CN104928643A - Method and device for manufacturing surface modification layer of metal material - Google Patents
Method and device for manufacturing surface modification layer of metal material Download PDFInfo
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- CN104928643A CN104928643A CN201510300707.9A CN201510300707A CN104928643A CN 104928643 A CN104928643 A CN 104928643A CN 201510300707 A CN201510300707 A CN 201510300707A CN 104928643 A CN104928643 A CN 104928643A
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Abstract
The invention provides a method and device for manufacturing a surface modification layer of a metal material. An ion implantation method is used for conducting surface modification on the metal material by using WS2 as a target material. The manufacturing method comprises the steps that the metal material is preprocessed; the metal material is put into a vacuum chamber, the surface modification layer of the metal material is generated by the ion implantation method with the WS2 being as the target material; and the metal material with the surface modification layer generated on the surface is dried and subjected to vacuum sealing for storage after being washed. The invention further discloses the device for manufacturing the surface modification layer of the metal material by the manufacturing method. According to the method and device, an ion implantation technology is used for preparing a tungsten disulfide solid lubrication function layer on the metal surface, so that the surface friction coefficient of a workpiece is obviously lowered under the premise that the dimension of the workpiece is not changed, and the tungsten disulfide solid lubrication function layer is applicable to lubrication of parts under the harsh conditions of high temperatures, high pressure, high vacuum, high loads, high rotating speeds, high radiation, strong corrosion, ultralow temperatures and the like.
Description
Technical field
The present invention relates to a kind of manufacture of metal surface properties modification layer, particularly a kind of ion injection method that adopts is with WS
2for manufacture method and the device of the metal surface properties modification layer of solid lubricant.
Background technology
Tungsten disulfide (WS
2) the modified layer preparation method of solid lubricant and technical study be one of the main direction of studying in solid lubrication field in the world at present.Tungsten disulfide has very low frictional coefficient, higher anti-extreme pressure energy, and its antioxidant property is than existing solid lubricant MoS
2good, be therefore applicable to the lubrication of part under the severe condition such as high temperature, high pressure, high vacuum, high loading, high rotating speed, high radiation, deep-etching, very low temperature.The U.S. takes the lead in tungsten disulfide to be applied to the military fields such as space shuttle, air fighter, military mechanical chain gear, is also applied in computer hard drive bearing, in the rotation in ultra-high vacuum system, slide unit simultaneously.Prior art mainly utilizes magnetron sputtering technique to prepare certain thickness curing tungsten film at material surface, and research direction then mainly concentrates on film preparation and reduces on the aerial frictional coefficient of film.Due to tungsten disulfide rete be that the lamellar structure of similar graphite, hardness are low, easily transfer or wearing and tearing in sliding process, the user demand of some special precision instruments lubrication can not be met completely, such as need pure free of contamination solid lubrication in space precision instrument field, do not allow rete to come off; On the bearing that High Temperature High Pressure vacuum environment uses, also do not allowed rete to peel off, otherwise the chip peeled off is attached to and high casting die easily occur high voltage arc causes the unstable or part injury of equipment.Therefore, how to prepare and both had favorable lubricating property, the tungsten disulfide modified layer that surfacial spalling can not occur again becomes current problem demanding prompt solution.
Ion implantation technique is a kind of Metal material surface modification method that development in recent years is formed, its principle is utilize highfield to need the acceleration of ions injected, by the workpiece surface in high speed ion bundle bombardment target chamber, make ion implantation in workpiece material, produce a large amount of high density dislocation, room, surface also can be made simultaneously decrystallized, play the effect improving material surface performance.Because traditional plated film is at workpiece material surface depositional coating, and ion implanted layer originally to be experienced ion implantation modification and being formed by workpiece material, therefore not Presence of an interface layering and bonding force problem between input horizon and matrix.Therefore adopt ion implantation technique to prepare the modified layer with tungsten disulfide solid lubricant function on the metal material to become and solve solid lubrication transfer film and to come off the developing direction of problem.
Summary of the invention
Technical problem to be solved by this invention is the problem come off for solid lubrication transfer film in prior art, provides a kind of and adopts ion implantation technique, with WS
2for manufacture method and the device thereof of the metal surface properties modification layer of solid lubricant, this metal surface properties modification layer has solid lubrication function.
To achieve these goals, the invention provides a kind of manufacture method of metal surface properties modification layer, wherein, adopt ion injection method with WS
2for target carries out surface modification to metallic substance, comprise the steps:
The pre-treatment of S100, metallic substance, carries out pre-treatment to metallic substance to be processed, removes the grease, rust spot and the impurity that are attached to described metal material surface;
S200, generation surface reforming layer, adopt ion injection method with WS
2for target generates metal surface properties modification layer.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, described step S200 comprises: described metallic substance is put into vacuum chamber, and described vacuum chamber is connected with MEVVA ion source, by described vacuum chamber to 1.0 × 10
-4pa ~ 5.0 × 10
-4pa, described MEVVA ion source is with WS
2for target carries out surface modification to described metallic substance, with the Surface Creation surface reforming layer at described metallic substance, wherein, the ionogenic ion implantation energy of described MEVVA is 50keV ~ 120keV, and the ionogenic ion implantation total dose of described MEVVA is 1.0 × 10
17ions/cm
2~ 5 × 10
17ions/cm
2;
The manufacture method of above-mentioned metal surface properties modification layer, wherein, after step S200, also comprise: sealing up for safekeeping of S300, metallic substance, described metallic substance after Surface Creation surface reforming layer is put into acetone soln cleaning 5 ~ 10 minutes post-dryings, and the described metallic substance vacuum-sealing after drying is sealed up for safekeeping.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, described ion source adopts the WS of 99%
2negative electrode carries out ion implantation.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, described metallic substance inwardly forms amorphous, crystallite and phase structure of alloy successively by surface.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, described step S100 comprises:
S101, remove the surperficial grease of described metallic substance, after surperficial grease with this metallic substance of metal grease removal removal of solvents, this metallic substance is put into free of contamination tetrachloroethylene solvent to soak 20 ~ 30 minutes, with the tetrachloroethylene solvent that rice paper exhaustion is residual after taking-up, use the surface of this metallic substance of absorbent cotton wiping again, finally use clean silk wiping.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, described step S100 also comprises:
S102, remove rust spot, with this metallic substance of metal-derusting clean-out system soaking and washing 10 ~ 20 minutes, wiped clean after taking out, to make its surface without micro-rust spot.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, described step S100 also comprises:
S103, removal impurity, this metallic substance is put into acetone solvent, and ultrasonic cleaning was taken out after 20 ~ 40 minutes, used clean silk to dry.
The manufacture method of above-mentioned metal surface properties modification layer, wherein, described step S100 also comprises:
S104, ultrasonic cleaning, put into deionized water by this metallic substance, and ultrasonic cleaning was taken out after 20 ~ 40 minutes, uses clean silk wiping, and be positioned in vacuum drying oven dry 2 ~ 4 hours.
In order to realize above-mentioned purpose better, present invention also offers a kind of metal surface properties modification layer manufacturing installation for above-mentioned metal surface properties modification layer manufacturing method.
Technique effect of the present invention is:
The present invention utilizes ion implantation technique to prepare the method for tungsten disulfide solid lubricant functional layer in metallic surface, under the prerequisite not changing workpiece size, significantly can reduce workpiece surface frictional coefficient, can be used for the lubrication of part under the severe condition such as high temperature, high pressure, high vacuum, high loading, high rotating speed, high radiation, deep-etching, very low temperature.Compared with prior art, the present invention adopts ion implantation technique to carry out surface modification to metal works, controls modified effect, the final effect realizing reducing frictional coefficient, improve workpiece lubricant effect by parameter such as adjustment Implantation Energy, implantation dosage etc.Modified material friction coefficient is low, friction durability is long, because modifying element directly squeezes into basal body structure inside, thus form modified layer on top layer, therefore modified layer and metallic substance are still integral material, there is not bonding force problem, and rear workpiece size precision does not change before modified, therefore this technology is suitable for for the precision component surface modification under the limiting conditions such as high pressure high vacuum very low temperature.The aerial frictional coefficient of tungsten disulfide solid lubricant film of prior art is commonly 0.05-0.25, and the metallic substance of modification of the present invention, with the loaded load of 50g under ambient temperature and moisture, the rotating speed of 100r/min carries out sliding frictional wear test, its friction durability can reach 2h, and skin friction coefficient is less than 0.2.
Describe the present invention below in conjunction with the drawings and specific embodiments, but not as a limitation of the invention.
Accompanying drawing explanation
Fig. 1 is manufacture method schema of the present invention;
Fig. 2 is ion implanted layer schematic diagram of the present invention;
Fig. 3 is the sectional view of metallic substance of the present invention;
Fig. 4 is the frictional wear graphic representation after the present invention generates surface reforming layer;
Fig. 5 is the frictional wear curve that metallic substance does not generate surface reforming layer;
Fig. 6 is the manufacturing installation structural representation of one embodiment of the invention.
Wherein, Reference numeral
1 metallic substance
2 vacuum chambers
3 ion sources
4 surface reforming layers
5 worktable
Embodiment
Below in conjunction with accompanying drawing, structural principle of the present invention and principle of work are described in detail:
Be manufacture method schema of the present invention see Fig. 1, Fig. 1.The manufacture method of metal surface properties modification layer of the present invention, adopts ion injection method with WS
2for target is to the surface modification of metallic substance 1, comprise the steps:
The pre-treatment of step S100, metallic substance 1, carries out pre-treatment to metallic substance 1 to be processed, removes the grease, rust spot and the impurity that are attached to described metallic substance 1 surface;
Described step S100 comprises:
S101, remove the surperficial grease of described metallic substance 1, with metal except after fatsolvent (such as sodium hydroxide, sodium carbonate, ten water sodium phosphates, water glass, washing composition, inhibiter, aqueous solvent etc.) removes the surperficial grease of this metallic substance 1, this metallic substance 1 is put into free of contamination tetrachloroethylene solvent to soak 20 ~ 30 minutes, with the tetrachloroethylene solvent that rice paper exhaustion is residual after taking-up, use the surface of this metallic substance 1 of absorbent cotton wiping again, finally use clean silk wiping.
Described step S100 also comprises:
S102, remove rust spot, with this metallic substance of metal-derusting clean-out system soaking and washing 110 ~ 20 minutes, wiped clean after taking out, to make its surface without micro-rust spot.
Described step S100 also comprises:
S103, removal impurity, this metallic substance 1 is put into acetone solvent, and ultrasonic cleaning was taken out after 20 ~ 40 minutes, used clean silk to dry.When drying, the smooth surface of this metallic substance 1 carries out wiping in the same direction, ensure that the surface of this metallic substance 1 does not have water stain and impurities left; Privileged sites (working face) the emphasis wiping of this metallic substance 1, other positions (non-working surface) of this metallic substance 1 ensure that its surface does not have water stain and impurities left.Meanwhile, silk that is contaminated, that soak is not used to carry out wiping to it.
Described step S100 also comprises:
S104, ultrasonic cleaning, put into deionized water by this metallic substance 1, and ultrasonic cleaning was taken out after 20 ~ 40 minutes, uses clean silk wiping, and be positioned in vacuum drying oven dry 2 ~ 4 hours.
Step S200, generation metal surface properties modification layer 4, adopt ion implantation technique with WS
2for target generates metal surface properties modification layer.In the present embodiment, specifically comprise: described metallic substance 1 is put into vacuum chamber 2, described vacuum chamber 2 is connected with MEVVA ion source 3, and described vacuum chamber 2 is evacuated to 1.0 × 10
-4pa ~ 5.0 × 10
-4pa, described MEVVA ion source 3 is with WS
2for target carries out surface modification to described metallic substance 1, with the Surface Creation surface reforming layer 4 at described metallic substance 1, wherein, described MEVVA ion source 3 adopts the WS of 99%
2negative electrode carries out ion implantation, and the ion implantation energy of described MEVVA ion source 3 is 50keV ~ 120keV, and the ion implantation total dose of described MEVVA ion source 3 is 1.0 × 10
17ions/cm
2~ 5 × 10
17ions/cm
2, described metallic substance 1 inwardly forms amorphous, crystallite and phase structure of alloy successively by surface, and the skin friction coefficient of described metallic substance 1 is 0.2;
Be ion implanted layer schematic diagram of the present invention see Fig. 2 and Fig. 3, Fig. 2, Fig. 3 is the sectional view of metallic substance of the present invention.Sectional view utilizes ion beam etching to make, after injection, the sectional view of this metallic substance 1 can find, after this metallic substance 1 is ion implantation, surface reforming layer 4 modified layer and this metallic substance 1 there will not be demixing phenomenon, in conjunction with good, therefore there is not the surfacial spalling situation appearance caused in conjunction with problem, meet the service requirements of precision parts.
Be that the present invention generates the frictional wear graphic representation after surface reforming layer see Fig. 4 and Fig. 5, Fig. 4, Fig. 5 is the frictional wear curve that metallic substance does not generate surface reforming layer.Contrast this metallic substance 1 before ion implantation after frictional wear curve can find, through ion implantation WS
2after surface modification, the skin friction coefficient of this metallic substance 1 is significantly reduced, and is down to 0.16 from 0.7, significantly improves the lubricant effect on this metallic substance 1 surface; Through ion implantation WS
2this metallic substance 1 frictional wear curve than before ion implantation more steadily, fluctuate little, illustrate that its oilness keeps better, modified layer is uniform and stable.
In the present embodiment, also can comprise: sealing up for safekeeping of step S300, metallic substance 1, the described metallic substance 1 after Surface Creation surface reforming layer 4 be put into acetone soln cleaning 5 ~ 10 minutes post-dryings, and above-mentioned metallic substance 1 vacuum-sealing after drying is sealed up for safekeeping.
In the present embodiment, also can comprise:
Step S400, surface examination, this metallic substance 1 after effects on surface process carries out Surface testing.
See the manufacturing installation structural representation that Fig. 6, Fig. 6 are one embodiment of the invention.Metal surface properties modification layer 4 manufacturing installation of the manufacture method for above-mentioned metal surface properties modification layer 4 of the present invention, comprise vacuum chamber 2, ion source 3 (preferred MEVVA ion source), be provided with worktable 5 in vacuum chamber 2, wherein ion source 3 is positioned at directly over metallic substance 1 to be processed at the roof place of vacuum chamber 5.
During work, this metallic substance 1 is put on the worktable 5 of vacuum chamber 2, opens the mechanical pump of ion source 3, molecular pump and circulating water system, 1.0 × 10 are evacuated to vacuum chamber 2
-4pa ~ 5.0 × 10
-4pa, while the worktable 5 of vacuum chamber 2 rotates along own axes uniform speed slow, carries out surface modification with ion source 3 to this metallic substance 1.Wherein, the ion implantation energy of ion source 3 is 50keV ~ 120keV, and the ion implantation total dose of ion source 3 is 1.0 × 10
17ions/cm
2~ 5 × 10
17ions/cm
2.The increase that the degree of depth is injected along with element in the top layer of this metallic substance 1 after surface treatment forms amorphous, crystallite and alloy phase, that is, inwardly form amorphous, crystallite and alloy phase successively by the top layer of this metallic substance 1.This metallic substance 1 after surface treatment is put into after acetone cleans 5-10 minute and dries again, its vacuum-sealing is sealed up for safekeeping.
Afterwards, this metallic substance 1 after effects on surface process carries out Surface testing, and result shows, and higher W, S peak (W-tungsten peak, S peak-sulphur peak) detected at the near surface of this metallic substance 1, and along with the degree of depth increases, W, S content reduces gradually; The new alloy phase containing W, S is detected in ion implanted layer; Compared with before ion implantation, the skin friction coefficient of this metallic substance 1 reduces, and reaches about 0.2.
The WS that the present invention utilizes ion implantation technique to prepare
2wS in surface reforming layer
2be injected directly into this metallic substance inner, ion implantation modification layer is by this metallic substance and the WS be injected into
2composition, with traditional WS
2film is compared, and metal surface properties modification layer of the present invention has following advantage:
There is not film-substrate cohesion problem, modified layer peeling phenomenon can not occur; Can not lose efficacy in wet environment; Than traditional WS
2coating abrasion performance is better, but is subject to the restriction of the input horizon degree of depth, modified layer in friction durability than traditional WS
2slightly low.Wherein, the final modified layer degree of depth of ion implantation parameter influence, Implantation Energy is higher, and inject the degree of depth larger, the modified layer degree of depth of formation is also darker; Implantation dosage is larger, and the ion content injecting metallic substance is higher, larger to the influence of metallic substance performance.
Certainly; the present invention also can have other various embodiments; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art are when making various corresponding change and distortion according to the present invention, but these change accordingly and are out of shape the protection domain that all should belong to the claim appended by the present invention.
Claims (10)
1. a manufacture method for metal surface properties modification layer, is characterized in that, adopts ion injection method with WS
2for target is to the surface modification of metallic substance, comprise the steps:
The pre-treatment of S100, metallic substance, carries out pre-treatment to metallic substance to be processed, removes the grease, rust spot and the impurity that are attached to described metal material surface;
S200, generation metal surface properties modification layer, adopt ion injection method with WS
2for target generates metal surface properties modification layer.
2. the manufacture method of metal surface properties modification layer as claimed in claim 1, it is characterized in that, described step S200 comprises: described metallic substance is put into vacuum chamber, and described vacuum chamber is connected with ion source, by described vacuum chamber to 1.0 × 10
-4pa ~ 5.0 × 10
-4pa, described ion source is with WS
2for target carries out surface modification to described metallic substance, with the Surface Creation surface reforming layer at described metallic substance, wherein, described ionogenic ion implantation energy is 50keV ~ 120keV, and described ionogenic ion implantation total dose is 1.0 × 10
17ions/cm
2~ 5 × 10
17ions/cm
2.
3. the manufacture method of metal surface properties modification layer as claimed in claim 1 or 2, is characterized in that, after step S200, also comprise:
Sealing up for safekeeping of S300, metallic substance, puts into acetone soln cleaning 5 ~ 10 minutes post-dryings, and the above-mentioned metallic substance vacuum-sealing after drying is sealed up for safekeeping by the described metallic substance after Surface Creation surface reforming layer.
4. the manufacture method of metal surface properties modification layer as claimed in claim 1 or 2, is characterized in that, described ion source adopts the WS of 99%
2negative electrode carries out ion implantation.
5. the manufacture method of metal surface properties modification layer as claimed in claim 1 or 2, it is characterized in that, described metallic substance inwardly forms amorphous, crystallite and phase structure of alloy successively from surface.
6. the manufacture method of metal surface properties modification layer as claimed in claim 1 or 2, it is characterized in that, described step S100 comprises:
S101, remove the surperficial grease of described metallic substance, after surperficial grease with this metallic substance of metal grease removal removal of solvents, this metallic substance is put into free of contamination tetrachloroethylene solvent to soak 20 ~ 30 minutes, with the tetrachloroethylene solvent that rice paper exhaustion is residual after taking-up, use the surface of this metallic substance of absorbent cotton wiping again, finally use clean silk wiping.
7. the manufacture method of metal surface properties modification layer as claimed in claim 6, it is characterized in that, described step S100 also comprises:
S102, remove rust spot, with this metallic substance of metal-derusting clean-out system soaking and washing 10 ~ 20 minutes, wiped clean after taking out, to make its surface without micro-rust spot.
8. the manufacture method of metal surface properties modification layer as claimed in claim 6, it is characterized in that, described step S100 also comprises:
S103, removal impurity, this metallic substance is put into acetone solvent, and ultrasonic cleaning was taken out after 20 ~ 40 minutes, used clean silk to dry.
9. the manufacture method of metal surface properties modification layer as claimed in claim 6, it is characterized in that, described step S100 also comprises:
S104, ultrasonic cleaning, put into deionized water by this metallic substance, and ultrasonic cleaning was taken out after 20 ~ 40 minutes, uses clean silk wiping, and be positioned in vacuum drying oven dry 2 ~ 4 hours.
10. the metal surface properties modification layer manufacturing installation for the manufacture method of any one metal surface properties modification layer in the claims 1-9.
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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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|---|---|---|---|
| CN201410450072 | 2014-09-05 | ||
| CN2014104500726 | 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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| CN104928643B CN104928643B (en) | 2018-04-24 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106868467A (en) * | 2017-03-02 | 2017-06-20 | 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 |
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|---|---|---|---|---|
| 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
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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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106868467A (en) * | 2017-03-02 | 2017-06-20 | 北京航空航天大学 | A kind of ion implanting or injection and depositing system |
| 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 |
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