CN110512250A - Anode oxide film and preparation method thereof - Google Patents
Anode oxide film and preparation method thereof Download PDFInfo
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- CN110512250A CN110512250A CN201810491328.6A CN201810491328A CN110512250A CN 110512250 A CN110512250 A CN 110512250A CN 201810491328 A CN201810491328 A CN 201810491328A CN 110512250 A CN110512250 A CN 110512250A
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- Prior art keywords
- oxide film
- metal
- anode oxide
- alloying
- metal oxide
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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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The present invention provides a kind of anode oxide film, it is formed on the surface of a metallic matrix, the anode oxide film has multiple micropores, the anode oxide film includes the first metal oxide and the second metal oxide, second metal oxide is uniformly distributed in first metal oxide, and first metal oxide is different with the refractive index of second metal oxide.Present invention simultaneously provides a kind of production methods of anode oxide film.The diffusing reflection rate of above-mentioned anode oxide film is higher, can visually be rendered as white appearance, above-mentioned production method production is simple and efficiency is higher.
Description
Technical field
The present invention relates to anodization, especially a kind of anode oxide film and preparation method thereof.
Background technique
Metal product generally will do it anodized such as aluminium/aluminium alloy, magnesium/magnesium alloy or titanium/titanium alloy, with
Its surface forms corrosion resistance and the preferable anode oxide film of wearability.To keep product surface color diversified, after anodic oxidation
Dyeing processing or spray treatment can be carried out to product.In some cases, some products may require that form the anodic oxidation of white
Film.However, meeting in the preferable white oxide film of the usually more difficult formation texture of existing anodic oxidation colouring method or production method
Highly toxic chemical agent is used, processing procedure is not environmentally.
Summary of the invention
In view of the above situation, it is necessary to a kind of anode oxide film is provided, to solve the above problems.
In view of the above situation, there is a need to provide a kind of production method of anode oxide film, to solve the above problems.
A kind of anode oxide film is formed on the surface of a metallic matrix, and the anode oxide film has multiple micropores, institute
Stating anode oxide film includes the first metal oxide and the second metal oxide, and second metal oxide is uniformly distributed in institute
It states in the first metal oxide, and first metal oxide is different with the refractive index of second metal oxide.
A kind of production method of anode oxide film a, comprising the following steps: metallic matrix is provided；In the metallic matrix
Physical vapour deposition (PVD) is carried out on surface, to form an alloying intermediate deposit, the alloying intermediate deposit includes the first metal
And it is uniformly distributed in the second metal in first metal；Anodized is carried out to the alloying intermediate deposit, with
The anode oxide film with multiple micropores is formed, the anode oxide film includes the first metal oxide and is uniformly distributed in described
The second metal oxide in first metal oxide；The anode oxide film is polished.
In above-mentioned anode oxide film, second metal oxide is uniformly distributed in first metal oxide, and
Second metal oxide is different from the refractive index of the first metal oxide, and therefore, the anode oxide film is with higher
Diffusing reflection rate.When the nearly all visible wavelength for the incident light being incident on anode oxide film is diffusely reflected, the anodic oxygen
Change film and be visually presented as white or linen appearance, visual texture is preferable.
The production method of above-mentioned anode oxide film includes the steps that physical vapour deposition (PVD) and anodic oxidation, and production is simple and imitates
Rate is higher.In addition, above-mentioned production method is without the use of excessive chemical agent, it is more environmentally friendly.
Detailed description of the invention
Fig. 1 is the metallic matrix of embodiment provided by the present invention and the diagrammatic cross-section of anode oxide film.
Fig. 2 is the metallic matrix of embodiment provided by the present invention and the diagrammatic cross-section of alloying intermediate deposit.
Fig. 3 is the flow chart of the production method of the anode oxide film of embodiment provided by the present invention.
Main element symbol description
| Anode oxide film | 10 |
| First metal oxide | 11 |
| Second metal oxide | 12 |
| Micropore | 101 |
| Metallic matrix | 20 |
| Alloying intermediate deposit | 30 |
The present invention that the following detailed description will be further explained with reference to the above drawings.
Specific embodiment
To better understand the objects, features and advantages of the present invention, with reference to the accompanying drawing and specific real
Applying mode, the present invention will be described in detail.It should be noted that in the absence of conflict, presently filed embodiment and reality
The feature applied in mode can be combined with each other.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, described embodiment
It is only some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this field is general
Logical technical staff all other embodiment obtained without making creative work, belongs to protection of the present invention
Range.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that the limitation present invention.
Term " and or " used herein includes any and all groups of one or more relevant listed items
It closes.
Referring to Fig. 1, the embodiment of the present invention provides a kind of anode oxide film 10, it is formed in the table of a metallic matrix 20
On face, there are multiple micropores 101 on the anode oxide film 10, the anode oxide film 10 includes 11 He of the first metal oxide
Second metal oxide 12, second metal oxide 12 are uniformly distributed in first metal oxide 11, and described
First metal oxide 11 is different with the refractive index of second metal oxide 12.The anode oxide film 10 with a thickness of 1
~15 microns (um), the aperture of the micropore 101 is 10~200 nanometers (nm).
The metallic matrix 20 can be aluminium, aluminium alloy, magnesium, magnesium alloy, titanium or titanium alloy etc..
First metal is aluminum metal, and second metal is selected from as one of metals such as titanium, magnesium, zirconium, barium.It is described
The weight ratio of first metal oxide 11 is greater than 80% and less than 100%, and the weight ratio of second metal oxide 12 is greater than 0
And less than 20%.
In the anode oxide film, the refractive index of first metal oxide 11 and second metal oxide 12 is not
Together, and second metal oxide 12 is uniformly distributed in first metal oxide 11, thus anode oxide film 10
Diffusing reflection rate is higher.Therefore, the nearly all visible wavelength for the incident light being incident on anode oxide film 10 can be diffusely reflected,
To which anode oxide film 10 can visually be rendered as white or linen appearance.
Referring to Fig. 1 to Fig. 3, the production method of the anode oxide film 10 of the embodiment of the present invention includes following step
It is rapid:
Step S110 provides a metallic matrix 20.
The metallic matrix 20 can be aluminium alloy, and the metallic matrix 20 can pass through the modes such as die cast or machining
It is made.It is appreciated that metallic matrix 20 can also be aluminium, magnesium, magnesium alloy, titanium or titanium alloy.
Step S120 carries out physical vapour deposition (PVD) on the surface of metallic matrix 20, to form an alloying intermediate deposit
30。
Specifically, degreasing degreasing processing first is carried out to the metallic matrix 20, so that the surface of the metallic matrix 20 is clear
It is clean.In the present embodiment, the technique of the degreasing degreasing processing are as follows: using commercially available inorganic non-metallic degreasing agent or common neutrality
After cleaning agent is configured to aqueous solution, metallic matrix 20 is put into and wherein impregnates or carries out ultrasonic cleaning, then to cleaning
Metallic matrix 20 afterwards is washed and is dried.
Then, to degreasing degreasing, treated that metallic matrix 20 carries out is plasma-activated.In the present embodiment, inertia is utilized
The plasma source of gas ionization carries out surface cleaning and activation to degreasing degreasing treated metallic matrix 20.
Then, the first metal and the second metal are ionized, and in institute in regulatable electric field and magnetic field environment
State it is plasma-activated after metallic matrix 20 on form fine and close alloying intermediate deposit 30.The alloying intermediate deposit 30
Including the first metal and the second metal being uniformly distributed in first metal.The alloying intermediate deposit 30 with a thickness of
5~20um.In the present embodiment, using in the spraying of electron evaporation, thermal resistance evaporation, induction evaporation mode, arc evaporation and cathode
At least one mode the first metal and the second metal are ionized.
First metal is aluminum metal, and second metal is selected from as one of metals such as titanium, magnesium, zirconium, barium.In shape
At the alloying intermediate deposit 30 in, the weight ratio of first metal is greater than 80% and less than 100%, second gold medal
The weight ratio of category is greater than 0 and less than 20%.The second metal even dispersion is in the first metal.
In the present embodiment, using arc process or sputtering method it is described it is plasma-activated after metallic matrix 20 on formed and cause
Close alloying intermediate deposit 30.The specific process parameter of above-mentioned arc process is as follows: target source current 50A~120A, bias
60V~150V, argon gas flow velocity 20SCCM~100SCCM, vacuum pressure 0.1Pa~0.3Pa in furnace, 30~300 points of plated film time
Clock；The specific process parameter of above-mentioned sputtering method is as follows: power 5kW~10kW, bias 60V~150V, argon gas flow velocity
20SCCM~100SCCM, vacuum pressure 0.1Pa~0.3Pa in furnace, plated film time 30~300 minutes.
When making alloying intermediate deposit 30, it can be used while including first metal and the bimetallic list
Branch target, by adjusting the first metal described in single branch target and the bimetallic relative scale, to adjust in alloying
Between component ratio in coating 30.Alternatively, it is separate targets that first metal and second metal, which is respectively adopted, pass through tune
The freeization parameter of whole two separate targets, to adjust the component ratio in alloying intermediate deposit 30.
Step S130 carries out anodized to alloying intermediate deposit 30, to form the sun with multiple micropores 101
Pole oxidation film 10.
Specifically, firstly, degreasing degreasing processing is carried out to the metallic matrix 20 with alloying intermediate deposit 30, so that institute
State the surface cleaning of alloying intermediate deposit 30.In present embodiment, the technique of above-mentioned degreasing degreasing processing are as follows: match cleaning agent
After being set to aqueous solution, then the metallic matrix 20 with alloying intermediate deposit 30 is put into and is wherein impregnated 5~15 minutes.Degreasing removes
The metallic matrix 20 with the alloying intermediate deposit 30 is washed and dried after oil processing.Above-mentioned cleaning agent is can
Remove the alkaline cleaner of grease.
Then, anodized is carried out to degreasing degreasing treated alloying intermediate deposit 30.Specifically, the sun
Pole oxidation processes are that have the metallic matrix 20 of alloying intermediate deposit 30 as anode, and in temperature using graphite plate as cathode
Degree passes through anodic oxidation to carry out anodized to the surface of alloying intermediate deposit 30 in 20 DEG C~40 DEG C of electrolyte
Field-enhanced dissolution has the anode oxide film 10 of multiple micropores 101, the multiple 101 ordered arrangement of micropore far from being formed.The sun
Pole oxidation film 10 with a thickness of 1~15um, the aperture of the micropore 101 is 10~200nm.
The electrolyte includes acid reagent and water.The acid reagent is selected from sulfuric acid, oxalic acid, phosphoric acid, citric acid, winestone
Sour is one or more.The volume fraction of the acid reagent in the electrolytic solution is 2%~20%.The anodized
Voltage is 8V~30V, and the processing time is 40~60 minutes.
It is formed, the anode oxide film 10 since anode oxide film 10 carries out anodic oxidation by alloying intermediate deposit 30
It simultaneously include the first metal oxide 11 and the second metal oxide 12, second metal oxide 12 is uniformly distributed in first
In metal oxide 11.The weight ratio of first metal oxide 11 is greater than 80% and less than 100%, second metal oxygen
The weight ratio of compound 12 is greater than 0 and less than 20%.
After anodic oxidation, anode oxide film 10 is carried out to ultrasonic washing in clean water at room temperature, to remove anodic oxygen
Change electrolyte remaining in film 10.
Step S140 polishes anode oxide film 10.
Due to foring surface dissolving layer (not shown) on the surface of anode oxide film 10 in anode oxidation process, therefore,
Carrying out polishing to anode oxide film 10 can remove the surface dissolving layer, to obtain the smooth anode oxide film 10 in surface.Institute
Stating polishing method can be mechanical polishing or chemical polishing.
It is appreciated that in other embodiments, step S140 can cancel.
It is appreciated that after step s 140, also sealing pores can be carried out to anode oxide film 10, to enhance anodic oxidation
The wearability of film 10.
Above-mentioned anode oxide film 10 includes the first metal oxide 11 and the second metal oxide 12, second gold medal simultaneously
Belong to oxide 12 to be uniformly distributed in the first metal oxide 11, and second metal oxide 12 and the first metal oxide
11 refractive index is different, therefore, the anode oxide film 10 diffusing reflection rate with higher.When being incident on anode oxide film
When nearly all visible wavelength of incident light is diffusely reflected, anode oxide film is visually presented as white or linen outer
It sees, visual texture is preferable.
The production method of above-mentioned anode oxide film 10 includes the steps that physical vapour deposition (PVD) and anodic oxidation, production it is simple and
Efficiency is higher.Above-mentioned production method is without the use of excessive chemical agent, more environmentally friendly.It is made by above-mentioned production method white
The anode oxide film 10 of color, without the use of traditional organic molecule dyestuff, it is old that light fading etc. occurs in avoidable anode oxide film
Change phenomenon.
In addition, above-mentioned production method is suitable for the substrate of various metals material, the scope of application is wider.Also, passing through object
When physical vapor deposition legal system makees alloying intermediate deposit 30, the composition ratio of above-mentioned alloying intermediate deposit 30 can be freely adjusted.
Finally it should be noted that embodiment of above is only used to illustrate the technical scheme of the present invention and not to limit it, although ginseng
It is described the invention in detail according to better embodiment, those skilled in the art should understand that, it can be to this hair
Bright technical solution is modified or equivalent replacement, without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. a kind of anode oxide film is formed on the surface of a metallic matrix, it is characterised in that: the anode oxide film has more
A micropore, the anode oxide film include the first metal oxide and the second metal oxide, and second metal oxide is equal
It is even to be distributed in first metal oxide, and the refractive index of first metal oxide and second metal oxide
It is different.
2. anode oxide film as described in claim 1, it is characterised in that: first metal is aluminum metal, second gold medal
Belong to selected from being one of titanium, magnesium, zirconium, barium, the weight ratio of first metal oxide is greater than 80% and less than 100%, institute
The weight ratio for stating the second metal oxide is greater than 0 and less than 20%.
3. anode oxide film as described in claim 1, it is characterised in that: the anode oxide film with a thickness of 1~15 micron,
The aperture of the micropore is 10~200 nanometers.
4. a kind of production method of anode oxide film, comprising the following steps:
One metallic matrix is provided；
Physical vapour deposition (PVD) is carried out, on the surface of the metallic matrix to form an alloying intermediate deposit, the alloying
Intermediate deposit includes the first metal and the second metal for being uniformly distributed in first metal；
Anodized is carried out to the alloying intermediate deposit, it is described to form the anode oxide film with multiple micropores
Anode oxide film includes the first metal oxide and the second metal oxide for being uniformly distributed in first metal oxide.
5. the production method of anode oxide film as claimed in claim 4, it is characterised in that: first metal is aluminium, described
Second metal be selected from be one of titanium, magnesium, zirconium, barium, the alloying intermediate deposit with a thickness of 5~20 microns, described
In alloying intermediate deposit, the weight ratio of first metal is greater than 80% and less than 100%, the bimetallic weight ratio
Greater than 0 and less than 20%.
6. the production method of anode oxide film as claimed in claim 5, it is characterised in that: the anode oxide film with a thickness of
1~15 micron, the aperture of the micropore is 10~200 nanometers, and the weight ratio of first metal oxide is greater than 80% and small
In 100%, the weight ratio of second metal oxide is greater than 0 and less than 20%.
7. the production method of anode oxide film as claimed in claim 5, it is characterised in that: form the alloying intermediate deposit
The step of specifically include:
Degreasing degreasing processing is carried out to the metallic matrix；
To degreasing degreasing, treated that the metallic matrix carries out is plasma-activated；
First metal and second metal are ionized, and regulatable electric field in magnetic field environment described
The fine and close alloying intermediate deposit is formed on the metallic matrix after plasma-activated.
8. the production method of anode oxide film as claimed in claim 7, it is characterised in that: living in plasma using arc process
The alloying intermediate deposit is formed on the metallic matrix after change, the specific process parameter of the arc process is as follows: target
Source current 50A~120A, bias 60V~150V, argon gas flow velocity 20SCCM~100SCCM, vacuum pressure 0.1Pa in furnace~
0.3Pa, plated film time 30~300 minutes.
9. the production method of anode oxide film as claimed in claim 7, it is characterised in that: using sputtering method in the plasma
The alloying intermediate deposit is formed on metallic matrix after body activation, the specific process parameter of the sputtering method is as follows: power supply
Power 5kW~10kW, bias 60V~150V, argon gas flow velocity 20SCCM~100SCCM, vacuum pressure 0.1Pa~0.3Pa in furnace,
Plated film time 30~300 minutes.
10. the production method of anode oxide film as claimed in claim 5, it is characterised in that: the anodization step is specific
Include:
Using graphite plate as cathode, the metallic matrix with the alloying intermediate deposit is 20 in temperature as anode
DEG C~40 DEG C of electrolyte in anodized, the anodized are carried out to the surface of the alloying intermediate deposit
Voltage be 8V~30V, processing the time be 40~60 minutes.
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| CN201810491328.6A CN110512250A (en) | 2018-05-21 | 2018-05-21 | Anode oxide film and preparation method thereof |
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| CN201810491328.6A CN110512250A (en) | 2018-05-21 | 2018-05-21 | Anode oxide film and preparation method thereof |
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| CN110512250A true CN110512250A (en) | 2019-11-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113529149A (en) * | 2020-04-22 | 2021-10-22 | 北京小米移动软件有限公司 | Shell manufacturing method, shell and electronic equipment |
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| CN1739062A (en) * | 2003-05-31 | 2006-02-22 | 崔海龙 | Surface reflection type metallic screen and method of manufacturing the same |
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Application publication date: 20191129 |