CN105140597A - Method for preparing heterojunction photoelectrode of photoelectrochomical cell through semiconductor nanomaterial recombination - Google Patents

Method for preparing heterojunction photoelectrode of photoelectrochomical cell through semiconductor nanomaterial recombination Download PDF

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CN105140597A
CN105140597A CN201510459214.XA CN201510459214A CN105140597A CN 105140597 A CN105140597 A CN 105140597A CN 201510459214 A CN201510459214 A CN 201510459214A CN 105140597 A CN105140597 A CN 105140597A
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znfe
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李亮
田维
刘琼
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Suzhou University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M14/00—Electrochemical current or voltage generators not provided for in groups H01M6/00 - H01M12/00; Manufacture thereof
    • H01M14/005—Photoelectrochemical storage cells
    • 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
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

Abstract

The invention discloses a method for preparing a heterojunction photoelectrode of a photoelectrochomical cell through semiconductor nanomaterial recombination. A synthetic iron oxide nanorod is compounded with zinc ferrite in a spinel structure to prepare a heterojunction anode. The semiconductor heterojunction photoelectrode built by the method has the effects of promoting effective separation of electron hole pairs, reducing recombination and accelerating charge transportation. According to the electrode, the defect that a single semiconductor carrier is low in migration rate can be overcome; the photoelectric conversion efficiency of the traditional single semiconductor electrode is improved; the water photolysis efficiency is improved; and the method is relatively simple in preparation method, can be produced on a large scale and has potential application value.

Description

The method of photoelectrochemical cell heterojunction photovoltaic pole is prepared by semiconductor nano material compound
Technical field
The present invention relates to a kind of preparation method of photoelectric chemical battery electrode, particularly relate to a kind of method being prepared photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound.
Background technology
Hydrogen Energy is a kind of best free of contamination green energy resource, because the product of combustion of hydrogen is water, can not have any pollution to environment.Now efficiently common hydrogen manufacturing mode mainly brine electrolysis, but this but needs extra energy, limits its development.Solar energy is a kind of inexhaustible, nexhaustible natural resources, the solar energy shining earth surface is every year equivalent to 10000 times of worldwide energy total amount consumed and 1/10 of whole world fossil energy total amount, therefore utilizes solar photolysis water hydrogen to be one of best method utilizing solar energy.And now by the photocatalysis of semi-conducting material, and the means such as assembling photoelectrochemical cell are utilize sunlight to carry out decomposition water to produce hydrogen and provide new possible approaches.
Since Fujishima and Honda of Japan in 1972 finds TiO 2can since the paper publishing of decomposition water under UV-irradiation, research different in a large number is mostly devoted to by improving light absorption and improve the efficiency that these two main aspects of carrier transport improve photocatalytic water, and prepares different semi-conducting material and nano-structure design is the important means that can realize these two kinds of demands.
Just improve light absorption aspect, the means that can carry out mainly contain: (1) band gap is modified.Adulterated by intrinsic or extrinsic doping, change the bandgap structure of material, make it the red shift of spectral absorption limit, reach the object of the more sunlights of absorption; (2) dye sensitization or quantum dot sensitized.Can extra sunlight be absorbed as dye sensitization or quantum dot sensitized material itself, thus add the light absorption of homogenous material.
Just improve carrier transport aspect, the means that can carry out have: (1) builds heterojunction.Heterojunction can utilize its internal electric field to suppress the compound of electron hole pair, accelerates the separation of charge carrier; (2) co-catalyst is modified.Co-catalyst can accelerate the reactant reaction in electronics or hole and electrolyte; (3) plasma effect.Plasma material not only can produce unnecessary hot electron, can also produce localized electromagnetic field, accelerates electron hole and is separated.
Certainly also have other means to improve close absorption and improve carrier transport ability.In brief, the electrode utilizing semi-conducting material to prepare is have very much prospect and feasible method to utilize decomposing water with solar energy hydrogen manufacturing.Believe the effort by numerous researcher, after the shortcomings such as breakthrough photocatalytic water efficiency is low, decomposing water with solar energy hydrogen manufacturing will be that future one is to the important industry of benefiting the earth.
Because above-mentioned content, the design people, actively in addition research and innovation, to founding a kind of method being prepared photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound, make it have more value in industry.
Summary of the invention
For solving the problems of the technologies described above, the object of this invention is to provide one and preparing simply, the method being prepared photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound of photocatalytic water efficiency can be improved.
A kind of method being prepared photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound that the present invention proposes, this heterojunction photovoltaic pole is by iron oxide (α-Fe 2o 3) and zinc ferrite (ZnFe 2o 4) bi-material is composited, prepares hydrogen, it is characterized in that: comprise the following steps for decomposition water:
Step (1) synthesis α-Fe 2o 3nanometer stick array;
Step (1.1) α-Fe 2o 3nanometer rods leads to many water heat transfer, by conductive substrates respectively at alcohol, and each ultrasonic cleaning 15 minutes in acetone and deionized water;
Step (1.2) is prepared by Iron(III) chloride hexahydrate, urea and the mixed uniformly aqueous solution of ammonium fluoride;
Step (1.3) measures this aqueous solution of 10mL and is positioned in the teflon-lined autoclave of 20mL volume, cleaned conductive substrates conducting surface down, be placed in this autoclave liner at a certain angle, then autoclave is heated to 120 DEG C, and react 6 hours at such a temperature, after reaction terminates, to be cooled after room temperature, take out sample;
Step (1.4) is scrubbed sample respectively in deionized water and alcohol, then dries 2 hours in 80 DEG C in atmosphere, finally in Muffle furnace, is sintering 2 hours in 550 DEG C, and then in 750 DEG C, is sintering 15 minutes, obtain required α-Fe 2o 3nanometer stick array sample;
Step (2) prepares α-Fe 2o 3and ZnFe 2o 4composite sample (α-Fe 2o 3/ ZnFe 2o 4);
Step (2.1) ZnFe 2o 4prepare by α-Fe 2o 3surface oxidation zinc annealing in process obtains, the α-Fe of synthesis in step (1.4) 2o 3nanorods Samples puts into ALD (atomic layer deposition system) reaction cavity of 200 DEG C, with diethyl zinc and H 2o respectively as zinc source and oxygen source, at α-Fe 2o 3nanorods Samples deposits ZnO;
Step (2.2) is placed in Muffle furnace sample the sintering 10 hours of annealing at 550 DEG C, after cool to room temperature, take out in sodium hydroxide solution that sample puts into 1mol/L and remove residual ZnO in 10 hours, then after rinsing in a large amount of deionized waters and washing, dry, finally obtain α-Fe 2o 3/ ZnFe 2o 4heterojunction photovoltaic pole sample.
As the further improvement of the inventive method, the conductive substrates described in step (1.1) is FTO (fluorine-doped tin oxide) electro-conductive glass.
As the further improvement of the inventive method, Iron(III) chloride hexahydrate in the aqueous solution described in step (1.2), urea and ammonium fluoride, molar concentration is 0.1mol/L.
As the further improvement of the inventive method, the ZnO deposition described in step (2.1) is at α-Fe 2o 3thickness on Nanorods Samples is 20-80 nanometer.
By such scheme, the present invention at least has the following advantages: utilize α-Fe 2o 3with ZnFe 2o 4the heterojunction photovoltaic chemical cell electrode that two kinds of semiconductor material compounds obtain, the nanorod structure of one dimension can increase the specific area of electrode, strengthens and falls into luminous effect, due to the internal electric field effect of heterojunction, outer ZnFe 2o 4electronics is transferred to α-Fe from its conduction band rapidly 2o 3conduction band, simultaneously α-Fe 2o 3the hole of valence band can be transferred to ZnFe rapidly 2o 4valence band on, then with in electrolyte reducing substances reaction.The single α of this heterojunction photovoltaic ultimate ratio-Fe 2o 3the photoelectric current under the voltage of 1.23V of nanorod electrodes improves 1.6-8 doubly.Therefore the method can overcome the shortcoming of single semiconductor especially Fe, provides practicable means for improving photocatalytic water efficiency.
The heterojunction semiconductor optoelectronic pole built by this method has promotion electron hole pair and is effectively separated, reduce the effect of compound and accelerated charge transmission, this electrode can overcome the low shortcoming of single semiconductor carriers mobility, improve traditional single semi-conducting electrode electricity conversion, improve photocatalytic water efficiency, this method preparation process is fairly simple, and can large-scale production, has potential using value.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of specification, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
SEM (scanning electron microscopy) figure of the combination electrode material structure of Fig. 1 prepared by the present invention;
Fig. 2 is the performance diagram of the light decomposition water of Different electrodes of the present invention under different voltage.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
The invention provides a kind of technology of preparing of photoelectrochemical cell decomposition water work electrode.By the method for composite semiconductor nano material during described work electrode, prepare novel photoelectric chemical battery electrode.Concrete grammar for first to synthesize α-Fe by hydro thermal method in FTO conductive substrates 2o 3nano wire rod, then passes through ALD technology at α-Fe 2o 3nanometer rods deposits ZnO, and sintering of finally annealing obtains α-Fe 2o 3/ ZnFe 2o 4heterojunction.After the electrode material of preparation is made into electrode, the work electrode as photoelectrochemical cell of use, Pt electrode is as to electrode.After illumination is mapped to work electrode, bi-material respectively oneself sends electron hole pair, and after separation, electronics passes to the H in Pt electrode and electrolyte +there is reduction reaction 2H ++ 2e -→ H 2.Reduzate in hole and electrolyte reacts.By such reaction, achieve the light-catalyzed reaction of semi-conducting material, achieve the decomposing hydrogen-production to water.
Embodiment one: by FTO (fluorine-doped tin oxide) electro-conductive glass respectively at alcohol, each ultrasonic cleaning 15 minutes in acetone and deionized water.Preparation comprises the Iron(III) chloride hexahydrate of 0.1mol/L, the Homogeneous phase mixing aqueous solution of the urea of 0.1mol/L and the ammonium fluoride of 0.1mol/L.Measure this solution of 10mL in the teflon-lined autoclave of 20mL volume, above-mentioned cleaned electro-conductive glass conducting surface down, be placed in this autoclave liner at a certain angle, then autoclave be heated to 120 DEG C, and react 6 hours at such a temperature.After reaction terminates, to be cooled after room temperature, take out sample.Finally sample being scrubbed respectively in deionized water and alcohol, dry 2 hours for 80 DEG C in then in air, finally and then sintering 15 minutes in 550 DEG C of sintering in 750 DEG C after 2 hours in Muffle furnace, obtaining required α-Fe 2o 3nanometer stick array sample.The α-Fe of above-mentioned synthesis 2o 3nanorods Samples puts into ALD (atomic layer deposition system) reaction cavity of 200 DEG C.With diethyl zinc and H 2o respectively as zinc source and oxygen source, at α-Fe 2o 3nanometer rods deposits the ZnO of 60 nanometer thickness.Then sample is annealed sintering 10 hours in Muffle furnace at 550 DEG C.After cool to room temperature, take out in sodium hydroxide solution that sample puts into 1mol/L and remove residual ZnO in 10 hours.Rinse after washing again in a large amount of deionized waters, dry, finally obtain α-Fe 2o 3/ ZnFe 2o 4heterojunction sample.Sample topography as shown in Figure 1.By the photoelectrochemical cell of this electrode assembling under the voltage of 1.23V, electric current reaches 0.29mA/cm2, and α-Fe 2o 3the electric current of nanometer rods only has 0.03mA/cm2, improves more than 8 times.
Embodiment two: by FTO (fluorine-doped tin oxide) electro-conductive glass respectively at alcohol, each ultrasonic cleaning 15 minutes in acetone and deionized water.Preparation comprises the Iron(III) chloride hexahydrate of 0.1mol/L, the Homogeneous phase mixing aqueous solution of the urea of 0.1mol/L and the ammonium fluoride of 0.1mol/L.Measure this solution of 10mL in the teflon-lined autoclave of 20mL volume, above-mentioned cleaned electro-conductive glass conducting surface down, be placed in this autoclave liner at a certain angle, then autoclave be heated to 120 DEG C, and react 6 hours at such a temperature.After reaction terminates, to be cooled after room temperature, take out sample.Finally sample being scrubbed respectively in deionized water and alcohol, dry 2 hours for 80 DEG C in then in air, finally and then sintering 15 minutes in 550 DEG C of sintering in 750 DEG C after 2 hours in Muffle furnace, obtaining required α-Fe 2o 3nanometer stick array sample.The α-Fe of above-mentioned synthesis 2o 3nanorods Samples puts into ALD (atomic layer deposition system) reaction cavity of 200 DEG C.With diethyl zinc and H 2o, respectively as zinc source and oxygen source, α-Fe2O3 nanometer rods deposits the ZnO of 40 nanometer thickness.Then sample is annealed sintering 10 hours in Muffle furnace at 550 DEG C.After cool to room temperature, take out in sodium hydroxide solution that sample puts into 1mol/L and remove residual ZnO in 10 hours.Rinse after washing again in a large amount of deionized waters, dry, finally obtain α-Fe 2o 3/ ZnFe 2o 4heterojunction sample.As shown in Figure 2, by the photoelectrochemical cell of this electrode assembling under the voltage of 1.23V, current ratio α-Fe 2o 3the electric current of nanometer rods improves more than 1.6 times.
Embodiment three: by FTO (fluorine-doped tin oxide) electro-conductive glass respectively at alcohol, each ultrasonic cleaning 15 minutes in acetone and deionized water.Preparation comprises the Iron(III) chloride hexahydrate of 0.1mol/L, the Homogeneous phase mixing aqueous solution of the urea of 0.1mol/L and the ammonium fluoride of 0.1mol/L.Measure this solution of 10mL in the teflon-lined autoclave of 20mL volume, above-mentioned cleaned electro-conductive glass conducting surface down, be placed in this autoclave liner at a certain angle, then autoclave be heated to 120 DEG C, and react 6 hours at such a temperature.After reaction terminates, to be cooled after room temperature, take out sample.Finally sample being scrubbed respectively in deionized water and alcohol, dry 2 hours for 80 DEG C in then in air, finally and then sintering 15 minutes in 550 DEG C of sintering in 750 DEG C after 2 hours in Muffle furnace, obtaining required α-Fe 2o 3nanometer stick array sample.The α-Fe of above-mentioned synthesis 2o 3nanorods Samples puts into ALD (atomic layer deposition system) reaction cavity of 200 DEG C.With diethyl zinc and H 2o respectively as zinc source and oxygen source, at α-Fe 2o 3nanometer rods deposits the ZnO of 80 nanometer thickness.Then sample is annealed sintering 10 hours in Muffle furnace at 550 DEG C.After cool to room temperature, take out in sodium hydroxide solution that sample puts into 1mol/L and remove residual ZnO in 10 hours.Rinse after washing again in a large amount of deionized waters, dry, finally obtain α-Fe 2o 3/ ZnFe 2o 4heterojunction sample.As shown in Figure 2, by the photoelectrochemical cell of this electrode assembling under the voltage of 1.23V, current ratio α-Fe 2o 3the electric current of nanometer rods improves more than 2.3 times.
The above is only the preferred embodiment of the present invention; be not limited to the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.

Claims (4)

1. prepared a method for photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound, this heterojunction photovoltaic pole is by iron oxide (α-Fe 2o 3) and zinc ferrite (ZnFe 2o 4) bi-material is composited, prepares hydrogen, it is characterized in that: comprise the following steps for decomposition water:
Step (1) synthesis α-Fe 2o 3nanometer stick array;
Step (1.1) α-Fe 2o 3nanometer rods leads to many water heat transfer, by conductive substrates respectively at alcohol, and each ultrasonic cleaning 15 minutes in acetone and deionized water;
Step (1.2) is prepared by Iron(III) chloride hexahydrate, urea and the mixed uniformly aqueous solution of ammonium fluoride;
Step (1.3) measures this aqueous solution of 10mL and is positioned in the teflon-lined autoclave of 20mL volume, cleaned conductive substrates conducting surface down, be placed in this autoclave liner at a certain angle, then autoclave is heated to 120 DEG C, and react 6 hours at such a temperature, after reaction terminates, to be cooled after room temperature, take out sample;
Step (1.4) is scrubbed sample respectively in deionized water and alcohol, then dries 2 hours in 80 DEG C in atmosphere, finally in Muffle furnace, is sintering 2 hours in 550 DEG C, and then in 750 DEG C, is sintering 15 minutes, obtain required α-Fe 2o 3nanometer stick array sample;
Step (2) prepares α-Fe 2o 3and ZnFe 2o 4composite sample (α-Fe 2o 3/ ZnFe 2o 4);
Step (2.1) ZnFe 2o 4prepare by α-Fe 2o 3surface oxidation zinc annealing in process obtains, the α-Fe of synthesis in step (1.4) 2o 3nanorods Samples puts into ALD (atomic layer deposition system) reaction cavity of 200 DEG C, with diethyl zinc and H 2o respectively as zinc source and oxygen source, at α-Fe 2o 3nanorods Samples deposits ZnO;
Step (2.2) is placed in Muffle furnace sample the sintering 10 hours of annealing at 550 DEG C, after cool to room temperature, take out in sodium hydroxide solution that sample puts into 1mol/L and remove residual ZnO in 10 hours, then after rinsing in a large amount of deionized waters and washing, dry, finally obtain α-Fe 2o 3/ ZnFe 2o 4heterojunction photovoltaic pole sample.
2. the method being prepared photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound according to claim 1, be is characterized in that: the conductive substrates described in step (1.1) is FTO (fluorine-doped tin oxide) electro-conductive glass.
3. the method being prepared photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound according to claim 1, it is characterized in that: Iron(III) chloride hexahydrate in the aqueous solution described in step (1.2), urea and ammonium fluoride, molar concentration is 0.1mol/L.
4. the method being prepared photoelectrochemical cell heterojunction photovoltaic pole by semiconductor nano material compound according to claim 1, be is characterized in that: the ZnO deposition described in step (2.1) is at α-Fe 2o 3thickness on Nanorods Samples is 20-80 nanometer.
CN201510459214.XA 2015-07-30 2015-07-30 Method for preparing heterojunction photoelectrode of photoelectrochomical cell through semiconductor nanomaterial recombination Pending CN105140597A (en)

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CN105601124A (en) * 2016-01-08 2016-05-25 福州大学 Method for preparing porous alpha-Fe2O3 photo-anode
CN106268830A (en) * 2016-08-08 2017-01-04 辽宁大学 A kind of Fe2o3/ ZnFe2o4composite photo-catalyst and its preparation method and application
CN106542498A (en) * 2016-11-25 2017-03-29 罗雷 A kind of photodissociation water installations and preparation method thereof
CN108321378A (en) * 2018-03-05 2018-07-24 西北大学 A kind of preparation method of metal oxide@metal composites/graphene nucleocapsid semi-conducting material with heterojunction boundary effect
US20230227993A1 (en) * 2022-01-18 2023-07-20 Qingdao university of technology Photoanode film for the photocathode protection and the durability improvement of a reinforcing bar in concretes, the preparation method thereof and a method of using the photoanode film for the photocathode protection and the durability improvement of a reinforcing bar in concretes

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CN105568313A (en) * 2015-12-11 2016-05-11 苏州大学 3D branch semiconductor nano heterojunction photoelectrode material and preparing method thereof
CN105601124A (en) * 2016-01-08 2016-05-25 福州大学 Method for preparing porous alpha-Fe2O3 photo-anode
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CN106268830A (en) * 2016-08-08 2017-01-04 辽宁大学 A kind of Fe2o3/ ZnFe2o4composite photo-catalyst and its preparation method and application
CN106268830B (en) * 2016-08-08 2019-01-01 辽宁大学 A kind of Fe2O3/ZnFe2O4Composite photo-catalyst and its preparation method and application
CN106542498A (en) * 2016-11-25 2017-03-29 罗雷 A kind of photodissociation water installations and preparation method thereof
CN108321378A (en) * 2018-03-05 2018-07-24 西北大学 A kind of preparation method of metal oxide@metal composites/graphene nucleocapsid semi-conducting material with heterojunction boundary effect
CN108321378B (en) * 2018-03-05 2020-04-24 西北大学 Preparation method of metal oxide @ metal compound/graphene core-shell semiconductor material with heterojunction interface effect
US20230227993A1 (en) * 2022-01-18 2023-07-20 Qingdao university of technology Photoanode film for the photocathode protection and the durability improvement of a reinforcing bar in concretes, the preparation method thereof and a method of using the photoanode film for the photocathode protection and the durability improvement of a reinforcing bar in concretes
US11761110B2 (en) * 2022-01-18 2023-09-19 Qingdao university of technology Photoanode film for the photocathode protection and the durability improvement of a reinforcing bar in concretes, the preparation method thereof and a method of using the photoanode film for the photocathode protection and the durability improvement of a reinforcing bar in concretes

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Application publication date: 20151209