CN115124353B - Layered composite ceramic cylindrical roller and preparation method thereof - Google Patents
Layered composite ceramic cylindrical roller and preparation method thereof Download PDFInfo
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- CN115124353B CN115124353B CN202210834891.5A CN202210834891A CN115124353B CN 115124353 B CN115124353 B CN 115124353B CN 202210834891 A CN202210834891 A CN 202210834891A CN 115124353 B CN115124353 B CN 115124353B
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 100
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 82
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 9
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 9
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- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
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- 229910052684 Cerium Inorganic materials 0.000 claims description 2
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
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- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 5
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 10
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 10
- 238000005096 rolling process Methods 0.000 description 9
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
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- 229910001873 dinitrogen Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- 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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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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Abstract
The invention relates to the technical field of silicon nitride ceramics, in particular to a layered composite ceramic cylindrical roller and a preparation method thereof. The preparation method provided by the invention comprises the following steps: mixing the sintering aid coated silicon nitride material, a binder, a dispersant and water, and carrying out first ball milling to obtain first slurry; mixing the sintering aid coated silicon nitride material, the reinforcing phase, the binder, the dispersant and water, and carrying out second ball milling to obtain second slurry; injecting the first slurry into a cylindrical roller die, performing first standing to obtain an outer layer of a blank, injecting the second slurry, performing second standing to obtain an inner layer of the blank, and sequentially demolding and maintaining to obtain the blank; sequentially carrying out glue discharging, air pressure sintering and hot isostatic pressing treatment on the green body to obtain a layered composite ceramic cylindrical roller; the reinforcing phase is one or more of titanium nitride, titanium carbide and tungsten carbide. The layered composite ceramic cylindrical roller prepared by the invention not only has higher mechanical property, but also has excellent anti-corrosion property.
Description
Technical Field
The invention relates to the technical field of silicon nitride ceramics, in particular to a layered composite ceramic cylindrical roller and a preparation method thereof.
Background
The mixed ceramic bearing using silicon nitride as the rolling body has the advantages of light weight, wear resistance, corrosion resistance, electric insulation, self-lubrication and the like, and is suitable for being applied under severe working conditions of high rotating speed, heavy load, poor lubrication and the like. The focus of attention is always on how to improve the impact resistance of silicon nitride ceramic rolling elements. When the silicon nitride ceramic rolling element is prepared, reinforcing phases such as titanium nitride, titanium carbide and tungsten carbide are generally added, the fracture toughness of the silicon nitride ceramic rolling element is improved in a particle toughening mode, and then the impact resistance of the silicon nitride ceramic rolling element is improved, but the addition of the reinforcing phases such as titanium nitride, titanium carbide and tungsten carbide can reduce the resistivity of the silicon nitride ceramic rolling element, and is not beneficial to the application of the silicon nitride ceramic rolling element in a strong-electric corrosion environment.
Disclosure of Invention
The invention aims to provide a layered composite ceramic cylindrical roller and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a layered composite ceramic cylindrical roller, which comprises the following steps:
mixing the sintering aid coated silicon nitride material, a binder, a dispersant and water, and carrying out first ball milling to obtain first slurry;
mixing the sintering aid coated silicon nitride material, the reinforcing phase, the binder, the dispersant and water, and carrying out second ball milling to obtain second slurry;
injecting the first slurry into a cylindrical roller die, performing first standing to obtain an outer layer of a blank, injecting the second slurry, performing second standing to obtain an inner layer of the blank, and sequentially performing demoulding and maintenance to obtain the blank;
sequentially carrying out glue discharging, air pressure sintering and hot isostatic pressing treatment on the green body to obtain the layered composite ceramic cylindrical roller;
the reinforcing phase is one or more of titanium nitride, titanium carbide and tungsten carbide.
Preferably, the preparation method of the sintering aid-coated silicon nitride material comprises the following steps:
mixing silicon nitride, a sintering aid precursor and water to obtain mixed slurry;
and (3) carrying out hydrolysis reaction on the mixed slurry under an alkaline condition, and then sequentially drying and calcining to obtain the sintering aid coated silicon nitride material.
Preferably, the mass ratio of the silicon nitride to the sintering aid in the sintering aid-coated silicon nitride material is (85-95) to (5-15);
the alkaline condition is pH = 9-11;
the calcining temperature is 500-800 ℃, and the heat preservation time is 2-4 h.
Preferably, in the first slurry, the mass ratio of the bonding assistant coated silicon nitride material to the binder to the dispersant is 100 (0.5-3) to (0.5-3);
the mass solid content of the first slurry is more than or equal to 70%, and the viscosity is less than or equal to 1000 mPa.
Preferably, in the second slurry, the mass ratio of the sintering aid coated silicon nitride material to the reinforcing phase is 100 (5-30); the ratio of the mass of the binder to the total mass of the sintering aid-coated silicon nitride material and the reinforcing phase is (0.5-3): 100; the ratio of the mass of the dispersing agent to the total mass of the sintering aid coated silicon nitride material and the reinforcing phase is (0.5-3): 100.
Preferably, the mass solid content of the second slurry is more than or equal to 63 percent, and the viscosity is less than or equal to 1000 mPa.
Preferably, the binder is one or more of polyethylene glycol, acrylic resin, polyvinyl alcohol and carboxymethyl cellulose;
the dispersant is one or more of polyethyleneimine, ammonium polyacrylate, ammonium citrate and tetramethyl ammonium hydroxide;
the average grain diameter of the reinforcing phase is less than or equal to 3 mu m.
Preferably, the gas used for the gas pressure sintering is nitrogen;
the temperature of the air pressure sintering is 1600-1800 ℃, and the time is 2-6 h; the pressure of the nitrogen is 0.6-0.9 MPa.
Preferably, the hot isostatic pressing treatment is performed in a nitrogen atmosphere;
the hot isostatic pressing treatment temperature is 1700-1900 ℃, the time is 1-3 h, and the pressure of the nitrogen atmosphere is 100-200 MPa.
The invention also provides the layered composite ceramic cylindrical roller prepared by the preparation method in the technical scheme.
The invention provides a preparation method of a layered composite ceramic cylindrical roller, which comprises the following steps: mixing the sintering aid coated silicon nitride material, a binder, a dispersant and water, and carrying out first ball milling to obtain first slurry; mixing the sintering aid coated silicon nitride material, the reinforcing phase, the binder, the dispersant and water, and carrying out second ball milling to obtain second slurry; injecting the first slurry into a cylindrical roller die, performing first standing to obtain an outer layer of a blank, injecting the second slurry, performing second standing to obtain an inner layer of the blank, and sequentially performing demoulding and maintenance to obtain the blank; sequentially carrying out glue discharging, air pressure sintering and hot isostatic pressing treatment on the green body to obtain the layered composite ceramic cylindrical roller; the reinforcing phase is one or more of titanium nitride, titanium carbide and tungsten carbide. The ceramic cylindrical roller blank with the layered composite structure is prepared by slip casting, and sintering densification of the layered composite ceramic cylindrical roller blank is realized by utilizing hot isostatic pressing. The composition of the first slurry is regulated and controlled to ensure that the layer (outer layer) of the first slurry has higher hardness and electrical insulation, and the wear resistance and the electrical corrosion resistance of the ceramic roller are improved; and a reinforcing phase is added into the second slurry, so that the layer (inner layer) where the reinforcing phase is arranged has higher fracture toughness, and the impact resistance of the ceramic roller is improved. And because the inner layer and the outer layer are different in composition, the thermal expansion coefficient of the inner layer material is far larger than that of the outer layer material, so that residual stress can be generated, the fatigue resistance of the ceramic cylindrical roller is integrally improved, the Hertz stress causing fatigue failure of the ceramic roller in the rolling contact process is reduced, and the fatigue life and the reliability of the ceramic cylindrical roller are improved.
Drawings
Fig. 1 is a schematic structural diagram of a layered composite ceramic cylindrical roller product according to embodiments 1 to 3.
Detailed Description
The invention provides a preparation method of a layered composite ceramic cylindrical roller, which comprises the following steps:
mixing the sintering aid coated silicon nitride material, a binder, a dispersant and water, and performing first ball milling to obtain first slurry;
mixing the sintering aid coated silicon nitride material, the reinforcing phase, the binder, the dispersant and water, and carrying out second ball milling to obtain second slurry;
injecting the first slurry into a cylindrical roller die, performing first standing to obtain an outer layer of a blank, injecting the second slurry, performing second standing to obtain an inner layer of the blank, and sequentially performing demoulding and maintenance to obtain the blank;
sequentially carrying out glue discharging, air pressure sintering and hot isostatic pressing treatment on the green body to obtain the layered composite ceramic cylindrical roller;
the reinforcing phase is one or more of titanium nitride, titanium carbide and tungsten carbide.
In the present invention, unless otherwise specified, all the starting materials for the preparation are commercially available products well known to those skilled in the art.
The method comprises the steps of mixing a sintering aid coated silicon nitride material, a binder, a dispersant and water, and carrying out first ball milling to obtain first slurry; and mixing the sintering aid coated silicon nitride material, the reinforcing phase, the binder, the dispersant and water, and carrying out second ball milling to obtain second slurry.
In the present invention, the preparation method of the sintering aid-coated silicon nitride material preferably includes the following steps:
mixing silicon nitride, a sintering aid precursor and water to obtain mixed slurry;
and (3) carrying out hydrolysis reaction on the mixed slurry under an alkaline condition, and then sequentially drying and calcining to obtain the sintering aid-coated silicon nitride material.
According to the invention, silicon nitride, a sintering aid precursor and water are mixed to obtain mixed slurry.
In the present invention, α -Si in the silicon nitride 3 N 4 The phase content is preferably 80% or more, more preferably 80 to 90%, most preferably 90%; the average particle diameter D50 is preferably 1.5 μm or less, more preferably 1.1 to 1.5. Mu.m, most preferably 1.1. Mu.m.
In the present invention, the sintering aid precursor is preferably a soluble metal salt; the soluble metal salt is preferably a soluble metal nitrate or a soluble metal hydrochloride; the metal in the soluble metal salt is preferably one or more of aluminum, magnesium, yttrium, lanthanum, cerium, neodymium, erbium, ytterbium and lutetium; when the metal is more than two of the specific choices, the proportion of the specific materials is not limited in any way, and the specific materials can be mixed according to any proportion. In the invention, the purity of the sintering aid precursor is preferably more than or equal to 99%.
In the present invention, the mass ratio of the silicon nitride to the sintering aid precursor is preferably calculated from a compounding ratio of "the mass ratio of the silicon nitride to the sintering aid in the sintering aid-coated silicon nitride material is preferably (85 to 95): 5 to 15), and more preferably (88 to 92): 8 to 12".
In the present invention, the water is preferably deionized water.
In the present invention, the mixing time is preferably 4 to 6 hours, more preferably 4.5 to 5.5 hours; the mixing method is not particularly limited, and may be performed in a manner known to those skilled in the art.
In the present invention, the mass solid content of the mixed slurry is preferably 30 to 50%.
After the mixed slurry is obtained, the mixed slurry is subjected to hydrolysis reaction under an alkaline condition, and then is dried and calcined in sequence to obtain the sintering aid-coated silicon nitride material.
In the present invention, the alkaline condition is preferably pH =9 to 11; the alkaline condition is preferably realized by adjusting the mixed slurry by using a pH regulator; the pH regulator is preferably ammonia water or a sodium hydroxide solution with the mass concentration of 5%; the concentration of the aqueous ammonia in the present invention is not particularly limited, and may be a concentration known to those skilled in the art.
In the present invention, the time for the hydrolysis reaction is preferably 2 to 4 hours. The hydrolysis reaction is preferably carried out under stirring, and the rotation speed of the stirring is not limited in any way, and the rotation speed is known to those skilled in the art, and the sintering aid precursor is sufficiently hydrolyzed within the time range.
In the present invention, the drying is preferably performed by vacuum drying; the temperature of the vacuum drying is preferably 80 ℃; the vacuum drying time is not limited in any way in the present invention, and the time known to those skilled in the art can be used up to a constant weight.
In the present invention, the calcination is preferably performed in an air atmosphere or a nitrogen atmosphere. The calcination temperature is preferably 500-800 ℃, more preferably 550-750 ℃, and most preferably 600-700 ℃; the time is preferably 2 to 4 hours, more preferably 2.5 to 3.5 hours.
After the calcination, the present invention also preferably includes passing the product obtained after the calcination through a 50 mesh screen.
In the invention, the sintering aid coated silicon nitride material is used as a raw material for preparing the layered composite ceramic cylindrical roller, and the advantages of preventing the hydrolysis of silicon nitride powder and improving the solid content of the grouting forming slurry are achieved.
In the invention, the binder is preferably one or more of polyethylene glycol, acrylic resin, polyvinyl alcohol and carboxymethyl cellulose; when the binder is more than two of the above specific choices, the invention does not have any special limitation on the proportion of the specific substances, and the specific substances are mixed according to any proportion.
In the invention, the dispersant is preferably one or more of polyethyleneimine, ammonium polyacrylate, ammonium citrate and tetramethylammonium hydroxide; when the dispersant is more than two of the above specific choices, the invention does not have any special limitation on the proportion of the specific substances, and the specific substances can be mixed according to any proportion.
In the present invention, the water is preferably deionized water.
In the invention, in the first slurry, the mass ratio of the sintering aid coated silicon nitride material, the binder and the dispersant is preferably (0.5-3) to (0.5-3) of 100, more preferably (1.0-2.5) to (1.0-2.5) of 100, and most preferably (1.5-2.0) to (1.5-2.0) of 100.
In the invention, the rotating speed of the first ball mill is preferably more than or equal to 100r/min, and more preferably more than or equal to 150r/min; the time is preferably 6 to 12 hours, more preferably 8 to 10 hours.
In the invention, the mass solid content of the first slurry is preferably equal to or more than 70%, more preferably 70-80%, and most preferably 72%; the viscosity is preferably 1000 mPas or less, more preferably 500 to 800 mPas.
In the invention, the reinforcing phase is one or more of titanium nitride, titanium carbide and tungsten carbide; when the reinforcing phases are more than two of the specific choices, the proportion of the specific substances is not limited in any way, and the specific substances can be mixed according to any proportion. In the present invention, the average particle diameter (D50) of the reinforcing phase is preferably 3 μm or less.
In the present invention, the mass ratio of the sintering aid-coated silicon nitride material to the reinforcing phase in the second slurry is preferably 100 (5 to 30), and more preferably 100 (10 to 25). In the present invention, the ratio of the mass of the binder to the total mass of the sintering aid-coated silicon nitride material and the reinforcing phase is preferably (0.5 to 3): 100, and more preferably (1.0 to 2.5): 100. In the present invention, the ratio of the mass of the dispersant to the total mass of the sintering aid-coated silicon nitride material and the reinforcing phase is preferably (0.5 to 3): 100, and more preferably (1.0 to 2.5): 100.
In the invention, the rotating speed of the second ball mill is preferably more than or equal to 100r/min, more preferably more than or equal to 150r/min; the time is preferably 6 to 12 hours, more preferably 8 to 10 hours.
In the invention, the mass solid content of the second slurry is preferably equal to or more than 63 percent, and more preferably 68-70 percent; the viscosity is preferably 1000 mPas or less, more preferably 300 to 400 mPas.
In the invention, the binder has the functions of improving the strength of the blank and preventing cracking; the dispersant has the functions of increasing the solid content of the slurry and reducing the viscosity of the slurry; the reinforcing phase serves to improve the fracture toughness of the ceramic roller.
After the first slurry and the second slurry are obtained, the first slurry is injected into a cylindrical roller die to carry out first standing to obtain an outer layer of a blank, the second slurry is injected into the cylindrical roller die to carry out second standing to obtain an inner layer of the blank, and demoulding and maintenance are sequentially carried out to obtain the blank.
Before the first slurry and the second slurry are injected into the cylindrical roller die, the first slurry and the second slurry are preferably subjected to vacuum defoaming respectively; the vacuum defoaming process is not limited in any way, and can be carried out by a process well known to those skilled in the art.
In the present invention, the material of the cylindrical roller mold is preferably gypsum or resin.
In the present invention, the time for the first standing is preferably 1 to 10 hours, more preferably 3 to 8 hours, and most preferably 4 to 6 hours.
After the first standing is completed, the present invention preferably further comprises removing excess slurry that is not solidified after the standing. The removal is preferably by pouring the excess slurry out of an inclined cylindrical roller die.
In the present invention, the time for the second standing is preferably 10 to 30 hours, and more preferably 15 to 25 hours.
The demolding process is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art.
In the present invention, the curing is preferably performed in a constant temperature and humidity environment; the curing temperature is preferably 30-50 ℃, more preferably 35-45 ℃, and most preferably 38-42 ℃; the humidity is preferably 60 to 80%, more preferably 65 to 75%, most preferably 68 to 75%; the time is preferably 24h. In the present invention, the curing is preferably performed in a constant temperature and humidity chamber.
After the maintenance is finished, the invention also preferably comprises drying; the drying temperature is preferably 110-150 ℃, and more preferably 120-140 ℃; the heating rate of heating to the drying temperature is preferably 3-30 ℃/h, more preferably 5-25 ℃/h; the time is preferably 2 to 10 hours, more preferably 4 to 8 hours. In the present invention, the drying is preferably performed in a microwave drying oven.
In the present invention, the gel removal is preferably performed in air, nitrogen or vacuum; the rubber discharging temperature is preferably 400-600 ℃, more preferably 450-550 ℃, and most preferably 480-520 ℃; the time is preferably 2 to 10 hours, more preferably 4 to 8 hours, most preferably 5 to 6 hours. In the present invention, the degumming is preferably performed in a degumming oven.
In the invention, the gas used for the gas pressure sintering is preferably nitrogen; the temperature of the air pressure sintering is preferably 1600-1800 ℃, more preferably 1650-1750 ℃, and most preferably 1680-1720 ℃; the time is preferably 2 to 6 hours, more preferably 3 to 5 hours; the pressure of the nitrogen gas is preferably 0.6 to 0.9MPa.
In the present invention, the hot isostatic pressing treatment is preferably performed in a nitrogen atmosphere; the temperature of the hot isostatic pressing treatment is preferably 1700-1900 ℃, more preferably 1750-1850 ℃, and most preferably 1780-1820 ℃; the time is preferably 1 to 3 hours, more preferably 1.5 to 2.5 hours, and most preferably 1.8 to 2.2 hours; the pressure of the nitrogen atmosphere is preferably 100 to 200MPa, more preferably 120 to 180MPa, and most preferably 130 to 160MPa.
In the invention, the hot isostatic pressing treatment has the effect and advantage of improving the compactness and reliability of the ceramic roller.
After the hot isostatic pressing treatment is completed, the invention also preferably comprises machining; the machining process is not limited in any way, and the layered composite ceramic cylindrical roller with the actually required size and shape can be obtained by adopting the process well known to the skilled person.
The invention also provides the layered composite ceramic cylindrical roller prepared by the preparation method in the technical scheme.
The layered composite ceramic cylindrical roller and the method for manufacturing the same according to the present invention will be described in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
Preparing raw materials:
silicon nitride powder: alpha-Si 3 N 4 The phase content was 90%, the average particle diameter D50 was 1.1. Mu.m;
precursor of sintering aid: the mass ratio of the aluminum nitrate to the yttrium nitrate is 1:1, the purity of the aluminum nitrate to the yttrium nitrate is more than or equal to 99%, and the mass ratio of the silicon nitride powder to the sintering aid precursor finally formed into the sintering aid is 92;
the binder is polyethylene glycol;
the dispersant is polyethyleneimine;
the reinforcing phase is titanium nitride, the purity is more than or equal to 99 percent, and the D50 is 1 mu m;
the preparation process comprises the following steps:
stirring and mixing silicon nitride powder, a sintering aid precursor and deionized water for 4 hours to obtain mixed slurry (the mass solid content is 40%);
adjusting the pH value of the obtained mixed slurry to 9 by ammonia water, stirring for 3h until the sintering aid precursor is fully hydrolyzed, performing vacuum drying (80 ℃) and calcination (the calcination temperature is 600 ℃, the calcination time is 4h, and the atmosphere is air), and sieving by a 50-mesh sieve to obtain a sintering aid-coated silicon nitride material;
mixing and ball-milling 36kg of sintering aid coated silicon nitride material, 0.18kg of binder, 0.54kg of dispersant and deionized water for 8 hours to obtain first slurry (the mass solid content is 72%, and the viscosity is 500mPa & s);
mixing 36kg of sintering aid coated silicon nitride material, 7.2kg of reinforcing phase, 0.22kg of binder, 0.65kg of dispersant and deionized water, and performing ball milling for 12 hours to obtain second slurry (the mass solid content is 68%, and the viscosity is 300mPa & s);
respectively carrying out vacuum defoaming treatment on the first slurry and the second slurry, injecting the first slurry into a cylindrical roller mold, standing for 3 hours, then inclining the cylindrical roller mold to pour out redundant slurry, injecting the second slurry, standing for 20 hours until the slurry is completely cured, demolding, putting into a constant-temperature constant-humidity box with the temperature of 40 ℃ and the humidity of 70% for curing for 24 hours, and then putting into a microwave drying box for drying (the temperature is 110 ℃, the time is 6 hours, and the heating rate is 10 ℃/h) to obtain a blank;
and (2) placing the blank into a glue discharging furnace to discharge glue (the temperature is 600 ℃, the heat preservation time is 3h, and the atmosphere is air), placing the blank after glue discharging into air pressure sintering (the temperature is 1700 ℃, the heat preservation time is 3h, and the nitrogen pressure is 0.9 MPa), performing hot isostatic pressing (the temperature is 1750 ℃, the heat preservation time is 2h, and the nitrogen pressure is 150 MPa) to obtain a ceramic roller blank, and machining to obtain a layered composite ceramic cylindrical roller finished product, wherein the structural schematic diagram is shown in figure 1, the nominal diameter D1 is 8mm, the inner layer diameter D2 is 5mm, and the nominal length L is 10mm.
Example 2
Preparing raw materials:
silicon nitride powder: alpha-Si 3 N 4 The phase content was 90%, the average particle diameter D50 was 1.1. Mu.m;
the sintering aid precursor comprises aluminum nitrate and yttrium nitrate with the mass ratio of 1:1, wherein the purity of the aluminum nitrate and the purity of the yttrium nitrate are both more than or equal to 99%, and the mass ratio of the silicon nitride powder to the sintering aid precursor finally formed is 90;
the binder is acrylic resin;
the dispersant is ammonium polyacrylate;
the reinforcing phase is titanium carbide, the purity is more than or equal to 99 percent, and the D50 is 1 mu m;
the preparation process comprises the following steps:
stirring and mixing silicon nitride powder, a sintering aid precursor and deionized water for 6 hours to obtain mixed slurry (the mass solid content is 40%);
adjusting the pH value of the obtained mixed slurry to 10 by ammonia water, stirring for 2h until the sintering aid precursor is fully hydrolyzed, performing vacuum drying (80 ℃) and calcination (the calcination temperature is 700 ℃, the calcination time is 3h, and the atmosphere is nitrogen), and sieving by a 50-mesh sieve to obtain a sintering aid-coated silicon nitride material;
mixing 40kg of sintering aid coated silicon nitride material, 0.6kg of binder, 1kg of dispersant and deionized water, and carrying out ball milling for 10h to obtain first slurry (the mass solid content is 75%, and the viscosity is 600mPa & s);
mixing 40kg of sintering aid coated silicon nitride material, 12kg of reinforcing phase, 0.78kg of binder, 1.3kg of dispersant and deionized water, and ball-milling for 10 hours to obtain second slurry (the mass solid content is 70%, and the viscosity is 400mPa & s);
respectively carrying out vacuum defoaming treatment on the first slurry and the second slurry, injecting the first slurry into a cylindrical roller mold, standing for 5 hours, inclining the cylindrical roller mold to pour out redundant slurry, injecting the second slurry, standing for 25 hours until the slurry is completely cured, demolding, putting into a constant-temperature constant-humidity box with the temperature of 50 ℃ and the humidity of 80% for curing for 24 hours, and then putting into a microwave drying box for drying (the temperature is 150 ℃, the heat preservation time is 3 hours, and the heating rate is 5 ℃/h) to obtain a blank;
and (2) placing the blank into a glue discharging furnace for glue discharging (the temperature is 550 ℃, the heat preservation time is 3h, and the atmosphere is nitrogen), then placing the blank subjected to glue discharging into air pressure sintering (the temperature is 1750 ℃, the heat preservation time is 4h, and the nitrogen air pressure is 0.6 MPa), then performing hot isostatic pressing (the temperature is 1850 ℃, the heat preservation time is 1h, and the nitrogen pressure is 200 MPa) to obtain a ceramic roller blank, and machining to obtain a layered composite ceramic cylindrical roller finished product, wherein the structural schematic diagram is shown in figure 1, the nominal diameter D1 is 15mm, the inner layer diameter D2 is 10mm, and the nominal length L is 22mm.
Example 3
Preparing raw materials:
silicon nitride powder: alpha-Si 3 N 4 Phase content 90%, mean particleThe diameter D50 is 1.1 μm;
precursor of sintering aid: the mass ratio of the aluminum nitrate to the yttrium nitrate is 1:1, the purity of the aluminum nitrate to the yttrium nitrate is more than or equal to 99%, and the mass ratio of the silicon nitride powder to the sintering aid precursor finally formed sintering aid is 90;
the binder is polyvinyl alcohol;
the dispersant is ammonium citrate;
the reinforced phase is tungsten carbide, the purity is more than or equal to 99 percent, and the D50 is 1 mu m;
the preparation process comprises the following steps:
stirring and mixing silicon nitride powder, a sintering aid precursor and deionized water for 5 hours to obtain mixed slurry (the mass solid content is 40%);
adjusting the pH value of the obtained mixed slurry to 11 by using a sodium hydroxide solution with the mass concentration of 5%, stirring for 4h until the sintering aid precursor is fully hydrolyzed, performing vacuum drying (80 ℃) and calcination (the calcination temperature is 800 ℃, the heat preservation time is 2h, and the atmosphere is nitrogen), and sieving by using a 50-mesh sieve to obtain a sintering aid-coated silicon nitride material;
mixing 50kg of sintering aid coated silicon nitride material, 1kg of binder, 1kg of dispersant and deionized water, and carrying out ball milling for 12h to obtain first slurry (the mass solid content is 78%, and the viscosity is 700mPa & s);
mixing 50kg of sintering aid coated silicon nitride material, 2.5kg of reinforcing phase, 1.05kg of binder, 1.05kg of dispersant and deionized water, and performing ball milling for 10 hours to obtain second slurry (the mass solid content is 72%, and the viscosity is 500mPa & s);
respectively carrying out vacuum defoaming treatment on the first slurry and the second slurry, injecting the first slurry into a cylindrical roller mold, standing for 6 hours, then inclining the cylindrical roller mold to pour out redundant slurry, injecting the second slurry, standing for 30 hours until the slurry is completely cured, demolding, putting into a constant-temperature constant-humidity box with the temperature of 30 ℃ and the humidity of 60% for curing for 24 hours, and then putting into a microwave drying box for drying (the temperature is 120 ℃, the heat preservation time is 4 hours, and the heating rate is 20 ℃/h) to obtain a blank;
and (2) placing the blank into a glue discharging furnace to discharge glue (the temperature is 550 ℃, the heat preservation time is 3h, and the atmosphere is nitrogen), then placing the blank after glue discharging into air pressure sintering (the temperature is 1650 ℃, the heat preservation time is 2h, and the nitrogen air pressure is 0.9 MPa), then carrying out hot isostatic pressing treatment (the temperature is 1800 ℃, the heat preservation time is 1h, and the nitrogen pressure is 180 MPa) to obtain a ceramic roller blank, and carrying out machining to obtain a layered composite ceramic cylindrical roller finished product, wherein the structural schematic diagram is shown in figure 1, wherein the nominal diameter D1 is 40mm, the inner layer diameter D2 is 30mm, and the nominal length L is 65mm.
Comparative example 1
Preparing raw materials:
silicon nitride powder: alpha-Si 3 N 4 The phase content was 90%, the average particle diameter D50 was 1.1. Mu.m;
precursor of sintering aid: the mass ratio of the aluminum nitrate to the yttrium nitrate is 1:1, the purity of the aluminum nitrate to the yttrium nitrate is more than or equal to 99%, and the mass ratio of the silicon nitride powder to the sintering aid precursor finally formed sintering aid is 90;
the binder is polyvinyl alcohol;
the dispersant is ammonium polyacrylate;
the preparation process comprises the following steps:
stirring and mixing silicon nitride powder, a sintering aid precursor and deionized water for 6 hours to obtain mixed slurry (the mass solid content is 40%);
adjusting the pH value of the obtained mixed slurry to 10 by ammonia water, stirring for 2h until the sintering aid precursor is fully hydrolyzed, performing vacuum drying (80 ℃) and calcination (the calcination temperature is 700 ℃, the heat preservation time is 3h, and the atmosphere is nitrogen), and sieving by a 50-mesh sieve to obtain a sintering aid-coated silicon nitride material;
mixing 40kg of sintering aid coated silicon nitride material, 0.8kg of binder, 1kg of dispersant and deionized water, and carrying out ball milling for 10h to obtain slurry (the mass solid content is 75%, and the viscosity is 600mPa & s);
after the slurry is subjected to vacuum defoaming treatment, injecting the slurry into a cylindrical roller mold, standing for 30 hours until the slurry is completely cured, demolding, putting into a constant-temperature constant-humidity box with the temperature of 50 ℃ and the humidity of 80% for curing for 24 hours, and then putting into a microwave drying box for drying (the temperature is 150 ℃, the heat preservation time is 3 hours, and the heating rate is 5 ℃/h) to obtain a blank;
and (3) placing the blank into a glue discharging furnace for glue discharging (the temperature is 550 ℃, the heat preservation time is 3h, and the atmosphere is nitrogen), then placing the blank subjected to glue discharging into air pressure sintering (the temperature is 1750 ℃, the heat preservation time is 4h, and the nitrogen air pressure is 0.6 MPa), then performing hot isostatic pressing (the temperature is 1850 ℃, the heat preservation time is 1h, and the nitrogen pressure is 150 MPa) to obtain a ceramic roller blank, and machining to obtain a ceramic cylindrical roller finished product with the nominal diameter of 15mm and the nominal length of 22mm.
Comparative example 2
Preparing raw materials:
silicon nitride powder: alpha-Si 3 N 4 Has a phase content of 90% and an average particle diameter D50 of 1.1 μm;
precursor of sintering aid: the mass ratio of the aluminum nitrate to the yttrium nitrate is 1:1, the purity of the aluminum nitrate to the yttrium nitrate is more than or equal to 99%, and the mass ratio of the silicon nitride powder to the sintering aid precursor finally formed sintering aid is 90;
the binder is polyvinyl alcohol;
the dispersant is ammonium polyacrylate;
the reinforced phase is tungsten carbide, the purity is more than or equal to 99 percent, and the D50 is 1 mu m;
the preparation process comprises the following steps:
stirring and mixing silicon nitride powder, the sintering aid precursor and deionized water for 6 hours to obtain mixed slurry (the mass solid content is 40%);
adjusting the pH value of the obtained mixed slurry to 10 by ammonia water, stirring for 2h until the sintering aid precursor is fully hydrolyzed, performing vacuum drying (80 ℃) and calcination (the calcination temperature is 700 ℃, the heat preservation time is 3h, and the atmosphere is nitrogen), and sieving by a 50-mesh sieve to obtain a sintering aid-coated silicon nitride material;
mixing 40kg of sintering aid coated silicon nitride material, 2kg of reinforcing phase, 0.84kg of binder, 1.05kg of dispersant and deionized water, and carrying out ball milling for 10h to obtain slurry (the mass solid content is 70%, and the viscosity is 400mPa & s);
after the slurry is subjected to vacuum defoaming treatment, injecting the slurry into a cylindrical roller die, standing for 25 hours until the slurry is completely cured, putting the cylindrical roller die into a constant-temperature and constant-humidity box with the temperature of 50 ℃ and the humidity of 80% for curing for 24 hours, and then putting the cylindrical roller die into a microwave drying box for drying (the temperature is 150 ℃, the heat preservation time is 3 hours, and the heating rate is 5 ℃/h) to obtain a blank;
and (3) placing the blank into a glue discharging furnace for glue discharging (the temperature is 550 ℃, the heat preservation time is 3h, and the atmosphere is nitrogen), then placing the blank subjected to glue discharging into air pressure sintering (the temperature is 1750 ℃, the heat preservation time is 4h, and the nitrogen air pressure is 0.6 MPa), then performing hot isostatic pressing (the temperature is 1850 ℃, the heat preservation time is 1h, and the nitrogen pressure is 150 MPa) to obtain a ceramic roller blank, and machining to obtain a ceramic cylindrical roller finished product with the nominal diameter of 15mm and the nominal length of 22mm.
Test example 1
The performance of the layered composite ceramic cylindrical rollers of examples 1 to 3 and the ceramic cylindrical rollers of comparative examples 1 to 2 was tested;
measuring the porosity by adopting an Archimedes drainage method;
adopting an indentation method to measure and calculate Vickers hardness and fracture toughness;
the layered composite ceramic cylindrical rollers described in examples 1 to 3 and the ceramic rollers described in comparative examples 1 to 2 were processed into notched roller test pieces by the notched ball processing method specified in ISO 19843-2018, and the notched roller test pieces were subjected to the strength test, and the test results are shown in table 1:
TABLE 1 test results of the layered composite ceramic cylindrical rollers described in examples 1 to 3 and the ceramic rollers described in comparative examples 1 to 2
The strength of the notched roller sample may indirectly reflect the fatigue strength of the ceramic roller. As can be seen from Table 1, the outer layer of the layered composite ceramic cylindrical roller has higher hardness, the inner layer has higher fracture toughness, and the whole layered composite ceramic cylindrical roller has higher fatigue strength, so that the Hertz stress causing the fatigue failure of the ceramic roller in the rolling contact process is favorably reduced, and the fatigue life and the reliability of the ceramic roller are improved. In addition, the outer layer does not contain a conductive reinforcing phase, so that the electric insulation property is higher, and the anti-corrosion performance of the ceramic roller can be obviously improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The preparation method of the layered composite ceramic cylindrical roller is characterized by comprising the following steps of:
mixing the sintering aid coated silicon nitride material, a binder, a dispersant and water, and carrying out first ball milling to obtain first slurry;
mixing the sintering aid coated silicon nitride material, the reinforcing phase, the binder, the dispersant and water, and performing second ball milling to obtain second slurry;
injecting the first slurry into a cylindrical roller die, performing first standing to obtain an outer layer of a blank, injecting the second slurry, performing second standing to obtain an inner layer of the blank, and sequentially performing demoulding and maintenance to obtain the blank;
sequentially carrying out glue discharging, air pressure sintering and hot isostatic pressing treatment on the green body to obtain the layered composite ceramic cylindrical roller;
the reinforcing phase is one or more of titanium nitride, titanium carbide and tungsten carbide;
the preparation method of the sintering aid coated silicon nitride material comprises the following steps:
mixing silicon nitride, a sintering aid precursor and water to obtain mixed slurry;
carrying out hydrolysis reaction on the mixed slurry under an alkaline condition, and then sequentially drying and calcining to obtain the sintering aid-coated silicon nitride material;
the mass ratio of the silicon nitride to the sintering aid in the sintering aid-coated silicon nitride material is (85-95): 5-15);
the alkaline condition is pH =9 to 11;
the calcining temperature is 500 to 800 ℃, and the heat preservation time is 2 to 4 hours;
the precursor of the sintering aid is soluble metal salt; the soluble metal salt is soluble metal nitrate or soluble metal hydrochloride; the metal in the soluble metal salt is one or more of aluminum, magnesium, yttrium, lanthanum, cerium, neodymium, erbium, ytterbium and lutetium.
2. The preparation method of claim 1, wherein in the first slurry, the mass ratio of the sintering aid coated silicon nitride material to the binder to the dispersant is 100 (0.5 to 3): 0.5 to 3);
the mass solid content of the first slurry is more than or equal to 70%, and the viscosity is less than or equal to 1000 mPa.
3. The preparation method of claim 1, wherein in the second slurry, the mass ratio of the sintering aid coated silicon nitride material to the reinforcing phase is 100 (5-30); the ratio of the mass of the binder to the total mass of the sintering aid-coated silicon nitride material and the reinforcing phase is (0.5-3): 100; the ratio of the mass of the dispersing agent to the total mass of the sintering aid coated silicon nitride material and the reinforcing phase is (0.5-3): 100.
4. The production method according to claim 1 or 3, wherein the second slurry has a mass solid content of 63% or more and a viscosity of 1000 mPas or less.
5. The preparation method according to claim 1, 2 or 3, wherein the binder is one or more of polyethylene glycol, acrylic resin, polyvinyl alcohol and carboxymethyl cellulose;
the dispersant is one or more of polyethyleneimine, ammonium polyacrylate, ammonium citrate and tetramethyl ammonium hydroxide;
the average grain diameter of the reinforcing phase is less than or equal to 3 mu m.
6. The method according to claim 1, wherein the gas used for the gas pressure sintering is nitrogen;
the temperature of the air pressure sintering is 1600 to 1800 ℃, and the time is 2 to 6 hours; the pressure of the nitrogen is 0.6 to 0.9MPa.
7. The method of claim 1, wherein the hot isostatic pressing treatment is performed in a nitrogen atmosphere;
the hot isostatic pressing treatment temperature is 1700-1900 ℃, the time is 1-3h, and the pressure of the nitrogen atmosphere is 100-200MPa.
8. The layered composite ceramic cylindrical roller prepared by the preparation method of any one of claims 1~7.
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| CN108046808A (en) * | 2018-01-05 | 2018-05-18 | 广东工业大学 | A kind of Si3N4Functionally gradient material (FGM) and preparation method thereof |
| CN109942302A (en) * | 2019-03-20 | 2019-06-28 | 广东工业大学 | A kind of boride activeness and quietness silicon nitride ceramics and preparation method thereof |
| CN111825454A (en) * | 2019-08-29 | 2020-10-27 | 宁波伏尔肯科技股份有限公司 | Preparation method of layered structure ceramic ring for mechanical seal |
| CN110698207A (en) * | 2019-11-08 | 2020-01-17 | 陕西科技大学 | Silicon nitride-based layered ceramic composite material and preparation method thereof |
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| CN113135762A (en) * | 2021-05-13 | 2021-07-20 | 中材高新氮化物陶瓷有限公司 | Large-size silicon nitride ceramic ball and preparation method thereof |
| CN113800919A (en) * | 2021-10-26 | 2021-12-17 | 中材高新氮化物陶瓷有限公司 | High-precision silicon nitride ceramic microsphere and preparation method and application thereof |
| CN113880592A (en) * | 2021-11-08 | 2022-01-04 | 北京理工大学 | Preparation process of high-hardness high-toughness silicon nitride ceramic complex structural member |
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Effective date of registration: 20231208 Address after: No. 122 Yumin Road, High tech Zone, Zibo City, Shandong Province, 255035 Patentee after: Zhongcai Precision Bearing Co.,Ltd. Address before: 255000 No.9, North Road, development zone, high tech Zone, Zibo City, Shandong Province Patentee before: SINOMA ADVANCED NITRIDE CERAMICS Co.,Ltd. |