CN104911629A - Synthesis method of composite electrode - Google Patents

Synthesis method of composite electrode Download PDF

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CN104911629A
CN104911629A CN201510365555.0A CN201510365555A CN104911629A CN 104911629 A CN104911629 A CN 104911629A CN 201510365555 A CN201510365555 A CN 201510365555A CN 104911629 A CN104911629 A CN 104911629A
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titanium dioxide
deionized water
fto substrate
combined electrode
graphene oxide
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CN104911629B (en
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范伟强
余小强
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Changshu intellectual property operation center Co.,Ltd.
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Jiangsu University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/133Renewable energy sources, e.g. sunlight

Abstract

The invention belongs to the technical field of photoelectrochemistry, and in particular relates to a synthesis method of a composite electrode. The synthesis method of the composite electrode comprises the following steps of: synthesizing an anatase type titanium dioxide nanowire matrix on a fluorine-doped tin oxide (FTO) substrate by a hydrothermal synthesis method; continuously growing a crystal redstone type titanium dioxide nanowire matrix on the anatase type titanium dioxide nanowire matrix by a sol-gel method; synthesizing a reduced graphene oxide film on the surface of titanium dioxide (TiO2) by a spin-coating method; and finally depositing cuprous oxide on the surface of the reduced graphene oxide film by a chemical deposition method. The titanium dioxide/reduced graphene oxide/cuprous oxide prepared by the simple hydrothermal synthesis method, sol-gel method and chemical deposition method is a composite three-dimensional photoelectrode which has the advantages of excellent chemical stability and photoelectrochemical properties. The synthesis method of the composite electrode has the advantages that the process is simple; the repeatability is high; the used materials are cheap and easily available; and the environment-friendly requirement is met.

Description

A kind of synthetic method of combined electrode
Technical field
The invention belongs to PhotoelectrochemicalTechnique Technique field, refer in particular to a kind of synthetic method of combined electrode .first hydrothermal synthesis method synthesizing anatase type titanium dioxide (TiO on FTO substrate is utilized 2) nano wire matrix, then utilize the brilliant red stone-type titanium dioxide (TiO of sol-gel method continued growth on it 2) nano wire matrix, use spin-coating method at titanium dioxide (TiO subsequently 2) surface synthesis redox graphene (RGO) film, finally on this basis by the cuprous (Cu of chemical deposition deposited oxide 2o).
Background technology
Along with the aggravation of global energy problem, as a promising solution, photoelectrochemistry hydrogen production by water decomposition, has attracted global concern; In this process, the efficiency of photo cathode and stability are the key characters in photoelectrochemistry hydrolytic process, and metal-oxide semiconductor (MOS) is because having good efficiency and the selected candidate material as photo cathode in photoelectrochemistry hydrolysis of stability.
Titanium dioxide (TiO 2) be a kind of important metal oxide semiconductor material, be widely studied and should have used light anode material, due to the physics and chemistry character of its excellence, as chemical stability, photostabilization, nontoxicity, and cheap for manufacturing cost.
Redox graphene (RGO) is a kind of material with very strong electroconductibility, and has good light stability, chemical stability, nontoxicity.
Red copper oxide (Cu 2o) be a kind of metal oxide semiconductor material typically with visible light-responded ability, due to the band gap that it is narrower, good matrix material can be formed with other materials.
Summary of the invention
The object of the present invention is to provide a kind of simple titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) synthetic method of combined electrode.
The present invention adopts liquid phase method under low temperature on FTO substrate, first prepare the titanium dioxide (TiO of the relatively homogeneous Detitanium-ore-type of pattern through hydro-thermal reaction 2) nano wire, then prepared the titanium dioxide (TiO of brilliant red stone-type again through calcining by sol-gel method 2) nano wire, then spin-coating method is at titanium dioxide (TiO 2) nanowire surface synthesizes one deck redox graphene (RGO) film, finally by chemical deposition at redox graphene surface deposition Red copper oxide (Cu 2o).
The preparation method of this combined electrode carries out according to the following step:
The concentrated hydrochloric acid of 15mL and the deionized water of 15mL are put into jar agitation by A.
B dropwise adds 0.35mL ~ 0.7mL tetra-n-butyl titanate, stirs to clarification.
The solution that step B obtains by C is transferred in the reactor of tetrafluoroethylene liner, puts into cleaned FTO substrate wherein, and be warming up to constant temperature 6h at 180 DEG C of temperature, naturally cooling, obtains anatase crystal TiO 2nano wire.
FTO substrate taking-up deionized water wash after the hydro-thermal that step C obtains by D is clean.
1mL acetic acid and 50mL ethanol are put into jar agitation by E.
F dropwise adds 0.75mL tetra-n-butyl titanate wherein, stirs to clarification.
The FTO substrate that step D obtains by G steeps the solution 1h in step F.
The FTO substrate seasoning that step G obtains by H, puts into retort furnace and is warming up to 450 DEG C of constant temperature 2h with the temperature rise rate of 2 DEG C/min, can obtain the homogeneous double-deck anatase octahedrite of pattern/brilliant red stone titanium dioxide (TiO 2) nano wire.
The clean seasoning of FTO substrate taking-up deionized water wash that step H obtains by J.
K obtains graphene oxide colloidal sol by graphene oxide powder ultrasonic dispersion deionized water.
Surface preparation has the FTO substrate of two-layer titanium dioxide to be positioned on spin coating instrument by L, graphene oxide colloidal sol is added drop-wise to the on-chip two-layer titanium dioxide of FTO on the surface, spin coating 3 ~ 5 times.
Tube furnace 400 DEG C of calcining 2h in a nitrogen atmosphere put into by FTO substrate after spin coating by M.
O step M is obtained FTO substrate immerse copper sulfate and Sulfothiorine mixing solutions, deionized water, sodium hydroxide solution and deionized water successively; Each immersion time 10 ~ 20s, circulates after 30 ~ 90 times and takes out seasoning; Titanium dioxide (the TiO that pattern is homogeneous can be obtained 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) complex light electrode.
Further, the concentration of graphene oxide colloidal sol is 1g/L.
Further, in copper sulfate and Sulfothiorine mixing solutions, the concentration of copper sulfate and Sulfothiorine is 1mol/L; The concentration of sodium hydroxide solution is also 1mol/L.
Combined electrode in the present invention thing phase, structure and performance characterization by x-ray diffractometer, field emission scanning electron microscope (SEM) measure.
Another object of the present invention, is to provide prepared titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) combined electrode is for the application of photoelectric current.
Titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) combined electrode photoelectric current test procedure under xenon source irradiates is as follows: carry out under CHI 852C type electrochemical workstation, add the sodium sulfate (Na of 0.5mol/L in electrolyzer 2sO 4) as electrolytic solution, add silver chloride electrode as reference electrode, add platinum electrode as to electrode, titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) combined electrode is as working electrode, carries out cyclic voltammetry scan.
beneficial effect
Utilize simple Hydrothermal Synthesis, sol-gel method and the titanium dioxide (TiO prepared by chemical deposition 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) for compound 3 ties up optoelectronic pole, it is good that this material has good chemical stability, the advantage that photoelectrochemical behaviour is good, and present invention process is simple, reproducible, and material therefor is cheap and easy to get, meets environmental friendliness requirement.
Accompanying drawing explanation
Fig. 1 is titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) the X-ray diffraction analysis figure (XRD) of complex light electrode, do not have the peak of other materials in x-ray diffractometer figure, this collection of illustrative plates shows, the Red copper oxide (Cu prepared by chemical deposition 2o) be pure phase Red copper oxide (Cu 2o), itself and the cuprous (Cu of standard oxidation 2o) card (06-0249) matches, and can prove wherein TiO 2/ RGO/Cu 2o is pure phase.
Fig. 2 is titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) scanning electron microscope (SEM) photograph (SEM) of complex light electrode, test shows, at room temperature, synthesized combined electrode is by the titanium dioxide (TiO of nano wire pattern 2), redox graphene (RGO) nanometer sheet, Red copper oxide (Cu 2o) nanoparticle/flower compound pattern composition, Fig. 2 (a) is double-deck TiO 2nano wire SEM schemes, and (b) is double-deck TiO 2-RGO SEM schemes, and (c) is TiO 2-Cu 2o SEM schemes, and (d) and (e) is Cu 2the TiO that O cycle index is 30 times 2-RGO-Cu 2o SEM schemes, and (f) and (g) is respectively Cu 2o cycle index 60 times and the TiO of 90 times 2-RGO-Cu 2o SEM schemes, and (h) is Cu 2the TiO that O cycle index is 60 times 2-RGO-Cu 2o cross section SEM schemes.
Fig. 3 titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) the cyclic voltammetric linear graph of complex light electrode, the bright load of linear graph stave has the combined electrode performance of three kinds of materials best, and works as Cu 2the single soak time of O is 10s, and when immersion number of times is 60 times, performance is best, and photoelectric current peak value is 0.1mA/cm 2.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, and to make those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
A kind of titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) preparation method of combined electrode carries out according to following step:
The concentrated hydrochloric acid of 15mL and the deionized water of 15mL are put into jar agitation by A.
B dropwise adds 0.35mL tetra-n-butyl titanate, stirs to clarification.
The solution that step B obtains by C is transferred in the reactor of tetrafluoroethylene liner, puts into cleaned FTO substrate wherein, and be warming up to constant temperature 6h at 180 DEG C of temperature, naturally cooling, obtains anatase crystal TiO 2nano wire.
FTO substrate taking-up deionized water wash after the hydro-thermal that step C obtains by D is clean.
1mL acetic acid and 50mL ethanol are put into jar agitation by E.
F dropwise adds 0.75mL tetra-n-butyl titanate wherein, stirs to clarification.
The FTO substrate that step D obtains by G steeps the solution 1h in step F.
The FTO substrate seasoning that step G obtains by H, puts into retort furnace and is warming up to 450 DEG C of constant temperature 2h with the temperature rise rate of 2 DEG C/min, can obtain the homogeneous double-deck anatase octahedrite of pattern/brilliant red stone titanium dioxide (TiO 2) nano wire.
The clean seasoning of FTO substrate taking-up deionized water wash that step H obtains by J.
K obtains graphene oxide colloidal sol by graphene oxide powder ultrasonic dispersion deionized water.
Surface preparation has the FTO substrate of two-layer titanium dioxide to be positioned on spin coating instrument by L, graphene oxide colloidal sol is added drop-wise to the on-chip two-layer titanium dioxide of FTO on the surface, spin coating 3 times.
Tube furnace 400 DEG C of calcining 2h in a nitrogen atmosphere put into by FTO substrate after spin coating by M.
O step M is obtained FTO substrate immerse copper sulfate and Sulfothiorine mixing solutions, deionized water, sodium hydroxide solution and deionized water successively; Each immersion time 10s, circulates after 30 times and takes out seasoning; Titanium dioxide (the TiO that pattern is homogeneous can be obtained 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) complex light electrode; The concentration of graphene oxide colloidal sol is 1g/L, and in copper sulfate and Sulfothiorine mixing solutions, the concentration of copper sulfate and Sulfothiorine is 1mol/L; The concentration of sodium hydroxide solution is also 1mol/L.
Addition through changing tetrabutyl titanate can regulate TiO 2content, regulate TiO with this 2the diameter of nano wire.
embodiment 2
A kind of titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) preparation method of combined electrode carries out according to following step:
The concentrated hydrochloric acid of 15mL and the deionized water of 15mL are put into jar agitation by A.
B dropwise adds 0.35mL tetra-n-butyl titanate, stirs to clarification.
The solution that step B obtains by C is transferred in the reactor of tetrafluoroethylene liner, puts into cleaned FTO substrate wherein, and be warming up to constant temperature 6h at 180 DEG C of temperature, naturally cooling, obtains anatase crystal TiO 2nano wire.
FTO substrate taking-up deionized water wash after the hydro-thermal that step C obtains by D is clean.
1mL acetic acid and 50mL ethanol are put into jar agitation by E.
F dropwise adds 0.75mL tetra-n-butyl titanate wherein, stirs to clarification.
The FTO substrate that step D obtains by G steeps the solution 1h in step F.
The FTO substrate seasoning that step G obtains by H, puts into retort furnace and is warming up to 450 DEG C of constant temperature 2h with the temperature rise rate of 2 DEG C/min, can obtain the homogeneous double-deck anatase octahedrite of pattern/brilliant red stone titanium dioxide (TiO 2) nano wire.
The clean seasoning of FTO substrate taking-up deionized water wash that step H obtains by J.
K obtains graphene oxide colloidal sol by graphene oxide powder ultrasonic dispersion deionized water.
Surface preparation has the FTO substrate of two-layer titanium dioxide to be positioned on spin coating instrument by L, graphene oxide colloidal sol is added drop-wise to the on-chip two-layer titanium dioxide of FTO on the surface, spin coating 5 times.
Tube furnace 400 DEG C of calcining 2h in a nitrogen atmosphere put into by FTO substrate after spin coating by M.
O step M is obtained FTO substrate immerse copper sulfate and Sulfothiorine mixing solutions, deionized water, sodium hydroxide solution and deionized water successively; Each immersion time 10s, circulates after 30 times and takes out seasoning; Titanium dioxide (the TiO that pattern is homogeneous can be obtained 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) complex light electrode.
By the thickness regulating the spin coating number of times of graphite oxide can regulate RGO nanometer sheet.
embodiment 3
The concentrated hydrochloric acid of 15mL and the deionized water of 15mL are put into jar agitation by A.
B dropwise adds 0.35mL tetra-n-butyl titanate, stirs to clarification.
The solution that step B obtains by C is transferred in the reactor of tetrafluoroethylene liner, puts into cleaned FTO substrate wherein, and be warming up to constant temperature 6h at 180 DEG C of temperature, naturally cooling, obtains anatase crystal TiO 2nano wire.
FTO substrate taking-up deionized water wash after the hydro-thermal that step C obtains by D is clean.
1mL acetic acid and 50mL ethanol are put into jar agitation by E.
F dropwise adds 0.75mL tetra-n-butyl titanate wherein, stirs to clarification.
The FTO substrate that step D obtains by G steeps the solution 1h in step F.
The FTO substrate seasoning that step G obtains by H, puts into retort furnace and is warming up to 450 DEG C of constant temperature 2h with the temperature rise rate of 2 DEG C/min, can obtain the homogeneous double-deck anatase octahedrite of pattern/brilliant red stone titanium dioxide (TiO 2) nano wire.
The clean seasoning of FTO substrate taking-up deionized water wash that step H obtains by J.
K obtains graphene oxide colloidal sol by graphene oxide powder ultrasonic dispersion deionized water.
Surface preparation has the FTO substrate of two-layer titanium dioxide to be positioned on spin coating instrument by L, graphene oxide colloidal sol is added drop-wise to the on-chip two-layer titanium dioxide of FTO on the surface, spin coating 3 times.
Tube furnace 400 DEG C of calcining 2h in a nitrogen atmosphere put into by FTO substrate after spin coating by M.
O step M is obtained FTO substrate immerse copper sulfate and Sulfothiorine mixing solutions, deionized water, sodium hydroxide solution and deionized water successively; Each immersion time 20s, circulates after 30 times and takes out seasoning; Titanium dioxide (the TiO that pattern is homogeneous can be obtained 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) complex light electrode.
By regulating the immersion time to regulate and control Cu 2the content of O.
embodiment 4
A kind of titanium dioxide (TiO 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) preparation method of combined electrode carries out according to following step:
The concentrated hydrochloric acid of 15mL and the deionized water of 15mL are put into jar agitation by A.
B dropwise adds 0.35mL tetra-n-butyl titanate, stirs to clarification.
The solution that step B obtains by C is transferred in the reactor of tetrafluoroethylene liner, puts into cleaned FTO substrate wherein, and be warming up to constant temperature 6h at 180 DEG C of temperature, naturally cooling, obtains anatase crystal TiO 2nano wire.
FTO substrate taking-up deionized water wash after the hydro-thermal that step C obtains by D is clean.
1mL acetic acid and 50mL ethanol are put into jar agitation by E.
F dropwise adds 0.75mL tetra-n-butyl titanate wherein, stirs to clarification.
The FTO substrate that step D obtains by G steeps the solution 1h in step F.
The FTO substrate seasoning that step G obtains by H, puts into retort furnace and is warming up to 450 DEG C of constant temperature 2h with the temperature rise rate of 2 DEG C/min, can obtain the homogeneous double-deck anatase octahedrite of pattern/brilliant red stone titanium dioxide (TiO 2) nano wire.
The clean seasoning of FTO substrate taking-up deionized water wash that step H obtains by J.
K obtains graphene oxide colloidal sol by graphene oxide powder ultrasonic dispersion deionized water.
Surface preparation has the FTO substrate of two-layer titanium dioxide to be positioned on spin coating instrument by L, graphene oxide colloidal sol is added drop-wise to the on-chip two-layer titanium dioxide of FTO on the surface, spin coating 5 times.
Tube furnace 400 DEG C of calcining 2h in a nitrogen atmosphere put into by FTO substrate after spin coating by M.
O step M is obtained FTO substrate immerse copper sulfate and Sulfothiorine mixing solutions, deionized water, sodium hydroxide solution and deionized water successively; Each immersion time 10s, circulates after 60 times and takes out seasoning; Titanium dioxide (the TiO that pattern is homogeneous can be obtained 2)/redox graphene (RGO)/Red copper oxide (Cu 2o) complex light electrode.
By regulating Cu 2the circulation time (respectively soaking at four beakers is once a cycle number) of O can regulate and control Cu 2the content of O.

Claims (7)

1. the synthetic method of a combined electrode, it is characterized in that: described combined electrode is that titanium dioxide/redox graphene/Red copper oxide compound 3 ties up optoelectronic pole, under employing low temperature, liquid phase method first prepares the titanium dioxide nano thread of the relatively homogeneous Detitanium-ore-type of pattern on FTO substrate through hydro-thermal reaction, then prepared the titanium dioxide nano thread of brilliant red stone-type again through calcining by sol-gel method, then spin-coating method is adopted to synthesize one deck oxidation graphene film on double-deck Detitanium-ore-type/brilliant red stone-type titanium dioxide nano thread surface that pattern is homogeneous, finally by chemical deposition at oxidation graphene film surface deposition Red copper oxide.
2. the synthetic method of a kind of combined electrode as claimed in claim 1, is characterized in that concrete steps are as follows: obtain graphene oxide colloidal sol by graphene oxide powder ultrasonic dispersion deionized water; There is the FTO substrate of double-deck Detitanium-ore-type/brilliant red stone-type titanium dioxide nano thread to be positioned on spin coating instrument surface preparation, graphene oxide colloidal sol is added drop-wise to the on-chip two-layer titanium dioxide of FTO on the surface, spin coating 3 ~ 5 times; FTO substrate after spin coating is put into tube furnace calcine in a nitrogen atmosphere; FTO substrate after calcining is immersed copper sulfate and Sulfothiorine mixing solutions, deionized water, sodium hydroxide solution and deionized water successively; Each immersion time 10 ~ 20s, circulates after 30 ~ 90 times and takes out seasoning; Pattern homogeneous titanium dioxide/redox graphene/Red copper oxide complex light electrode can be obtained.
3. the synthetic method of a kind of combined electrode as claimed in claim 2, is characterized in that: described calcining refers to 400 DEG C of calcining 2h.
4. the synthetic method of a kind of combined electrode as claimed in claim 2, is characterized in that: the concentration of graphene oxide colloidal sol is 1g/L.
5. the synthetic method of a kind of combined electrode as claimed in claim 2, is characterized in that: in copper sulfate and Sulfothiorine mixing solutions, the concentration of copper sulfate and Sulfothiorine is 1mol/L; The concentration of sodium hydroxide solution is also 1mol/L.
6. the synthetic method of a kind of combined electrode as claimed in claim 2, is characterized in that: the FTO substrate after calcining is immersed copper sulfate and Sulfothiorine mixing solutions, deionized water, sodium hydroxide solution and deionized water successively; Each immersion time 10s, circulates after 60 times and takes out seasoning.
7. as claimed in claim 1 or 2 the combined electrode prepared of preparation method in photoelectrochemistry hydrolysis reaction as the purposes of working electrode.
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CN108546959A (en) * 2018-05-22 2018-09-18 广东工业大学 A kind of reduction-state graphene oxide and preparation method thereof
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CN115165991B (en) * 2022-07-06 2023-11-07 岭南师范学院 Preparation method of reduced glutathione photoelectrochemical sensor

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