CN106367796A - Preparation method for laminated titanium dioxide/cadmium selenide/gold composite thin film - Google Patents

Preparation method for laminated titanium dioxide/cadmium selenide/gold composite thin film Download PDF

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Publication number
CN106367796A
CN106367796A CN201611004606.8A CN201611004606A CN106367796A CN 106367796 A CN106367796 A CN 106367796A CN 201611004606 A CN201611004606 A CN 201611004606A CN 106367796 A CN106367796 A CN 106367796A
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titanium dioxide
cadmium selenide
thin film
gold
titanium
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CN106367796B (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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Taiyuan University of Technology
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/26—Anodisation of refractory metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic 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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • C23C28/00—Coating 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
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings 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
    • 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
    • C23C28/00—Coating 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
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings 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
    • C23C28/345—Coatings 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
    • C23C28/3455—Coatings 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials

Abstract

The invention relates to a preparation method for a laminated titanium dioxide/cadmium selenide/gold composite thin film. According to a special structure deposited through precious metal after semiconductor coupling, a titanium dioxide nanotube thin film is prepared on a titanium sheet through an anode oxidization method; a titanium dioxide/cadmium selenide nano thin film is prepared through an electrochemical method; the titanium dioxide/cadmium selenide thin film is subjected to gold plating so that the titanium dioxide/cadmium selenide/gold composite thin film can be prepared, and the product is in the shape of a dark red film; the thin film is composed of titanium dioxide nanotubes; the nanotubes are uniform and compact and are arranged in order; the tube diameter is smaller than or equal to 100 nanometers, and the tube length is smaller than or equal to 7 microns; cadmium selenide particles are in shapes of nanospheres, and the particle diameter is smaller than or equal to 20 nanometers; gold particles are attached to the upper portions of the cadmium selenide nanoparticles, and combination is firm; and the titanium dioxide/cadmium selenide/gold composite thin film can obviously absorb ultraviolet light and visible light, generates 4 mA/cm<2> current under irradiation of a 100 W xenon lamp with a light filter with the cut-off lambda smaller than or equal to 420 nanometers and can be used during photo-hydrolysis hydrogen production and in photovoltaic products.

Description

A kind of preparation method of stacking shape titanium dioxide/cadmium selenide/gold laminated film
Technical field
The present invention relates to a kind of preparation method of stacking shape titanium dioxide/cadmium selenide/gold laminated film, belong to inorganic functional material Material preparation and the technical field of application.
Background technology
Solar energy, as a kind of renewable and clean energy resource, is the first-selected energy solving energy shortage and environmental pollution, utilizes Transition material solar energy can be converted into electric energy and chemical energy；Titanium dioxide stable performance, aboundresources, nontoxic, wide General it is applied to the fields such as solaode, 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 in terms of visible ray for the titanium dioxide；Photoproduction in titanium dioxide Electronics and being quickly combined of hole also result in photocatalysis efficiency reduction；In order to improve the absorption to visible ray for the titanium dioxide, open up Wide spectrum response range, needs to do modification to titanium dioxide, and one is to widen spectral absorption scope, and two is suppression light induced electron and sky Being combined of cave, can meet the demand of these two aspects using narrow-band semiconductor sensitized titanium dioxide；After semiconductors coupling, light absorbs Spectrum is widened, and improves the photoresponse to visible ray for the quasiconductor；Again due to cadmium selenide conduction band positions than titanium dioxide conduction band More negative, thus improve the efficiency of transmission of electronics and hole, be conducive to electronics to separate with hole；Based on this reason, use selenium Cadmium is coupled with titanium dioxide, deposits cadmium selenide nano particles using electrochemical method, be prepared on titania nanotube To titanium dioxide/cadmium selenide hetero-junction thin-film；Because the electric conductivity of interracial contact is poor, the mobility in light induced electron and hole is relatively Slowly, lead to 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 flow towards certain direction；The work function of noble metal would generally be higher than quasiconductor Work function, electrons constantly migrate to metal, and hole is left on quasiconductor, prevent the compound of electronics and hole, thus Improve photocatalysis efficiency.
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 on titanium substrate, raw material is done using sodium tartrate, selenium oxide, Caddy (Cleary), sunk with electrochemistry Area method makes titanium dioxide/cadmium selenide nano thin film, processes through magnetron sputtering metal spraying, and prepared stacking shape titanium dioxide/cadmium selenide/ Golden laminated film, to improve titanium dioxide to the absorption of visible ray and its separation of photogenerated charge and transmission.
Technical scheme
The present invention use chemical substance be: ammonium fluoride, gold, sodium tartrate, selenium oxide, Caddy (Cleary), ethylene glycol, hydrochloric acid, Acetone, dehydrated alcohol, deionized water, platinized platinum, titanium sheet, calomel piece；It is as follows that a combination thereof prepares consumption: with gram, milliliter, millimeter for counting Amount 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, dry after cleaning；
The titanium sheet dried is placed in another beaker, adds dehydrated alcohol 100ml, soaking and washing 10min, dry in the air after cleaning Dry；
The titanium sheet dried is placed in another beaker, adds deionized water 100ml, soaking and washing 10min, dry in the air after cleaning Dry；
2. clean platinized platinum
Platinized platinum is placed in beaker, adds acetone 100ml, soaking and washing 10min, dry after cleaning；
The platinized platinum drying is placed in another beaker, adds dehydrated alcohol 100ml, soaking and washing 10min, dry in the air after cleaning Dry；
The platinized platinum drying is placed in another beaker, adds deionized water 100ml, soaking and washing 10min, dry in the air after cleaning 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, and stirring 15min, so as to dissolving, becomes electrolyte；
4. anodic oxidation is prepared titanium deoxid film and is carried out in glass electrolysis bath, in electrolyte, is done with titanium sheet Anode, platinized platinum do negative electrode, under direct current 50v voltage, in magneton whipping process, titania nanotube battle array is generated on titanium sheet Row thin film；
Anelectrode is installed, anode titanium sheet is installed in left part position in electrolysis bath, and is lifted by hang spring；
Negative electrode is installed, right station installs negative electrode platinized platinum in electrolysis bath, and is lifted by hang spring；
The electrolyte prepared is added in electrolysis bath, electrolyte will flood titanium sheet and platinized platinum；
Magneton agitator is placed in electrolysis bath inner bottom part；
Open DC source, voltage 50v, 25 DEG C of electrolyte temperature, electrolysis time 60min, magneton stirring in electrolytic process Device stirs electrolyte；
In electrolytic process, titanium dioxide nano-pipe array thin film is generated on titanium sheet；
Close DC source after anodic oxidation, take out titanium sheet, deionized water is rinsed；
5. it is vacuum dried, titanium sheet and titanium dioxide nano-pipe array thin film thereon are placed in quartz container, then put In vacuum drying oven be dried, 50 DEG C of baking temperature, vacuum 2pa, drying time 15min；
6. heat treatment, titanium sheet and titanium dioxide nano-pipe array thin film thereon is placed in quartz container, is subsequently placed in In heat-treatment furnace, airtight；Temperature is heated to 450 DEG C from 25 DEG C with the heating rate of 2 DEG C/min by heater, insulation 120min, then cools to 25 DEG C with the furnace, generates the titanium dioxide nano-pipe array thin film of Anatase in titanium sheet；
(2) prepare titanium dioxide/cadmium selenide thin film
Prepare titanium dioxide/cadmium selenide thin film with electrochemical deposition method, with titanium sheet and titania nanotube battle array thereon Row thin film is working electrode, and platinized platinum is to electrode, and calomel piece is reference electrode, deposits on titanium dioxide nano-pipe array thin film Cadmium selenide, generates titanium dioxide/cadmium selenide thin film in titanium sheet；
1. prepare electrolyte
Weigh sodium tartrate 0.386g ± 0.001g, selenium oxide 0.044g ± 0.001g, Caddy (Cleary) 4.56g ± 0.001g, Measure deionized water 200ml ± 0.001ml, add in beaker, stir 20min, become electrolyte；
2. clean calomel piece
Calomel piece is placed in beaker, adds acetone 100ml, soaking and washing 10min, dry after cleaning；
The calomel drying piece is placed in another beaker, adds dehydrated alcohol 100ml, soaking and washing 10min, dry in the air after cleaning Dry；
The calomel drying piece is placed in another beaker, adds deionized water 100ml, soaking and washing 10min, dry in the air after cleaning Dry；
3. electrode is installed
In glass electrolysis bath, in centre position, reference electrode calomel piece is installed, is lifted by hang spring；
In glass electrolysis bath, 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 electrolysis bath, install to electrode platinized platinum in right station, lifted by hang spring；
4. add electrolyte
The selenizing cadmium electrolyte prepared is added in glass electrolysis bath, electrolyte will flood reference electrode, working electrode, right Electrode；
5. open electrochemical workstation, using cyclic voltammetry, electric potential scanning is interval to be -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 on working electrode titanium sheet；
6. soak, clean
Titanium sheet is placed in beaker, adds dehydrated alcohol 100ml, soak 5min；
Then titanium sheet is placed in another beaker, adds deionized water 100ml, clean 10min；
Dry after cleaning；
7. vacuum heat
Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, airtight；
Open vacuum pump, extract furnace air, make in stove invariablenes pressure of liquid in 2pa；
Temperature is heated to 200 DEG C from 25 DEG C with the heating rate of 2 DEG C/min by heater, is incubated 120min；
Then stop heating, cool to 25 DEG C with the furnace；
Titanium dioxide/cadmium selenide thin film is generated after cooling；
(3) prepare titanium dioxide/cadmium selenide/gold laminated film
The preparation of titanium dioxide/cadmium selenide/gold laminated film is carried out in vacuum sputtering instrument, is in vacuum state Under, with gold for target source, gold-plated nano-particle on titanium dioxide/cadmium selenide thin film；
1. open vacuum sputtering instrument, gold target is fixed on the fixed mount at top, gold target is down；
2. the titanium sheet of attachment titanium dioxide/cadmium selenide thin film is fixed in the machine carousel of vacuum sputtering instrument bottom, two Titanium oxide/cadmium selenide thin film is upward；
3. close vacuum sputtering instrument, and airtight；
4. open vacuum pump, extract instrument chamber air, make instrument intracavity invariablenes pressure of liquid in 2pa；
5. machine carousel, rotating disk revolution 20r/min are opened；
6. open the DC source on gold target top, running voltage is 100v, electric current 20ma, rated power 0.3kw；
Titanium dioxide/cadmium selenide/gold laminated film is generated on titanium sheet；
7. vacuum heat
Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, airtight；
Open vacuum pump, extract furnace air, make in stove invariablenes pressure of liquid in 2pa；
Temperature is heated to 200 DEG C from 25 DEG C with the heating rate of 2 DEG C/min, temperature retention time 120min by heater；
Then stop heating, cool to 25 DEG C with the furnace；
Generate titanium dioxide/cadmium selenide/gold laminated film in titanium plate surface；
(4) detection, analysis, sign
The pattern of the titanium dioxide/cadmium selenide/gold laminated film of preparation, composition, Chemical Physics performance are carried out detecting, divide Analysis, sign；
With scanning electron microscope, morphology analysis are carried out to titanium dioxide/cadmium selenide/gold laminated film；
With x-ray diffraction instrument, diffracted intensity analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film；
With electrochemical workstation, instantaneous photoresponse analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film；Electric current is with electricity Pressure mutation analysises；
Carry out ultraviolet-visible absorption with ultraviolet-visible spectrophotometer to titanium dioxide/cadmium selenide/gold laminated film to divide Analysis；
Conclusion: titanium dioxide/cadmium selenide/gold laminated film is that kermesinus is membranaceous, and thin film is made up of titania nanotube, Caliber≤100nm, pipe range≤7 μm, tube wall is attached with cadmium selenide nano particles, particle diameter≤20nm, 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, produces 4ma/cm under the 100w xenon lamp with cut-off λ≤420nm optical filter irradiates2Electric current；
(5) product storage
Titanium dioxide/cadmium selenide/gold the laminated film of preparation is stored in amber transparent glass container, airtight lucifuge storage Deposit, moistureproof, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, be according to after semiconductor coupling through noble metal loading Unique texture, is worked electrode using titanium sheet, ammonium fluoride and ethylene glycol are done electrolyte, prepared using anodizing in titanium sheet Titanic oxide nano tube thin-film；Raw material is done with selenium oxide, Caddy (Cleary), sodium tartrate does coating material, deionized water makees solvent, Hydrochloric acid makees ph regulator, prepares titanium dioxide/cadmium selenide nano thin film using electrochemical process on titanic oxide nano tube thin-film, Gold-plated on titanium dioxide/cadmium selenide thin film make titanium dioxide/cadmium selenide/gold laminated film, product be kermesinus membranaceous, thin Film is made up 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 xenon with cut-off λ≤420nm optical filter 4ma/cm is produced under light irradiation2Electric current, can use in light hydrolytic hydrogen production, photovoltaic products.
Brief description
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, titanium dioxide/cadmium selenide/gold laminated film instantaneous photoresponse collection of illustrative plates
Fig. 6, titanium dioxide/cadmium selenide/gold laminated film electric current is with change in voltage collection of illustrative plates
Fig. 7, titanium dioxide/cadmium selenide/gold laminated film ultraviolet-visible absorption collection of illustrative plates
In figure is shown, list of numerals is as follows:
1. electrochemical workstation, 2. the first display screen, 3. the first display lamp, 4. the first on and off switch, 5. the first unidirectional current Source controller, 6. electrolysis bath, 7. the first DC source, 8. the first hang spring, 9. the second hang spring, 10. the 3rd hang spring, 11. titanium sheet electricity Pole, 12. calomel electrodes, 13. platinum plate electrodes, 14. magneton agitators, 15. electrolyte, 16. vacuum sputtering instrument, 17. instrument lids, 18. Electric cabinet, 19. second display screens, 20. second display lamps, 21. second source switches, 22. second DC power control devices, 23. Wheel controller, 24. controller for vacuum pumps, 25. workbench, 26. machine carousel, 27. first fixed seats, 28. band titanium dioxide/ The titanium sheet of cadmium selenide thin film, 29. second DC sources, 30. gold targets, 31. second fixed seats, 32. instrument chambeies, 33. vacuum pumps, 34. Vacuum valve, 35. vacuum tubes.
Specific embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, for preparing titanium dioxide/cadmium selenide thin film state diagram, each portion position, annexation are correct, according to quantity Proportioning, sequentially operates.
The value of the chemical substance that preparation uses is to determine by the scope pre-setting, with gram, milliliter, millimeter for metering Unit.
Prepare titanium dioxide/cadmium selenide thin film to carry out in electrolysis bath, be with titanium sheet Nano tube array of titanium dioxide Thin film is working electrode, and platinized platinum is to electrode, and calomel piece is reference electrode, SEDIMENTARY SELENIUM on titanium dioxide nano-pipe array thin film Cadmium, generates titanium dioxide/cadmium selenide thin film；
Electrolysis bath 6 is rectangle, and electrolysis bath 6 bottom is electrochemical workstation 1, is provided with the first display on electrochemical workstation Screen the 2, first display lamp 3, the first on and off switch 4, the first DC power control device 5；It is the first unidirectional current on the top of electrolysis bath 6 Source 7；In electrolysis bath 6, left part is provided with titanium sheet electrode 11, and is connected with the first DC source 7 by the first hang spring 8；In electrolysis bath 6 Interior middle part is provided with calomel electrode 12, and is connected with the first DC source 7 by the second hang spring 9；In electrolysis bath 6, right part is provided with Platinum plate electrode 13, and be connected with the first DC source 7 by the 3rd hang spring 10；It is provided with magneton agitator 14 in electrolysis bath 6 inner bottom part； Hold electrolyte 15 in electrolysis bath 6, electrolyte 15 will flood titanium sheet electrode 11, calomel electrode 12, platinum plate electrode 13.
Shown in Fig. 2, it is that magnetron sputtering prepares titanium dioxide/cadmium selenide/gold thin film state diagram, each portion position, annexation Correct, sequentially operate.
Carry out in the gold-plated instrument in vacuum sputtering of titanium dioxide/cadmium selenide/gold laminated film, be in vacuum state Under, with gold for target source, in titanium dioxide/gold-plated nano-particle in cadmium selenide thin film top；
Vacuum sputtering instrument is vertical, and vacuum sputtering instrument 16 bottom is electric cabinet 18, top is instrument lid 17, inside is instrument chamber 32；It is provided with workbench 25 in vacuum sputtering instrument 16 inner bottom part, be provided with machine carousel 26 on workbench 25 top, and fixing by first Seat 27 is fixing, puts the titanium sheet 28 with titanium dioxide/cadmium selenide thin film on machine carousel 26 top；It is provided with instrument lid 17 top Two DC sources 29, the second DC source 29 bottom connects the gold target 30 in instrument chamber 32, and gold target 30 is fixing by the second fixed seat 31； Be provided with vacuum pump 33 in the left part of vacuum sputtering instrument 16, vacuum pump 33 top is provided with vacuum valve 34, vacuum tube 35, and with instrument chamber 32 Connection；Second display screen 19, the second display lamp 20, second source switch the 21, second DC source control are provided with electric cabinet 18 Device 22 processed, wheel controller 23, controller for vacuum pump 24.
Shown in Fig. 3, it is titanium dioxide/cadmium selenide/gold laminated film shape appearance figure, shown in figure, titania nanotube is equal Even densification, arrangement is neat, caliber≤100nm, pipe range≤7 μm, and cadmium selenide granule is in that nanometer is spherical, particle diameter≤20nm；Gold Granule is uniformly distributed along tube wall and pipe seam, is attached together with cadmium selenide granule, particle diameter≤10nm.
Shown in Fig. 4, it is titanium dioxide/cadmium selenide/gold laminated film x-ray diffraction intensity collection of illustrative plates, shown in figure, vertical coordinate For diffracted intensity, abscissa is the angle of diffraction, and in figure is visible, and gold, cadmium selenide and titanium dioxide exist simultaneously, illustrate titanium dioxide/ Cadmium selenide/gold laminated film is successfully prepared.
Shown in Fig. 5, it is titanium dioxide/cadmium selenide/gold laminated film instantaneous photoresponse collection of illustrative plates, (a) is titanium dioxide/selenizing Cadmium/instantaneous the photoresponse curve of gold laminated film, (b) is 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 lamp with cut-off λ≤420nm optical filter irradiates Respond, 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 change in voltage collection of illustrative plates, (a) be titanium dioxide/ With voltage change curve, (b) is titanium dioxide nano-pipe array thin film electric current with change in voltage to cadmium selenide/gold laminated film electric current Curve, laminated film open-circuit voltage is 1.04v, and short circuit current is 4.05ma/cm2, than titanium dioxide nano-pipe array thin film Short circuit current is obviously improved.
Shown in Fig. 7, be titanium dioxide/cadmium selenide/gold laminated film ultraviolet-visible absorption collection of illustrative plates, (a) be titanium dioxide/ Cadmium selenide/gold laminated film ultraviolet-visible absorption curve, (b) is titanium dioxide nano-pipe array thin film ultraviolet-visible absorption Curve, in figure is visible, and laminated film has obvious absorption to the visible ray of 400-600nm, and absorbance compares nano titania The absorbance of pipe array film is significantly increased.

Claims (3)

1. a kind of stacking shape titanium dioxide/cadmium selenide/gold laminated film preparation method it is characterised in that:
The chemical substance using is: ammonium fluoride, gold, sodium tartrate, selenium oxide, Caddy (Cleary), ethylene glycol, hydrochloric acid, acetone, anhydrous second Alcohol, deionized water, platinized platinum, titanium sheet, calomel piece；It is as follows that a combination thereof prepares consumption: with gram, milliliter, millimeter as measurement 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, dry after cleaning；
The titanium sheet dried is placed in another beaker, adds dehydrated alcohol 100ml, soaking and washing 10min, dry after cleaning；
The titanium sheet dried is placed in another beaker, adds deionized water 100ml, soaking and washing 10min, dry after cleaning；
2. clean platinized platinum
Platinized platinum is placed in beaker, adds acetone 100ml, soaking and washing 10min, dry after cleaning；
The platinized platinum drying is placed in another beaker, adds dehydrated alcohol 100ml, soaking and washing 10min, dry after cleaning；
The platinized platinum drying is placed in another beaker, adds deionized water 100ml, soaking and washing 10min, dry after cleaning；
3. prepare electrolyte
Weigh ammonium fluoride 1.48g ± 0.001g, measure ethylene glycol 196ml ± 0.001ml, deionized water 4ml ± 0.001ml, plus Enter in beaker, stirring 15min, so as to dissolving, becomes electrolyte；
4. anodic oxidation is prepared titanium deoxid film and is carried out in glass electrolysis bath, in electrolyte, with titanium sheet do anode, Platinized platinum cooks negative electrode, under direct current 50v voltage, in magneton whipping process, Nano tube array of titanium dioxide is generated on titanium sheet thin Film；
Anelectrode is installed, anode titanium sheet is installed in left part position in electrolysis bath, and is lifted by hang spring；
Negative electrode is installed, right station installs negative electrode platinized platinum in electrolysis bath, and is lifted by hang spring；
The electrolyte prepared is added in electrolysis bath, electrolyte will flood titanium sheet and platinized platinum；
Magneton agitator is placed in electrolysis bath inner bottom part；
Open DC source, voltage 50v, 25 DEG C of electrolyte temperature, electrolysis time 60min, in electrolytic process, magneton agitator stirs Mix electrolyte；
In electrolytic process, titanium dioxide nano-pipe array thin film is generated on titanium sheet；
Close DC source after anodic oxidation, take out titanium sheet, deionized water is rinsed；
5. it is vacuum dried, titanium sheet and titanium dioxide nano-pipe array thin film thereon are placed in quartz container, be subsequently placed in true In empty drying baker be dried, 50 DEG C of baking temperature, vacuum 2pa, drying time 15min；
6. heat treatment, titanium sheet and titanium dioxide nano-pipe array thin film thereon is placed in quartz container, is subsequently placed at heat In reason stove, airtight；Temperature is heated to 450 DEG C from 25 DEG C with the heating rate of 2 DEG C/min by heater, is incubated 120min, Then cool to 25 DEG C with the furnace, the titanium dioxide nano-pipe array thin film of Anatase is generated on titanium sheet；
(2) prepare titanium dioxide/cadmium selenide thin film
Prepare titanium dioxide/cadmium selenide thin film with electrochemical deposition method, thin with titanium sheet and Nano tube array of titanium dioxide thereon Film is working electrode, and platinized platinum is to electrode, and calomel piece is reference electrode, deposits selenizing on titanium dioxide nano-pipe array thin film Cadmium, generates titanium dioxide/cadmium selenide thin film in titanium sheet；
1. prepare electrolyte
Weigh sodium tartrate 0.386g ± 0.001g, selenium oxide 0.044g ± 0.001g, Caddy (Cleary) 4.56g ± 0.001g, measure Deionized water 200ml ± 0.001ml, adds in beaker, stirs 20min, become electrolyte；
2. clean calomel piece
Calomel piece is placed in beaker, adds acetone 100ml, soaking and washing 10min, dry after cleaning；
The calomel drying piece is placed in another beaker, adds dehydrated alcohol 100ml, soaking and washing 10min, dry after cleaning；
The calomel drying piece is placed in another beaker, adds deionized water 100ml, soaking and washing 10min, dry after cleaning；
3. electrode is installed
In glass electrolysis bath, in centre position, reference electrode calomel piece is installed, is lifted by hang spring；
In glass electrolysis bath, in left part position installment work electrode, i.e. titanium sheet and two Nano tube array of titanium dioxide thereon Thin film, and lifted by hang spring；
In glass electrolysis bath, install to electrode platinized platinum in right station, lifted by hang spring；
4. add electrolyte
By prepare selenizing cadmium electrolyte add glass electrolysis bath in, electrolyte to flood reference electrode, working electrode, to electricity Pole；
5. open electrochemical workstation, using cyclic voltammetry, electric potential scanning is interval to be -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 on working electrode titanium sheet；
6. soak, clean
Titanium sheet is placed in beaker, adds dehydrated alcohol 100ml, soak 5min；
Then titanium sheet is placed in another beaker, adds deionized water 100ml, clean 10min；
Dry after cleaning；
7. vacuum heat
Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, airtight；
Open vacuum pump, extract furnace air, make in stove invariablenes pressure of liquid in 2pa；
Temperature is heated to 200 DEG C from 25 DEG C with the heating rate of 2 DEG C/min by heater, is incubated 120min；
Then stop heating, cool to 25 DEG C with the furnace；
Titanium dioxide/cadmium selenide thin film is generated after cooling；
(3) prepare titanium dioxide/cadmium selenide/gold laminated film
The preparation of titanium dioxide/cadmium selenide/gold laminated film is carried out in vacuum sputtering instrument, is under vacuum conditions, with Gold is target source, gold-plated nano-particle on titanium dioxide/cadmium selenide thin film；
1. open vacuum sputtering instrument, gold target is fixed on the fixed mount at top, gold target is down；
2. the titanium sheet of attachment titanium dioxide/cadmium selenide thin film is fixed in the machine carousel of vacuum sputtering instrument bottom, titanium dioxide Titanium/cadmium selenide thin film is upward；
3. close vacuum sputtering instrument, and airtight；
4. open vacuum pump, extract instrument chamber air, make instrument intracavity invariablenes pressure of liquid in 2pa；
5. machine carousel, rotating disk revolution 20r/min are opened；
6. open the DC source on gold target top, running voltage is 100v, electric current 20ma, rated power 0.3kw；
Titanium dioxide/cadmium selenide/gold laminated film is generated on titanium sheet；
7. vacuum heat
Titanium sheet is placed in quartz container, is subsequently placed in vacuum heat treatment furnace, airtight；
Open vacuum pump, extract furnace air, make in stove invariablenes pressure of liquid in 2pa；
Temperature is heated to 200 DEG C from 25 DEG C with the heating rate of 2 DEG C/min, temperature retention time 120min by heater；
Then stop heating, cool to 25 DEG C with the furnace；
Generate titanium dioxide/cadmium selenide/gold laminated film in titanium plate surface；
(4) detection, analysis, sign
The pattern of titanium dioxide/cadmium selenide/gold laminated film of preparation, composition, Chemical Physics performance carried out detect, analyze, Characterize；
With scanning electron microscope, morphology analysis are carried out to titanium dioxide/cadmium selenide/gold laminated film；
With x-ray diffraction instrument, diffracted intensity analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film；
With electrochemical workstation, instantaneous photoresponse analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film；Electric current becomes with voltage Change analysis；
With ultraviolet-visible spectrophotometer, ultraviolet-visible absorption analysis is carried out to titanium dioxide/cadmium selenide/gold laminated film；
Conclusion: titanium dioxide/cadmium selenide/gold laminated film is that kermesinus is membranaceous, and thin film is made up of titania nanotube, caliber ≤ 100nm, pipe range≤7 μm, tube wall is attached with cadmium selenide nano particles, particle diameter≤20nm, 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, produces 4ma/cm under the 100w xenon lamp with cut-off λ≤420nm optical filter irradiates2Electric current；
(5) product storage
Titanium dioxide/cadmium selenide/gold the laminated film of preparation is stored in amber transparent glass container, airtight lucifuge storage, Moistureproof, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
2. the preparation method of a kind of stacking shape titanium dioxide/cadmium selenide/gold laminated film according to claim 1, it is special Levy and be:
Prepare titanium dioxide/cadmium selenide thin film to carry out in electrolysis bath, be with titanium sheet titanium dioxide nano-pipe array thin film For working electrode, platinized platinum is to electrode, and calomel piece is reference electrode, deposits selenizing on titanium dioxide nano-pipe array thin film Cadmium, generates titanium dioxide/cadmium selenide thin film；
Electrolysis bath (6) is rectangle, and electrolysis bath (6) bottom is electrochemical workstation (1), is provided with first and shows on electrochemical workstation Display screen (2), the first display lamp (3), the first on and off switch (4), the first DC power control device (5)；Top in electrolysis bath (6) For the first DC source (7)；In electrolysis bath (6), left part is provided with titanium sheet electrode (11), and by the first hang spring (8) and the first direct current Power supply (7) connects；In electrolysis bath (6), middle part is provided with calomel electrode (12), and by the second hang spring (9) and the first unidirectional current Source (7) connects；In electrolysis bath (6), right part is provided with platinum plate electrode (13), and by the 3rd hang spring (10) and the first DC source (7) Connect；It is provided with magneton agitator (14) in electrolysis bath (6) inner bottom part；Electrolyte (15), electrolyte is held in electrolysis bath (6) (15) titanium sheet electrode (11), calomel electrode (12), platinum plate electrode (13) will be flooded.
3. the preparation method of a kind of stacking shape titanium dioxide/cadmium selenide/gold laminated film according to claim 1, it is special Levy and be:
Carry out in the gold-plated instrument in vacuum sputtering of titanium dioxide/cadmium selenide/gold laminated film, be under vacuum conditions, with Gold is target source, in titanium dioxide/gold-plated nano-particle in cadmium selenide thin film top；
Vacuum sputtering instrument is vertical, and vacuum sputtering instrument (16) bottom is electric cabinet (18), top is instrument lid (17), inside is instrument chamber (32)；It is provided with workbench (25) in vacuum sputtering instrument (16) inner bottom part, be provided with machine carousel (26) on workbench (25) top, and Fixing by the first fixed seat (27), put the titanium sheet with titanium dioxide/cadmium selenide thin film (28) on machine carousel (26) top；? Instrument lid (17) top is provided with the second DC source (29), and the second DC source (29) bottom connects the gold target in instrument chamber (32) (30), gold target (30) is fixing by the second fixed seat (31)；It is provided with vacuum pump (33), vacuum pump in the left part of vacuum sputtering instrument (16) (33) top is provided with vacuum valve (34), vacuum tube (35), and connects with instrument chamber (32)；Electric cabinet (18) is provided with the second display Screen (19), the second display lamp (20), second source switch (21), the second DC power control device (22), wheel controller (23), Controller for vacuum pump (24).
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