CN113235291B - Boron carbide-molybdenum disulfide hybrid filler, preparation and application thereof, self-lubricating fabric liner material, and preparation and application thereof - Google Patents

Boron carbide-molybdenum disulfide hybrid filler, preparation and application thereof, self-lubricating fabric liner material, and preparation and application thereof Download PDF

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CN113235291B
CN113235291B CN202110577687.5A CN202110577687A CN113235291B CN 113235291 B CN113235291 B CN 113235291B CN 202110577687 A CN202110577687 A CN 202110577687A CN 113235291 B CN113235291 B CN 113235291B
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boron carbide
molybdenum disulfide
self
lubricating
liner material
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CN113235291A (en
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袁军亚
刘梦
张招柱
杨明明
姜葳
赵鑫
储凡杰
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
    • D—TEXTILES; PAPER
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    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
    • D06M15/41—Phenol-aldehyde or phenol-ketone resins
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/22—Polymers or copolymers of halogenated mono-olefins
    • D—TEXTILES; PAPER
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds

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Abstract

The invention provides a boron carbide-molybdenum disulfide hybrid filler, preparation and application thereof, a self-lubricating fabric liner material, and preparation and application thereof, and belongs to the technical field of solid lubrication. According to the invention, the boron carbide-molybdenum disulfide hybrid filler is introduced into the polyimide fiber-polytetrafluoroethylene fiber self-lubricating fabric liner material, and the excellent friction reducing and wear resisting properties are given to the self-lubricating fabric liner material by exerting the bearing and wear resisting functions of boron carbide and the interlayer sliding property (friction reducing and lubricating effect) of molybdenum disulfide, so that the synergistic enhancement effect on the tribological property of the self-lubricating fabric liner material is realized. In addition, the molybdenum disulfide loaded on the surfaces of the boron carbide particles can improve the dispersion of boron carbide in the fabric liner and inhibit the agglomeration effect of the molybdenum disulfide, and the friction performance of the self-lubricating fabric liner material is remarkably enhanced.

Description

Boron carbide-molybdenum disulfide hybrid filler, preparation and application thereof, self-lubricating fabric liner material, and preparation and application thereof
Technical Field
The invention relates to the technical field of solid lubrication, in particular to a boron carbide-molybdenum disulfide hybrid filler, preparation and application thereof, and a self-lubricating fabric liner material, and preparation and application thereof.
Background
The friction consumes about 1/3 of primary energy in the world, and the abrasion causes about 60% of machine parts to fail, so that the reduction of the friction abrasion in the operation process of the machine parts is particularly critical and urgent. The self-lubricating fabric liner is used as a key component of the self-lubricating joint bearing, and the frictional wear performance of the self-lubricating fabric liner directly determines the service performance and the service life of the self-lubricating joint bearing. With the rapid development of science and technology, mechanical parts need to run stably under more severe working conditions, and are particularly applied to self-lubricating joint bearings in the field of high-end lubrication, so that higher requirements are provided for the frictional wear performance of self-lubricating fabric liners.
Filler reinforcement is widely used as one of the most common friction modifying means for improving the frictional wear performance of polymer matrix composites. However, the improvement effect of a single reinforcing filler on the tribological performance of a polymer composite material is limited, and more researchers achieve the synergistic enhancement of the tribological performance of the composite material by adding a plurality of fillers or hybrid fillers. However, the existing fillers have limited effect of enhancing the tribological properties of the composite material.
Disclosure of Invention
The invention aims to provide a boron carbide-molybdenum disulfide hybrid filler, preparation and application thereof, and a self-lubricating fabric liner material, and preparation and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of boron carbide-molybdenum disulfide hybrid filler, which comprises the following steps:
mixing the boron carbide dispersion liquid, dopamine hydrochloride and polyethyleneimine, and carrying out amination modification reaction to obtain aminated boron carbide;
and mixing the aminated boron carbide, water, a molybdenum source and a sulfur source, and hybridizing to obtain the boron carbide-molybdenum disulfide hybrid filler.
Preferably, the dispersant used by the boron carbide dispersion liquid is Tris-HCl buffer solution; the concentration of the Tris-HCl buffer solution is 2mg/mL, and the pH value is 8.5; the dosage ratio of the boron carbide to the dispersant in the boron carbide dispersion liquid is (0.5-1) g:250 mL.
Preferably, the mass ratio of the boron carbide to the dopamine hydrochloride to the polyethyleneimine in the boron carbide dispersion liquid is (0.5-1): 0.5-1);
the temperature of the amination modification reaction is room temperature, and the time is 6-24 hours.
Preferably, the molybdenum source comprises sodium molybdate, ammonium molybdate or sodium molybdate; the sulfur source comprises thiourea; the mass ratio of the boron carbide to the molybdenum source to the sulfur source is (0.5-1) to (1-2);
the temperature of hybridization is 200-240 ℃, and the time is 12-36 h.
The invention provides a boron carbide-molybdenum disulfide hybrid filler prepared by the preparation method in the technical scheme, which comprises boron carbide particles, molybdenum disulfide nanoflowers loaded on the surfaces of the boron carbide particles, and a polydopamine-polyethyleneimine copolymer intermediate layer, wherein the intermediate layer is positioned between the boron carbide particles and the molybdenum disulfide nanoflowers.
The invention provides application of the boron carbide-molybdenum disulfide hybrid filler in the technical scheme in a self-lubricating fabric liner composite material.
The invention provides a preparation method of a boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material, which comprises the following steps:
mixing the boron carbide-molybdenum disulfide hybrid filler and a phenolic resin solution to obtain an impregnation solution;
and (3) repeatedly carrying out the processes of dipping and drying on the polyimide fiber-polytetrafluoroethylene fiber blended fabric in the dipping solution, and curing the obtained composite blended fabric to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
Preferably, the impregnation-drying process is repeated until the mass fraction of the mixture of the phenolic resin and the boron carbide-molybdenum disulfide hybrid filler in the composite blended fabric is 15-40%; the curing pressure is 0.01-3 MPa, the temperature is 150-250 ℃, and the heat preservation time is 0.5-3 h.
The invention provides a boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material prepared by the preparation method in the technical scheme, which comprises a self-lubricating fabric liner material and a boron carbide-molybdenum disulfide hybrid filler loaded on the self-lubricating fabric liner material.
The invention provides an application of the boron carbide-molybdenum disulfide hybrid filler in the technical scheme in a self-lubricating joint bearing.
The invention provides a preparation method of boron carbide-molybdenum disulfide hybrid filler, which comprises the following steps: mixing the boron carbide dispersion liquid, dopamine hydrochloride and polyethyleneimine, and carrying out amination modification reaction to obtain aminated boron carbide; and mixing the aminated boron carbide, water, a molybdenum source and a sulfur source, and hybridizing to obtain the boron carbide-molybdenum disulfide hybrid filler. The method comprises the steps of forming polydopamine-polyethyleneimine copolymer on the surface of boron carbide particles by utilizing the reaction of dopamine hydrochloride and polyethyleneimine through Michael addition and Schiff base, endowing rich amino functional groups on the surface of the boron carbide particles, then enabling a sulfur source and the amino functional groups on the surface of the boron carbide particles to generate electrostatic interaction, enabling the sulfur source to be attached to the surface of the boron carbide particles, enabling the sulfur source attached to the surface of the boron carbide particles to generate chemical reaction with a molybdenum source, enabling the generated molybdenum disulfide nanoflowers to uniformly grow on the surface of the boron carbide particles, forming boron carbide particles loaded with the molybdenum disulfide nanoflowers, and enabling the polydopamine-polyethyleneimine copolymer to be used as an intermediate layer and exist between the boron carbide particles and molybdenum disulfide nanocrystallization.
According to the invention, the prepared boron carbide-molybdenum disulfide hybrid filler is introduced into a polyimide fiber-polytetrafluoroethylene fiber self-lubricating fabric liner material, and the load-bearing and wear-resisting functions of boron carbide and the interlayer sliding performance (friction-reducing and lubricating effect) of molybdenum disulfide are exerted, so that the self-lubricating fabric liner material is endowed with excellent friction-reducing and wear-resisting properties, and the synergistic enhancement effect on the tribological performance of the self-lubricating fabric liner material is realized. In addition, because the surface of the boron carbide particle is lack of a reaction functional group, and the surface of the molybdenum disulfide nanoflower contains rich active functional groups (such as-OH), the molybdenum disulfide loaded on the surface of the boron carbide particle can promote the dispersion of the boron carbide-molybdenum disulfide hybrid filler in the fabric liner, and the growth of the molybdenum disulfide on the surface of the boron carbide can relieve the agglomeration effect of the molybdenum disulfide in the resin matrix due to high surface energy, so that the friction performance of the self-lubricating fabric liner material is remarkably enhanced.
Drawings
FIG. 1 is a graph of wear rate and coefficient of friction for self-lubricating fabric liner materials prepared in comparative example 1 and example 2;
FIG. 2 is an optical microscope photograph of the polyimide fiber/polytetrafluoroethylene fiber blended fabric and the composite blended fabric prepared in example 1;
FIG. 3 is an SEM image of commercially available boron carbide, aminated boron carbide prepared in example 3, and boron carbide-molybdenum disulfide hybrid prepared in example 3;
FIG. 4 is a Raman spectrum and an XRD spectrum of a commercially available boron carbide, a commercially available molybdenum disulfide, an aminated boron carbide prepared in example 4, and a boron carbide/molybdenum disulfide hybrid prepared in example 4;
fig. 5 is an optical microscope photograph of self-lubricating fabric liner materials prepared in comparative example 1 and example 4.
Detailed Description
The invention provides a preparation method of boron carbide-molybdenum disulfide hybrid filler, which comprises the following steps:
mixing the boron carbide dispersion liquid, dopamine hydrochloride and polyethyleneimine, and carrying out amination modification reaction to obtain aminated boron carbide;
and mixing the aminated boron carbide, water, a molybdenum source and a sulfur source, and hybridizing to obtain the boron carbide-molybdenum disulfide hybrid filler.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
According to the invention, boron carbide dispersion liquid, dopamine hydrochloride and polyethyleneimine are mixed and subjected to amination modification reaction to obtain aminated boron carbide. In the invention, the dispersant used in the boron carbide dispersion liquid is preferably Tris-HCl buffer solution; the concentration of the Tris-HCl buffer solution is preferably 2mg/mL, and the pH value is preferably 8.5; the preparation process of the Tris-HCl buffer solution is not particularly limited, and the Tris-HCl buffer solution with the concentration and the pH value can be obtained according to the well-known process in the field.
In the invention, the dosage ratio of the boron carbide to the dispersant in the boron carbide dispersion liquid is preferably (0.5-1) g:250mL, and more preferably (0.6-0.8) g:250 mL.
In the invention, the preparation process of the boron carbide dispersion liquid is preferably to mix boron carbide with Tris-HCl buffer solution and carry out uniform ultrasonic dispersion; the process of the ultrasound is not particularly limited in the present invention, and may be performed according to a process well known in the art. In the present invention, the particle size of the boron carbide is preferably 1 to 10 μm.
In the invention, the relative molecular mass of the polyethyleneimine is preferably 300-1000. In the invention, the mass ratio of the boron carbide, the dopamine hydrochloride and the polyethyleneimine in the boron carbide dispersion liquid is preferably (0.5-1): 0.5-1, and more preferably (0.6-0.8): 0.6-0.8. The process of mixing the boron carbide dispersion, dopamine hydrochloride and polyethyleneimine is not particularly limited, and may be performed according to a process known in the art.
In the invention, the temperature of the amination modification reaction is preferably room temperature, the time is preferably 6-24 h, and more preferably 12-18 h; the amination modification reaction is preferably carried out under stirring conditions, and the stirring speed is not particularly limited in the present invention, and the reaction can be carried out smoothly according to the procedures known in the art.
In the amination modification reaction process, dopamine hydrochloride and polyethyleneimine react with Michael addition and Schiff base to form polydopamine-polyethyleneimine copolymer on the surface of boron carbide particles, so that abundant amino functional groups are given to the surface of the boron carbide particles to realize amination modification, and a transition layer is formed on the surface of the boron carbide particles to facilitate subsequent realization of loading of molybdenum disulfide nanoflowers.
After the amination modification reaction is finished, the invention does not carry out any treatment, and directly carries out subsequent treatment on the obtained product (containing amination boron carbide).
After the aminated boron carbide is obtained, the aminated boron carbide, water, a molybdenum source and a sulfur source are mixed and hybridized to obtain the boron carbide-molybdenum disulfide hybrid filler.
In the present invention, the molybdenum source preferably comprises sodium molybdate, ammonium molybdate or sodium molybdate; the sulfur source preferably comprises thiourea; the mass ratio of the boron carbide, the molybdenum source and the sulfur source is preferably (0.5-1): 1-2, more preferably (0.6-0.8): 1.5-1.8; the mass ratio of the molybdenum source to the water is preferably (0.001-0.1) g:1 mL.
In the invention, the process of mixing the aminated boron carbide, the water, the molybdenum source and the sulfur source is preferably to disperse the aminated boron carbide in the water, add the molybdenum source and the sulfur source and stir for 0.5 h; the process of dispersing and stirring is not particularly limited in the present invention, and may be carried out according to a process well known in the art.
In the invention, the hybridization temperature is preferably 200-240 ℃, more preferably 210-230 ℃, and the time is preferably 12-36 h, more preferably 18-30 h.
In the hybridization process, a sulfur source and amino functional groups on the surfaces of boron carbide particles generate an electrostatic effect, so that the sulfur source is attached to the surfaces of the boron carbide particles, the sulfur source attached to the surfaces of the boron carbide particles and a molybdenum source perform a chemical reaction, and the obtained molybdenum disulfide nanoflowers uniformly grow on the surfaces of the boron carbide particles to form boron carbide particles loaded with the molybdenum disulfide nanoflowers, and meanwhile, a polydopamine-polyethyleneimine copolymer is used as an intermediate layer and positioned between the boron carbide particles and the molybdenum disulfide nanoflowers.
After the hybridization is finished, the obtained product is preferably sequentially filtered, washed and dried to obtain the boron carbide-molybdenum disulfide hybrid filler. The filtration, washing and drying processes are not particularly limited in the present invention and may be performed according to processes well known in the art. The specification of the boron carbide-molybdenum disulfide hybrid filler is not specially limited, and the boron carbide-molybdenum disulfide hybrid filler with the corresponding specification is prepared according to the conditions.
The invention provides a boron carbide-molybdenum disulfide hybrid filler prepared by the preparation method in the technical scheme, which comprises boron carbide particles, molybdenum disulfide nanoflowers loaded on the surfaces of the boron carbide particles, and a polydopamine-polyethyleneimine copolymer intermediate layer, wherein the intermediate layer is positioned between the boron carbide particles and the molybdenum disulfide nanoflowers.
The invention provides application of the boron carbide-molybdenum disulfide hybrid filler in the technical scheme in a self-lubricating fabric liner composite material. The method of the present invention is not particularly limited, and the method may be performed by a method known in the art.
The invention provides a preparation method of a boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material, which comprises the following steps:
mixing the boron carbide-molybdenum disulfide hybrid filler and a phenolic resin solution to obtain an impregnation solution;
and (3) repeatedly carrying out the processes of dipping and drying on the polyimide fiber-polytetrafluoroethylene fiber blended fabric in the dipping solution, and curing the obtained composite blended fabric to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
According to the invention, the boron carbide-molybdenum disulfide hybrid filler in the technical scheme is mixed with phenolic resin to obtain the impregnation liquid.
In the present invention, the solvent of the phenolic resin solution is preferably at least two of ethanol, acetone and ethyl acetate, and when the solvent of the phenolic resin is preferably two or three of the above, the ratio of different solvents in the present invention is not particularly limited, and any ratio may be used. In the invention, the mass concentration of the phenolic resin solution is preferably 0.1-0.3 g/mL, and more preferably 0.15-0.25 g/mL.
In the invention, the mass percentage of the boron carbide-molybdenum disulfide hybrid filler in the phenolic resin solution is preferably 0.5-5%, and more preferably 2-4%.
The process of mixing the boron carbide-molybdenum disulfide hybrid filler and the phenolic resin solution is not particularly limited, and the materials can be uniformly mixed according to the process known in the field.
After the impregnation liquid is obtained, the polyimide fiber-polytetrafluoroethylene fiber blended fabric is repeatedly impregnated in the impregnation liquid and dried, and the obtained composite blended fabric is cured to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
In the invention, the polyimide fiber-polytetrafluoroethylene fiber blended fabric is preferably woven by taking polytetrafluoroethylene fibers as warp yarns and polyimide fibers as weft yarns. The specification of the polytetrafluoroethylene fiber and the polyimide fiber is not particularly limited, and commercial products well known in the field can be selected; in the embodiment of the invention, the titer of the polytetrafluoroethylene fiber is specifically 400D, and the titer of the polyimide fiber is specifically 200D.
In the invention, the weave structure of the polyimide fiber-polytetrafluoroethylene fiber blended fabric is preferably one or more of plain weave, twill weave and satin weave; when the tissue structures of the polyimide fiber-polytetrafluoroethylene fiber blended fabric are several of the above, the distribution proportion and the mode of different tissue structures are not specially limited, and any proportion or mode can be adopted. In the invention, the warp density of the polyimide fiber-polytetrafluoroethylene fiber blended fabric is preferably 320-490 pieces/10 cm, and the weft density is preferably 290-350 pieces/10 cm. The specific weaving process is not particularly limited in the present invention, and the weaving process may be performed according to the process known in the art by using the warp density and the weft density.
In the present invention, it is preferable that the polyimide fiber-polytetrafluoroethylene fiber blended fabric is subjected to air plasma treatment before repeating the impregnation-drying process; the power of the air plasma treatment is preferably 40-300W, more preferably 100-250W, and the treatment time is preferably 5-30 min, more preferably 10-20 min. According to the invention, the surface of the fiber is etched through air plasma treatment, molecular chains on the surface of the fiber are broken, and active functional groups are introduced into the surface of the fiber, so that a chemical bonding effect is generated between the blended fabric and a phenolic resin matrix in the impregnation process, the interface bonding effect between the blended fabric and the phenolic resin is enhanced, and the friction performance of the self-lubricating fabric liner material is enhanced.
The specific process of impregnation-drying is not particularly limited in the present invention, and impregnation and drying are performed according to a process well known in the art to obtain a composite blended fabric. In an embodiment of the present invention, the drying manner is specifically drying.
The impregnation-drying process is preferably repeated until the mass fraction (namely the sizing amount) of the mixture of the phenolic resin and the boron carbide-molybdenum disulfide hybrid filler in the composite blended fabric is 15-40%, and more preferably 20-30%.
After the impregnation-drying process is completed, the mixture of the phenolic resin and the boron carbide-molybdenum disulfide hybrid filler is coated on the surface of the blended fabric to be used as a continuous phase of the composite material.
In the invention, the curing pressure is preferably 0.01-3 MPa, and more preferably 0.2-2.5 MPa; the temperature is preferably 150-250 ℃, more preferably 180-200 ℃, and further preferably 185-190 ℃; the heat preservation time is preferably 0.5-3 h, more preferably 1-2.2 h, and further preferably 1.5-2 h; the heating rate of the temperature to the curing temperature is preferably 3 to 10 ℃/min, and more preferably 5 to 8 ℃/min.
In order to facilitate the friction performance detection of the prepared boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material composite material, before the curing reaction, the invention preferably adopts a phenolic resin adhesive to stick the obtained composite blended fabric on the surface of a metal base material, and then the composite blended fabric is cured; the metal substrate is preferably bearing steel, more preferably 9Cr18Mo, 9Cr18MoV, 9Cr18, 4Cr13 or 17-4 PH. The process of the present invention is not particularly limited, and may be performed according to a process known in the art.
The invention provides a boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material prepared by the preparation method in the technical scheme, which comprises a self-lubricating fabric liner material and a boron carbide-molybdenum disulfide hybrid filler loaded on the self-lubricating fabric liner material.
The invention provides an application of the boron carbide-molybdenum disulfide hybrid filler in the technical scheme in a self-lubricating joint bearing. The method of the present invention is not particularly limited, and the method may be applied according to a method known in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following embodiments, the particle size of the boron carbide is 1 to 10 μm; the relative molecular mass of the polyethyleneimine is 600 or 1200; the fineness of the polytetrafluoroethylene fiber was 400D, and the fineness of the polyimide fiber was 200D.
Example 1
Preparing 250mL of Tris-HCl buffer solution (2mg/mL, pH 8.5), adding 0.5g of boron carbide, performing ultrasonic dispersion uniformly, adding 0.5g of dopamine hydrochloride and 0.5g of polyethyleneimine (molecular weight 600), stirring at room temperature for reaction for 24 hours, sequentially filtering, washing and drying the obtained product, dispersing the obtained product in 60mL of water, adding 0.5g of sodium molybdate and 1g of thiourea, stirring for 0.5 hour, transferring the obtained material to a 100mL reaction kettle, reacting at 200 ℃ for 36 hours, sequentially filtering, washing and drying the obtained product to obtain the boron carbide-molybdenum disulfide hybrid filler;
1g of phenol resin was dispersed in 7mL of an ethanol-ethyl acetate-acetone mixed solvent, ethanol: ethyl acetate: the volume ratio of acetone is 1:1:1, so as to obtain a phenolic resin solution; mixing the phenolic resin solution with 0.005g of boron carbide-molybdenum disulfide hybrid filler, wherein the boron carbide/molybdenum disulfide hybrid accounts for 0.5% of the mass of the phenolic resin, and thus obtaining an impregnation solution;
taking polytetrafluoroethylene fibers as warp yarns and polyimide fibers as weft yarns, weaving the warp yarns and the weft yarns by plain weaving according to the warp density of 400/10 cm and the weft density of 350/10 cm to obtain a polyimide fiber-polytetrafluoroethylene fiber blended fabric, carrying out air plasma modification treatment for 10min at 100W, repeatedly soaking and drying the obtained blended fabric in the soaking solution until the mass fraction of the mixture of the phenolic resin and the boron carbide/molybdenum disulfide hybrid in the obtained composite blended fabric reaches 30%, and obtaining the composite blended fabric;
adhering the composite blended fabric to the surface of a metal base material with the pH of 17-4 by using phenolic resin, heating to 180 ℃ at the heating rate of 5 ℃/min, and curing for 2h under the condition of 0.3MPa to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
Example 2
Preparing 250mL of Tris-HCl buffer solution (2mg/mL, pH 8.5), adding 0.6g of boron carbide, performing ultrasonic dispersion uniformly, adding 1g of dopamine hydrochloride and 1g of polyethyleneimine (molecular weight 1200), stirring at room temperature for 24 hours for reaction, sequentially filtering, washing and drying the obtained product, dispersing the obtained product in 60mL of water, adding 1g of sodium molybdate and 2g of thiourea, stirring for 0.5 hour, transferring the obtained material to a 100mL reaction kettle, reacting at 240 ℃ for 36 hours, sequentially filtering, washing and drying the obtained product to obtain the boron carbide-molybdenum disulfide hybrid filler;
1g of phenol resin was dispersed in 7mL of an ethanol-ethyl acetate-acetone mixed solvent, ethanol: ethyl acetate: the volume ratio of acetone is 1:1:1, so as to obtain a phenolic resin solution; mixing the phenolic resin solution with 0.02g of boron carbide-molybdenum disulfide hybrid filler, wherein the boron carbide/molybdenum disulfide hybrid accounts for 2% of the mass of the phenolic resin, and thus obtaining an impregnation solution;
taking polytetrafluoroethylene fibers as warp yarns and polyimide fibers as weft yarns, weaving by adopting twill weaving according to the warp density of 380 pieces/10 cm and the weft density of 350 pieces/10 cm to obtain a polyimide fiber-polytetrafluoroethylene fiber blended fabric, carrying out air plasma modification treatment for 10min at 100W, repeatedly soaking and drying the obtained blended fabric in the soaking solution until the mass fraction of the mixture of the phenolic resin and the boron carbide/molybdenum disulfide hybrid in the obtained composite blended fabric reaches 25%, and obtaining the composite blended fabric;
adhering the composite blended fabric to the surface of a metal base material with the pH of 17-4 by using phenolic resin, heating to 180 ℃ at the heating rate of 5 ℃/min, and curing for 2h under the condition of 0.3MPa to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
Example 3
Preparing 250mL of Tris-HCl buffer solution (2mg/mL, pH 8.5), adding 0.8g of boron carbide, performing ultrasonic dispersion uniformly, adding 0.8g of dopamine hydrochloride and 0.5g of polyethyleneimine (molecular weight 600), stirring at room temperature for 24 hours for reaction, sequentially filtering, washing and drying the obtained product, dispersing the obtained aminated boron carbide product in 70mL of water, adding 1g of sodium molybdate and 1.5g of thiourea, stirring for 0.5 hour, transferring the obtained material to a 100mL reaction kettle, reacting at 220 ℃ for 36 hours, sequentially filtering, washing and drying the obtained product to obtain a boron carbide-molybdenum disulfide hybrid filler;
1g of phenolic resin was dispersed in 5mL of an ethanol-ethyl acetate-acetone mixed solvent, ethanol: ethyl acetate: the volume ratio of acetone is 1:1:2, so that a phenolic resin solution is obtained; mixing the phenolic resin solution with 0.04g of boron carbide-molybdenum disulfide hybrid filler, wherein the boron carbide/molybdenum disulfide hybrid accounts for 4% of the mass of the phenolic resin, and thus obtaining an impregnation solution;
taking polytetrafluoroethylene fibers as warp yarns and polyimide fibers as weft yarns, weaving by adopting satin weaving according to the warp-wise density of 400/10 cm and the weft-wise density of 350/10 cm to obtain a polyimide fiber-polytetrafluoroethylene fiber blended fabric, carrying out air plasma modification treatment for 15min at 100W, repeatedly impregnating and drying the obtained blended fabric in the impregnating solution until the mass fraction of the mixture of the phenolic resin and the boron carbide/molybdenum disulfide hybrid in the obtained composite blended fabric reaches 30%, and thus obtaining the composite blended fabric;
adhering the composite blended fabric to the surface of a metal base material with the pH of 17-4 by using phenolic resin, heating to 190 ℃ at the heating rate of 5 ℃/min, and curing for 2h under the condition of 0.3MPa to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
Example 4
Preparing 250mL of Tris-HCl buffer solution (2mg/mL, pH 8.5), adding 0.6g of boron carbide, performing ultrasonic dispersion uniformly, adding 0.8g of dopamine hydrochloride and 0.5g of polyethyleneimine (molecular weight 1200), stirring at room temperature for 24 hours for reaction, sequentially filtering, washing and drying the obtained product, dispersing the obtained aminated boron carbide product in 70mL of water, adding 0.5g of sodium molybdate and 1g of thiourea, stirring for 0.5 hour, transferring the obtained material to a 100mL reaction kettle, reacting at 210 ℃ for 36 hours, sequentially filtering, washing and drying the obtained product to obtain the boron carbide-molybdenum disulfide hybrid filler;
1g of phenol resin was dispersed in 10mL of an ethanol-ethyl acetate-acetone mixed solvent, ethanol: ethyl acetate: the volume ratio of acetone is 1:1:1, so as to obtain a phenolic resin solution; mixing the phenolic resin solution with 0.03g of boron carbide-molybdenum disulfide hybrid filler, wherein the boron carbide/molybdenum disulfide hybrid accounts for 3% of the mass of the phenolic resin, and thus obtaining an impregnation solution;
taking polytetrafluoroethylene fibers as warp yarns and polyimide fibers as weft yarns, weaving the warp yarns and the weft yarns by plain weaving according to the warp density of 400/10 cm and the weft density of 300/10 cm to obtain a polyimide fiber-polytetrafluoroethylene fiber blended fabric, carrying out air plasma modification treatment for 10min at 150W, repeatedly soaking and drying the obtained blended fabric in the soaking solution until the mass fraction of the mixture of the phenolic resin and the boron carbide/molybdenum disulfide hybrid in the obtained composite blended fabric reaches 20%, and obtaining the composite blended fabric;
adhering the composite blended fabric to the surface of a metal base material with the pH of 17-4 by using phenolic resin, heating to 180 ℃ at the heating rate of 5 ℃/min, and curing for 2.2h under the condition of 0.2MPa to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
Comparative example 1
The only difference from example 2 is: and omitting the preparation process of the boron carbide-molybdenum disulfide hybrid filler and the mixing process of the boron carbide-molybdenum disulfide hybrid filler and the phenolic resin solution to prepare the self-lubricating fabric liner material which is not loaded with the boron carbide-molybdenum disulfide hybrid filler.
Performance testing
1) The boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material prepared in the examples 1-4 and the self-lubricating fabric liner material of the comparative example 1 are respectively subjected to a friction and wear performance test, and the test method comprises the following steps: the test conditions were: the pressure is 85MPa, the sliding friction linear velocity is 0.26m/s, the time is 120min, the temperature is room temperature, a basalt three-number friction wear testing machine is adopted, No. 45 steel with the diameter of 2mm is used as a friction couple, and the friction coefficient is automatically output after collected data is processed by a connected computer. And measuring the wear depth of the self-lubricating fabric liner material by using a digital display height gauge, and further calculating the wear volume of the fabric liner. Calculating the specific wear rate of the fabric gasket material by adopting a K-delta V/P-L formula, wherein the friction coefficient is automatically derived by an instrument, and the K-specific wear rate; Δ V-wear volume; p-application load; l-sliding distance, the test results obtained are shown in Table 1.
TABLE 1 Friction data for self-lubricating fabric backing materials prepared in examples 1-4 and comparative example 1
Figure BDA0003085042880000111
As can be seen from Table 1, the wear rate of the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric gasket material prepared in example 2 is 0.4X 10-14m3(Nm)-1Compared with comparative example 1, the wear resistance of the self-lubricating fabric liner is reduced by 85.7%, and the wear resistance of the self-lubricating fabric liner is remarkably improved.
FIG. 1 is a graph of wear rate and coefficient of friction for self-lubricating fabric liner materials prepared in comparative example 1 and example 2, wherein (a) is a graph comparing wear rates and (b) is a graph comparing coefficient of friction; as can be seen from FIG. 1, after the self-lubricating fabric liner is reinforced by the boron carbide/molybdenum disulfide hybrid, the wear rate of the fabric liner material is greatly reduced under the condition that the friction coefficient is basically kept unchanged.
2) The surface topography of the polyimide fiber/polytetrafluoroethylene fiber blended fabric and the composite blended fabric prepared in example 1 was measured, and the results are shown in fig. 2, in which (a) is an optical microscopic photograph of the polyimide fiber/polytetrafluoroethylene fiber blended fabric; (b) is an optical microscope photo of the composite blended fabric; as can be seen from fig. 2, after the polyimide fiber/polytetrafluoroethylene fiber blended fabric is immersed in the impregnation liquid of the phenolic resin and the boron carbide-molybdenum disulfide hybrid filler, the mixture of the phenolic resin and the boron carbide/molybdenum disulfide hybrid is coated on the surface of the fabric as a continuous phase.
3) SEM tests were performed on commercially available boron carbide, the aminated boron carbide prepared in example 3 (i.e., boron carbide-polydopamine/polyethyleneimine), and the boron carbide-molybdenum disulfide hybrid prepared in example 3, with the results shown in fig. 3; wherein (a) represents boron carbide; (b) represents aminated boron carbide; (c) represents a boron carbide-molybdenum disulfide hybrid; as can be seen from fig. 3, the surface of pure boron carbide is doped with small-sized boron carbide particles (a); coating a layer of polydopamine/polyethyleneimine copolymer on the surface of the aminated boron carbide, and obviously changing the surface appearance (b); in the boron carbide-molybdenum disulfide hybrid (c), the polydopamine-polyethyleneimine copolymer is coated on the surface of boron carbide particles, and the molybdenum disulfide nano-peanuts grow on the surface of the boron carbide particles.
4) For commercial boron carbide (B)4C) Commercial molybdenum disulfide (MoS)2) Aminated boron carbide prepared in example 4 (boron carbide-polydopamine/polyethyleneimine, B)4C-PDA/PEI) and the boron carbide/molybdenum disulfide hybrid prepared in example 4 (B)4C@MoS2) The results of the respective raman spectroscopy and XRD measurements are shown in fig. 4; wherein, (a) is a Raman spectrum chart of the four materials, and (b) is an XRD (X-ray diffraction) chart of the four materials, and the Raman spectrum and the XRD chart of figure 4 show that the boron carbide/molybdenum disulfide hybrid simultaneously has absorption peaks of boron carbide and molybdenum disulfide, thereby proving that the molybdenum disulfide nanoflowers successfully grow on the surface of boron carbide particles.
5) The self-lubricating fabric liner materials prepared in comparative example 1 and example 4 were subjected to surface topography characterization tests and the results are shown in fig. 5; wherein (a) represents the self-lubricating fabric liner material prepared in comparative example 1 and (b) represents the boron carbide/molybdenum disulfide hybrid reinforced self-lubricating fabric liner material prepared in example 4, it can be seen from fig. 5 that the fabric liner after the boron carbide/molybdenum disulfide hybrid is added appears black.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A preparation method of boron carbide-molybdenum disulfide hybrid filler comprises the following steps:
mixing the boron carbide dispersion liquid, dopamine hydrochloride and polyethyleneimine, and carrying out amination modification reaction to obtain aminated boron carbide;
mixing the aminated boron carbide, water, a molybdenum source and a sulfur source, and hybridizing to obtain a boron carbide-molybdenum disulfide hybrid filler;
the mass ratio of boron carbide, dopamine hydrochloride and polyethyleneimine in the boron carbide dispersion liquid is (0.5-1): 0.5-1); the temperature of the amination modification reaction is room temperature, and the time is 6-24 hours;
the mass ratio of the boron carbide to the molybdenum source to the sulfur source is (0.5-1) to (1-2); the temperature of hybridization is 200-240 ℃, and the time is 12-36 h.
2. The method according to claim 1, wherein the dispersant used for the boron carbide dispersion is a Tris-HCl buffer solution; the concentration of the Tris-HCl buffer solution is 2mg/mL, and the pH value is 8.5; the dosage ratio of the boron carbide to the dispersant in the boron carbide dispersion liquid is (0.5-1) g:250 mL.
3. The method of claim 1, wherein the molybdenum source comprises sodium molybdate, ammonium molybdate, or sodium molybdate; the sulfur source comprises thiourea.
4. The boron carbide-molybdenum disulfide hybrid filler prepared by the preparation method of any one of claims 1 to 3 comprises boron carbide particles, molybdenum disulfide nanoflowers loaded on the surfaces of the boron carbide particles, and a polydopamine-polyethyleneimine copolymer intermediate layer, wherein the intermediate layer is positioned between the boron carbide particles and the molybdenum disulfide nanoflowers.
5. Use of the boron carbide-molybdenum disulfide hybrid filler of claim 4 in a self-lubricating fabric backing composite.
6. A preparation method of a boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material comprises the following steps:
mixing the boron carbide-molybdenum disulfide hybrid filler of claim 4 with a phenolic resin solution to obtain an impregnation solution;
and (3) repeatedly carrying out the processes of dipping and drying on the polyimide fiber-polytetrafluoroethylene fiber blended fabric in the dipping solution, and curing the obtained composite blended fabric to obtain the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material.
7. The preparation method of claim 6, wherein the impregnation-drying process is repeated until the mixture of the phenolic resin and the boron carbide-molybdenum disulfide hybrid filler accounts for 15-40% of the composite blended fabric by mass; the curing pressure is 0.01-3 MPa, the temperature is 150-250 ℃, and the heat preservation time is 0.5-3 h.
8. The boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric liner material prepared by the preparation method of any one of claims 6 to 7, which is characterized by comprising a self-lubricating fabric liner material and a boron carbide-molybdenum disulfide hybrid filler loaded on the self-lubricating fabric liner material.
9. Use of the boron carbide-molybdenum disulfide hybrid reinforced self-lubricating fabric backing material of claim 8 in self-lubricating spherical plain bearings.
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