CN107857483A - A kind of preparation method of selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated construction - Google Patents

A kind of preparation method of selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated construction Download PDF

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CN107857483A
CN107857483A CN201711056273.8A CN201711056273A CN107857483A CN 107857483 A CN107857483 A CN 107857483A CN 201711056273 A CN201711056273 A CN 201711056273A CN 107857483 A CN107857483 A CN 107857483A
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titanium dioxide
cadmium
film
electro
selenium
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CN201711056273.8A
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CN107857483B (en
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申倩倩
薛晋波
朱留东
胡兰青
贾虎生
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太原理工大学
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES, OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/02Elemental selenium or tellurium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G11/00Compounds of cadmium
    • C01G11/02Sulfides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • 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
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES, OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/21Oxides
    • C03C2217/212TiO2
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES, OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/28Other inorganic materials
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES, OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/28Other inorganic materials
    • C03C2217/287Chalcogenides
    • C03C2217/288Sulfides

Abstract

The present invention relates to a kind of preparation method of selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure, it is the unique texture according to semiconductor coupling, titanium dioxide nanoplate array film is prepared on electro-conductive glass using hydrothermal synthesis method, selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is prepared using electrochemical process, product is that brownish red is membranaceous, film is made up of selenium/coated titanium dioxide nanoplate of cadmium sulfide laminated structure, nanometer sheet even compact, arrangement is neat, piece is thick≤500 nm, length of a film≤3 μm, cadmium selenide particle is spherical in nanometer, the nm of particle diameter≤40, the nm of cadmium sulfide particle diameter≤150, this preparation method technique is advanced, data are accurately full and accurate, it is the preparation method of advanced selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure.

Description

A kind of preparation of selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated construction Method

Technical field

The present invention relates to a kind of preparation method of selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure, category Inorganic functional material prepares and the technical field of application.

Background technology

Resource and environmental problem getting worse, solar energy are the alternative energy sources most cleaned, and semi-conducting material can be by solar energy Be converted to electric energy and chemical energy;It is titanium dioxide stable performance, aboundresources, nontoxic, be widely used in solar cell, The fields such as photocatalysis;The energy gap of titanium dioxide is Eg=3.2eV, can only absorb the ultraviolet portion of sunshine 5%, thus Limit practical application of the titanium dioxide in terms of visible ray;The quick of light induced electron and hole compound can also lead in titanium dioxide Photocatalysis efficiency is caused to reduce;In order to improve absorption of the titanium dioxide to visible ray, spectral response range is widened, it is necessary to titanium dioxide Titanium does modification, first, widen spectral absorption scope, second, suppressing the compound of light induced electron and hole, is sensitized using narrow-band semiconductor Titanium dioxide can meet the needs of these two aspects;After semiconductors coupling, red shift occurs for absorption spectrum, and improving semiconductor pair can See the photoresponse of light;Again because the conduction band positions of cadmium selenide, cadmium sulfide are all smaller than the conduction band positions of titanium dioxide, so as to improve Electronics and the efficiency of transmission in hole, are advantageous to the separation in electronics and hole;(001) of anatase titania, (100) and (101) three crystal faces can be 0.90Jm respectively-2、0.53J·m-2、0.44J·m-2, (001) crystal face is due to its high surface Can, there is higher activity in terms of the absorption and decomposition to reactant;Titanium dioxide nanoplate exposure with two-dimensional structure compared with More (001) crystal faces, there is unique advantage in photocatalysis field.

Cadmium selenide energy gap is 1.7eV, and electron hole mobility is big, and long lifespan, photoresponse haves a wide reach, its conduction band position Put smaller than the conduction band of titanium dioxide, coupled with titanium dioxide from cadmium selenide and its absorption spectrum can be not only widened to visible Light area, moreover it is possible to improve the efficiency of transmission of electron hole, realize higher photoelectric transformation efficiency;Cadmium sulfide energy gap is 2.4eV, Due to the phenomenon that simple cadmium selenide cladding titanium dioxide nano film has photoetch, photoelectric current is decayed, in cadmium selenide nano Cadmium sulfide nano layer is added between layer, it is coated to generate the adjustable selenium of photoresponse scope/cadmium sulfide laminated structure through Overheating Treatment Titanium dioxide nanosheet film, absorption spectrum can be not only widened, improve the efficiency of transmission of electron hole, realize that higher photoelectricity turns Efficiency is changed, and photoetch phenomenon can also be reduced, technique is also in scientific research.

The content of the invention

Goal of the invention

The purpose of the present invention is the situation for background technology, using hydrochloric acid, butyl titanate, ammonium titanium fluoride, urea as original Material, prepares titanium dioxide nanoplate, using sodium tartrate, selenium oxide, cadmium sulfate, sulphur using hydrothermal synthesis method on electro-conductive glass Sodium thiosulfate, sulfuric acid do raw material, and it is thin that selenium/coated titanium dioxide nanoplate of cadmium sulfide laminated structure is made with electrochemical deposition method Film, to improve the separation of absorption and its photogenerated charge of the titanium dioxide to visible ray and efficiency of transmission, and reduce photoetch.

Technical scheme

The chemical substance that the present invention uses is:Butyl titanate, hydrochloric acid, ammonium titanium fluoride, urea, sodium tartrate, selenium oxide, Cadmium sulfate, sodium thiosulfate, sulfuric acid, acetone, absolute ethyl alcohol, deionized water, platinized platinum, electro-conductive glass, silver chlorate;It, which is combined, prepares Dosage is as follows:It is measurement unit with gram, milliliter, millimeter

Preparation method is as follows:

(1) electro-conductive glass, platinized platinum, silver chloride film are pre-processed

1. clean electro-conductive glass

Electro-conductive glass is placed in beaker, acetone 100mL is added, soaking and washing 15min, is dried after cleaning;

The electro-conductive glass dried is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 15min, after cleaning Dry;

The electro-conductive glass dried is placed in another beaker, adds deionized water 100mL, soaking and washing 15min, after cleaning Dry;

2. clean platinized platinum

Platinized platinum is placed in beaker, acetone 100mL is added, soaking and washing 15min, is dried after cleaning;

The platinized platinum dried is placed in another beaker, absolute ethyl alcohol 100mL is added, soaking and washing 15min, is dried in the air after cleaning It is dry;

Platinized platinum after drying is placed in another beaker, deionized water 100mL is added, soaking and washing 15min, is dried in the air after cleaning It is dry;

3. clean silver chloride film

Silver chloride film is placed in beaker, acetone 100mL is added, soaking and washing 15min, is dried after cleaning;

Silver chloride film after drying is placed in another beaker, adds absolute ethyl alcohol 100mL, soaking and washing 15min, cleaning After dry;

Silver chloride film after drying is placed in another beaker, adds deionized water 100mL, soaking and washing 15min, cleaning After dry;

(2) hydrothermal synthesis method prepares titanium dioxide nanoplate array film

1. prepare reaction solution

Deionized water 30mL ± 0.001mL, hydrochloric acid 30mL ± 0.001mL, butyl titanate 1.5mL ± 0.001mL are measured, Weigh ammonium titanium fluoride 0.8g ± 0.001g, urea 0.8g ± 0.001g, add in beaker, stir 15min, make its dissolving, into anti- Answer liquid;

2. the electro-conductive glass cleaned after drying is put into the liner of reactor, the reaction solution configured is poured into liner In, closed reactor, reactor is put into heating furnace, 18h is incubated at 180 DEG C;

3. after heating and thermal insulation, reactor is taken out, is cooled to 25 DEG C;Open reactor, take out electro-conductive glass and thereon two TiOx nano chip arrays film;After titanium dioxide nanoplate array film by electro-conductive glass and thereon is cleaned with deionized water Dry;

4. being heat-treated, titanium dioxide nanoplate array film by electro-conductive glass and thereon is placed in quartz container, then It is placed in heat-treatment furnace, it is closed;Heater, 450 DEG C of heating-up temperature, 120min is incubated, then cools to 25 DEG C with the furnace;

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

Titanium dioxide/cadmium selenide thin film is prepared with electrochemical deposition method, nano titania with electro-conductive glass and thereon Chip arrays film is working electrode, platinized platinum be reference electrode to electrode, silver chlorate, on titanium dioxide nanoplate array film Cadmium selenide is deposited, titanium dioxide/cadmium selenide thin film is prepared on electro-conductive glass;

1. prepare selenizing cadmium electrolyte

Weigh sodium tartrate 0.194g ± 0.001g, selenium oxide 0.044g ± 0.001g, cadmium sulfate 0.248g ± 0.001g, deionized water 100mL ± 0.001mL is measured, added in beaker, 20min is stirred, into selenizing cadmium electrolyte;

2. electrode is installed

In glass electrolytic cell, reference electrode silver chloride film is installed in centre position, lifted by hang spring;

In glass electrolytic cell, in left part position installment work electrode, i.e. electro-conductive glass and nano titania thereon Chip arrays film, and lifted by hang spring;

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

3. add selenizing cadmium electrolyte

The selenizing cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, right 4/5ths of electrode;

4. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -0.9~-0.3V (relative to chlorine Change silver strip current potential), sweep speed 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 300s;In working electrode electro-conductive glass Upper generation titanium dioxide/cadmium selenide thin film;

5. immersion, cleaning

Titanium dioxide/cadmium selenide thin film by electro-conductive glass and thereon is placed in beaker, adds absolute ethyl alcohol 100mL, leaching Steep 5min;

Then titanium dioxide/cadmium selenide thin film by electro-conductive glass and thereon is placed in another beaker, adds deionized water 100mL, clean 10min;

Dried after cleaning;

(4) titanium dioxide/cadmium selenide/cadmium sulphide membrane is prepared

Titanium dioxide/cadmium selenide/cadmium sulphide membrane, titanium dioxide with electro-conductive glass and thereon are prepared with electrochemical deposition method Titanium/cadmium selenide thin film is working electrode, platinized platinum be reference electrode to electrode, silver chlorate, on titanium dioxide/cadmium selenide thin film Cadmium sulfide is deposited, titanium dioxide/cadmium selenide/cadmium sulphide membrane is prepared on electro-conductive glass;

1. formulating vulcanization cadmium electrolyte

Weigh sodium tartrate 0.194g ± 0.001g, sodium thiosulfate 1.28g ± 0.001g, cadmium sulfate 0.248g ± 0.001g, deionized water 100mL ± 0.001mL is measured, added in beaker, stir 20min, into vulcanization cadmium electrolyte;

2. electrode is installed

In glass electrolytic cell, reference electrode silver chloride film is installed in centre position, lifted by hang spring;

In glass electrolytic cell, in left part position installment work electrode, i.e. electro-conductive glass and titanium dioxide/selenizing thereon Cadmium film, and lifted by hang spring;

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

3. add vulcanization cadmium electrolyte

The vulcanization cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, right 4/5ths of electrode;

4. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -1.5V~0V (relative to chlorination Silver strip current potential), sweep speed 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 20min;On working electrode electro-conductive glass Generate titanium dioxide/cadmium selenide/cadmium sulphide membrane;

5. immersion, cleaning

Titanium dioxide/cadmium selenide/cadmium sulphide membrane by electro-conductive glass and thereon is placed in beaker, adds absolute ethyl alcohol 100mL, soak 5min;

Then titanium dioxide/cadmium selenide/cadmium sulphide membrane by electro-conductive glass and thereon is placed in another beaker, and addition is gone Ionized water 100mL, clean 10min;

Dried after cleaning;

(5) selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is prepared

Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is prepared with electrochemical deposition method, with conductive glass Glass and titanium dioxide/cadmium selenide/cadmium sulphide membrane thereon are working electrode, platinized platinum be reference electricity to electrode, silver chloride film Pole, cadmium selenide is deposited on titanium dioxide/cadmium selenide/cadmium sulphide membrane, selenium/cadmium sulfide laminated type knot is prepared on electro-conductive glass The coated titanium dioxide nanosheet film of structure;

1. prepare selenizing cadmium electrolyte

Weigh sodium tartrate 0.194g ± 0.001g, selenium oxide 0.044g ± 0.001g, cadmium sulfate 0.248g ± 0.001g, deionized water 100mL ± 0.001mL is measured, added in beaker, 20min is stirred, into selenizing cadmium electrolyte;

2. electrode is installed

In glass electrolytic cell, reference electrode silver chloride film is installed in centre position, lifted by hang spring;

In glass electrolytic cell, in left part position installment work electrode, i.e. electro-conductive glass and titanium dioxide/selenizing thereon Cadmium/cadmium sulphide membrane, and lifted by hang spring;

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

3. add selenizing cadmium electrolyte

The selenizing cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, right 4/5ths of electrode;

4. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -0.9~-0.3V (relative to chlorine Change silver strip current potential), sweep speed 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 150s;In working electrode electro-conductive glass Upper generation selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure;

5. immersion, cleaning

Selenium by electro-conductive glass and thereon/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is placed in beaker In, absolute ethyl alcohol 100mL is added, soaks 5min;

Then the selenium by electro-conductive glass and thereon/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is placed in separately In one beaker, deionized water 100mL is added, cleans 10min;

Dried after cleaning;

6. it is heat-treated, selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure by electro-conductive glass and thereon It is placed in quartz container, is subsequently placed in heat-treatment furnace, it is closed;Heater, 350 DEG C of heating-up temperature, 120min is incubated, so After cool to 25 DEG C with the furnace;

Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is generated on electro-conductive glass;

(6) test, analysis and characterization

To the selenium/pattern of the coated titanium dioxide nanosheet film of cadmium sulfide laminated structure, composition, Chemical Physics of preparation Performance carries out test, analysis and characterization;

Pattern point is carried out to selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure with SEM Analysis;

Material phase analysis is carried out to selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure with X-ray diffractometer;

Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is carried out with ultraviolet-visible spectrophotometer Ultraviolet-visible absorption is analyzed;

Instantaneous light sound is carried out to selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure with electrochemical workstation It should analyze, electric current is analyzed with voltage change;

Conclusion:Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure be brownish red it is membranaceous, film by selenium/ Cadmium sulfide laminated structure coated titanium dioxide nanoplate composition, wherein titanium dioxide nanoplate length≤3 μm, thickness≤ 500nm, nanometer sheet surface attachment have cadmium sulfide and cadmium selenide particle, cadmium selenide nano particles diameter≤40nm, cadmium sulfide particle Diameter≤150nm, the coated titanium dioxide nanosheet film film of selenium/cadmium sulfide laminated structure is to visible ray in 400-700nm Wavelength has obvious absorption, and 3mA/cm is produced under the 100W xenon lamps irradiation with cut-off λ≤420nm optical filters2Electric current;

(7) product storage

Amber transparent glass appearance is stored in selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure of preparation In device, closed lucifuge storage, 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, is to be directed to the unique texture after semiconductor coupling, adopts It is substrate with electro-conductive glass, deionized water, hydrochloric acid, butyl titanate, urea and fluotitanic acid ammonia do reaction solution, using Hydrothermal Synthesiss Method prepares titanium dioxide nanoplate array film on electro-conductive glass;Raw material, wine are done with selenium oxide, cadmium sulfate, sodium thiosulfate Stone acid sodium does coating material, and deionized water does solvent, detergent, and sulfuric acid does pH adjusting agent, using electrochemical process in titanium dioxide Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is prepared on titanium nano-chip arrays film, product is brownish red Membranaceous, film is made up of selenium/coated titanium dioxide nanoplate of cadmium sulfide laminated structure, wherein titanium dioxide nanoplate length≤ 3 μm, thickness≤500nm, nanometer sheet surface attachment have cadmium selenide nano particles, cadmium sulfide particle, cadmium selenide nano particles diameter ≤ 40nm, cadmium sulfide particle diameter≤150nm, selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is to visible Light has obvious absorption in 400-700nm wavelength, and 3 mA/ are produced under the 100W xenon lamps irradiation with cut-off λ≤420nm optical filters cm2Electric current, can be used in light hydrolytic hydrogen production, photovoltaic products.

Brief description of the drawings

Fig. 1, prepare the coated titanium dioxide nanosheet film state diagram of selenium/cadmium sulfide laminated structure

The coated titanium dioxide nanosheet film structure chart of Fig. 2, selenium/cadmium sulfide laminated structure

Fig. 3, titanium dioxide nanoplate array film shape appearance figure

Fig. 4, titanium dioxide/cadmium selenide thin film shape appearance figure

The coated titanium dioxide nanosheet film shape appearance figure of Fig. 5, selenium/cadmium sulfide laminated structure

The coated titanium dioxide nanosheet film X-ray diffraction intensity collection of illustrative plates of Fig. 6, selenium/cadmium sulfide laminated structure

The instantaneous photoresponse collection of illustrative plates of Fig. 7, selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure

The coated titanium dioxide nanosheet film electric current of Fig. 8, selenium/cadmium sulfide laminated structure is with voltage change collection of illustrative plates

The coated titanium dioxide nanosheet film ultraviolet-visible absorption collection of illustrative plates of Fig. 9, selenium/cadmium sulfide laminated structure

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

1st, electrochemical workstation, 2, display screen, 3, indicator lamp, 4, power switch, 5, DC power control device, 6, electrolysis Groove, 7, dc source, the 8, first hang spring, the 9, second hang spring, the 10, the 3rd hang spring, 11, electro-conductive glass and titanium dioxide/selenium thereon The membrane electrode of cadmium/cadmium sulfide, 12, silver chloride film, 13, platinum plate electrode, 14, magneton agitator, 15, selenizing cadmium electrolyte, 16th, electro-conductive glass, 17, titanium dioxide nanoplate array, 18, cadmium selenide nano film, 19, cadmium sulfide nano-film, 20, selenizing Cadmium nano thin-film.

Embodiment

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

Shown in Fig. 1, to prepare the coated titanium dioxide nanosheet film state diagram of selenium/cadmium sulfide laminated structure, each position Put, annexation will be matched correctly according to quantity, sequentially operate.

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

Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is prepared to carry out in electrolytic cell, be with Electro-conductive glass and titanium dioxide/cadmium selenide/cadmium sulphide membrane electrode thereon are working electrode, platinized platinum is to electrode, silver chlorate Piece is reference electrode, and cadmium selenide is deposited on titanium dioxide/cadmium selenide/cadmium sulphide membrane electrode in electro-conductive glass and thereon, raw Into selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure;

Electrolytic cell 6 is rectangle, and the bottom of electrolytic cell 6 is electrochemical workstation 1, and display screen is provided with electrochemical workstation 1 2nd, indicator lamp 3, power switch 4, DC power control device 5;It is dc source 7 on the top of electrolytic cell 6;It is left in electrolytic cell 6 Titanium dioxide/cadmium selenide/cadmium sulphide membrane electrode 11 of the portion provided with electro-conductive glass and thereon, and by the first hang spring 8 and direct current Source 7 connects;Middle part is provided with silver chloride film 12 in electrolytic cell 6, and is connected by the second hang spring 9 with dc source 7;It is being electrolysed Right part is provided with platinum plate electrode 13 in groove 6, and is connected by the 3rd hang spring 10 with dc source 7;Magneton is provided with the inner bottom part of electrolytic cell 6 Agitator 14;Hold selenizing cadmium electrolyte 15 in electrolytic cell 6, selenizing cadmium electrolyte 15 will flood electro-conductive glass and thereon Titanium dioxide/cadmium selenide/cadmium sulphide membrane electrode 11, silver chloride film 12,4/5ths of platinum plate electrode 13.

It is the coated titanium dioxide nanosheet film structure chart of selenium/cadmium sulfide laminated structure shown in Fig. 2, its structure is:Base Bottom is electro-conductive glass 16, is titanium dioxide nanoplate array film 17, in titanium dioxide nanoplate battle array on the top of electro-conductive glass 16 The top of row film 17 is cadmium selenide nano film 18, is cadmium sulfide nano-film 19 on the top of cadmium selenide nano film 18, in sulphur The top of cadmium nano thin-film 19 is cadmium selenide nano film 20.

It is titanium dioxide nanoplate array film shape appearance figure shown in Fig. 3, schemes shown in a, titanium dioxide nanoplate uniformly causes Close, arrangement is neat, piece thickness≤400nm, length of a film≤2.5 μm, exposes more (001) high activity crystal face;Scheme shown in b, to expose Larger face be (001) high activity crystal face.

It is titanium dioxide/cadmium selenide thin film shape appearance figure shown in Fig. 4, schemes shown in a, selenium/cadmium sulfide laminated structure coated two TiOx nano piece filmhaving apolarizedlight is neat, piece thickness≤400nm, length of a film≤2.5 μm;Scheme shown in b, cadmium selenide particle even compact Titanium dioxide nanoplate array is coated on, cadmium selenide particle is spherical in nanometer, particle diameter≤40nm.

It is the coated titanium dioxide nanosheet film shape appearance figure of selenium/cadmium sulfide laminated structure shown in Fig. 5, schemes shown in a, selenium/ The coated titanium dioxide nanosheet film arrangement of cadmium sulfide laminated structure is neat, piece thickness≤500nm, length of a film≤3 μm;Scheme shown in b, It is coated on titanium dioxide nanoplate array cadmium selenide particle, cadmium sulfide particle even compact, cadmium selenide particle is spherical in nanometer, Particle diameter≤40nm, cadmium sulfide particle diameter≤150nm.

It is the coated titanium dioxide nanosheet film X ray diffraction intensity figures of selenium/cadmium sulfide laminated structure shown in Fig. 6 Spectrum, abscissa are the angle of diffraction, and ordinate is diffracted intensity, and a is the X-ray diffraction intensity figure of titanium dioxide nanoplate array film Spectrum, b are the diffracted intensity collection of illustrative plates of the coated titanium dioxide nanosheet film X ray of selenium/cadmium sulfide laminated structure, and a is visible in figure, The θ of the angle of diffraction 2 corresponds to anatase crystal titanium dioxide respectively when being 25.28 °, 37.8 °, 38.57 °, 48.05 ° and 55.06 ° (101), (004), (112), (200) and (211) crystallographic plane diffraction peak;B is visible in figure, and the θ of the angle of diffraction 2 is right respectively when being 25.35 ° (111) crystallographic plane diffraction peak of cubic cadmium selenide and (002) crystallographic plane diffraction peak of hexagonal structure cadmium selenide are answered, the θ of the angle of diffraction 2 is (040), (033), (020) crystal face for corresponding to orthorhombic forms cadmium sulfide at 25.28 °, 26.48 °, 36.99 ° and 26.51 ° respectively are spread out Penetrate (002) crystallographic plane diffraction peak of peak and hexagonal structure cadmium sulfide;In figure a and b in general, when the θ of the angle of diffraction 2 be 42 ° -45 ° and At 49 ° -51 °, there is projection in b figures, sulphur, selenium, cadmium composition are obtained by searching powder diffraction data standard committee card Ternary compound card: JCPDS 49-1459(CdS0.75Se0.25)、JCPDS 49-1460(CdS0.52Se0.48) and JCPDS 50-0720(CdS0.42Se0.58) and JCPDS 50-0721 (CdS0.33Se0.67), wherein CdS1-xSexX=0.25, 0.48th, 0.58 and 0.67, cadmium selenide, cadmium sulfide, sulphur selenium cadmium ternary compound and titanium dioxide exist simultaneously, illustrate selenium/vulcanization The coated titanium dioxide nanosheet film of cadmium laminated structure is successfully prepared.

It is the instantaneous photoresponse collection of illustrative plates of selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure shown in Fig. 7, a is The instantaneous photoresponse curve of titanium dioxide nanoplate array film, b are selenium/coated titanium dioxide nanoplate of cadmium sulfide laminated structure Instantaneous film photoresponse curve, selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure of preparation is with cut-off λ There is obvious photoresponse under the 100W xenon lamps irradiation of≤420nm optical filters, and density of photocurrent is than titanium dioxide nanoplate array The density of photocurrent of film is significantly increased.

Shown in Fig. 8, be the coated titanium dioxide nanosheet film electric current of selenium/cadmium sulfide laminated structure with voltage change figure Spectrum, a be titanium dioxide nanoplate array film electric current with voltage change curve, b is selenium/coated dioxy of cadmium sulfide laminated structure Change titanium nanometer sheet film electric current with voltage change curve, laminated film open-circuit voltage is 1.04V, short circuit current 3mA/cm2, than The short circuit current of titanium dioxide nanoplate array film is obviously improved.

It is the coated titanium dioxide nanosheet film ultraviolet-visible absorption figure of selenium/cadmium sulfide laminated structure shown in Fig. 9 Spectrum, a is titanium dioxide nanoplate array film ultraviolet-visible absorption curve, and b is selenium/coated dioxy of cadmium sulfide laminated structure Change titanium nanometer sheet film ultraviolet-visible absorption curve, visible in figure, laminated film has significantly to 400-700nm visible ray Absorb, and absorptivity is significantly increased than the absorptivity of titanium dioxide nanoplate array film.

Claims (3)

  1. A kind of 1. preparation method of selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure, it is characterised in that:
    The chemical substance used is:Butyl titanate, hydrochloric acid, ammonium titanium fluoride, urea, sodium tartrate, selenium oxide, cadmium sulfate, sulphur Sodium thiosulfate, sulfuric acid, acetone, absolute ethyl alcohol, deionized water, platinized platinum, electro-conductive glass, silver chlorate;It is as follows that it combines preparation dosage: It is measurement unit with gram, milliliter, millimeter
    Preparation method is as follows:
    (1) electro-conductive glass, platinized platinum, silver chloride film are pre-processed
    1. clean electro-conductive glass
    Electro-conductive glass is placed in beaker, acetone 100mL is added, soaking and washing 15min, is dried after cleaning;
    The electro-conductive glass dried is placed in another beaker, absolute ethyl alcohol 100mL is added, soaking and washing 15min, is dried in the air after cleaning It is dry;
    The electro-conductive glass dried is placed in another beaker, deionized water 100mL is added, soaking and washing 15min, is dried in the air after cleaning It is dry;
    2. clean platinized platinum
    Platinized platinum is placed in beaker, acetone 100mL is added, soaking and washing 15min, is dried after cleaning;
    The platinized platinum dried is placed in another beaker, absolute ethyl alcohol 100mL is added, soaking and washing 15min, is dried after cleaning;
    Platinized platinum after drying is placed in another beaker, deionized water 100mL is added, soaking and washing 15min, is dried after cleaning;
    3. clean silver chloride film
    Silver chloride film is placed in beaker, acetone 100mL is added, soaking and washing 15min, is dried after cleaning;
    Silver chloride film after drying is placed in another beaker, absolute ethyl alcohol 100mL is added, soaking and washing 15min, is dried in the air after cleaning It is dry;
    Silver chloride film after drying is placed in another beaker, deionized water 100mL is added, soaking and washing 15min, is dried in the air after cleaning It is dry;
    (2) hydrothermal synthesis method prepares titanium dioxide nanoplate array film
    1. prepare reaction solution
    Deionized water 30mL ± 0.001mL, hydrochloric acid 30mL ± 0.001mL, butyl titanate 1.5mL ± 0.001mL are measured, is weighed Ammonium titanium fluoride 0.8g ± 0.001g, urea 0.8g ± 0.001g, add in beaker, stir 15min, make its dissolving, into reaction solution;
    2. the electro-conductive glass cleaned after drying is put into the liner of reactor, the reaction solution configured is poured into liner, it is close Reactor is closed, reactor is put into heating furnace, 18h is incubated at 180 DEG C;
    3. after heating and thermal insulation, reactor is taken out, is cooled to 25 DEG C;Reactor is opened, takes out electro-conductive glass and titanium dioxide thereon Titanium nano-chip arrays film;Titanium dioxide nanoplate array film by electro-conductive glass and thereon dries in the air after being cleaned with deionized water It is dry;
    4. being heat-treated, titanium dioxide nanoplate array film by electro-conductive glass and thereon is placed in quartz container, is subsequently placed in It is closed in heat-treatment furnace;Heater, 450 DEG C of heating-up temperature, 120min is incubated, then cools to 25 DEG C with the furnace;
    (3) titanium dioxide/cadmium selenide thin film is prepared
    Titanium dioxide/cadmium selenide thin film is prepared with electrochemical deposition method, titanium dioxide nanoplate battle array with electro-conductive glass and thereon Row film is working electrode, platinized platinum be reference electrode to electrode, silver chlorate, deposited on titanium dioxide nanoplate array film Cadmium selenide, titanium dioxide/cadmium selenide thin film is prepared on electro-conductive glass;
    1. selenizing cadmium electrolyte processed
    Sodium tartrate 0.194g ± 0.001g, selenium oxide 0.044g ± 0.001g, cadmium sulfate 0.248g ± 0.001g are weighed, is measured Deionized water 100mL ± 0.001mL, add in beaker, 20min is stirred, into selenizing cadmium electrolyte;
    2. electrode is installed
    In glass electrolytic cell, reference electrode silver chloride film is installed in centre position, lifted by hang spring;
    In glass electrolytic cell, in left part position installment work electrode, i.e. electro-conductive glass and titanium dioxide nanoplate battle array thereon Row film, and lifted by hang spring;
    In glass electrolytic cell, install to electrode platinized platinum in right station, lifted by hang spring;
    3. add selenizing cadmium electrolyte
    The selenizing cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, to electrode 4/5ths;
    4. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -0.9~-0.3V (relative to silver chlorate Piece current potential), sweep speed 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 300s;It is raw on working electrode electro-conductive glass Into titanium dioxide/cadmium selenide thin film;
    5. immersion, cleaning
    Titanium dioxide/cadmium selenide thin film by electro-conductive glass and thereon is placed in beaker, adds absolute ethyl alcohol 100mL, immersion 5min;
    Then titanium dioxide/cadmium selenide thin film by electro-conductive glass and thereon is placed in another beaker, adds deionized water 100mL, clean 10min;
    Dried after cleaning;
    (4) titanium dioxide/cadmium selenide/cadmium sulphide membrane is prepared
    Titanium dioxide/cadmium selenide/cadmium sulphide membrane is prepared with electrochemical deposition method, titanium dioxide with electro-conductive glass and thereon/ Cadmium selenide thin film is working electrode, platinized platinum be reference electrode to electrode, silver chlorate, on titanium dioxide/cadmium selenide thin film sink Product cadmium sulfide, prepares titanium dioxide/cadmium selenide/cadmium sulphide membrane on electro-conductive glass;
    1. formulating vulcanization cadmium electrolyte
    Sodium tartrate 0.194g ± 0.001g, sodium thiosulfate 1.28g ± 0.001g, cadmium sulfate 0.248g ± 0.001g are weighed, Deionized water 100mL ± 0.001mL is measured, is added in beaker, stirs 20min, into vulcanization cadmium electrolyte;
    2. electrode is installed
    In glass electrolytic cell, reference electrode silver chloride film is installed in centre position, lifted by hang spring;
    In glass electrolytic cell, in left part position installment work electrode, i.e. electro-conductive glass and titanium dioxide/cadmium selenide 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;
    3. add vulcanization cadmium electrolyte
    The vulcanization cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, to electrode 4/5ths;
    4. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -1.5V~0V (relative to silver chloride film Current potential), sweep speed 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 20min;Generated on working electrode electro-conductive glass Titanium dioxide/cadmium selenide/cadmium sulphide membrane;
    5. immersion, cleaning
    Titanium dioxide/cadmium selenide/cadmium sulphide membrane by electro-conductive glass and thereon is placed in beaker, adds absolute ethyl alcohol 100mL, Soak 5min;
    Then titanium dioxide/cadmium selenide/cadmium sulphide membrane by electro-conductive glass and thereon is placed in another beaker, adds deionization Water 100mL, clean 10min;
    Dried after cleaning;
    (5) selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is prepared
    Prepare selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure with electrochemical deposition method, with electro-conductive glass and Titanium dioxide/cadmium selenide/cadmium sulphide membrane thereon is working electrode, platinized platinum be reference electrode to electrode, silver chloride film, Cadmium selenide is deposited on titanium dioxide/cadmium selenide/cadmium sulphide membrane, selenium/cadmium sulfide laminated structure bag is prepared on electro-conductive glass Apply titanium dioxide nanosheet film;
    1. prepare selenizing cadmium electrolyte
    Sodium tartrate 0.194g ± 0.001g, selenium oxide 0.044g ± 0.001g, cadmium sulfate 0.248g ± 0.001g are weighed, is measured Deionized water 100mL ± 0.001mL, add in beaker, 20min is stirred, into selenizing cadmium electrolyte;
    2. electrode is installed
    In glass electrolytic cell, reference electrode silver chloride film is installed in centre position, lifted by hang spring;
    In glass electrolytic cell, in left part position installment work electrode, i.e., electro-conductive glass and titanium dioxide/cadmium selenide thereon/ Cadmium sulphide membrane, and lifted by hang spring;
    In glass electrolytic cell, install to electrode platinized platinum in right station, lifted by hang spring;
    3. add selenizing cadmium electrolyte
    The selenizing cadmium electrolyte of preparation is added in glass electrolytic cell, electrolyte will flood reference electrode, working electrode, to electrode 4/5ths;
    4. opening electrochemical workstation, using cyclic voltammetry, electric potential scanning section is -0.9~-0.3V (relative to silver chlorate Piece current potential), sweep speed 0.01V/s, 25 DEG C of electrolyte temperature, electrolysis time 150s;It is raw on working electrode electro-conductive glass Into selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure;
    5. immersion, cleaning
    Selenium by electro-conductive glass and thereon/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is placed in beaker, is added Enter absolute ethyl alcohol 100mL, soak 5min;
    Then the selenium by electro-conductive glass and thereon/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is placed in another burning In cup, deionized water 100mL is added, cleans 10min;
    Dried after cleaning;
    6. being heat-treated, selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure by electro-conductive glass and thereon is placed in In quartz container, it is subsequently placed in heat-treatment furnace, it is closed;Heater, 350 DEG C of heating-up temperature, it is incubated 120min, Ran Housui Stove is cooled to 25 DEG C;
    Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is generated on electro-conductive glass;
    (6) test, analysis and characterization
    To the selenium/pattern of the coated titanium dioxide nanosheet film of cadmium sulfide laminated structure, composition, Chemical Physics performance of preparation Carry out test, analysis and characterization;
    Morphology analysis is carried out to selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure with SEM;
    Material phase analysis is carried out to selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure with X-ray diffractometer;
    Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is carried out with ultraviolet-visible spectrophotometer ultraviolet Visible absorption is analyzed;
    Instantaneous photoresponse point is carried out to selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure with electrochemical workstation Analysis, electric current are analyzed with voltage change;
    Conclusion:Selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure is that brownish red is membranaceous, and film is by selenium/vulcanization The coated titanium dioxide nanoplate composition of cadmium laminated structure, wherein titanium dioxide nanoplate length≤3 μm, thickness≤500nm, receive Rice piece surface attachment has a cadmium sulfide and cadmium selenide particle, and cadmium selenide nano particles diameter≤40nm, cadmium sulfide particle diameter≤ 150nm, the coated titanium dioxide nanosheet film film of selenium/cadmium sulfide laminated structure have to visible ray in 400-700nm wavelength It is obvious to absorb, produce 3mA/cm under the 100W xenon lamps irradiation with cut-off λ≤420nm optical filters2Electric current;
    (7) product storage
    Amber transparent glass container is stored in selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure of preparation In, closed lucifuge storage, moistureproof, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity 10%.
  2. A kind of 2. preparation of selenium according to claim 1/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure Method, it is characterised in that:
    Described substrate is electro-conductive glass (16), be titanium dioxide nanoplate array film (17) on electro-conductive glass (16) top, It is cadmium selenide nano film (18) on titanium dioxide nanoplate array film (17) top, on cadmium selenide nano film (18) top It is cadmium selenide nano film (20) on cadmium sulfide nano-film (19) top for cadmium sulfide nano-film (19).
  3. A kind of 3. preparation of selenium according to claim 1/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure Method, it is characterised in that:
    Prepare selenium/coated titanium dioxide nanosheet film of cadmium sulfide laminated structure to carry out in electrolytic cell, be with conduction Glass and titanium dioxide/cadmium selenide/cadmium sulphide membrane electrode thereon are working electrode, platinized platinum is to be to electrode, silver chloride film Reference electrode, deposits cadmium selenide on titanium dioxide/cadmium selenide/cadmium sulphide membrane electrode in electro-conductive glass and thereon, and generation selenium/ The coated titanium dioxide nanosheet film of cadmium sulfide laminated structure;
    Electrolytic cell (6) is rectangle, and electrolytic cell (6) bottom is electrochemical workstation (1), is provided with electrochemical workstation (1) aobvious Display screen (2), indicator lamp (3), power switch (4), DC power control device (5);It is dc source on the top of electrolytic cell (6) (7);Electro-conductive glass and titanium dioxide/cadmium selenide/cadmium sulphide membrane electrode (11) thereon are provided with electrolytic cell (6) interior left part, And it is connected by the first hang spring (8) with dc source (7);Silver chloride film (12) is provided with electrolytic cell (6) interior middle part, and by Two hang springs (9) are connected with dc source (7);Platinum plate electrode (13) is provided with electrolytic cell (6) interior right part, and by the 3rd hang spring (10) It is connected with dc source (7);Magneton agitator (14) is provided with electrolytic cell (6) inner bottom part;Cadmium selenide is held in electrolytic cell (6) Electrolyte (15), selenizing cadmium electrolyte (15) will flood electro-conductive glass and titanium dioxide/cadmium selenide thereon/cadmium sulphide membrane electricity Pole (11), silver chloride film (12), 4/5ths of platinum plate electrode (13).
CN201711056273.8A 2017-11-01 Preparation method of titanium dioxide nanosheet films coated with selenium/cadmium sulfide laminated structures CN107857483B (en)

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