CN110064575A - A kind of two-dimensional material solid lubricating film and preparation method thereof - Google Patents
A kind of two-dimensional material solid lubricating film and preparation method thereof Download PDFInfo
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- CN110064575A CN110064575A CN201910337782.0A CN201910337782A CN110064575A CN 110064575 A CN110064575 A CN 110064575A CN 201910337782 A CN201910337782 A CN 201910337782A CN 110064575 A CN110064575 A CN 110064575A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
Abstract
The present invention provides a kind of preparation method of two-dimensional material solid lubricating film, it the described method comprises the following steps: by two-dimensional material dispersion in workpiece surface, the workpiece is dried after coating, adhesive force promotion processing is carried out to the workpiece after drying, i.e., obtains the two-dimensional material solid lubricating film in the workpiece surface.The preparation method has many advantages, such as that low in cost, raw material sources are extensive, prepared film thickness is controllable, stability is high, adhesion property is good, good mechanical property, dense uniform, surfacing, purity is higher, coefficient of friction is smaller, it is still able to maintain excellent greasy property under the extreme conditions such as ultrahigh vacuum, high speed, high temperature and pressure, heavy duty, has a good application prospect in fields of industrial manufacturing such as machining, aerospace, material and opto-electronic devices.
Description
Technical field
The invention belongs to lubricant coating preparation technical field, it is related to a kind of two-dimensional material solid lubricating film and its preparation side
Method.
Background technique
The arrival in modern industrialization epoch is also faced with resource exhaustion and the challenge of energy crisis.Mechanical equipment it is continuous
Often there is fretting wear phenomenons for operating, and according to statistics, more than the disposable energy in 1/3 world, therefore fretting wear has lost
It is imperative to research and develop new lubriation material.Lubriation material is broadly divided into gaseous state, liquid, semisolid and solid according to form and moistens at present
Sliding material.With flourishing for the Space Causes such as China's aerospace, it is true that traditional lubriation material can no longer meet superelevation
Application demand under the extreme environmental conditions such as sky, high speed, heavy duty, high temperature and pressure, therefore lubriation material and its technology of preparing are mentioned
Higher requirement is gone out.Solid lubricating film due to excellent space adaptability, low-friction coefficient and high-wear resistance,
And various extreme environmental conditions can be successfully managed, in fields such as machining, aerospace, material and opto-electronic devices
There is actual application.
Two-dimensional material is from being found 2004, just by the concern of industry and academia.Due in its layer with relatively strong
Chemistry key connection, and interlayer is combined with weak Van der Waals force, so that the shear strength of interlayer is lower, interlayer is easily sheared
Sliding, therefore there is low friction characteristic and self-lubricating property.In addition, the friction between two-dimensional material film and friction pair can turn
The friction of interlayer inside two-dimensional material, and when the size of two-dimensional material is sufficiently small (20 nanometers of <) are turned to, nanoparticle can
Finely to repair the coarse position of surface of friction pair, the fretting wear as caused by workpiece surface roughness is reduced, thus effectively
Coefficient of friction and wear rate are reduced, achievees the purpose that lubrication.
Two-dimensional material composite lubricating film preparation method mainly includes that mull technique, thermal spraying, plating, chemical plating, gas phase are heavy at present
Product etc..Mull technique has many advantages, such as at low cost, simple process, but there are the binding forces of film and substrate poor, surface roughness
The disadvantages of big, will cause large effect to its tribological property.The adaptable strong, material of hot spray process selects wide, coating
The advantages that thickness is controllable, but there is also coatings and substrate binding performance is poor, surface roughness is big disadvantage.Plating and chemical plating tool
Have the shortcomings that energy consumption is high, pollution is big, seriously limits their application and development.In recent years, gas phase deposition technology has become
The method for manufacturing thin film of comparative maturity.Nanoscale, 2018,10,19979-19986 method systems deposited using pulse laser
The standby coating with ultralow friction coefficient, coefficient of friction under vacuum environment is down to 0.004-0.006.CN107815645A is public
The preparation method for having opened a kind of low-friction coefficient molybdenum-disulfide radical metal composite solid lubricant film, first in substrate surface pre-deposition
Then the pre- binder course of Ti or Al carries out magnetron sputtering to metal targets and molybdenum disulfide target to get two sulphur of low-friction coefficient is arrived
Change molybdenum base metal composite solid lubricant film.CN104928622A discloses a kind of preparation side of tungsten disulfide solid lubricant film
Method, this method are thin in the surface of metal material matrix formation tungsten disulfide solid lubricant using Magnetically filtered vacuum arc deposition
Film.CN101398123A utilizes double-target radio frequency sputtering technology alternating deposit tungsten layer and molybdenum layer, then should by low temperature ion sulfuration
Tungsten/molybdenum multilayer film is prepared for tungsten disulfide/molybdenum disulfide solid lubrication multilayer film.It is solid that CN1114984A discloses a kind of cosputtering
Body composite lubricating film and preparation method thereof, prepared film have low-friction coefficient, excellent mechanical characteristic, longer wear-resisting longevity
Life and good humidity air characteristics.But gas phase deposition technology is generally relatively high to the requirement of equipment, condition requires ratio
Harsher, this just results in the raising of production cost significantly, therefore also limits its further development.CN106544668A is public
The preparation method for having opened a kind of molybdenum disulfide solid lubricating film, by handling first substrate surface, then by two sulphur
Change molybdenum powder and is placed into the unidirectional reciprocal opposite grinding of progress between substrate, the available and compact film of substrate.This method is suitable
Quickly prepared in large area, but there are film compactness it is poor, waste of material is serious the disadvantages of.
So far, still lack one kind and not only met simple, efficient, inexpensive technique requirement, but also be able to satisfy film thickness
Degree is controllable, stability is high, adhesion property is good, good mechanical property, dense uniform, surfacing, purity is higher, coefficient of friction is smaller
The two-dimensional material solid lubricating film preparation method of equal quality requirements, just there is an urgent need to this technologies of Devoting Major Efforts To Developing for this, thus real
Breakthrough in existing technology of preparing, to accelerate its practical application.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of two-dimensional material solid lubricating film and preparation method thereof, institute
Stating preparation method has many advantages, such as that easy to operate, low in cost, raw material sources are extensive, can prepare gradient, compound and multilayer
Membrane structure, prepared film thickness is controllable, stability is high, adhesion property is good, good mechanical property, dense uniform, surface
It is smooth, purity is higher, coefficient of friction is smaller, be still able to maintain under the extreme conditions such as ultrahigh vacuum, high speed, high temperature and pressure, heavy duty
Excellent greasy property has good in fields of industrial manufacturing such as machining, aerospace, material and opto-electronic devices
Application prospect.
In order to achieve the above objectives, the invention adopts the following technical scheme:
It is an object of the present invention to provide a kind of preparation methods of two-dimensional material solid lubricating film, which is characterized in that
It the described method comprises the following steps:
Two-dimensional material dispersion is dried the workpiece after workpiece surface, coating, to described after drying
Workpiece carries out adhesive force promotion processing, i.e., obtains the two-dimensional material solid lubricating film in workpiece surface.
It is repeated at least once more after the workpiece is dry by the two-dimensional material as currently preferred technical solution
The step of dispersion is dried the workpiece after workpiece surface, coating adheres to the workpiece after dry
Power promotion processing, i.e., obtain at least two layers compound two-dimensional material solid lubricating film in the workpiece surface.
As currently preferred technical solution, the two-dimensional material includes graphite, hexagonal boron nitride, two sulphur of transition metal
In compounds of group, two-dimentional transition metal carbide, nitride or carbonitride, graphite phase carbon nitride or black phosphorus any one or
At least two combination.
Preferably, the transition metal in two chalcogenide of transition metal be the periodic table of elements in IVB, VB, VIB,
In VIIB or VIII group element any one or at least two combination.
Preferably, the chalcogen in two chalcogenide of transition metal is any one in S, Se or Te element
Or at least two combination.
Preferably, the chemical composition of the two-dimentional transition metal carbide, nitride or carbonitride is Mn+1Xn, wherein M
For in transition metal Ti, V, Cr or Nb element any one or at least two combination；X is C element, N element or first for C
Element and N element；N is 1,2 or 3.
Preferably, the size of the two-dimensional material is 1nm~5 μm, such as 1nm, 5nm, 10nm, 50nm, 0.1 μm, 1 μm or 5 μ
M etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable, and preferably 1nm~
500nm。
Preferably, the number of plies of the two-dimensional material is 1~10000 layer, such as 1 layer, 5 layers, 10 layers, 50 layers, 100 layers, 200
Layer, 300 layers, 400 layers, 550 layers, 700 layers, 1000 layers, 1200 layers, 1500 layers, 2000 layers, 2500 layers, 3000 layers, 4500 layers,
6000 layers, 7000 layers, 8000 layers, 9000 layers or 10000 layers etc., it is not limited to cited numerical value, in the numberical range
Other unlisted numerical value are equally applicable.
The size of the two-dimensional material and the number of plies can quality to film and greasy property generate large effect.Preferably
Size and the number of plies can guarantee the quality of prepared film, and the friction between two-dimensional material film and friction pair is effective
It is converted into the friction of interlayer inside two-dimensional material, and finely repairs the coarse position of surface of friction pair, is rubbed to be effectively reduced
Coefficient and wear rate are wiped, achievees the purpose that lubrication.
As currently preferred technical solution, which is characterized in that the solvent of the two-dimensional material dispersion liquid includes N- first
Base pyrrolidones, n-vinyl pyrrolidone, N- cyclohexyl pyrrolidone, n-octylpyrrolidone, N- dodecyl pyrrolidine
Ketone, gamma-butyrolacton, formamide, N-METHYLFORMAMIDE, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl are sub-
Sulfone, benzene, chlorobenzene, bromobenzene, benzonitrile, benzaldehyde, Ergol, benzyl ether, tetrahydrofuran, acetone, butanone, methanol, ethyl alcohol,
In isopropanol or water any one or at least two combination, the combination is typical but non-limiting example has: N- methyl pyrrole
The combination of pyrrolidone and n-vinyl pyrrolidone, the combination of N-Methyl pyrrolidone and N- cyclohexyl pyrrolidone, N- octyl
The combination of pyrrolidones and N-dodecylpyrrolidone, the combination of formamide and N-METHYLFORMAMIDE, N, N- dimethyl formyl
The combination of amine and n,N-dimethylacetamide, the combination of dimethyl sulfoxide and ammonium hydroxide, N-Methyl pyrrolidone, N- vinyl pyrrole
The combination of alkanone and N- cyclohexyl pyrrolidone, the combination of first alcohol and water, second alcohol and water combination, N-Methyl pyrrolidone and second
The combination of alcohol or n-octylpyrrolidone, the combination of first alcohol and water etc..
Preferably, the concentration of the two-dimensional material dispersion liquid be 0.1~50mg/mL, as 0.1mg/mL,
1mg/mL、5mg/mL、10mg/mL、12.5mg/mL、15mg/mL、20mg/mL、25mg/mL、30mg/mL、35mg/
ML, 38mg/mL, 40mg/mL, 45mg/mL or 50mg/mL etc., it is not limited to cited numerical value, in the numberical range its
His unlisted numerical value is equally applicable, preferably 1~20mg/mL.
Preferred type of solvent can guarantee that two-dimensional material is evenly dispersed in a solvent in the present invention, not occur significantly to roll into a ball
Poly-, this can cause very big influence to the quality of film, further influence its greasy property.The two-dimensional material dispersion liquid it is dense
When degree is less than 0.1mg/mL, dispersion liquid concentration is lower, and the film of known thickness to be obtained needs duplicate number more, so that
Technique becomes complicated, against the original intention being simple and efficient；When the concentration of the two-dimensional material dispersion liquid is greater than 50mg/mL, dispersion liquid
Reach hypersaturated state, causes the waste of material.
As currently preferred technical solution, the preparation method of the two-dimensional material dispersion liquid includes: by two-dimensional material
It is mixed with solvent and ultrasonic.
Preferably, the power of the ultrasound be 50~1000W, as 50W, 100W, 200W, 300W, 400W, 500W, 600W,
700W, 800W, 900W or 1000W etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range
It is equally applicable, preferably 100~500W.
When the power of ultrasound of the present invention is less than 50W, power is too low, and ultrasonic effect is unobvious；The power of the ultrasound
When greater than 1000W, two-dimensional material dispersion liquid has reached stable state, will cause the waste of the energy, at the beginning of energy-efficient
Inner feelings.
Preferably, the time of the ultrasound be 0.5~120h, as 0.5h, 1h, 5h, 10h, 20h, 30h, 40h, 50h,
60h, 70h, 80h, 90h, 100h, 110h or 120h etc., it is not limited to cited numerical value, in the numberical range, other are not
The numerical value enumerated is equally applicable, preferably 1~50h.
When the time of ultrasound of the present invention is less than 0.5h, the time is too short, and ultrasonic effect is unobvious；The time of the ultrasound
When greater than 120h, two-dimensional material dispersion liquid has reached stable state, will cause the waste of the energy, at the beginning of energy-efficient
Inner feelings.
Preferred ultrasonic power can guarantee that two-dimensional material is evenly dispersed in a solvent with the time and not reunite significantly, from
And the preferable solid lubricating film of quality is obtained, and then play excellent greasy property.
As currently preferred technical solution, the method for the coating includes that drop coating, spin coating, dip-coating, spraying or electricity are heavy
One of product or at least two combination, combination typical case but non-limiting example has: the combination of drop coating and spin coating, dip-coating
Combination or spin coating, the combination of dip-coating and spraying with spraying combination, dip-coating and electro-deposition etc..
As currently preferred technical solution, the material of the workpiece includes metal and/or nonmetallic.
Preferably, the metal includes iron and ferroalloy, aluminium and aluminium alloy, copper and copper alloy, titanium or titanium alloy, magnesium and magnesium
In alloy, bearing metal or hard alloy any one or at least two combination.Wherein, the combination can be the conjunction of copper aluminium
Gold, ferroaluminium, ferro-titanium, magnesium alloy etc..
Preferably, described nonmetallic including any one in glass, ceramics, carbon simple substance, rock, timber, plastics or rubber
Kind or at least two combination, the combination is typical but non-limiting example has: combination, ceramics and the carbon simple substance of glass and ceramics
Combination, the combination of rock and timber, the combination of timber and plastics or rubber and the combination of ceramics etc..Wherein, described combine is
The composite material that any at least two material passes through the compound formation of either method.
As currently preferred technical solution, the surface of the workpiece is plane and/or curved surface.
As currently preferred technical solution, the method for the drying includes vacuum drying, air drying, heating drying
Any one in freeze-drying or at least two combination, the combination is typical but non-limiting example has: vacuum drying with
The heat up dry combination of dry combination, vacuum drying and the combination of air drying, freeze-drying and heating, heating is dry and cold
Dry combination or vacuum drying is lyophilized, heating is dried and frozen dry combination etc..
As currently preferred technical solution, the method that the adhesive force promotes processing includes hot pressing, solvent post-processing
In thermal annealing any one or at least two combination, the combination is typical but non-limiting example has: hot pressing and solvent
Combination, solvent post-processing and combination or hot pressing and the combination of thermal annealing of thermal annealing of post-processing etc..
Preferably, the temperature of the hot pressing is 50~1000 DEG C, such as 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, 300 DEG C, 400
DEG C, 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C or 1000 DEG C etc., it is not limited to cited numerical value, the numerical value model
Other unlisted numerical value are equally applicable in enclosing, and preferably 100~800 DEG C.
Preferably, the solvent post-processing is that pure solvent is coated on workpiece surface, is carried out after coating to the workpiece
It is dry.Pure solvent can be penetrated into spontaneously inside film, repair the defect inside film, so that membrane pores rate is reduced and caused
Densification, and be compacted film using the effect of gravity, to improve adhesion of thin film.
Preferably, the solvent that the solvent post-processing uses includes N-Methyl pyrrolidone, n-vinyl pyrrolidone, N-
Cyclohexyl pyrrolidone, n-octylpyrrolidone, N-dodecylpyrrolidone, gamma-butyrolacton, formamide, N- methyl formyl
Amine, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, benzene, chlorobenzene, bromobenzene, benzonitrile, benzaldehyde, benzene
Any one in benzyl formate, benzyl ether, tetrahydrofuran, acetone, butanone, methanol, ethyl alcohol, isopropanol or water or at least two
Combination, the combination is typical but non-limiting example has: the combination of N-Methyl pyrrolidone and n-vinyl pyrrolidone, N-
The combination of methyl pyrrolidone and N- cyclohexyl pyrrolidone, n-octylpyrrolidone and N-dodecylpyrrolidone group
Conjunction, formamide and the combination of N-METHYLFORMAMIDE, the combination of n,N-Dimethylformamide and n,N-dimethylacetamide, dimethyl
The combination of sulfoxide and ammonium hydroxide, N-Methyl pyrrolidone, n-vinyl pyrrolidone and N- cyclohexyl pyrrolidone combination, methanol
The combination of combination, second alcohol and water, the combination of N-Methyl pyrrolidone and ethyl alcohol or n-octylpyrrolidone, first alcohol and water with water
Combination etc..
Preferably, the temperature of the thermal annealing be 50~1000 DEG C, such as 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, 300 DEG C,
400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C or 1000 DEG C etc., it is not limited to cited numerical value, the numerical value
Other unlisted numerical value are equally applicable in range, and preferably 100~800 DEG C.
Preferred adhesive force, which promotes the method for processing and parameter, can significantly improve prepared film in workpiece surface
Mechanical performance, while making film obtain superior apparent mass and stability, and then improve its greasy property.
The second purpose of the present invention is to provide the two-dimensional material solid profits that any of the above-described kind of preparation method of one kind is prepared
Sliding film.
Preferably, the solid lubricating film with a thickness of 1nm~1mm, such as 1nm, 10nm, 100nm, 500nm, 1 μm, 5 μ
M, 10 μm, 50 μm, 100 μm, 200 μm, 300 μm, 400 μm, 550 μm, 700 μm, 1mm etc., it is not limited to cited number
Value, other interior unlisted numerical value of the numberical range are equally applicable, preferably 100nm~100 μm.
Compared with prior art, the present invention at least has the advantages that
(1) present invention provides a kind of two-dimensional material solid lubricating film and preparation method thereof, and the preparation method is at low cost
It is honest and clean, raw material sources are extensive；
(2) present invention provides a kind of two-dimensional material solid lubricating film and preparation method thereof, and the preparation method is prepared into
The two-dimensional material solid lubricating film thickness arrived is controllable, stability is high, adhesion property is good, good mechanical property, dense uniform, surface
It is smooth, purity is higher, coefficient of friction is smaller and space adaptability is good；
(3) present invention provides a kind of two-dimensional material solid lubricating film and preparation method thereof, the preparation method technique letter
Singly, the problem of efficiently, overcoming the prior art at high cost, complex process, has a good application prospect.
Detailed description of the invention
Fig. 1 a is the disk bearing steel workpiece photo in embodiment 1；
Fig. 1 b is the ball bearing steel workpiece photo in embodiment 1；
Fig. 2 a is the obtained photo coated with molybdenum disulfide solid lubricating film disk bearing steel workpiece of embodiment 1；
Fig. 2 b is the obtained photo coated with molybdenum disulfide solid lubricating film ball bearing steel workpiece of embodiment 1；
Fig. 3 is the microscope figure that the obtained molybdenum disulfide solid lubricating film (disc surfaces) of embodiment 1 amplifies 10 times
Piece；
Fig. 4 a is the obtained photo coated with boron nitride solids composite lubricating film disk bearing steel workpiece of embodiment 2；
Fig. 4 b is the obtained photo coated with boron nitride solids composite lubricating film ball bearing steel workpiece of embodiment 2；
Fig. 5 a is the obtained photo coated with graphene solid lubricating film disk bearing steel workpiece of embodiment 3；
Fig. 5 b is the obtained photo coated with graphene solid lubricating film ball bearing steel workpiece of embodiment 3.
The present invention is described in more detail below.But following examples is only simple example of the invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, of the invention is typical but non-limiting
Embodiment is as follows:
Embodiment 1
The molybdenum disulfide that 1g average grain diameter is 5nm is added in 100mL acetone, with the ultrasonic power ultrasound 120h of 50W.
In sample 5mL drop coating to bearing steel workpiece after taking ultrasound, solvent volatilization is made by way of 100 DEG C of heat dryings completely, weight
Multiple above-mentioned steps 5 times, 1mL n,N dimethylformamide (DMF) is then sprayed into film surface, spontaneously dries it completely,
It is finally handled 1 hour by 200 degree of vacuum annealings, the molybdenum disulfide solid lubricating film that thickness is about 100 μm can be obtained.
Fig. 1 a is the disk bearing steel workpiece photo in embodiment 1；
Fig. 1 b is the ball bearing steel workpiece photo in embodiment 1；
Fig. 2 a is the obtained photo coated with molybdenum disulfide solid lubricating film disk bearing steel workpiece of embodiment 1；
Fig. 2 b is the obtained photo coated with molybdenum disulfide solid lubricating film ball bearing steel workpiece of embodiment 1；
It can be seen that disk (plane) and ball (curved surface) bearing steel workpiece surface can prepare two sulphur from Fig. 2 a and Fig. 2 b
Change molybdenum solid lubricating film, prepared film purity is higher, surfacing, and stability is high.It is not bright after the experiment of ball disk opposite grinding
Aobvious trace residual, shows higher mechanical performance.
Fig. 3 is the microscope figure that the obtained molybdenum disulfide solid lubricating film (disc surfaces) of embodiment 1 amplifies 10 times
Piece, it can be seen that prepared molybdenum disulfide solid lubricating film dense uniform, surfacing, adhesion are good.
Embodiment 2
The boron nitride that 1g average grain diameter is 400nm is added in 100mL isopropanol, with the ultrasonic power ultrasound of 250W
100h.Sample 5mL after taking ultrasound is sprayed on bearing steel workpiece, is evaporated completely solvent by way of 250 DEG C of heat dryings
Entirely, it repeats the above steps 5 times, finally handles 1 hour, can be obtained on bearing steel workpiece surface by 200 DEG C of vacuum annealings
The boron nitride solids composite lubricating film that thickness is about 100 μm.
Fig. 4 a is the obtained photo coated with boron nitride solids composite lubricating film disk bearing steel workpiece of embodiment 2；
Fig. 4 b is the obtained photo coated with boron nitride solids composite lubricating film ball bearing steel workpiece of embodiment 2.
It can be seen that disk (plane) and ball (curved surface) bearing steel workpiece surface can prepare nitridation from Fig. 4 a and Fig. 4 b
Boron solid lubricating film, prepared film very high purity, surfacing, stability are high.Without obvious after the experiment of ball disk opposite grinding
Trace residual, shows higher mechanical performance.
Embodiment 3
The graphene that 1g average grain diameter is 100nm is added in 100mL N-Methyl pyrrolidone (NMP), with 250W's
Ultrasonic power ultrasound 100h.Sample 5mL after taking ultrasound is sprayed on bearing steel workpiece, by way of 250 DEG C of heat dryings
Make solvent volatilization completely, repeat the above steps 10 times, is finally handled 1 hour by 200 DEG C of vacuum annealings, it can be in bearing steel
Workpiece surface obtains the graphene solid lubricating film that thickness is about 200 μm.
Fig. 5 a is the obtained photo coated with graphene solid lubricating film disk bearing steel workpiece of embodiment 3；
Fig. 5 b is the obtained photo coated with graphene solid lubricating film ball bearing steel workpiece of embodiment 3.
It can be seen that disk (plane) and ball (curved surface) bearing steel workpiece surface can prepare graphite from Fig. 5 a and Fig. 5 b
Alkene solid lubricating film, prepared film very high purity, surfacing, stability are high.Without obvious after the experiment of ball disk opposite grinding
Trace residual, shows higher mechanical performance.
Embodiment 4
In addition to bearing steel is changed to titanium alloy, other preparation methods and condition are same as Example 1, can be in titanium alloy work
Part surface obtains molybdenum disulfide solid lubricating film.
Experimental example 5
Using the omnipotent friction and wear test instrument of Burker UMT-3 high temperature to molybdenum disulfide solid lubrication made from embodiment 1
Film carries out frictional behaviour test, and vacuum environment, friction velocity 240mm/min, application load is 100N, and temperature is set as 80
DEG C, measuring coefficient of friction is about 0.02.Vacuum test illustrates that the space of molybdenum disulfide solid lubricating film made from embodiment 1 is suitable
Answering property is good.
Experimental example 6
Boron nitride solids made from embodiment 2 are lubricated using Burker UMT-3 high temperature omnipotent friction and wear test instrument thin
Film carries out frictional behaviour test, friction velocity 400mm/min, and application load is 500N, and temperature is set as 1000 DEG C, measures friction
Coefficient is about 0.1.Its coefficient of friction is tested at 1000 DEG C still down to 0.1, and it is good to illustrate that it has high-temperature stability.
Experimental example 7
It is thin to graphene solid lubrication made from embodiment 3 using the omnipotent friction and wear test instrument of Burker UMT-3 high temperature
Film carries out frictional behaviour test, friction velocity 800mm/min, and application load is 200N, and temperature is set as 500 DEG C, measures friction
Coefficient is about 0.05.
The Applicant declares that the present invention is explained by the above embodiments detailed construction feature of the invention, but the present invention is simultaneously
It is not limited to above-mentioned detailed construction feature, that is, does not mean that the present invention must rely on above-mentioned detailed construction feature and could implement.Institute
Belong to those skilled in the art it will be clearly understood that any improvement in the present invention, to the equivalence replacement of component selected by the present invention
And increase, selection of concrete mode of accessory etc., all of which fall within the scope of protection and disclosure of the present invention.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of two-dimensional material solid lubricating film, which is characterized in that the described method comprises the following steps:
Two-dimensional material dispersion is dried the workpiece after workpiece surface, coating, to the workpiece after drying
Adhesive force promotion processing is carried out, i.e., obtains the two-dimensional material solid lubricating film in the workpiece surface.
2. preparation method according to claim 1, which is characterized in that after the workpiece is dry, be repeated at least once more by
The step of two-dimensional material dispersion is dried the workpiece after workpiece surface, coating, to described after drying
Workpiece carries out adhesive force promotion processing, i.e., it is thin to obtain at least two layers compound two-dimensional material solid lubrication in the workpiece surface
Film.
3. preparation method according to claim 1 or 2, which is characterized in that the two-dimensional material includes graphite, six sides nitridation
Boron, two chalcogenide of transition metal, two-dimentional transition metal carbide, nitride or carbonitride, graphite phase carbon nitride or black
In phosphorus any one or at least two combination；
Preferably, the transition metal in two chalcogenide of transition metal is IVB, VB, VIB, VIIB in the periodic table of elements
In VIII group element any one or at least two combination；
Preferably, the chalcogen in two chalcogenide of transition metal be S, Se or Te element in any one or extremely
Few two kinds of combination；
Preferably, the chemical composition of the two-dimentional transition metal carbide, nitride or carbonitride is Mn+1Xn, wherein M be
Cross in metal Ti, V, Cr or Nb element any one or at least two combination；X is C element, N element or for C element and
N element；N is 1,2 or 3；
Preferably, the size of the two-dimensional material is 1nm~5 μm, preferably 1nm~500nm；
Preferably, the number of plies of the two-dimensional material is 1~10000 layer.
4. preparation method according to claim 1-3, which is characterized in that the solvent of the two-dimensional material dispersion liquid
Including N-Methyl pyrrolidone, n-vinyl pyrrolidone, N- cyclohexyl pyrrolidone, n-octylpyrrolidone, N- dodecane
Base pyrrolidones, gamma-butyrolacton, formamide, N-METHYLFORMAMIDE, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, two
Methyl sulfoxide, benzene, chlorobenzene, bromobenzene, benzonitrile, benzaldehyde, Ergol, benzyl ether, tetrahydrofuran, acetone, butanone, first
In alcohol, ethyl alcohol, isopropanol or water any one or at least two combination；
Preferably, the concentration of the two-dimensional material dispersion liquid is 0.1~50mg/mL, preferably 1~20mg/mL.
5. preparation method according to claim 1-4, which is characterized in that the preparation of the two-dimensional material dispersion liquid
Method includes: that two-dimensional material is mixed to simultaneously ultrasound with solvent；
Preferably, the power of the ultrasound is 50~1000W, preferably 100~500W；
Preferably, the time of the ultrasound is 0.5~120h, preferably 1~50h；
Preferably, the method for the coating includes one of drop coating, spin coating, dip-coating, spraying or electro-deposition or at least two
Combination.
6. preparation method according to claim 1-5, which is characterized in that the material of the workpiece includes metal
And/or it is nonmetallic；
Preferably, the metal includes that iron and ferroalloy, aluminium and aluminium alloy, copper and copper alloy, titanium or titanium alloy, magnesium and magnesium close
In gold, bearing metal or hard alloy any one or at least two combination；
Preferably, it is described it is nonmetallic including in glass, ceramics, carbon simple substance, rock, timber, plastics or rubber any one or
At least two combination.
7. preparation method according to claim 1-6, which is characterized in that the surface of the workpiece be plane and/
Or curved surface.
8. preparation method according to claim 1-7, which is characterized in that the method for the drying includes that vacuum is dry
Dry, air drying, heating be dry or freeze-drying in any one or at least two combination.
9. preparation method according to claim 1-8, which is characterized in that the method that the adhesive force promotes processing
Including hot pressing, solvent post-processing or thermal annealing in any one or at least two combination；
Preferably, the temperature of the hot pressing is 50~1000 DEG C, preferably 100~800 DEG C；
Preferably, the solvent that the solvent post-processing uses includes N-Methyl pyrrolidone, n-vinyl pyrrolidone, N- hexamethylene
Base pyrrolidones, n-octylpyrrolidone, N-dodecylpyrrolidone, gamma-butyrolacton, formamide, N-METHYLFORMAMIDE, N,
Dinethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide, benzene, chlorobenzene, bromobenzene, benzonitrile, benzaldehyde, benzoic acid
In benzyl ester, benzyl ether, tetrahydrofuran, acetone, butanone, methanol, ethyl alcohol, isopropanol or water any one or at least two group
It closes；
Preferably, the temperature of the thermal annealing is 50~1000 DEG C, preferably 100~800 DEG C.
10. a kind of two-dimensional material solid lubricating film, which is characterized in that the solid lubricating film is any by claim 1~9
Item the method is prepared；
Preferably, the solid lubricating film with a thickness of 1nm~1mm, preferably 100nm~100 μm.
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