CN116120073B - Silicon nitride ceramic cutter and preparation method thereof - Google Patents
Silicon nitride ceramic cutter and preparation method thereof Download PDFInfo
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- CN116120073B CN116120073B CN202211710960.8A CN202211710960A CN116120073B CN 116120073 B CN116120073 B CN 116120073B CN 202211710960 A CN202211710960 A CN 202211710960A CN 116120073 B CN116120073 B CN 116120073B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 85
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 63
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 50
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 claims abstract description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 18
- 229910000077 silane Inorganic materials 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 16
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 16
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 16
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 14
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 10
- 230000000996 additive effect Effects 0.000 claims abstract description 10
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims abstract description 10
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 229910000085 borane Inorganic materials 0.000 claims abstract description 5
- 238000007740 vapor deposition Methods 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 45
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 19
- 239000008187 granular material Substances 0.000 claims description 18
- 238000001513 hot isostatic pressing Methods 0.000 claims description 18
- 238000003825 pressing Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000005299 abrasion Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 9
- 230000001070 adhesive effect Effects 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 9
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 8
- 239000001488 sodium phosphate Substances 0.000 claims description 8
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 8
- 238000005452 bending Methods 0.000 abstract description 6
- 238000005469 granulation Methods 0.000 abstract description 3
- 230000003179 granulation Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 13
- 238000012360 testing method Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 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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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
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Abstract
The application discloses a silicon nitride ceramic cutter and a preparation method thereof, and relates to the technical field of ceramic cutters. When the silicon nitride ceramic cutter is used, silicon nitride, titanium nitride, aluminum oxide and zirconium oxide are used as raw materials, self-made wear-resistant auxiliary agents are added for granulation, then sintering is carried out to obtain a ceramic cutter matrix, and finally processing treatment is carried out on the surface of the matrix to obtain the wear-resistant high-strength silicon nitride ceramic cutter; the self-made wear-resistant additive is prepared by generating lithium aluminate crystals on the surfaces of lanthanum hexaboride and yttrium oxide, so that the bending strength and wear resistance of a cutter matrix are enhanced; when the surface of the cutter matrix is processed, micro-arc oxidation treatment is carried out first, and then plasma vapor deposition is carried out under the atmosphere of nitrogen, borane and silane, so that the wear resistance and the bending strength of the cutter are further enhanced.
Description
Technical Field
The application relates to the technical field of ceramic cutter preparation, in particular to a silicon nitride ceramic cutter and a preparation method thereof.
Background
Silicon nitride ceramics have been widely used in cutting tools, bearings, high-pressure plungers, seal rings, wear-resistant elements, and the like because of their excellent high temperature resistance, wear resistance, corrosion resistance, high hardness, and the like. When the silicon nitride ceramic is used as a cutter material for cutter preparation, the friction factor of the silicon nitride ceramic is low, so that the silicon nitride ceramic is suitable for cutting cutters with large feeding amount or intermittent cutting of cast iron, high-temperature alloy, nickel-based alloy and the like, but in the high-speed cutting process, the chemical stability of the silicon nitride ceramic cutter is reduced, the surface of the silicon nitride ceramic cutter is worn, and even severe crater wear is generated; therefore, the application researches and prepares the silicon nitride ceramic cutter with high strength, wear resistance.
Disclosure of Invention
The application aims to provide a silicon nitride ceramic cutter and a preparation method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the application provides the following technical scheme: a silicon nitride ceramic cutter is prepared by processing the surface of a ceramic cutter matrix.
Preferably, the ceramic cutter matrix is prepared by mixing raw materials with self-made wear-resistant auxiliary agents, granulating, and sintering.
Preferably, the raw materials include silicon nitride, titanium nitride, aluminum oxide, and zirconium oxide.
Preferably, the self-made wear-resistant auxiliary agent is prepared by generating lithium aluminate crystals on the surfaces of lanthanum hexaboride and yttrium oxide.
Preferably, the processing treatment is to perform micro-arc oxidation treatment on the ceramic cutter matrix, and then perform plasma vapor deposition in nitrogen, borane and silane atmosphere.
Preferably, the preparation method of the silicon nitride ceramic cutter comprises the following specific steps:
(1) Mixing lanthanum hexaboride, yttrium oxide, lithium carbonate and aluminum oxide, performing ball milling, wherein the ball milling medium is absolute ethyl alcohol, the ball material ratio is 9:1, performing ball milling for 50-80 min, drying, sieving with a 80-100 mesh sieve, transferring into a sintering furnace, heating to 900-1000 ℃, and sintering for 2-4 h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to the mass ratio of 80:3:9:2:3-100:5:15:4:5, ball milling in a ball mill, ball milling for 8-12 hours at the ball material ratio of 9:1, transferring to a calciner, calcining for 30-50 minutes at 800-900 ℃, adding an adhesive with the mass of 0.01-0.03 times of that of the silicon nitride, granulating, preparing granules, and finally performing dry pressing and hot isostatic pressing treatment to prepare a ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic knife matrix;
(4) Transferring the ceramic cutter matrix subjected to micro-arc oxidation treatment between positive and negative electrodes in a vacuum furnace, heating to 280-350 ℃ in the atmosphere of diborane, silane and nitrogen, electrifying for 20-50 min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
Preferably, in the step (1): the mass ratio of lanthanum hexaboride to yttrium oxide to lithium carbonate to aluminum oxide is 1:1:0.4:0.4-1:1.2:0.6:0.6.
Preferably, in the step (2): in the dry pressing process, the granules are dry pressed for 20 to 40 minutes under the pressure of 60 to 80 MPa; the temperature is 1000-1200 deg.c and the pressure is 150-180 MPa during hot isostatic pressing.
Preferably, in the step (3): when in micro-arc oxidation treatment, a ceramic cutter matrix is taken as an anode, a stainless steel electrolytic tank is taken as a cathode, the pulse voltage is 450-500V, the negative pulse voltage is 100-150V, the pulse frequency is 400-500 Hz, and the duty ratio is 25-35%; the electrolyte comprises the following components: 12-14 g/L of sodium aluminate, 6-10 g/L of sodium phosphate, 0.04-0.08 mol/L of glycerol and 1-4 g/L of silicon carbide.
Preferably, in the step (4): in the mixed gas of diborane, silane and nitrogen, the volume ratio of diborane, silane and nitrogen is 1:1:8-2:1:10.
Compared with the prior art, the application has the following beneficial effects:
when the silicon nitride ceramic cutter is used, silicon nitride, titanium nitride, aluminum oxide and zirconium oxide are used as raw materials, self-made wear-resistant auxiliary agents are added for granulation, then sintering is carried out to obtain a ceramic cutter matrix, and finally processing treatment is carried out on the surface of the matrix to obtain the wear-resistant high-strength silicon nitride ceramic cutter;
the self-made wear-resistant auxiliary agent is a ternary sintering auxiliary agent prepared by mixing lanthanum hexaboride, yttrium oxide and lithium aluminate crystals, lithium aluminate crystals are generated on the surfaces of the lanthanum hexaboride and the yttrium oxide, the self-made wear-resistant auxiliary agent in an irregular shape is formed by connecting the lithium aluminate crystals, after the self-made wear-resistant agent is mixed with silicon nitride, titanium nitride, aluminum oxide and zirconium oxide, part of particles enter pores of the self-made wear-resistant agent and react with silicon dioxide on the surfaces of the silicon nitride particles to form a liquid phase, so that dissolution and diffusion are promoted, the raw materials are sintered to be more densified, the bending strength of a cutter matrix is enhanced, the surface of a ceramic cutter matrix prepared by sintering after granulation is rough, and the wear resistance of a cutter is enhanced;
when the surface of the cutter matrix is processed, micro-arc oxidation treatment is carried out firstly, and under the action of instantaneous high temperature and high pressure generated by arc discharge, a porous alumina ceramic film grows in situ on the surface of the cutter matrix, so that the rough surface of the cutter matrix is converted into a denser nanoscale rough surface, and the wear resistance of the ceramic cutter is further enhanced; and then carrying out plasma vapor deposition in the atmosphere of nitrogen, borane and silane, wherein the borane and the silane collide with each other and decompose into free radicals, so that the free radicals react with the surface of the tool to form a boron nitride film, and the bending strength of the ceramic tool is further enhanced.
Detailed Description
The technical solutions of the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
In order to more clearly explain the method provided by the application, the following examples are used for describing in detail the methods for testing the indexes of the silicon nitride ceramic tools prepared in the examples and comparative examples as follows:
abrasion resistance: the silicon nitride ceramic tools prepared in examples and comparative examples were subjected to wear rate testing under the same conditions using a reciprocating sliding type frictional wear testing machine.
Flexural strength: the silicon nitride ceramic tools prepared in examples and comparative examples were subjected to bending strength test on test specimens using a three-point bending method using a tensile tester, with a span of 30mm and a loading speed of 0.5 mm/min.
Example 1
(1) Mixing lanthanum hexaboride, yttrium oxide, lithium carbonate and aluminum oxide according to a mass ratio of 1:1:0.4:0.4, performing ball milling, wherein a ball milling medium is absolute ethyl alcohol, a ball material ratio is 9:1, performing ball milling for 50min, drying, sieving with a 80-mesh sieve, transferring into a sintering furnace, heating to 900 ℃, and sintering for 2h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to a mass ratio of 80:3:9:2:3, ball milling in a ball mill, wherein the ball material ratio is 9:1, transferring to a calciner after ball milling for 8 hours, calcining for 30 minutes at 800 ℃, adding an adhesive with the mass of 0.01-0.03 times of that of the silicon nitride, granulating to obtain granules, and finally performing dry pressing and hot isostatic pressing treatment, wherein the granules are dry pressed for 20 minutes under 60MPa during dry pressing; when in hot isostatic pressing, the temperature is 1000 ℃ and the pressure is 150MPa, so as to prepare the ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic cutter matrix, taking the ceramic cutter matrix as an anode, taking a stainless steel electrolytic tank as a cathode, wherein the pulse voltage is 450V, the negative pulse voltage is 100V, the pulse frequency is 400Hz, and the duty ratio is 25%; the electrolyte comprises the following components: 12g/L of sodium aluminate, 6g/L of sodium phosphate, 0.04mol/L of glycerol and 1g/L of silicon carbide;
(4) Transferring the ceramic cutter matrix subjected to micro-arc oxidation treatment between positive and negative electrodes in a vacuum furnace, heating to 280 ℃ in the atmosphere of mixed gas of diborane, silane and nitrogen, wherein the volume ratio of diborane, silane and nitrogen is 1:1:8, conducting power on treatment for 20min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
Example 2
(1) Mixing lanthanum hexaboride, yttrium oxide, lithium carbonate and aluminum oxide according to a mass ratio of 1:1.1:0.5:0.5, performing ball milling, wherein a ball milling medium is absolute ethyl alcohol, a ball material ratio is 9:1, performing ball milling for 65min, drying, sieving with a 90-mesh sieve, transferring into a sintering furnace, heating to 950 ℃, and sintering for 3h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to a mass ratio of 90:4:12:3:4, ball milling in a ball mill, wherein a ball material ratio is 9:1, ball milling for 10 hours, transferring into a calciner, calcining for 40 minutes at 850 ℃, adding an adhesive with silicon nitride mass of 0.02 times for granulating to obtain granules, and finally performing dry pressing and hot isostatic pressing treatment, wherein the granules are dry pressed for 30 minutes under 70MPa during dry pressing; when in hot isostatic pressing, the temperature is 1100 ℃ and the pressure is 165MPa, so as to prepare the ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic cutter matrix, wherein the ceramic cutter matrix is taken as an anode, a stainless steel electrolytic tank is taken as a cathode, the pulse voltage is 475V, the negative pulse voltage is 125V, the pulse frequency is 450Hz, and the duty ratio is 30%; the electrolyte comprises the following components: 13g/L of sodium aluminate, 8g/L of sodium phosphate, 0.06mol/L of glycerol and 2g/L of silicon carbide;
(4) Transferring the ceramic cutter matrix subjected to micro-arc oxidation treatment between positive and negative electrodes in a vacuum furnace, heating to 315 ℃ in the atmosphere of mixed gas of diborane, silane and nitrogen, carrying out electrifying treatment for 35min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
Example 3
(1) Mixing lanthanum hexaboride, yttrium oxide, lithium carbonate and aluminum oxide according to a mass ratio of 1:1.2:0.6:0.6, performing ball milling, wherein a ball milling medium is absolute ethyl alcohol, a ball material ratio is 9:1, performing ball milling for 80min, drying, sieving with a 100-mesh sieve, transferring into a sintering furnace, heating to 1000 ℃, and sintering for 4h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to a mass ratio of 100:5:15:4:5, ball milling in a ball mill, wherein a ball material ratio is 9:1, ball milling for 12 hours, transferring to a calciner, calcining for 50 minutes at 900 ℃, adding an adhesive with silicon nitride mass of 0.03 times for granulating to obtain granules, and finally performing dry pressing and hot isostatic pressing treatment, wherein the granules are dry pressed for 40 minutes under 80MPa during dry pressing; when in hot isostatic pressing, the temperature is 1200 ℃ and the pressure is 180MPa, so as to prepare the ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic cutter matrix, wherein the ceramic cutter matrix is taken as an anode, a stainless steel electrolytic tank is taken as a cathode, the pulse voltage is 500V, the negative pulse voltage is 150V, the pulse frequency is 500Hz, and the duty ratio is 35%; the electrolyte comprises the following components: 14g/L of sodium aluminate, 10g/L of sodium phosphate, 0.08mol/L of glycerol and 4g/L of silicon carbide;
(4) Transferring the ceramic cutter matrix subjected to micro-arc oxidation treatment between positive and negative electrodes in a vacuum furnace, heating to 350 ℃ in the atmosphere of mixed gas of diborane, silane and nitrogen, carrying out electrifying treatment for 50min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
Comparative example 1
(1) Mixing lanthanum hexaboride and yttrium oxide according to a mass ratio of 1:1.1, performing ball milling, wherein a ball milling medium is absolute ethyl alcohol, a ball material ratio is 9:1, performing ball milling for 65min, drying, sieving with a 90-mesh sieve, transferring into a sintering furnace, heating to 950 ℃, and sintering for 3h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to a mass ratio of 90:4:12:3:4, ball milling in a ball mill, wherein a ball material ratio is 9:1, ball milling for 10 hours, transferring into a calciner, calcining for 40 minutes at 850 ℃, adding an adhesive with silicon nitride mass of 0.02 times for granulating to obtain granules, and finally performing dry pressing and hot isostatic pressing treatment, wherein the granules are dry pressed for 30 minutes under 70MPa during dry pressing; when in hot isostatic pressing, the temperature is 1100 ℃ and the pressure is 165MPa, so as to prepare the ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic cutter matrix, wherein the ceramic cutter matrix is taken as an anode, a stainless steel electrolytic tank is taken as a cathode, the pulse voltage is 475V, the negative pulse voltage is 125V, the pulse frequency is 450Hz, and the duty ratio is 30%; the electrolyte comprises the following components: 13g/L of sodium aluminate, 8g/L of sodium phosphate, 0.06mol/L of glycerol and 2g/L of silicon carbide;
(4) Transferring the ceramic cutter matrix subjected to micro-arc oxidation treatment between positive and negative electrodes in a vacuum furnace, heating to 315 ℃ in the atmosphere of mixed gas of diborane, silane and nitrogen, carrying out electrifying treatment for 35min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
Comparative example 2
(1) Mixing lanthanum hexaboride, yttrium oxide and lithium aluminate according to a mass ratio of 1:1.1:1, performing ball milling, wherein a ball milling medium is absolute ethyl alcohol, a ball material ratio is 9:1, performing ball milling for 65min, drying, and sieving with a 90-mesh sieve to obtain a self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to a mass ratio of 90:4:12:3:4, ball milling in a ball mill, wherein a ball material ratio is 9:1, ball milling for 10 hours, transferring into a calciner, calcining for 40 minutes at 850 ℃, adding an adhesive with silicon nitride mass of 0.02 times for granulating to obtain granules, and finally performing dry pressing and hot isostatic pressing treatment, wherein the granules are dry pressed for 30 minutes under 70MPa during dry pressing; when in hot isostatic pressing, the temperature is 1100 ℃ and the pressure is 165MPa, so as to prepare the ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic cutter matrix, wherein the ceramic cutter matrix is taken as an anode, a stainless steel electrolytic tank is taken as a cathode, the pulse voltage is 475V, the negative pulse voltage is 125V, the pulse frequency is 450Hz, and the duty ratio is 30%; the electrolyte comprises the following components: 13g/L of sodium aluminate, 8g/L of sodium phosphate, 0.06mol/L of glycerol and 2g/L of silicon carbide;
(4) Transferring the ceramic cutter matrix subjected to micro-arc oxidation treatment between positive and negative electrodes in a vacuum furnace, heating to 315 ℃ in the atmosphere of mixed gas of diborane, silane and nitrogen, carrying out electrifying treatment for 35min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
Comparative example 3
(1) Mixing lanthanum hexaboride, yttrium oxide, lithium carbonate and aluminum oxide according to a mass ratio of 1:1.1:0.5:0.5, performing ball milling, wherein a ball milling medium is absolute ethyl alcohol, a ball material ratio is 9:1, performing ball milling for 65min, drying, sieving with a 90-mesh sieve, transferring into a sintering furnace, heating to 950 ℃, and sintering for 3h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to a mass ratio of 90:4:12:3:4, ball milling in a ball mill, wherein a ball material ratio is 9:1, ball milling for 10 hours, transferring into a calciner, calcining for 40 minutes at 850 ℃, adding an adhesive with silicon nitride mass of 0.02 times for granulating to obtain granules, and finally performing dry pressing and hot isostatic pressing treatment, wherein the granules are dry pressed for 30 minutes under 70MPa during dry pressing; when in hot isostatic pressing, the temperature is 1100 ℃ and the pressure is 165MPa, so as to prepare the ceramic knife matrix;
(3) Transferring the ceramic cutter matrix between positive and negative electrodes in a vacuum furnace, heating to 315 ℃ in the atmosphere of mixed gas of diborane, silane and nitrogen, conducting electrifying for 35min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
Comparative example 4
(1) Mixing lanthanum hexaboride, yttrium oxide, lithium carbonate and aluminum oxide according to a mass ratio of 1:1.1:0.5:0.5, performing ball milling, wherein a ball milling medium is absolute ethyl alcohol, a ball material ratio is 9:1, performing ball milling for 65min, drying, sieving with a 90-mesh sieve, transferring into a sintering furnace, heating to 950 ℃, and sintering for 3h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to a mass ratio of 90:4:12:3:4, ball milling in a ball mill, wherein a ball material ratio is 9:1, ball milling for 10 hours, transferring into a calciner, calcining for 40 minutes at 850 ℃, adding an adhesive with silicon nitride mass of 0.02 times for granulating to obtain granules, and finally performing dry pressing and hot isostatic pressing treatment, wherein the granules are dry pressed for 30 minutes under 70MPa during dry pressing; when in hot isostatic pressing, the temperature is 1100 ℃ and the pressure is 165MPa, so as to prepare the ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic cutter matrix, wherein the ceramic cutter matrix is taken as an anode, a stainless steel electrolytic tank is taken as a cathode, the pulse voltage is 475V, the negative pulse voltage is 125V, the pulse frequency is 450Hz, and the duty ratio is 30%; the electrolyte comprises the following components: 13g/L of sodium aluminate, 8g/L of sodium phosphate, 0.06mol/L of glycerol and 2g/L of silicon carbide, and preparing the silicon nitride ceramic cutter.
Effect example
The following table 1 gives the results of performance analysis of silicon nitride ceramic tools employing examples 1 to 3 of the present application and comparative examples 1 to 4:
TABLE 1
| Flexural Strength MPa | Wear Rate (. Times.10) -8 mm 3 /(N·m)) | |
| Example 1 | 981 | 10.73 |
| Example 2 | 983 | 11.25 |
| Example 3 | 974 | 10.06 |
| Comparative example 1 | 825 | 16.86 |
| Comparative example 2 | 854 | 16.31 |
| Comparative example 3 | 972 | 20.85 |
| Comparative example 4 | 891 | 12.96 |
As is evident from comparison of the experimental data of examples and comparative examples in Table 1, the silicon nitride ceramic tools prepared in examples 1, 2 and 3 were superior in bending strength and wear resistance.
It will be evident to those skilled in the art that the application is not limited to the details of the foregoing illustrative embodiments, and that the present application may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the application being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. The silicon nitride ceramic cutter is characterized in that the silicon nitride ceramic cutter is manufactured by processing the surface of a ceramic cutter matrix;
the ceramic cutter matrix is prepared by mixing raw materials with self-made wear-resistant auxiliary agents, granulating, and sintering;
the raw materials comprise silicon nitride, titanium nitride, aluminum oxide and zirconium oxide;
the self-made wear-resistant auxiliary agent is prepared by generating lithium aluminate crystals on the surfaces of lanthanum hexaboride and yttrium oxide;
the processing treatment is that the ceramic cutter matrix is firstly subjected to micro-arc oxidation treatment, and then is subjected to plasma vapor deposition in the atmosphere of nitrogen, borane and silane.
2. The preparation method of the silicon nitride ceramic cutter is characterized by comprising the following specific steps of:
(1) Mixing lanthanum hexaboride, yttrium oxide, lithium carbonate and aluminum oxide, performing ball milling, wherein the ball milling medium is absolute ethyl alcohol, the ball material ratio is 9:1, performing ball milling for 50-80 min, drying, sieving with a 80-100 mesh sieve, transferring into a sintering furnace, heating to 900-1000 ℃, and sintering for 2-4 h to obtain the self-made wear-resistant auxiliary agent;
(2) Mixing silicon nitride, titanium nitride, aluminum oxide, zirconium oxide and an abrasion-resistant additive according to the mass ratio of 80:3:9:2:3-100:5:15:4:5, ball milling in a ball mill, ball milling for 8-12 hours at the ball material ratio of 9:1, transferring to a calciner, calcining for 30-50 minutes at 800-900 ℃, adding an adhesive with the mass of 0.01-0.03 times of that of the silicon nitride, granulating, preparing granules, and finally performing dry pressing and hot isostatic pressing treatment to prepare a ceramic knife matrix;
(3) Performing micro-arc oxidation treatment on the ceramic knife matrix;
(4) Transferring the ceramic cutter matrix subjected to micro-arc oxidation treatment between positive and negative electrodes in a vacuum furnace, heating to 280-350 ℃ in the atmosphere of diborane, silane and nitrogen, electrifying for 20-50 min, and cooling to room temperature to obtain the silicon nitride ceramic cutter.
3. The method of producing a silicon nitride ceramic tool according to claim 2, wherein in the step (1): the mass ratio of lanthanum hexaboride to yttrium oxide to lithium carbonate to aluminum oxide is 1:1:0.4:0.4-1:1.2:0.6:0.6.
4. The method of producing a silicon nitride ceramic tool according to claim 2, wherein in the step (2): in the dry pressing process, the granules are dry pressed for 20 to 40 minutes under the pressure of 60 to 80 MPa; the temperature is 1000-1200 deg.c and the pressure is 150-180 MPa during hot isostatic pressing.
5. The method of producing a silicon nitride ceramic tool according to claim 2, wherein in the step (3): when in micro-arc oxidation treatment, a ceramic cutter matrix is taken as an anode, a stainless steel electrolytic tank is taken as a cathode, the pulse voltage is 450-500V, the negative pulse voltage is 100-150V, the pulse frequency is 400-500 Hz, and the duty ratio is 25-35%; the electrolyte comprises the following components: 12-14 g/L of sodium aluminate, 6-10 g/L of sodium phosphate, 0.04-0.08 mol/L of glycerol and 1-4 g/L of silicon carbide.
6. The method of producing a silicon nitride ceramic tool according to claim 2, wherein in the step (4): in the mixed gas of diborane, silane and nitrogen, the volume ratio of diborane, silane and nitrogen is 1:1:8-2:1:10.
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