CN111606717A - Preparation method of high-strength and high-hardness silicon nitride wear-resistant sheet - Google Patents
Preparation method of high-strength and high-hardness silicon nitride wear-resistant sheet Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-strength high-hardness silicon nitride wear-resistant sheet, which is prepared by mixing silicon nitride (Si)3N4) Mixing titanium carbonitride (TiCN) and a sintering aid, stirring and grinding to obtain silicon nitride formula powder, carrying out dry pressing on the silicon nitride formula powder to obtain a silicon nitride wear-resistant sheet molding blank, and carrying out plastic packaging and cold isostatic pressing on the silicon nitride wear-resistant sheet molding blank to obtain a wear-resistant sheet blank; sintering the wear-resistant sheet blank in an inert or reducing atmosphere with the gas pressure of 1-10MPa to obtain a wear-resistant sheet finished product blank; and carrying out vibration grinding polishing and washing on the obtained wear-resistant plate finished product blank in water to finally obtain the silicon nitride wear-resistant plate. Compared with the prior art, the silicon nitride wear-resistant plate prepared by optimizing the formula and the process parameters has the advantages of good wear resistance, uniform size, high yield and the like, and is widely applied to steelWear-resistant paster on the surface of pipelines and storage bins of factories, ports and mining machinery.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a preparation method of a high-strength high-hardness silicon nitride wear-resistant sheet.
Background
Silicon nitride ceramics are special ceramic materials with optimal comprehensive properties, and the silicon nitride has high strength, high hardness, high fracture toughness, good thermal shock resistance and low friction coefficient, and is widely applied to a plurality of fields of photovoltaics, automobiles, metallurgy, chemical industry, energy, environmental protection, aerospace and the like.
The wear-resistant ceramic material commonly used at present is alumina Al2O3Ceramics, aluminium oxide Al2O3The ceramic has good insulating property, chemical stability, mechanical property and low price. Si3N4Ceramic and Al2O3Ceramics have irreplaceable advantages over ceramics. Si3N4The bending strength of the ceramic is as high as 600-1000MPa, while Al2O3The flexural strength of the ceramic is about 300MPa, so that Si3N4The bending strength of the ceramic is Al2O3The bending strength of the ceramic is more than twice that of the ceramic, and the impact resistance is better; si3N4The density of the ceramic was 3.2g/cm3Specific to Al2O3Density of ceramic (3.64 g/cm)3) Smaller, silicon nitride abrasion resistant patches can be thinner and lighter under the same conditions. Si3N4Ceramic phase to Al2O3The ceramic has smaller thermal expansion coefficient and better thermal shock resistance. Silicon nitride Si3N4Compared with alumina ceramics, the ceramic has obvious advantages in the aspects of strength, toughness, thermal expansion coefficient, thermal shock resistance, wear resistance, corrosion resistance and the like, and can be widely applied to wear-resistant patches on the surfaces of pipelines and storage bins of steel plants, ports and mining machinery.
Chinese patent CN109467441A discloses a biomedical silicon nitride composition and a preparation method of silicon nitride ceramics, relating to the field of orthopedic biomedical ceramics. The method comprises the steps of providing a biomedical silicon nitride composition, wherein the biomedical silicon nitride composition comprises 70-98% by weight of silicon nitride and 2-30% by weight of additives, and the additives are at least two of magnesium oxide, yttrium oxide, aluminum oxide, ytterbium oxide, strontium oxide, cerium oxide, titanium carbide and boron nitride; molding the biomedical silicon nitride composition to obtain a part to be sintered; sintering the to-be-sintered part to obtain a sintered part; and carrying out post-treatment on the sintered part to obtain the biomedical silicon nitride ceramic part. By adding 2-30 wt% of additive into the silicon nitride ceramic powder, various properties of the obtained silicon nitride ceramic product can be improved, and the silicon nitride ceramic powder is more suitable for clinical requirements of orthopedic implants. According to the scheme, the raw materials are subjected to ball milling treatment and then granulated by using a spray granulator, and the silicon nitride mixture with uniform particle size distribution can be obtained by adopting the method, but in the spray granulation process, the uniformity of the particle size of the silicon nitride mixture is greatly influenced by granulation temperature, pressure, feeding speed and stirring time.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a high-strength and high-hardness silicon nitride wear-resistant sheet.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-strength high-hardness silicon nitride wear-resistant sheet mainly comprises the following steps
The method comprises the following steps:
the method comprises the following steps: silicon nitride (Si)3N4) Mixing and grinding titanium carbonitride (TiCN) and a sintering aid in a stirring mill by taking zirconia balls and absolute ethyl alcohol as grinding media, drying and sieving to obtain silicon nitride formula powder, carrying out dry pressing on the silicon nitride formula powder to obtain a silicon nitride wear-resistant sheet molding blank, and carrying out plastic packaging and cold isostatic pressing treatment on the silicon nitride molding blank to obtain a wear-resistant sheet blank;
step two: sintering the wear-resistant sheet blank obtained in the step one in an inert or reducing atmosphere with the gas pressure of 1-10MPa to obtain a wear-resistant sheet finished product blank;
step three: and D, performing vibration grinding polishing washing on the wear-resistant plate finished product blank obtained in the step two in water to finally obtain the silicon nitride wear-resistant plate.
In the above method for preparing high-strength and high-hardness silicon nitride wear-resistant plate, step one is to obtain silicon nitride (Si)3N4) Titanium carbonitride (TiCN) and a sintering aid are prepared from the following components in parts by weight: silicon nitride (Si)3N4)88-93 parts, 1-3 parts of titanium carbonitride (TiCN) and 6-9 parts of sintering aid.
In the above method for preparing high-strength and high-hardness silicon nitride wear-resistant plate, step one is to obtain silicon nitride (Si)3N4) Mixing titanium carbonitride (TiCN) and sintering aid in a grinder, stirring and grinding for 24-60 hours until the components are uniform, and the particle size is less than 1 micron.
In the preparation method of the high-strength and high-hardness silicon nitride wear-resistant sheet, the dry pressing process in the step one is to pressurize the formula powder in a steel die to 2-10MPa according to a dry pressing pressure curve, and maintain the pressure for 1-10S to prepare a silicon nitride wear-resistant sheet molding blank.
In the preparation method of the high-strength and high-hardness silicon nitride wear-resistant sheet, the dry-pressing forming pressure curve is pressurized to 2-10MPa at the rate of 0.4-2 MPa/S.
In the preparation method of the high-strength and high-hardness silicon nitride wear-resistant sheet, the cold isostatic pressing process in the step one is to place the molded blank body in water after being molded, pressurize to 90-150MPa according to a cold isostatic pressing curve, and maintain the pressure for 30-90S.
In the preparation method of the high-strength and high-hardness silicon nitride wear-resistant sheet, the cold isostatic pressing curve is pressurized to 90-150MPa at the rate of 0.4-2 MPa/S.
In the preparation method of the high-strength and high-hardness silicon nitride wear-resistant plate, the sintering process in the second step is carried out in an inert or reducing atmosphere with the gas pressure of 1-10MPa, the sintering temperature is 1650-1800 ℃ and the sintering time is 2-4 hours.
In the above method for preparing a high-strength and high-hardness silicon nitride wear resistant sheet, the sintering aid is yttrium oxide (Y)2O3) And magnesium oxide (MgO), wherein yttrium oxide (Y)2O3)1-2 parts; 5-7 parts of magnesium oxide (MgO).
In the above method for preparing a high-strength and high-hardness silicon nitride wear resistant sheet, the sintering aid is yttrium oxide (Y)2O3) And cerium oxide (CeO)2) Composition of, wherein yttrium oxide (Y)2O3)2-3 parts of a solvent; cerium oxide (CeO)2)4-6 parts.
Compared with the prior art, the invention has the advantages that:
1. the invention designs a preparation method of a high-strength and high-hardness silicon nitride wear-resistant sheet, and the prepared silicon nitride wear-resistant sheet has the advantages of good wear resistance, uniform size, high yield and the like compared with the existing silicon nitride wear-resistant sheet by optimizing a formula and process parameters.
2. The silicon nitride wear-resistant sheet prepared by the invention has the advantages of high strength, good toughness, good impact resistance and wear resistance, clean surface and complete edges and corners, and can be used as a wear-resistant paster on the surfaces of pipelines and bins of steel plants, ports and mining machinery without reprocessing.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the present invention.
The invention will be explained in more detail below with reference to specific examples:
the first embodiment is as follows:
a preparation method of a high-strength high-hardness silicon nitride wear-resistant sheet mainly comprises the following steps:
the method comprises the following steps: 88 parts of silicon nitride (Si)3N4) 3 parts of titanium carbonitride (TiCN), 2 parts of yttrium oxide (Y)2O3) And 7 parts of magnesium oxide (MgO) are mixed and ground in a grinder by taking zirconia balls and absolute ethyl alcohol as grinding media, the mixture is stirred for 24 hours until the components are uniform, the particle size is less than 1 micron, and silicon nitride formula powder is obtained by drying and sieving, wherein yttrium oxide (Y) is2O3) And magnesium oxide (MgO) is used as a sintering aid, the silicon nitride formula powder is pressurized to 2MPa at the speed of 0.4MPa/S according to a dry-pressing molding pressure curve in a steel die, the pressure is maintained for 10S to prepare a silicon nitride wear-resistant sheet molding blank, the obtained molding blank is placed in water after being molded, the pressure is increased to 90MPa at the speed of 0.4MPa/S according to a cold isostatic pressure curve, and the pressure is maintained for 90S to obtain a wear-resistant sheet blank;
step two: sintering the wear-resistant sheet blank obtained in the step one for 4 hours at the temperature of 1650 ℃ in 1MPa high-purity nitrogen to obtain a wear-resistant sheet finished product blank, wherein the purity of the high-purity nitrogen is more than or equal to 99.999 percent;
step three: and D, performing vibration grinding polishing washing on the wear-resistant plate finished product blank obtained in the step two in water to finally obtain the silicon nitride wear-resistant plate.
Example two:
a preparation method of a high-strength high-hardness silicon nitride wear-resistant sheet mainly comprises the following steps:
the method comprises the following steps: 93 parts of silicon nitride (Si)3N4)1 part of titanium carbonitride (TiCN), 1 part of yttrium oxide (Y)2O3) And 5 parts of magnesium oxide (MgO) are mixed and ground in a grinder by taking zirconia balls and absolute ethyl alcohol as grinding media, the mixture is stirred for 60 hours until the components are uniform, the particle size is less than 1 micron, and silicon nitride formula powder is obtained by drying and sieving, wherein yttrium oxide (Y) is2O3) And magnesium oxide (MgO) is used as a sintering aid, the silicon nitride formula powder is pressurized to 10MPa at the speed of 2MPa/S according to a dry-pressing molding pressure curve in a steel die, the pressure is maintained for 1S to prepare a silicon nitride wear-resistant sheet molding blank, the obtained molding blank is placed in water after being molded, the pressure is increased to 150MPa at the speed of 2MPa/S according to a cold isostatic pressing curve, and the pressure is maintained for 30S to obtain a wear-resistant sheet blank;
step two: sintering the wear-resistant sheet blank obtained in the step one in 5Mpa high-purity nitrogen for 2 hours at the temperature of 1800 ℃ to obtain a wear-resistant sheet finished product blank, wherein the purity of the high-purity nitrogen is more than or equal to 99.999%;
step three: and D, performing vibration grinding polishing washing on the wear-resistant plate finished product blank obtained in the step two in water to finally obtain the silicon nitride wear-resistant plate.
Example three:
a preparation method of a high-strength high-hardness silicon nitride wear-resistant sheet mainly comprises the following steps:
the method comprises the following steps: 88 parts of silicon nitride (Si)3N4) 3 parts of titanium carbonitride (TiCN), 3 parts of yttrium oxide (Y)2O3) And 6 parts of cerium oxide (CeO)2) Mixing and grinding zirconia balls and absolute ethyl alcohol serving as grinding media in a grinder, stirring for 24 hours until the components are uniform, and obtaining silicon nitride formula powder after drying and sieving, wherein yttrium oxide (Y) is2O3) And cerium oxide (CeO)2) The silicon nitride formula powder is used as a sintering aid, the silicon nitride formula powder is pressurized to 2MPa at the speed of 0.4MPa/S in a steel die according to a dry pressing forming pressure curve, the pressure is maintained for 10S to prepare a silicon nitride wear-resistant sheet forming blank body, the obtained forming blank body is placed in water after being molded, the pressure is pressurized to 90MPa at the speed of 0.4MPa/S according to a cold isostatic pressing curve, and the pressure is maintained for 90S to obtain a wear-resistant sheet blank body;
step two: sintering the wear-resistant sheet blank obtained in the step one for 4 hours at 1650 ℃ in 5MPa high-purity nitrogen to obtain a wear-resistant sheet finished product blank, wherein the purity of the high-purity nitrogen is more than or equal to 99.999 percent;
step three: and D, performing vibration grinding polishing washing on the wear-resistant plate finished product blank obtained in the step two in water to finally obtain the silicon nitride wear-resistant plate.
Example four:
a preparation method of a high-strength high-hardness silicon nitride wear-resistant sheet mainly comprises the following steps:
the method comprises the following steps: 93 parts of silicon nitride (Si)3N4)1 part of titanium carbonitride (TiCN), 2 parts of yttrium oxide (Y)2O3) And 4 parts of cerium oxide (CeO)2) Mixing and grinding zirconia balls and absolute ethyl alcohol serving as grinding media in a grinder, stirring for 60 hours until the components are uniform, and obtaining silicon nitride formula powder after drying and sieving, wherein yttrium oxide (Y) is2O3) And cerium oxide (CeO)2) The silicon nitride formula powder is used as a sintering aid, the silicon nitride formula powder is pressurized to 10MPa at the speed of 2MPa/S in a steel die according to a dry pressing forming pressure curve, the pressure is maintained for 1S to prepare a silicon nitride wear-resistant sheet forming blank body, the obtained forming blank body is placed in water after being molded and sealed, the pressure is pressurized to 150MPa at the speed of 2MPa/S according to a cold isostatic pressing curve, and the pressure is maintained for 30S to obtain a wear-resistant sheet blank body;
step two: sintering the wear-resistant sheet blank obtained in the step one in high-purity nitrogen of 10MPa at the temperature of 1800 ℃ for 2 hours to obtain a wear-resistant sheet finished product blank, wherein the purity of the high-purity nitrogen is more than or equal to 99.999 percent;
step three: and D, performing vibration grinding polishing washing on the wear-resistant plate finished product blank obtained in the step two in water to finally obtain the silicon nitride wear-resistant plate.
The sintering process in the preparation method can be carried out in high-purity nitrogen, or can be carried out in inert gas such as argon or reducing atmosphere such as hydrogen.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention 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.
Claims (10)
1. A preparation method of a high-strength and high-hardness silicon nitride wear-resistant sheet is characterized by comprising the following steps: the preparation method of the high-strength and high-hardness silicon nitride wear-resistant sheet mainly comprises the following steps:
the method comprises the following steps: silicon nitride (Si)3N4) Mixing and grinding titanium carbonitride (TiCN) and a sintering aid in a stirring mill by taking zirconia balls and absolute ethyl alcohol as grinding media, drying and sieving to obtain silicon nitride formula powder, carrying out dry pressing on the silicon nitride formula powder to obtain a silicon nitride wear-resistant sheet molding blank, and carrying out plastic packaging and cold isostatic pressing treatment on the silicon nitride molding blank to obtain a wear-resistant sheet blank;
step two: sintering the wear-resistant sheet blank obtained in the step one in an inert or reducing atmosphere with the gas pressure of 1-10MPa to obtain a wear-resistant sheet finished product blank;
step three: and D, performing vibration grinding polishing washing on the wear-resistant plate finished product blank obtained in the step two in water to finally obtain the silicon nitride wear-resistant plate.
2. The method for preparing the high-strength and high-hardness silicon nitride wear-resistant sheet according to claim 1, wherein the method comprises the following steps: step one of said silicon nitride (Si)3N4) Titanium carbonitride (TiCN) and sintering aid are composed ofThe preparation comprises the following components in parts by weight: silicon nitride (Si)3N4)88-93 parts, 1-3 parts of titanium carbonitride (TiCN) and 6-9 parts of sintering aid.
3. The method for preparing a high-strength and high-hardness silicon nitride abrasion-resistant sheet according to claim 1 or 2, wherein: step one of said silicon nitride (Si)3N4) Mixing titanium carbonitride (TiCN) and sintering aid in a grinder, and stirring for 24-60 hours until the components are uniform, wherein the grain diameter of the grains is less than 1 micron.
4. The method for preparing the high-strength and high-hardness silicon nitride wear-resistant sheet according to claim 1, wherein the method comprises the following steps: and step one, the dry pressing forming process is to pressurize the formula powder in a steel die to 2-10MPa according to a dry pressing forming pressure curve, and maintain the pressure for 1-10S to obtain a silicon nitride forming blank.
5. The method for preparing the high-strength and high-hardness silicon nitride wear-resistant sheet according to claim 4, wherein the method comprises the following steps: the dry pressing pressure curve is pressurized to 2-10MPa at a rate of 0.4-2 MPa/S.
6. The method for preparing the high-strength and high-hardness silicon nitride wear-resistant sheet according to claim 1, wherein the method comprises the following steps: and the cold isostatic pressing process in the step one is to place the molded blank body in water after plastic packaging, pressurize to 90-150MPa according to a cold isostatic pressing curve, and maintain the pressure for 30-90S.
7. The method for preparing the high-strength and high-hardness silicon nitride wear-resistant sheet according to claim 6, wherein the method comprises the following steps: the cold isostatic pressure curve is pressurized to 90-150MPa at a rate of 0.4-2 MPa/S.
8. The method for preparing the high-strength and high-hardness silicon nitride wear-resistant sheet according to claim 1, wherein the method comprises the following steps: the sintering process in the second step is carried out in an inert or reducing atmosphere with the gas pressure of 1-10MPa, the sintering temperature is 1650-1800 ℃, and the sintering time is 2-4 hours.
9. The method for preparing a high-strength and high-hardness silicon nitride abrasion-resistant sheet according to claim 1 or 2, wherein: the sintering aid is formed by yttrium oxide (Y)2O3) And magnesium oxide (MgO), wherein yttrium oxide (Y)2O3)1-2 parts; 5-7 parts of magnesium oxide (MgO).
10. The method for preparing a high-strength and high-hardness silicon nitride abrasion-resistant sheet according to claim 1 or 2, wherein: the sintering aid is formed by yttrium oxide (Y)2O3) And cerium oxide (CeO)2) Composition of, wherein yttrium oxide (Y)2O3)2-3 parts of a solvent; cerium oxide (CeO)2)4-6 parts.
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