CN109402564A - A kind of AlCrSiN and AlCrSiON double-layer nanometer composite coating and preparation method thereof - Google Patents
A kind of AlCrSiN and AlCrSiON double-layer nanometer composite coating and preparation method thereof Download PDFInfo
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- CN109402564A CN109402564A CN201811355670.XA CN201811355670A CN109402564A CN 109402564 A CN109402564 A CN 109402564A CN 201811355670 A CN201811355670 A CN 201811355670A CN 109402564 A CN109402564 A CN 109402564A
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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
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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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
- C23C14/0676—Oxynitrides
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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
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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
- 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
- C23C28/04—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 only coatings of inorganic non-metallic material
- C23C28/044—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 only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
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Abstract
The invention discloses a kind of AlCrSiN and AlCrSiON double-layer nanometer composite coatings and preparation method thereof, and the hard alloy to be coated after cleaning is placed in coating machine, carry out aura cleaning；It is then turned on Cr target, arc ource electric current is adjusted to 90A, adjusts pulsed bias each Bombardment and cleaning 2min at -800V, -600V, -400V, -200V respectively；It is passed through argon gas 50sccm, nitrogen 200sccm, adjusting pulsed bias is -100V, deposits CrN metal nitride transition zone 20min；Cr target is closed, opens two AlCrSi targets, electric current 90A, argon gas 50sccm, nitrogen 600sccm, temperature is heated to be 450 DEG C, and bias is first arranged, and gradient increases from 80V to 200V, depositing Al CrSiN coating 90min；After be passed through oxygen 20sccm, from 200V to 80V, gradient declines bias, depositing Al CrSiON coating 90min.The nano-composite coating that the present invention develops hardness with higher, toughness, wearability, with matrix bond strength with higher.
Description
Technical field
The invention belongs to coat preparing technology fields, and in particular to a kind of AlCrSiN and AlCrSiON double-layer nanometer is compound
Coating and preparation method thereof.
Background technique
Nowadays, with the fast development of the manufacturing technology trend of globalization, requirement to mechanical processing industry cutting technology by
Step improves.The appearance of cutter coat makes processing high efficiency, accuracy, degree of specialization all be conducive to manufacturing progress, thus
Cutting-Tool Coating Technology obtains the extensive concern of world's every country.The extensive use of various high-strength alloys and chilled cast iron, vapour
The continuous improvement of car engine Thin Wall Cylinder Blocks, cylinder cap, crankshaft, the machining accuracy of camshaft and efficiency requirements, these are all to high speed
Cutting technology proposes new demand.It selects suitable cutting tool coating material to cutter material consumption is reduced, obtains good processing
Precision and surface quality, improving service life, efficiency of cutting of hardworking material cutter etc. all has decisive role.Cutter applies
The usage environment of layer is very harsh and complicated, and usual coating surface will bear 900-1000 DEG C or more of high temperature and more than 1GPa's
Stress loading.Therefore the design of coating will comprehensively consider its bond strength, hardness, toughness, thermal stability and chemical stability, friction
The factors such as coefficient, thermally conductive and thermal expansion coefficient.
Nano-composite coating is to be embedded in a kind of composite construction formed in very thin amorphous layer by isolated nanocrystal
Coating.Nanocrystalline hardness is high, and amorphous phase plasticity is good, and two-phase interface cohesive energy is high, and crystal phase and amorphous phase are thermodynamically in point
From trend；It is tiny it is nanocrystalline in can not form dislocation, intercrystalline thin amorphous layer can effectively stop Grain Boundary Sliding, a large amount of two
Phase interface increases micro-crack extension resistance, therefore this coating has high rigidity, high tenacity, excellent wear-resisting property and Gao Wenre
Stability.In recent years, the advantages that AlCrSiN nano-composite coating is due to its excellent wearability, inoxidizability and high rigidity, quilt
Think to be very suitable for one of the high-quality thin-film applied to tool surface.Al element in coating can play solution strengthening effect, in height
Fine and close Al can be formed under the conditions of temperature in coating outer surface2O3、Cr2O3Protective layer, to improve in coating mechanical processing process
Inoxidizability and thermal stability；Si element can form the composite junction that amorphous SiNx layer is wrapped in (Al, Cr) N nanocrystal
Structure.And the inoxidizability and thermal stability of coating can be improved by adding oxygen element in nitride coatings, while can also be with
Change the mechanical property of coating.But the hardness of simple AlCrSiON coating, wearability and have with the bond strength of matrix
Wait improve.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of AlCrSiN and AlCrSiON double-layer nanometers
Composite coating and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of AlCrSiN and AlCrSiON double-layer nanometer composite coating, has been sequentially depositing CrN mistake on hard alloy substrate
Cross layer, AlCrSiN coating and AlCrSiON coating.
A kind of AlCrSiN and AlCrSiON double-layer nanometer composite coating the preparation method is as follows:
Step 1: the hard alloy to be coated after cleaning is placed in coating machine, and the base vacuum of vacuum chamber is evacuated to 2
×10-3Pa opens heating system for furnace body and is warming up to 400 DEG C；It is passed through 400sccm argon gas, adjusts pulsed bias to -800V, brightness
Light cleans 20min；
Step 2: adjusting argon gas is 100sccm, opens Cr target, and arc ource electric current is adjusted to 90A, adjusts pulsed bias difference
Each Bombardment and cleaning 2min at -800V, -600V, -400V, -200V；
Step 3: being passed through argon gas 50sccm, nitrogen 200sccm, and adjusting pulsed bias is -100V, deposits CrN nitride metal
Object transition zone 20min；
Step 4: closing Cr target, opens two AlCrSi targets, electric current 90A, argon gas 50sccm, nitrogen 600sccm, temperature
Degree is heated to be 450 DEG C, and bias is first arranged, and from 80V to 200V, gradient increases, depositing Al CrSiN coating 90min；After be passed through oxygen
20sccm, from 200V to 80V, gradient declines bias, depositing Al CrSiON coating 90min.
The advantages and benefits of the present invention are:
1. the nano-composite coating that the present invention develops hardness with higher and toughness, wear-resisting property are good.
2. the nano-composite coating that the present invention develops high-temperature thermal stability performance with higher and corrosion resisting property, can be used for height
Rapid-curing cutback machining field.
3. uniform coating thickness and compact structure that the present invention develops, with matrix bond strength with higher.
4. the nano-composite coating preparation process that the present invention develops is reproducible, have a wide range of application, there is very strong reality
The property used.
Detailed description of the invention
Fig. 1 is the XRD diffraction spectrogram of AlCrSiN and AlCrSiON double-layer nanometer composite coating prepared by embodiment one.
Fig. 2 is the surface topography map of AlCrSiN and AlCrSiON double-layer nanometer composite coating prepared by embodiment one.
Fig. 3 is the Cross Section Morphology figure of AlCrSiN and AlCrSiON double-layer nanometer composite coating prepared by embodiment one.
Fig. 4 is the scratch shape appearance figure of AlCrSiN and AlCrSiON double-layer nanometer composite coating prepared by embodiment two.
Fig. 5 is the friction coefficient curve of AlCrSiN and AlCrSiON double-layer nanometer composite coating prepared by embodiment two.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, combined with specific embodiments below furtherly
Bright technical solution of the present invention.
Embodiment one
The present embodiment is the depositing coating on the single crystalline Si piece ((100) be orientated) mirror-finished, specimen size is 40 ×
20×0.7mm；Sample is first respectively cleaned by ultrasonic 20 minutes in acetone and alcoholic solution respectively, is then dried up with high pure nitrogen, then
Face target is placed in vacuum chamber on sample frame.Filming equipment uses AIP-650 type arc ion plating machine, cathode targets choosing
With metal Cr (purity 99.9wt.%) and alloy AlCrSi (6:3:1), metal Cr is used for the Bombardment and cleaning and deposition of matrix surface
Transition zone, alloy AlCrS are used for depositing coating, and working gas selects high-purity Ar and N2 (purity is 99.99%)；AlCrSiN
With AlCrSiON double-layer nanometer composite coating the preparation method is as follows:
Step 1: the base vacuum of vacuum chamber is evacuated to 2 × 10-3Pa opens heating system for furnace body and is warming up to 400 DEG C；
It is passed through 400sccm argon gas, adjusts pulsed bias to -800V, operating pressure is maintained at 2 × 10-3Pa, aura clean 20min；
Step 2: adjusting argon gas is 100sccm, opens Cr target, and arc ource electric current is adjusted to 90A, adjusts pulsed bias difference
Each Bombardment and cleaning 2min at -800V, -600V, -400V, -200V；
Step 3: being passed through argon gas 50sccm, nitrogen 200sccm, and adjusting pulsed bias is -100V, deposits CrN nitride metal
Object transition zone 20min；
Step 4: closing Cr target, opens two AlCrSi targets, electric current 90A, argon gas 50sccm, nitrogen 600sccm, temperature
Degree is heated to be 450 DEG C, and bias is first arranged, and from 80V to 200V, gradient increases, depositing Al CrSiN coating 90min；After be passed through oxygen
20sccm, from 200V to 80V, gradient declines bias, depositing Al CrSiON coating 90min.
Fig. 1 is the diffraction spectrogram of AlCrSiN and AlCrSiON double-layer nanometer composite coating manufactured in the present embodiment, by Fig. 1
It is found that the main phase of coating is fcc- (Al, Cr) N, preferred orientation concentrates on (200) diffraction maximum when 2 θ=43.7 °；2 θ=
Occurs the fcc-AlN phase along the growth of (111) crystal face at 37.5 °；It is dissolved phenomenon caused by 65 ° or so due to crystal grain refinement,
To " steamed bun peak " occur；Oxide phase is not detected in coating, this is because oxygen atom is solid-solution in (Al, Cr) N phase.
Fig. 2 and Fig. 3 is respectively the surface topography map and Cross Section Morphology of AlCrSiN and AlCrSiON double-layer nanometer composite coating
Figure, it can be seen that coating surface has some bulky grains and drop, this is because high temperature arc spot is unstable in AlCrSi target apparent motion
It is fixed, cause energy in target Dispersion on surface, cause the variation of plasma density, is deposited directly to painting in the particle of target surface evaporation
Layer surface, since particle is quickly cooled to matrix there are the temperature difference；By Cross Section Morphology figure it may be seen that coating
Without obvious structure feature, this is because crystal grain refinement, the amorphous phase in coating inhibits grain growth, increases grain boundary area,
Stop Grain Boundary Sliding and crack propagation, and coating toughness can be improved.
Embodiment two
The present embodiment is in the hard alloy on piece depositing coating mirror-finished, and specimen size is 25 × 25 × 2mm, examination
Sample is first respectively cleaned by ultrasonic 20 minutes in acetone and alcoholic solution respectively, is then dried up with high pure nitrogen, then face target is placed
In in vacuum chamber on sample frame.Filming equipment uses AIP-650 type arc ion plating machine, and cathode targets select pure metal Cr
(purity 99.9wt.%) and alloy AlCrSi (6:3:1), working gas select high-purity Ar and N2 (purity is 99.99%).
AlCrSiN and AlCrSiON double-layer nanometer composite coating the preparation method is as follows:
Step 1: the base vacuum of vacuum chamber is evacuated to 2 × 10-3Pa opens heating system for furnace body and is warming up to 400 DEG C；
It is passed through 400sccm argon gas, adjusts pulsed bias to -800V, operating pressure is maintained at 2 × 10-3Pa, aura clean 20min；
Step 2: then adjusting argon gas is 100sccm, opens Cr target, and arc ource electric current is adjusted to 90A, adjusts pulsed bias
Each Bombardment and cleaning 2min at -800V, -600V, -400V, -200V respectively；
Step 3: being passed through argon gas 50sccm, nitrogen 200sccm, and adjusting pulsed bias is -100V, deposits CrN nitride metal
Object transition zone 20min；
Step 4: closing Cr target, opens two AlCrSi targets, electric current 90A, argon gas 50sccm, nitrogen 600sccm, elder generation
Bias is arranged, and from 80V to 200V, gradient increases, depositing Al CrSiN coating 90min；After be passed through oxygen 20sccm, bias is from 200V
Decline to 80V gradient, depositing Al CrSiON coating 90min.
Fig. 4 is the compound scratch shape applied after scarification tests film-substrate cohesion of AlCrSiN and AlCrSiON double-layer nanometer
The critical load of looks, coating reachesAlCrSiN and AlCrSiON double-layer nanometer composite coating hardness is up toGpa。
As shown in figure 5, coating average friction coefficient is 0.68, and average wear rate passes through by frictional experiment and the detection to polishing scratch
Test is 1.79 × 10-3μm3/ N.mm has excellent wear-resisting property.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (2)
1. a kind of AlCrSiN and AlCrSiON double-layer nanometer composite coating, it is characterised in that: successively sink on hard alloy substrate
Product has CrN transition zone, AlCrSiN coating and AlCrSiON coating.
2. the preparation method of AlCrSiN and AlCrSiON double-layer nanometer composite coating described in claim 1, which is characterized in that
The following steps are included:
Step 1: the hard alloy to be coated after cleaning is placed in coating machine, and the base vacuum of vacuum chamber is evacuated to 2 × 10-3Pa opens heating system for furnace body and is warming up to 400 DEG C；It is passed through 400sccm argon gas, adjusts pulsed bias to -800V, aura is clear
Wash 20min；
Step 2: adjusting argon gas is 100sccm, opens Cr target, and arc ource electric current is adjusted to 90A, adjust pulsed bias respectively-
Each Bombardment and cleaning 2min under 800V, -600V, -400V, -200V；
Step 3: being passed through argon gas 50sccm, nitrogen 200sccm, and adjusting pulsed bias is -100V, deposits CrN metal nitride mistake
Cross a layer 20min；
Step 4: closing Cr target, open two AlCrSi targets, electric current 90A, argon gas 50sccm, nitrogen 600sccm, and temperature adds
Heat is 450 DEG C, and bias is first arranged, and from 80V to 200V, gradient increases, depositing Al CrSiN coating 90min；After be passed through oxygen
20sccm, from 200V to 80V, gradient declines bias, depositing Al CrSiON coating 90min.
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Cited By (6)
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| CN110079766A (en) * | 2019-05-27 | 2019-08-02 | 国宏工具系统（无锡）股份有限公司 | A kind of highly-efficient processing high temperature alloy nano-composite coating technique |
| CN111549322A (en) * | 2020-06-18 | 2020-08-18 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | AlCrTiSiN/AlCrTiSiON multilayer composite coating and preparation process thereof |
| CN111647856A (en) * | 2020-06-18 | 2020-09-11 | 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 AlCrTiSiN/AlCrTiSiON multilayer composite coating |
| CN113174562A (en) * | 2021-03-17 | 2021-07-27 | 广东工业大学 | Self-organized nanostructure oxynitride hard coating and preparation method and application thereof |
| CN114959575A (en) * | 2022-05-26 | 2022-08-30 | 安徽工业大学 | Insulating wear-resistant protective coating for thin film sensor, preparation method and application thereof |
| CN115505886A (en) * | 2022-09-23 | 2022-12-23 | 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 |
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| CN111647856A (en) * | 2020-06-18 | 2020-09-11 | 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 AlCrTiSiN/AlCrTiSiON multilayer composite coating |
| CN113174562A (en) * | 2021-03-17 | 2021-07-27 | 广东工业大学 | Self-organized nanostructure oxynitride hard coating and preparation method and application thereof |
| CN114959575A (en) * | 2022-05-26 | 2022-08-30 | 安徽工业大学 | Insulating wear-resistant protective coating for thin film sensor, preparation method and application thereof |
| CN114959575B (en) * | 2022-05-26 | 2024-01-02 | 安徽工业大学 | Insulating wear-resistant protective coating for film sensor, preparation method and application thereof |
| CN115505886A (en) * | 2022-09-23 | 2022-12-23 | 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 |
| 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 |
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