CN109267010B - Flexible photoelectric corrosion thin film of titanium oxide and preparation method thereof - Google Patents

Flexible photoelectric corrosion thin film of titanium oxide and preparation method thereof Download PDF

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CN109267010B
CN109267010B CN201811445726.0A CN201811445726A CN109267010B CN 109267010 B CN109267010 B CN 109267010B CN 201811445726 A CN201811445726 A CN 201811445726A CN 109267010 B CN109267010 B CN 109267010B
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titanium oxide
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费佳蕾
谷卓欣
吴红艳
张成远
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Nanjing University of Information Science and Technology
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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
    • 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
    • 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 invention relates to a flexible photoelectric corrosion film of titanium oxide and a preparation method thereof, wherein the titanium oxide film is sputtered and deposited on the surface of a stainless steel foil substrate by virtue of the discharge action of double-cathode glow plasma, and the substrate is ultrasonically cleaned by acetone; and then putting the pretreated substrate on a sample table in a plasma furnace to finish the preparation of the titanium oxide film on the surface of the sample. The invention takes high-purity metal elements as the target material, and in order to improve the supply quantity and the supply efficiency of element reaction, double-layer glow plasma discharge is formed around the substrate and the target material, and the film forming only needs 10-30min. The thin film obtained by the invention is interpenetrated with the substrate, so that the bonding strength between the substrate and the thin film is high. The film obtained by the invention has high surface quality, low preparation method cost, no pollution, simpler process flow, almost no influence on the performance of the matrix and no damage to the matrix.

Description

Flexible photoelectric corrosion thin film of titanium oxide and preparation method thereof
Technical Field
The invention relates to the technical field of film preparation, in particular to a flexible photoelectric corrosion film of a titanium oxide compound and a preparation method thereof.
Background
The past decades have witnessed a rapid development of global economy, but at the same time have brought about a number of environmental and energy problems. TiO 22It has been widely used in the field of photocatalysis due to its strong oxidizing power, non-toxicity, high chemical stability and photostability. However, due to TiO2The wider band gap makes the utilization rate of sunlight not high. TiO with oxygen vacanciesxWith TiO being2The incomparable conductivity and visible light response capability attract people's attention.
The titanium dioxide nano material is one of important materials for hydrogen production and environmental pollution treatment. TiO 22There are the following common crystalline phases: tetragonal anatase, tetragonal rutile, orthorhombic brookite. The rutile phase and the anatase phase have higher photoactivity, but the utilization of sunlight is limited due to the wider band gap. TiO 2xIs a series of sub-oxygen state compounds with oxygen defects, and has TiO2Incomparable conductivity and photoresponse and cost advantage, therefore TiOxBecomes a material with great research value and wide application prospect. TiO 2xThe oxygen defects present in the material affect the material itselfLight absorption and conductivity, TiOxCompared with TiO2The forbidden band is narrow, and the response capability to visible light is strong; TiO 2xHas high electrical conductivity, and, in addition, TiOxHas chemical inertness and stable electrochemical stability in corrosive media. This makes it widely applicable in the field of optoelectronics, such as inert electrodes and batteries.
The existing methods for preparing titanium oxide thin films include spray pyrolysis method, sol-gel method, self-assembly electrochemical anodic oxidation method, chemical bath deposition method and the like, but the thin films prepared by the chemical preparation methods have complex chemical compositions, thick thickness and uneven coating. At present, the preparation of the film by a plasma physical sputtering deposition method has not been researched.
Disclosure of Invention
The invention provides a method for preparing a titanium oxide film on a stainless steel foil substrate by a plasma physical sputtering deposition method aiming at the problems of high quality, large area and the like of the titanium oxide film in the aspect of rapid preparation, and the process has the advantages of good controllability, high speed, low cost, good uniformity of the prepared film, single composition and suitability for large area preparation.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a flexible photoelectric corrosion film of titanium oxide and a preparation method thereof comprise the following steps:
1) ultrasonically cleaning a stainless steel foil substrate by using acetone and deionized water respectively, putting the pretreated substrate on an objective table in a plasma sputtering furnace body, and covering the objective table by using a heat-insulating sleeve, wherein titanium above a sample is used as a source electrode target material;
2) a layer of plasma glow discharge is formed on the surface of the substrate, a layer of plasma glow discharge area is formed on the surface of the target material, the two layers of plasma glow discharge areas are overlapped to enhance the film forming efficiency, the glow discharge improves the surface activation capability of the substrate, and a mutual diffusion interface layer is formed between the substrate and the target material element;
3) opening the plasma sputtering film forming equipment and a cold water pump, pumping the air pressure of the film coating furnace body to 2-5Pa by using a mechanical pump, and then using a molecular pumpPumping the furnace body back bottom to (3-6) × 10-4Pa, keeping the furnace in a high vacuum state;
4) filling argon into the furnace, and pumping to the ultimate vacuum degree again to discharge the air in the furnace;
5) argon and oxygen are filled into the furnace body in proportion, a workpiece power supply is turned on, 300-350V voltage is applied, and the sample is pre-bombarded for 10-30 minutes;
6) adjusting the working voltage and the source voltage after the pre-bombardment to make the workpiece and the source reach the working temperature, stabilizing various process parameters and starting heat preservation and film coating;
7) turning off the source power supply, cathode power supply and gas source in sequence, and pumping the vacuum furnace to (2-5) x 10-4Pa vacuum degree, cooling to room temperature, discharging and taking out to obtain Fe-Cr-Ni co-doped TixOyForming a multi-element composite alloy layer in the film.
In the step 1), the stainless steel foil substrate is ultrasonically cleaned for 2-4 hours respectively by acetone and deionized water.
In the step 1), the polar distance between the sample and the target material is kept between 18 and 22 mm.
And 4) filling argon into the furnace to 15-25Pa, pumping to the ultimate vacuum degree, and repeating for 2-3 times to discharge the air in the furnace as far as possible.
In the step 5), the volume ratio of the argon to the oxygen is 5:1-9:1, so that the pressure of the furnace body reaches 35 Pa.
In step 6), after the pre-bombardment, the working voltage is adjusted to 350-.
In the multi-element composite alloy layer, the component distribution of Fe-Cr-Ni matrix composite elements is stable, and the mass percent of Ti and O is obviously changed along with the argon-oxygen ratio.
The mass percentage of Ti in the surface layer of the material is 3.27-7.08%, the mass percentage of O is 12.29-20.44%, and the mass percentage change interval of Ti and O is between 0.1-0.5.
The invention provides a target material element which takes titanium as a titanium oxide sputtering, a titanium oxide film is sputtered and deposited on the surface of a stainless steel foil substrate by virtue of the discharge action of double-cathode glow plasma, and the substrate is ultrasonically cleaned by acetone; and then putting the pretreated substrate on a sample table in a plasma furnace to finish the preparation of the titanium oxide film on the surface of the sample.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention takes high-purity metal elements as the target material, and in order to improve the supply quantity and the supply efficiency of element reaction, double-layer glow plasma discharge is formed around the substrate and the target material, and the film forming only needs 10-30min.
2. The thin film obtained by the invention is interpenetrated with the substrate, so that the bonding strength between the substrate and the thin film is high.
3. The film obtained by the invention has high surface quality, low preparation method cost, no pollution, simpler process flow, almost no influence on the performance of the matrix and no damage to the matrix.
Drawings
FIG. 1: transient time-optical current spectrum of the titanium oxide film prepared by the embodiment of the invention.
FIG. 2: tafel curve of the titanium oxide film prepared by the embodiment of the invention.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
a method for sputtering and depositing a titanium oxide film on the surface of a stainless steel foil substrate by using titanium as a target material element sputtered by a titanium oxide through the discharge action of double-cathode glow plasma comprises the following process steps:
(1) and ultrasonically cleaning a stainless steel foil substrate by using acetone, putting the pretreated substrate on an objective table in a plasma sputtering furnace body, and covering the objective table by using a heat-insulating sleeve, wherein titanium above a sample is a source electrode target material, the distance between the sample and the target material is the polar distance of a workpiece, and the polar distance is kept at 20 mm.
(2) A layer of plasma glow discharge is formed on the surface of the substrate, a layer of plasma glow discharge area is formed on the surface of the target material, and the film forming efficiency is enhanced by overlapping the two plasma glow discharge areas.
(3) Opening plasma sputtering film forming equipment and a cold water pump matched with the equipment, pumping the air pressure of a film coating furnace body to 3Pa by using a mechanical pump, and further pumping the air pressure of the furnace body to 3 multiplied by 10 by using a molecular pump-4Pa, keeping the furnace in a high vacuum state;
(4) and (4) filling argon into the furnace to 15Pa, pumping the furnace to the ultimate vacuum degree again, and repeating the steps for 3 times so as to remove the air in the furnace as far as possible.
(5) Argon and oxygen are filled into the furnace body in a ratio of 5:1, so that the air pressure of the furnace body reaches 35Pa, a workpiece power supply is turned on, 300V voltage is applied, the sample is pre-bombarded for about 10 minutes, the sample is cleaned on one hand, and the surface is activated on the other hand, so that the adsorption of active atoms is facilitated.
(6) And after the pre-bombardment, adjusting the working pressure to 350V, adjusting the source voltage to a test value of 850V, enabling the workpiece and the source to reach the working temperature of 550 ℃, stabilizing various process parameters, and starting to carry out heat preservation for 30min for film coating.
(7) And (3) closing the source power supply, the cathode power supply and the gas source in sequence, then pumping the vacuum furnace to a vacuum degree of 3 x 10 < -4 > Pa, and cooling the vacuum furnace to room temperature along with the furnace.
(8) The content of each component of the titanium oxide film prepared by the process is observed by EDS (electron-discharge spectroscopy) energy spectrum analysis and is shown in Table 1. The element energy spectrum analysis of the film shows that when the argon-oxygen ratio is 5:1, the mass percent of Ti and O in the film is 1:4, and the composite elements in the Fe-Cr-Ni matrix are doped with Ti togetherxOyA composite alloy layer containing multiple elements is formed in the film. When the ultraviolet lamp is turned on, the stable value of the photocurrent is 0.28mA, and the self-corrosion potential is-408 mV.
Example 2:
a method for sputtering and depositing a titanium oxide film on the surface of a stainless steel foil substrate by using titanium as a target material element sputtered by a titanium oxide through the discharge action of double-cathode glow plasma comprises the following process steps:
(1) and ultrasonically cleaning a stainless steel foil substrate by using acetone, putting the pretreated substrate on an objective table in a plasma sputtering furnace body, and covering the objective table by using a heat-insulating sleeve, wherein titanium above a sample is a source electrode target material, the distance between the sample and the target material is the polar distance of a workpiece, and the polar distance is kept at 20 mm.
(2) A layer of plasma glow discharge is formed on the surface of the substrate, a layer of plasma glow discharge area is formed on the surface of the target material, and the film forming efficiency is enhanced by overlapping the two plasma glow discharge areas.
(3) Opening plasma sputtering film forming equipment and a cold water pump matched with the equipment, pumping the air pressure of a film coating furnace body to 3Pa by using a mechanical pump, and further pumping the air pressure of the furnace body to 6 multiplied by 10 by using a molecular pump-4Pa, keeping the furnace in a high vacuum state.
(4) And (4) filling argon into the furnace to 15Pa, pumping the furnace to the ultimate vacuum degree again, and repeating the steps for 3 times so as to remove the air in the furnace as far as possible.
(5) Argon and oxygen are filled into the furnace body in a ratio of 7:1, so that the air pressure of the furnace body reaches 35Pa, a workpiece power supply is turned on, 300V voltage is applied, the sample is pre-bombarded for about 10 minutes, the sample is cleaned on one hand, and the surface is activated on the other hand, so that the adsorption of active atoms is facilitated.
(6) And after the pre-bombardment, adjusting the working pressure to 350V, adjusting the source voltage to a test value of 850V, enabling the workpiece and the source to reach the working temperature of 550 ℃, stabilizing various process parameters, and starting to carry out heat preservation for 30min for film coating.
(7) And (3) closing the source power supply, the cathode power supply and the gas source in sequence, then pumping the vacuum furnace to a vacuum degree of 4 x 10 < -4 > Pa, and cooling the vacuum furnace to room temperature along with the furnace.
(8) The content of each component of the titanium oxide film prepared by the process is observed by EDS (electron-discharge spectroscopy) energy spectrum analysis and is shown in Table 1. The element energy spectrum analysis of the film shows that when the argon-oxygen ratio is 7:1, the mass percent of Ti and O in the film is about 2:5, and the composite elements in the Fe-Cr-Ni matrix are co-doped with TixOyA composite alloy layer containing multiple elements is formed in the film. When the ultraviolet lamp is turned on, the stable value of photocurrent is 0.18mA, and the self-corrosion potential is-417 mV.
Example 3:
a method for sputtering and depositing a titanium oxide film on the surface of a stainless steel foil substrate by using titanium as a target material element sputtered by a titanium oxide through the discharge action of double-cathode glow plasma comprises the following process steps:
(1) and ultrasonically cleaning a stainless steel foil substrate by using acetone, putting the pretreated substrate on an objective table in a plasma sputtering furnace body, and covering the objective table by using a heat-insulating sleeve, wherein titanium above a sample is a source electrode target material, the distance between the sample and the target material is the polar distance of a workpiece, and the polar distance is kept at 20 mm.
(2) A layer of plasma glow discharge is formed on the surface of the substrate, a layer of plasma glow discharge area is formed on the surface of the target material, and the film forming efficiency is enhanced by overlapping the two plasma glow discharge areas.
(3) Opening plasma sputtering film forming equipment and a cold water pump matched with the equipment, pumping the air pressure of a film coating furnace body to 3Pa by using a mechanical pump, and further pumping the air pressure of the furnace body to 6 multiplied by 10 by using a molecular pump-4Pa, keeping the furnace in a high vacuum state.
(4) And (4) filling argon into the furnace to 15Pa, pumping to the ultimate vacuum degree again, and repeating for 2-3 times so as to remove the air in the furnace as far as possible.
(5) Argon and oxygen are filled into the furnace body in a ratio of 9:1, so that the air pressure of the furnace body reaches 35Pa, a workpiece power supply is turned on, 300V voltage is applied, the sample is pre-bombarded for about 10 minutes, the sample is cleaned on one hand, and the surface is activated on the other hand, so that the adsorption of active atoms is facilitated.
(6) And after the pre-bombardment, adjusting the working pressure to 350V, adjusting the source voltage to a test value of 850V, enabling the workpiece and the source to reach the working temperature of 550 ℃, stabilizing various process parameters, and starting to carry out heat preservation for 30min for film coating.
(7) And (3) closing the source power supply, the cathode power supply and the gas source in sequence, then pumping the vacuum furnace to a vacuum degree of 5 x 10 < -4 > Pa, and cooling the vacuum furnace to room temperature along with the furnace.
(8) The content of each component of the titanium oxide film prepared by the process is observed by EDS (electron-discharge spectroscopy) energy spectrum analysis and is shown in Table 1. The element energy spectrum analysis of the film shows that when the argon-oxygen ratio is 9:1, the mass percent of Ti and O in the film is about 1:6, and the composite elements in the Fe-Cr-Ni matrix are codopedInto TixOyA composite alloy layer containing multiple elements is formed in the film. When the ultraviolet lamp is turned on, the stable value of photocurrent is 0.22mA, and the self-corrosion potential is-476 mV.
Table 1 shows EDS spectra of the titanium oxide thin films prepared in three examples of the present invention. The percentage contents of each element in the films prepared under the conditions of different argon oxygen ratios can be seen from the table that the component distribution of Fe-Cr-Ni matrix composite elements is stable, the mass percentages of Ti and O are obviously different along with the change of the argon oxygen ratios, and the oxygen pressure is increased along with the reduction of the argon pressure, so that the number of argon particles impacting oxygen particles in a glow discharge area is reduced, the number of oxygen ions in the films is reduced on the contrary, the mass percentage change interval of the Ti and the O is between 0.1 and 0.5, and finally the Fe-Cr-Ni matrix elements are doped into the Ti by mutual permeationxOyForming a multi-element composite alloy layer in the film.
TABLE 1
Figure GDA0002786609440000051
FIG. 1 is a transient time-optical current spectrum of a titanium oxide thin film prepared according to an example of the present invention. When the ultraviolet lamp is turned off, the photocurrents of the three samples are almost zero; the ultraviolet lamp is turned on, the photocurrent value rises instantly and rapidly, and reaches a steady state gradually along with the change of time.
FIG. 2 is a Tafel plot of a titanyl compound film prepared in accordance with an example of the present invention. Under the irradiation of an ultraviolet lamp, the Tafel curve of the titanium oxide film is shifted to the left, which shows that under the illumination condition, the titanium oxide film has the photo-cathode protection performance.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.

Claims (8)

1. A titanium oxide flexible photoelectric corrosion film and a preparation method thereof are characterized in that: the method comprises the following steps:
1) ultrasonically cleaning a stainless steel foil substrate by using acetone and deionized water respectively, putting the pretreated substrate on an objective table in a plasma sputtering furnace body, and covering the objective table by using a heat-insulating sleeve, wherein titanium above a sample is used as a source electrode target material;
2) a layer of plasma glow discharge is formed on the surface of the substrate, a layer of plasma glow discharge area is formed on the surface of the target material, the two layers of plasma glow discharge areas are overlapped to enhance the film forming efficiency, the glow discharge improves the surface activation capability of the substrate, and a mutual diffusion interface layer is formed between the substrate and the target material element;
3) opening plasma sputtering film forming equipment and cold water pump, pumping the air pressure of the film coating furnace body to 2-5Pa by using mechanical pump, and pumping the vacuum degree of the back bottom of the furnace body to (3-6) multiplied by 10 by using molecular pump-4Pa, keeping the furnace in a high vacuum state;
4) filling argon into the furnace, and pumping to the ultimate vacuum degree again to discharge the air in the furnace;
5) argon and oxygen are filled into the furnace body in proportion, a workpiece power supply is turned on, 300-350V voltage is applied, and the sample is pre-bombarded for 10-30 minutes;
6) adjusting the working voltage and the source voltage after the pre-bombardment to make the workpiece and the source reach the working temperature, stabilizing various process parameters and starting heat preservation and film coating;
7) turning off the source power supply, cathode power supply and gas source in sequence, and pumping the vacuum furnace to (2-5) x 10-4Pa vacuum degree, cooling to room temperature, discharging and taking out to obtain Fe-Cr-Ni co-doped TixOyForming a multi-element composite alloy layer in the film.
2. The flexible photo-voltaic corrosion thin film of titanium oxy compound according to claim 1, characterized in that: in the step 1), the stainless steel foil substrate is ultrasonically cleaned for 2-4 hours respectively by acetone and deionized water.
3. The flexible photo-voltaic corrosion thin film of titanium oxy compound according to claim 1, characterized in that: in the step 1), the polar distance between the sample and the target material is kept between 18 and 22 mm.
4. The flexible photo-voltaic corrosion thin film of titanium oxy compound according to claim 1, characterized in that: and 4) filling argon into the furnace to 15-25Pa, pumping to the ultimate vacuum degree, and repeating for 2-3 times to discharge the air in the furnace as far as possible.
5. The flexible photo-voltaic corrosion thin film of titanium oxy compound according to claim 1, characterized in that: in the step 5), the volume ratio of the argon to the oxygen is 5:1-9:1, so that the pressure of the furnace body reaches 35 Pa.
6. The flexible photo-voltaic corrosion thin film of titanium oxy compound according to claim 1, characterized in that: in step 6), after the pre-bombardment, the working voltage is adjusted to 350-.
7. The flexible photo-voltaic corrosion thin film of titanium oxy compound according to claim 1, characterized in that: in the multi-element composite alloy layer, the component distribution of Fe-Cr-Ni matrix composite elements is stable, and the mass percent of Ti and O is obviously changed along with the argon-oxygen ratio.
8. The flexible photo-voltaic corrosion thin film of titanium oxy compound according to claim 1, characterized in that: the mass percentage of Ti in the surface layer of the material is 3.27-7.08%, the mass percentage of O is 12.29-20.44%, and the mass percentage change interval of Ti and O is between 0.1-0.5.
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