CN116553937A - Silicon nitride composite ceramic material for sealing ring and preparation method thereof - Google Patents
Silicon nitride composite ceramic material for sealing ring and preparation method thereof Download PDFInfo
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- CN116553937A CN116553937A CN202310268289.4A CN202310268289A CN116553937A CN 116553937 A CN116553937 A CN 116553937A CN 202310268289 A CN202310268289 A CN 202310268289A CN 116553937 A CN116553937 A CN 116553937A
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- silicon nitride
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- nitride composite
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 69
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000007789 sealing Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 41
- 239000000853 adhesive Substances 0.000 claims abstract description 5
- 230000001070 adhesive effect Effects 0.000 claims abstract description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 18
- 239000010452 phosphate Substances 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000498 ball milling Methods 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 13
- 239000000945 filler Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000011268 mixed slurry Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229910000151 chromium(III) phosphate Inorganic materials 0.000 claims description 7
- IKZBVTPSNGOVRJ-UHFFFAOYSA-K chromium(iii) phosphate Chemical compound [Cr+3].[O-]P([O-])([O-])=O IKZBVTPSNGOVRJ-UHFFFAOYSA-K 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 230000000737 periodic effect Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 claims description 2
- 239000004137 magnesium phosphate Substances 0.000 claims description 2
- 229960002261 magnesium phosphate Drugs 0.000 claims description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 claims description 2
- 235000010994 magnesium phosphates Nutrition 0.000 claims description 2
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 2
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 13
- 230000035939 shock Effects 0.000 abstract description 11
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 4
- 238000005452 bending Methods 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 2
- 229910052582 BN Inorganic materials 0.000 description 19
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 19
- 239000000843 powder Substances 0.000 description 18
- 239000002245 particle Substances 0.000 description 14
- 239000000395 magnesium oxide Substances 0.000 description 11
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 11
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 11
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 10
- 229910000423 chromium oxide Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000009768 microwave sintering Methods 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000007542 hardness measurement Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/6306—Binders based on phosphoric acids or phosphates
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- C04B35/634—Polymers
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- C04B35/64—Burning or sintering processes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract
The invention provides a silicon nitride composite ceramic material for a sealing ring, which comprises, by weight, 60-80 parts of silicon nitride and Ti 3 C 2 3-5 parts, M X O Y 8-15 parts of adhesive and 2-6 parts of binder. The silicon nitride composite ceramic material prepared by the invention has small pore, high density and volume density of more than 3.2g/cm 2 . Has higher heat conductivity coefficient and smaller linear expansion coefficient, and is not cracked when bearing thermal shock. As a means ofWhen the sealing ring material is used, the sealing ring material has enough strength, rigidity and corrosion resistance, small deformation during use and can still maintain the tightness when the working condition fluctuates; high bending strength, excellent thermal shock resistance and better toughness, the plastic is not deformed under the working condition of high temperature and high pressure, and has long service life.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a silicon nitride composite ceramic material for a sealing ring and a preparation method thereof.
Background
The sealing ring is the most main element for forming the mechanical seal, the service performance and the service life of the mechanical seal are determined to a great extent, the sealing performance directly influences the working performance and the quality of the whole system, and the system function is reduced due to poor sealing. In many sealing forms, various sealing elements using rubber as raw materials have a large proportion in practical engineering, but the sealing performance of the rubber sealing element is difficult to be satisfactory under the working conditions of high temperature, low temperature, large temperature difference, corrosive medium, long service life and the like due to the inherent characteristics of the rubber sealing element. The ceramic sealing ring has the characteristics of wear resistance, good sealing performance, high temperature resistance and convenient replacement, and the service life of the ceramic sealing ring is prolonged greatly compared with that of a common rubber sealing ring. Chinese patent No. CN 107353009A discloses a method for preparing multiphase toughened silicon carbide ceramic comprising graphene, which comprises ball milling silicon carbide, alumina, carbon black, graphene powder and PVA in water to obtain slurry, press molding in a mold, drying, and reactive sintering to obtain the final product.
The ceramic material used for the sealing ring is required to have enough strength and rigidity, small deformation in use, enough strength and corrosion resistance and long service life. And has good thermal shock resistance, higher thermal conductivity coefficient and smaller linear expansion coefficient, and does not crack when bearing thermal shock.
Disclosure of Invention
Aiming at the problems, the invention provides a silicon nitride composite ceramic material for a sealing ring, and the prepared silicon nitride composite ceramic material has small pores, high density and volume density of more than 3.2g/cm 2 . When used as a sealing ring material, the sealing ring has enough strength, rigidity and corrosion resistance, small deformation in use and sealing performance when working conditions fluctuate; high bending strengthAnd simultaneously has excellent thermal shock resistance and better toughness, does not deform under the working condition of high temperature and high pressure, and has long service life.
The invention provides a silicon nitride composite ceramic material for a sealing ring, which comprises, by weight, 60-80 parts of silicon nitride and Ti 3 C 2 3-5 parts, M X O Y 8-15 parts of adhesive and 2-6 parts of binder.
Preferably, the silicon nitride is a silicon nitride having a particle diameter D50 of 100nm to 1.0 μm and 1nm to 100 nm.
Further preferably, the mass ratio of the silicon nitride having the particle diameter D50 of 100nm to 1.0 μm to the silicon nitride having the particle diameter D50 of 1nm to 100nm is 7 to 9:1.
Preferably, the Ti is 3 C 2 The particle size D50 of (2) is less than 0.5 μm.
In order to further enhance the hardness and wear resistance of the ceramic material, 3-5 parts of Ti is added in the invention 3 C 2 . However, the inventors found in experiments that if Ti 3 C 2 Excessive addition content can lead the silicon nitride to be in line with the high density of the ceramic material and influence the corrosion resistance of the ceramic material.
Preferably, said M X O Y Wherein M is one of the second periodic metal element and the third periodic metal element, X is more than or equal to 1 and less than or equal to 4, and Y is more than or equal to 1 and less than or equal to 4; preferably, M is at least one of magnesium, aluminum and chromium.
The M is X O Y Includes MO neutralization M 2 O 3 In (a) and (b); MO neutralization M 2 O 3 The mass ratio of (3-5) to (5-8);
preferably, said M X O Y Magnesium oxide and chromium oxide.
Further preferably, the mass ratio of the magnesium oxide to the chromium oxide is 3-5:5-8.
Further preferably, the chromia has a particle size D50 of less than 1 μm.
The silicon nitride composite ceramic material also comprises 3-10 parts of filler;
preferably, the filler is one or more of boron nitride, silicon oxide, silicon carbide and mica.
Preferably, the filler is boron nitride.
Further preferably, the boron nitride is a flaky boron nitride powder.
Further preferably, the thickness of the boron nitride powder is 0.1-0.2 micrometers, and the length and width are 10-20 micrometers.
According to the invention, when the magnesium oxide and the chromium oxide with the mass ratio of 3-5:5-8 are used, the boron nitride with the thickness of 0.1-0.2 microns and the length and width of 10-20 microns is used as the filler, and the boron nitride is matched with PVA and a phosphate inorganic binder for use together, the prepared silicon nitride ceramic material has small pores, high density, higher heat conductivity coefficient, smaller heat expansion coefficient, excellent thermal shock resistance, better toughness and small deformation during use.
The inventors found in experiments that by adding M X O Y The sintering densification of the ceramic material can be effectively promoted. When PVA and phosphate inorganic binder are used together, the prepared silicon nitride composite ceramic material has more excellent high-temperature resistance and smaller thermal expansion coefficient. The inventors analyzed, probably due to the PVA co-operating phosphate inorganic binder, that has less cure shrinkage and water resistance. The inventor finds that when the magnesium oxide and the chromium oxide are used in the mass ratio of 3-5:5-8, the normal-temperature cohesiveness can be effectively enhanced without affecting the high-temperature cohesiveness, and the shrinkage rate of the ceramic material in sintering can be further reduced. The analysis is probably due to the fact that the used chromium ions can promote the formation of an amorphous structure, the disorder degree of the system is increased, the stress generated by the chromium phosphate system in the phase change process is reduced, and the stability of the binder is greatly improved. The specific boron nitride is used as the filler, so that the linear expansion coefficient of the adhesive is consistent with that of the adhered base material, and the adhered piece is ensured not to generate excessive thermal stress to cause adhesion failure when being used under high-temperature conditions. Meanwhile, the flaky boron nitride material can be combined with chromium oxide and magnesium oxide to enhance the uniform dispersion of the flaky boron nitride material in a system, so that the compactness of the material is further improved, and the thermal shock resistance, the strength and the toughness of the silicon nitride ceramic composite material are enhanced.
Preferably, the binder is one or more of PVA or phosphate inorganic binders.
Preferably, the binder is a PVA and phosphate inorganic binder.
Further preferably, the mass ratio of PVA to phosphate inorganic binder is 3-5:1.
Preferably, the phosphate inorganic binder is one or more of aluminum phosphate, magnesium phosphate, chromium phosphate and zirconium phosphate.
Further preferably, the phosphate inorganic binder is chromium phosphate.
The second aspect of the invention provides a preparation method of a silicon nitride composite ceramic material for a sealing ring, which comprises the following specific steps:
s1, mixing: dissolving raw materials except a binder in ethanol, performing ball milling, and drying slurry obtained by ball milling to obtain a mixture;
s2, forming: dissolving the mixture and the binder in ethanol, mixing, and stirring to obtain mixed slurry; injecting the mixed slurry into a mold, airing and demolding to obtain
To a green ceramic material;
s3, sintering: and (3) placing the green body to be sintered into a sintering furnace, heating to 1500-2000 ℃, preserving heat for 3-5h, and cooling to obtain the ceramic material.
Preferably, in the step S1, the ball milling speed is 2000-2500r/min, the ball milling time is 1-5h, and the ball milling medium is silicon nitride pellets with the diameter of 0.6-0.8 mm.
Preferably, the sintering step in the step S3 specifically includes: placing the molded blank into a sintering furnace, and performing microwave sintering in a microwave sintering device under a protective atmosphere, wherein the frequency range of microwaves is 2.45GHz, the temperature of microwave sintering is firstly increased to 300-350 ℃, the temperature is kept for 2-3h, and the heating rate is 80 ℃/h; heating to 1500-2000 deg.C, maintaining for 3-5h at 150 deg.C/h and 2-4MPa; naturally cooling to obtain the finished silicon nitride composite ceramic.
Compared with the prior art, the invention has the following beneficial effects:
the silicon nitride composite ceramic material prepared by the invention has small pore space, high density and volume density3.2g/cm 2 . Has higher heat conductivity coefficient and smaller linear expansion coefficient, and is not cracked when bearing thermal shock. When used as a sealing ring material, the sealing ring has enough strength, rigidity and corrosion resistance, small deformation in use and sealing performance when working conditions fluctuate; high bending strength, excellent thermal shock resistance and better toughness, the plastic is not deformed under the working condition of high temperature and high pressure, and has long service life.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be noted that the following examples are further illustrative of the present invention and are not intended to be limiting.
Examples
Example 1
In one aspect, the embodiment provides a silicon nitride composite ceramic material for a sealing ring, wherein the silicon nitride composite ceramic material comprises, by weight, 70 parts of silicon nitride and 70 parts of Ti 3 C 2 4 parts, M X O Y 12 parts of filler 7 parts and 3.5 parts of binder.
The silicon nitride is silicon nitride with the particle size D50 of 300nm and 50nm, and the mass ratio of the silicon nitride with the particle size D50 of 300nm and 50nm is 8:1, and is purchased from the company of Fosman technology (Beijing).
Ti 3 C 2 The particle diameter D50 of the powder is less than 0.5 mu m, and the powder is purchased from metal materials Co., ltd.
M X O Y The magnesium oxide and the chromium oxide with the mass ratio of 4:7 have the granularity D50 of less than 1 mu m and are purchased from Beijing Gaokang new material science and technology Co.
The filler is flaky boron nitride powder, the thickness of the boron nitride powder is 0.1-0.2 microns, the length and width are 10-20 microns, and the boron nitride powder is purchased from the macro metal materials limited company in Qinghai county.
The binder is PVA and phosphate inorganic binder with the mass ratio of 4:1; PVA is PVA17-92, purchased from Shandong Xin Heng chemical Co., ltd; the phosphate inorganic binder is chromium phosphate.
The second aspect of the embodiment provides a preparation method of a silicon nitride composite ceramic material for a sealing ring, which comprises the following specific steps:
s1, mixing: dissolving raw materials except a binder in ethanol, performing ball milling for 3 hours at a ball milling rate of 2300r/min, wherein a ball milling medium is silicon nitride pellets with a diameter of 0.6-0.8mm, and drying slurry obtained by ball milling to obtain a mixture;
s2, forming: dissolving the mixture and the binder in ethanol, mixing, and stirring to obtain mixed slurry; injecting the mixed slurry into a mold, airing and demolding to obtain a ceramic material green body;
s3, sintering: placing the molded blank into a sintering furnace, and performing microwave sintering in a microwave sintering device under a protective atmosphere, wherein the frequency range of microwaves is 2.45GHz, the temperature of the microwave sintering is firstly increased to 330 ℃, the temperature is kept for 2 hours, and the heating rate is 80 ℃/h; heating to 1800 ℃, preserving heat for 4 hours, wherein the heating rate is 150 ℃/h, and the pressure is 3MPa; naturally cooling to obtain the finished silicon nitride composite ceramic.
Example 2
In one aspect, the embodiment provides a silicon nitride composite ceramic material for a sealing ring, wherein the silicon nitride composite ceramic material comprises, by weight, 60 parts of silicon nitride and 60 parts of Ti 3 C 2 3 parts, M X O Y 8 parts of filler, 3 parts of binder and 3 parts of adhesive.
The silicon nitride is silicon nitride with the particle size D50 of 300nm and 50nm, and the mass ratio of the silicon nitride with the particle size D50 of 300nm and 50nm is 8:1, and is purchased from the company of Fosman technology (Beijing).
Ti 3 C 2 The particle diameter D50 of the powder is less than 0.5 mu m, and the powder is purchased from metal materials Co., ltd.
M X O Y The magnesium oxide and the chromium oxide with the mass ratio of 4:7 have the granularity D50 of less than 1 mu m and are purchased from Beijing Gaokang new material science and technology Co.
The filler is flaky boron nitride powder, the thickness of the boron nitride powder is 0.1-0.2 microns, the length and width are 10-20 microns, and the boron nitride powder is purchased from the macro metal materials limited company in Qinghai county.
The binder is PVA and phosphate inorganic binder with the mass ratio of 4:1; PVA is PVA17-92, purchased from Shandong Xin Heng chemical Co., ltd; the phosphate inorganic binder is chromium phosphate.
In a second aspect of this embodiment, a method for preparing a silicon nitride composite ceramic material for a seal ring is provided, and the specific steps are the same as in embodiment 1.
Example 3
In one aspect, the embodiment provides a silicon nitride composite ceramic material for a sealing ring, wherein the silicon nitride composite ceramic material comprises, by weight, 80 parts of silicon nitride and 80 parts of Ti 3 C 2 5 parts, M X O Y 15 parts of filler 10 parts and 6 parts of binder.
The silicon nitride is silicon nitride with the particle size D50 of 300nm and 50nm, and the mass ratio of the silicon nitride with the particle size D50 of 300nm and 50nm is 8:1, and is purchased from the company of Fosman technology (Beijing).
Ti 3 C 2 The particle diameter D50 of the powder is less than 0.5 mu m, and the powder is purchased from metal materials Co., ltd.
M X O Y The magnesium oxide and the chromium oxide with the mass ratio of 4:7 have the granularity D50 of less than 1 mu m and are purchased from Beijing Gaokang new material science and technology Co.
The filler is flaky boron nitride powder, the thickness of the boron nitride powder is 0.1-0.2 microns, the length and width are 10-20 microns, and the boron nitride powder is purchased from the macro metal materials limited company in Qinghai county.
The binder is PVA and phosphate inorganic binder with the mass ratio of 4:1; PVA is PVA17-92, purchased from Shandong Xin Heng chemical Co., ltd; the phosphate inorganic binder is chromium phosphate.
In a second aspect of this embodiment, a method for preparing a silicon nitride composite ceramic material for a seal ring is provided, and the specific steps are the same as in embodiment 1.
Example 4
In one aspect, the present embodiment provides a silicon nitride composite ceramic material for a seal ring, where the specific embodiment is the same as example 1, and the difference between the embodiment 1 is M X O Y Magnesium oxide and chromium oxide in a mass ratio of 3:5.
In a second aspect of this embodiment, a method for preparing a silicon nitride composite ceramic material for a seal ring is provided, and the specific steps are the same as in embodiment 1.
Comparative example 1
In one aspect, the present embodiment provides a silicon nitride composite ceramic material for a seal ring, where the specific embodiment is the same as example 1, and the difference between the embodiment 1 is M X O Y Is magnesium oxide.
In a second aspect of this embodiment, a method for preparing a silicon nitride composite ceramic material for a seal ring is provided, and the specific steps are the same as in embodiment 1.
Comparative example 2
In one aspect, the present embodiment provides a silicon nitride composite ceramic material for a seal ring, where the specific embodiment is the same as example 1, and the difference between the embodiment 1 is M X O Y Magnesium oxide and chromium oxide in a mass ratio of 4:1.
In a second aspect of this embodiment, a method for preparing a silicon nitride composite ceramic material for a seal ring is provided, and the specific steps are the same as in embodiment 1.
Comparative example 3
In one aspect, the present embodiment provides a silicon nitride composite ceramic material for a seal ring, and the specific embodiment is the same as embodiment 1, and differs from embodiment 1 in that the binder is PVA.
In a second aspect of this embodiment, a method for preparing a silicon nitride composite ceramic material for a seal ring is provided, and the specific steps are the same as in embodiment 1.
Comparative example 4
In one aspect, the present embodiment provides a silicon nitride composite ceramic material for a seal ring, and a specific embodiment is the same as that of embodiment 1.
The second aspect of the embodiment provides a preparation method of a silicon nitride composite ceramic material for a sealing ring, which comprises the following specific steps:
s1, mixing: dissolving raw materials except a binder in ethanol, performing ball milling for 3 hours at a ball milling rate of 2300r/min, wherein a ball milling medium is silicon nitride pellets with a diameter of 0.6-0.8mm, and drying slurry obtained by ball milling to obtain a mixture;
s2, forming: dissolving the mixture and the binder in ethanol, mixing, and stirring to obtain mixed slurry; injecting the mixed slurry into a mold, airing and demolding to obtain a ceramic material green body;
s3, sintering: placing the molded blank into a sintering furnace, and performing microwave sintering in a microwave sintering device under a protective atmosphere, wherein the frequency range of microwaves is 2.45GHz, the temperature of microwave sintering is raised to 1800 ℃, the temperature is kept for 4 hours, the heating rate is 150 ℃/h, and the pressure is 3MPa; naturally cooling to obtain the finished silicon nitride composite ceramic.
Performance testing
1. Volumetric density testing: the bulk density was tested according to the national standard "ceramic body apparent porosity, bulk Density test method (QB/T1642-2012)".
2. Flexural strength: the test was carried out according to the GB/T6569-86 test method.
3. Thermal shock resistance: heating a sample to 1200 ℃ and preserving heat for 10 minutes, then immersing the sample into water at 20 ℃ rapidly (less than 2 seconds), circulating for 20 times, observing whether cracking and other phenomena occur on the surface of the material, and if no change occurs, marking the material as qualified; if a cracking phenomenon such as a crack occurs, the test piece is judged as being unqualified.
4. Hardness testing: hardness testing was performed using a vickers hardness tester.
The silicon carbide composite ceramic materials of examples 1 to 4 and comparative examples 1 to 4 were subjected to the above performance test, and the test results are shown in table 1 below.
TABLE 1
| Examples | Flexural Strength/MPa | Thermal shock resistance | Hardness (GPa) |
| Example 1 | 987 | Qualified product | 19.6 |
| Example 2 | 969 | Qualified product | 18.8 |
| Example 3 | 982 | Qualified product | 19.1 |
| Example 4 | 973 | Qualified product | 19.4 |
| Comparative example 1 | 886 | Failure to pass | 17.1 |
| Comparative example 2 | 893 | Failure to pass | 17.5 |
| Comparative example 3 | 914 | Failure to pass | 16.6 |
| Comparative example 4 | 931 | Failure to pass | 16.1 |
Claims (10)
1. A silicon nitride composite ceramic material for a sealing ring is characterized by comprising, by weight, 60-80 parts of silicon nitride and 60-80 parts of Ti 3 C 2 3-5 parts, M X O Y 8-15 parts of adhesive and 2-6 parts of binder, wherein: m is one of the second periodic metal element and the third periodic metal element, X is more than or equal to 1 and less than or equal to 4, and Y is more than or equal to 1 and less than or equal to 4.
2. The silicon nitride composite ceramic material for a seal ring according to claim 1, wherein M is at least one of magnesium, aluminum, and chromium.
3. A silicon nitride composite ceramic material for a seal ring according to claim 2, wherein said M X O Y Wherein X is more than or equal to 1 and less than or equal to 2, Y is more than or equal to 1 and less than or equal to 3.
4. A silicon nitride composite ceramic material for a seal ring according to claim 3, wherein said M X O Y Includes MO neutralization M 2 O 3 In (a) and (b); MO neutralization M 2 O 3 The mass ratio of (3-5) to (5-8).
5. A silicon nitride composite ceramic material for a seal ring according to claim 1, further comprising 3-10 parts of filler.
6. A silicon nitride composite ceramic material for a seal ring according to claim 1, wherein the binder is one or a mixture of PVA or phosphate inorganic binders.
7. A silicon nitride composite ceramic material for a seal ring according to claim 6, wherein said binder is PVA and phosphate inorganic binder.
8. A silicon nitride composite ceramic material for a seal ring according to claim 7, wherein the mass ratio of PVA to phosphate inorganic binder is 3-5:1.
9. The silicon nitride composite ceramic material for a seal ring according to claim 8, wherein the phosphate inorganic binder is one or more of aluminum phosphate, magnesium phosphate, chromium phosphate, zirconium phosphate.
10. A method for preparing a silicon nitride composite ceramic material for a seal ring according to any one of claims 1 to 9, characterized by the specific steps of:
s1, mixing: dissolving raw materials except a binder in ethanol, performing ball milling, and drying slurry obtained by ball milling to obtain a mixture;
s2, forming: dissolving the mixture and the binder in ethanol, mixing, and stirring to obtain mixed slurry; injecting the mixed slurry into a mold, airing and demolding to obtain a ceramic material green body;
s3, sintering: and (3) placing the green body to be sintered into a sintering furnace, heating to 1500-2000 ℃, preserving heat for 3-5h, and cooling to obtain the ceramic material.
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