CN105601124A - Method for preparing porous alpha-Fe2O3 photo-anode - Google Patents

Method for preparing porous alpha-Fe2O3 photo-anode Download PDF

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Publication number
CN105601124A
CN105601124A CN201610009196.XA CN201610009196A CN105601124A CN 105601124 A CN105601124 A CN 105601124A CN 201610009196 A CN201610009196 A CN 201610009196A CN 105601124 A CN105601124 A CN 105601124A
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porous
light anode
fto
fluoride
film
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CN201610009196.XA
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CN105601124B (en
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侯乙东
郑冲
丁正新
戴文新
王心晨
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Fuzhou University
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Fuzhou University
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention discloses a method for preparing a porous alpha-Fe2O3 photo-anode and belongs to the technical field of photoelectric water decomposition. The method uses fluorine doped SnO2 conductive glass (FTO) as a substrate, a FeOOH film uniformly grows on an FTO surface through hydrothermal reaction, and then a photo-anode material of an alpha-Fe2O3 film with pores formed in the surface is prepared through microwave assisted heating. The method is simple in operation, mild in reaction condition, short in reaction period and high in repeatability, raw materials are cheap and are easy to obtain, complicated and expensive devices are not needed, the preparation cost is low, the prepared material has excellent oxygen production performance when being applied to photoelectric water decomposition, the photoelectric current density can be up to 2.4 mA/cm<2> under the simulated sunlight irradiation compared with a reversible hydrogen electrode 1.23 V, and the method has wide application prospect on the aspect of development of sustainable clean energy.

Description

One is prepared porous α-Fe2O3The method of light anode
Technical field
The invention belongs to photoelectric decomposition water technical field, be specifically related to one and prepare porousα-Fe2O3The method of light anode.
Background technology
Hydrogen is a kind of material of clean, reusable edible, is considered to a kind of desirable energy carrier, can change efficiently available available energy into and does not bring environmental problem. The hydrogen manufacturing of photoelectric decomposition water is to have one of prospect, the cleanest hydrogen production process most, but owing to dividing in photoelectrolysis in the process of water, producing oxygen process is the reaction that a relative difficult occurs, and improves this problem of hydrogen generation efficiency and is widely studied so exploitation has highly active smooth anode material. In numerous smooth anode materials,α-Fe2O3Because it has suitable band structure, sunshine good absorbing, non-toxic inexpensive and good chemical stability and receive much concern. At present, preparationα-Fe2O3The main method of light anode has aumospheric pressure cvd method, spray heating decomposition, colloidal sol spraying process etc., but prepared by these methodsα-Fe2O3Also there are some problems in light anode: as also not high in the performance of optoelectronic pole; Preparation process more complicated and costliness.
The present invention adopts the hydro-thermal method FeOOH that grows on FTO, and prepared and had cellular structure by Microwave-assisted firingα-Fe2O3Film, its safe preparation process, nontoxic and the prices of raw and semifnished materials are cheap, and it is good that resulting materials photoelectricity produces oxygen performance, is a kind of light anode material preferably.
Summary of the invention
The object of the present invention is to provide one to prepare porousα-Fe2O3The method of light anode, the method is simple, does not need complicated instrument, simple to operate in preparation process, and cost is low, is conducive to large-scale production, and prepared has a porousα-Fe2O3The light anode material of film has excellent photoelectrocatalysis and produces oxygen performance.
For achieving the above object, the present invention adopts following technical scheme:
One is prepared porousα-Fe2O3The method of light anode comprises the following steps:
1) by FTO(fluorine doping SnO2Electro-conductive glass) sheet removes chemical greasy dirt with acetone and absolute ethyl alcohol ultrasonic cleaning 20min respectively, then rinses well by deionized water, and natural air drying is stand-by;
2), using trivalent iron salt as source of iron, fluoride, as fluorine source, is mixed with and contains 0 ~ 0.5mol/LF-With 0.1 ~ 1.0mol/LFe3+Solution, then toward wherein adding titanium source, make Ti4+/Fe3+Atomic ratio be 0 ~ 0.1, stir and obtain solution A;
3) clean FTO sheet is placed in hydrothermal reaction kettle, and pours solution A in still, compactedness is controlled at 50 ~ 80%, then seal hydrothermal reaction kettle, put it in electric heating constant-temperature blowing drying box, react 4 ~ 24h at 80 ~ 120 DEG C, reaction finishes rear naturally cooling;
4) open hydrothermal reaction kettle, FTO sheet is taken out, repeatedly rinse by a large amount of deionized waters, in electric heating constant-temperature blowing drying box, at 60 ~ 100 DEG C, be dried 1 ~ 3h, must be coated with the FTO sheet of FeOOH film;
5) the FTO sheet that is coated with FeOOH film is lain in the porcelain boat that strong microwave absorption medium is housed in advance, after Microwave-assisted firing 3 ~ 20min, take out, make surface and there is porousα-Fe2O3The light anode material of film.
Step 2) described trivalent iron salt comprises ferric trichloride, ferric nitrate and ferric sulfate; Described fluoride comprises sodium fluoride, ammonium fluoride and potassium fluoride; Described titanium source comprises dichloro oxygen titanium and isopropyl titanate.
Described in step 5), strong microwave absorption medium is graphite or silicon carbide powder.
The porous that described method makesα-Fe2O3Light anode can be used for the hydrogen manufacturing of photoelectric decomposition water.
Material prepared by the present invention is porousα-Fe2O3Film, it is mainly used in the hydrogen manufacturing of photoelectric decomposition water.
Effect of the present invention and superiority are:
(1) method that the present invention adopts simple hydro-thermal and Microwave-assisted firing to combine is prepared porousα-Fe2O3Film, its preparation method is simple, easy and simple to handle, mild condition.
(2), under simulated solar irradiation irradiation, during with respect to reversible hydrogen electrode 1.23V, density of photocurrent can reach 2.4mA/cm2。
(3) preparation method of the present invention is simple, and the material obtaining is easy to application, is conducive to apply in suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the XRD figure of the light anode material prepared of embodiment 1.
Fig. 2 is porous prepared by embodiment 1α-Fe2O3The scanning electron microscope (SEM) photograph of film.
Fig. 3 is that embodiment 1 makes light anode in 1.0mol/LNaOH electrolyte solution, under illumination and the linear volt-ampere scan light electrochemical response curve of dark state.
Detailed description of the invention
In order to make content of the present invention more be convenient to understand, below in conjunction with detailed description of the invention, technical solutions according to the invention are described further, but the present invention is not limited only to this.
Embodiment 1
Porousα-Fe2O3The preparation process of light anode comprises: FTO sheet is removed to chemical greasy dirt with acetone and absolute ethyl alcohol ultrasonic cleaning 20min respectively, then rinse well by deionized water, natural air drying is stand-by; By 3.0mmol ferric trichloride, 4.0mmol potassium fluoride and 6.0μThe isopropyl titanate of mol is dissolved in 20mL deionized water; It is that 30mL liner is in the stainless steel cauldron of polytetrafluoro material that solution is transferred to volume, and a slice is of a size of to 2 × 4cm2Clean FTO sheet be placed in reactor, at 100 DEG C of reaction 10h, after reaction finishes, make it naturally cooling, product, through a large amount of deionized water washings, obtains FeOOH film after dry 2h at 80 DEG C, then is lain in the porcelain boat that graphite is housed in advance in electric heating constant-temperature blowing drying box, auxiliary heating 12min in micro-wave oven, obtains described porousα-Fe2O3Film.
Embodiment 2
Porousα-Fe2O3The preparation process of light anode comprises: FTO sheet is removed to chemical greasy dirt with acetone and absolute ethyl alcohol ultrasonic cleaning 20min respectively, then rinse well by deionized water, natural air drying is stand-by; By 15mmol ferric nitrate, 7.5mmol ammonium fluoride and 1.5mmol isopropyl titanate are dissolved in 15mL deionized water, and it is that 30mL liner is in the stainless steel cauldron of polytetrafluoro material that solution is transferred to volume, and a slice is of a size of to 2 × 4cm2Clean FTO be placed in reactor, at 80 DEG C of reaction 24h, after reaction finishes, make it naturally cooling, product, through a large amount of deionized water washings, obtains FeOOH film after dry 1h at 100 DEG C, then is lain in the porcelain boat that silicon carbide powder is housed in advance in electric heating constant-temperature blowing drying box, auxiliary heating 3min in micro-wave oven, obtains described porousα-Fe2O3Film.
Embodiment 3
Porousα-Fe2O3The preparation process of light anode comprises:: FTO sheet is removed to chemical greasy dirt with acetone and absolute ethyl alcohol ultrasonic cleaning 20min respectively, then rinse well by deionized water, natural air drying is stand-by; By 12mmol ferric trichloride, the dichloro oxygen titanium of 2.4mmol sodium fluoride and 0.3mmol is dissolved in 24mL deionized water, and it is that 30mL liner is in the stainless steel cauldron of polytetrafluoro material that solution is transferred to volume, gets a slice and is of a size of 2 × 4cm2Clean FTO be placed in reactor, at 120 DEG C of reaction 4h, after reaction finishes, make it naturally cooling, product, through a large amount of deionized water washings, obtains FeOOH film after dry 3h at 60 DEG C in electric heating constant-temperature blowing drying box, and just it lies in the porcelain boat that silicon carbide powder is housed in advance, auxiliary heating 20min in micro-wave oven, obtains described porousα-Fe2O3Film.
Prepared porousα-Fe2O3Light anode is applied to photoelectric decomposition water, the test condition of its performance: in three-electrode system, the 1.0mol/LNaOH aqueous solution is electrolyte solution,α-Fe2O3Membrane electrode is working electrode, and silver-silver chloride electrode is reference electrode, and platinum electrode is to electrode, and the sweep speed of current-voltage curve is 20mV/s; Light source is solar simulator, energy density 100mW/cm2. Sample test result as shown in Figure 3. As shown in Figure 3, porous of the present inventionα-Fe2O3Light anode is under simulated solar irradiation irradiation, and during with respect to reversible hydrogen electrode 1.23V, density of photocurrent can reach 2.4mA/cm2, illustrate that its photoelectricity produces oxygen functional.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.

Claims (4)

1. prepare porous for one kindα-Fe2O3The method of light anode, is characterized in that: comprise the following steps:
1) FTO sheet is removed to chemical greasy dirt with acetone and absolute ethyl alcohol ultrasonic cleaning 20min respectively, then rinse well by deionized water, natural air drying is stand-by;
2), using trivalent iron salt as source of iron, fluoride, as fluorine source, is mixed with and contains 0 ~ 0.5mol/LF-With 0.1 ~ 1.0mol/LFe3+Solution, then toward wherein adding titanium source, make Ti4+/Fe3+Atomic ratio be 0 ~ 0.1, stir and obtain solution A;
3) clean FTO sheet is placed in hydrothermal reaction kettle, and pours solution A in still, compactedness is controlled at 50 ~ 80%, then seal hydrothermal reaction kettle, put it in electric heating constant-temperature blowing drying box, react 4 ~ 24h at 80 ~ 120 DEG C, reaction finishes rear naturally cooling;
4) open hydrothermal reaction kettle, FTO sheet is taken out, repeatedly rinse by a large amount of deionized waters, in electric heating constant-temperature blowing drying box, at 60 ~ 100 DEG C, be dried 1 ~ 3h, must be coated with the FTO sheet of FeOOH film;
5) the FTO sheet that is coated with FeOOH film is lain in the porcelain boat that strong microwave absorption medium is housed in advance, after Microwave-assisted firing 3 ~ 20min, take out, make surface and there is porousα-Fe2O3The light anode material of film.
2. prepare according to claim 1 porousα-Fe2O3The method of light anode, is characterized in that: step 2) described trivalent iron salt comprises ferric trichloride, ferric nitrate and ferric sulfate;
Described fluoride comprises sodium fluoride, ammonium fluoride and potassium fluoride;
Described titanium source comprises dichloro oxygen titanium and isopropyl titanate.
3. prepare according to claim 1 porousα-Fe2O3The method of light anode, is characterized in that: described in step 5), strong microwave absorption medium is graphite or silicon carbide powder.
4. the porous that method makes as claimed in claim 1α-Fe2O3Light anode, is characterized in that: for the hydrogen manufacturing of photoelectric decomposition water.
CN201610009196.XA 2016-01-08 2016-01-08 One kind prepares porous α Fe2O3The method of light anode Active CN105601124B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106676565A (en) * 2016-12-09 2017-05-17 吉林大学 Fe2-xTixO3/FTO photo-anode preparing technology and treatment method capable of improving photocurrent density of photo-anode
CN106783196A (en) * 2016-11-11 2017-05-31 中山大学 A kind of preparation method of polyhedron ferric oxide nano-material
CN107268022A (en) * 2017-06-12 2017-10-20 太原理工大学 α‑Fe2O3The preparation method and application of nano stick array photo-anode material
CN107313065A (en) * 2017-07-14 2017-11-03 西南大学 Iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode and its preparation method and application
CN107313064A (en) * 2017-06-12 2017-11-03 太原理工大学 Metal boron or the α Fe of phosphide modification2O3The preparation method and application of light anode material
CN109453777A (en) * 2018-11-26 2019-03-12 中国华能集团清洁能源技术研究院有限公司 α-Fe is improved based on ternary layered double-metal hydroxide2O3The method of photoelectrocatalysis hydrogen production by water decomposition performance
CN111364050A (en) * 2020-03-11 2020-07-03 华侨大学 Preparation method of titanium-doped iron oxide photo-anode with high photoelectric water decomposition performance
CN113201766A (en) * 2021-05-06 2021-08-03 云南大学 Preparation method of hematite photoanode
CN114255999A (en) * 2021-03-08 2022-03-29 台州学院 Photo-generated anti-corrosion electrode material and preparation method and application thereof

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106783196A (en) * 2016-11-11 2017-05-31 中山大学 A kind of preparation method of polyhedron ferric oxide nano-material
CN106676565A (en) * 2016-12-09 2017-05-17 吉林大学 Fe2-xTixO3/FTO photo-anode preparing technology and treatment method capable of improving photocurrent density of photo-anode
CN107268022A (en) * 2017-06-12 2017-10-20 太原理工大学 α‑Fe2O3The preparation method and application of nano stick array photo-anode material
CN107313064A (en) * 2017-06-12 2017-11-03 太原理工大学 Metal boron or the α Fe of phosphide modification2O3The preparation method and application of light anode material
CN107313065A (en) * 2017-07-14 2017-11-03 西南大学 Iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode and its preparation method and application
CN107313065B (en) * 2017-07-14 2019-01-04 西南大学 Iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode and its preparation method and application
CN109453777A (en) * 2018-11-26 2019-03-12 中国华能集团清洁能源技术研究院有限公司 α-Fe is improved based on ternary layered double-metal hydroxide2O3The method of photoelectrocatalysis hydrogen production by water decomposition performance
CN111364050A (en) * 2020-03-11 2020-07-03 华侨大学 Preparation method of titanium-doped iron oxide photo-anode with high photoelectric water decomposition performance
CN114255999A (en) * 2021-03-08 2022-03-29 台州学院 Photo-generated anti-corrosion electrode material and preparation method and application thereof
WO2022188503A1 (en) * 2021-03-08 2022-09-15 台州学院 Photogenerated anti-corrosion electrode material and preparation method and application thereof
CN113201766A (en) * 2021-05-06 2021-08-03 云南大学 Preparation method of hematite photoanode
CN113201766B (en) * 2021-05-06 2022-03-29 云南大学 Preparation method of hematite photoanode

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