CN113620715A - Preparation method of high-toughness high-lubrication silicon nitride ceramic skate - Google Patents
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- A—HUMAN NECESSITIES
- A63—SPORTS; GAMES; AMUSEMENTS
- A63C—SKATES; SKIS; ROLLER SKATES; DESIGN OR LAYOUT OF COURTS, RINKS OR THE LIKE
- A63C1/00—Skates
- A63C1/30—Skates with special blades
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/00—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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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention discloses a preparation method of a high-toughness high-lubrication silicon nitride ceramic skate, which comprises the following components in parts by weight: a-Si3N469-85.5 parts of powder and Lu2O3‑Al2O34-10 parts of MgO, 10-20 parts of yttrium-stabilized zirconia powder and 0.5-1.5 parts of graphene; firstly, weighing raw materials, mixing the raw materials, putting the raw materials into a ball milling tank, and grinding the raw materials into slurry; secondly, placing the slurry in an oven for drying, crushing, grinding and sieving to obtain mixed powder; thirdly, dry-pressing and molding the mixed powder, and then carrying out cold isostatic pressing treatment at the pressure of 200 and 300MPa to obtain a blank body; fourthly, the green body is put into a crucibleHeating to 500-1000 ℃ in an inert atmosphere, and carrying out heat preservation and pre-sintering; filling nitrogen into the crucible, heating to 1700-1900 ℃, preserving heat for air pressure sintering, cooling to 1200 ℃ after the sixth sintering is finished, and then cooling to room temperature along with the furnace; and seventhly, processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate. The silicon nitride ceramic material prepared by the invention has the bending strength of 1000MPa, the fracture toughness of 10MPa.ml/2, the friction coefficient and the wear resistance lubricity are obviously improved, and the silicon nitride ceramic material is suitable for manufacturing silicon nitride ceramic skates.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a preparation method of a high-toughness high-lubrication silicon nitride ceramic skate.
Background
In skating sports, the most important factor of the competitive level is the service performance of the ice skate besides the personal skill of athletes, such as transmission capability, plastic deformation resistance, brittle fracture resistance, long-time wear resistance and the like of pedaling force, the physical property and the mechanical property of the blade in the mechanical structure of the ice skate are one of the main factors determining the quality level of the ice skate, and the factors relate to the overall strength of the blade, the hardness of the blade edge, the surface roughness of an ice-contacting surface and the like, and the existing ceramic material is difficult to meet the requirements of high strength and high lubrication.
In the patent of a silicon nitride ceramic material with high thermal conductivity and high strength and a preparation method thereof, Shanghai silicate research institute, Zengyuping and Wang is to take a rare earth metal simple substance and an alkaline earth metal oxide as sintering aids, and reduce defects in a silicon nitride crystal lattice and reduce scattering of phonons by regulating and controlling liquid phase composition, thereby improving the thermal conductivity. The thermal conductivity of the prepared silicon nitride ceramic material can reach more than 125.7W/(m.K), the bending strength can be improved (up to 985MPa), the fracture toughness can be improved (up to 9.86MPa.ml/2), and the application requirements of the silicon nitride ceramic in the fields of high-density and high-power semiconductor devices and high-power electronic and electric devices can be met.
The wide application of the technology in the patent "research on the preparation process of zirconia-reinforced silicon nitride ceramics" is that silicon nitride is used as a base, 15-40% of yttrium-stabilized zirconia powder, alumina powder and talcum powder are added, the raw materials are put into a ball mill for ball milling and mixing, and are subjected to isostatic pressing after being sieved and aged for a certain time, and then the blank after being fettled is sintered under the conditions of high temperature and high purity nitrogen to form a zirconia-reinforced silicon nitride ceramic blank.
In the patent 'a preparation method of a high-strength wear-resistant titanium alloy' of Sian traffic university Liu Ma Bao, Liang and the like, titanium-based powder and high-purity graphite balls are simultaneously added into a three-dimensional vibration powder mixer to carry out three-dimensional vibration powder mixing; performing discharge plasma activation and densification sintering on the powder after three-dimensional vibration powder mixing; the preparation of the high-strength wear-resistant titanium alloy is completed through the steps. The prepared high-strength wear-resistant titanium alloy has a continuous three-dimensional graphene space network structure inside, so that the strength and the wear resistance of the titanium alloy are greatly improved. The hardness reaches more than 472HV, the yield strength reaches more than 1264MPa, and the compressive strength reaches more than 1651 MPa.
The Fujian institute of engineering can bin, Wanqiangting et al in the patent "a high-hardness high wear-resisting titanium alloy machine preparation method and application" further alloy elements such as Pd, Au, Ag, Rh, etc. on the basis of Ti, Pt binary alloy, can obviously improve the alloy hardness, because the selected alloying element has higher chemical stability, therefore can improve corrosion resistance and biocompatibility of the alloy; moreover, the main crystal phase of the alloy is Ti3Pt intermetallic compound, the microhardness value of the alloy is more than 700HV and is much higher than that of pure titanium, namely the traditional medical titanium alloy, and the problem of poor wear resistance can be effectively relieved; in addition, Pt, Pd, Au, Ag, Rh and the like are precious metal elements, have high chemical stability and high corrosion resistance in a physiological environment, and can effectively reduce ion precipitation and reduce biotoxicity.
The hardness of the titanium alloy of the ice skate blade material is more than 400-700HV, the hardness of the ceramic material is generally more than 1000HV, and the ceramic has outstanding advantages in wear resistance. The performance of the existing ceramic material is mainly improved in the aspects of heat conductivity and bending strength, the toughness and the lubricity can not meet the use requirement of the ice skate temporarily, the strength is mostly below 1000MPa, and the strength of the material required by the movement of the ice skate can not be achieved.
The invention aims to meet the requirements of high strength, high toughness, high lubrication, no abrasion and the like of the silicon nitride ceramic ice skate, and aims to develop the silicon nitride ceramic ice skate with high toughness and high lubrication.
Disclosure of Invention
The invention solves the defects of the prior art and provides a preparation method of a high-strength, high-toughness and high-lubrication silicon nitride ceramic skate blade.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a high-toughness high-lubrication silicon nitride ceramic skate comprises the following components in parts by weight: a-Si3N469-85.5 parts of powder and Lu2O3-Al2O3-4-10 parts of MgO, 10-20 parts of yttrium-stabilized zirconia powder and 0.5-1.5 parts of graphene;
weighing raw materials in proportion, mixing, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, placing in a nylon ball milling tank, placing in a silicon nitride grinding ball, and grinding by using a planetary ball mill to obtain slurry;
step two, drying the slurry in an oven at 60-80 ℃ for 4-6h, crushing and grinding the dried powder, and sieving the powder through a 100-140-mesh standard sieve to obtain uniformly mixed powder;
step three, dry-pressing the mixed powder under the pressure of 5-20MPa, and then carrying out cold isostatic pressing treatment under the pressure of 200-300MPa to obtain a blank;
step four, placing the blank into a platinum crucible, raising the temperature to 500-1000 ℃ at the heating rate of 2-5 ℃/min under the inert atmosphere, and preserving the heat for 4-6h for pre-sintering;
step five, filling nitrogen into the platinum crucible to ensure that the pressure of the nitrogen is 2-7MPa, raising the temperature to 1700-1900 ℃ at the speed of 10 ℃/min, preserving the heat for 4h, and carrying out air pressure sintering;
step six, after sintering, cooling to 1200 ℃ at a cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace;
and step seven, processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
And the temperature of the oven in the second step is 70 ℃ by way of limitation, and the drying time is 5 h.
As another limitation, the mesh number of the standard sieve in the second step is 120 meshes.
As another limitation, the dry-pressing pressure in the third step is 10-15MPa, and the cold isostatic pressing pressure is 240-260 MPa.
As another limitation, the inert atmosphere of step four is an Ar inert atmosphere.
As another limitation, the nitrogen pressure in step five is 4-5 MPa.
As another limitation, the insulation temperature in step five is 1800 ℃.
Compared with the prior art, the invention has the technical progress that:
(1) al in the composite sintering aid2O3Is favorable for dissolving silicon nitride particles, MgO is a sintering aid with low melting point, is favorable for reducing the sintering temperature of silicon nitride, and improves the compactness, Lu2O3The ceramic material is beneficial to improving the strength of a ceramic crystal boundary, and the surface can be oxidized to form a protective layer in the friction process;
(2) the graphene has good lubricating property, and the addition of the graphene can reduce the friction coefficient and the wear rate of the composite ceramic cutter material, thereby playing the roles of reducing and resisting wear;
in conclusion, the bending strength of the silicon nitride ceramic material prepared by the invention can reach more than 1000MPa, the fracture toughness can reach more than 10MPa.ml/2, the friction coefficient and the wear resistance lubricity are also obviously improved, and the silicon nitride ceramic material is suitable for manufacturing silicon nitride ceramic skates.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a process diagram of the preparation of the silicon nitride ceramic ice skate blade of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the present invention.
The silicon nitride ceramic material prepared by the invention adopts Rtec friction and wear testing machine to carry out friction and wear test on the silicon nitride ceramic material by people such as Lisonghua, Lishuang, Shenyang building university, and the like, and uses a 3D laser microscope to measure the wear appearance and the wear depth; developing a Umeshmeshment user subprogram for calculating the wear depth based on the corrected Archard model, and providing a wear process simulation method based on the combination of a finite element and the user subprogram; and comparing the test result with the numerical simulation result to determine the wear coefficient of the silicon nitride ceramic.
Shanxu, Shanxi university of science and technology utilizes vertical universal friction wear testing machine to study the tribology performance of silicon nitride ceramic round pin sample and austenitic stainless steel dish under different humidity, adopts the joining in marriage vice mode of selling the lower wall. A silicon nitride pin sample is fixed on a rotating shaft by adopting a clamp, a stainless steel disc sample is fixed on a base, the pin sample is contacted with the end face of the disc sample under the action of pressure, and the rotation of the shaft causes the sliding friction between the upper sample and the lower sample. All rubbing tests were carried out at room temperature with relative humidities of 30%, 60%, 90%, respectively. All the measurement results can be displayed on a computer screen in real time, and simultaneously, a test curve is recorded and stored, and friction factor analysis and wear rate calculation are carried out on the test curve.
Example 1
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 4 parts of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 10 parts of yttrium-stabilized zirconia powder as reinforcing phase, 0.5 part of graphene as lubricating material, and 85.5 parts of a-Si3N4Mixing the powders, adding polyvinylpyridineThe pyrrolidone, the isopropanol and the absolute ethyl alcohol are ground into slurry by ball milling.
(2) And (3) drying the slurry in an oven at 70 ℃ for 5h, crushing and grinding the dried powder, and sieving the powder by a 120-mesh standard sieve to obtain uniformly mixed powder.
(3) And (3) dry-pressing and molding the mixed powder under the pressure of 20MPa, and then carrying out cold isostatic pressing treatment under the pressure of 250MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 700 ℃ at the speed of 5 ℃/min under the Ar atmosphere, and preserving the heat at 700 ℃ for 5h for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible, so that the nitrogen pressure is 2MPa, heating to 1800 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering, wherein the heat preservation time is 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
Example 2
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 4 parts of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 10 parts of yttrium-stabilized zirconia powder as reinforcing phase, 1 part of graphene as lubricating material, and 85 parts of a-Si3N4Mixing the powder, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, and grinding by ball milling to obtain slurry.
(2) And (3) drying the slurry in a 60 ℃ oven for 6h, crushing and grinding the dried powder, and sieving the powder with a 100-mesh standard sieve to obtain uniformly mixed powder.
(3) And (3) dry-pressing and molding the mixed powder under the pressure of 5MPa, and then carrying out cold isostatic pressing treatment under the pressure of 240MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 600 ℃ at the speed of 2 ℃/min under the Ar atmosphere, and preserving the heat at 600 ℃ for 5h for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible, so that the nitrogen pressure is 3MPa, heating to 1900 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering, wherein the heat preservation time is 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
Example 3
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 5 parts of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 15 parts of yttrium-stabilized zirconia powder as reinforcing phase, 1 part of graphene as lubricating material, 79 parts of a-Si3N4Mixing the powder, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, and grinding by ball milling to obtain slurry.
(2) And (3) drying the slurry in a 60 ℃ oven for 6h, crushing and grinding the dried powder, and sieving the powder with a 100-mesh standard sieve to obtain uniformly mixed powder.
(3) And (3) dry-pressing the mixed powder under the pressure of 10MPa for forming, and then carrying out cold isostatic pressing treatment under the pressure of 260MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 500 ℃ at the heating rate of 2 ℃/min under the Ar atmosphere, and preserving the heat at 500 ℃ for 6h for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible to ensure that the nitrogen pressure is 4MPa, heating to 1900 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering for 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
Example 4
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 5 parts of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 15 parts of yttrium stable oxygenZirconium powder as reinforcing phase, 1.5 parts of graphene as lubricating material, and 78.5 parts of a-Si3N4Mixing the powder, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, and grinding by ball milling to obtain slurry.
(2) And (3) drying the slurry in an oven at 70 ℃ for 5h, crushing and grinding the dried powder, and sieving the powder by a 120-mesh standard sieve to obtain uniformly mixed powder.
(3) And (3) dry-pressing and molding the mixed powder under the pressure of 15MPa, and then carrying out cold isostatic pressing treatment under the pressure of 200MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 700 ℃ at the speed of 5 ℃/min under the Ar atmosphere, and preserving the heat at 700 ℃ for 5h for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible to ensure that the nitrogen pressure is 3.5MPa, heating to 1800 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering, wherein the heat preservation time is 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
Example 5
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 6 portions of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 15 parts of yttrium-stabilized zirconia powder as reinforcing phase, 1 part of graphene as lubricating material, 78 parts of a-Si3N4Mixing the powder, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, and grinding by ball milling to obtain slurry.
(2) And (3) drying the slurry in an oven at 80 ℃ for 4h, crushing and grinding the dried powder, and sieving the powder through a standard sieve of 140 meshes to obtain uniformly mixed powder.
(3) And (3) dry-pressing and molding the mixed powder under the pressure of 18MPa, and then carrying out cold isostatic pressing treatment under the pressure of 270MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 1000 ℃ at the speed of 4 ℃/min under the Ar atmosphere, and preserving the heat at 1000 ℃ for 4h for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible, so that the nitrogen pressure is 5MPa, heating to 1700 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering, wherein the heat preservation time is 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
Example 6
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 7 parts of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 20 parts of yttrium-stabilized zirconia powder as reinforcing agent, 1 part of graphene as lubricating material, and 72 parts of a-Si3N4Mixing the powder, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, and grinding by ball milling to obtain slurry.
(2) And (3) drying the slurry in an oven at 80 ℃ for 4h, crushing and grinding the dried powder, and sieving the powder through a standard sieve of 140 meshes to obtain uniformly mixed powder.
(3) And (3) dry-pressing and molding the mixed powder under the pressure of 9MPa, and then carrying out cold isostatic pressing treatment under the pressure of 280MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 900 ℃ at the speed of 4 ℃/min under the Ar atmosphere, and preserving the heat at 900 ℃ for 4h for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible to ensure that the nitrogen pressure is 4.5MPa, heating to 1700 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering, wherein the heat preservation time is 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
Example 7
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 8 portions of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 20 parts of yttrium-stabilized zirconia powder as reinforcing phase, 1 part of graphene as lubricating material, and 71 parts of a-Si3N4Mixing the powder, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, and grinding by ball milling to obtain slurry.
(2) And (3) drying the slurry in an oven at 70 ℃ for 5h, crushing and grinding the dried powder, and sieving the powder by a 120-mesh standard sieve to obtain uniformly mixed powder.
(3) And (3) dry-pressing and molding the mixed powder under the pressure of 20MPa, and then carrying out cold isostatic pressing treatment under the pressure of 300MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 700 ℃ at the speed of 5 ℃/min under the Ar atmosphere, and preserving the heat at 700 ℃ for 5h for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible, so that the nitrogen pressure is 6MPa, heating to 1800 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering, wherein the heat preservation time is 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
Example 8
Preparation method of high-toughness high-lubrication silicon nitride ceramic skate
(1) In 10 parts of Lu2O3-Al2O3-MgO composite sintering aid as sintering aid, 20 parts of yttrium-stabilized zirconia powder as reinforcing phase, 1 part of graphene as lubricating material, and 69 parts of a-Si3N4Mixing the powder, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, and grinding by ball milling to obtain slurry.
(2) And (3) drying the slurry in a 75 ℃ oven for 5h, crushing and grinding the dried powder, and sieving the powder through a 120-mesh standard sieve to obtain uniformly mixed powder.
(3) And (3) dry-pressing and molding the mixed powder under the pressure of 13MPa, and then carrying out cold isostatic pressing treatment under the pressure of 220MPa to obtain a blank.
(4) And (3) putting the blank into a platinum crucible, heating to 800 ℃ at the speed of 3 ℃/min under the Ar atmosphere, and preserving the temperature for 5h at 800 ℃ for presintering treatment.
(5) And (3) filling nitrogen into the platinum crucible, so that the nitrogen pressure is 7MPa, heating to 1800 ℃ at the speed of 10 ℃/min, and carrying out air pressure sintering, wherein the heat preservation time is 4h.
(6) After sintering, cooling to 1200 ℃ at the cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace.
(7) And processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
The performance parameters of the present example are shown in Table (1)
TABLE 1
| Sample(s) | Bending strength (MPa) | Fracture toughness (MPa.ml/2) | Coefficient of friction | Hardness (GPa) |
| Example 1 | 996±13 | 9.6±0.27 | 0.65 | 14.2±0.22 |
| Example 2 | 965±27 | 9.5±0.22 | 0.64 | 13.9±0.33 |
| Example 3 | 1006±23 | 9.3±0.16 | 0.56 | 14.0±0.16 |
| Example 4 | 996±33 | 9.3±0.19 | 0.54 | 13.3±0.13 |
| Example 5 | 1116±33 | 11.3±0.22 | 0.45 | 14.0±0.40 |
| Example 6 | 1106±23 | 10.3±0.16 | 0.65 | 13.6±0.23 |
| Example 7 | 966±15 | 9.3±0.13 | 0.69 | 13.5±0.23 |
| Example 8 | 954±13 | 9.1±0.15 | 0.73 | 13.2±0.16 |
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (7)
1. A preparation method of a high-toughness high-lubrication silicon nitride ceramic skate is characterized by comprising the following steps: the composition comprises the following components in parts by weight: a-Si3N469-85.5 parts of powder and Lu2O3-Al2O34-10 parts of MgO, 10-20 parts of yttrium-stabilized zirconia powder and 0.5-1.5 parts of graphene;
weighing raw materials in proportion, mixing, adding polyvinylpyrrolidone, isopropanol and absolute ethyl alcohol, placing in a nylon ball milling tank, placing in a silicon nitride grinding ball, and grinding by using a planetary ball mill to obtain slurry;
step two, drying the slurry in an oven at 60-80 ℃ for 4-6h, crushing and grinding the dried powder, and sieving the powder through a 100-140-mesh standard sieve to obtain uniformly mixed powder;
step three, dry-pressing the mixed powder under the pressure of 5-20MPa, and then carrying out cold isostatic pressing treatment under the pressure of 200-300MPa to obtain a blank;
step four, placing the blank into a platinum crucible, raising the temperature to 500-1000 ℃ at the heating rate of 2-5 ℃/min under the inert atmosphere, and preserving the heat for 4-6h for pre-sintering;
step five, filling nitrogen into the platinum crucible to ensure that the pressure of the nitrogen is 2-7MPa, raising the temperature to 1700-1900 ℃ at the speed of 10 ℃/min, preserving the heat for 4h, and carrying out air pressure sintering;
step six, after sintering, cooling to 1200 ℃ at a cooling rate of 10 ℃/min, and then cooling to room temperature along with the furnace;
and step seven, processing the prepared silicon nitride ceramic material to prepare the silicon nitride ceramic ice skate.
2. The preparation method of the high-toughness high-lubrication silicon nitride ceramic ice skate blade as claimed in claim 1, characterized in that: and in the second step, the temperature of the oven is 70 ℃, and the drying time is 5 hours.
3. The preparation method of the high-toughness high-lubrication silicon nitride ceramic ice skate blade as claimed in claim 1, characterized in that: and in the second step, the mesh number of the standard sieve is 120 meshes.
4. The preparation method of the high-toughness high-lubrication silicon nitride ceramic ice skate blade as claimed in claim 1, characterized in that: in the third step, the dry pressing pressure is 10-15MPa, and the cold isostatic pressing pressure is 240-260 MPa.
5. The preparation method of the high-toughness high-lubrication silicon nitride ceramic ice skate blade as claimed in claim 1, characterized in that: and the inert atmosphere in the fourth step is Ar inert atmosphere.
6. The preparation method of the high-toughness high-lubrication silicon nitride ceramic ice skate blade as claimed in claim 1, characterized in that: and in the fifth step, the nitrogen pressure is 4-5 MPa.
7. The preparation method of the high-toughness high-lubrication silicon nitride ceramic ice skate blade as claimed in claim 1, characterized in that: in the fifth step, the insulation temperature is 1800 ℃.
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