CN116444916B - Wear-resistant polytetrafluoroethylene lip sheet material and preparation method thereof - Google Patents

Wear-resistant polytetrafluoroethylene lip sheet material and preparation method thereof Download PDF

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CN116444916B
CN116444916B CN202310340458.0A CN202310340458A CN116444916B CN 116444916 B CN116444916 B CN 116444916B CN 202310340458 A CN202310340458 A CN 202310340458A CN 116444916 B CN116444916 B CN 116444916B
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polytetrafluoroethylene
blank
wear
mixed powder
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CN116444916A (en
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唐慧
范涛
张万平
周志锋
何礼荣
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Jiangmen Geleiyate Fluid Sealing Technology Co ltd
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Jiangmen Geleiyate Fluid Sealing Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/003—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor characterised by the choice of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/006—Pressing and sintering powders, granules or fibres
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
    • C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2003/085—Copper
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract

The application relates to the technical field of polytetrafluoroethylene materials, in particular to a wear-resistant polytetrafluoroethylene lip sheet material and a preparation method thereof. The scheme breaks through the conventional processing method, the mixed powder A and the mixed powder B are compounded for blank pressing, a sandwich blank structure of a bottom layer, a base blank and a surface layer is formed, and compared with the conventional mixed material blank pressing process, the wear resistance and the comprehensive mechanical property of a product can be greatly improved through the arrangement of the sandwich structure. The application has reasonable process design and proper proportion of each component, and the prepared lip sheet material has excellent wear resistance, higher overall strength, higher practicability and can be applied to processing sealing elements.

Description

Wear-resistant polytetrafluoroethylene lip sheet material and preparation method thereof
Technical Field
The application relates to the technical field of polytetrafluoroethylene materials, in particular to a wear-resistant polytetrafluoroethylene lip sheet material and a preparation method thereof.
Background
In various machines, the seal is used to prevent leakage of fluid or solid particles from between adjacent joint surfaces of parts, and to prevent intrusion of foreign substances such as dust, air, moisture, etc. into the device, so that the choice of material for the seal is critical to the machine; polytetrafluoroethylene has excellent high and low temperature resistance and chemical corrosion resistance, and almost all strong acids, strong alkali, strong oxidants and salts have no influence on polytetrafluoroethylene, and based on the excellent performance, polytetrafluoroethylene is mostly adopted as a sealing element material in the prior art.
But the application of the wear-resistant polytetrafluoroethylene is limited in actual production, and based on the situation, the application discloses a wear-resistant polytetrafluoroethylene lip sheet material and a preparation method thereof, and the processing of a high wear-resistant material is realized through the scheme, so that the technical problem to be solved in the prior art is urgent.
Disclosure of Invention
The application aims to provide a wear-resistant polytetrafluoroethylene lip sheet material and a preparation method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the application provides the following technical scheme:
a preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 180-200 ℃ for 1-2 hours, naturally cooling, then introducing fluorine gas and nitrogen mixed gas, heating to 400-420 ℃ at a heating rate of 5-6 ℃/min, and performing fluorination reaction to obtain fluorinated graphene;
(2) Taking polytetrafluoroethylene powder, drying for 2-3 hours at 110-120 ℃, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 10-20 min to obtain mixed powder A;
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler, and stirring for 5-10 min to obtain mixed powder B;
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 23-25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of a die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 23-25 ℃ to obtain a blank;
placing the blank body in a sintering furnace, heating to 320-330 ℃ at a speed of 2-3 ℃/min, preserving heat for 3-4 h, heating to 370-380 ℃, preserving heat for 3-4 h, cooling to 320-330 ℃, preserving heat for 1-2 h, and naturally cooling to obtain the lip material.
In the more optimized scheme, in the step (2), the mixing powder A comprises the following components in parts by weight: 20 to 30 weight percent of polyimide powder, 0.3 to 0.4 weight percent of metal powder, 8 to 10 weight percent of glass fiber and the balance of polytetrafluoroethylene powder.
In the more optimized scheme, in the step (2), the mixing powder B comprises the following components in parts by weight: 10-15 wt% of carbon fiber, 20-30 wt% of polyimide powder, 2-3 wt% of fluorinated graphene, 3-5 wt% of hard filler and the balance of polytetrafluoroethylene powder.
In the more optimized scheme, in the step (1), the fluorine-carbon ratio of the fluorinated graphene is 0.5-0.6; the volume ratio of fluorine to nitrogen in the mixed gas is (2-3): (7-8).
In the more optimized scheme, in the step (3), the thickness of the bottom layer is 45-50% of the base blank, and the thickness of the surface layer is 50-60% of the base blank.
In an optimized scheme, the hard filler is one or two of silicon nitride and boron nitride; the metal powder is one or two of copper powder and nickel powder.
In an optimized scheme, the hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1, a step of; the metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
the more optimized scheme, the compression molding technological parameters are as follows: the pressing pressure is 32-35 MPa, and the pressure maintaining time is 5-8 min.
According to the more optimized scheme, the wear-resistant polytetrafluoroethylene lip material is prepared by the preparation method of any one of the wear-resistant polytetrafluoroethylene lip materials.
Compared with the prior art, the application has the following beneficial effects:
the application discloses a wear-resistant polytetrafluoroethylene lip sheet material and a preparation method thereof, wherein the scheme breaks through the conventional processing method, and a mixed powder A and a mixed powder B are compounded to carry out blank pressing to form a sandwich blank structure of a bottom layer, a base blank and a surface layer.
When the scheme is implemented, polytetrafluoroethylene powder and polyimide powder are mixed, metal powder and glass fiber are added to obtain mixed powder A, wherein the introduction of the polyimide powder and the metal powder can improve the wear resistance of the lip material, and the glass fiber can be used as a reinforcing material to improve the comprehensive strength of a base blank part; then, polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler are mixed to obtain mixed powder B, the mixed powder B is used as a bottom layer and a surface layer, and a ligand base blank forms a sandwich composite structure, and the steps have the following specific effects: on one hand, the hardness of the base blank is lower than that of the bottom layer and the surface layer, so that when the base blank is actually worn, the hardness difference between the base blank and the surface layer or the bottom layer is utilized to realize buffering, and compared with a conventional single-layer structure, the wear resistance is greatly improved, and the wear rate is reduced; on the other hand, the base blank part also has excellent wear resistance, and the service life of the product can be greatly prolonged.
On the basis of the scheme, carbon fiber, fluorinated graphene and hard filler are added into the mixed powder B, wherein the hard filler is compounded by silicon nitride and boron nitride to improve the hardness of a surface layer or a bottom layer, and the hardness difference is realized by utilizing the carbon fiber matched with the hard filler; in addition, the fluorine-carbon ratio of the fluorinated graphene is limited to be 0.5-0.6, and the enhancement effect of the fluorinated graphene in the conventional process can be improved along with the increase of the fluorine-carbon ratio, but because the carbon fiber is matched with the hard filler, the fluorine-carbon ratio is limited to be 0.5-0.6, the lubrication effect is improved, the formation of a transfer film on the friction surface is promoted, and the overall abrasion resistance effect is reduced instead when the fluorine-carbon ratio exceeds the range.
The application discloses a wear-resistant polytetrafluoroethylene lip sheet material and a preparation method thereof, which are reasonable in process design and proper in proportion of each component, and the prepared lip sheet material has excellent wear resistance, higher overall strength, can be applied to processing of sealing elements, and has higher practicability.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
In the embodiment, the thickness of the graphene sheet layer is 20-30 nm, the average sheet diameter is 100 mu m, and the carbon element is 96.7wt%; the average particle size of the polytetrafluoroethylene powder is 4.5 mu m; the polyimide powder has an average particle diameter of 30 μm; the average particle diameter of the metal powder is 0.1 mu m; glass fiber diameter 10 μm, aspect ratio 4:1, a step of; the carbon fiber diameter is 10 μm, and the length-diameter ratio is 5:1, a step of; the average grain size of the boron nitride and the silicon nitride is 100nm.
Example 1: a preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 180 ℃ for 2 hours, naturally cooling, then introducing mixed gas of fluorine gas and nitrogen gas, heating to 400 ℃ at a heating rate of 5 ℃/min, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.5-0.6; the volume ratio of fluorine to nitrogen in the mixed gas is 2:8.
(2) Taking polytetrafluoroethylene powder, drying at 110 ℃ for 3 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 10 minutes to obtain mixed powder A; in the mixed powder A, the dosages of the components are as follows: 25wt% of polyimide powder, 0.4wt% of metal powder, 8wt% of glass fiber and the balance of polytetrafluoroethylene powder. The metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler, and stirring for 5min to obtain mixed powder B; in the mixed powder B, the dosage of each component is as follows: 15wt% of carbon fiber, 20wt% of polyimide powder, 2.5wt% of fluorinated graphene, 4wt% of hard filler and the balance of polytetrafluoroethylene powder. The hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1.
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of the die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 25 ℃ to obtain a blank; the thickness of the bottom layer is 50% of the base blank, the thickness of the surface layer is 60% of the base blank, and the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
And (3) placing the blank body in a sintering furnace, heating to 320 ℃ at a speed of 2 ℃/min, preserving heat for 4 hours, heating to 370 ℃, preserving heat for 4 hours, cooling to 320 ℃, preserving heat for 2 hours, and naturally cooling to obtain the lip material.
Example 2: a preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 190 ℃ for 1.5 hours, naturally cooling, then introducing mixed gas of fluorine and nitrogen, heating to 410 ℃ at a heating rate of 5 ℃/min, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.5-0.6; the volume ratio of fluorine to nitrogen in the mixed gas is 2:8.
(2) Taking polytetrafluoroethylene powder, drying at 115 ℃ for 2.5 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 15 minutes to obtain mixed powder A; in the mixed powder A, the dosages of the components are as follows: 25wt% of polyimide powder, 0.4wt% of metal powder, 8wt% of glass fiber and the balance of polytetrafluoroethylene powder. The metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler, and stirring for 8min to obtain mixed powder B; in the mixed powder B, the dosage of each component is as follows: 15wt% of carbon fiber, 20wt% of polyimide powder, 2.5wt% of fluorinated graphene, 4wt% of hard filler and the balance of polytetrafluoroethylene powder. The hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1.
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of the die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 25 ℃ to obtain a blank; the thickness of the bottom layer is 50% of the base blank, the thickness of the surface layer is 60% of the base blank, and the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
Placing the blank body in a sintering furnace, heating to 325 ℃ at a speed of 2 ℃/min, preserving heat for 3.5h, heating to 375 ℃, preserving heat for 3.5h, cooling to 325 ℃, preserving heat for 1.5h, and naturally cooling to obtain the lip material.
Example 3: a preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 200 ℃ for 1h, naturally cooling, then introducing mixed gas of fluorine gas and nitrogen gas, heating to 420 ℃ at a heating rate of 5 ℃/min, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.5-0.6; the volume ratio of fluorine to nitrogen in the mixed gas is 2:8.
(2) Taking polytetrafluoroethylene powder, drying at 120 ℃ for 2 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 20 minutes to obtain mixed powder A; in the mixed powder A, the dosages of the components are as follows: 25wt% of polyimide powder, 0.4wt% of metal powder, 8wt% of glass fiber and the balance of polytetrafluoroethylene powder. The metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler, and stirring for 10min to obtain mixed powder B; in the mixed powder B, the dosage of each component is as follows: 15wt% of carbon fiber, 20wt% of polyimide powder, 2.5wt% of fluorinated graphene, 4wt% of hard filler and the balance of polytetrafluoroethylene powder. The hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1.
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of the die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 25 ℃ to obtain a blank; the thickness of the bottom layer is 50% of the base blank, the thickness of the surface layer is 60% of the base blank, and the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
And (3) placing the blank body in a sintering furnace, heating to 330 ℃ at a speed of 2 ℃/min, preserving heat for 3 hours, heating to 380 ℃, preserving heat for 3 hours, cooling to 330 ℃, preserving heat for 1 hour, and naturally cooling to obtain the lip material.
Comparative example 1: comparative example 1 a control experiment was performed using example 2 as a control group, and the fluorine-carbon ratio of the fluorinated graphene in comparative example 1 was 0.9 to 1.
A preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 190 ℃ for 1.5 hours, naturally cooling, then introducing mixed gas of fluorine and nitrogen, heating to 410 ℃ at a heating rate of 5 ℃/min, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.9-1; the volume ratio of fluorine to nitrogen in the mixed gas is 2:8.
(2) Taking polytetrafluoroethylene powder, drying at 115 ℃ for 2.5 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 15 minutes to obtain mixed powder A; in the mixed powder A, the dosages of the components are as follows: 25wt% of polyimide powder, 0.4wt% of metal powder, 8wt% of glass fiber and the balance of polytetrafluoroethylene powder. The metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler, and stirring for 8min to obtain mixed powder B; in the mixed powder B, the dosage of each component is as follows: 15wt% of carbon fiber, 20wt% of polyimide powder, 2.5wt% of fluorinated graphene, 4wt% of hard filler and the balance of polytetrafluoroethylene powder. The hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1.
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of the die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 25 ℃ to obtain a blank; the thickness of the bottom layer is 50% of the base blank, the thickness of the surface layer is 60% of the base blank, and the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
Placing the blank body in a sintering furnace, heating to 325 ℃ at a speed of 2 ℃/min, preserving heat for 3.5h, heating to 375 ℃, preserving heat for 3.5h, cooling to 325 ℃, preserving heat for 1.5h, and naturally cooling to obtain the lip material.
Comparative example 2: comparative example 2 a control experiment was performed using example 2 as a control group, and a green body was obtained by press molding of mixed powder a in comparative example 2.
A preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Taking polytetrafluoroethylene powder, drying at 115 ℃ for 2.5 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 15 minutes to obtain mixed powder A; in the mixed powder A, the dosages of the components are as follows: 25wt% of polyimide powder, 0.4wt% of metal powder, 8wt% of glass fiber and the balance of polytetrafluoroethylene powder. The metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
(2) Placing the mixed powder A into a grinding tool, pressing and forming at 25 ℃, and demolding to form a blank; the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
Placing the blank body in a sintering furnace, heating to 325 ℃ at a speed of 2 ℃/min, preserving heat for 3.5h, heating to 375 ℃, preserving heat for 3.5h, cooling to 325 ℃, preserving heat for 1.5h, and naturally cooling to obtain the lip material.
Comparative example 3: comparative example 3 a control experiment was performed using example 2 as a control group, and a green body was obtained by press molding of mixed powder B in comparative example 3.
A preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 190 ℃ for 1.5 hours, naturally cooling, then introducing mixed gas of fluorine and nitrogen, heating to 410 ℃ at a heating rate of 5 ℃/min, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.5-0.6; the volume ratio of fluorine to nitrogen in the mixed gas is 2:8.
(2) Mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler, and stirring for 8min to obtain mixed powder B; in the mixed powder B, the dosage of each component is as follows: 15wt% of carbon fiber, 20wt% of polyimide powder, 2.5wt% of fluorinated graphene, 4wt% of hard filler and the balance of polytetrafluoroethylene powder. The hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1.
(3) Placing the mixed powder B into a grinding tool, pressing and forming at 25 ℃, and demolding to obtain a blank; the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
Placing the blank body in a sintering furnace, heating to 325 ℃ at a speed of 2 ℃/min, preserving heat for 3.5h, heating to 375 ℃, preserving heat for 3.5h, cooling to 325 ℃, preserving heat for 1.5h, and naturally cooling to obtain the lip material.
Comparative example 4: comparative example 4 a control experiment was performed using example 2 as a control group, and no hard filler was introduced into comparative example 4.
A preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 190 ℃ for 1.5 hours, naturally cooling, then introducing mixed gas of fluorine and nitrogen, heating to 410 ℃ at a heating rate of 5 ℃/min, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.5-0.6; the volume ratio of fluorine to nitrogen in the mixed gas is 2:8.
(2) Taking polytetrafluoroethylene powder, drying at 115 ℃ for 2.5 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 15 minutes to obtain mixed powder A; in the mixed powder A, the dosages of the components are as follows: 25wt% of polyimide powder, 0.4wt% of metal powder, 8wt% of glass fiber and the balance of polytetrafluoroethylene powder. The metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber and fluorinated graphene, and stirring for 8min to obtain mixed powder B; in the mixed powder B, the dosage of each component is as follows: 15wt% of carbon fiber, 20wt% of polyimide powder, 2.5wt% of fluorinated graphene and the balance of polytetrafluoroethylene powder. The hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1.
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of the die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 25 ℃ to obtain a blank; the thickness of the bottom layer is 50% of the base blank, the thickness of the surface layer is 60% of the base blank, and the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
Placing the blank body in a sintering furnace, heating to 325 ℃ at a speed of 2 ℃/min, preserving heat for 3.5h, heating to 375 ℃, preserving heat for 3.5h, cooling to 325 ℃, preserving heat for 1.5h, and naturally cooling to obtain the lip material.
Comparative example 5: comparative example 5 a control experiment was performed using comparative example 4 as a control group, no hard filler was introduced into comparative example 5, and the fluorocarbon ratio was 0.9 to 1%.
A preparation method of wear-resistant polytetrafluoroethylene lip material comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 190 ℃ for 1.5 hours, naturally cooling, then introducing mixed gas of fluorine and nitrogen, heating to 410 ℃ at a heating rate of 5 ℃/min, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.9-1; the volume ratio of fluorine to nitrogen in the mixed gas is 2:8.
(2) Taking polytetrafluoroethylene powder, drying at 115 ℃ for 2.5 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 15 minutes to obtain mixed powder A; in the mixed powder A, the dosages of the components are as follows: 25wt% of polyimide powder, 0.4wt% of metal powder, 8wt% of glass fiber and the balance of polytetrafluoroethylene powder. The metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1.
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber and fluorinated graphene, and stirring for 8min to obtain mixed powder B; in the mixed powder B, the dosage of each component is as follows: 15wt% of carbon fiber, 20wt% of polyimide powder, 2.5wt% of fluorinated graphene and the balance of polytetrafluoroethylene powder. The hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1.
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of the die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 25 ℃ to obtain a blank; the thickness of the bottom layer is 50% of the base blank, the thickness of the surface layer is 60% of the base blank, and the thickness of the blank body is 4mm. The press forming process parameters are as follows: the pressing pressure was 35MPa and the dwell time was 8min.
Placing the blank body in a sintering furnace, heating to 325 ℃ at a speed of 2 ℃/min, preserving heat for 3.5h, heating to 375 ℃, preserving heat for 3.5h, cooling to 325 ℃, preserving heat for 1.5h, and naturally cooling to obtain the lip material.
Detection experiment:
1. the lip materials prepared in examples 1 to 3 and comparative examples 1 to 5 were processed to form test pieces having dimensions of 20 mm. Times.12 mm. Times.4 mm, the wear resistance of the facing was examined by a frictional wear test, the mating member was a GCr15 steel ball, the diameter was 6mm, the hardness was 63HRC, the load was 10N, the sliding speed was 0.08m/s, the sliding distance was 600m, and the wear rate was measured and calculated.
Project Example 1 Example 2 Example 3 Comparative example 1
Wear rate 10 -15 m 3 /(N×m) 4.48 4.37 4.41 5.24
Project Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5
Wear rate 10 -15 m 3 /(N×m) 14.37 10.13 8.46 7.92
Conclusion: the application discloses a wear-resistant polytetrafluoroethylene lip sheet material and a preparation method thereof, which are reasonable in process design and proper in proportion of each component, and the prepared lip sheet material has excellent wear resistance, higher overall strength, can be applied to processing of sealing elements, and has higher practicability.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present application, and the present application is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present application has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (4)

1. A preparation method of wear-resistant polytetrafluoroethylene lip material is characterized by comprising the following steps: the method comprises the following steps:
(1) Placing graphene in a high-pressure reaction kettle, vacuumizing, performing heat treatment at 180-200 ℃ for 1-2 hours, naturally cooling, then introducing mixed gas of fluorine and nitrogen, heating to 400-420 ℃, and performing fluorination reaction to obtain fluorinated graphene; the fluorine-carbon ratio of the fluorinated graphene is 0.5-0.6; the volume ratio of fluorine to nitrogen in the mixed gas is (2-3): (7-8);
(2) Taking polytetrafluoroethylene powder, drying at 110-120 ℃ for 2-3 hours, mixing the polytetrafluoroethylene powder with polyimide powder, adding metal powder and glass fiber, and mixing for 10-20 minutes to obtain mixed powder A; the metal powder is compounded by copper powder and nickel powder, and the mass ratio is 4:1, a step of;
mixing polytetrafluoroethylene powder, polyimide powder, carbon fiber, fluorinated graphene and hard filler, and stirring for 5-10 min to obtain mixed powder B; the hard filler is compounded by silicon nitride and boron nitride, and the mass ratio is 1:1, a step of;
in the mixed powder A, the dosages of the components are as follows: 20-30wt% of polyimide powder, 0.3-0.4wt% of metal powder, 8-10wt% of glass fiber and the balance of polytetrafluoroethylene powder; in the mixed powder B, the dosage of each component is as follows: 10-15 wt% of carbon fiber, 20-30 wt% of polyimide powder, 2-3 wt% of fluorinated graphene, 3-5 wt% of hard filler and the balance of polytetrafluoroethylene powder;
(3) Placing the mixed powder A into a grinding tool, pressing and forming at 23-25 ℃, and demolding to form a base blank; paving mixed powder B at the bottom of a die to form a bottom layer, placing a base blank on the bottom layer, paving the mixed powder B on the surface of the base blank to form a surface layer, and performing compression molding at 23-25 ℃ to obtain a blank;
placing the blank body in a sintering furnace, heating to 320-330 ℃, preserving heat for 3-4 hours, heating to 370-380 ℃, preserving heat for 3-4 hours, cooling to 320-330 ℃, preserving heat for 1-2 hours, and naturally cooling to obtain the lip material.
2. The method for preparing the wear-resistant polytetrafluoroethylene lip material according to claim 1, wherein the method comprises the following steps: in the step (3), the thickness of the bottom layer is 45-50% of that of the base blank, and the thickness of the surface layer is 50-60% of that of the base blank.
3. The method for preparing the wear-resistant polytetrafluoroethylene lip material according to claim 1, wherein the method comprises the following steps: the press forming process parameters are as follows: the pressing pressure is 32-35 MPa, and the pressure maintaining time is 5-8 min.
4. The wear-resistant polytetrafluoroethylene prepared by the preparation method of the wear-resistant polytetrafluoroethylene lip material according to any one of claims 1-3.
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