a prepressed blank after prepressing and forming into a sintering mold; B) and (3) sintering: putting the pre-pressed blank in the step A) and the sintering mould into discharge plasma sintering equipment or hot-pressing sintering equipment for sintering; C) discharging: and taking out the mold after the temperature in the equipment is cooled to room temperature, and demolding to obtain the high-strength boron nitride ceramic block. The invention obtains the high-strength boron nitride ceramic by sintering the nano cubic boron nitride powder with single grain diameter.
Description
Technical Field
The invention relates to the technical field of structural ceramic preparation, in particular to high-strength boron nitride ceramic and a preparation method thereof.
Background
Hexagonal boron nitride (hBN) ceramics are typically bulk materials formed by sintering hexagonal boron nitride powder, an advanced structural ceramic. It has excellent physical properties including high insulation, low dielectric coefficient, high thermal conductivity, and excellent thermal shock resistance, and thus is widely used. However, due to the special layered structure of the hexagonal boron nitride ceramic, the bonding force in the C axis direction is far smaller than the bonding force perpendicular to the C axis direction, the crystal mainly grows in the plate surface direction, and the growth in the thickness direction is slower, so that a flaky crystal structure is formed, and the flaky crystal structure forms a card bridging structure when being sintered, so that the mutual supporting effect is achieved, and the material shrinkage is hindered, so that the obtained hBN ceramic has low density, and the influence of weak van der waals force between layers is added, so that the prepared hexagonal boron nitride ceramic has poor mechanical properties and low strength, and the further development and application of the hexagonal boron nitride ceramic are greatly limited.
Because hexagonal boron nitride ceramics are difficult to sinter, the relative density of pure hexagonal boron nitride can only reach about 70 percent after sintering, for example, the density of the hexagonal boron nitride ceramics prepared by taking high-purity hexagonal boron nitride powder as a raw material is only about 56 percent in the method for preparing the high-purity hexagonal boron nitride ceramics by pressureless sintering with the application number of 201410422994.6, and in order to improve the density of the hexagonal boron nitride ceramics, most methods are to add a sintering aid, such as B, in the sintering process2O3、Y2O3、Al2O3、SiO2And AlN, etc., the density of hexagonal boron nitride obtained by adding a sintering aid is somewhat improved, but the high-temperature use properties thereof are reduced. For example, the preparation method of the high-density hexagonal boron nitride ceramic material with the application number of 201410393724.7 discloses that SiO is coated on the surface of hBN powder2Realization of SiO2The sintering aid is uniformly distributed, and a high-density hBN block is obtained by spark plasma sintering or hot isostatic pressing sintering, but the surface of hBN powder is coated with SiO2The process is complex, and the density of the prepared high-density h-BN block is only 86.4 percent at most, and the compression strength is 79MPa at most.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a high-strength boron nitride ceramic and a preparation method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of high-strength boron nitride ceramic comprises the following steps:
A) charging: weighing a certain mass of single-particle-size nano cubic boron nitride powder, prepressing and forming, and putting a prepressed blank after prepressing and forming into a sintering mold;
B) and (3) sintering: putting the pre-pressed blank in the step A) and the sintering mould into discharge plasma sintering equipment or hot-pressing sintering equipment for sintering;
C) discharging: and taking out the mold after the temperature in the equipment is cooled to room temperature, and demolding to obtain the high-strength boron nitride ceramic block.
The technical scheme of the invention is further improved as follows: the sintering mould in the step A) is a graphite mould, and the prepressing blank and the graphite mould are separated by graphite paper.
The technical scheme of the invention is further improved as follows: the prepressing molding in the step A) is carried out to apply pressure in two directions, and the pressure is 5 MPa-10 MPa.
The technical scheme of the invention is further improved as follows: the grain diameter of the single grain diameter nanometer cubic boron nitride powder in the step A) is 10 nm-500 nm.
The technical proposal of the invention is further improved in that the sintering step in the step B) is to apply pre-pressure and vacuumize until the vacuum degree is higher than 1 × 10-1And applying sintering pressure after Pa, heating to the sintering temperature after the sintering pressure is stable, closing the heating program after high-temperature sintering and releasing pressure.
The technical scheme of the invention is further improved as follows: the prepressing pressure applied in the step B) is 5MPa to 10MPa, the sintering pressure is 30MPa to 50MPa, the sintering temperature is 1400 ℃ to 2000 ℃, and the heat preservation time is 1min to 30 min.
The technical scheme of the invention is further improved as follows: the sintering mode in the step B) is spark plasma sintering or hot-pressing sintering.
The technical scheme of the invention is further improved as follows: the temperature rising rate of the step B) is 50-150 ℃/min.
The application also provides the high-strength boron nitride ceramic prepared by the preparation method, wherein the compressive strength is not lower than 500MPa, and the compressive strain is not lower than 8%.
Due to the adoption of the technical scheme, the invention has the technical progress that:
the invention relates to a high-strength boron nitride ceramic and a preparation method thereof.
The nanometer cubic boron nitride powder with single grain size is used, the phase change of the boron nitride powder occurs in the sintering process, the outer layer of the cubic boron nitride powder is graphitized to become hexagonal boron nitride, the central part of the powder still keeps the cubic structure, and the transition phase exists in the middle.
When in prepressing forming, the powder is exerted with pressure in two directions, the nanometer cubic boron nitride powder in the compression mould is exerted with force in two directions, the upper and lower pressure gradients of the prepressing blank are reduced, the overlarge upper and lower pressure gradients caused by unidirectional pressure application are avoided, the difference between the upper and lower densities of the prepressing blank is large, the integral density of the sintered block is further influenced, the powder can be compressed more compactly by bidirectional pressure application, and the subsequent sintering of the prepressing blank is facilitated.
The sintering pressure is set to be 30-50 MPa, the pressure range can control the phase change speed of the cubic boron nitride, not only ensures that the powder is not completely changed into the hexagonal boron nitride after being completely sintered, but also prevents the crystal grains from growing too fast and ensures the compactness of the prepared boron nitride ceramic.
Graphite paper separates graphite mould and pre-pressing base, prevents that pre-pressing base and graphite mould sintering together lead to being difficult to the demolding in the sintering process and obtain the block, also avoids forcibly taking off the block and cause the damage to graphite mould, can improve the life of mould.
Drawings
FIG. 1(a) is an X-ray diffraction spectrum of a product produced in example 1 of the present invention, and FIG. 1(b) is a uniaxial compressive stress strain curve of the product produced in example 1 of the present invention;
FIG. 2(a) is an X-ray diffraction spectrum of a product produced in example 2 of the present invention, and FIG. 2(b) is a uniaxial compressive stress strain curve of the product produced in example 2 of the present invention;
FIG. 3(a) is an X-ray diffraction spectrum of a product produced in example 3 of the present invention, and FIG. 3(b) is a uniaxial compressive stress strain curve of the product produced in example 3 of the present invention;
FIG. 4(a) is an X-ray diffraction spectrum of a product of example 4 of the present invention, and FIG. 4(b) is a uniaxial compressive stress strain curve of the product of example 4 of the present invention;
FIG. 5(a) is an X-ray diffraction spectrum of a product produced in example 5 of the present invention, and FIG. 5(b) is a uniaxial compressive stress strain curve of the product produced in example 5 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples:
example 1
The preparation method of the high-strength boron nitride ceramic comprises the following steps:
A) charging: weighing 2g of single-particle-size nano cubic boron nitride powder, wherein the particle size of the single-particle-size nano cubic boron nitride powder is 50nm, pre-pressing and forming, wherein the pre-pressing and forming is bidirectional pressure application, the pressure is 10MPa, the pre-pressed blank after pre-pressing and forming is placed into a sintering mold, the sintering mold is a graphite mold, and the pre-pressed blank and the graphite mold are separated by graphite paper;
B) sintering, namely putting the prepressing blank in the step A) and a sintering mold into a spark plasma sintering device for sintering, wherein the sintering mode is spark plasma sintering, the sintering step is to apply prepressing force firstly, the prepressing force is 10MPa, and vacuumizing is carried out until the vacuum degree is higher than 1 × 10-1Applying sintering pressure after Pa, wherein the sintering pressure is 30MPa, heating to the sintering temperature after the sintering pressure is stable, the heating rate is 150 ℃/min, the sintering temperature is 1600 ℃, the heat preservation time is 4min, and closing the heating program and releasing the pressure after high-temperature sintering;
the spark plasma sintering equipment used in this example was SPS-3.20MK-IV, Sumitomo Stone coal mining Co., Ltd;
C) discharging: and taking out the mold after the temperature in the equipment is cooled to room temperature, and demolding to obtain the high-strength boron nitride ceramic block.
The invention is used for testing the compression strength of the prepared high-strength boron nitride ceramic, and the test sample is a cylinder, and the size of the test sample is 3mm in diameter and 4.5mm in height.
The high-strength boron nitride ceramic prepared by the method for preparing the high-strength boron nitride ceramic of the present example is an opaque block, and as shown in fig. 1(a), the high-strength boron nitride ceramic block is a nano polycrystalline block composed of hexagonal boron nitride (hBN) and a small amount of cubic boron nitride (cBN), and as shown in fig. 1(b), the high-strength boron nitride ceramic block has a compressive strength of 935MPa and a compressive strain of 12%.
Example 2
The process steps of the preparation method of the high-strength boron nitride ceramic of the embodiment are similar to those of the embodiment 1, and specific process parameters different from those of the embodiment 1 are shown in the example 2 column in the table 1.
The high-strength boron nitride ceramic prepared by the method for preparing a high-strength boron nitride ceramic of this example is an opaque block, and as shown in fig. 2(a), the high-strength boron nitride ceramic block is a nano polycrystalline block composed of hexagonal boron nitride (hBN) and a small amount of cubic boron nitride (cBN), and as shown in fig. 2(b), the high-strength boron nitride ceramic block has a compressive strength of 820MPa and a compressive strain of 11%.
Example 3
The process steps of the preparation method of the high-strength boron nitride ceramic of the embodiment are similar to those of the embodiment 1, and specific process parameters different from those of the embodiment 1 are shown in the example 3 column in the table 1.
The high-strength boron nitride ceramic prepared by the method for preparing a high-strength boron nitride ceramic of this example is an opaque block, and as shown in fig. 3(a), the high-strength boron nitride ceramic block is a nano polycrystalline block composed of hexagonal boron nitride (hBN) and a small amount of cubic boron nitride (cBN), and as shown in fig. 3(b), the high-strength boron nitride ceramic block has a compressive strength of 707MPa and a compressive strain of 10.3%.
Example 4
The process steps of the preparation method of the high-strength boron nitride ceramic of the embodiment are similar to those of the embodiment 1, and specific process parameters different from those of the embodiment 1 are shown in the example 4 column in the table 1.
The high-strength boron nitride ceramic prepared by the method for preparing a high-strength boron nitride ceramic of this example is an opaque block, and as shown in fig. 4(a), the high-strength boron nitride ceramic block is a nano polycrystalline block composed of hexagonal boron nitride (hBN) and a small amount of cubic boron nitride (cBN), and as shown in fig. 4(b), the high-strength boron nitride ceramic block has a compressive strength of 615MPa and a compressive strain of 9.8%.
Example 5
The process steps of the preparation method of the high-strength boron nitride ceramic of the embodiment are similar to those of the embodiment 1, and specific process parameters different from those of the embodiment 1 are shown in the example 5 column in the table 1.
The high-strength boron nitride ceramic prepared by the method for preparing a high-strength boron nitride ceramic of this example is an opaque block, and as shown in fig. 5(a), the high-strength boron nitride ceramic block is a nano polycrystalline block composed of hexagonal boron nitride (hBN) and a small amount of cubic boron nitride (cBN), and as shown in fig. 5(b), the high-strength boron nitride ceramic block has a compressive strength of 520MPa and a compressive strain of 8.8%.
TABLE 1 EXAMPLES 1-5 parameter comparison Table of preparation method of high-strength boron nitride ceramics
TABLE 2 COMPARATIVE TABLE OF COMPARATIVE CHARACTERISTICS OF COMPENSATION AND SINGLE-AXIS COMPRESSION STRESS OF HIGH-STRENGTH BORON NITRIDE CERAMICS IN EXAMPLES 1-5
Claims (9)
1. A preparation method of high-strength boron nitride ceramics is characterized by comprising the following steps: the high-strength boron nitride ceramic is a nano polycrystalline block material with an outer layer of hexagonal boron nitride and a central layer still retaining a cubic boron nitride structure, and the preparation method comprises the following steps:
A) charging: weighing a certain mass of single-particle-size nano cubic boron nitride powder, prepressing and forming, and putting a prepressed blank after prepressing and forming into a sintering mold;
B) and (3) sintering: putting the pre-pressed blank in the step A) and a sintering mold into discharge plasma sintering equipment or hot-pressing sintering equipment for sintering, wherein the sintering pressure is 30-50 MPa;
C) discharging: and taking out the mold after the temperature in the equipment is cooled to room temperature, and demolding to obtain the high-strength boron nitride ceramic block.
2. The method of claim 1, wherein the method comprises the steps of: the sintering mould in the step A) is a graphite mould, and the prepressing blank and the graphite mould are separated by graphite paper.
3. The method of claim 1, wherein the method comprises the steps of: and B) performing pre-pressing forming in the step A) to form bidirectional applied pressure, wherein the pressure is 5-10 MPa.
4. The method of claim 1, wherein the method comprises the steps of: the grain diameter of the single-grain-diameter nano cubic boron nitride powder in the step A) is 10 nm-500 nm.
5. The method according to claim 1, wherein the sintering step in step B) is performed by applying a pre-pressure and evacuating to a vacuum degree higher than 1 × 10-1And applying sintering pressure after Pa, heating to the sintering temperature after the sintering pressure is stable, closing the heating program after high-temperature sintering and releasing pressure.
6. The method of claim 5, wherein the method comprises the following steps: the pre-pressure applied in the step B) is 5 MPa-10 MPa, the sintering temperature is 1400 ℃ to 2000 ℃, and the heat preservation time is 1 min-30 min.
7. The method of claim 1, wherein the method comprises the steps of: the sintering mode in the step B) is spark plasma sintering or hot-pressing sintering.
8. The method of claim 1, wherein the method comprises the steps of: the temperature rise rate of the step B) is 50-150 ℃/min.
9. The high-strength boron nitride ceramic prepared by the preparation method according to any one of claims 1 to 8, wherein: the compressive strength is not lower than 500MPa, and the compressive strain is not lower than 8%.
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