CN107904556A - One kind prepares patterning function film method based on templated deposition - Google Patents
One kind prepares patterning function film method based on templated deposition Download PDFInfo
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- CN107904556A CN107904556A CN201710991617.8A CN201710991617A CN107904556A CN 107904556 A CN107904556 A CN 107904556A CN 201710991617 A CN201710991617 A CN 201710991617A CN 107904556 A CN107904556 A CN 107904556A
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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
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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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
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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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
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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
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
Patterning function film method is prepared based on templated deposition the present invention relates to one kind, it is that film made from existing congenic method is more difficult to realize that oil storage lubricates in surface crater for solving, wear resistant friction reducing is poor, and specific surface area is smaller, it is relatively difficult to achieve to visible ray selective absorbing and reflection so that degradation efficiency and the poor technical problem of light absorption utilization ratio and design.Technical points are as follows：The surface nano-structure with nano-tube array structure is prepared in the metal surface such as titanium and aluminium using anodizing technology first, then nano surface pipe structure is removed using chemically or mechanically method, patterned template structure is left in metal base surface；Physical gas phase deposition technology is recycled to prepare function film in metal pattern surface deposition.The function film that deposition is made in the above method also has patterning pattern, on the one hand can improve the combination power of film and matrix, on the other hand can increase the specific surface area of film, is conducive to play the functions such as the photocatalysis of film.
Description
Technical field
It is more particularly to a kind of that patterning function film side is prepared based on templated deposition the present invention relates to a kind of function film
Method.
Background technology
Film is a kind of thin and flexible transparent sheet, is made of plastics, adhesive, rubber or other materials, scientific
Explanation is：By atom, two-dimensional material that molecule or ion deposition are formed in substrate surface.Function film is that one kind has, and is being rubbed
The field extensive use such as scouring damage, photocatalysis, photovoltaic, some of function films are titanium deoxid film.Titanium dioxide due to
Its high index of refraction and relatively solid property, this high-index material are used for visible ray and near infrared range, almost each
TiO2Steam and follow a principle：Negligible absorbability is obtained in workable spectral regions, can so reduce oxygen
The limitation of pressure and temperature and the limitation for steaming speed；Titanium deoxid film needs to help plating using IAD, and oxygen input port is being kept off
Below plate.Some existing films have the function of to pattern, the application number 201010206997.8 as disclosed in Chinese patent literature,
Data of publication of application 2010.11.24, denomination of invention " have titanium deoxid film of nanoscale patterns and preparation method thereof "；Such as
The application number 200410100812.X disclosed in Chinese patent literature, publication date June 14 in 2006, denomination of invention " patterning two
The preparation method of titanium oxide micro-structure "；Application number 201611093131.4 as disclosed in Chinese patent literature, data of publication of application
2017.05.31, denomination of invention " a kind of side for the titanium dioxide pattern that noresidue layer is prepared using room temperature transfer stamping technique
Method ".But above-mentioned patterned film and similar product are less using metallic matrix preparation, especially with nano-tube array structure system
It is standby, it is also less to can apply to surface oil storage, and photocatalysis, photovoltaic art.
The content of the invention
To overcome above-mentioned deficiency, the purpose of the present invention is provide a kind of prepare based on templated deposition to this area to pattern work(
Energy film process, solving it, film made from existing congenic method is more difficult to realize that oil storage lubricates in surface crater, wear resistant friction reducing
Property it is poor, and specific surface area is smaller, it is more difficult to realizes to visible ray selective absorbing and reflection, so that degradation efficiency and light are inhaled
Receive the poor technical problem of utilization ratio.The purpose is to what is be achieved through the following technical solutions.
One kind prepares patterning function film method based on templated deposition, and this method is using anodizing technology processing structure
Patterned template structure, then prepares function film in template surface using physical gas-phase deposite method deposition.Its main points is this
Method comprises the following steps：（1）Nano-tube array structure is prepared in metal base surface using anodizing technology, nanotube
Average length is 1 μm -50 μm, and the average diameter of nanotube is 20-150nm, and metallic matrix includes pure titanium, titanium alloy, fine aluminium, aluminium
Alloy, or its combination.（2）The nanometer of removal or the formation of mechanical oscillation method stripping metal matrix surface is dissolved using chemical solvent
Pipe structure, patterned formwork structure is constructed in metal base surface.（3）The metallic matrix that surface is formed to template is sent into vacuum
Room, vacuum chamber carry out forvacuum, and back end vacuum is less than 3 ' 10-3Pa, and vacuum chamber is heated as needed.（4）The back of the body
After bottom vacuum and heating-up temperature reach requirement, sputter clean target 2-3min, ion sputtering etch cleaner sample 1-2min to be plated.
Etching bias used is 900-1200V, and sample is etched more than three times, the gradually increase from low to high of etching bias, and each bias is carved
Lose time 2-3min.Target used is single target or more targets, and target material surface needs to be blocked with liner plate during sputter clean target, described to splash
Penetrate cleaning target and use inert gas argon gas.（5）Using physical gas phase deposition technology in the Metal Substrate body surface with formwork structure
Face deposition prepares TiO2, AlN, TiN, TiAlN, CrN, CrAlN, ZnO function film.Physical gas phase deposition technology used includes steaming
Plating, magnetron sputtering and multi-arc ion coating.
Electrolyte solution used in step 1 Anodic Oxidation is the electrolyte aqueous solution containing fluorine ion, with the gold
Category base material is anode, anodized is carried out to the metal base, so that at least one main table of the metal base
Generation has nano-tube array structure on face.The electrolyte aqueous solution containing fluorine ion includes fluoride selected from the group below：
Ammonium fluoride, potassium fluoride, sodium fluoride, or its combination；The electrolyte aqueous solution containing fluorine ion includes addition selected from the group below
Agent：Deionized water, glycerine, ethylene glycol, methanol, or its combination.
Present invention production preparation facilitates feasible, and film surface pit oil storage lubrication is convenient, and wear resistant friction reducing effect is good, compares surface
Product increase, degradation efficiency and light absorption utilization ratio are good；Its particularly suitable as photocatalytic degradation and photoelectric conversion requirement compared with
High fretting wear, photocatalysis, the film of photovoltaic art use.
Brief description of the drawings
Fig. 1 is that the present invention prepares patterning function film method schematic diagram based on anodic oxidation templated deposition.
Fig. 2 is that anodic oxidation Titanium base of the present invention forms nano-tube array stripping rear surface formation patterned surface pattern
Figure.
Fig. 3 is patterned surface pattern deposition 100nm thickness N dopings TiO of the present invention2Shape appearance figure after film.
Fig. 4 is present invention patterning N doping TiO2The abosrption spectrogram of film.
Embodiment
In conjunction with attached drawing, structure of the present invention and use are further described.As Figure 1-Figure 4, the implementation of this method
Example step is as follows：（1）Surface preparation is carried out to pure titanium metal base material, first cleans 2- in 5-20wt.% sodium hydrate aqueous solutions
10min, alkali wash water temperature are 40-150 DEG C.After being cleaned with clear water, 2~10min of cleaning in pickle is put into, pickle proportioning is
Hydrofluoric acid（10ml）：Nitric acid（40ml）：Deionized water（300ml）.Pure titanium metal base material after pickling is then in acetone soln
Ultrasonic cleaning, air-dries after taking-up.（2）It is configured to the electrolysis of fluorides liquid of electrochemical anodic oxidation, NH in electrolyte4F contains
It is 2wt.% to measure as 0.25wt.%, deionized water content, remaining composition is ethylene glycol.（3）Shake in electrolyte aqueous solution to pure titanium
Dynamic diaphragm carries out anodized, and it is graphite electrode to electrode that anodized is used, electrolyte temperature in oxidizing process
For 20 DEG C, anodic oxidation voltage 60V, oxidization time 60min.（4）Can be the nanotube oxide of formation by mechanical oscillation
Peel off, the bowl-shape nano-tube array template of class is formed on matrix, as shown in Figure 2.（5）Surface is formed to the metallic matrix of template
Vacuum chamber is sent into, vacuum chamber carries out forvacuum, and back end vacuum is less than 3 ' 10-3Pa.（6）The pure titanium target material 2- of sputter clean
3min, argon ion sputtering etch cleaner template sample 1-2min to be plated.（7）Using magnetron sputtering technique with formwork structure
Metal base surface deposition prepares the TiO of N doping2Function film.
Sample surface morphology after above-described embodiment deposition film, as shown in figure 3, film has obvious template characteristic shape
Looks, function film prepared by absorption spectrum test display have high absworption peak in visible light wave range, which can be efficiently
Photocatalytic degradation and photoelectric conversion are carried out using visible ray.
In conclusion this method builds patterned template structure using anodizing technology processing, then in template surface
Function film is prepared using physical gas-phase deposite method deposition.Patterned film made from this method has in fretting wear, light
The fields such as catalysis, photovoltaic are with a wide range of applications；Meanwhile such as the pit of film surface realizes storage in fretting wear application
Oil lubrication acts on, and significantly improves the wear resistant friction reducing effect of film.In photocatalysis and photovoltaic art, pattern structure increases film
Specific surface area, realizes the absorption and use efficiency of the degradation efficiency and light that to visible ray selective absorbing and reflection, improve film.
Claims (10)
1. one kind prepares patterning function film method based on templated deposition, this method is using anodizing technology processing structure figure
Case formwork structure, then prepares function film in template surface using physical gas-phase deposite method deposition；It is characterized in that：Should
Method comprises the following steps：
（1）Nano-tube array structure is prepared in metal base surface using anodizing technology；
（2）The nano-tube array formed using chemically or mechanically method stripping metal matrix surface, is formed in metal base surface
Patterned formwork structure；
（3）The metallic matrix that surface is formed to template is sent into vacuum chamber, and vacuum chamber carries out forvacuum, and back end vacuum is less than 3 '
10-3Pa, and vacuum chamber is heated as needed；
（4）After back end vacuum and heating-up temperature reach requirement, sputter clean target 2-3min, ion sputtering etch cleaner sample to be plated
Product 1-2min；
（5）Function film is prepared in the metal base surface deposition with formwork structure using physical gas phase deposition technology.
2. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
Metallic matrix includes pure titanium, titanium alloy, fine aluminium, aluminium alloy, or its combination in rapid 1.
3. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
Electrolyte solution used in rapid 1 Anodic Oxidation is the electrolyte aqueous solution containing fluorine ion, right using the metal base as anode
The metal base carries out anodized, so that generation has nanometer at least one main surface of the metal base
Pipe array structure.
4. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
Electrolyte aqueous solution containing fluorine ion described in rapid 1 includes fluoride selected from the group below：Ammonium fluoride, potassium fluoride, sodium fluoride, or
It is combined；The electrolyte aqueous solution containing fluorine ion includes additive selected from the group below：Deionized water, glycerine, second two
Alcohol, methanol, or its combination.
5. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
The average length of nanotube described in rapid 1 is 1 μm -50 μm；The average diameter of the nanotube is 20-150nm.
6. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
The chemically or mechanically method of stripping nano pipe array structure includes chemical solvent dissolving removal or the stripping of mechanical oscillation method in rapid 2
From.
7. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
It is 900-1200V that bias used is etched in rapid 4, and sample is etched more than three times, the gradually increase from low to high of etching bias, each partially
Press etch period 2-3min.
8. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
Target used is single target or more targets in rapid 4, and target material surface needs to be blocked with liner plate during sputter clean target, the sputter clean target
Material uses inert gas argon gas.
9. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
Physical gas phase deposition technology used includes evaporation, magnetron sputtering and multi-arc ion coating in rapid 5.
10. according to claim 1 prepare patterning function film method based on templated deposition, it is characterised in that the step
Function film used includes TiO in rapid 52、AlN、TiN、TiAlN、CrN、CrAlN、ZnO。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110318080A (en) * | 2019-08-02 | 2019-10-11 | 吉林大学 | Form-material cooperates with bionical Anti-erosion function surface structure and preparation method thereof |
| CN112030118A (en) * | 2020-07-31 | 2020-12-04 | 中国原子能科学研究院 | Preparation method of deuterated polyethylene nanowire array target |
| CN113122846A (en) * | 2021-04-03 | 2021-07-16 | 郑小宝 | Aluminum alloy metal plated part |
| CN113122845A (en) * | 2021-04-03 | 2021-07-16 | 郑小宝 | Preparation method of aluminum alloy metal plated part |
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| US20040151926A1 (en) * | 2003-01-23 | 2004-08-05 | Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel Ltd.) | Aluminum alloy member superior in corrosion resistance and plasma resistance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110318080A (en) * | 2019-08-02 | 2019-10-11 | 吉林大学 | Form-material cooperates with bionical Anti-erosion function surface structure and preparation method thereof |
| CN112030118A (en) * | 2020-07-31 | 2020-12-04 | 中国原子能科学研究院 | Preparation method of deuterated polyethylene nanowire array target |
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