CN104928643B - A kind of manufacture method and device of metal surface properties modification layer - Google Patents
A kind of manufacture method and device of metal surface properties modification layer Download PDFInfo
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- CN104928643B CN104928643B CN201510300707.9A CN201510300707A CN104928643B CN 104928643 B CN104928643 B CN 104928643B CN 201510300707 A CN201510300707 A CN 201510300707A CN 104928643 B CN104928643 B CN 104928643B
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Abstract
A kind of manufacture method and device of metal surface properties modification layer, use ion injection method with WS2The surface of metal material is modified for target, which includes the pretreatment of metal material；The metal material is put into vacuum chamber, uses ion injection method with WS2Metal surface properties modification layer is generated for target；Drying after metal material cleaning after Surface Creation surface reforming layer and vacuum sealing are sealed up for safekeeping.The invention also discloses the metal surface properties modification layer manufacture device for above-mentioned manufacture method.The present invention prepares tungsten disulfide solid lubricant functional layer in metal surface using ion implantation technique, workpiece surface friction coefficient can be significantly reduced on the premise of workpiece size is not changed, the lubrication available for part under the harsh conditions such as high temperature, high pressure, high vacuum, high load capacity, high rotating speed, high radiation, deep-etching, ultralow temperature.
Description
Technical field
The present invention relates to a kind of manufacture of metal surface properties modification layer, particularly one kind use ion injection method with
WS2For the manufacture method and device of the metal surface properties modification layer of solid lubricant.
Background technology
Tungsten disulfide (WS2) solid lubricant modified layer preparation method and technical study be at present in the world solid moisten
One of the main direction of studying in sliding field.Tungsten disulfide has very low friction coefficient, and higher anti-extreme pressure energy, its is anti-oxidant
The existing solid lubricant MoS of performance ratio2It is good, thus suitable for high temperature, high pressure, high vacuum, high load capacity, high rotating speed, high radiation,
The lubrication of part under the harsh conditions such as deep-etching, ultralow temperature.The U.S. take the lead in by tungsten disulfide be applied to space shuttle, fighter plane,
The military fields such as military machinery chain drive, while also applied in computer hard drive bearing, ultra-high vacuum system
Rotation, on slide unit.The prior art mainly prepares certain thickness two sulphur using magnetron sputtering technique in material surface
Change tungsten film, research direction is then concentrated mainly on film preparation and reduces in the aerial friction coefficient of film.Due to curing
Tungsten film layer is that lamellar structure, the hardness of similar graphite is low, easily shifts or wear in sliding process, it is impossible to it is special to fully meet some
The use demand of kind precision instrument lubrication, for example pure free of contamination solid lubrication is needed in space precision instrument field, do not permit
Permitted there is film layer to come off；On the bearing that high temperature and pressure vacuum environment uses, film layer peeling, the chip otherwise peeled off are also not allow for
It is attached on high casting die and high voltage arc easily occurs and cause equipment unstable or part injury.Therefore, how to prepare both has well
Greasy property, but the tungsten disulfide modified layer that surface peeling will not occur becomes current urgent problem to be solved.
Ion implantation technique is to develop a kind of Metal material surface modification method of formation in recent years, its principle is using strong
Electric field accelerates the ion for needing to inject, and high-speed ion beam is bombarded the workpiece surface in target chamber, makes ion implanting to workpiece material
In material, a large amount of high density dislocations, room are produced, while can also make surface decrystallized, plays the role of improving material surface performance.
Since traditional plated film is in workpiece material surface depositional coating, and ion implanted layer is ion implanting of originally being experienced by workpiece material changes
Property and formed, therefore between implanted layer and matrix there is no interface debonding and combine power problem.Therefore ion implanting skill is used
Art is prepared on the metal material has the function of that the modified layer of tungsten disulfide solid lubricant becomes solution solid lubrication transfer membrane and comes off
The developing direction of problem.
The content of the invention
The technical problems to be solved by the invention are for the problem of solid lubrication transfer membrane comes off in the prior art, there is provided
One kind uses ion implantation technique, with WS2For the manufacture method and its dress of the metal surface properties modification layer of solid lubricant
Put, which has the function of solid lubrication.
To achieve these goals, the present invention provides a kind of manufacture method of metal surface properties modification layer, wherein, adopt
With ion injection method with WS2Surface modification is carried out to metal material for target, is included the following steps：
The pretreatment of S100, metal material, pre-process metal material to be processed, and removal is attached to the metal
Grease, rust spot and the impurity of material surface；
S200, generation surface reforming layer, use ion injection method with WS2Metal surface properties modification is generated for target
Layer.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, the step S200 includes：By the metal material
Material is put into vacuum chamber, and the vacuum chamber is connected with MEVVA ion guns, by the vacuum chamber to 1.0 × 10-4Pa~
5.0×10-4Pa, the MEVVA ion guns are with WS2Surface modification is carried out to the metal material for target, with the metal
The Surface Creation surface reforming layer of material, wherein, the ion implantation energies of the MEVVA ion guns is 50keV~120keV, institute
The ion implanting accumulated dose for stating MEVVA ion guns is 1.0 × 1017ions/cm2~5 × 1017ions/cm2；
The manufacture method of above-mentioned metal surface properties modification layer, wherein, after step S200, further include：S300, gold
Belong to sealing up for safekeeping for material, the metal material after Surface Creation surface reforming layer is put into acetone soln and is cleaned 5~10 minutes
After dry, and the metal material vacuum sealing after drying is sealed up for safekeeping.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, the ion gun uses 99% WS2Cathode into
Row ion implanting.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, the metal material is by the inside shape successively in surface
Into amorphous, crystallite and phase structure of alloy.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, the step S100 includes：
S101, the surface grease for removing the metal material, the surface oil that fatsolvent removes the metal material is removed with metal
After fat, which is put into free of contamination tetrachloroethylene solvent and is soaked 20~30 minutes, it is residual with rice paper exhaustion after taking-up
The tetrachloroethylene solvent stayed, then the surface of the metal material is wiped with absorbent cotton, finally wiped with clean silk.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, the step S100 is further included：
S102, remove rust spot, with the metal-derusting cleaning agent soaking and washing metal material 10~20 minutes, is wiped after taking-up
Totally, so that its surface is without micro- rust spot.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, the step S100 is further included：
S103, remove impurity, which is put into acetone solvent, and ultrasonic cleaning 20~take out after forty minutes, makes
Dried with clean silk.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, the step S100 is further included：
S104, ultrasonic cleaning, which is put into deionized water, and ultrasonic cleaning 20~take out after forty minutes, makes
Wiped with clean silk, and be positioned in vacuum drying oven drying 2~4 it is small when.
In order to which above-mentioned purpose is better achieved, present invention also offers one kind to be used for above-mentioned metal surface properties modification layer system
Make the metal surface properties modification layer manufacture device of method.
The technical effects of the invention are that：
The method that the present invention prepares tungsten disulfide solid lubricant functional layer in metal surface using ion implantation technique, can be
Workpiece surface friction coefficient is significantly reduced on the premise of not changing workpiece size, available for high temperature, high pressure, high vacuum, high load capacity,
The lubrication of part under the harsh conditions such as high rotating speed, high radiation, deep-etching, ultralow temperature.Compared with prior art, the present invention using from
Sub- injection technique carries out surface modification to metal works, and modified effect is controlled by adjusting parameters such as Implantation Energy, implantation dosages
Fruit, it is final to realize the effect for reducing friction coefficient, improving workpiece lubricant effect.Modified material friction coefficient is low, the wear-resisting longevity
Life length, since modifying element is directly squeezed into inside basal body structure, so that modified layer is formed on top layer, therefore modified layer and metal material
Material is still integral material, there is no combination power problem, and rear workpiece size precision does not change before modified, therefore the technology is applicable in
It is modified for the precision component surface under the limiting conditions such as high pressure high vacuum ultralow temperature.The tungsten disulfide solid lubricant of the prior art
The aerial friction coefficient of film is commonly 0.05-0.25, and the metal material that the present invention is modified, under ambient temperature and moisture with
The loaded load of 50g, the rotating speed of 100r/min carry out sliding frictional wear test, its friction durability is up to 2h, mantle friction system
Number is less than 0.2.
Below in conjunction with the drawings and specific embodiments, the present invention will be described in detail, but not as a limitation of the invention.
Brief description of the drawings
Fig. 1 is the manufacturing method of the present invention flow chart；
Fig. 2 is ion implanted layer schematic diagram of the present invention；
Fig. 3 is the sectional view of metal material of the present invention；
Fig. 4 is the fretting wear curve map after present invention generation surface reforming layer；
Fig. 5 is the fretting wear curve that metal material does not generate surface reforming layer；
Fig. 6 is the manufacture device structure diagram of one embodiment of the invention.
Wherein, reference numeral
1 metal material
2 vacuum chambers
3 ion guns
4 surface reforming layers
5 workbench
Embodiment
The structural principle and operation principle of the present invention are described in detail below in conjunction with the accompanying drawings：
Referring to Fig. 1, Fig. 1 is the manufacturing method of the present invention flow chart.The manufacture of the metal surface properties modification layer of the present invention
Method, uses ion injection method with WS2The surface of metal material 1 is modified for target, is included the following steps：
Step S100, the pretreatment of metal material 1, pre-processes metal material 1 to be processed, and removal is attached to institute
State the grease, rust spot and impurity on 1 surface of metal material；
The step S100 includes：
S101, the surface grease for removing the metal material 1, with metal remove fatsolvent (such as sodium hydroxide, sodium carbonate,
Ten water sodium phosphates, sodium metasilicate, detergent, corrosion inhibiter, aqueous solvent etc.) remove the surface grease of the metal material 1 after, by the metal
Material 1, which is put into free of contamination tetrachloroethylene solvent, to be soaked 20~30 minutes, with the remaining tetrachloro-ethylene of rice paper exhaustion after taking-up
Solvent, then the surface of the metal material 1 is wiped with absorbent cotton, finally wiped with clean silk.
The step S100 is further included：
S102, remove rust spot, with the metal-derusting cleaning agent soaking and washing metal material 110~20 minutes, is wiped after taking-up
Wipe totally, so that its surface is without micro- rust spot.
The step S100 is further included：
S103, remove impurity, which is put into acetone solvent, and ultrasonic cleaning 20~take out after forty minutes, makes
Dried with clean silk.When drying, wiped in the same direction on the smooth surface of the metal material 1, ensure the metal
The surface of material 1 does not have water stain and impurity residual；Privileged sites (working face) emphasis of the metal material 1 wipes, the metal material
Other positions (non-working surface) of material 1 ensure that its surface does not have water stain and impurity residual.Meanwhile without using being contaminated, soaked
Wet silk wipes it.
The step S100 is further included：
S104, ultrasonic cleaning, which is put into deionized water, and ultrasonic cleaning 20~take out after forty minutes, makes
Wiped with clean silk, and be positioned in vacuum drying oven drying 2~4 it is small when.
Step S200, metal surface properties modification layer 4 is generated, uses ion implantation technique with WS2Metal is generated for target
Material surface modifying layer.In the present embodiment, specifically include：The metal material 1 is put into vacuum chamber 2, the vacuum chamber 2 with
MEVVA ion guns 3 connect, and the vacuum chamber 2 is evacuated to 1.0 × 10-4Pa~5.0 × 10-4Pa, the MEVVA ion guns
3 with WS2Surface modification is carried out to the metal material 1 for target, with the Surface Creation surface reforming layer of the metal material 1
4, wherein, the MEVVA ion guns 3 use 99% WS2Cathode carries out ion implanting, the ion note of the MEVVA ion guns 3
It is 50keV~120keV to enter energy, and the ion implanting accumulated dose of the MEVVA ion guns 3 is 1.0 × 1017ions/cm2~5 ×
1017ions/cm2, the metal material 1 inwardly sequentially forms amorphous, crystallite and phase structure of alloy, the metal material by surface
1 skin-friction coefficient is 0.2；
Referring to Fig. 2 and Fig. 3, Fig. 2 is ion implanted layer schematic diagram of the present invention, and Fig. 3 is the sectional view of metal material of the present invention.
Sectional view is that the sectional view of the metal material 1 is it can be found that the metal material 1 after injection using made of ion beam etching
After ion implanting, 4 modified layer of surface reforming layer and the metal material 1 are not in lamination, are well combined, therefore there is no knot
Surface peeling conditions caused by conjunction problem occur, and meet the requirement of precision parts.
It is the fretting wear curve map after present invention generation surface reforming layer referring to Fig. 4 and Fig. 5, Fig. 4, Fig. 5 is metal material
Material does not generate the fretting wear curve of surface reforming layer.Fretting wear curve after contrasting the metal material 1 before ion implantation
It can be found that ion implanted WS2Surface is modified, and the skin-friction coefficient of the metal material 1 is greatly reduced, from 0.7
0.16 is down to, significantly improves the lubricant effect on 1 surface of metal material；Ion implanted WS2The metal material 1 friction mill
Damage before curve ratio ion implanting it is more steady, fluctuation is small, illustrate its lubricity keep preferably, modified layer it is uniform and stable.
In the present embodiment, it may also include：Step S300, metal material 1 is sealed up for safekeeping, after the Surface Creation surface reforming layer 4
The metal material 1 be put into acetone soln cleaning 5~dry after ten minutes, it is and the above-mentioned metal material 1 after drying is true
Sky is sealed up for safekeeping.
In the present embodiment, it may also include：
Step S400, surface examination, Surface testing is carried out to the metal material 1 after surface treatment.
Referring to Fig. 6, Fig. 6 is the manufacture device structure diagram of one embodiment of the invention.The present invention's is used for above-mentioned metal
4 manufacture device of metal surface properties modification layer of the manufacture method of material surface modifying layer 4, including vacuum chamber 2, ion gun 3 are (excellent
Select MEVVA ion guns), be provided with workbench 5 in vacuum chamber 2, wherein ion gun 3 at the roof of vacuum chamber 5 positioned to be processed
The surface of metal material 1.
During work, which is put on the workbench 5 of vacuum chamber 2, opens mechanical pump, the molecular pump of ion gun 3
And circulation, 1.0 × 10 are evacuated to vacuum chamber 2-4Pa~5.0 × 10-4Pa, vacuum chamber 2 workbench 5 along from
While body axis uniform speed slow rotates, surface modification is carried out to the metal material 1 with ion gun 3.Wherein, ion gun 3 from
Sub- Implantation Energy is 50keV~120keV, and the ion implanting accumulated dose of ion gun 3 is 1.0 × 1017ions/cm2~5 ×
1017ions/cm2.The top layer of the metal material 1 after surface treatment forms amorphous, crystallite with the increase of element injection depth
And alloy phase, i.e. amorphous, crystallite and alloy phase are inwardly formed by the top layer of the metal material 1 successively.By being somebody's turn to do after surface treatment
Metal material 1 is put into cleaned 5-10 minutes in acetone after dry again, its vacuum sealing is sealed up for safekeeping.
Afterwards, Surface testing is carried out to the metal material 1 after surface treatment, the results show that in the table of the metal material 1
Face nearby detects higher W, S peak (W- tungsten peak, S peaks-sulphur peak), and as depth increases, W, S content gradually reduce；Noted in ion
Enter and the new alloy phase containing W, S is detected in layer；Compared with before ion implanting, the skin-friction coefficient of the metal material 1 reduces, and reaches
To 0.2 or so.
The WS that the present invention is prepared using ion implantation technique2WS in surface reforming layer2It is injected directly into the metal material
Inside, ion implantation modification layer is by the metal material and the WS being injected into2Composition, with traditional WS2Film is compared, metal of the invention
Material surface modifying layer has the advantage that：
There is no film-substrate cohesion problem, and modified layer peeling phenomenon will not occur；It will not fail in wet environment；Than passing
Unite WS2Coating abrasion performance is more preferable, but is subject to implanted layer depth limit, and modified layer is in terms of friction durability than traditional WS2It is slightly lower.
Wherein, ion implanting parameter influences final modified layer depth, and Implantation Energy is higher, and injection depth is bigger, the modification layer depth of formation
Degree is also deeper；Implantation dosage is bigger, and the ion concentration injected in metal material is higher, to the influence of metal material performance
It is bigger.
Certainly, the present invention can also have other various embodiments, ripe in the case of without departing substantially from spirit of the invention and its essence
Know those skilled in the art and make various corresponding changes and deformation in accordance with the present invention, but these change and become accordingly
Shape should all belong to the protection domain of appended claims of the invention.
Claims (7)
1. a kind of manufacture method of metal surface properties modification layer, it is characterised in that use ion injection method with WS2For target
The surface of metal material is modified, is included the following steps：
The pretreatment of S100, metal material, pre-process metal material to be processed, and removal is attached to the metal material
Grease, rust spot and the impurity on surface；
S200, generation metal surface properties modification layer, use ion injection method with WS2Metal material surface is generated for target to change
Property layer, further comprises：The metal material is put into vacuum chamber, the vacuum chamber is connected with ion gun, by the vacuum
Room is evacuated to 1.0 × 10-4Pa~5.0 × 10-4Pa, the ion gun is with WS2Surface is carried out to the metal material for target
It is modified, with the Surface Creation surface reforming layer of the metal material, wherein, the ion implantation energy of the ion gun is
50keV~120keV, the ion implanting accumulated dose of the ion gun is 1.0 × 1017ions/cm2~5 × 1017ions/cm2；
Wherein, the metal material inwardly sequentially forms amorphous, crystallite and phase structure of alloy from surface.
2. the manufacture method of metal surface properties modification layer as claimed in claim 1, it is characterised in that step S200 it
Afterwards, further include：
S300, metal material are sealed up for safekeeping, and the metal material after Surface Creation surface reforming layer is put into acetone soln clearly
Wash 5~dry after ten minutes, and the above-mentioned metal material vacuum sealing after drying is sealed up for safekeeping.
3. the manufacture method of metal surface properties modification layer as claimed in claim 1, it is characterised in that the ion gun uses
99% WS2Cathode carries out ion implanting.
4. the manufacture method of metal surface properties modification layer as claimed in claim 1, it is characterised in that the step S100 bags
Include：
S101, the surface grease for removing the metal material, after the surface grease that fatsolvent removes the metal material is removed with metal,
The metal material is put into free of contamination tetrachloroethylene solvent and is soaked 20~30 minutes, with rice paper exhaustion remaining four after taking-up
Vinyl chloride solvent, then the surface of the metal material is wiped with absorbent cotton, finally wiped with clean silk.
5. the manufacture method of metal surface properties modification layer as claimed in claim 4, it is characterised in that the step S100 is also
Including：
S102, remove rust spot, with the metal-derusting cleaning agent soaking and washing metal material 10~20 minutes, is wiped after taking-up
Only, so that its surface is without micro- rust spot.
6. the manufacture method of metal surface properties modification layer as claimed in claim 4, it is characterised in that the step S100 is also
Including：
S103, remove impurity, which is put into acetone solvent, ultrasonic cleaning 20~take out after forty minutes, using dry
Net silk is dried.
7. the manufacture method of metal surface properties modification layer as claimed in claim 4, it is characterised in that the step S100 is also
Including：
S104, ultrasonic cleaning, which is put into deionized water, ultrasonic cleaning 20~take out after forty minutes, using dry
Net silk wipes, and when being positioned over that drying 2~4 is small in vacuum drying oven.
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| CN201510300707.9A CN104928643B (en) | 2014-09-05 | 2015-06-03 | A kind of manufacture method and device of metal surface properties modification layer |
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| CN2014104500726 | 2014-09-05 | ||
| CN201410450072 | 2014-09-05 | ||
| CN201510300707.9A CN104928643B (en) | 2014-09-05 | 2015-06-03 | A kind of manufacture method and device of metal surface properties modification layer |
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| CN104928643A CN104928643A (en) | 2015-09-23 |
| CN104928643B true CN104928643B (en) | 2018-04-24 |
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| CN106868467B (en) * | 2017-03-02 | 2019-02-15 | 北京航空航天大学 | A kind of ion implanting or injection and depositing system |
| CN112323035A (en) * | 2020-08-24 | 2021-02-05 | 机械科学研究总院集团有限公司 | Preparation method of self-lubricating wear-resistant film for gear surface |
| CN114457317A (en) * | 2021-12-22 | 2022-05-10 | 北京机械工业自动化研究所有限公司 | Preparation method of ion implantation nano-reinforcing layer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854547A (en) * | 2004-12-22 | 2006-11-01 | 北京师范大学 | Self-lubricating friction-reducing bearing of multiple ionic mixed injection |
| CN102506041A (en) * | 2011-11-09 | 2012-06-20 | 黄锦滨 | Novel oil pumping unit horse head pin and preparation method thereof |
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2015
- 2015-06-03 CN CN201510300707.9A patent/CN104928643B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854547A (en) * | 2004-12-22 | 2006-11-01 | 北京师范大学 | Self-lubricating friction-reducing bearing of multiple ionic mixed injection |
| CN102506041A (en) * | 2011-11-09 | 2012-06-20 | 黄锦滨 | Novel oil pumping unit horse head pin and preparation method thereof |
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