CN105441870B - A kind of high rigidity, low-friction coefficient, the properties of solid self-lubricant coating of low wear rate - Google Patents
A kind of high rigidity, low-friction coefficient, the properties of solid self-lubricant coating of low wear rate Download PDFInfo
- Publication number
- CN105441870B CN105441870B CN201410407656.5A CN201410407656A CN105441870B CN 105441870 B CN105441870 B CN 105441870B CN 201410407656 A CN201410407656 A CN 201410407656A CN 105441870 B CN105441870 B CN 105441870B
- Authority
- CN
- China
- Prior art keywords
- lubricant coating
- properties
- tib
- solid self
- coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Lubricants (AREA)
Abstract
The invention provides a kind of new TiB2‑WS2Properties of solid self-lubricant coating and preparation method thereof.The coating is by hard phase TiB2With lubricating phase WS2Two-phase is combined, and has fibrous growth structure.The lubricant coating has good wearability and high rigidity, it can be used on a variety of matrixes or workpiece, the friction, lubrication effect being adapted under the special operation conditions such as vacuum, intense radiation and high-speed motion, and preparation method is simple, it is workable, controllability is good, is easy to industrialized production, there is preferable economic benefit.
Description
Technical field
The invention belongs to solid lubricant coating field.Specifically, had concurrently the invention provides a kind of low-friction coefficient high hard
Properties of solid self-lubricant coating of degree and preparation method thereof.
Background technology
With the development of modern processing manufacturing industry, increasing object needs to rub to be born in superhigh temperature, ultralow temperature, height
Worked under the special operation conditions such as lotus, high vacuum, intense radiation and high-speed motion, therefore the requirement of harshness is proposed to lubriation material.Pass
The lubricating oil of system, lubricating grease due to environmental pollution it is big, it is volatile, cannot be used for the shortcomings of vacuum environment and be difficult to meet special work
Requirement under condition, therefore it is significant to develop solid lubricant coating.
It is preferable that solid lubricant coating refers to that coating coating in the presence of unlubricated liquid or lubricating grease has in itself
Greasy property (performance indications be low-friction coefficient, low wear rate) is so as to realizing the use under special operation condition.Solid lubrication applies
Layer is typically by softer metal such as Ag, Pb, Sn, In etc., or graphite, MoS by layer structure2、WS2、MoSe2、WSe2, BN etc.,
And the lubriation material such as part of the metal oxide, fluoride, phosphate composition.These lubriation materials are general all softer, rubbed
These lubriation materials can not only adhere to object in journey or the surface of workpiece forms solid lubricant film, and can be in antithesis material
Expect that surface forms transfer membrane, friction occurred to reduce friction inside lubricant, reduced abrasion, so as to play lubrication.
Prior art is using coating technique that these lubriation materials are single or be deposited on the surface shape of workpiece in combination
Improve the greasy property of friction surface into lubricant coating, but this kind of method requires very strict to matrix or workpiece surface,
Ask matrix or workpiece surface that there is higher hardness.If matrix hardness is low, friction surface can occur in the presence of bearing capacity
Microprotrusion and penetrate softer lubricant coating so that rubbing action occurs between matrix, lubricant coating will not play any work
With.Therefore the crucial part of solid lubrication is exactly one layer of softer lubricant coating of formation on hard substrate, referred to as " soft+hard "
Structure.As Wang by magnetron sputtering method Rockwell hardness be 42 carbon steel on deposited one layer of WS2- Ag nano combined painting
Layer, discovery have certain frictional behaviour.
Although above-mentioned solid lubricant coating technology has obtained larger development, to coated substrate or workpiece material
Selection requires very tight, and matrix or workpiece material must possess higher hardness.In order to overcome this technical deficiency, solid is widened
The scope of application of lubricant coating.Such as United States Patent (USP) US4826365, US8349474B2 document etc. is sunk on hard coat
One layer of lubricating layer of product prepare the multilayer or laminated construction of lubricating layer and hard layer, utilizes the lubricity and hard layer of lubricating layer
The method that anti-load is combined overcomes above-mentioned deficiency, but this method preparation technology complexity, equipment requirement height, poor repeatability,
Coating Costco Wholesale is high.Secondly, the multilayer of this " soft+hard " or the properties of solid self-lubricant coating of laminated construction, softer lubricating layer
It is easy to be consumed in friction process, and causes coating poor lubricity wear rate high, not wear-resisting.
In summary, this area still lacks a kind of properties of solid self-lubricant coating, the coating itself just have higher hardness and
Have preferable greasy property concurrently, and preparation technology is simple, can be in a variety of matrixes or workpiece surface as wear-resisting lubricant coating.
The content of the invention
It is an object of the invention to provide a kind of new properties of solid self-lubricant coating of excellent performance and preparation method thereof.
The first aspect of the present invention provides a kind of properties of solid self-lubricant coating, and the coating includes hard phase TiB2And lubrication
Phase WS2。
In another preference, described solid lubricant coating is in fibrous growth structure, and coating is fine and close, electrical resistivity range
For the μ Ω .cm of 70 μ Ω .cm~135.
In another preference, the total atom number based on properties of solid self-lubricant coating, described solid lubricant coating each element
Atomic percent be：
16.5at%~24.5at% Ti；
47.1at%~67.7at% B；
5.5at%~14.0at% W；
1.7at%~5.8at% S.
In another preference, other impurities (or impurity element) content is 1.7at%~5.8at%.
In another preference, described impurity element includes O, H, C.
In another preference, the TiB of described solid lubricant coating hard phase2The mass fraction for accounting for whole coating is
40wt%~63wt%.
In another preference, hard phase TiB in solid lubricant coating of the present invention2For crystal structure, phase is lubricated
WS2For non crystalline structure.
In another preference, hard phase TiB in described solid lubricant coating2Crystallite dimension is in 50nm~100nm.
In another preference, described hard phase TiB2Particle be made up of multiple crystal grain, the size of wherein crystal grain is
20nm~100nm, preferably 20nm~40nm.
In another preference, the solid lubricant coating is tested in the range of 2 θ=20 °~70 ° using X-ray diffraction method
There is TiB in 28.5 ° and 58.5 °2Diffraction maximum (0001) and (0002).
In another preference, the X-ray diffractogram of described properties of solid self-lubricant coating is as shown in Figure 4 or basic such as Fig. 4
It is shown, preferably Fig. 4 (b) or the structure shown in 4 (c).
In another preference, described properties of solid self-lubricant coating has following one or more features：
(a) 1.5 μm~4.5 μm of coating layer thickness；
(b) conductivity scope is the μ Ω .cm of 70 μ Ω .cm~200 μ Ω .cm, preferably 70 μ Ω .cm~135；
(c) surface roughness Ra≤10nm of coating, preferably Ra≤5nm；
(d) surface topography of coating is scanned using atomic force ESEM, is presented as shown in Fig. 3 (a) or 3 (b) or basic
Above as shown in Fig. 3 (a) or 3 (b), the pattern preferably shown in Fig. 3 (a).
In another preference, the frictional behaviour of properties of solid self-lubricant coating shows that coefficient of friction is 0.1-0.6, preferably
It is more preferably 0.2-0.4 for 0.15-0.5.
In another preference, the wearability of properties of solid self-lubricant coating shows that wear rate is 1.0 × 10-17To 8.0 ×
10-16m3/ Nm, preferably 2.0 × 10-17To 5.0 × 10-16m3/N·m。
Wherein, the test of the coefficient of friction and wear rate uses (the UMT-3 fretting wears of reciprocating friction wear tester
Machine CETR, the U.S.), measurement parameter is set to：Antithesis ball is diameter 6mm Al2O3Ball, load 2N, abrasion distance are 102m, speed
It is 10200 turns to spend for 50mm/s, oscillation cycle.
In another preference, the wear rate determines under the conditions of being 50% in envionmental humidity.
In another preference, the wear rate is 1.0 × 10-16To 9.0 × 10-15m3/ Nm, preferably 2.0 ×
10-16To 5.0 × 10-15m3/ Nm, and wear rate determines under the conditions of envionmental humidity is 30%.
The second aspect of the present invention provides a kind of properties of solid self-lubricant coating prepared described in the first aspect of the present invention
Method, including step：
(i) base material, TiB are provided2Ceramic target and WS2Target；
(ii) vacuumize process, after reaching required back end vacuum condition, using double target co-sputtering method, TiB will be come from2Target
Ti, B and from WS2W, S cosputtering of target are simultaneously deposited on described base material, form properties of solid self-lubricant coating as mentioned.
In another preference, described properties of solid self-lubricant coating is compounded to form on base material.
In another preference, the base material is workpiece.
In another preference, described base material is selected from the group：Metal, alloy, ceramics and rigid plastics.
In another preference, described base material is cleaned base material.
In another preference, described TiB2Target source is selected from the group：TixB1-x, x=0.2~0.4.
In another preference, described WS2Target source is selected from the group：WyS1-y, y=0.3~0.5.
In another preference, deposition pressure is 0.2Pa~1.2Pa, preferably 0.2Pa~0.6Pa.
In another preference, substrate temperature is 200 DEG C~700 DEG C, preferably 300 DEG C~500 DEG C.
In another preference, substrate negative voltage is -30V~-60V.
In another preference, the method for described matrix cleaning is cleaned for Chemical cleaning and/or plasma glow.
Chemical cleaning：Matrix or workpiece are sequentially placed into concentration as 30%~60% cleanser solution, acetone, anhydrous second
Respectively be cleaned by ultrasonic 10~20min in alcohol, deionized water, then temperature be dried in 80 DEG C~100 DEG C of drying box 1~2h or
Use purity for 99.99% high-purity N2Drying.
Plasma glow cleans：Matrix or workpiece after Chemical cleaning is got well are put into rotatable matrix frame in vacuum chamber
On, when the back end pressure of vacuum chamber is less than or equal to 1 × 10-3After Pa, argon gas is filled with and by pressure control in 1Pa~3Pa or so, so
Radio-frequency power supply (power 100~200W, frequency 40-70MHz) and substrate bias (- 100~-250V) are opened afterwards, are produced using argon gas
Raw plasma etches 10~20min to substrate so that hydrone, gas molecule or the dust particale of substrate surface attachment
It is etched completely away.
In another preference, intermediate layer is deposited first in the substrate surface cleaned, then be total to by above-mentioned double targets
Sputtering method deposits one layer of TiB in described transition layer surface2-WS2Solid lubricant coating, described intermediate layer are selected from following
At least one of component：Ti、Al、Ni.
In another preference, TiB2Target Sputtering power density is：2.5~4.7W/cm2, WS2Target Sputtering power density is：
0.2~2.5W/cm2。
TiB2Ceramic target and WS2The Sputtering power density of target and the TiB2-WS2TiB in solid lubricant coating2Hard phase
And WS2It is relevant to lubricate the two-phase proportion composition of phase, and then the structure of the solid lubricant coating can be influenceed.
The third aspect of the present invention provides a kind of high-abrasive material.Described high-abrasive material contains base material, and positioned at institute
State the properties of solid self-lubricant coating as described in the first aspect of the invention on base material.
The fourth aspect of the present invention provides a kind of product.The product contains solid as described in the first aspect of the invention
Self-lubricating coat in use.
In another preference, described product includes bearing, piston and the product for needing solid lubrication.
It should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the invention and have in below (eg embodiment)
It can be combined with each other between each technical characteristic of body description, so as to form new or preferable technical scheme.As space is limited, exist
This no longer tires out one by one states.
Brief description of the drawings
The equipment that Fig. 1 shows depositing coating.
Fig. 2 shows the TiB that comparative example 1, embodiment 1, embodiment 2 and embodiment 5 are prepared respectively2 -WS2Solid lubrication applies
The scanning electron microscope (SEM) photograph of layer.Wherein (a) is comparative example 1, and (b) is embodiment 1, and (c) is embodiment 2, and (d) is embodiment 5.
Figure (a) is the preparation of comparative example 1 without WS2The solid lubricant coating of incorporation, it can be seen that coating is in the form of a column brilliant knot
Structure, structure is than more loose.With WS2Incorporation, the column structure of coating shown in figure (b) fades away, and works as WS2Mass fraction
For 54.7wt% when, shows fibrous growth structure shown in figure (c), coating structure becomes very fine and close.Work as WS2Quality point
When number is more than 64.9wt%, such as scheme shown in (d), the crystal grain of coating becomes very thin and close.
Fig. 3 shows embodiment 2, the TiB that embodiment 5 is prepared respectively2-WS2Solid lubricant coating atomic force ESEM
Figure.Wherein (a) is embodiment 2, and (b) is embodiment 5.
WS is worked as in figure (a) display2Mass fraction when being 54.7wt%, Coating Surface Roughness Ra=4nm, figure (b) is aobvious
Show WS2When increasing to 70.1wt% of mass fraction, Coating Surface Roughness Ra=3nm.
Fig. 4 shows the TiB that comparative example 1, embodiment 1, embodiment 3 and embodiment 5 are prepared respectively2-WS2Solid lubrication applies
The XRD spectra of layer.Wherein (a) is comparative example 1, and (b) is embodiment 1, and (c) is embodiment 3, and (d) is embodiment 5.
Scheme the TiB that (a) shows pure hard phase2For crystal structure, occurs TiB respectively in 2 θ=27.6 ° and 2 θ=56.9 °2
Typically (0001) and (0002) diffraction maximum.With WS2Incorporation, the weakened of the two diffraction maximums, peak shape broadens, and this says
Understand WS2Incorporation cause coating crystal grains fine；Secondly WS2Incorporation cause TiB2(0001) and (0002) diffraction maximum point
Do not offset, deviation angle is respectively 2.1 ° and 1.5 °.When WS mass fraction is more than 64.9wt%, as schemed (d) institute
Show that coating becomes non crystalline structure.Figure (c) is shown in 2 θ=33.5 ° and 43.9 ° WS occur respectively2(101) and (006) diffraction
Peak, this illustrates WS2Incorporation and hard phase TiB2Form two-phase composite construction, rather than W-S-B-Ti solid solution
Body structure.
Fig. 5 shows the friction for the solid lubricant coating that comparative example 1, comparative example 2, embodiment 1 and embodiment 2 are prepared respectively
Coefficient figure.
Compared to 1 pure TiB of comparative example2The profit prepared with the stainless steel bases of comparative example 2M2, Example 1 and Example 2 of the present invention
Sliding coating coefficient of friction significantly reduces, and is reduced to 0.2.
Fig. 6 shows the frictional wear experiment for the solid lubricant coating that comparative example 1, embodiment 1 and embodiment 5 are prepared respectively
Figure.Wherein (a) is comparative example 1, and (b) is embodiment 1, and (c) is embodiment 5.
Scheme 1 pure TiB of (a) display comparison example2Wear scar width it is wider, abrasive dust is more, there is many gullies, wearability in polishing scratch
Difference.Scheme (b) and show TiB prepared by the embodiment of the present invention 22-WS2Solid lubricant coating, wear scar width is narrower, polishing scratch unusual light,
Abrasive dust is carefully few, and wearability is good.As the WS of incorporation2When mass fraction is more than 64.9wt%, such as scheme shown in (c), although mill now
Trace narrower in width is 54 μm, but occurs ploughing phenomena in polishing scratch, and this is WS2Mix excessive coating hardness it is relatively low caused by,
Coating abrasion performance is poor.
Embodiment
The present inventor, by largely screening and testing, has been made a kind of new first by long-term in-depth study extensively
The properties of solid self-lubricant coating of type.The coating has higher hardness (H >=40GPa), compared with low-friction coefficient (μ≤0.2) and relatively low mill
Loss rate (10-16m3/ Nm the orders of magnitude), in room temperature to there is preferable greasy property in the range of 650 DEG C, can in a variety of matrixes or
Used on workpiece and improve the wearability of object, and be adapted to use under the special operation conditions such as high vacuum.In addition it is provided by the invention
The preparation method processing step of properties of solid self-lubricant coating is simple, workable, controllability is good, is easy to industrialized production.Herein
On the basis of complete the present invention.
Term
As used herein, term " properties of solid self-lubricant coating ", " solid lubricant coating ", " self-lubricating solid painting of the present invention
Layer ", " lubricant coating of the present invention ", " coating of the present invention ", " wear-resistant coating of the present invention " are used interchangeably, and are referred both to hard phase and profit
It is sliding mutually to pass through the nano combined material layer being covered on base material formed.Specifically, refer to described in first aspect present invention " Gu
Body self-lubricating coat in use ".
Properties of solid self-lubricant coating
The properties of solid self-lubricant coating of the present invention is by hard phase TiB2With lubrication phase WS2It is combined through two-phase.WS2Make
To lubricate phase, one side heat endurance is high, and operating temperature can play rubbing under high temperature and vacuum environment from room temperature to 650 DEG C
Lubrication is wiped, and it is little to the sensitiveness of ambient humidity in friction process.Another aspect and TiB2Have etc. most materials
Preferable wellability, it is easily formed nano composite structure, but WS2Its own hardness it is relatively low (<10GPa).TiB2Have as hard phase
Have high rigidity (>44GPa), high thermal stability and excellent anti-wear performance.
The experiment of the present invention unexpectedly shows, when to the TiB of hard phase2Middle addition WS2When lubricating phase, in certain limit with
WS2The increase of content, not only makes TiB2Crystal grain can attenuate and can be with the TiB of hard phase2Stronger gelling is formed to make
With being embodied on coating structure, first, realizing hard phase TiB2With lubricating phase WS2Two-phase composite construction, two are so that
Coating substantially becomes fine and close.The TiB of this soft phase gelling hard phase of the present invention2-WS2Solid lubricant coating hardness is higher, lubrication
Performance is good.
In another preference, described solid lubricant coating is in fibrous growth structure, and coating is fine and close, electrical resistivity range
For the μ Ω .cm of 70 μ Ω .cm~135.
In another preference, the total atom number based on properties of solid self-lubricant coating, described solid lubricant coating each element
Atomic percent be：
16.5at%~24.5at% Ti；
47.1at%~67.7at% B；
5.5at%~14.0at% W；
1.7at%~5.8at% S；
In another preference, other impurities (or impurity element) content is 1.7at%~5.8at%.
In another preference, described impurity element includes O, H, C.
In another preference, described properties of solid self-lubricant coating has following one or more features：
(a) 1.5 μm~4.5 μm of coating layer thickness；
(b) conductivity is in the μ Ω .cm of 70 μ Ω .cm~200, the μ Ω .cm of preferably 70 μ Ω .cm~135；
(c) surface roughness Ra≤10nm of coating, preferably Ra≤5nm；
(d) surface topography of coating is scanned using atomic force ESEM, is presented as shown in Fig. 3 (a) or 3 (b) or basic
Above as shown in Fig. 3 (a) or 3 (b), the pattern preferably shown in Fig. 3 (a).
In another preference, the solid lubricant coating is tested in the range of 2 θ=20 °~70 ° using X-ray diffraction method
There is TiB in 28.5 ° and 58.5 °2Diffraction maximum (0001) and (0002).
In another preference, the X-ray diffractogram of described properties of solid self-lubricant coating is as shown in Figure 4 or basic such as Fig. 4
It is shown, preferably Fig. 4 (b) or the structure shown in 4 (c).
Hard phase
It is not particularly limited suitable for the hard phase of the present invention, can is various hard phases commonly used in the art, it is representative
Example include (but being not limited to)：TiB2, TiN, diamond, TiC, TiCN, TiAlN, AlCrN etc. and combinations thereof it is (or compound
Thing).
A kind of preferable hard phase example is TiB2。
It is highly preferred that hard phase is crystal structure.
Another kind of preferable hard phase TiB2The mass fraction for accounting for whole coating is 30wt%~75wt%, preferably
40wt%~63wt%.
Another kind of preferable hard phase TiB2Particle size range be 50nm~300nm, preferably 100~200nm.
Another kind of preferable hard phase TiB2Particle be made up of multiple crystal grain, wherein the size of crystal grain be 20nm~
100nm, preferably 20nm~40nm.
Lubricate phase
Mutually it is not particularly limited suitable for the lubrication of the present invention, can is various lubrication phases commonly used in the art.It is representative
Example include (but being not limited to)：WS2、MoS2、MoSe2、WSe2, BN, and various softer metal such as Ag, Pb, Sn, In
Deng, or its combination.
A kind of preferable lubrication is mutually WS2。
It is highly preferred that lubrication phase WS2For non crystalline structure.
In another preference, the mass fraction that lubrication mutually accounts for whole coating is 30wt%~50wt%, preferably
36wt%~40wt%.
In another preference, lubrication is mutually two-phase composite construction with hard phase.
In another preference, lubrication mutually wraps up completely and closely hard phase, forms the structure as Behavior of Hardened Cement Paste.
In another preference, the Jacket thickness for lubricating phase is the 5%~10% of hard phase particle diameter.
Properties of solid self-lubricant coating product (product form)
The invention provides it is a kind of with high rigidity, low-friction coefficient, low wear rate properties of solid self-lubricant coating and contain
Have or high-abrasive material and product using the coating.
A kind of preferable high-abrasive material contains base material, and the properties of solid self-lubricant coating of the present invention on the base material.
In another preference, the product containing properties of solid self-lubricant coating of the present invention includes (but being not limited to)：Bearing, piston
And other need the product of solid lubrication.
Equipment
Present invention also offers the equipment for preparing coating of the present invention.
Referring to Fig. 1, a kind of representational depositing coating device include with the sample stage 2 of grid bias power supply 1, intermediate frequency power supply 3,
Intermediate frequency power supply 4 and baffle plate 7.By TiB during use2Ceramic target 5 is connected with intermediate frequency power supply 3, by WS2Target 6 is connected with intermediate frequency power supply 4.
Preparation method
Present invention also offers the preparation method of properties of solid self-lubricant coating as described in the present invention, generally includes following step
Suddenly：
(i) base material, TiB are provided2Ceramic target and WS2Target；
(ii) vacuumize process, after reaching required back end vacuum condition, using double target co-sputtering method, TiB will be come from2Target
Ti, B and from WS2W, S cosputtering of target are simultaneously deposited on described base material, form consolidating as described in the first aspect of the invention
Body self-lubricating coat in use.
In another preference, described properties of solid self-lubricant coating is compounded to form on base material.
In another preference, the base material is workpiece.
In another preference, described base material is selected from the group：Metal, alloy, ceramics and rigid plastics.
In another preference, described base material is cleaned base material.
In another preference, described TiB2Target source is selected from the group：TixB1-x, x=0.2~0.4.
In another preference, described WS2Target source is selected from the group：WyS1-y, y=0.3~0.5.
In another preference, deposition pressure is 0.2Pa~1.2Pa, preferably 0.2Pa~0.6Pa.
In another preference, substrate temperature is 200 DEG C~700 DEG C, preferably 300 DEG C~500 DEG C.
In another preference, substrate negative voltage is -30V~-60V.
In another preference, the method for described matrix cleaning is cleaned for Chemical cleaning and/or plasma glow.
Chemical cleaning：Matrix or workpiece are sequentially placed into concentration as 30%~60% cleanser solution, acetone, anhydrous second
Respectively be cleaned by ultrasonic 10~20min in alcohol, deionized water, then temperature be dried in 80 DEG C~100 DEG C of drying box 1~2h or
Use purity for 99.99% high-purity N2Drying.
Plasma glow cleans：Matrix or workpiece after Chemical cleaning is got well are put into rotatable matrix frame in vacuum chamber
On, when the back end pressure of vacuum chamber is less than or equal to 1 × 10-3After Pa, argon gas is filled with and by pressure control in 1Pa~3Pa or so, so
Radio-frequency power supply (power 100~200W, frequency 40-70MHz) and substrate bias (- 100~-250V) are opened afterwards, are produced using argon gas
Raw plasma etches 10~20min to substrate so that hydrone, gas molecule or the dust particale of substrate surface attachment
It is etched completely away.
In another preference, intermediate layer is deposited first in the substrate surface cleaned, then be total to by above-mentioned double targets
Sputtering method deposits one layer of TiB in described transition layer surface2-WS2Solid lubricant coating, described intermediate layer are selected from following
At least one of component：Ti、Al、Ni.
In another preference, TiB2Target Sputtering power density is：2.5~4.7W/cm2, WS2Target Sputtering power density is：
0.2~2.5W/cm2。
TiB2Ceramic target and WS2The Sputtering power density of target and the TiB2-WS2TiB in solid lubricant coating2Hard phase
And WS2It is relevant to lubricate the two-phase proportion composition of phase, and then the structure of the solid lubricant coating can be influenceed.
Main advantages of the present invention include：
(1) providing one kind has higher hardness (H >=40GPa), compared with low-friction coefficient (μ≤0.2) and compared with low wear rate
(10-16m3/ Nm the orders of magnitude) properties of solid self-lubricant coating, the coating is in room temperature to having preferable lubricity in the range of 650 DEG C
Can, it can be used on a variety of matrixes or workpiece and improve the wearability of object, and be adapted to use under the special operation conditions such as high vacuum.
(2) solid lubricant coating of the invention is prepared using magnetron sputtering method, the method and traditional multilayer or lamination solid
Lubricant coating method is compared, have processing step is simple, workable, controllability is good, is easy to the characteristics of industrialized production, have
Preferable economic benefit and commercial promise.
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.The experimental method of unreceipted actual conditions in the following example, generally according to conventional strip
Part, or according to the condition proposed by manufacturer.Unless otherwise indicated, otherwise percentage and number are percentage by weight and weight
Number.
Embodiment 1-10 and comparative example 1-2
(1) using high-speed steel, alloy, glass, ceramics and Si pieces as TiB2-WS2The matrix of solid lubricant coating.
(2) before the deposition, matrix first passes through Chemical cleaning and plasma glow cleaning in advance.
(3) depositing Ti B2-WS2Solid lubricant coating, by TiB2Ceramic target and WS2Target is connected with intermediate frequency power supply respectively, works as the back of the body
Bottom vacuum is better than 5 × 10-5Pa, Ar gas is passed through, regulation air pressure is 0.5Pa, as the deposition parameter shown in table 1, carries out double targets and splashes altogether
Penetrate to obtain TiB2-WS2Solid lubricant coating.
The magnetron sputtering deposition parameter details of embodiment 1~10 and comparative example 1 and 2 are shown in Table 1.
Table 1
TiB2-WS2Solid lubricant coating structure and performance characterization
The present invention assesses the TiB prepared in embodiment using following experimental method2-WS2The architectural feature of solid lubricant coating
And mechanical performance.
The sign of coating structure：TiB is measured using EDS2-WS2The atom composition of solid lubricant coating, it configures EDAX Si
(Li) pop one's head in, calibrated by ZAF, each sample selectes an area and is not less than 40mm2Region, measure the average value of its composition.
Using Hitachi's-S4800 ESEMs (ejecting gun voltage 4kV) to TiB2-WS2Solid lubricant coating pattern is seen
Examine.
Using AIST-NT SmartSPMTM1000 atomic force ESEMs are to TiB2-WS2The surface of solid lubricant coating
Scanned.
It is incident using Cu K alpha rays using German Bruker D8 Advance diffractometers, X-ray tube control in 40kV and
40mA, measure each TiB2-WS2The crystal structure of solid lubricant coating, K is filtered out using nickel filterβRay.
The hardness measurement of coating is carried out on MTS Nano G200 nano-indenter test instrument.Wherein testing pressure head is using gold
Hard rock Berkovich pressure heads, it is 200nm to eliminate substrate effect maximum compression distance (within the 15% of thickness).Each sample
Product measure 6 points, average.
Frictional wear experiment is carried out on reciprocating friction wear tester (UMT), coefficient of friction and abrasion to coating
Amount is analyzed.Antithesis ball is diameter 6mm Al2O3 balls, and load 2N, abrasion distance is 102m, speed 50mm/s, past
The multiple cycle is 10200 turns.And grinding defect morphology is carried out using FEI Quanta TM 250FEG type scanning electron Electronic Speculum (SEM)
Characterize, accelerating potential 4kV.
The structure composition and performance characteristic of embodiment 1~10 and the coating of comparative example 1 and 2 are as shown in table 2.
Table 2
Note：RH=30% in table, RH=50% are respectively that the relative humidity of environment is 30% and 50%.
From the results shown in Table 2, with lubrication phase WS2Incorporation, hard phase TiB2Mass fraction become in decline
Gesture, the hardness of respective coatings are gradually lowered, and 20GPa is reduced to from 40GPa.Suitable WS2Lubricating phase content can be in coating
Hardness significantly reduces the coefficient of friction of coating in the case of declining less (40GPa or so), 0.2 is reduced to, such as embodiment 1-3 institutes
Show.The solid lubricant coating of preparation is set to have higher hardness H=40GPa and low-friction coefficient μ=0.2 concurrently in itself, so as to reduce
Friction, reduce abrasion (wear rate<2.8×10-16m3/ N.m), play lubrication.
All it is incorporated as referring in this application in all documents that the present invention refers to, it is independent just as each document
It is incorporated as with reference to such.In addition, it is to be understood that after the above-mentioned instruction content of the present invention has been read, those skilled in the art can
To be made various changes or modifications to the present invention, these equivalent form of values equally fall within the model that the application appended claims are limited
Enclose.
Claims (10)
1. a kind of properties of solid self-lubricant coating, it is characterised in that described coating includes following components or consisted of the following composition：
(1) hard phase TiB2；
(2) phase WS is lubricated2；
Wherein, the hard phase TiB2With lubrication phase WS2Two-phase generates the properties of solid self-lubricant coating, and hard by nano combined
Phase TiB2For crystal structure, lubrication phase WS2For non crystalline structure；Described hard phase TiB2Account for the matter of the properties of solid self-lubricant coating
Amount fraction is 40wt%~63wt%；
Described properties of solid self-lubricant coating is in fibrous growth structure；
The lubrication mutually wraps up completely and closely hard phase, forms the structure as Behavior of Hardened Cement Paste；
The Jacket thickness of the lubrication phase is the 5%~10% of hard phase particle diameter.
2. properties of solid self-lubricant coating as claimed in claim 1, it is characterised in that the total atom based on properties of solid self-lubricant coating
Count, the atomic percent of each element is selected from the group in coating：
16.5at%~28.2at% Ti；
36.6at%~67.7at% B；
5.5at%~28.3at% W；
1.7at%~15.2at% S.
3. properties of solid self-lubricant coating as claimed in claim 1, it is characterised in that hard phase TiB2Particle size range be
50nm~300nm.
4. properties of solid self-lubricant coating as claimed in claim 1, it is characterised in that using X-ray diffraction method 2 θ=20 °~
The properties of solid self-lubricant coating is tested in the range of 70 ° has TiB in 28.5 ° and 58.5 °2Diffraction maximum (0001) and (0002).
5. properties of solid self-lubricant coating as claimed in claim 1, it is characterised in that prepared using the method for double target co-sputtering.
6. properties of solid self-lubricant coating as claimed in claim 1, described properties of solid self-lubricant coating has following one or more
Performance：
(a) lubricity：Coefficient of friction is 0.1-0.6；
(b) wearability：Wear rate is 1.0 × 10-17To 8.0 × 10-16m3/N·m。
A kind of 7. method for preparing properties of solid self-lubricant coating as claimed in claim 1, it is characterised in that methods described includes step
Suddenly：
(i) base material, TiB are provided2Ceramic target and WS2Target；
(ii) vacuumize process, after reaching required back end vacuum condition, using double target co-sputtering method, TiB will be come from2The Ti of target,
B and from WS2W, S cosputtering of target are simultaneously deposited on described base material, form described properties of solid self-lubricant coating.
8. preparation method as claimed in claim 7, it is characterised in that in the step (ii), put on described TiB2Pottery
The power density of porcelain target is 2.5W/cm2~4.7W/cm2, put on WS2The power density of target is 0.2W/cm2~
2.5W/cm2。
A kind of 9. high-abrasive material, it is characterised in that described high-abrasive material contains base material, and on the base material such as power
Profit requires the properties of solid self-lubricant coating described in 1.
10. a kind of workpiece, it is characterised in that the workpiece contains any described properties of solid self-lubricant coating in claim 1-6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410407656.5A CN105441870B (en) | 2014-08-18 | 2014-08-18 | A kind of high rigidity, low-friction coefficient, the properties of solid self-lubricant coating of low wear rate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410407656.5A CN105441870B (en) | 2014-08-18 | 2014-08-18 | A kind of high rigidity, low-friction coefficient, the properties of solid self-lubricant coating of low wear rate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105441870A CN105441870A (en) | 2016-03-30 |
| CN105441870B true CN105441870B (en) | 2018-03-30 |
Family
ID=55552493
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410407656.5A Active CN105441870B (en) | 2014-08-18 | 2014-08-18 | A kind of high rigidity, low-friction coefficient, the properties of solid self-lubricant coating of low wear rate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105441870B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110653432A (en) * | 2019-10-09 | 2020-01-07 | 天津大学 | Self-lubricating extrusion screw tap |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105755440B (en) * | 2016-04-19 | 2019-04-02 | 中国科学院宁波材料技术与工程研究所 | A kind of hard coat of seawater corrosion resistance and preparation method thereof |
| CN108251803B (en) * | 2016-12-29 | 2020-06-02 | 深圳先进技术研究院 | TiB2Self-lubricating coating, preparation method thereof and wear-resistant component |
| CN110387527B (en) * | 2019-07-29 | 2021-07-13 | 缙云县先锋工具有限公司 | High-hardness self-lubricating composite coating for circular saw blade and preparation method thereof |
| CN110735110B (en) * | 2019-08-02 | 2021-09-10 | 缙云县先锋工具有限公司 | Soft-hard combined composite coating for circular saw blade and preparation method thereof |
| CN112176297A (en) * | 2020-09-25 | 2021-01-05 | 吉林大学 | Double-phase structure composite film and preparation method and application thereof |
| CN112609156B (en) * | 2020-11-20 | 2023-09-12 | 江苏科技大学 | Wide-temperature-range self-lubricating film material with thermal cycle service capability and preparation method thereof |
| CN114033799B (en) * | 2021-11-29 | 2024-02-27 | 江苏科技大学 | Method for processing composite lubrication structure of sliding bearing based on electron beam curing |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757788A (en) * | 2005-09-30 | 2006-04-12 | 上海交通大学 | Method of preparing antifriction I1F-WS2/IF-MoS2 composite film by magnetic controlled sputtering |
| CN101398123A (en) * | 2007-09-29 | 2009-04-01 | 中国人民解放军装甲兵工程学院 | WS2/MoS2 solid lubrication multilayer film and method for making same |
| CN102094172A (en) * | 2010-12-03 | 2011-06-15 | 无锡润鹏复合新材料有限公司 | Method for preparing TiWN/MoS2 composite film |
| CN102658688A (en) * | 2012-04-27 | 2012-09-12 | 赛屋（天津）涂层技术有限公司 | Molybdenum disulfide/titanium nitride composite film and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4480687B2 (en) * | 2006-03-03 | 2010-06-16 | 和仁 相良 | Method for producing solid lubricating film and method for improving lubricating characteristics |
-
2014
- 2014-08-18 CN CN201410407656.5A patent/CN105441870B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757788A (en) * | 2005-09-30 | 2006-04-12 | 上海交通大学 | Method of preparing antifriction I1F-WS2/IF-MoS2 composite film by magnetic controlled sputtering |
| CN101398123A (en) * | 2007-09-29 | 2009-04-01 | 中国人民解放军装甲兵工程学院 | WS2/MoS2 solid lubrication multilayer film and method for making same |
| CN102094172A (en) * | 2010-12-03 | 2011-06-15 | 无锡润鹏复合新材料有限公司 | Method for preparing TiWN/MoS2 composite film |
| CN102658688A (en) * | 2012-04-27 | 2012-09-12 | 赛屋（天津）涂层技术有限公司 | Molybdenum disulfide/titanium nitride composite film and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| "Preparation and characterization of low-friction TiB2-based coatings by incorporation of C or MoS2";R.Gilmore，et al.;《Surface and Coatings Technology》;19981231;第105卷;第45-48、50页 * |
| "WS2基固体润滑涂层摩擦性能研究";侯锁霞等;《润滑与密封》;20130430;第38卷(第4期);第82、85页 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110653432A (en) * | 2019-10-09 | 2020-01-07 | 天津大学 | Self-lubricating extrusion screw tap |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105441870A (en) | 2016-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105441870B (en) | A kind of high rigidity, low-friction coefficient, the properties of solid self-lubricant coating of low wear rate | |
| Tyagi et al. | A critical review of diamond like carbon coating for wear resistance applications | |
| Renevier et al. | Advantages of using self-lubricating, hard, wear-resistant MoS2-based coatings | |
| Zeng et al. | Study on atmospheric tribology performance of MoS2–W films with self-adaption to temperature | |
| CN107500782B (en) | Preparation method of modified antifriction wear-resistant corrosion-resistant nano ceramic powder material for additive manufacturing | |
| JP4730753B2 (en) | Diamond-like carbon hard multilayer film and members with excellent wear resistance and sliding resistance | |
| Xu et al. | Microstructure and tribological behaviors of MoN-Cu nanocomposite coatings sliding against Si3N4 ball under dry and oil-lubricated conditions | |
| WO2020093784A1 (en) | Multi-component composite sulfide solid lubricating film, preparation method therefor and use thereof | |
| CN104032268B (en) | High-hardness and low-friction coefficient VAlSiN wear-resistant coating layer | |
| Murakami et al. | High-temperature tribological properties of spark-plasma-sintered Al2O3 composites containing barite-type structure sulfates | |
| Bin et al. | Application of ultra-smooth composite diamond film coated WC–Co drawing dies under water-lubricating conditions | |
| Sun et al. | Evaluation of cold sprayed graphene nanoplates–Inconel 718 composite coatings | |
| Guo et al. | Fabrication and tribological properties of textured diamond coatings on WC-Co cemented carbide surfaces | |
| Zhang et al. | Microstructure evolution and wear resistance of nitride/aluminide coatings on the surface of Ti-coated 2024 Al alloy during plasma nitriding | |
| CN101665941A (en) | Method for preparing diamond-like composite coating on surface of magnesium alloy | |
| Guo et al. | Deposition of TiSiN coatings by arc ion plating process | |
| Londoño-Menjura et al. | Influence of deposition temperature on WTiN coatings tribological performance | |
| Zhang et al. | Preparation and characterization of MoS2-TiL/MoS2-TiH nano multilayer coating with excellent wear properties | |
| Guo et al. | Microstructure and properties of the Cp/AlSn coatings deposited by magnetron sputtering/multi-arc ion plating | |
| Kim et al. | Long-term low-friction of Ti-overcoated and-doped DLCs: Robustly developed carbonous transfer layer with titanium | |
| Kong et al. | Effect of MoS2 content on friction and wear properties of Mo and S co-doped CrN coatings at 25–600° C | |
| Zhou et al. | Tribological properties and self-repairing functionality of Ti6Al4V-multilayer graphene-ag composites | |
| CN106756816B (en) | A kind of VC/a-C:H nano-composite coating of matrix surface and preparation method thereof | |
| Guo et al. | Effects of bilayer number and thickness ratio on structure and properties of (Cr, N)-DLC/DLC multilayer films | |
| Ren et al. | Design and tribological performance of CrN/Mo2N/MoSx composite coating in wide temperature range inspired by oxidation kinetics principle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |