CN108118304A - Nano-composite coating and its preparation process - Google Patents
Nano-composite coating and its preparation process Download PDFInfo
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- CN108118304A CN108118304A CN201711400848.3A CN201711400848A CN108118304A CN 108118304 A CN108118304 A CN 108118304A CN 201711400848 A CN201711400848 A CN 201711400848A CN 108118304 A CN108118304 A CN 108118304A
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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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
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
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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
- C23C14/14—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
- 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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates 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
- 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
- C23C14/3485—Sputtering using pulsed power to the target
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- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to hard coat field is prepared in use physical vapour deposition (PVD) (PVD) method deposition, in particular to a kind of nano-composite coating and its preparation process.The preparation process of nano-composite coating, comprises the following steps：Nano-composite coating is settled on matrix using the compound mode of high-power impulse magnetron sputtering and DC pulse magnetron sputtering.The preparation process is simple, reproducible, and easy industrialized production, and the obtained nano-composite coating has higher hardness and toughness, good wear-resisting property, and the combination power between institutional framework densification, coating and matrix is strong.
Description
Technical field
The present invention relates in preparing hard coat field using physical vapour deposition (PVD) (PVD) method deposition, in particular to
A kind of nano-composite coating and its preparation process.
Background technology
In recent years, application of the hard coat on cutting tool, mold and component of machine is more and more extensive.Utilize hard
Coating, which carries out material surface protection, becomes an important channel for improving material property, this not change material overall performance
On the premise of pass through the film that a floor height hardness is deposited in material surface, it is not only economical but also can greatly improve material uses the longevity
Life.
TiB2For the magnesium-yttrium-transition metal compound with hexagonal crystal system C32 structures, boron atom face and titanium atom face alternately go out
Two dimensional surface net structure is now formed, unique crystal structure and electronic structure determine TiB2With a series of excellent reasons
Change performance：High rigidity, high-melting-point, high conductivity and thermal conductivity, excellent chemical stability etc..Boron atom and titanium atom mainly with
Covalent bonding together, hardness can be up to 68GPa after spatter film forming.But TiB2Coating as wear-resistant coating in use very
It is easily broken, the texture of column crystal makes it have anisotropy, and its crystal boundary perpendicular to surface provides short crackle
Extensions path substantially reduces its toughness.In order to improve TiB2The toughness of coating and anti-friction performance, can be in TiB2In mix
It is miscellaneous to obtain ternary or quaternary system into carbon elimination, nitrogen, prepare the multi-element coating with nano composite structure.
Nano-composite coating is to be embedded in shape in undefined structure (such as a-BN) by isolated nanocrystal (such as nc-TiN)
Into a kind of composite structure coating, for this composite coating, amorphous phase has mirror to repulsive force for dislocation, can prevent position
Wrong movement, and amorphous materials can preferably accommodate the mispairing of the crystal grain of random orientation, therefore with very high intensity
With excellent performance.Therefore this coating has high rigidity, high tenacity, excellent wear-resisting property, chemical stability and high warm surely
It is qualitative, it is suitable for cutting tool, mold and component of machine surface.Nanometer composite Ti-B-N coatings are by suitable nitrogen
It is doped in TiB2In coating, formed and nanocrystalline TiN/TiB is wrapped in amorphous BN phases2Composite construction.
But existing nano-composite coating is prepared using arc ion plating or DC pulse magnetron sputtering technique, is obtained
Nano-composite coating often there are rough surface, have large-size molten drop particle or with basal body binding force it is poor the shortcomings of.
The content of the invention
The present invention provides a kind of preparation process of nano-composite coating, the present invention utilizes high power pulse and DC pulse
Combined magnetic-controlled sputter technology deposits nano-composite coating on matrix surface, before guarantee high deposition rate, low deposition temperature
It puts, can deposit that acquisition is smooth fine and close and good with matrix reaction bonded, and high rigidity has both the nano-composite coating of high tenacity.
The present invention also provides a kind of nano-composite coating, which has higher hardness and toughness, well
Wear-resisting property, and institutional framework is fine and close, the combination power between coating and matrix is strong.
What the present invention was realized in：
A kind of preparation process of nano-composite coating, comprises the following steps：
Nanometer is settled on matrix using the mode that high-power impulse magnetron sputtering and DC pulse magnetron sputtering combine to answer
Close coating.
A kind of nano-composite coating is prepared by the preparation process of above-mentioned nano-composite coating.
The beneficial effects of the invention are as follows：The nano-composite coating preparation process of the present invention is simple, reproducible, and easily
Industrialized production；Nano combined painting is prepared by the compound mode of high-power impulse magnetron sputtering and DC pulse magnetron sputtering
Layer has higher hardness and toughness, good wear-resisting property, and the combination power between institutional framework densification, coating and matrix is strong.
Description of the drawings
It in order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of scope, for those of ordinary skill in the art, without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the electron-microscope scanning figure of experimental example 1 of the present invention.
Specific embodiment
It, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The nano-composite coating and its preparation process of the embodiment of the present invention are specifically described below.
A kind of preparation process of nano-composite coating, comprises the following steps：
S1, matrix surface pretreatment；
According to demand, suitable matrix is selected, matrix is metallic matrix, ceramic matrix or contains polymorphous matrix；
It is preferred that metallic matrix is alloy substrate, hard alloy substrate is more preferably；
It is preferred that it is polycrystalline diamond or polycrystal cubic boron nitride matrix containing polymorphous matrix.
It should be noted that metallic matrix can also include the matrix of simple metal, ceramic matrix can also include metal and make pottery
Porcelain.
By matrix surface after blasting treatment, it is placed in the Full-automatic ultrasonic cleaner for filling alkalinous metal cleaning solution
Oil is cleaned by ultrasonic and dry.
S2, preheating
Matrix by pretreatment is packed into vacuum film-coated furnace, vacuumizes, treats that vacuum degree reaches 1~5.0 × 10-3Pa
When, 350~550 DEG C are heated to vacuum drying oven.
S3, surface clean etching；
Before high-power impulse magnetron sputtering and DC pulse magnetron sputtering, etching is carried out to matrix surface,
Etching matrix under high energy electron and metal ion collective effect improves film substrate bond strength.
Etching include Glow Discharge Cleaning, Glow Discharge Cleaning be pressure be 0.3~0.9Pa, Dc bias for-
700~-500V, in the environment of carry out Glow Discharge Cleaning 5~15min；
Pressure is preferably 0.4~0.8Pa；More preferably 0.5~0.7Pa；
Dc bias is preferably -650~-550V.
Specifically, the vacuum degree of vacuum chamber maintains 1~5.0 × 10-3Pa is passed through argon gas and matrix surface progress aura is put
Electricity cleaning.The laggard row metal target build-up of luminance Bombardment and cleaning of Glow Discharge Cleaning, metal targets build-up of luminance Bombardment and cleaning is by high power arteries and veins
The control of magnetron sputtering power supply is rushed, is 0.5~2.5kW in power supply average output power, biases to bang in the environment of -300~-100V
Hit 5~20min of cleaning；
Average output power is preferably 1-2kW；Bias is preferably -250~-150V.
Specifically, carry out opening high-power impulse magnetron sputtering power supply after Glow Discharge Cleaning.
S4, transition zone is formed；
Before settling nano-composite coating, sputtered on matrix and form transition zone；Transition zone can be nano-composite coating with
Matrix, which combines, provides good combination power, promotes the wear-resisting property of nano-composite coating, and extending sputtering has nano-composite coating
The service life of matrix.
It is preferred that transition zone is obtained using high-power impulse magnetron sputtering.High-power impulse magnetron sputtering passes through one
(1~3kW/cm2 is common to one high pulse peak power density of short time (100~500 μ s) application in a pulse period
100 times or more of magnetron sputtering) high plasma density and ionization level are obtained, it can then obtain smooth fine and close and and base
The film that precursor reactant is well combined.
Specifically, after etching, reduction is biased into -100~-60V, and deposited metal forms transition zone, deposition temperature
400~600 DEG C of degree, 10~40min of sedimentation time.
It is prepared by S5, nano-composite coating；
Nanometer is settled on matrix using the compound mode of high-power impulse magnetron sputtering and DC pulse magnetron sputtering to answer
Coating is closed, i.e., nano-composite coating is settled on transition zone.High-power impulse magnetron sputtering has the effect of height ionization, can sink
Drop obtain it is smoother fine and close and with the good film of matrix reaction bonded, meanwhile, DC pulse magnetron sputtering has good heavy
Reduction of speed rate reduces depositing temperature, and effectively inhibits electric arc and generate and then eliminate the paintings such as resulting rough surface, particle be big
Layer defects.
Further, the target of high-power impulse magnetron sputtering is metal targets；Preferably, metal targets are transition gold
Belong to, more preferably titanium.Metal targets fusing point opposing metallic compound target is relatively low, using high-power impulse magnetron sputtering profit
High metal ionization level can be realized with higher pulse peak power and relatively low pulse duty factor, is promoted in nano-composite coating
Tenor, further promoted nano-composite coating intensity and rub proofness.And transition metal has good crystal structure
And electronic structure so that transition metal has excellent physicochemical property, can further promote the intensity and wear-resisting property of matrix.
Except titanium, the transition metal such as crome metal, metal zirconium, metallic silicon, metallic nickel can also be used.
Further, the target of DC pulse magnetron sputtering is metallic compound target, it is preferable that metallic compound target
For transistion metal compound, more preferably transition metal boron compound.It can be ensured using DC pulse magnetron sputtering more excellent
Sedimentation rate, relatively low depositing temperature, meanwhile, the transistion metal compound of use can ensure to be formed in nano-composite coating
Amorphous phase wraps up the composite construction of nano.Further electedly, transistion metal compound is high-power impulse magnetron sputtering
Metal targets compound, then ensure nano-composite coating in ingredient it is consistent, provided for nano-composite coating more excellent
Mechanical strength and wear-resisting property.Nanocrystalline formation can further be wrapped up convenient for amorphous using transition metal boron compound.Example
Such as, metal targets are Titanium, and transistion metal compound is the compound of Titanium, further using titanium boride.
Further, when high-power impulse magnetron sputtering and DC pulse magnetron sputtering combine sputtering, operating pressure is
0.4~0.9Pa；
Bias is -100~-60V, is preferably -90~-70V, more preferably -80~-75V；
Depositing temperature is 300~500 DEG C；Preferably 350-450 DEG C；More preferably 400-420 DEG C；
DC pulse magnetron sputtering transistion metal compound target average output power is 5.5~9.5kW, is preferably 6-
8kW。
Further, high-power impulse magnetron sputtering and DC pulse magnetron sputtering are in inert gas and anti-with reference to sputtering
It answers and sputtering is carried out at the same time under the atmosphere of gas mixing；
It is preferred that the throughput of the reaction gas and the throughput of the inert gas and the throughput of the reaction gas
The ratio between summation is 0.2-0.5:1；Preferably 0.3-0.4:1.
Inert gas can be argon gas, and reaction gas is nitrogen.Stringent control settlement condition when depositing nano-composite coating
And the flow of nitrogen, obtained nano-composite coating compact structure, high rigidity, high tenacity.
Specifically, after forming transition zone, reaction gas i.e. nitrogen is passed through in first vacuum chamber, and (purity of nitrogen is
99.999%), the ratio between the throughput of nitrogen and the throughput of the inert gas are 0.2-0.5:1, then strictly control work
Pressure, bias-voltage, average output power etc..
The present invention also provides a kind of nano-composite coating, the preparation process including above-mentioned nano-composite coating is prepared into
It arrives.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of preparation processes of nano-composite coating, comprise the following steps：
S1, matrix surface pretreatment
Matrix elects hard alloy as.Matrix surface is placed in after blasting treatment and fills the full-automatic of alkalinous metal cleaning solution
It deoils, be cleaned by ultrasonic and dry in supersonic wave cleaning machine.
S2, preheating
Hard alloy substrate by pretreatment is packed into vacuum film-coated furnace, is vacuumized, treat vacuum degree reach 3.0 ×
During 10-3Pa, 350 DEG C~550 DEG C are heated to vacuum drying oven.
S3, surface clean etching；
The vacuum degree of vacuum chamber maintains 4 × 10-3Then Pa is passed through argon gas in vacuum chamber and carries out aura to matrix surface
Discharge Cleaning.It in pressure is 0.3Pa that Discharge Cleaning, which is, and Dc bias carries out Glow Discharge Cleaning 5min in the environment of being -700V.
Specifically, carry out opening high-power impulse magnetron sputtering power supply, average output power 0.5kW after Discharge Cleaning；
It biases as Bombardment and cleaning 5min in the environment of -300V.
S4, transition zone is formed；
After cleaning, reduction is biased into -100V, and deposited metal titanium 10min forms transition zone, 400 DEG C of depositing temperature.
It is prepared by S5, nano-composite coating；
After forming transition zone, reaction gas i.e. nitrogen (purity of nitrogen is 99.999%), nitrogen are passed through in first vacuum chamber
The ratio between the throughput of throughput and the inert gas be 0.2:1, then operating pressure is 0.4Pa；DC pulse magnetic control splashes
Penetrate titanium diboride, average output power 5.5；High-power impulse magnetron sputtering Titanium target is biased as -100V, deposition
Temperature is 300 DEG C.
The present embodiment also provides a kind of nano-composite coating, is prepared by above-mentioned nano-composite coating.
Embodiment 2
A kind of nano combined painting that a kind of preparation process of nano-composite coating provided in this embodiment is provided with embodiment 1
The preparation process of layer, basic operation is consistent, and different is only that, the raw material of operating condition and selection changes.
Raw material：Matrix is metallic matrix, and metal targets are crome metal, and metallic compound target is chromium boride.
Operating condition：Vacuum degree is 5.0 × 10-3Pa, Discharge Cleaning be pressure be 0.9Pa；Dc bias is -500V's
Glow Discharge Cleaning 15min is carried out under environment.Metal targets build-up of luminance Bombardment and cleaning is to be biased in average output power for 2.5kW
For Bombardment and cleaning 20min in the environment of -100V.
After cleaning, reduction is biased into -60V, and deposited metal chromium 40min forms transition zone, 600 DEG C of depositing temperature.
Reaction gas nitrogen is subsequently passed, the ratio between the throughput of nitrogen and the throughput of inert gas are 0.5:1, high power
When pulsed magnetron sputtering and DC pulse magnetron sputtering compound action, operating pressure 0.9Pa；DC pulse magnetron sputtering is put down
Equal output power is 9.5kW；It biases as -60V；Depositing temperature is 500 DEG C.
Embodiment 3
A kind of nano combined painting that a kind of preparation process of nano-composite coating provided in this embodiment is provided with embodiment 1
The preparation process of layer, basic operation is consistent, and different is only that, the raw material of operating condition and selection changes.
Raw material：Matrix is cermet, and metal targets are metal zirconium, and metallic compound target is zirconium diboride.
Operating condition：Vacuum degree be 2.0 × 10-3Pa, Discharge Cleaning be pressure be 0.4Pa；Dc bias is -650V
In the environment of carry out Glow Discharge Cleaning 10min.Metal targets build-up of luminance bombardment be average output power be 1kW bias for-
Bombardment and cleaning 15min in the environment of 250V.
After cleaning, reduction is biased into -90V, and deposited metal zirconium 20min forms transition zone, 500 DEG C of depositing temperature.
The ratio between the throughput of nitrogen and the throughput of inert gas are 0.3:1, high-power impulse magnetron sputtering and direct current arteries and veins
When rushing magnetron sputtering compound action, operating pressure 0.7Pa；The average output power of DC pulse magnetron sputtering is 6kW；Bias
For -90V；Depositing temperature is 350 DEG C.
Embodiment 4
A kind of nano combined painting that a kind of preparation process of nano-composite coating provided in this embodiment is provided with embodiment 1
The preparation process of layer, basic operation is consistent, and different is only that, the raw material of operating condition and selection changes.
Raw material：Matrix is polycrystal cubic boron nitride, and metal targets are metallic silicon, and metallic compound target is silicon boride.
Operating condition：Vacuum degree be 3.0 × 10-3Pa, Discharge Cleaning be pressure be 0.8Pa；Dc bias is -550V
In the environment of carry out Glow Discharge Cleaning 7min.It in average output power is 2kW biass for -150V that the bombardment of metal targets build-up of luminance, which is,
In the environment of Bombardment and cleaning 10min.
After cleaning, reduction is biased into -70V, and deposited metal silicon 30min forms transition zone, 450 DEG C of depositing temperature.
The ratio between the throughput of nitrogen and the throughput of inert gas are 0.4:1, high-power impulse magnetron sputtering and direct current arteries and veins
When rushing magnetron sputtering compound action, operating pressure 0.5Pa；The average output power of DC pulse magnetron sputtering is 8kW；Bias
For -70V；Depositing temperature is 450 DEG C.
Embodiment 5
A kind of nano combined painting that a kind of preparation process of nano-composite coating provided in this embodiment is provided with embodiment 1
The preparation process of layer, basic operation is consistent, and different is only that, the raw material of operating condition and selection changes.
Raw material：Matrix is polycrystalline diamond, and metal targets are metallic nickel, and metallic compound target is nickel borides.
Operating condition：Vacuum degree be 4.0 × 10-3Pa, Discharge Cleaning be pressure be 0.5Pa；Dc bias is -600V
In the environment of carry out Glow Discharge Cleaning 12min.Metal targets build-up of luminance bombardment be average output power be 1.5kW bias for-
Bombardment and cleaning 12min in the environment of 200V.
After cleaning, reduction is biased into -80V, and deposited metal nickel 25min forms transition zone, 550 DEG C of depositing temperature.
The ratio between the throughput of nitrogen and the throughput of inert gas are 0.25:1, high-power impulse magnetron sputtering and direct current arteries and veins
When rushing magnetron sputtering compound action, operating pressure 0.6Pa；The average output power of DC pulse magnetron sputtering is 7kW；Bias
For -80V；Depositing temperature is 400 DEG C.
Embodiment 6
A kind of nano combined painting that a kind of preparation process of nano-composite coating provided in this embodiment is provided with embodiment 1
The preparation process of layer, basic operation is consistent, and different is only that, the raw material of operating condition and selection changes.
Raw material：Matrix is ceramic matrix, and metal targets are tungsten, and metallic compound target is tungsten boride.
Operating condition：Vacuum degree is 3.5 × 10-3Pa, Discharge Cleaning be pressure be 0.65Pa；Dc bias is -580V
In the environment of carry out Glow Discharge Cleaning 8min.Metal targets build-up of luminance bombardment be average output power be 0.9kW bias for-
Bombardment and cleaning 18min in the environment of 235V.
After cleaning, reduction is biased into -85V, and deposited metal tungsten 37min forms transition zone, 530 DEG C of depositing temperature.
The ratio between the throughput of nitrogen and the throughput of inert gas are 0.35:1, high-power impulse magnetron sputtering and direct current arteries and veins
When rushing magnetron sputtering compound action, operating pressure 0.5Pa；The average output power of DC pulse magnetron sputtering is 7.5kW；Partially
It presses as -75V；Depositing temperature is 420 DEG C.
Comparative example:It uses the raw material of embodiment 1 and preparation method to prepare nano-composite coating, and difference lies in only adopt
With DC pulse magnetron sputtering.
Experimental example 1
Electron-microscope scanning is carried out to the nano-composite coating that the embodiment of the present invention 1 and comparative example are prepared, concrete outcome is such as
Shown in Fig. 1.
It is the nano-composite coating cross-section morphology figure that the embodiment of the present invention 1 is prepared according to (a) in Fig. 1, it is known that obtain
Nano-composite coating, surface is smooth, compact structure, in high-power impulse magnetron sputtering and the compound work of DC pulse magnetron sputtering
Under, amorphous package nanocrystalline structure can realize intermixing, and coating has both high rigidity and high tenacity.It is pair according to (b) in Fig. 1
The nano-composite coating cross-section morphology figure that ratio is prepared, it is known that the nano-composite coating of acquisition is in the form of a column crystals growth, unfavorable
In the extension for preventing crackle, coating has certain brittleness.
Experimental example 2
To the nano-composite coating that the embodiment of the present invention 1 and comparative example are prepared, hardness is tested by nano-hardness tester,
The test of sound emission scratching instrument combines power, the hardness of nano-composite coating obtained by 1 two kinds of preparation methods of result table as shown in table 1 below
With with reference to power
Embodiment 1 is relatively compared using high-power impulse magnetron sputtering and DC pulse magnetron sputtering are compound according to table 1
The nano-composite coating that example is obtained only with DC pulse magnetron sputtering has higher hardness, and coating has stronger with matrix
With reference to power.
In conclusion the nano-composite coating preparation process of the present invention is simple, it is reproducible, and easily industrial metaplasia
Production；The nano-composite coating prepared has higher hardness and toughness, good wear-resisting property, and institutional framework densification, painting
Combination power between layer and matrix is strong.
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the invention, for this field
For technical staff, the invention may be variously modified and varied.Within the spirit and principles of the invention, that is made is any
Modification, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation process of nano-composite coating, which is characterized in that comprise the following steps：
Nano combined painting is settled on matrix using the compound mode of high-power impulse magnetron sputtering and DC pulse magnetron sputtering
Layer.
2. the preparation process of nano-composite coating according to claim 1, which is characterized in that high-power impulse magnetron sputtering
Target be metal targets；Preferably, the metal targets are transition metal, more preferably titanium；
The target of DC pulse magnetron sputtering is metallic compound target, it is preferable that the metallic compound target is transition gold
Belong to compound, more preferably transition metal boron compound.
3. the preparation process of nano-composite coating according to claim 1, which is characterized in that high-power impulse magnetron sputtering
It is to be carried out at the same time sputtering under inert gas and the atmosphere of reaction gas mixing with the compound sputtering of DC pulse magnetron sputtering；
It is preferred that the throughput of the reaction gas and the throughput of the inert gas and the throughput summation of the reaction gas
The ratio between be 0.2-0.5:1；Preferably 0.3-0.4:1.
4. according to the preparation process of claim 1-3 any one of them nano-composite coatings, which is characterized in that high power pulse
Magnetron sputtering and DC pulse magnetron sputtering compound tense, operating pressure are 0.4~0.9Pa；
Bias is -100~-60V, is preferably -90~-70V, more preferably -80~-75V；
Depositing temperature is 300~500 DEG C；Preferably 350-450 DEG C；More preferably 400-420 DEG C；
DC pulse magnetron sputtering power supply average output power is 5.5~9.5kW, is preferably 6-8kW.
5. according to the preparation process of claim 1-3 any one of them nano-composite coatings, which is characterized in that utilize high power
Before pulsed magnetron sputtering and the compound sputtering of DC pulse magnetron sputtering, sputtering on the matrix forms transition zone；
It is preferred that the transition zone is obtained using high-power impulse magnetron sputtering.
6. according to the preparation process of claim 1-3 any one of them nano-composite coatings, which is characterized in that utilize high power
Before pulsed magnetron sputtering and DC pulse magnetron sputtering combine sputtering, etching is carried out to described matrix；
It is preferred that etching includes Glow Discharge Cleaning and metal targets build-up of luminance Bombardment and cleaning；
More preferably；Metal targets build-up of luminance Bombardment and cleaning is controlled by high-power impulse magnetron sputtering power supply.
7. the preparation process of nano-composite coating according to claim 6, which is characterized in that Discharge Cleaning is to be in pressure
0.3~0.9Pa, Dc bias carry out 5~15min of Glow Discharge Cleaning in the environment of being -700~-500V；
Pressure is preferably 0.4~0.8Pa；More preferably 0.5~0.7Pa；
Dc bias is preferably -650~-550V.
8. the preparation process of nano-composite coating according to claim 6, which is characterized in that the bombardment of metal targets build-up of luminance is clear
Wash be high-power impulse magnetron sputtering power supply average output power be 0.5~2.5kW, bias the environment for -300~-100V
5~20min of lower Bombardment and cleaning；
Average output power is preferably 1-2kW；Bias is preferably -250~-150V.
9. according to the preparation process of claim 1-3 any one of them nano-composite coatings, which is characterized in that described matrix is
Metallic matrix, ceramic matrix contain polymorphous matrix；
It is preferred that the metallic matrix is alloy substrate, hard alloy substrate is more preferably；
It is preferred that it is described containing polymorphous matrix be polycrystalline diamond or polycrystal cubic boron nitride matrix.
10. a kind of nano-composite coating, which is characterized in that it passes through the preparation work of nano-composite coating described in claim 1
Skill is prepared.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111500990A (en) * | 2020-06-01 | 2020-08-07 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | Zr-Ti-B-N nano composite coating and preparation method thereof |
| CN112725754A (en) * | 2020-12-15 | 2021-04-30 | 南京航空航天大学 | Coating material, preparation method and alloy material |
| CN113718195A (en) * | 2021-08-31 | 2021-11-30 | 中国科学院宁波材料技术与工程研究所 | High-pressure-resistant abrasion-resistant protective composite coating and preparation method and application thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463391A (en) * | 2015-01-09 | 2016-04-06 | 天津职业技术师范大学 | A kind of nanocrystalline ZrB2 superhard coating and its preparation method |
| CN105887012A (en) * | 2016-01-11 | 2016-08-24 | 天津职业技术师范大学 | Preparation technology of Zr-B-N nano-composite coating |
| CN106893991A (en) * | 2017-02-27 | 2017-06-27 | 天津职业技术师范大学 | Preparation process of Zr-B-O-N nano composite coating |
-
2017
- 2017-12-22 CN CN201711400848.3A patent/CN108118304A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105463391A (en) * | 2015-01-09 | 2016-04-06 | 天津职业技术师范大学 | A kind of nanocrystalline ZrB2 superhard coating and its preparation method |
| CN105887012A (en) * | 2016-01-11 | 2016-08-24 | 天津职业技术师范大学 | Preparation technology of Zr-B-N nano-composite coating |
| CN106893991A (en) * | 2017-02-27 | 2017-06-27 | 天津职业技术师范大学 | Preparation process of Zr-B-O-N nano composite coating |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111500990A (en) * | 2020-06-01 | 2020-08-07 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | Zr-Ti-B-N nano composite coating and preparation method thereof |
| CN111500990B (en) * | 2020-06-01 | 2022-05-24 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | Zr-Ti-B-N nano composite coating and preparation method thereof |
| CN112725754A (en) * | 2020-12-15 | 2021-04-30 | 南京航空航天大学 | Coating material, preparation method and alloy material |
| CN112725754B (en) * | 2020-12-15 | 2021-12-21 | 南京航空航天大学 | A kind of coating material, preparation method and alloy material |
| CN113718195A (en) * | 2021-08-31 | 2021-11-30 | 中国科学院宁波材料技术与工程研究所 | High-pressure-resistant abrasion-resistant protective composite coating and preparation method and application thereof |
| CN114717516A (en) * | 2022-03-01 | 2022-07-08 | 中国科学院宁波材料技术与工程研究所 | TiAl/Ti with strong bonding and high corrosion resistance2Preparation method of AlC coating |
| CN114717516B (en) * | 2022-03-01 | 2024-05-31 | 中国科学院宁波材料技术与工程研究所 | Strongly-combined high corrosion-resistant TiAl/Ti2Preparation method of AlC coating |
| CN114672779A (en) * | 2022-04-13 | 2022-06-28 | 上海大学 | A kind of preparation method of TiB2/Ti composite coating |
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