CN110698207A - Silicon nitride-based layered ceramic composite material and preparation method thereof - Google Patents

Silicon nitride-based layered ceramic composite material and preparation method thereof Download PDF

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CN110698207A
CN110698207A CN201911088241.5A CN201911088241A CN110698207A CN 110698207 A CN110698207 A CN 110698207A CN 201911088241 A CN201911088241 A CN 201911088241A CN 110698207 A CN110698207 A CN 110698207A
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silicon nitride
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陈威
王昭勋
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a silicon nitride-based layered ceramic composite material and a preparation method thereof, belonging to the field of ceramic materials2O3And Y2O3The mixture is a sintering aid, the ceramic powder is mixed, ground and sieved, the mixed powder and molybdenum powder are weighed in multiple parts, the mixture is placed into a metal die to be cold-pressed to form a biscuit, and the biscuit is sintered under the conditions of the nitrogen atmosphere, the temperature of 1750-1850 ℃ and the pressure of 25-35 MPa to obtain the silicon nitride-based layered ceramic composite material. So that the layered ceramic composite material based on silicon nitride not only retains higher hardness, but also has good toughness.

Description

Silicon nitride-based layered ceramic composite material and preparation method thereof
Technical Field
The invention relates to the field of ceramic materials, in particular to a silicon nitride-based layered ceramic composite material and a preparation method thereof.
Background
Silicon nitride material is an important structural ceramic material, has the properties of high hardness, low density, high temperature resistance and the like, and can be used for manufacturing mechanical structures such as bearings, turbine blades, mechanical seal rings, permanent molds and the like. However, practical applications of silicon nitride materials have been limited due to brittleness problems associated with ceramic materials. Therefore, it is necessary to provide a method capable of improving the toughness of the silicon nitride material to expand the application range of the silicon nitride material.
Disclosure of Invention
The invention aims to provide a silicon nitride-based layered ceramic composite material and a preparation method thereof, wherein the layered ceramic has a bionic structure similar to a shell layer of a pearl shell, and the fracture toughness of a ceramic material is improved to a great extent.
The invention is realized by the following technical scheme:
the preparation method of the silicon nitride-based layered ceramic composite material comprises the following steps:
step 1, weighing ceramic powder and molybdenum powder, wherein the ceramic powder comprises a main material and a sintering aid, the main material is a mixture of silicon nitride and hexagonal boron nitride or silicon nitride, the mass of the hexagonal boron nitride accounts for 0-20% of the mass of the ceramic powder, and the mass of the sintering aid accounts for 8% -12% of the mass of all the ceramic powder; wherein the mass of the molybdenum powder is 19-33% of that of the ceramic powder;
step 2, uniformly mixing the main materials weighed in the step 1 with the sintering aid to obtain a mixture;
step 3, grinding and sieving the mixture obtained in the step 2 to obtain mixed powder;
step 4, dividing the molybdenum powder weighed in the step 1 into N parts, and dividing the mixed powder obtained in the step 3 into N +1 parts;
step 5, paving the N parts of molybdenum powder and the N +1 parts of mixed powder obtained in the step 4 in a cold pressing mold in a staggered manner, performing cold pressing molding, and obtaining a biscuit after molding;
and 6, putting the biscuit obtained in the step 5 into a sintering mold, prepressing, and sintering in a nitrogen atmosphere to obtain the layered ceramic composite material.
Further, in the step 2, when the main material and the sintering aid are mixed, the weighed main material and the sintering aid are placed in a ball milling tank through ball milling and mixing, zirconium dioxide grinding balls are added, then alcohol is poured, the mixture is fully and uniformly mixed by a planetary ball mill, and the speed of the planetary ball mill is 50 r.min-1～150r·min-1The ball milling time is 5-6 h.
Further, in the step 2, the mass of the added zirconium dioxide grinding ball is 2 times of the mass of the ceramic powder, and the mass of the alcohol is 2 times of the mass of the ceramic powder.
Further, in step 6, graphite paper is laid in the sintering mold when the biscuit is loaded into the sintering mold.
Further, in step 1, the purity of silicon nitride is 99.99%, and alpha phase>94% with an average particle size of 0.3 μm in a volume fraction of 90%, 99.6% purity of hexagonal boron nitride, an average particle size of 0.5 μm, Al2O3And Y2O3Purity of>99.5%, and the average particle diameter was 1 μm.
Further, in step 1, Al2O3And Y2O3In the mixture sintering aid, Al2O3And Y2O3The mass ratio of (2:3) to (3: 2).
The invention provides a layered ceramic composite material based on silicon nitride, which is prepared based on the preparation method provided by the invention.
Furthermore, the silicon nitride-based layered ceramic composite material is of a layered structure and comprises molybdenum powder layers and ceramic powder layers which are arranged in a staggered mode, wherein the molybdenum powder layers are N layers, the ceramic powder layers are N +1 layers, and N is larger than or equal to 1.
Furthermore, the thickness ratio of the molybdenum powder layer to the ceramic powder layer is (1:14) - (1: 9).
The invention provides a layered ceramic composite material based on silicon nitride, which is prepared based on the preparation method provided by the invention.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a preparation method of a layered ceramic composite material based on silicon nitride, which is based on the principle that cracks can deflect, bend or branch in a layered structure, realizes the toughening of a ceramic material, simulates the structure of a shell layer of pearl oyster to prepare the silicon nitride layered ceramic material, obtains a biscuit by a method of layering and staggering powder paving of silicon nitride and molybdenum, and prepares the composite material with a bionic layered structure by hot-pressing sintering. The problem of sudden fracture of the silicon nitride material can be well overcome. The bionic layered structure can effectively improve the characteristics of single silicon nitride ceramic material such as high brittleness, low toughness and the like, and the preparation method is simple and easy to popularize.
The molybdenum has the characteristics of good high-temperature strength, high hardness, high density, strong corrosion resistance, small thermal expansion coefficient, good electric and thermal conductivity and the like. Molybdenum and silicon nitride can generate chemical reaction in the sintering process, and further silicon-molybdenum compounds with high hardness and high melting point are formed, so that the combination of the ceramic powder layer and the molybdenum layer is facilitated. Also, molybdenum can be oxidized to MoO at high temperatures3，MoO3Has certain lubricating property.
Further, in step 6, graphite paper is laid in the sintering mold when the biscuit is placed in the sintering mold, so that demolding of the prepared material is facilitated.
Further, in step 1, the purity of silicon nitride is 99.99%, and alpha phase>94% with an average particle size of 0.3 μm in a volume fraction of 90%, 99.6% purity of hexagonal boron nitride, an average particle size of 0.5 μm, Al2O3And Y2O3Purity of>99.5 percent, the average grain diameter is 1 mu m, and the alpha-phase silicon nitride is subjected to phase change conversion into a beta phase at high temperature, which is beneficial to improving the compactness of the material.
A layered ceramic composite material based on silicon nitride comprises a molybdenum powder layer and a ceramic powder layer which are arranged in a staggered mode, wherein the molybdenum powder layer is N layers, the ceramic powder layer is N +1 layers, and N is larger than or equal to 1. Based on the principle that cracks can deflect, bend or branch in a laminated structure, the toughening of the ceramic material is realized, the bionic laminated structure can effectively improve the characteristics of large brittleness, low toughness and the like of a single silicon nitride ceramic material, and the preparation method is simple and easy to popularize.
Drawings
FIG. 1 is a schematic view of a cold-pressed metal mold;
FIG. 2 is a schematic diagram of a sintered graphite mold configuration;
FIG. 3 is a schematic diagram of the sintering temperature variation of the hot pressing sintering process;
FIG. 4 is an XRD pattern of a layered ceramic composite material based on silicon nitride obtained in example 2;
FIG. 5 is a microscopic view of the fracture morphology of the layered silicon nitride-based ceramic composite obtained in example 2;
FIG. 6 is an XRD pattern of a layered ceramic composite material based on silicon nitride obtained in example 4;
FIG. 7 is a microscopic view of the fracture morphology of the layered ceramic composite based on silicon nitride obtained in example 4.
In the drawings: 1. the device comprises an upper pressure head, 2, powder, 3, a sleeve, 4, a lower pressure head, 5, an outer sleeve, 6, a base, 8, an upper die, 9, an inner lining, 10, a middle sleeve, 11 and a lower die.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
1) preparing materials: weighing 24.56g of silicon nitride and 2.72g of Al according to the mass ratio2O3And Y2O3And 8.25g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% with an average grain size of 0.3 μm and a volume fraction of 90%, a purity of 99.6% for hexagonal boron nitride, an average grain size of 0.5 μm, Al2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.63g, Y2O3It was 1.09 g.
2) Ball milling and mixing: weighing silicon nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, adjusting the fluid viscosity, and fully mixing by using a planetary ball mill at the speed of 50 r-min-1The ball milling time is 5 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
3) Drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
4) sieving: and grinding the mixture after evaporation to dryness, and sieving the mixture by using a 160-mesh sieve to obtain mixed powder.
5) Weighing powder: evenly dividing the mixed powder into 8 parts, wherein the mass of each part of the mixed powder is 3.41 g; the metal molybdenum powder was divided into 7 parts on average, and the mass of each part of the metal powder was 1.18 g.
6) Cold pressing and charging: the mixed powder and the molybdenum powder are sequentially paved into a cold-pressing die, the cold-pressing die is a metal die, and fig. 1 shows a structural schematic diagram of the metal die. The cold pressing die comprises an upper pressing head 1, a sleeve 3 and a lower pressing head 4, wherein the lower end of the upper pressing head 1 and the upper end of the lower pressing head 4 are arranged in the sleeve 3, and powder 2 is arranged between the upper pressing head 1 and the lower pressing head 4.
7) Cold press molding: and placing the cold pressing die filled with the powder in a QYL 50 jack refitting and pressurizing device for pressurizing, wherein the pressure is 30MPa, and the heat preservation and pressure maintaining time is 10min, so as to obtain a biscuit. And taking the formed biscuit out of the metal mold.
8) Hot-pressing and charging: stacking graphite paper with the thickness of 0.1mm on the periphery of a sintering mold to facilitate demolding, and putting the molded biscuit into the sintering mold for prepressing, wherein the sintering mold is a graphite mold, and fig. 2 is a structural schematic diagram of the graphite mold; the graphite mold comprises an upper mold 8, a lining cylinder 9, a middle sleeve 10, a lower mold 11, an outer sleeve 5 and a base 6, wherein the lining cylinder 9, the middle sleeve 10 and the outer sleeve 5 are coaxially installed from inside to outside, the lower mold 11 and the upper mold 8 are installed in the lining cylinder 9, the base 6 is located below the lower mold 11, and powder 2 is installed between the upper mold and the lower mold.
9) Hot-pressing and sintering: placing the sintering mold filled with the powder in a HIGH MULTI-stage 5000 sintering furnace, sintering after installation and debugging, wherein the temperature change of the hot-pressing sintering process is shown in figure 3: under the protection of nitrogen atmosphere, the temperature is 1800 ℃, the pressure is 30MPa, and the heat preservation and pressure maintaining time is 30 min. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain the first silicon nitride-based layered ceramic composite material.
The silicon nitride-based layered ceramic composite material is of a layered structure and comprises 7 molybdenum powder layers and 8 ceramic powder layers which are arranged in a staggered mode. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 9. See table 1 for vickers hardness and fracture toughness for the first silicon nitride based layered ceramic composite.
Example 2
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
step 1), batching: weighing 25.0g of silicon nitride and 2.77g of Al according to the mass ratio2O3And Y2O3A mixture sintering aid, and 6.87g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% with an average grain size of 0.3 μm and a volume fraction of 90%, a purity of 99.6% for hexagonal boron nitride, an average grain size of 0.5 μm, Al2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.66g, Y2O3It was 1.11 g.
Step 2) ball milling and mixing: weighing silicon nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, adjusting the fluid viscosity, and fully mixing by using a planetary ball mill at the speed of 100 r.min-1The ball milling time is 5.5 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
Step 3), drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
step 4) sieving: and grinding the dried mixture, and sieving the ground mixture by using a 130-mesh sieve to obtain mixed powder.
Step 5), weighing powder: evenly dividing the mixed powder into 8 parts, wherein the mass of each part of the mixed powder is 3.47 g; the metal molybdenum powder was divided into 7 parts on average, and the mass of each part of the metal powder was 0.98 g.
Step 6), cold pressing and charging: and spreading the mixed powder and the molybdenum powder into a metal die in sequence.
Step 7), cold press molding: and (3) placing the mould filled with the powder in a pressure device modified according to a QYL 50 jack for pressurization, wherein the pressure is 25MPa, and the heat preservation and pressure maintaining time is 10min, so as to obtain a biscuit. And taking the formed biscuit out of the metal mold.
Step 8) hot-pressing and charging: graphite paper with the thickness of 0.1mm is laid on the periphery of the die to facilitate demoulding, and the formed biscuit is put into the graphite die for prepressing.
Step 9), hot-pressing sintering: placing the mould filled with the powder in a HIGH MULTILTI 5000 multifunctional sintering furnace, sintering after installation and debugging, wherein the hot-pressing sintering process comprises the following steps: and (3) protecting in nitrogen atmosphere, keeping the temperature at 1750 ℃, the pressure at 35MPa and the heat preservation and pressure maintaining time for 30 min. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain a second silicon nitride-based layered ceramic composite material. The silicon nitride-based layered ceramic composite material prepared by the method is of a layered structure and comprises 7 molybdenum powder layers and 8 ceramic powder layers which are arranged in a staggered mode. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 11.
Referring to FIG. 4, for XRD analysis of a second silicon nitride-based layered ceramic composite (11SN0-Mo), the alpha phase silicon nitride has been completely converted to the beta phase. Referring to fig. 5, a microstructure of the fracture morphology of the second silicon nitride based layered ceramic composite, cracks are deflected between the layers. See table 1 for vickers hardness and fracture toughness for a second silicon nitride based layered ceramic composite.
Example 3
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
step 1), batching: 25.46g of silicon nitride and 2.83g of Al are weighed according to the mass ratio2O3And Y2O3A mixture sintering aid, and 5.47g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% with an average grain size of 0.3 μm and a volume fraction of 90%, a purity of 99.6% for hexagonal boron nitride, an average grain size of 0.5 μm, Al2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.13g, Y2O3It was 1.70 g.
Step 2) ball milling and mixing: weighing silicon nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, adjusting the fluid viscosity, and fully mixing uniformly by using a planetary ball mill at the speed of 150 r.min-1The ball milling time is 6 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
Step 3), drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
step 4) sieving: and grinding the dried mixture, and sieving the ground mixture by using a 100-mesh sieve to obtain mixed powder.
Step 5), weighing powder: evenly dividing the mixed powder into 8 parts, wherein the mass of each part of the mixed powder is 3.54 g; the metal molybdenum powder was divided into 7 parts on average, and the mass of each part of the metal powder was 0.78 g.
Step 6), cold pressing and charging: and spreading the mixed powder and the molybdenum powder into a metal die in sequence.
Step 7), cold press molding: and (3) placing the mould filled with the powder in a pressure device modified according to a QYL 50 jack for pressurization, wherein the pressure is 35MPa, and the heat preservation and pressure maintaining time is 5min, so as to obtain a biscuit. And taking the formed biscuit out of the metal mold.
Step 8) hot-pressing and charging: graphite paper with the thickness of 0.1mm is laid on the periphery of the die to facilitate demoulding, and the formed biscuit is put into the graphite die for prepressing.
Step 9), hot-pressing sintering: placing the mould filled with the powder in a HIGH MULTILTI 5000 multifunctional sintering furnace, sintering after installation and debugging, wherein the hot-pressing sintering process comprises the following steps: under the protection of nitrogen atmosphere, the temperature is 1850 ℃, the pressure is 25MPa, and the heat preservation and pressure maintaining time is 30 min. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain a third silicon nitride-based layered ceramic composite material.
The layered ceramic composite material based on silicon nitride prepared by the method consists of a ceramic material layer consisting of silicon nitride or silicon nitride and hexagonal boron nitride and a molybdenum layer. The molybdenum powder layers and the ceramic powder layers are arranged in a staggered mode, the molybdenum powder layers are 7, and the ceramic powder layers are 8. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 14.
Example 4
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
step 1), batching: weighing 17.6g of silicon nitride, 5.02g of hexagonal boron nitride and 2.52g of Al according to the mass ratio2O3And Y2O3A mixture sintering aid, and 8.25g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% with an average grain size of 0.3 μm and a volume fraction of 90%, a purity of 99.6% for hexagonal boron nitride, an average grain size of 0.5 μm, Al2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.51g of Y2O3It was 1.01 g.
Step 2) ball milling and mixing: weighing silicon nitride, boron nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, adjusting the fluid viscosity, and fully mixing by using a planetary ball mill at the speed of 50 r-min-1The ball milling time is 5 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
Step 3), drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
step 4) sieving: and grinding the dried mixture, and sieving the ground mixture by using a 160-mesh sieve to obtain mixed powder.
Step 5), weighing powder: evenly dividing the mixed powder into 8 parts, wherein the mass of each part of the mixed powder is 3.14 g; the metal molybdenum powder was divided into 7 parts on average, and the mass of each part of the metal powder was 1.18 g.
Step 6), cold pressing and charging: and spreading the mixed powder and the molybdenum powder into a metal die in sequence.
Step 7), cold press molding: and (3) placing the mould filled with the powder in a pressure device modified according to a QYL 50 jack for pressurizing, wherein the pressure is 30MPa, and the heat preservation and pressure maintaining time is 7.5min to obtain a biscuit. And taking the formed biscuit out of the metal mold.
Step 8) hot-pressing and charging: graphite paper with the thickness of 0.1mm is laid on the periphery of the die to facilitate demoulding, and the formed biscuit is put into the graphite die for prepressing.
Step 9), hot-pressing sintering: placing the mould filled with the powder into a HIGH MULTI-stage 5000 sintering furnace, sintering after installation and debugging, wherein the temperature change of the hot-pressing sintering process is shown in figure 3: under the protection of nitrogen atmosphere, the temperature is 1800 ℃, the pressure is 30MPa, and the heat preservation and pressure maintaining time is 30 min. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain a third silicon nitride-based layered ceramic composite material.
The layered ceramic composite material based on silicon nitride prepared by the method consists of a ceramic material layer consisting of silicon nitride or silicon nitride and hexagonal boron nitride and a molybdenum layer. The molybdenum powder layers and the ceramic powder layers are arranged in a staggered mode, the molybdenum powder layers are 7, and the ceramic powder layers are 8. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 9.
Referring to FIG. 6, for XRD analysis of a third silicon nitride-based layered ceramic composite (9SN20-Mo), the alpha phase silicon nitride had all been converted to the beta phase. Referring to fig. 7, a fracture morphology micrograph of a third silicon nitride-based layered ceramic composite was shown where cracks were deflected between layers. See table 1 for vickers hardness and fracture toughness for a fourth silicon nitride-based layered ceramic composite.
Example 5
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
step 1), batching: 20.98g of silicon nitride, 2.62g of hexagonal boron nitride and 2.62g of Al are weighed according to the mass ratio2O3And Y2O3A mixture sintering aid, and 8.25g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% with an average grain size of 0.3 μm and a volume fraction of 90%, a purity of 99.6% for hexagonal boron nitride, an average grain size of 0.5 μm, Al2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.31g, Y2O3It was 1.31 g.
Step 2) ball milling and mixing: weighing silicon nitride, boron nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, adjusting the fluid viscosity, and fully mixing by using a planetary ball mill at the speed of 100 r.min-1The ball milling time is 5.5 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
Step 3), drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
step 4) sieving: and grinding the dried mixture, and sieving the ground mixture by using a 160-mesh sieve to obtain mixed powder.
Step 5), weighing powder: evenly dividing the mixed powder into 8 parts, wherein the mass of each part of the mixed powder is 3.28 g; the metal molybdenum powder was divided into 7 parts on average, and the mass of each part of the metal powder was 1.18 g.
Step 6), cold pressing and charging: and spreading the mixed powder and the molybdenum powder into a metal die in sequence.
Step 7), cold press molding: and (3) placing the mould filled with the powder in a pressure device modified according to a QYL 50 jack for pressurizing, wherein the pressure is 30MPa, and the heat preservation and pressure maintaining time is 10min to obtain a biscuit. And taking the formed biscuit out of the metal mold.
Step 8) hot-pressing and charging: graphite paper with the thickness of 0.1mm is laid on the periphery of the die to facilitate demoulding, and the formed biscuit is put into the graphite die for prepressing.
Step 9), hot-pressing sintering: and placing the mold filled with the powder into a HIGH MULTILTI 5000 multifunctional sintering furnace, sintering after installation and debugging, and keeping the temperature at 1800 ℃, the pressure at 30MPa and the heat preservation and pressure maintaining time at 30min under the protection of nitrogen atmosphere. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain a fifth silicon nitride-based layered ceramic composite material.
The silicon nitride-based layered ceramic composite material prepared by the method is of a layered structure and comprises 7 molybdenum powder layers and 8 ceramic powder layers which are arranged in a staggered mode. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 9.
Example 6
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
step 1), batching: weighing 25.23g of silicon nitride and 2.80g of Al according to the mass ratio2O3And Y2O3A mixture sintering aid, and 5.94g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% of Al, having an average particle diameter of 0.3 μm and a volume fraction of 90%2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.68g, Y2O3It was 1.12 g.
Step 2) ball milling and mixing: weighing silicon nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, adjusting the fluid viscosity, and fully mixing uniformly by using a planetary ball mill at the speed of 150 r.min-1The ball milling time is 6 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
Step 3), drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
step 4) sieving: and grinding the dried mixture, and sieving the ground mixture by using a 160-mesh sieve to obtain mixed powder.
Step 5), weighing powder: averagely dividing the mixed powder into 4 parts, wherein the mass of each part of the mixed powder is 7 g; the metal molybdenum powder was divided into 3 parts on average, and the mass of each part of the metal powder was 1.98 g.
Step 6), cold pressing and charging: and spreading the mixed powder and the molybdenum powder into a metal die in sequence.
Step 7), cold press molding: and (3) placing the mould filled with the powder in a pressure device modified according to a QYL 50 jack for pressurizing, wherein the pressure is 30MPa, and the heat preservation and pressure maintaining time is 10min to obtain a biscuit. And taking the formed biscuit out of the metal mold.
Step 8) hot-pressing and charging: graphite paper with the thickness of 0.1mm is laid on the periphery of the die to facilitate demoulding, and the formed biscuit is put into the graphite die for prepressing.
Step 9), hot-pressing sintering: placing the mold filled with the powder in a HIGH MULTI-stage 5000 sintering furnace, sintering after installation and debugging, wherein the hot-pressing sintering process is shown in figure 3: under the protection of nitrogen atmosphere, the temperature is 1800 ℃, the pressure is 30MPa, and the heat preservation and pressure maintaining time is 30 min. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain a sixth silicon nitride-based layered ceramic composite material.
The silicon nitride-based layered ceramic composite material prepared by the method is of a layered structure and comprises 3 molybdenum powder layers and 4 ceramic powder layers which are arranged in a staggered mode. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 11.
Example 7
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
step 1), batching: weighing 25.02g of silicon nitride and 2.18g of Al according to the mass ratio2O3And Y2O3A mixture sintering aid, and 8.25g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% of Al, having an average particle diameter of 0.3 μm and a volume fraction of 90%2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.09g of Y2O3It was 1.09 g.
Step 2) ball milling and mixing: weighing silicon nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, and adjusting the viscosity of the fluid to ensure that the mixture sintering aid powder is mixed with the alcoholMixing with planetary ball mill at 150 r.min-1The ball milling time is 6 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
Step 3), drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
step 4) sieving: and grinding the dried mixture, and sieving the ground mixture by using a 160-mesh sieve to obtain mixed powder.
Step 5), weighing powder: evenly dividing the mixed powder into 8 parts, wherein the mass of each part of the mixed powder is 3.40 g; the metal molybdenum powder was divided into 7 parts on average, and the mass of each part of the metal powder was 1.18 g.
Step 6), cold pressing and charging: and spreading the mixed powder and the molybdenum powder into a metal die in sequence.
Step 7), cold press molding: and (3) placing the mould filled with the powder in a pressure device modified according to a QYL 50 jack for pressurizing, wherein the pressure is 30MPa, and the heat preservation and pressure maintaining time is 10min to obtain a biscuit. And taking the formed biscuit out of the metal mold.
Step 8) hot-pressing and charging: graphite paper with the thickness of 0.1mm is laid on the periphery of the die to facilitate demoulding, and the formed biscuit is put into the graphite die for prepressing.
Step 9), hot-pressing sintering: placing the mould filled with the powder into a HIGH MULTI-stage 5000 sintering furnace, sintering after installation and debugging, wherein the temperature change of the hot-pressing sintering process is shown in figure 3: under the protection of nitrogen atmosphere, the temperature is 1800 ℃, the pressure is 30MPa, and the heat preservation and pressure maintaining time is 30 min. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain a seventh silicon nitride-based layered ceramic composite material.
The silicon nitride-based layered ceramic composite material prepared by the method is of a layered structure and comprises 7 molybdenum powder layers and 8 ceramic powder layers which are arranged in a staggered mode. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 9.
Example 8
A preparation method of a layered ceramic composite material based on silicon nitride comprises the following steps:
step 1), batching: weighing 24.20g of silicon nitride and 3.30g of Al according to the mass ratio2O3And Y2O3A mixture sintering aid, and 8.25g of molybdenum powder. Wherein, the purity of the silicon nitride is 99.99 percent, and the alpha phase>94% of Al, having an average particle diameter of 0.3 μm and a volume fraction of 90%2O3And Y2O3Purity of>99.5% of Al having an average particle diameter of 1 μm2O31.65g of Y2O3It was 1.65 g.
Step 2) ball milling and mixing: weighing silicon nitride and Al2O3And Y2O3Placing the mixture sintering aid powder into a ball milling tank, adding zirconium dioxide pellets, pouring alcohol, adjusting the fluid viscosity, and fully mixing uniformly by using a planetary ball mill at the speed of 150 r.min-1The ball milling time is 6 h; wherein, the amount of the added zirconium dioxide balls is 2 times of the weight of the materials, and the amount of the added wine is 2 times of the weight of the materials.
Step 3), drying: putting the ball-milled powder into an oven, heating and evaporating to dryness, and stirring while evaporating until all alcohol is lost, and simultaneously preventing agglomeration;
step 4) sieving: and grinding the dried mixture, and sieving the ground mixture by using a 160-mesh sieve to obtain mixed powder.
Step 5), weighing powder: evenly dividing the mixed powder into 8 parts, wherein the mass of each part of the mixed powder is 3.44 g; the metal molybdenum powder was divided into 7 parts on average, and the mass of each part of the metal powder was 1.18 g.
Step 6), cold pressing and charging: and spreading the mixed powder and the molybdenum powder into a metal die in sequence.
Step 7), cold press molding: and (3) placing the mould filled with the powder in a pressure device modified according to a QYL 50 jack for pressurizing, wherein the pressure is 30MPa, and the heat preservation and pressure maintaining time is 10min to obtain a biscuit. And taking the formed biscuit out of the metal mold.
Step 8) hot-pressing and charging: graphite paper with the thickness of 0.1mm is laid on the periphery of the die to facilitate demoulding, and the formed biscuit is put into the graphite die for prepressing.
Step 9), hot-pressing sintering: placing the mould filled with the powder into a HIGH MULTI-stage 5000 sintering furnace, sintering after installation and debugging, wherein the temperature change of the hot-pressing sintering process is shown in figure 3: under the protection of nitrogen atmosphere, the temperature is 1800 ℃, the pressure is 30MPa, and the heat preservation and pressure maintaining time is 30 min. And (3) demolding, opening the furnace cover after the furnace temperature is reduced to room temperature, taking out the mold, taking out the sintered sample from the mold, and removing the graphite paper adhered to the sample to obtain the eighth silicon nitride-based layered ceramic composite material.
The silicon nitride-based layered ceramic composite material prepared by the method is of a layered structure and comprises 7 molybdenum powder layers and 8 ceramic powder layers which are arranged in a staggered mode. The thickness ratio of the molybdenum powder layer to the ceramic powder layer is 1: 9.
The vickers hardness tester is used for inspecting the hardness and the toughness of the silicon nitride-based layered ceramic composite materials with different layer structures, and when the table 1 shows different layer structures, the vickers hardness and the fracture toughness of the silicon nitride-based layered ceramic composite material provided by the embodiment of the invention are high. Referring to table 1, fig. 5 and fig. 7, the following conclusions can be drawn: the silicon nitride-based layered ceramic composite material prepared by the preparation method of the silicon nitride-based layered ceramic composite material provided by the invention has high toughness, and solves the problem that the silicon nitride material in the prior art is easy to break due to the brittleness of the ceramic body, so that the material fails, the service life of parts is influenced, and the high hardness of the ceramic material is reserved.
TABLE 1 Vickers hardness and fracture toughness of layered ceramic composites of different layer structures
The embodiments of the present invention are merely illustrative of the spirit of the present invention, and those skilled in the art can modify the described embodiments or substitute them with similar ones without departing from the spirit of the present invention.

Claims (9)

1. A preparation method of a layered ceramic composite material based on silicon nitride is characterized by comprising the following steps:
step 1, weighing ceramic powder and molybdenum powder, wherein the ceramic powder comprises a main material and a sintering aid, the main material is a mixture of silicon nitride and hexagonal boron nitride or silicon nitride, the mass of the hexagonal boron nitride accounts for 0-20% of the mass of the ceramic powder, and the mass of the sintering aid accounts for 8% -12% of the mass of all the ceramic powder; wherein the mass of the molybdenum powder is 19-33% of that of the ceramic powder;
step 2, uniformly mixing the main materials weighed in the step 1 with the sintering aid to obtain a mixture;
step 3, grinding and sieving the mixture obtained in the step 2 to obtain mixed powder;
step 4, dividing the molybdenum powder weighed in the step 1 into N parts, and dividing the mixed powder obtained in the step 3 into N +1 parts;
step 5, paving the N parts of molybdenum powder and the N +1 parts of mixed powder obtained in the step 4 in a cold pressing mold in a staggered manner, performing cold pressing molding, and obtaining a biscuit after molding;
and 6, putting the biscuit obtained in the step 5 into a sintering mold, prepressing, and sintering in a nitrogen atmosphere to obtain the layered ceramic composite material.
2. The method of claim 1, wherein the main material and the sintering aid are mixed in step 2 by ball milling, the weighed main material and sintering aid are placed in a ball milling pot, zirconium dioxide grinding balls are added, alcohol is added, and the mixture is fully mixed by a planetary ball mill at a speed of 50 r.min-1～150r·min-1The ball milling time is 5-6 h.
3. The method of claim 2, wherein in step 2, the added zirconia grinding balls have a mass 2 times that of the ceramic powder, and the alcohol has a mass 2 times that of the ceramic powder.
4. The method for preparing a layered silicon nitride-based ceramic composite material according to claim 1, wherein in step 6, graphite paper is laid in the sintering mold while the green body is loaded in the sintering mold.
5. The method of claim 1, wherein in step 1, the purity of the silicon nitride is 99.99%, and the alpha phase is>94% with an average particle size of 0.3 μm in a volume fraction of 90%, 99.6% purity of hexagonal boron nitride, an average particle size of 0.5 μm, Al2O3And Y2O3Purity of>99.5%, and the average particle diameter was 1 μm.
6. The method of claim 1, wherein Al is added in step 12O3And Y2O3In the mixture sintering aid, Al2O3And Y2O3The mass ratio of (2:3) to (3: 2).
7. A layered ceramic composite material based on silicon nitride, characterized in that it is prepared based on the preparation method according to any one of claims 1 to 6.
8. The layered silicon nitride-based ceramic composite material as claimed in claim 7, wherein the layered silicon nitride-based ceramic composite material has a layered structure comprising a molybdenum powder layer and a ceramic powder layer which are arranged in a staggered manner, wherein the molybdenum powder layer is N layers, the ceramic powder layer is N +1 layers, and N is greater than or equal to 1.
9. The layered silicon nitride-based ceramic composite material according to claim 7, wherein the thickness ratio of the molybdenum powder layer to the ceramic powder layer is (1:14) - (1: 9).
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