CN109267010A - A kind of titanium oxygen compound flexible optoelectronic corrosion film and preparation method thereof - Google Patents
A kind of titanium oxygen compound flexible optoelectronic corrosion film and preparation method thereof Download PDFInfo
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- CN109267010A CN109267010A CN201811445726.0A CN201811445726A CN109267010A CN 109267010 A CN109267010 A CN 109267010A CN 201811445726 A CN201811445726 A CN 201811445726A CN 109267010 A CN109267010 A CN 109267010A
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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
- C23C14/0021—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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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Abstract
The present invention relates to a kind of titanium oxygen compound flexible optoelectronic corrosion films and preparation method thereof, and by twin cathode glow plasma discharge process in stainless steel foil matrix surface sputtering sedimentation titanium oxygen compound film, matrix is cleaned by ultrasonic with acetone；The matrix pre-processed is put into the preparation that sample surfaces titanium oxygen compound film is completed on the sample table in plasma furnace later.The present invention is using high pure metal element as target, in order to improve the supply and efficiency of supply of element reaction, double-deck glow plasma discharge is formed around substrate and target, film forming only needs 10-30min.Mutual infiltration has occurred between the film and matrix that the present invention obtains, therefore the bond strength between matrix and film is high.The film surface quality that the present invention obtains is high, and preparation method is at low cost, and pollution-free, process flow is relatively simple, on the performance of matrix itself almost without influence, not damaging substrate.
Description
Technical field
The present invention relates to technical field of film preparation, and in particular to a kind of titanium oxygen compound flexible optoelectronic corrosion film and its
Preparation method.
Background technique
The fast development of global economy has been witnessed in the past few decades, but has also brought many environment at the same time and the energy is asked
Topic.TiO2Due to its powerful oxidability, nontoxic, high chemical stability and photostability, photocatalysis has been widely used in it
Field.However due to TiO2Keep it not high to the utilization rate of sunlight with wider band gap.TiO with Lacking oxygenxHave
TiO2Incomparable electric conductivity and visible light-responded ability, has attracted the attention of people.
Titanium dioxide nano material is for one of hydrogen manufacturing and the important materials curbed environmental pollution.TiO2Have following common
Crystal phase: tetragonal anatase, tetragonal rutile, iris brockite.Wherein Rutile Type and Anatase have higher
Photolytic activity, however due to limiting its utilization to sunlight with wider band gap.TiOxIt is a series of with oxygen defect
Sub- oxygen state compound, have TiO2Incomparable electric conductivity and photoresponse ability, and there are cost advantages, therefore
TiOxSum as great researching value possesses the material of wide application prospect.TiOxPresent in oxygen defect affect material sheet
The absorbing properties and electric conductivity of body, TiOxCompared to TiO2Forbidden band is relatively narrow, has stronger responding ability to visible light；
TiOxWith high conductivity, in addition, TiOxThere is chemical inertness and more stable electrochemical stability in corrosive medium.This makes
It is obtained to be widely used in the photoelectric fields such as inert electrode and battery.
The preparation method of current existing titanium oxygen compound film has spray pyrolysis, sol-gel method, self assembly electrification
Anodizing, chemical bath deposition method etc., but the prepared film chemical complicated composition come out of above-mentioned chemical preparation process,
The thickness of film is thicker, and coats uneven.The film preparation is prepared not yet by plasma physics sputter deposition at present
There is research.
Summary of the invention
The present invention titanium oxygen compound film high quality, large area etc. quickly in terms of preparation aiming at the problem that, proposition with etc.
The method that the method for ion physical sputtering sedimentation prepares titanium oxygen compound film on stainless steel foil matrix, the process controllability
Well, speed is fast, at low cost, and the uniformity of film being prepared is good, and constituent is single, is suitble to large area preparation.
To achieve the above object, present invention provide the technical scheme that
A kind of titanium oxygen compound flexible optoelectronic corrosion film and preparation method thereof, comprising the following steps:
1) use acetone and deionized water to be cleaned by ultrasonic respectively stainless steel foil matrix, by the matrix pre-processed be put into etc. from
It on the son sputtering intracorporal objective table of furnace, and is covered with muff, the titanium above sample is source electrode target；
2) substrate surface forms one layer of plasma glow discharge, while target material surface also forms one layer of plasma glow discharge
Area, the overlapping enhancing film forming efficiency in two layers plasma glow discharge area, glow discharge improve matrix surface activation capacity, promote and target
Counterdiffusion boundary layer is formed between material element；
3) plasma sputtering film-forming apparatus and water supply pump are opened, plated film furnace body air pressure is evacuated to 2-5Pa using mechanical pump, then
Furnace body back end vacuum degree is evacuated to (3-6) × 10 using molecular pump-4Pa makes to keep high vacuum state in furnace；
4) it will be filled with argon gas in furnace, then be extracted into final vacuum again, the air in furnace is discharged；
5) argon gas and oxygen are filled in proportion to furnace body, open workpiece power supply and simultaneously apply 300-350V voltage, to sample into
Pre- bombardment in row 10-30 minutes；
6) operating voltage and source voltage are adjusted after pre- bombardment, so that workpiece and source electrode is reached operating temperature, stablizes each work
Skill parameter simultaneously starts to keep the temperature plated film；
7) source electrode power supply, cathode power and gas source are successively closed, then will be evacuated to (2-5) × 10 in vacuum drying oven-4Pa vacuum
Degree, be cooled to room temperature come out of the stove taking-up be co-doped with to get to Fe-Cr-Ni into TixOyMultielement composite alloy layer is formed in film.
In step 1), stainless steel foil matrix uses acetone and each cleaning of deionized water ultrasound 2-4 hours respectively.
In step 1), interpolar between sample and target is away from being maintained at 18-22mm.
In step 4), it will be filled with argon gas in furnace to 15-25Pa, then be extracted into final vacuum, repeats 2-3 times, with as far as possible
The air in furnace is discharged.
In step 5), argon gas and oxygen volume ratio are 5:1-9:1, so that furnace body air pressure reaches 35Pa.
In step 6), adjusts operating voltage to 300-350V after pre- bombardment, source voltage is transferred to 800-950V, makes workpiece
Reach 500-650 DEG C of operating temperature with source electrode, stablize each technological parameter and starts to keep the temperature 30min plated film.
In multielement composite alloy layer, the component distributing of Fe-Cr-Ni matrix complex element is relatively stable, and the matter of Ti and O
Percentage is measured with more more obvious than changing with argon oxygen.
The mass percentage of Ti is 3.27%-7.08% in material surface, and the mass percentage of O is 12.29%-
The mass percent constant interval of 20.44%, Ti and O are between 0.1-0.5.
The present invention provides a kind of target elements sputtered using titanium as titanium oxygen compound, put by twin cathode glow plasma
Matrix is cleaned by ultrasonic by electro ultrafiltration in stainless steel foil matrix surface sputtering sedimentation titanium oxygen compound film with acetone；Later
The matrix pre-processed is put into the preparation that sample surfaces titanium oxygen compound film is completed on the sample table in plasma furnace.
Compared with prior art, the beneficial effects of the present invention are:
1. the present invention is using high pure metal element as target, in order to improve the supply and efficiency of supply of element reaction, in base
Double-deck glow plasma discharge is formed around piece and target, film forming only needs 10-30min.
2. mutual infiltration has occurred between film and matrix that the present invention obtains, therefore the bond strength between matrix and film
It is high.
3. the film surface quality that the present invention obtains is high, and preparation method is at low cost, and pollution-free, process flow is more simple
It is single, on the performance of matrix itself almost without influence, not damaging substrate.
Detailed description of the invention
Fig. 1: the transient time-photoelectric current spectrogram of the titanium oxygen compound film of preparation of the embodiment of the present invention.
Fig. 2: the Tafel curve of the titanium oxygen compound film of preparation of the embodiment of the present invention.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1:
A kind of target elements sputtered using titanium as titanium oxygen compound, by twin cathode glow plasma discharge process stainless
The method of steel foil matrix surface sputtering sedimentation titanium oxygen compound film, technical process and steps are as follows:
(1) stainless steel foil matrix is cleaned by ultrasonic with acetone, the matrix pre-processed is put into plasma sputtering furnace
It on intracorporal objective table, and is covered with muff, the titanium above sample is source electrode target, and the spacing between sample and target is work
The interpolar of part is away from, interpolar away from being maintained at 20mm.
(2) substrate surface forms one layer of plasma glow discharge, while target material surface also forms one layer of plasma glow and puts
Electric area, by the overlapping enhancing film forming efficiency in two layers of plasma glow discharge area.
(3) plasma sputtering film-forming apparatus and water supply pump matched with its etc. are opened, using mechanical pump by plated film furnace body
Air pressure is evacuated to 3Pa, reuses molecular pump for furnace body air pressure and is further evacuated to 3 × 10-4Pa makes to keep high vacuum state in furnace；
(4) it will be filled with argon gas in furnace to 15Pa, be extracted into final vacuum again, and so on 3 times, to exclude furnace as far as possible
Interior air.
(5) being filled with the ratio of argon gas and oxygen to furnace body is 5:1, so that furnace body air pressure reaches 35Pa, opens workpiece power supply
And apply 300V voltage, pre- bombardment in 10 minutes or so is carried out to sample, on the one hand sample is cleaned, on the other hand activates table
Face in order to active atomic absorption.
(6) it is adjusted to 350V operating air pressure after pre- bombardment, source voltage is adjusted to test value 850V, makes workpiece and source electrode
Reach 550 DEG C of operating temperature, stablize each technological parameter and starts to keep the temperature 30min plated film.
(7) source electrode power supply, cathode power and gas source are successively closed, then will be evacuated to 3 × 10-4Pa vacuum degree in vacuum drying oven,
And furnace cooling is to room temperature.
(8) titanium oxygen compound film prepared by the technique observes containing for each constituent of film by EDS energy spectrum analysis
Amount, is shown in Table 1.The element energy spectrum analysis of film shows when argon oxygen ratio is 5:1, the mass percent of Ti and O in the film
For 1:4, complex element is co-doped with into Ti in e-Cr-Ni matrixxOyThe composite alloy layer containing multielement is formed in film.Ultraviolet lamp is opened
Qi Shi, the stationary value of photoelectric current are 0.28mA, and corrosion potential is -408mV.
Embodiment 2:
A kind of target elements sputtered using titanium as titanium oxygen compound, by twin cathode glow plasma discharge process stainless
The method of steel foil matrix surface sputtering sedimentation titanium oxygen compound film, technical process and steps are as follows:
(1) stainless steel foil matrix is cleaned by ultrasonic with acetone, the matrix pre-processed is put into plasma sputtering furnace
It on intracorporal objective table, and is covered with muff, the titanium above sample is source electrode target, and the spacing between sample and target is work
The interpolar of part is away from, interpolar away from being maintained at 20mm.
(2) substrate surface forms one layer of plasma glow discharge, while target material surface also forms one layer of plasma glow and puts
Electric area, by the overlapping enhancing film forming efficiency in two layers of plasma glow discharge area.
(3) plasma sputtering film-forming apparatus and water supply pump matched with its etc. are opened, using mechanical pump by plated film furnace body
Air pressure is evacuated to 3Pa, reuses molecular pump for furnace body air pressure and is further evacuated to 6 × 10-4Pa makes to keep high vacuum state in furnace.
(4) it will be filled with argon gas in furnace to 15Pa, be extracted into final vacuum again, and so on 3 times, to exclude furnace as far as possible
Interior air.
(5) being filled with the ratio of argon gas and oxygen to furnace body is 7:1, so that furnace body air pressure reaches 35Pa, opens workpiece power supply
And apply 300V voltage, pre- bombardment in 10 minutes or so is carried out to sample, on the one hand sample is cleaned, on the other hand activates table
Face in order to active atomic absorption.
(6) it is adjusted to 350V operating air pressure after pre- bombardment, source voltage is adjusted to test value 850V, makes workpiece and source electrode
Reach 550 DEG C of operating temperature, stablize each technological parameter and starts to keep the temperature 30min plated film.
(7) source electrode power supply, cathode power and gas source are successively closed, then will be evacuated to 4 × 10-4Pa vacuum degree in vacuum drying oven,
And furnace cooling is to room temperature.
(8) titanium oxygen compound film prepared by the technique observes containing for each constituent of film by EDS energy spectrum analysis
Amount, is shown in Table 1.The element energy spectrum analysis of film shows when argon oxygen ratio is 7:1, the mass percent of Ti and O in the film
Complex element is co-doped with into Ti in about 2:5, e-Cr-Ni matrixxOyThe composite alloy layer containing multielement is formed in film.Ultraviolet lamp
When unlatching, photoelectric current stationary value is 0.18mA, and corrosion potential is -417mV.
Embodiment 3:
A kind of target elements sputtered using titanium as titanium oxygen compound, by twin cathode glow plasma discharge process stainless
The method of steel foil matrix surface sputtering sedimentation titanium oxygen compound film, technical process and steps are as follows:
(1) stainless steel foil matrix is cleaned by ultrasonic with acetone, the matrix pre-processed is put into plasma sputtering furnace
It on intracorporal objective table, and is covered with muff, the titanium above sample is source electrode target, and the spacing between sample and target is work
The interpolar of part is away from, interpolar away from being maintained at 20mm.
(2) substrate surface forms one layer of plasma glow discharge, while target material surface also forms one layer of plasma glow and puts
Electric area, by the overlapping enhancing film forming efficiency in two layers of plasma glow discharge area.
(3) plasma sputtering film-forming apparatus and water supply pump matched with its etc. are opened, using mechanical pump by plated film furnace body
Air pressure is evacuated to 3Pa, reuses molecular pump for furnace body air pressure and is further evacuated to 6 × 10-4Pa makes to keep high vacuum state in furnace.
(4) it will be filled with argon gas in furnace to 15Pa, be extracted into final vacuum again, and so on 2-3 times, to exclude as far as possible
Air in furnace.
(5) being filled with the ratio of argon gas and oxygen to furnace body is 9:1, so that furnace body air pressure reaches 35Pa, opens workpiece power supply
And apply 300V voltage, pre- bombardment in 10 minutes or so is carried out to sample, on the one hand sample is cleaned, on the other hand activates table
Face in order to active atomic absorption.
(6) it is adjusted to 350V operating air pressure after pre- bombardment, source voltage is adjusted to test value 850V, makes workpiece and source electrode
Reach 550 DEG C of operating temperature, stablize each technological parameter and starts to keep the temperature 30min plated film.
(7) source electrode power supply, cathode power and gas source are successively closed, then will be evacuated to 5 × 10-4Pa vacuum degree in vacuum drying oven,
And furnace cooling is to room temperature.
(8) titanium oxygen compound film prepared by the technique observes containing for each constituent of film by EDS energy spectrum analysis
Amount, is shown in Table 1.The element energy spectrum analysis of film shows when argon oxygen ratio is 9:1, the mass percent of Ti and O in the film
Complex element is co-doped with into Ti in about 1:6, e-Cr-Ni matrixxOyThe composite alloy layer containing multielement is formed in film.Ultraviolet lamp
When unlatching, photoelectric current stationary value is 0.22mA, and corrosion potential is -476mV.
Table 1 is the EDS power spectrum of titanium oxygen compound film prepared by three embodiments of the invention.Under the conditions of different argon oxygen ratios
Each element percentage composition in the film prepared, the component distributing of Fe-Cr-Ni matrix complex element is more it can be seen from table
Stablize, and the mass percent of Ti and O is with more different than the more obvious proportion of variation with argon oxygen, and with argon gas gas
Pressure drop is low, and oxygen pneumatic increases, and reduces so that glow discharge zone argon particle hits oxygen number of particles, oxonium ion quantity is anti-in film
And reduce, the mass percent constant interval of Ti and O are ultimately formed and are passed through with Fe-Cr-Ni matrix element between 0.1-0.5
It mutually seeps and is incorporated into TixOyMultielement composite alloy layer is formed in film.
Table 1
Fig. 1 is the transient time-optogalvanic spectra of the titanium oxygen compound film of preparation of the embodiment of the present invention.Ultraviolet lamp lamp is closed
When, the photoelectric current of three samples is almost nil；Ultraviolet lamp is opened, photocurrent values moment rises rapidly, and with the change of time
Change progressivelyes reach stable state.
Fig. 2 is the Tafel curve of the titanium oxygen compound film of preparation of the embodiment of the present invention.Under ultraviolet light irradiation, titanyl
The Tafel curve for closing object film moves to left, and illustrates under illumination condition, and titanium oxygen compound film has photo-catelectrode protection performance.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, any ripe
Professional and technical personnel is known, without departing from the scope of the present invention, according to the technical essence of the invention, to the above reality
Any simple modifications, equivalent substitutions and improvements etc. made by example are applied, it is fallen within the scope of protection of the technical scheme of the present invention
It is interior.
Claims (8)
1. a kind of titanium oxygen compound flexible optoelectronic corrosion film and preparation method thereof, it is characterised in that: the following steps are included:
1) it uses acetone and deionized water to be cleaned by ultrasonic respectively stainless steel foil matrix, the matrix pre-processed is put into plasma and is splashed
It penetrates on the intracorporal objective table of furnace, and is covered with muff, the titanium above sample is source electrode target；
2) substrate surface forms one layer of plasma glow discharge, while target material surface also forms a floor plasma glow discharge area,
The overlapping enhancing film forming efficiency in two layers plasma glow discharge area, glow discharge improve matrix surface activation capacity, promote and target
Counterdiffusion boundary layer is formed between element；
3) plasma sputtering film-forming apparatus and water supply pump are opened, plated film furnace body air pressure is evacuated to 2-5Pa using mechanical pump, is reused
Furnace body back end vacuum degree is evacuated to (3-6) × 10 by molecular pump-4Pa makes to keep high vacuum state in furnace；
4) it will be filled with argon gas in furnace, then be extracted into final vacuum again, the air in furnace is discharged；
5) it is filled with argon gas and oxygen in proportion to furnace body, opens workpiece power supply and applies 300-350V voltage, 10- is carried out to sample
Pre- bombardment in 30 minutes；
6) operating voltage and source voltage are adjusted after pre- bombardment, workpiece and source electrode is made to reach operating temperature, stablize each technique ginseng
It counts and starts to keep the temperature plated film；
7) source electrode power supply, cathode power and gas source are successively closed, then will be evacuated to (2-5) × 10 in vacuum drying oven-4Pa vacuum degree, it is cold
But arrive room temperature come out of the stove taking-up be co-doped with to get to Fe-Cr-Ni into TixOyMultielement composite alloy layer is formed in film.
2. titanium oxygen compound flexible optoelectronic corrosion film according to claim 1 and preparation method thereof, it is characterised in that: step
It is rapid 1) in, stainless steel foil matrix uses acetone and each cleaning of deionized water ultrasound 2-4 hours respectively.
3. titanium oxygen compound flexible optoelectronic corrosion film according to claim 1 and preparation method thereof, it is characterised in that: step
It is rapid 1) in, interpolar between sample and target is away from being maintained at 18-22mm.
4. titanium oxygen compound flexible optoelectronic corrosion film according to claim 1 and preparation method thereof, it is characterised in that: step
It is rapid 4) in, argon gas will be filled in furnace to 15-25Pa, then be extracted into final vacuum, repeated 2-3 times, to be discharged in furnace as far as possible
Air.
5. titanium oxygen compound flexible optoelectronic corrosion film according to claim 1 and preparation method thereof, it is characterised in that: step
It is rapid 5) in, argon gas and oxygen volume ratio are 5:1-9:1, so that furnace body air pressure reaches 35Pa.
6. titanium oxygen compound flexible optoelectronic corrosion film according to claim 1 and preparation method thereof, it is characterised in that: step
It is rapid 6) in, adjust operating voltage to 300-350V after pre- bombardment, source voltage be transferred to 800-950V, reaches workpiece and source electrode
500-650 DEG C of operating temperature, stablizes each technological parameter and start to keep the temperature 30min plated film.
7. titanium oxygen compound flexible optoelectronic corrosion film according to claim 1 and preparation method thereof, it is characterised in that: more
In elements compounding alloy-layer, the component distributing of Fe-Cr-Ni matrix complex element is relatively stable, and the mass percent of Ti and O with
With argon oxygen than change it is more obvious.
8. titanium oxygen compound flexible optoelectronic corrosion film according to claim 1 and preparation method thereof, it is characterised in that: material
The mass percentage for expecting Ti in surface layer is 3.27%-7.08%, and the mass percentage of O is 12.29%-20.44%, Ti and
The mass percent constant interval of O is between 0.1-0.5.
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| CN112281124A (en) * | 2020-09-18 | 2021-01-29 | 山东宏旺实业有限公司 | Preparation method of common sand wire drawing surface titanium stainless steel coil |
| CN113073300A (en) * | 2021-03-25 | 2021-07-06 | 南京信息工程大学 | Method for plating high-purity zinc sulfide film on surface of non-metallic material in penetrating manner |
| CN113394554A (en) * | 2020-03-13 | 2021-09-14 | 昆山哈勃电波电子科技有限公司 | Method for preparing antenna by adopting TDP printing process |
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| CN113584450A (en) * | 2021-08-04 | 2021-11-02 | 南京信息工程大学 | Oxygen plasma etched zirconium dioxide film and preparation method thereof |
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| CN109267010B (en) | 2021-03-23 |
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