CN110079779A - A kind of high-performance ceramic coating and the preparation method and application thereof - Google Patents
A kind of high-performance ceramic coating and the preparation method and application thereof Download PDFInfo
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- CN110079779A CN110079779A CN201910298530.1A CN201910298530A CN110079779A CN 110079779 A CN110079779 A CN 110079779A CN 201910298530 A CN201910298530 A CN 201910298530A CN 110079779 A CN110079779 A CN 110079779A
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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
- C23C14/48—Ion implantation
-
- 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
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
-
- 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
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
-
- 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
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/586—Nitriding
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of high-performance ceramic coatings and the preparation method and application thereof, material poor controllability existing for traditional plating method of the preparation method mainly for ceramic coating, film substrate bond strength is low, is difficult to the problem of complicated workpiece surface forms uniform coating, proposes that seeping the complex technique combined with gas ion using metal ion implantation is prepared.Specifically includes the following steps: (1) pre-processes matrix, metal ion is then injected in matrix surface using metal ion implantation, forms metal coating；(2) metal coating surface infiltration N, C or O ion in step (1), high-performance ceramic coating described in in-situ preparation are seeped by gas ion.The bond strength of the ceramic coating and substrate that are prepared by the method is high, and coating composition is controllable, and substrate applicability is wide, and can be in complicated workpiece surface uniform deposition.
Description
Technical field
The present invention relates to field of material surface treatment, more particularly to a kind of high-performance ceramic coating and preparation method thereof with
Using.
Background technique
High performance ceramic coating adds high temperature inorganic material institute on the basis of keeping original matrix structure intensity
The good characteristics such as the high temperature resistant that has, wear-resistant, resistant to chemical etching, can solve existing for high-tech application material it is thermo-labile,
The problems such as perishable, not wear-resisting is one of current most potential new type high temperature material, obtains the wide of industry and academia
General concern.
Many kinds of, the preparation method multiplicity, comprising: hot spray process, sol-gel method, self propagating high temperature of ceramic coating
Synthetic method, electric spark deposition method, chemical vapour deposition technique and physical vaporous deposition etc..Wherein, physical vapor deposition (PVD)
It is under vacuum conditions, using low-voltage, the arc-discharge technique of high current, to evaporate target using gas discharge and make to be steamed
Hair substance and gas all ionize, and using the acceleration of electric field, make to be evaporated substance and its reaction product is deposited on workpiece
On technology, comprising: vacuum evaporation, sputter coating, ion plating.In recent years, it is combined by multiple technologies, PVD technique obtains
Biggish development, to derive a variety of advanced PVD techniques, such as: reaction magnetocontrol sputtering technology (RMS), pulse laser are heavy
Product (PLD), plasma molecular beam epitaxial growth technology (PA-MBE), magnetron sputtering pulse laser deposition (MSPLD), ionization
Magnetron sputtering (IMS), vacuum plasma spray coating (VPS) etc. prepare the new technology of ceramic coating.
However, the controllability of traditional coating technique depositing coating is poor, it is difficult to be formed uniformly in complicated workpiece surface
Ceramic coating.Further, since the elastic modulus difference of ceramic coating and substrate is big, film base binding performance is poor.Therefore, how to mention
The controllability of high material, enhances the bond strength of ceramic coating and substrate, and how to be coated with uniformly on complex part surface
Ceramic coating is particularly important, and provides good technical foundation for the preparation of high-performance ceramic coating.
Metal Ion Injection Technology is will to be evenly injected into intrinsic silicon by the energetic ion of electric field acceleration, and then make
Matrix surface performance is improved, and coating composition changes in gradient with depth, implanted layer and by between implanted layer without apparent
The anchoring strength of coating at interface, acquisition is high.Also, desire metallic cementation can be monometallic and can also be more metal or alloy, Neng Goujing
Really control implantation dosage and injection depth, have wide range of applications.The Metal Ion Injection Technology being concerned at present have MEVVA from
Component injection technique and double-layer glow ion penetration technology.Gas ion seeps technology by the way of glow discharge for N, C, O, CO2
Equal gas ionizations, the gas ion that ionization obtains are bombarded to workpiece surface at a high speed by electric field acceleration, generate cathodic sputtering effect
It answers, penetrates into diffusion into the surface and form permeation body sheath.If Metal Ion Injection Technology is seeped technology with gas ion to be used in combination
With regard to being able to solve the problem of ceramic coating binding performance difference.Metal Ion Injection Technology enable metal ion intrinsic silicon with
Change in depth distribution gradient, then technology is seeped by gas ion and realizes graded ceramics, obtain the ceramic coating of even compact.
Coating and matrix elastic modulus difference are small, and film base binding performance is good.
Summary of the invention
The object of the present invention is to provide a kind of high-performance ceramic coating and the preparation method and application thereof, this method mainly for
Material poor controllability existing for traditional plating method of ceramic coating, film substrate bond strength is low, is difficult in complicated workpiece surface
The problem of depositing homogeneous coatings, proposes that seeping the complex technique combined with gas ion using metal ion implantation is prepared.
To achieve the goals above, the invention adopts the following technical scheme.
A kind of preparation method of high-performance ceramic coating, comprising the following steps:
(1) matrix is pre-processed, bombardment is carried out to matrix surface using Ar ion or application voltage in vacuum environment
Except surface impurity；
(2) metal ion is uniformly injected into matrix surface using Metal Ion Injection Technology, forms metal coating；
(3) technology is seeped using gas ion, the ion of N, C or O is penetrated into metal coating, in-situ preparation has gradient-structure
Ceramic coating.
Further, in step (1), basis material is metal, ceramics, polymer.
Further, in step (2), metal ion be cerium ion, aluminium ion, titanium ion, chromium ion, vanadium ion, zinc from
Son, niobium ion, zirconium ion, molybdenum ion, palladium ion, tantalum ion, tungsten ion.
Further, in step (2), metal ion implantation uses MEVVA ion source injection technique.It is specifically that metal is true
The high desnity metal plasma that empty arc discharge generates is drawn by electrode, and the metal ion beam for being accelerated as carrying energy penetrates into
Matrix surface depths, to change the performance of substrate surface.The technology can control material composition well, can be injected identical
Different ions also can be injected in metal ion, form alloy.
Further, the injecting voltage of the MEVVA ion source is the kV of 10 kV ~ 200, implantation dosage 1015~1017
icon·cm-2, beam current density is 5 ~ 500 μ A/cm2, injection length is 1 ~ 180 min.
Further, in step (2), ion first uses glow discharge ionized gas during seeping, then carries out ion infiltration.Tool
Body is first by N2、O2、CO2Equal gas ionizations, the gas ion that ionization obtains are bombarded at a high speed to workpiece surface by electric field acceleration, are produced
Raw cathodic sputtering effect, the metal ion for penetrating into surface and injection generate ceramic coating.The coating close to growth in situ, ingredient with
Inject depth variation and distribution gradient, substrate and coating performance difference are smaller, bond strength height, good combination property.
Further, in the step (2), ion loads back bias voltage 100 to step (1) treated matrix during seeping
~ 500 V, and 200 ~ 600 DEG C are warming up to matrix.
Preferably, the injecting voltage of MEVVA ion source is 100kV, and the back bias voltage of load is 500V, and matrix is warming up to 500
℃。
The present invention also aims to disclose high-performance ceramic coating made from above-mentioned preparation method.
Further, the high-performance ceramic coating with a thickness of 50 nm ~ 10 μm.
The present invention also aims to disclose above-mentioned high-performance ceramic coating in cutter, energy storage tank or semiconductor devices
Application.
Due to using the technology described above, the beneficial effects of the present invention are: it is of the invention compared with traditional plated film mode
The preparation method of high-performance ceramic coating can form uniform ceramic coating in complicated workpiece surface, and treatment temperature is lower,
Basis material applicability is wide, can be prepared in metal, ceramics, polymer surfaces.It, can by using ion implanting means
Coating composition is controlled well, can adjust thicknesses of layers by controlling the implantation dosage of metal ion, as needed control gold
Belong to ion implanting depth, maximum value can achieve about 100 nm, and film-substrate cohesion is stronger, is not easy to peel off.It as needed both can be with
Identical metal ion is injected into substrate, and different metal ions also can be injected and form alloy.Skill is seeped by gas ion
Art realizes ceramic, can generate a variety of ceramic coatings such as oxide, nitride and carbide.Ceramic layer is with growth in situ
It is main, and gradient distribution is presented with the variation of case depth in the ingredient of coating.
Detailed description of the invention
Fig. 1 is high-performance ceramic coating preparation process schematic diagram of the invention；
Wherein, 1- matrix, 2- metal coating, 3- ceramic coating；
Fig. 2 is the XPS analysis result of high-performance ceria oxide ceramics coating prepared by the method for embodiment 1 in the present invention；
Fig. 3 is the afm image of high-performance ceria oxide ceramics coating prepared by the method for embodiment 1 in the present invention；
Wherein, before (a)-ion implanting, after (b)-ion implanting.
Specific embodiment
Below by specific embodiment, invention is further described in detail.Following embodiment only to the present invention carry out into
One step explanation, should not be construed as limiting the invention.
Embodiment 1
The present embodiment prepares CeO in matrix magnesium surface2Ceramic coating.Matrix 1 is cleaned with alcohol before experiment, is put after dry
Enter vacuum chamber using Ar ionic cleaning surface contamination.Coating preparation process is as shown in Figure 1.Firstly, MEVVA ion source uses
Metal vacuum arc discharge generates highdensity Ce ion, by Ce Ion Extraction and is accelerated as carrying energy by electrode extraction system
Ion beam, injecting voltage are 100 kV.Carry can ion beam by 1 surface of Ce ion implanting matrix, Ce elements in matrix 1 in gradient
Distribution forms metal coating 2.In injection process, vacuum chamber pressure 10-3Pa, Ce ion implantation dosage are 1016 icon·cm-2, beam current density is 250 μ A/cm2, injection length is 90 min.By controlling Ce ion implantation dosage, Implantation Energy and line
Density can accurately control the distribution of the concentration and depth of injection ion.Then ion oxidizing technology is used, glow discharge is passed through
Oxygen is ionized into high energy gas ion, -300 V of bias is loaded on matrix, and be warming up to 400 DEG C of diffusions for making oxonium ion
Ability enhancing more efficiently penetrates into intrinsic silicon and forms fine and close ceria oxide ceramics coating 3.It finally obtains with a thickness of 1 μm
CeO2Ceramic coating.During entirely seeping oxygen, high energy gas ion constantly bombards aluminising layer surface, so that surface is in
The state of activation is conducive to the further diffusion of oxygen.Fine and close cerium oxide is finally obtained, and coating is in material composition, knot
Structure, density and the variation that gradient is functionally presented, film base binding performance are good.
In order to more easily understand ion implanting and oxidation effectiveness, walked using XPS etching function to according to above-mentioned implementation
Suddenly the ceria oxide ceramics coating longitudinal direction ingredient prepared is analyzed, as a result as shown in Fig. 2, abscissa is that XPS etch period (indicates
Profile depth), ordinate indicates each element atomic percentage, and ingredient Ce and O divides in gradient in the coating as we can see from the figure
Cloth, O constituent content reduce with the increase of depth, and the trend of first increases and then decreases is presented in Ce constituent content, this is because
Ce ion is directly injected into intrinsic silicon, and the content on surface is relatively fewer.The afm images of sample surfaces is as shown in figure 3, can be with
Matrix surface is relatively rough (a in Fig. 3) before seeing injection, and matrix surface is smoothened (in Fig. 3 after injecting metal ion
B), it is smooth to illustrate that metal ion implantation can play the role of coating surface.
Embodiment 2
The preparation method of high-performance ceramic coating is applied to energy industry by the present embodiment, plates oxygenerating in hydrogen storage gas tank inner surface
Aluminized coating.
Hydrogen storage gas tank material generally uses steel (Q345R), however in the storing process of hydrogen, hydrogen atom readily diffuses into
In steel, hydrogen molecule is ultimately become, pressure is generated in material internal, stress is caused to concentrate.It, can be in steel if being more than the strength degree of steel
Inside generates tiny crackle, eventually leads to fracture, that is, Hydrogen Brittleness Phenomena.Al is coated in hydrogen storage gas tank inner surface2O3Ceramics apply
Layer can effectively prevent that Hydrogen Brittleness Phenomena occurs.Hydrogen needs certain energy to destroy aluminium and oxygen in the diffusion process of aluminum oxide coating layer
Associative key, and then play good hydrogen-evolution retardation.And Al2O3Ceramic coating itself has very high hardness, excellent wear-resisting
Property and chemical stability, can protect metallic matrix well.
Hydrogen storage gas tank cleans matrix 1 with alcohol before experiment as matrix 1 in the present embodiment, is put into after dry true
Empty room uses Ar ionic cleaning surface contamination.Coating preparation process is as shown in Figure 1.Firstly, MEVVA ion source uses metal
Vacuum arc discharge generates highdensity Al ion, by Al Ion Extraction and is accelerated as carrying the ion of energy by electrode extraction system
Beam, injecting voltage are 100 kV.Carry can ion beam by Al ion implanting hydrogen storage gas tank inner surface, aluminium element in matrix in gradient
Distribution forms metal coating 2.In injection process, vacuum chamber pressure 10-3Pa, Al ion implantation dosage are 1016 icon·cm-2, beam current density is 250 μ A/cm2, injection length is 90 min.By controlling Al ion implantation dosage, Implantation Energy and line
Density can accurately control the distribution of the concentration and depth of injection ion.Then ion oxidizing technology is used, glow discharge is passed through
Oxygen is ionized into high energy gas ion, -300 V of bias is loaded on hydrogen storage gas tank, and be warming up to 400 DEG C to make oxonium ion
Diffusivity enhancing more efficiently penetrates into intrinsic silicon and forms fine and close alumina ceramic coating 3.Finally obtain with a thickness of
1 μm of Al2O3Ceramic coating.During entirely seeping oxygen, high energy gas ion constantly bombards aluminising layer surface, so that surface
State in activation is conducive to the further diffusion of oxygen.Fine and close aluminum oxide coating layer is finally obtained, and coating is in material group
At, structure, density and functionally the variation of gradient is presented, film base binding performance is good.
Embodiment 3
The preparation method of high-performance ceramic coating is applied to semiconductor field by the present embodiment, is coated with AlN on invar alloy surface
Coating.
AlN has high breakdown field strength, high heat conductance, high resistivity, high chemistry and high thermal stability, is good semiconductor
Material.The example method is similar to Example 1, first injects Al ion on invar alloy surface using MEVVA technology of ion source, then
The matrix surface of technology after treatment is seeped using ion and penetrates into N element, 10 μm of in-situ preparation of the AlN pottery with gradient-structure
Porcelain coating.In injection process, vacuum chamber pressure 10-3 Pa, MEVVA ion source injecting voltage are 200 kV, Al ion implanting agent
Amount is 1017 icon·cm-2, beam current density is 500 μ A/cm2, injection length is 180 min.Ion adds matrix during seeping
- 500 V of bias is carried, and is warming up to 600 DEG C.
Embodiment 4
The present embodiment prepares the Al of 100 nm on the surface steel Q345R2O3Ceramic coating.In injection process, the injection of MEVVA ion source
Voltage is 10 kV, and Al ion implantation dosage is 1015 icon·cm-2, beam current density is 5 μ A/cm2, injection length is 1 min.
Ion loads -100 V of bias to matrix during seeping, and is warming up to 200 DEG C.Other experiment parameters and preparation process with reality
It is identical to apply example 1.
The above content is specific embodiment is combined, further detailed description of the invention, and it cannot be said that this hair
Bright specific implementation is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, it is not taking off
Under the premise of from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to protection of the invention
Range.
Claims (10)
1. a kind of preparation method of high-performance ceramic coating, which comprises the following steps:
(1) matrix (1) is pre-processed, metal ion is then injected on matrix (1) surface using metal ion implantation, is formed
Metal coating (2)；
(2) it is seeped by gas ion and penetrates into N, C or O ion, height described in in-situ preparation in metal coating (2) surface of step (1)
Performance ceramic coating (3).
2. the preparation method of high-performance ceramic coating according to claim 1, which is characterized in that pre- in the step (1)
Processing is to carry out bombardment removal surface impurity to matrix surface using Ar ion or application voltage in vacuum environment.
3. the preparation method of high-performance ceramic coating according to claim 1, it is characterised in that: in the step (1) from
Son injection is injected using MEVVA ion source.
4. the preparation method of high-performance ceramic coating according to claim 3, which is characterized in that the MEVVA ion source
Injecting voltage is the kV of 10 kV ~ 200, implantation dosage 1015~1017 icon·cm-2, beam current density is 5 ~ 500 μ A/cm2, note
The angle of incidence is 1 ~ 180 min.
5. the preparation method of high-performance ceramic coating according to claim 1, which is characterized in that golden in the step (1)
Category ion be cerium ion, aluminium ion, titanium ion, chromium ion, vanadium ion, zinc ion, niobium ion, zirconium ion, molybdenum ion, palladium from
Son, tantalum ion or tungsten ion；The material of matrix is metal, ceramics or polymer in the step (1).
6. the preparation method of high-performance ceramic coating according to claim 1, which is characterized in that in the step (2), first
By glow discharge ionized gas, then carry out ion infiltration.
7. the preparation method of high-performance ceramic coating according to claim 1, which is characterized in that in the step (2), from
Son loads 100 ~ 500 V of back bias voltage to step (1) treated matrix during seeping, and is warming up to 200 ~ 600 DEG C to matrix.
8. high-performance ceramic coating made from any one of the claim 1-7 preparation method.
9. high-performance ceramic coating according to claim 8, which is characterized in that the high-performance ceramic coating with a thickness of 50
nm~10 μm。
10. application of the high-performance ceramic coating of claim 8 or 9 in cutter, energy storage tank or semiconductor devices.
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| CN110608457A (en) * | 2019-09-29 | 2019-12-24 | 杭州老板电器股份有限公司 | Pot rack and manufacturing method thereof |
| CN113811106A (en) * | 2020-06-11 | 2021-12-17 | 维达力实业（赤壁）有限公司 | Preparation method of shell, shell and application |
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| CN110608457A (en) * | 2019-09-29 | 2019-12-24 | 杭州老板电器股份有限公司 | Pot rack and manufacturing method thereof |
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| CN113811106B (en) * | 2020-06-11 | 2023-06-27 | 维达力科技股份有限公司 | Shell preparation method, shell and application |
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