CN111302810A - Low-noise silicon nitride ceramic-based friction material and preparation method and application thereof - Google Patents

Low-noise silicon nitride ceramic-based friction material and preparation method and application thereof Download PDF

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CN111302810A
CN111302810A CN202010157499.2A CN202010157499A CN111302810A CN 111302810 A CN111302810 A CN 111302810A CN 202010157499 A CN202010157499 A CN 202010157499A CN 111302810 A CN111302810 A CN 111302810A
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powder
ceramic
sintering
pressing
friction material
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CN111302810B (en
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曾宇平
尹金伟
左开慧
夏咏锋
姚冬旭
梁汉琴
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention provides a low-noise silicon nitride ceramic-based friction material and a preparation method and application thereof, wherein Si is3N4Ceramic-based friction material, characterized in that it is made of Si3N4Powder, BN powder, β -Si3N4The crystal whisker, the ceramic fiber and the metal oxide powder are used as main raw materials and are prepared by uniformly mixing and sintering, wherein in the raw materials, Si3N445-92% of powder, 2-40% of BN powder and β -Si3N42-10% of whisker, 2-20% of ceramic fiber, 2-15% of metal oxide and β -Si3N4Whisker and ceramic fiberThe mass ratio of the vitamin is 1: (1-10).

Description

Low-noise silicon nitride ceramic-based friction material and preparation method and application thereof
Technical Field
The invention relates to a low-noise Si3N4A ceramic-based friction material, in particular to a friction material containing Si3N4A matrix phase, a BN lubricant phase, and β -Si3N4A friction material of crystal whisker and ceramic fiber reinforced phase, a preparation method and application thereof.
Background
With the development of high-speed vehicles such as airplanes, trains, automobiles and the like, the requirements on the reliability and stability of friction parts are higher and higher, and a lot of friction materials are replaced by novel materials in the continuous development process. Commonly used friction materials include organic materials, metallic materials, ceramic materials, etc., wherein the ceramic friction materials have received much attention in recent years due to their excellent high temperature resistance and low wear properties. However, during use, when ceramic abrasive dust accumulates on the friction surface, abrasive wear is easily formed, and the wear rate of the material is increased; on the other hand, the ceramic material with high hardness and high elastic modulus is easy to generate abnormal sound in the friction process, so that noise pollution is caused, and the comfort level of drivers and passengers is reduced.
Vibration of the friction member, high friction coefficient, high hardness friction surface, high frequency vibration of the abrasive dust particles, and the like are important sources of friction noise. Particularly, under some dry friction conditions, no lubricating medium is involved, the friction force and the friction vibration are severe, and the friction noise is more serious. The currently applied ceramic friction material is prepared by hard ceramics, and the generation of noise cannot be effectively inhibited under the condition of ensuring low abrasion; or the soft inorganic lubricating material and the metal are compounded to form the ceramic semi-metal friction material, so that the wear rate of the material is higher and the mechanical property of the material is lower under the conditions of reducing friction and noise, and the material cannot be used for preparing structural components with bearing or transmission effects.
In conclusion, the development of ceramic friction materials with high mechanical strength and low friction noise is particularly urgent.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide Si3N4The ceramic-based friction material has the advantages of low friction noise, high mechanical property, excellent wear resistance and stable friction coefficient, can meet the use requirements of high wear resistance and long service life of the material, and simultaneously meets the application requirement of low noise.
In a first aspect, the present application provides Si3N4Ceramic-based friction material based on Si3N4Powder, BN powder, β -Si3N4The crystal whisker, the ceramic fiber and the metal oxide powder are used as main raw materials and are prepared by uniformly mixing and sintering, wherein in the raw materials, Si3N445-92% of powder, 2-40% of BN powder and β -Si3N42-10% of whisker, 2-20% of ceramic fiber, 2-15% of metal oxide and β -Si3N4The mass ratio of the crystal whisker to the ceramic fiber is 1: (1-10).
Si as above3N4Ceramic-based friction material, the main component of which is Si3N4Matrix, BN lubricating phase and β -Si3N4The crystal whisker reinforced phase contains a certain amount of metal oxide and a certain amount of ceramic fiber, wherein BN forms a lubricating film in the friction process to reduce abrasion and noise, and improves the density of the internal crystal boundary of the material to improve the sound resistance so as to realize the purpose of reducing the friction noise, and meanwhile, the ceramic fiber is used as the reinforced phase to reduce the reduction of the mechanical property of the material caused by the introduction of BN, and β -Si is used as the auxiliary material3N4The introduction of whiskers realizes isotropic enhancement at a micrometer scale, and ceramic fibers and β -Si3N4The combined action of the whiskers can realize the synergistic action of large-scale fiber reinforcement and micro-scale whisker reinforcement of the material, and the material has better mechanical property and wear resistance than the traditional single fiber or whisker reinforcement mechanism3N4The content of the whisker is designed in a targeted way, and the scientific proportion is limitedSo as to fully play the synergistic strengthening effect of the BN phase and the boron nitride phase and effectively relieve the reduction of the mechanical property of the material caused by the introduction of the BN phase. The material is Si3N4As a base material, it has good self-lubricating properties compared to other materials such as Al2O3、ZrO2SiC, etc., Si3N4The base material can effectively reduce the friction coefficient of the material in the friction process and reduce the friction noise. Si prepared by the invention3N4The ceramic-based friction material has the advantages of low friction noise, high mechanical property, excellent wear resistance and stable friction coefficient, and can be applied to manufacturing wear-resistant structural members such as friction plates, bearings, sealing rings and the like. Si as above3N4The hardness of the ceramic-based friction material can be 1-12 GPa, the elastic modulus can be 45-287 GPa, the abrasion loss is low, and the noise is low.
Preferably, the ceramic fibers are selected from Si3N4、SiC、BN、Al3O4、SiO2One or a combination of several of the fibers.
Preferably, the metal oxide powder is selected from Al2O3、MgO、Y2O3、Sc2O3、Sm2O3、Lu2O3、Er2O3One or a combination of several of them.
Preferably, Si3N4The average particle size of the powder is 0.2-10 μm, the average particle size of the BN powder is 0.05-20 μm, β -Si3N4The average diameter of the crystal whisker is 0.1-5 μm, and the average length is 0.3-20 μm; the average diameter of the ceramic fiber is 0.1-100 μm, and the average length is 100 μm-1 cm; the metal oxide powder has an average particle diameter of 0.1 to 20 μm.
Preferably, the sintering method is hot-pressing sintering, pressureless sintering or air pressure sintering.
In a second aspect, the present application provides a method for preparing any of the ceramic based friction materials described above, comprising the steps of:
a) weighing Si according to the proportion3N4Powder, BN powder, β -Si3N4Whiskers, ceramic fibers andmetal oxide powder;
b) ball milling to uniformly mix the powder to prepare raw material powder;
b) and pouring the raw material powder obtained in the previous step into a mould for hot-pressing sintering, wherein the hot-pressing pressure is 5-50 MPa, the sintering temperature is 1500-1750 ℃, the sintering time is 1-4 hours, and the environment atmosphere is nitrogen.
In a third aspect, the present application provides a method for preparing any of the ceramic based friction materials described above, comprising the steps of:
a) weighing Si according to the proportion3N4Powder, BN powder, β -Si3N4Whiskers, ceramic fibers, and metal oxide powders;
b) ball milling to uniformly mix the powder to prepare raw material powder;
c) pressing and molding the raw material powder obtained in the previous step, and performing cold isostatic pressing treatment to obtain a ceramic blank;
d) and carrying out pressureless sintering on the ceramic blank, wherein the sintering temperature is 1500-1750 ℃, the sintering time is 1-4 hours, and the environment atmosphere is nitrogen.
In a fourth aspect, the present application provides a method for preparing any of the above ceramic based friction materials, comprising the steps of:
a) weighing Si according to the proportion3N4Powder, BN powder, β -Si3N4Whiskers, ceramic fibers, and metal oxide powders;
b) ball milling to uniformly mix the powder to prepare raw material powder;
c) pressing and molding the raw material powder obtained in the previous step, and performing cold isostatic pressing treatment to obtain a ceramic blank;
d) and (3) putting the ceramic blank into a furnace for air pressure sintering, wherein the sintering temperature is 1500-1850 ℃, the sintering time is 1-4 hours, the air pressure is 0.1-10 MPa, and the environment atmosphere is nitrogen.
Preferably, the pressing method is dry pressing, and the dry pressing pressure is 10-100 MPa; the cold isostatic pressure is 50-400 MPa.
In a fifth aspect, the present application provides a wear resistant structural member using any of the aboveSi3N4And (3) preparing the ceramic-based friction material.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
Si according to one embodiment of the present invention3N4Ceramic-based friction material comprising Si3N4Matrix, BN lubricating phase and β -Si3N4A whisker reinforcing phase and a certain content of ceramic fiber. The Si is3N4The ceramic-based friction material may be Si3N4Powder, BN powder, β -Si3N4The crystal whisker, the ceramic fiber and the metal oxide powder are used as main raw materials, and are prepared by uniformly mixing and sintering.
In some embodiments, the feedstock is formed from Si3N4Powder, BN powder, β -Si3N4Whisker, ceramic fiber and metal oxide powder.
Si3N4The powder is used as a matrix raw material, and the mass fraction of the powder can be 45-92%, and preferably 45-65%. Si3N4The average particle size of the powder may be 0.2 to 10 μm, preferably 0.2 to 2 μm.
The mass fraction of the BN powder can be 2-40%. If the mass fraction of the BN powder is lower than 2%, the friction noise is large, and the friction coefficient is unstable; if the mass fraction of the BN powder is higher than 40%, the abrasion amount of the material is high. The mass fraction of the BN powder is preferably 20 to 40% from the viewpoint of noise reduction. The average particle size of the BN powder may be 0.05 to 20 μm, preferably 0.2 to 5 μm.
β-Si3N4The mass fraction of the whiskers can be 2-10%, preferably 4-8%, if β -Si3N4If the mass fraction of the whiskers is less than 2%, the strength of the material is insufficient, and if β -Si is used3N4The mass fraction of the whisker is higher than 10 percent, the material is difficult to densify, and the mechanical property is reduced β -Si3N4The average diameter of the whiskers can be 0.1-5 μm, preferably 0.2-1 μm, and the average length can be 0.3-20 μmPreferably 0.5 to 5 μm, and the average aspect ratio may be 3 to 50, preferably 3 to 10.
The mass fraction of the ceramic fiber can be 2-20%, and if the mass fraction of the ceramic fiber is less than 2%, the material is easy to wear; if the mass fraction of the ceramic fiber is more than 20%, the friction coefficient of the material is unstable, and the material preparation cost is high. Preferably, the mass fraction of the ceramic fiber is 2-15%, more preferably 4-10%, so that the ceramic fiber has high mechanical strength and low friction noise, and the preparation cost is controllable. The ceramic fiber may be Si3N4、SiC、BN、Al3O4、SiO2One or more of the fibers, wherein Si is preferred3N4The fiber is made of the same material as the base material, so that better thermal matching can be realized, and microcracks are not easily generated at the interface due to thermal mismatch. The ceramic fibers may have an average diameter of 0.1 to 100 μm, an average length of 100 μm to 1cm, and an average aspect ratio of 102～106。
β-Si3N4The mass ratio of the crystal whisker to the ceramic fiber is 1: (1-10), when the content is beyond the range, the good synergistic strengthening effect of the two is difficult to realize, the mechanical property of the material is reduced, and the wear resistance is reduced. The mass ratio is preferably 1 (2-5), and within the range, the synergistic strengthening effect is optimal.
The metal oxide powder may be used as a sintering aid, and may be selected from Al, for example2O3、MgO、Y2O3、Sc2O3、Sm2O3、Lu2O3、Er2O3And the like in one or a combination of several. The mass fraction of the metal oxide powder may be 2 to 15%. In some embodiments, the metal oxide powder is Al2O3Powder and Y2O3Powder of Al2O3The mass fraction of the powder in all raw material powder can be 1-10%, and Y is2O3The mass fraction of the powder in all raw material powders can be 1-10%. The average particle diameter of the metal oxide powder may be 0.1 to 20 μm, preferably 0.1 to 5 μm.
The method of mixing the raw materials may be a method commonly used in the art, such as ball milling and the like. During ball milling, the dispersing medium may be absolute ethyl alcohol and the grinding balls may be silicon nitride balls. The mass ratio of the raw material powder, the dispersion medium and the grinding balls can be (1-3): (1-3): (1-3). The ball milling speed can be 50-500 r/min, and the ball milling time can be 1-48 hours. The resulting slurry was dried and sieved to obtain a mixture powder. The drying temperature can be 50-80 ℃. The sieving is, for example, a 100 mesh sieve.
Sintering the mixture powder to obtain Si3N4A ceramic based friction material.
In some embodiments, the sintering is hot press sintering. And filling the mixture powder into a hot-pressing die for hot-pressing sintering to obtain the required ceramic material. The hot pressing pressure can be 5-50 MPa, preferably 20-40 MPa. The sintering temperature can be 1500-1750 ℃, and is preferably 1600-1700 ℃. The temperature rise rate to the sintering temperature can be 5-20 ℃/min. The sintering time can be 1-4 hours. The ambient atmosphere may be nitrogen.
In some embodiments, the sintering mode is pressureless sintering. First, the mixture powder is made into a ceramic body. For example, the ceramic body can be obtained by pressing into a specified shape and then carrying out cold isostatic pressing. The pressing mode can be dry pressing, and the dry pressing pressure can be 10-100 MPa, preferably 20-50 MPa. The cold isostatic pressure may be 50 to 400MPa, preferably 200 to 400 MPa. And then, putting the ceramic blank into a high-temperature furnace for sintering to obtain the required ceramic material. The sintering temperature can be 1500-1750 ℃, and is preferably 1600-1750 ℃. The temperature rise rate to the sintering temperature can be 5-20 ℃/min. The sintering time can be 1-4 hours. The ambient atmosphere may be nitrogen.
In some embodiments, the sintering mode is gas pressure sintering. First, the mixture powder is made into a ceramic body, and the preparation method thereof can be as described above. And then, putting the ceramic blank into a gas pressure sintering furnace for sintering to obtain the required ceramic material. The sintering temperature can be 1500-1850 ℃, and is preferably 1600-1850 ℃. The temperature rise rate to the sintering temperature can be 5-20 ℃/min. The sintering time can be 1-4 hours. The pressure is 0.1 to 10MPa, preferably 0.5 to 5 MPa. The ambient atmosphere may be nitrogen.
Compared with the prior art, the low-noise Si provided by the application3N4Ceramic-based friction material comprising Si3N4Matrix phase, BN lubricating phase, β -Si3N4A whisker-reinforced phase and a ceramic fiber-reinforced phase, which may have Si together3N4Wear resistance of ceramics, lubrication of BN β -Si3N4The crystal whisker and the ceramic fiber have double reinforcing effects, have the characteristics of high mechanical property, good wear resistance, low friction noise and stable friction coefficient, and the BN lubricating phase in the system can obviously improve the wear resistance and stability of the friction part under the dry friction condition, reduce noise pollution and have very high practical value, for example, the BN lubricating phase can be used for preparing wear-resistant structural members such as friction plates, bearings, sealing rings and the like.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
The test method comprises the following steps:
hardness: the test was carried out according to GB/T16534-2009 Fine ceramics Room temperature hardness test method using a Wilson-WolpertTukon2100B Vickers hardness tester.
Modulus of elasticity: the test is carried out by adopting an Instron-5566 universal material testing machine according to GB10700-2006-T bending method for testing the elastic modulus of fine ceramics.
Wear loss: the material abrasion loss test adopts a vertical universal material friction abrasion tester.
Noise: the test is carried out by adopting an HNT16040 type sound level meter according to GB-3096-2008 sound environment quality standard.
Example 1
21g of the total weight was weighedBN powder having a median particle diameter of 0.5 μm, 50g of Si having a median particle diameter of 0.5 μm3N4Powder, 5g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N410g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, and 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Raising the temperature to 1750 ℃ at the temperature of 10 ℃/min, applying the hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then relieving the pressure and reducing the temperature, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this example and the properties of the composite material obtained are shown in Table 1.
Example 2
21g of BN powder having a median particle size of 0.5 μm and 50g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 5g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N410g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, and 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
And (3) dry-pressing the mixture powder raw material obtained in the previous step into a specified shape by adopting a steel die at the pressure of 20MPa, performing cold isostatic pressing treatment at 200MPa, and maintaining the pressure for 10 minutes to obtain a ceramic blank.
Sintering the ceramic blank in a high temperature furnace, introducing N2Heating to 1750 deg.C at 10 deg.C/min, and holding for a while2 hours, and then cooling along with the furnace to obtain the required ceramic material.
The raw material components required for this example and the properties of the composite material obtained are shown in Table 1.
Example 3
21g of BN powder having a median particle size of 0.5 μm and 50g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 5g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N410g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, and 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
And (3) dry-pressing the mixture powder raw material obtained in the previous step into a specified shape by adopting a steel die at the pressure of 20MPa, performing cold isostatic pressing treatment at 200MPa, and maintaining the pressure for 10 minutes to obtain a ceramic blank.
Sintering the ceramic blank in a pressure sintering furnace, introducing N2The atmosphere is 1MPa, the temperature is raised to 1750 ℃ at the speed of 10 ℃/min, the heat preservation time is 2 hours, and then the ceramic material is obtained after furnace cooling.
The raw material components required for this example and the properties of the composite material obtained are shown in Table 1.
Example 4
2g of BN powder having a median particle size of 0.5 μm and 85g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 2g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N4Whiskers, 4g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, 5g of Y having a median particle diameter of 1 μm2O3Powder and 2g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Raising the temperature to 1750 ℃ at the temperature of 10 ℃/min, applying the hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then relieving the pressure and reducing the temperature, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this example and the properties of the composite material obtained are shown in Table 1.
Example 5
20g of BN powder having a median particle size of 0.5 μm and 50g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 3g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N4Whiskers, 15g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, 8g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Raising the temperature to 1750 ℃ at the temperature of 10 ℃/min, applying the hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then relieving the pressure and reducing the temperature, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this example and the properties of the composite material obtained are shown in Table 1.
Example 6
35g of BN powder having a median particle size of 0.5 μm and 45g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 2g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N44g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, and 9g of Y having a median particle diameter of 1 μm2O3Powder and 5g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, rolling and ball-milling the mixture for 3 hours, and turningThe speed is 300 r/min, and uniform and stable slurry is prepared.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Raising the temperature to 1750 ℃ at the temperature of 10 ℃/min, applying the hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then relieving the pressure and reducing the temperature, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this example and the properties of the composite material obtained are shown in Table 1.
Comparative example 1
25.5g of BN powder having a median particle size of 0.5 μm and 60.5g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
And (3) dry-pressing the mixture powder raw material obtained in the previous step into a specified shape by adopting a steel die at the pressure of 20MPa, performing cold isostatic pressing treatment at 200MPa, and maintaining the pressure for 10 minutes to obtain a ceramic blank.
Sintering the ceramic blank in a high temperature furnace, introducing N2Raising the temperature to 1750 ℃ at the temperature of 10 ℃/min in the atmosphere, preserving the temperature for 2 hours, and then cooling along with the furnace to obtain the required ceramic material.
The raw material components required for this comparative example and the properties of the composite material obtained are shown in Table 1.
Comparative example 2
86g of Si with a median particle size of 0.5 μm were weighed3N4Powder, 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
And (3) dry-pressing the mixture powder raw material obtained in the previous step into a specified shape by adopting a steel die at the pressure of 20MPa, performing cold isostatic pressing treatment at 200MPa, and maintaining the pressure for 10 minutes to obtain a ceramic blank.
Sintering the ceramic blank in a pressure sintering furnace, introducing N2The atmosphere is 1MPa, the temperature is raised to 1750 ℃ at the speed of 10 ℃/min, the heat preservation time is 2 hours, and then the ceramic material is obtained after furnace cooling.
The raw material components required for this comparative example and the properties of the composite material obtained are shown in Table 1.
Comparative example 3
71g of Si with a median particle size of 0.5 μm were weighed3N4Powder, 5g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N410g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, and 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
And (3) dry-pressing the mixture powder raw material obtained in the previous step into a specified shape by adopting a steel die at the pressure of 20MPa, performing cold isostatic pressing treatment at 200MPa, and maintaining the pressure for 10 minutes to obtain a ceramic blank.
Sintering the ceramic blank in a pressure sintering furnace, introducing N2The atmosphere is 1MPa, the temperature is raised to 1750 ℃ at the speed of 10 ℃/min, the heat preservation time is 2 hours, and then the ceramic material is obtained after furnace cooling.
The raw material components required for this comparative example and the properties of the composite material obtained are shown in Table 1.
Comparative example 4
21g of BN powder having a median particle size of 0.5 μm and 50g of Si having a median particle size of 0.5 μm were weighed out3N4Powder 15g of 0.2 μm average diameterβ -Si with a length of 3 μm3N4Whiskers, 10g of Y having a median particle size of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Heating to 1700 ℃ at the temperature of 10 ℃/min in the atmosphere, applying hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then decompressing and cooling, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this comparative example and the properties of the composite material obtained are shown in Table 1.
Comparative example 5
21g of BN powder having a median particle size of 0.5 μm and 50g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 15g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, and 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Heating to 1700 ℃ at the temperature of 10 ℃/min in the atmosphere, applying hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then decompressing and cooling, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this comparative example and the properties of the composite material obtained are shown in Table 1.
Comparative example 6
21g of BN powder having a median particle size of 0.5 μm and 50g of Si having a median particle size of 0.5 μm were weighed out3N410g of powder having an average diameter of 0.2 μm,β -Si with an average length of 3 μm3N4Whiskers, 5g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Heating to 1700 ℃ at the temperature of 10 ℃/min in the atmosphere, applying hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then decompressing and cooling, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this comparative example and the properties of the composite material obtained are shown in Table 1.
Comparative example 7
21g of BN powder having a median particle size of 0.5 μm and 50g of Si having a median particle size of 0.5 μm were weighed out3N4Powder, 1g β -Si with an average diameter of 0.2 μm and an average length of 3 μm3N4Whiskers, 14g of SiC fibers having an average diameter of 10 μm and an average length of 1mm, 10g of Y having a median particle diameter of 1 μm2O3Powder and 4g of Al having a median particle diameter of 1 μm2O3Adding 100g of absolute ethyl alcohol and 100g of silicon nitride grinding balls into the powder, and performing rolling ball milling for 3 hours at the rotating speed of 300 r/min to prepare uniform and stable slurry.
And drying the slurry at 50-80 ℃ for 3 hours, and sieving the dried slurry with a 100-mesh sieve to obtain mixture powder.
Filling the mixture powder into a hot-pressing die, putting the hot-pressing die into a hot-pressing sintering furnace, and introducing N2Heating to 1700 ℃ at the temperature of 10 ℃/min in the atmosphere, applying hot pressing pressure of 20MPa, keeping the temperature and the pressure for 2 hours, then decompressing and cooling, and cooling along with the furnace to obtain the required silicon nitride-based composite material.
The raw material components required for this comparative example and the properties of the composite material obtained are shown in Table 1.
TABLE 1 Components and Properties of the materials prepared in the examples
Figure BDA0002404613230000101
Note: noise high > medium > low > none
As can be seen from the above examples and comparative examples, the material system containing BN can significantly reduce the friction noise during friction process, and meanwhile, a certain proportion of β -Si is contained3N4The whiskers and the SiC fibers can have excellent mechanical properties and wear resistance, and in comparative example 1, only BN is added without β -Si3N4Whiskers and SiC fibers, although the frictional noise was low, the amount of abrasion of the material was high, and comparative example 2 contained no BN and β -Si3N4Whiskers and SiC fibers, having a low abrasion loss but a high friction noise, comparative example 3 containing no BN and containing only β -Si3N4Whiskers and SiC fibers having a low abrasion loss but a high frictional noise, comparative example 4 containing BN and β -Si3N4Whiskers, no SiC fibers, had a high abrasion loss of the material despite low frictional noise, comparative example 5, which contained BN and SiC fibers, did not contain β -Si3N4Whiskers, although having low frictional noise, had a high abrasion loss, comparative examples 6 and 7 contained BN, and also contained SiC fibers and β -Si3N4Whiskers, although having the advantages of low abrasion loss and low frictional noise, had higher abrasion loss than example 1, indicating unreasonable SiC fibers and β -Si3N4The reinforcing effect produced by the proportion of the whiskers is not good.

Claims (10)

1. Si3N4Ceramic-based friction material, characterized in that it is made of Si3N4Powder, BN powder, β -Si3N4The crystal whisker, the ceramic fiber and the metal oxide powder are used as main raw materials and are prepared by uniformly mixing and sintering, wherein in the raw materials, Si3N445-92% of powder, 2-40% of BN powder and β -Si3N42-10% of whisker, 2-20% of ceramic fiber and metal oxygenThe mass fraction of the compound is 2-15%, β -Si3N4The mass ratio of the crystal whisker to the ceramic fiber is 1: (1-10).
2. Si according to claim 13N4Ceramic-based friction material, characterized in that said ceramic fibers are selected from Si3N4、SiC、BN、Al3O4、SiO2One or a combination of several of the fibers.
3. Si according to claim 1 or 23N4The ceramic-based friction material is characterized in that the metal oxide powder is selected from Al2O3、MgO、Y2O3、Sc2O3、Sm2O3、Lu2O3、Er2O3One or a combination of several of them.
4. Si according to any one of claims 1 to 33N4Ceramic-based friction material, characterized in that Si3N4The average particle size of the powder is 0.2-10 μm, the average particle size of the BN powder is 0.05-20 μm, β -Si3N4The average diameter of the crystal whisker is 0.1-5 μm, and the average length is 0.3-20 μm; the average diameter of the ceramic fiber is 0.1-100 μm, and the average length is 100 μm-1 cm; the metal oxide powder has an average particle diameter of 0.1 to 20 μm.
5. Si according to any one of claims 1 to 43N4The ceramic-based friction material is characterized in that the sintering method is hot-pressing sintering, pressureless sintering or air pressure sintering.
6. Si according to any one of claims 1 to 43N4The preparation method of the ceramic-based friction material is characterized by comprising the following steps of:
a) weighing Si according to the proportion3N4Powder, BN powder, β -Si3N4Whisker and potteryCeramic fiber and metal oxide powder;
b) ball milling to uniformly mix the powder to prepare raw material powder;
b) and pouring the raw material powder obtained in the previous step into a mould for hot-pressing sintering, wherein the hot-pressing pressure is 5-50 MPa, the sintering temperature is 1500-1750 ℃, the sintering time is 1-4 hours, and the environment atmosphere is nitrogen.
7. Si according to any one of claims 1 to 43N4The preparation method of the ceramic-based friction material is characterized by comprising the following steps of:
a) weighing Si according to the proportion3N4Powder, BN powder, β -Si3N4Whiskers, ceramic fibers, and metal oxide powders;
b) ball milling to uniformly mix the powder to prepare raw material powder;
c) pressing and molding the raw material powder obtained in the previous step, and performing cold isostatic pressing treatment to obtain a ceramic blank;
d) and carrying out pressureless sintering on the ceramic blank, wherein the sintering temperature is 1500-1750 ℃, the sintering time is 1-4 hours, and the environment atmosphere is nitrogen.
8. Si according to any one of claims 1 to 43N4The preparation method of the ceramic-based friction material is characterized by comprising the following steps of:
a) weighing Si according to the proportion3N4Powder, BN powder, β -Si3N4Whiskers, ceramic fibers, and metal oxide powders;
b) ball milling to uniformly mix the powder to prepare raw material powder;
c) pressing and molding the raw material powder obtained in the previous step, and performing cold isostatic pressing treatment to obtain a ceramic blank;
d) and (3) putting the ceramic blank into a furnace for air pressure sintering, wherein the sintering temperature is 1500-1850 ℃, the sintering time is 1-4 hours, the air pressure is 0.1-10 MPa, and the environment atmosphere is nitrogen.
9. The preparation method according to claim 7 or 8, wherein the pressing method is dry pressing, and the dry pressing pressure is 10-100 MPa; the cold isostatic pressure is 50-400 MPa.
10. A wear-resistant structural member, characterized in that Si according to any one of claims 1 to 5 is used3N4And (3) preparing the ceramic-based friction material.
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