CN107761063B - A kind of high-temperature oxidation resistant self-lubricating laminated coating and preparation method thereof - Google Patents
A kind of high-temperature oxidation resistant self-lubricating laminated coating and preparation method thereof Download PDFInfo
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- CN107761063B CN107761063B CN201710776116.8A CN201710776116A CN107761063B CN 107761063 B CN107761063 B CN 107761063B CN 201710776116 A CN201710776116 A CN 201710776116A CN 107761063 B CN107761063 B CN 107761063B
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3464—Sputtering using more than one target
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
-
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
- C23C28/42—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by the composition of the alternating layers
Abstract
The present invention discloses a kind of high-temperature oxidation resistant self-lubricating laminated coating and preparation method thereof.The coating successively by matrix (1) prime coat (2) and alternate multiple (3) form, the alternate multiple (3) is sequentially overlapped and is constituted by AlCrSiN layers (4) and MoAlSiN layers (5).Preparation method is cleaned by matrix, and ion sputtering cleaning is formed using electric arc ion-plating deposition prime coat and alternate multiple step.Coating prepared by the present invention has the characteristics that hardness is high, high-temperature oxidation resistance is good, coefficient of friction is low, can increase substantially the service performance and service life at high temperature such as cutter, mold.Preparation method of the present invention is simple, technology controlling and process is good, environmentally protective, at low cost, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to field of surface engineering technique, it is specifically designed a kind of high-temperature oxidation resistant self-lubricating laminated coating and its system
Preparation Method, present invention can apply to the anti-oxidant self-lubricating abrasion-resistant damage processing of various metals workpiece surface.
Background technique
AlCrSiN(or CrAlSiN) the features such as coating has hardness high, and wear-resisting property is good, and high-temperature oxidation resistance is good, mesh
It is preceding to have widely applied in workpiece surfaces such as cutter, molds.Cutter, which can generate a large amount of frictional heat, during the cutting process makes part
Temperature increases rapidly, although AlCrSiN coating has good antioxygenic property, AlCrSiN coating coefficient of friction is high, rubs
Wiping coefficient can reach 1.0 or more, on the one hand high coefficient of friction increases wear rate；On the other hand can aggravate to cut frictional heat
Generation, these factors will accelerate coating failure.The coefficient of friction of coating is reduced, coefficient of friction especially at high temperature can
To reduce the generation of frictional heat, the service performance and service life of cutter are improved.MoO3With good greasy property, in coating
When middle addition Mo, aoxidize Mo to form MoO due to generating frictional heat in use process3Self-lubricating phase, to reduce interface mill
Damage improves coating service life.S.A. [S.A. Glatz, C.M. Koller, the H. Bolvardi, S. such as Glatz
Kolozsvári, H. Riedl, P.H. Mayrhofer. Influence of Mo on the structure and
the tribomechanical properties ofarc evaporated Ti-Al-N. Surface and Coatings
Technology, 2017,311:330-336.] it reports and adds Mo in TiAlN coating, research finds that addition Mo can be with
The coefficient of friction of coating is reduced, wear rate is reduced, improves wear-resisting property, but coating high temperature resistance is insufficient.It studies at present
Although MoAlSiN coating can obtain preferable self-lubricating property, coating high temperature resistant is insufficient, generally used below at 650 DEG C.
Summary of the invention
The purpose of the present invention is in view of the above problems and insufficient, a kind of high-temperature oxidation resistant self-lubricating laminated coating material is provided
Material, which can provide 900 DEG C of even higher temperature stabilities and high-temperature oxidation resistance, while have low coefficient of friction
With good wear-resisting property.
It is a further object to provide a kind of preparation methods of high-temperature oxidation resistant self-lubricating laminated coating, should
It is preparation method simple process and low cost, environmentally protective, it is easy to accomplish industrialized production.
High-temperature oxidation resistant self-lubricating laminated coating of the present invention by matrix 1 prime coat 2 and 3 groups of alternate multiple
At the alternate multiple is sequentially overlapped and is constituted by AlCrSiN layer 4 and MoAlSiN layer 5, wherein 4 single monolayer thick of AlCrSiN layer
Degree is 50 ~ 300nm, and 5 thickness in monolayer of MoAlSiN layer is 30 ~ 200nm, and laminated coating overall thickness is 1 ~ 10 μm.
Matrix of the present invention is hard alloy, high-speed steel, mould steel or bearing steel.
Prime coat of the present invention is layers of chrome, titanium layer, zirconium layer or tungsten layer.
The preparation method of high-temperature oxidation resistant self-lubricating laminated coating of the present invention, successively comprises the steps of:
(1) matrix is subjected to degreasing and rust removal cleaning, is put into vacuum chamber after drying；
(2) vacuum chamber is evacuated to lower than 5 × 10-3Pa is passed through argon gas into vacuum chamber, and air pressure is 0.1 ~ 0.8Pa, and bias is
200 ~ 800V carries out sputter clean to matrix using ion source；
(3) it deposits prime coat: opening cathode arc chromium target, titanium target, zirconium target or tungsten target, 0.3 ~ 0.8Pa of ar pressure, bias
50 ~ 200 V, 50 ~ 300nm of thickness；
(4) deposit alternate multiple: be passed through nitrogen, matrix rotates in vacuum chamber, 1 ~ 8rmp of revolving speed, air pressure be 0.5 ~
6Pa, temperature are 200 ~ 500 DEG C, under conditions of bias is 20 ~ 300V, are closed by alternately opening AlCrSi alloys target and MoAlSi
Gold target forms multilayered structure.
Al content is 40 ~ 70 at.% in the AlCrSi alloys target, and Si content is 5 ~ 15 at.%, surplus Cr.
Al content is 13 ~ 50 at.% in the MoAlSi alloys target, and Si content is 5 ~ 20 at.%, surplus Mo.
The present invention uses AlCrSiN and MoAlSiN alternating multilayered structure, and high Al content can provide in AlCrSiN layers
Good high-temperature oxidation resistance, and Mo aoxidizes the MoO of formation at high temperature in MoAlSiN layers3It can be improved good from profit
Slip energy, therefore, this alternating multilayered structure have good high-temperature oxidation resistance, low coefficient of friction, high wearability
Energy.In addition, coating hardness can be improved due to the presence at a large amount of interfaces in alternate multiple；Alternating multilayered structure can also alleviate coating
Internal stress improves coating and basal body binding force；Moreover, multilayer interface can prevent oxidized diffusion process, coating is further increased
Antioxygenic property.AlCrSiN the and MoAlSiN alternate multiple coating oxidation resistance temperature that the present invention deposits up to 900 DEG C or more,
Hardness is greater than HV2800, and coefficient of friction is lower than 0.5.
Preparation method of the present invention is simple, and technology controlling and process is good, environmentally protective, at low cost, it is easy to accomplish industrialized production.
Detailed description of the invention
Fig. 1 is AlCrSiN and MoAlSiN laminated coating structural schematic diagram.
1. matrix；2. prime coat；3. alternate multiple；4.AlCrSiN layers；5.MoAlSiN layers.
Specific embodiment
Embodiment 1
(1) hard alloy substrate is subjected to degreasing and rust removal cleaning, is put into vacuum chamber after drying；
(2) vacuum chamber is evacuated to lower than 5 × 10-3Pa, argon gas, air pressure 0.2Pa are passed through into vacuum chamber, and bias is
500V carries out sputter clean to matrix using ion source；
(3) it deposits prime coat: opening cathode arc titanium target, ar pressure 0.3Pa, bias 50V, thickness 200nm；
(4) it deposits alternate multiple: being passed through nitrogen, matrix rotates in vacuum chamber, revolving speed 2rmp, is 1.0Pa, temperature in air pressure
Degree is 500 DEG C, under conditions of bias is 20V, forms multilayer knot by alternately opening AlCrSi alloys target and MoAlSi alloys target
Structure, AlCrSiN layers of single monolayer thick are 60nm, and MoAlSiN layers of single monolayer thick are 30nm, and overall thickness is 2.5 μm.Wherein Al in AlCrSi target
Content is 70 at.%, and Cr content is 20 at.%, and Si content is 10 at.%；Mo content is 67 at.% in MoAlSi target, and Al contains
Amount is 13 at.%, and Si content is 20 at.%.
AlCrSiN the and MoAlSiN laminated coating hardness of preparation is HV3530, and oxidation resistance temperature is greater than 900 DEG C, friction system
Number is 0.36, and coating has excellent wear-resisting property and antioxygenic property.
Embodiment 2
(1) hard alloy substrate is subjected to degreasing and rust removal cleaning, is put into vacuum chamber after drying；
(2) vacuum chamber is evacuated to lower than 5 × 10-3Pa, argon gas, air pressure 0.5Pa are passed through into vacuum chamber, and bias is
800V carries out sputter clean to matrix using ion source；
(3) it deposits prime coat: opening cathode arc Cr target, ar pressure 0.4Pa, bias 80V, thickness 300nm；
(4) it deposits alternate multiple: being passed through nitrogen, matrix rotates in vacuum chamber, revolving speed 4rmp, is 2.0Pa, temperature in air pressure
Degree is 300 DEG C, under conditions of bias is 100V, forms multilayer knot by alternately opening AlCrSi alloys target and MoAlSi alloys target
Structure, AlCrSiN layers of single monolayer thick are 120nm, and MoAlSiN layers of single monolayer thick are 60nm, and overall thickness is 4.2 μm.Wherein in AlCrSi target
Al content is 60 at.%, and Cr content is 25 at.%, and Si content is 15at.%；Mo content is 55 at.% in MoAlSi target, and Al contains
Amount is 30 at.%, and Si content is 15 at.%.
AlCrSiN the and MoAlSiN laminated coating hardness of preparation is HV3300, and oxidation resistance temperature is greater than 900 DEG C, friction system
Number is 0.42, and coating has excellent wear-resisting property.
Embodiment 3
(1) hard alloy substrate is subjected to degreasing and rust removal cleaning, is put into vacuum chamber after drying；
(2) vacuum chamber is evacuated to lower than 5 × 10-3Pa, argon gas, air pressure 0.5Pa are passed through into vacuum chamber, and bias is
200V carries out sputter clean to matrix using ion source；
(3) it deposits prime coat: opening cathode arc Zr target, ar pressure 0.6Pa, bias 120V, thickness 100nm；
(4) it deposits alternate multiple: being passed through nitrogen, matrix rotates in vacuum chamber, revolving speed 3rmp, is 4.0Pa, temperature in air pressure
Degree is 400 DEG C, under conditions of bias is 200V, forms multilayer knot by alternately opening AlCrSi alloys target and MoAlSi alloys target
Structure, AlCrSiN layers of single monolayer thick are 200nm, and MoAlSiN layers of single monolayer thick are 120nm, and overall thickness is 5.1 μm.Wherein in AlCrSi target
Al content is 50 at.%, and Cr content is 48 at.%, and Si content is 8at.%；Mo content is 50 at.% in MoAlSi target, and Al contains
Amount is 40 at.%, and Si content is 10at.%.
AlCrSiN the and MoAlSiN laminated coating hardness of preparation is HV3050, and oxidation resistance temperature is greater than 900 DEG C, friction system
Number is 0.46, and coating has excellent wear-resisting property and antioxygenic property.
Embodiment 4
(1) hard alloy substrate is subjected to degreasing and rust removal cleaning, is put into vacuum chamber after drying；
(2) vacuum chamber is evacuated to lower than 5 × 10-3Pa, argon gas, air pressure 0.8Pa are passed through into vacuum chamber, and bias is
600V carries out sputter clean to matrix using ion source；
(3) it deposits prime coat: opening cathode arc W target, ar pressure 0.8Pa, bias 200V, thickness 50nm；
(4) it deposits alternate multiple: being passed through nitrogen, matrix rotates in vacuum chamber, revolving speed 4rmp, is 6.0Pa, temperature in air pressure
Degree is 200 DEG C, under conditions of bias is 300V, forms multilayer knot by alternately opening AlCrSi alloys target and MoAlSi alloys target
Structure, AlCrSiN layers of single monolayer thick are 300nm, and MoAlSiN layers of single monolayer thick are 200nm, and overall thickness is 5.8 μm.Wherein in AlCrSi target
Al content is 40 at.%, and Cr content is 55 at.%, and Si content is 5at.%；Mo content is 45 at.% in MoAlSi target, and Al contains
Amount is 50 at.%, and Si content is 5 at.%.
AlCrSiN the and MoAlSiN laminated coating hardness of preparation is HV2970, and oxidation resistance temperature is greater than 900 DEG C, friction system
Number is 0.48, and coating has excellent wear-resisting property and antioxygenic property.
Claims (6)
1. a kind of high-temperature oxidation resistant self-lubricating laminated coating, it is characterized in that high-temperature oxidation resistant self-lubricating laminated coating is successively by base
Prime coat (2) and alternate multiple (3) composition on body (1), the alternate multiple (3) is by AlCrSiN layers (4) and MoAlSiN
Layer (5) is sequentially overlapped composition, and wherein AlCrSiN layers of (3) thickness in monolayer are 50 ~ 300nm, and MoAlSiN layers of (4) thickness in monolayer are 30
~ 200nm, laminated coating overall thickness are 1 ~ 10 μm.
2. high-temperature oxidation resistant self-lubricating laminated coating according to claim 1, it is characterized in that the matrix (1) is hard
Alloy, high-speed steel, mould steel or bearing steel.
3. high-temperature oxidation resistant self-lubricating laminated coating according to claim 1, it is characterized in that the prime coat (2) is chromium
Layer, titanium layer, zirconium layer or tungsten layer.
4. the preparation method of high-temperature oxidation resistant self-lubricating laminated coating described in claim 1, it is characterized in that successively by following step
Rapid composition:
(1) matrix is subjected to degreasing and rust removal cleaning, is put into vacuum chamber after drying；
(2) vacuum chamber is evacuated to lower than 5 × 10-3Pa, is passed through argon gas into vacuum chamber, and air pressure is 0.1 ~ 0.8Pa, and bias is 200 ~
800V carries out sputter clean to matrix using ion source；
(3) prime coat is deposited: unlatching cathode arc chromium target, titanium target, zirconium target or tungsten target, 0.3 ~ 2Pa of ar pressure, bias 50 ~
200V, 50 ~ 300nm of thickness；
(4) it deposits alternate multiple: being passed through nitrogen, matrix rotates in vacuum chamber, 1 ~ 8rpm of revolving speed, is 0.5 ~ 6Pa, temperature in air pressure
Degree is 200 ~ 500 DEG C, under conditions of bias is 20 ~ 300 V, by alternately opening AlCrSi alloys target and MoAlSi alloys target shape
At multilayered structure.
5. the preparation method of high-temperature oxidation resistant self-lubricating laminated coating according to claim 4, it is characterized in that described
Al content is 40 ~ 70 at.% in AlCrSi alloys target, and Si content is 5 ~ 15 at.%, surplus Cr.
6. the preparation method of high-temperature oxidation resistant self-lubricating laminated coating according to claim 4, it is characterized in that described
Al content is 13 ~ 50 at.% in MoAlSi alloys target, and Si content is 5 ~ 20 at.%, surplus Mo.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2799372C1 (en) * | 2023-03-29 | 2023-07-05 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Казанский национальный исследовательский технический университет им. А.Н. Туполева - КАИ" | Method for applying a protective coating to a metal mold for casting magnesium alloys |
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| CN109161841B (en) * | 2018-07-27 | 2020-07-21 | 广东工业大学 | AlCrN/AlCrSiN superhard nano composite multilayer coating and preparation method and application thereof |
| CN112628381B (en) * | 2020-12-02 | 2022-05-10 | 东南大学 | Temperature self-adaptive lubricating gear and preparation method thereof |
| CN113025966B (en) * | 2021-02-26 | 2022-05-17 | 何阳轩 | Zr-based high-entropy alloy coating for prolonging service life of hot forging die and preparation method thereof |
| CN113529012B (en) * | 2021-07-21 | 2024-01-26 | 国网天津市电力公司电力科学研究院 | MoSi for modifying surface Al of power transmission and transformation equipment 2 Preparation method of-SiC coating |
| CN115505886B (en) * | 2022-09-23 | 2023-10-24 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | AlCrSiN/AlCrMoSiN nano multilayer composite coating with high hardness and high wear resistance and preparation method thereof |
| CN115404438B (en) * | 2022-09-23 | 2024-02-06 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | Preparation process of AlCrSiN/AlCrMoSiN nano multilayer composite coating with high hardness and high wear resistance |
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| JP5218834B2 (en) * | 2008-09-01 | 2013-06-26 | 三菱マテリアル株式会社 | Film forming method and film forming apparatus |
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| CN103757597B (en) * | 2014-02-07 | 2016-03-23 | 上海理工大学 | A kind of TiN/CrAlSiN nanocomposite laminated coating and preparation method thereof |
| CN104002516B (en) * | 2014-06-10 | 2016-02-10 | 上海理工大学 | A kind of CrAlN/MoS with high rigidity and low-friction coefficient 2laminated coating and preparation method thereof |
| CN105779948A (en) * | 2016-03-08 | 2016-07-20 | 武汉大学苏州研究院 | TiAlN/MoN multi-film composite coating and preparing method thereof |
| CN106191791A (en) * | 2016-07-06 | 2016-12-07 | 广东工业大学 | A kind of high temperature low friction Cr AlSiON nano-composite coating and preparation method thereof |
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| JP5218834B2 (en) * | 2008-09-01 | 2013-06-26 | 三菱マテリアル株式会社 | Film forming method and film forming apparatus |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2799372C1 (en) * | 2023-03-29 | 2023-07-05 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Казанский национальный исследовательский технический университет им. А.Н. Туполева - КАИ" | Method for applying a protective coating to a metal mold for casting magnesium alloys |
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