CN106367796B - A kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film - Google Patents

A kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film Download PDF

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CN106367796B
CN106367796B CN201611004606.8A CN201611004606A CN106367796B CN 106367796 B CN106367796 B CN 106367796B CN 201611004606 A CN201611004606 A CN 201611004606A CN 106367796 B CN106367796 B CN 106367796B
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titanium dioxide
cadmium selenide
gold
titanium
thin film
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CN201611004606.8A
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CN106367796A (en
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薛晋波
申倩倩
张苪境
周健兴
赵浩成
张爱琴
贾虎生
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太原理工大学
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/18Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5806Thermal treatment
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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    • C23COATING 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
    • C23CCOATING 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
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
    • C23C28/3455Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide layer
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00Electrolytic coating other than with metals
    • C25D9/04Electrolytic coating other than with metals with inorganic materials

Abstract

The present invention relates to a kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film, it is according to the unique texture through noble metal loading after semiconductor coupling, titanic oxide nano tube thin-film is prepared in titanium sheet using anodizing, titanium dioxide/cadmium selenide nano film is prepared using electrochemical process, it is gold-plated on titanium dioxide/cadmium selenide thin film that titanium dioxide/cadmium selenide/gold laminated film is made, product is membranaceous for kermesinus, film is made of titania nanotube, nanotube even compact, arrangement is neat, caliber≤100nm, pipe range≤7 μm, cadmium selenide particle is spherical in nanometer, particle diameter≤20nm;Gold grain is attached to cadmium selenide nano particles top, is firmly combined with;Titanium dioxide/cadmium selenide/gold laminated film has obvious absorption to ultraviolet light and visible ray, and 4mA/cm is produced under the 100W xenon lamps irradiation with cut-off λ≤420nm optical filters2Electric current, can use in light hydrolytic hydrogen production, photovoltaic products.

Description

A kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film

Technical field

The present invention relates to a kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film, belong to inorganic functional material Material prepares and the technical field of application.

Background technology

Solar energy is the preferred energy for solving energy shortage and environmental pollution, utilizes as a kind of renewable and clean energy resource Transition material solar energy can be converted into electric energy and chemical energy;It is titanium dioxide performance stabilization, aboundresources, nontoxic, it is wide It is general to be applied to the fields such as solar cell, photocatalysis;Due to the wider Eg=3.2eV of the energy gap of titanium dioxide, can only absorb The ultraviolet portion of sunlight 5%, thus limit practical application of the titanium dioxide in terms of visible ray;Photoproduction in titanium dioxide Electronics and the quick compound photocatalysis efficiency that also results in hole reduce;In order to improve absorption of the titanium dioxide to visible ray, open up Wide spectrum response range to titanium dioxide, it is necessary to do modification, first, spectral absorption scope is widened, second, suppressing light induced electron and sky Cave it is compound, can meet the needs of these two aspects using narrow-band semiconductor sensitized titanium dioxide;After semiconductors coupling, light absorbs Spectrum is widened, and improves photoresponse of the semiconductor to visible ray;Again due to cadmium selenide conduction band positions than titanium dioxide conduction band It is more negative, so as to improve the efficiency of transmission in electronics and hole, be conducive to the separation in electronics and hole;Based on this reason, selenium is used Cadmium is coupled with titanium dioxide, and cadmium selenide nano particles are deposited on titania nanotube using electrochemical method, are prepared into To titanium dioxide/cadmium selenide hetero-junction thin-film;Since the electric conductivity of interracial contact is poor, the mobility in light induced electron and hole compared with Slowly, cause the photocatalysis efficiency of hetero-junction thin-film relatively low;Noble metal gold can be formed with rectified action with semiconductor interface contacting surface Schottky junction, can promote the electric charge in space to be flowed towards some direction;The work function of noble metal would generally be higher than semiconductor Work function, electrons are constantly migrated to metal, and hole is left on semiconductor, prevent the compound of electronics and hole, so that Improve photocatalysis efficiency.

The content of the invention

Goal of the invention

The purpose of the present invention is the situation for background technology, in ammonium fluoride, ethylene glycol solution, using anodizing Titania nanotube is prepared in titanium substrate, raw material is done using sodium tartrate, selenium oxide, caddy, is sunk with electrochemistry Titanium dioxide/cadmium selenide nano film is made in area method, is handled through magnetron sputtering metal spraying, and obtained stacking shape titanium dioxide/cadmium selenide/ Golden laminated film, to improve the separation and transmission of absorption and its photogenerated charge of the titanium dioxide to visible ray.

Technical solution

The chemical substance that the present invention uses is:Ammonium fluoride, gold, sodium tartrate, selenium oxide, caddy, ethylene glycol, hydrochloric acid, Acetone, absolute ethyl alcohol, deionized water, platinized platinum, titanium sheet, calomel piece;It is as follows that it combines preparation dosage:By gram, milliliter, millimeter in terms of Measure unit

Preparation method is as follows:

(1) anodizing prepares titanium deoxid film

1. clean titanium sheet

Titanium sheet is placed in beaker, adds acetone 100mL, soaking and washing 10min, dries after cleaning;

The titanium sheet dried is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 10min, dries in the air after cleaning It is dry;

The titanium sheet dried is placed in another beaker, adds deionized water 100mL, soaking and washing 10min, dries in the air after cleaning It is dry;

2. clean platinized platinum

Platinized platinum is placed in beaker, adds acetone 100mL, soaking and washing 10min, dries after cleaning;

The platinized platinum dried is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 10min, dries in the air after cleaning It is dry;

The platinized platinum dried is placed in another beaker, adds deionized water 100mL, soaking and washing 10min, dries in the air after cleaning It is dry;

3. prepare electrolyte

Weigh ammonium fluoride 1.48g ± 0.001g, measure ethylene glycol 196mL ± 0.001mL, deionized water 4mL ± 0.001mL, adds in beaker, stirs 15min, makes its dissolving, into electrolyte;

4. anodic oxidation prepares titanium deoxid film and carried out in glass electrolytic cell, in electrolyte, done with titanium sheet Anode, platinized platinum do cathode, under direct current 50V voltages, and in magneton whipping process, titania nanotube battle array is generated in titanium sheet Row film;

Positive electrode is installed, anode titanium sheet is installed in left part position in electrolytic cell, and is lifted by hang spring;

Negative electrode is installed, right station installs cathode platinized platinum in electrolytic cell, and is lifted by hang spring;

The electrolyte of preparation is added in electrolytic cell, electrolyte will flood titanium sheet and platinized platinum;

Magneton blender is placed in bottom in electrolytic cell;

DC power supply is opened, voltage 50V, 25 DEG C, electrolysis time 60min of electrolyte temperature, magneton stirs in electrolytic process Device stirs electrolyte;

In electrolytic process, titanium dioxide nano-pipe array thin film is generated in titanium sheet;

DC power supply is closed after anodic oxidation, titanium sheet is taken out, uses deionized water rinsing;

5. being dried in vacuo, titanium dioxide nano-pipe array thin film by titanium sheet and thereon is placed in quartz container, is then put It is dry in vacuum drying chamber, 50 DEG C, vacuum 2Pa, drying time 15min of drying temperature;

6. being heat-treated, titanium dioxide nano-pipe array thin film by titanium sheet and thereon is placed in quartz container, is subsequently placed in It is closed in heat-treatment furnace;Heater, is heated to 450 DEG C from 25 DEG C, insulation with the heating rate of 2 DEG C/min by temperature 120min, then cools to 25 DEG C with the furnace, and the titanium dioxide nano-pipe array thin film of Anatase is generated in titanium sheet;

(2) titanium dioxide/cadmium selenide thin film is prepared

Titanium dioxide/cadmium selenide thin film is prepared with electrochemical deposition method, titania nanotube battle array with titanium sheet and thereon Row film is working electrode, and platinized platinum deposits to be reference electrode to electrode, calomel piece on titanium dioxide nano-pipe array thin film Cadmium selenide, generates titanium dioxide/cadmium selenide thin film in titanium sheet;

1. prepare electrolyte

Sodium tartrate 0.386g ± 0.001g, selenium oxide 0.044g ± 0.001g, caddy 4.56g ± 0.001g are weighed, Deionized water 200mL ± 0.001mL is measured, is added in beaker, 20min is stirred, into electrolyte;

2. clean calomel piece

Calomel piece is placed in beaker, adds acetone 100mL, soaking and washing 10min, dries after cleaning;

The calomel piece dried is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 10min, dries in the air after cleaning It is dry;

The calomel piece dried is placed in another beaker, adds deionized water 100mL, soaking and washing 10min, dries in the air after cleaning It is dry;

3. electrode is installed

In glass electrolytic cell, reference electrode calomel piece is installed in centre position, is lifted by hang spring;

In glass electrolytic cell, in left part position installment work electrode, i.e. titanium sheet and two titania nanotubes thereon Array film, and lifted by hang spring;

In glass electrolytic cell, install to electrode platinized platinum in right station, lifted by hang spring;

4. add electrolyte

The selenizing cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, right Electrode;

5. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -0.9V~-0.4V, sweep speed For 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 300s;

Titanium dioxide/cadmium selenide thin film is generated in working electrode titanium sheet;

6. immersion, cleaning

Titanium sheet is placed in beaker, adds absolute ethyl alcohol 100mL, soaks 5min;

Then titanium sheet is placed in another beaker, adds deionized water 100mL, clean 10min;

Dried after cleaning;

7. vacuum heat

Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, it is closed;

Vacuum pump is opened, extracts furnace air, makes in stove invariablenes pressure of liquid in 2Pa;

Heater, is heated to 200 DEG C from 25 DEG C by temperature with the heating rate of 2 DEG C/min, keeps the temperature 120min;

Then stop heating, cool to 25 DEG C with the furnace;

Titanium dioxide/cadmium selenide thin film is generated after cooling;

(3) titanium dioxide/cadmium selenide/gold laminated film is prepared

The preparation of titanium dioxide/cadmium selenide/gold laminated film carries out in vacuum sputtering instrument, is in vacuum state Under, with gold for target source, gold nano grain is plated on titanium dioxide/cadmium selenide thin film;

1. opening vacuum sputtering instrument, gold target is fixed on the fixed frame at top, gold target is downward;

2. the titanium sheet for adhering to titanium dioxide/cadmium selenide thin film is fixed in the machine carousel of vacuum sputtering instrument lower part, two Titanium oxide/cadmium selenide thin film is upward;

3. vacuum sputtering instrument is closed, and it is closed;

4. opening vacuum pump, instrument chamber air is extracted, makes instrument intracavitary invariablenes pressure of liquid in 2Pa;

5. machine carousel is opened, turntable revolution 20r/min;

6. open the DC power supply on gold target top, operating voltage 100V, electric current 20mA, rated power 0.3KW;

Titanium dioxide/cadmium selenide/gold laminated film is generated in titanium sheet;

7. vacuum heat

Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, it is closed;

Vacuum pump is opened, extracts furnace air, makes in stove invariablenes pressure of liquid in 2Pa;

Heater, is heated to 200 DEG C from 25 DEG C, soaking time 120min with the heating rate of 2 DEG C/min by temperature;

Then stop heating, cool to 25 DEG C with the furnace;

Titanium dioxide/cadmium selenide/gold laminated film is generated in titanium plate surface;

(4) test, analysis and characterization

The pattern, component, Chemical Physics performance of titanium dioxide/cadmium selenide/gold laminated film of preparation are detected, point Analysis, characterization;

Morphology analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film with scanning electron microscope;

Diffracted intensity analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film with X-ray diffractometer;

Instantaneous photoresponse analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film with electrochemical workstation;Electric current is with electricity Press mutation analysis;

Ultraviolet-visible absorption point is carried out to titanium dioxide/cadmium selenide/gold laminated film with ultraviolet-visible spectrophotometer Analysis;

Conclusion:Titanium dioxide/cadmium selenide/gold laminated film is membranaceous for kermesinus, and film is made of titania nanotube, Caliber≤100nm, pipe range≤7 μm, are attached with cadmium selenide nano particles, particle diameter≤20nm on tube wall, gold grain is attached to Cadmium selenide nano particles top, gold grain diameter≤10nm, titanium dioxide/cadmium selenide/gold laminated film is to visible ray in 400- 600nm wavelength has obvious absorption, and 4mA/cm is produced under the 100W xenon lamps irradiation with cut-off λ≤420nm optical filters2Electric current;

(5) product storage

Titanium dioxide/cadmium selenide/gold laminated film of preparation is stored in amber transparent glass container, closed lucifuge storage Deposit, moisture-proof, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.

Beneficial effect

The present invention has obvious advance with background technology compared with, be according to after semiconductor coupling through noble metal loading Unique texture, is worked electrode, ammonium fluoride and ethylene glycol are done electrolyte, prepared using anodizing in titanium sheet using titanium sheet Titanic oxide nano tube thin-film;Raw material is done with selenium oxide, caddy, sodium tartrate does coating material, and deionized water makees solvent, Hydrochloric acid does pH adjusting agent, prepares titanium dioxide/cadmium selenide nano film on titanic oxide nano tube thin-film using electrochemical process, Gold-plated on titanium dioxide/cadmium selenide thin film that titanium dioxide/cadmium selenide/gold laminated film is made, product is membranaceous for kermesinus, thin Film is made of titania nanotube, nanotube even compact, and arrangement is neat, caliber≤100nm, pipe range≤7 μm, cadmium selenide Grain is spherical in nanometer, particle diameter≤20nm;Gold grain is attached to cadmium selenide nano particles top, is firmly combined with;Titanium dioxide/ Cadmium selenide/gold laminated film has obvious absorption to ultraviolet light and visible ray, in the 100W xenons with cut-off λ≤420nm optical filters 4mA/cm is produced under light irradiation2Electric current, can use in light hydrolytic hydrogen production, photovoltaic products.

Brief description of the drawings

Fig. 1, prepare titanium dioxide/cadmium selenide thin film state diagram

Fig. 2, magnetron sputtering are gold-plated to prepare titanium dioxide/cadmium selenide/gold thin film state diagram

Fig. 3, titanium dioxide/cadmium selenide/gold laminated film shape appearance figure

Fig. 4, titanium dioxide/cadmium selenide/gold laminated film X-ray diffraction intensity collection of illustrative plates

Fig. 5, the instantaneous photoresponse collection of illustrative plates of titanium dioxide/cadmium selenide/gold laminated film

Fig. 6, titanium dioxide/cadmium selenide/gold laminated film electric current are with voltage change collection of illustrative plates

Fig. 7, titanium dioxide/cadmium selenide/gold laminated film ultraviolet-visible absorption collection of illustrative plates

Shown in figure, list of numerals it is as follows:

1. electrochemical workstation, 2. first display screens, 3. first indicator lights, 4. first power switches, 5. first direct currents Source controller, 6. electrolytic cells, 7. first DC power supplies, 8. first hang springs, 9. second hang springs, 10. the 3rd hang springs, 11. titanium sheet electricity Pole, 12. calomel electrodes, 13. platinum plate electrodes, 14. magneton blenders, 15. electrolyte, 16. vacuum sputtering instrument, 17. instrument lids, 18. Electric cabinet, 19. second display screens, 20. second indicator lights, 21. second sources switch, 22. second DC power control devices, 23. Wheel controller, 24. controller for vacuum pump, 25. workbench, 26. machine carousels, 27. first fixed seats, 28. band titanium dioxide/ The titanium sheet of cadmium selenide thin film, 29. second DC power supplies, 30. gold targets, 31. second fixed seats, 32. instrument chambers, 33. vacuum pumps, 34. Vacuum valve, 35. vacuum tubes.

Embodiment

Below in conjunction with attached drawing, the present invention will be further described:

Shown in Fig. 1, to prepare titanium dioxide/cadmium selenide thin film state diagram, each portion position, connection relation are correct, according to quantity Proportioning, sequentially operates.

The value for preparing the chemical substance used is determined by pre-set scope, is metering with gram, milliliter, millimeter Unit.

Prepare titanium dioxide/cadmium selenide thin film to carry out in electrolytic cell, be with titanium sheet Nano tube array of titanium dioxide Film is working electrode, and platinized platinum is to electrode, and calomel piece is reference electrode, the SEDIMENTARY SELENIUM on titanium dioxide nano-pipe array thin film Cadmium, generates titanium dioxide/cadmium selenide thin film;

Electrolytic cell 6 is rectangle, and 6 lower part of electrolytic cell is electrochemical workstation 1, and the first display is equipped with electrochemical workstation Shield the 2, first indicator light 3, the first power switch 4, the first DC power control device 5;It is the first direct current on the top of electrolytic cell 6 Source 7;Left part is equipped with titanium sheet electrode 11 in electrolytic cell 6, and is connected by the first hang spring 8 with the first DC power supply 7;In electrolytic cell 6 Interior middle part is equipped with calomel electrode 12, and is connected by the second hang spring 9 with the first DC power supply 7;Right part is equipped with electrolytic cell 6 Platinum plate electrode 13, and be connected by the 3rd hang spring 10 with the first DC power supply 7;Bottom is equipped with magneton blender 14 in electrolytic cell 6; Electrolyte 15 is held in electrolytic cell 6, electrolyte 15 will flood titanium sheet electrode 11, calomel electrode 12, platinum plate electrode 13.

Shown in Fig. 2, titanium dioxide/cadmium selenide/gold thin film state diagram, each portion position, connection relation are prepared for magnetron sputtering Correctly sequentially to operate.

The gold-plated of titanium dioxide/cadmium selenide/gold laminated film carries out in vacuum sputtering instrument, is in vacuum state Under, with gold for target source, in titanium dioxide/cadmium selenide thin film top plating gold nano grain;

Vacuum sputtering instrument is vertical, and 16 lower part of vacuum sputtering instrument is electric cabinet 18, top is instrument lid 17, inside is instrument chamber 32;Bottom is equipped with workbench 25 in vacuum sputtering instrument 16, machine carousel 26 is equipped with 25 top of workbench, and fixed by first Seat 27 is fixed, and the titanium sheet 28 with titanium dioxide/cadmium selenide thin film is put on 26 top of machine carousel;The is equipped with 17 top of instrument lid Two DC power supplies 29,29 lower part of the second DC power supply connect the gold target 30 in instrument chamber 32, and gold target 30 is fixed by the second fixed seat 31; Be equipped with vacuum pump 33 in the left part of vacuum sputtering instrument 16,33 top of vacuum pump is equipped with vacuum valve 34, vacuum tube 35, and with instrument chamber 32 Connection;Second display screen 19, the second indicator light 20, second source are equipped with electric cabinet 18 and switchs the 21, second DC power supply control Device 22 processed, wheel controller 23, controller for vacuum pump 24.

It is titanium dioxide/cadmium selenide/gold laminated film shape appearance figure, shown in figure, titania nanotube is equal shown in Fig. 3 Even densification, arrangement is neat, caliber≤100nm, pipe range≤7 μm, and cadmium selenide particle is spherical in nanometer, particle diameter≤20nm;Gold Particle is uniformly distributed along tube wall and pipe seam, is attached together with cadmium selenide particle, particle diameter≤10nm.

It is titanium dioxide/cadmium selenide/gold laminated film X-ray diffraction intensity collection of illustrative plates shown in Fig. 4, shown in figure, ordinate For diffracted intensity, abscissa is the angle of diffraction, as it can be seen that gold, cadmium selenide and titanium dioxide exist at the same time in figure, illustrate titanium dioxide/ Cadmium selenide/gold laminated film is successfully prepared.

It is the instantaneous photoresponse collection of illustrative plates of titanium dioxide/cadmium selenide/gold laminated film shown in Fig. 5, (a) is titanium dioxide/selenizing Cadmium/instantaneous the photoresponse curve of gold laminated film, (b) are the instantaneous photoresponse curve of titanium dioxide nano-pipe array thin film, preparation Titanium dioxide/cadmium selenide/gold laminated film has obvious light under the 100W xenon lamps irradiation with cut-off λ≤420nm optical filters Response, and density of photocurrent is significantly increased than the density of photocurrent of titanium dioxide nano-pipe array thin film.

Shown in Fig. 6, be titanium dioxide/cadmium selenide/gold laminated film electric current with voltage change collection of illustrative plates, (a) be titanium dioxide/ Cadmium selenide/gold laminated film electric current is titanium dioxide nano-pipe array thin film electric current with voltage change with voltage change curve, (b) Curve, laminated film open-circuit voltage are 1.04V, short circuit current flow 4.05mA/cm2, than titanium dioxide nano-pipe array thin film Short circuit current flow is obviously improved.

Be titanium dioxide/cadmium selenide/gold laminated film ultraviolet-visible absorption collection of illustrative plates shown in Fig. 7, (a) for titanium dioxide/ Cadmium selenide/gold laminated film ultraviolet-visible absorption curve, (b) are titanium dioxide nano-pipe array thin film ultraviolet-visible absorption Curve, as it can be seen that laminated film has the visible ray of 400-600nm obvious absorption in figure, and absorptivity compares nano titania The absorptivity of pipe array film is significantly increased.

Claims (3)

  1. A kind of 1. preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film, it is characterised in that:
    The chemical substance used is:Ammonium fluoride, gold, sodium tartrate, selenium oxide, caddy, ethylene glycol, hydrochloric acid, acetone, anhydrous second Alcohol, deionized water, platinized platinum, titanium sheet, calomel piece;It is as follows that it combines preparation dosage:It is measurement unit with gram, milliliter, millimeter
    Preparation method is as follows:
    (1) anodizing prepares titanium deoxid film
    1. clean titanium sheet
    Titanium sheet is placed in beaker, adds acetone 100mL, soaking and washing 10min, dries after cleaning;
    The titanium sheet dried is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 10min, dries after cleaning;
    The titanium sheet dried is placed in another beaker, adds deionized water 100mL, soaking and washing 10min, dries after cleaning;
    2. clean platinized platinum
    Platinized platinum is placed in beaker, adds acetone 100mL, soaking and washing 10min, dries after cleaning;
    The platinized platinum dried is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 10min, dries after cleaning;
    The platinized platinum dried is placed in another beaker, adds deionized water 100mL, soaking and washing 10min, dries after cleaning;
    3. prepare electrolyte
    Ammonium fluoride 1.48g ± 0.001g is weighed, ethylene glycol 196mL ± 0.001mL, deionized water 4mL ± 0.001mL is measured, adds Enter in beaker, stir 15min, make its dissolving, into electrolyte;
    4. anodic oxidation prepares titanium deoxid film and is carried out in glass electrolytic cell, in electrolyte, with titanium sheet do anode, Platinized platinum is cooked cathode, under direct current 50V voltages, and in magneton whipping process, it is thin that Nano tube array of titanium dioxide is generated in titanium sheet Film;
    Positive electrode is installed, anode titanium sheet is installed in left part position in electrolytic cell, and is lifted by hang spring;
    Negative electrode is installed, right station installs cathode platinized platinum in electrolytic cell, and is lifted by hang spring;
    The electrolyte of preparation is added in electrolytic cell, electrolyte will flood titanium sheet and platinized platinum;
    Magneton blender is placed in bottom in electrolytic cell;
    DC power supply is opened, voltage 50V, 25 DEG C, electrolysis time 60min of electrolyte temperature, magneton blender stirs in electrolytic process Mix electrolyte;
    In electrolytic process, titanium dioxide nano-pipe array thin film is generated in titanium sheet;
    DC power supply is closed after anodic oxidation, titanium sheet is taken out, uses deionized water rinsing;
    5. being dried in vacuo, titanium dioxide nano-pipe array thin film by titanium sheet and thereon is placed in quartz container, is subsequently placed in true It is dry in empty drying box, 50 DEG C, vacuum 2Pa, drying time 15min of drying temperature;
    6. being heat-treated, titanium dioxide nano-pipe array thin film by titanium sheet and thereon is placed in quartz container, is subsequently placed in hot place Manage in stove, it is closed;Heater, is heated to 450 DEG C from 25 DEG C by temperature with the heating rate of 2 DEG C/min, keeps the temperature 120min, Then 25 DEG C are cooled to the furnace, the titanium dioxide nano-pipe array thin film of Anatase is generated in titanium sheet;
    (2) titanium dioxide/cadmium selenide thin film is prepared
    Titanium dioxide/cadmium selenide thin film is prepared with electrochemical deposition method, Nano tube array of titanium dioxide with titanium sheet and thereon is thin Film is working electrode, and platinized platinum deposits selenizing to be reference electrode to electrode, calomel piece on titanium dioxide nano-pipe array thin film Cadmium, generates titanium dioxide/cadmium selenide thin film in titanium sheet;
    1. prepare electrolyte
    Sodium tartrate 0.386g ± 0.001g, selenium oxide 0.044g ± 0.001g, caddy 4.56g ± 0.001g are weighed, is measured Deionized water 200mL ± 0.001mL, adds in beaker, 20min is stirred, into electrolyte;
    2. clean calomel piece
    Calomel piece is placed in beaker, adds acetone 100mL, soaking and washing 10min, dries after cleaning;
    The calomel piece dried is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 10min, dries after cleaning;
    The calomel piece dried is placed in another beaker, adds deionized water 100mL, soaking and washing 10min, dries after cleaning;
    3. electrode is installed
    In glass electrolytic cell, reference electrode calomel piece is installed in centre position, is lifted by hang spring;
    In glass electrolytic cell, in left part position installment work electrode, i.e. titanium sheet and Nano tube array of titanium dioxide thereon is thin Film, and lifted by hang spring;
    In glass electrolytic cell, install to electrode platinized platinum in right station, lifted by hang spring;
    4. add electrolyte
    The selenizing cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, to electricity Pole;
    5. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -0.9V~-0.4V, and sweep speed is 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 300s;
    Titanium dioxide/cadmium selenide thin film is generated in working electrode titanium sheet;
    6. immersion, cleaning
    Titanium sheet is placed in beaker, adds absolute ethyl alcohol 100mL, soaks 5min;
    Then titanium sheet is placed in another beaker, adds deionized water 100mL, clean 10min;
    Dried after cleaning;
    7. vacuum heat
    Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, it is closed;
    Vacuum pump is opened, extracts furnace air, makes in stove invariablenes pressure of liquid in 2Pa;
    Heater, is heated to 200 DEG C from 25 DEG C by temperature with the heating rate of 2 DEG C/min, keeps the temperature 120min;
    Then stop heating, cool to 25 DEG C with the furnace;
    Titanium dioxide/cadmium selenide thin film is generated after cooling;
    (3) titanium dioxide/cadmium selenide/gold laminated film is prepared
    The preparation of titanium dioxide/cadmium selenide/gold laminated film carries out in vacuum sputtering instrument, be under vacuum conditions, with Gold is target source, and gold nano grain is plated on titanium dioxide/cadmium selenide thin film;
    1. opening vacuum sputtering instrument, gold target is fixed on the fixed frame at top, gold target is downward;
    2. the titanium sheet for adhering to titanium dioxide/cadmium selenide thin film is fixed in the machine carousel of vacuum sputtering instrument lower part, titanium dioxide Titanium/cadmium selenide thin film is upward;
    3. vacuum sputtering instrument is closed, and it is closed;
    4. opening vacuum pump, instrument chamber air is extracted, makes instrument intracavitary invariablenes pressure of liquid in 2Pa;
    5. machine carousel is opened, turntable revolution 20r/min;
    6. open the DC power supply on gold target top, operating voltage 100V, electric current 20mA, rated power 0.3KW;
    Titanium dioxide/cadmium selenide/gold laminated film is generated in titanium sheet;
    7. vacuum heat
    Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, it is closed;
    Vacuum pump is opened, extracts furnace air, makes in stove invariablenes pressure of liquid in 2Pa;
    Heater, is heated to 200 DEG C from 25 DEG C, soaking time 120min with the heating rate of 2 DEG C/min by temperature;
    Then stop heating, cool to 25 DEG C with the furnace;
    Titanium dioxide/cadmium selenide/gold laminated film is generated in titanium plate surface;
    (4) test, analysis and characterization
    The pattern, component, Chemical Physics performance of titanium dioxide/cadmium selenide/gold laminated film of preparation are detected, analyzed, Characterization;
    Morphology analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film with scanning electron microscope;
    Diffracted intensity analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film with X-ray diffractometer;
    Instantaneous photoresponse analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film with electrochemical workstation;Electric current becomes with voltage Change analysis;
    Ultraviolet-visible absorption analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film with ultraviolet-visible spectrophotometer;
    Conclusion:Titanium dioxide/cadmium selenide/gold laminated film is membranaceous for kermesinus, and film is made of titania nanotube, caliber ≤ 100nm, pipe range≤7 μm, are attached with cadmium selenide nano particles, particle diameter≤20nm on tube wall, gold grain is attached to selenizing Cadmium nano particle top, gold grain diameter≤10nm, titanium dioxide/cadmium selenide/gold laminated film is to visible ray in 400-600nm Wavelength has obvious absorption, and 4mA/cm is produced under the 100W xenon lamps irradiation with cut-off λ≤420nm optical filters2Electric current;
    (5) product storage
    Titanium dioxide/cadmium selenide/gold laminated film of preparation is stored in amber transparent glass container, closed lucifuge storage, Moisture-proof, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
  2. 2. a kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film according to claim 1, it is special Sign is:
    Prepare titanium dioxide/cadmium selenide thin film to carry out in electrolytic cell, be with titanium sheet titanium dioxide nano-pipe array thin film For working electrode, platinized platinum deposits selenizing to be reference electrode to electrode, calomel piece on titanium dioxide nano-pipe array thin film Cadmium, generates titanium dioxide/cadmium selenide thin film;
    Electrolytic cell (6) is rectangle, and electrolytic cell (6) lower part is electrochemical workstation (1), and it is aobvious that first is equipped with electrochemical workstation Display screen (2), the first indicator light (3), the first power switch (4), the first DC power control device (5);On the top of electrolytic cell (6) For the first DC power supply (7);Titanium sheet electrode (11) is equipped with electrolytic cell (6) interior left part, and by the first hang spring (8) and the first direct current Power supply (7) connects;Calomel electrode (12) is equipped with electrolytic cell (6) interior middle part, and by the second hang spring (9) and the first direct current Source (7) connects;Platinum plate electrode (13) is equipped with electrolytic cell (6) interior right part, and by the 3rd hang spring (10) and the first DC power supply (7) Connection;Magneton blender (14) is equipped with electrolytic cell (6) interior bottom;Electrolyte (15), electrolyte are held in electrolytic cell (6) (15) titanium sheet electrode (11), calomel electrode (12), platinum plate electrode (13) are flooded.
  3. 3. a kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film according to claim 1, it is special Sign is:
    The gold-plated of titanium dioxide/cadmium selenide/gold laminated film carries out in vacuum sputtering instrument, be under vacuum conditions, with Gold is target source, in titanium dioxide/cadmium selenide thin film top plating gold nano grain;
    Vacuum sputtering instrument is vertical, and vacuum sputtering instrument (16) lower part is electric cabinet (18), top is instrument lid (17), inside is instrument chamber (32);Workbench (25) is equipped with vacuum sputtering instrument (16) interior bottom, machine carousel (26) is equipped with workbench (25) top, and It is fixed by the first fixed seat (27), put the titanium sheet (28) with titanium dioxide/cadmium selenide thin film on machine carousel (26) top; Instrument lid (17) top is equipped with the second DC power supply (29), and the second DC power supply (29) lower part connects the gold target in instrument chamber (32) (30), gold target (30) is fixed by the second fixed seat (31);Vacuum pump (33), vacuum pump are equipped with the left part of vacuum sputtering instrument (16) (33) top is equipped with vacuum valve (34), vacuum tube (35), and is connected with instrument chamber (32);The second display is equipped with electric cabinet (18) Shield (19), the second indicator light (20), second source switch (21), the second DC power control device (22), wheel controller (23), Controller for vacuum pump (24).
CN201611004606.8A 2016-11-15 2016-11-15 A kind of preparation method for being laminated shape titanium dioxide/cadmium selenide/gold laminated film CN106367796B (en)

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