CN106119776B - A kind of nanotexturing CrN/WS2The preparation method of solid lubricating film - Google Patents

A kind of nanotexturing CrN/WS2The preparation method of solid lubricating film Download PDF

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CN106119776B
CN106119776B CN201610815941.XA CN201610815941A CN106119776B CN 106119776 B CN106119776 B CN 106119776B CN 201610815941 A CN201610815941 A CN 201610815941A CN 106119776 B CN106119776 B CN 106119776B
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target
crn
film
preparation
lubricating film
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CN106119776A (en
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王德生
胡明
翁立军
孙嘉奕
高晓明
姜栋
伏彦龙
杨军
王琴琴
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a kind of nanotexturing CrN/WS2The preparation method of solid lubricating film, specific steps are as follows: 1) substrate is cleaned using ultrasonic cleaning；2) substrate is cleaned with argon ion sputtering；3) there is the CrN layer of nanometer cone cell array structure using medium frequency magnetron sputtering technology deposition surface；4) WS is deposited by radiofrequency magnetron sputtering technology2Composite lubricating film layer.Membrane structure of the present invention is fine and close, and with being firmly combined for base material, the CrN of nanometer cone cell array structure provides good support and preservation WS2The effect of lubricating film, monolithic film membrane show the tribological property being obviously improved, have a good application prospect.

Description

A kind of nanotexturing CrN/WS2The preparation method of solid lubricating film
Technical field
The present invention relates to a kind of nanotexturing CrN/WS2The preparation method of solid lubricating film.
Background technique
Two chalcogen compound of magnesium-yttrium-transition metal is because having the anti-cold welding of good vacuum and greasy property, as a kind of good Solid lubricant is widely used to all kinds of moving components in space structure.It is fast with development with space technology, to entire More stringent requirements are proposed for the engineering reliability and working life of space equipment, and also there is an urgent need to have more high wear resistance and longevity The solid lubricant of life.In tungsten disulfide (WS2) greasy property promotion research in terms of, added by mechanical means or laser Work technology has the micro-structures such as periodic micro- hole, groove to the preparation of metal matrix material surface, later filling out by lubricant It fills, realizes storage of the micro-structure to lubricant, can reach the secondary continuous lubrication of friction and the raising in service life.In addition, passing through biology The deposition of texturing film at the nanoscale may be implemented in the technologies such as template, realizes the improvement of thin-film friction performance.It is overall For, in practical application in industry at this stage, there are apparent cost aspects and complex parts to use for laser texturing The nanotexturing film of limitation, the preparation of the technologies such as biological template cannot achieve the application under top load and high speed conditions. In addition, by traditional gas phase deposition technology, realizing nanotexturing WS under micro-/ nano scale2The research of composite lubricating film and That applies is then seldom.
Summary of the invention
The purpose of the present invention is to provide a kind of nanotexturing CrN/WS2The preparation method of solid lubricating film.
The present invention prepares the hard CrN film with textured structure by magnetron sputtering technique first on metallic matrix Layer, deposits WS later2Construct nanotexturing WS2Composite lubricating film layer realizes mentioning for thin-film friction performance and working life It is high.Film prepared by the present invention has CrN layers of the hard of nanometer cone cell array structure as supporting layer using surface, mating surface WS2Lubricant layer, to realize wear-resistant, the long-life the characteristic for improving thin film system.
One of key of the invention is to deposit CrN layers using medium frequency magnetron sputtering technology, by control deposition process Ar gas and reaction N2Flow-rate ratio, preparing, there is good (111) face preferred growth, surface nanometer cone cell array structure is presented CrN film layer, in this, as nanotexturing WS2The bottom of film.On the one hand, this nanostructured surface is conducive to improve film Combination between layer, can promote surface layer WS2The fine and close growth of film layer, on the other hand, this nano array structure is conducive to WS is saved in friction process2Lubricant realizes the raising of thin film system lubricating life.
The present invention relates to surface WS2Layer is prepared using radiofrequency magnetron sputtering technology.Vacuum coating of the present invention Equipment is equipped with medium frequency magnetron sputtering and rf magnetron sputtering target position simultaneously.After bottom CrN is deposited, by vacuum chamber Rotating mechanism, matrix is moved into radio-frequency sputtering WS2Target position carries out WS2The deposition of film layer.
A kind of nanotexturing CrN/WS2The preparation method of solid lubricating film, it is characterised in that the tool of the preparation method Body step are as follows:
1) target is installed
The Cr target of 60~90mm of diameter, 4~6mm of thickness, purity 99.99% is mounted on medium frequency magnetron sputtering target stand；It will be straight 60~90mm of diameter, 4~6mm of thickness, purity 99.99% WS2Target is mounted on rf magnetron sputtering target stand, is separately connected intermediate frequency and splashes Radio source and radio-frequency sputtering power supply；
2) basis material prepares installation
Basis material is successively cleaned by ultrasonic in acetone, dehydrated alcohol, is placed on vacuum chamber work rest after dry, and adjust Matrix is to target spacing to 60~90 mm；
3) Ar ion bombardment is handled
Vacuum chamber base vacuum is evacuated to 5.0 × 10-4~2.0 × 10-3Pa is filled with high-purity Ar gas, maintains air pressure to 1.5 ~5.0 Pa, ion bombardment -500~-1000V of voltage, 15~30 min of bombardment time；
4) CrN layers of deposition
N is filled with to vacuum chamber2, adjust N2With Ar throughput, maintain air pressure to 8.5 × 10-1~1.5Pa, bias add to -50 ~-100V opens mid frequency sputtering power supply, and target current is set as 1.2~1.6A, target voltage 250V~350V, and CrN layers of sputtering sedimentation, 30~60min of sputtering time；
5) WS2Layer deposition
Mid frequency sputtering power supply is closed, N is closed2, Ar throughput is adjusted to 1.0~1.5Pa of air pressure, and matrix is rotated to WS2Target Before, bias adds to -30~-100V, opens radio-frequency power supply, and power is adjusted to 250~400W, sputters 20~60 min, and plated film terminates After be naturally cooling to room temperature.
Described matrix is stainless steel.
Ar described in step 4) and N2Flow-rate ratio be 1.5~2.5.
Film thickness prepared by the present invention is 1.2~3 μm, the combination in film and matrix and film between layers Well, filmlubrication service life and pure WS2Film is compared and is significantly improved.
Detailed description of the invention
Fig. 1 is the Flied emission electromicroscopic photograph of the CrN with nanometer cone cell array structure prepared by embodiment 1.
Fig. 2 is the Flied emission electromicroscopic photograph of film prepared by embodiment 2.
Fig. 3 is the friction test curve of film prepared by embodiment 2.
Specific embodiment
Embodiment 1
It selects 9Cr18 steel as basis material, basis material is sequentially placed into each super in analysis pure acetone and dehydrated alcohol Sound cleans 15 minutes, is put into infrared baking oven and dries, is subsequently placed into vacuum chamber, by basis material coated surface and Cr target and WS2The distance between target is adjusted to 80 mm.
Vacuum chamber is evacuated, when background air pressure reaches 2.0 × 10-3After Pa, it is filled with argon gas to vacuum chamber, air pressure maintains 2.0Pa, ion bombardment 20 minutes；
It is passed through Ar and N2, Ar and N2Flow-rate ratio is 2:1, and air pressure is adjusted to 1.0 Pa, opens mid frequency sputtering power supply, and deposition CrN is thin Film.Holding target current is 1.5A, target voltage 300 V, workpiece bias -50V；Plated film 60 minutes；
About 0.7 μm of sample measurement film thickness is taken out, Fig. 1 is the surface of the rear film of mid frequency sputtering CrN and the field of section Emit surface sweeping electromicroscopic photograph, it can be seen that the surface CrN shows a nanometer cone cell array structure, and the cone structure period is about 150 Nm, about 120 nm of cone height.
Embodiment 2
It selects 9Cr18 steel as basis material, basis material is sequentially placed into each super in analysis pure acetone and dehydrated alcohol Sound cleans 15 minutes, is put into infrared baking oven and dries, is subsequently placed into vacuum chamber, by basis material coated surface and Cr target and WS2The distance between target is adjusted to 80 mm.
Vacuum chamber is evacuated, when background air pressure reaches 2.0 × 10-3After Pa, it is filled with argon gas to vacuum chamber, air pressure maintains 2.0Pa, ion bombardment 20 minutes；
It is passed through Ar and N2, Ar and N2Flow-rate ratio is 2:1, and air pressure is adjusted to 1.0 Pa, opens mid frequency sputtering power supply, and deposition CrN is thin Film.Holding target current is 1.5A, target voltage 300 V, workpiece bias -50V；Plated film 60 minutes；
Close N2, Ar flow is adjusted to air pressure 1.5Pa, is adjusted bias value -100V, is opened radio-frequency power supply, power is set 350W deposits WS2Film, 30 min of sedimentation time.
Taking out sample measurement film thickness is about 1.47 μm, 0.71 μm of CrN layer, WS20.76 μm of layer.Fig. 2 is film Field emission scanning electron microscope photo, Fig. 3 are the ball disk friction test curve of prepared film, wherein upper sample is 8 mm's of Φ 9Cr18 steel ball, lower sample are plated film sample, load 5N, 1000 r/min of revolving speed.By with the pure WS that is sputtered under the same terms2 Comparison, it can be seen that the friction durability of prepared texturing film is significantly larger than pure WS2Film.

Claims (2)

1. a kind of nanotexturing CrN/WS2The preparation method of solid lubricating film, it is characterised in that the specific step of the preparation method Suddenly are as follows:
1) target is installed
The Cr target of 60~90mm of diameter, 4~6mm of thickness, purity 99.99% is mounted on medium frequency magnetron sputtering target stand；By diameter 60 ~90mm, 4~6mm of thickness, purity 99.99% WS2Target is mounted on rf magnetron sputtering target stand, is separately connected mid frequency sputtering electricity Source and radio-frequency sputtering power supply；
2) basis material prepares installation
Basis material is successively cleaned by ultrasonic in acetone, dehydrated alcohol, is placed on vacuum chamber work rest after dry, and adjust matrix To target spacing to 60~90 mm；
3) Ar ion bombardment is handled
Vacuum chamber base vacuum is evacuated to 5.0 × 10-4~2.0 × 10-3Pa is filled with high-purity Ar gas, maintains air pressure to 1.5~5.0 Pa, ion bombardment -500~-1000V of voltage, 15~30 min of bombardment time；
4) CrN layers of deposition
N is filled with to vacuum chamber2, adjust N2With Ar throughput, maintain air pressure to 8.5 × 10-1~1.5Pa, bias adds to -50~- 100V, opens mid frequency sputtering power supply, and target current is set as 1.2~1.6A, target voltage 250V~350V, CrN layers of sputtering sedimentation, sputters 30~60min of time；The Ar and N2Flow-rate ratio be 1.5~2.5；
5) WS2Layer deposition
Mid frequency sputtering power supply is closed, N is closed2, Ar throughput is adjusted to 1.0~1.5Pa of air pressure, and matrix is rotated to WS2Before target, Bias adds to -30~-100V, opens radio-frequency power supply, and power is adjusted to 250~400W, sputters 20~60 min, after plated film from So it is cooled to room temperature.
2. preparation method as described in claim 1, it is characterised in that described matrix is stainless steel.
CN201610815941.XA 2016-09-12 2016-09-12 A kind of nanotexturing CrN/WS2The preparation method of solid lubricating film Active CN106119776B (en)

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CN107058948B (en) * 2017-02-14 2019-03-01 厦门大学 A kind of soft and rigid composite coating layer and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
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
CN101270700A (en) * 2007-03-21 2008-09-24 江苏省仪征活塞环厂 High abrasion-proof steel piston ring and its production technique
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Patent Citations (3)

* Cited by examiner, † Cited by third party
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
CN101270700A (en) * 2007-03-21 2008-09-24 江苏省仪征活塞环厂 High abrasion-proof steel piston ring and its production technique
CN101315100A (en) * 2007-05-30 2008-12-03 襄阳鹰牌荣华轴承有限公司 Plated film bearing

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Effect of N2 flow rate on microstructure and mechanical properties of PVD CrNx coatings for tribological application in seawater;Lei Shan等;《Surface & Coatings Technology》;20141231;第242卷;全文 *
Multilayered nanocrystalline CrN/TiAlN/MoS2 tribological thin film coatings: preparation and characterization;S Papp等;《IOP Conf.Series:MaterialsScienceandEngineering》;20131231;全文 *
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