CN103088381A - Preparation method of zinc-modified tungsten trioxide thin film photoelectrode - Google Patents

Preparation method of zinc-modified tungsten trioxide thin film photoelectrode Download PDF

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CN103088381A
CN103088381A CN2013100334597A CN201310033459A CN103088381A CN 103088381 A CN103088381 A CN 103088381A CN 2013100334597 A CN2013100334597 A CN 2013100334597A CN 201310033459 A CN201310033459 A CN 201310033459A CN 103088381 A CN103088381 A CN 103088381A
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film
electrode
zinc
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刘丽英
刘润
王萍
徐铸德
许宜铭
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Zhejiang University ZJU
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Abstract

The invention discloses a preparation method of a zinc-modified tungsten trioxide thin film photoelectrode, belonging to the field of preparation of inorganic photoelectrode materials. The preparation method disclosed by the invention is characterized by taking ITO (indium tin oxide) conductive glass as a substrate, taking an amorphous tungsten oxide thin film prepared by adopting an electrodeposition method as a basal body, uniformly modifying zinc on the amorphous tungsten oxide thin film through an impregnation method, and then performing heat treatment at a certain temperature in the air to obtain a novel zinc-modified tungsten trioxide thin film photoelectrode material. After the WO3 is modified by the Zn, a layer of ZnO thin film is formed on the surface of the WO3; and as the position of a valence band of the ZnO is more negative in comparison with the WO3, when light irradiates the thin film electrode, a photohole in the valence band of the WO3 can flow into the valance band of the ZnO under the action of electric field force, thus the compounding of photo-induced electrons of the WO3 and the hole is inhibited, and the purpose of improving photoelectric conversion efficiency and photoelectric catalysis capability is achieved. The preparation method disclosed by the invention has the advantages that the prepared thin film is uniform and good in adhesion with the substrate; and equipment adopted by the preparation method is simple, easy to operate, low in cost, environment-friendly and the like.

Description

A kind of preparation method of Zinc modified WO 3 film optoelectronic pole
Technical field
The present invention relates to a kind of method of Zinc modified WO 3 film optoelectronic pole, belong to inorganic photoelectric material fabricating technology field.Be specifically related to a kind ofly have higher photoelectric current and dyestuff is had the preparation method of the Zinc modified WO 3 film optoelectronic pole of high photoelectric catalytically active under simulated solar irradiation.
Background technology
Along with growth and the people of world population are more and more higher to the requirement of material biological level, the mankind increase sharply to degree of dependence and the demand of the energy, have caused the violent decline of fossil oil storage capacity on the earth, and have produced serious environmental problem.Therefore developing high-level efficiency, less energy-consumption, cleaning, can realizing the Energy conversion of suitability for industrialized production and pollute treatment technology is the target that national governments and scientists are pursued and paid close attention to.Through the research over more than 40 years and exploration, scientists has been focused on semi-conductor this class and has been had on excellent absorbing properties and stable physical and chemical performance material.Japanese scholars Fujishima in 1972 and Honda adopt monocrystalline n-TiO 2Carry out the success of solar energy photocatalytic hydrogen production by water decomposition, opened the prelude of conductor photocatalysis research, also make people recognize that solar energy converting is the application prospect of electric energy and chemical energy.Subsequently, Carey equals to report under the irradiation of UV-light in 1976, TiO 2Polychlorobiphenyl in suspension liquid gets final product whole dechlorinations through half an hour, and since then, semiconductor photoelectrode hydrogen production by water decomposition and photochemical catalytic oxidation are applied to water and pollute the extensive concern that process field causes numerous researchers.
At present, be titanium dioxide (TiO at optoelectronic pole Material Field most study 2), but TiO 2Belong to wide bandgap semiconductor, its energy gap (Eg) is 3.2eV, and corresponding photoabsorption sideband is 400nm, only has to be mapped to TiO more than or equal to the illumination of Eg when energy 2The time, can produce electron-hole (e --h +) right, so the utilization of sunlight is only limited to the ultraviolet region, and the UV-light part of the arrival earth only accounts for the 3%-4% of sunlight, has limited significantly TiO 2Application in the actual production life.The semiconductor material that research and comparison is many in addition is tungstic oxide (WO 3), as far back as 1976, Hodes etc. have published an article on the Nature magazine proved WO 3And TiO 2Equally can be used as photocatalyst and be used for PhotoelectrochemicalSystem System for Hydrogen Production.WO 3Not only have advantages of cheapness, the physicochemical property such as nontoxic, stable aspects, and have very strong photoelectric response ability.Although WO 3Have above advantage, but in practical study is used, WO 3There are two large restriction problems.The first, WO 3Energy gap is 2.5ev-2.8ev, and corresponding photoabsorption sideband is 440nm-500nm, has still limited it to arriving the utilization of earth surface sunlight; The second, WO 3Middle exciton diffusion length is shorter, e -And h +Can only move in the finite space, cause e --h +Right recombination rate is very high, and corresponding photoelectric transformation efficiency (IPCE) is very low.
In order to improve WO 3Photoelectrochemical behaviour, modification is a kind of important means.Usually the modification mode that adopts has: (1) is at WO 3Upper carried noble metal simple substance, as Pt, Ag, Au, Pd etc., but obviously precious metal is more expensive, is unfavorable for scale operation; (2) at WO 3Appropriate metal ion or the nonmetallic ion of doping in body, this method cost is relatively low, but atom doped amount is wayward, and when doping is high, can introduce more oxygen defect on the contrary, cause the electron-hole pair composite efficiency higher; (3) with WO 3Compound with other semiconductor materials, this method is utilized the energy band structure characteristics between semi-conductor, by the transfer in electronics or hole, makes effectively being separated of electron-hole.The present invention namely adopts (3) to plant the modification mode, and concrete grammar is with Zn (NO 3) 2Be starting material, adopt pickling process that zine ion is dispersed on tungsten oxide film, through Overheating Treatment, obtain at last ZnO/WO 3The compound film optoelectronic pole material.This kind method is simple, easy to operate, and with low cost, and parameter is easy to control.Zn modifies WO 3Afterwards at WO 3The surface formed the layer of ZnO film, due to valence band location and the WO of ZnO 3Compare more negative, when illumination is mapped to membrane electrode, WO 3Photohole on valence band can flow in the valence band of ZnO under the effect of electrical forces, thereby has suppressed WO 3Light induced electron and hole compound reached the purpose that improves photoelectric transformation efficiency and photoelectrocatalysis ability.
The background technology reference
[1] Fujishima, A.; Honda, K. Nature, 1972, 238(5358): 37-38.
[2] Carey, J. H.; Lawrence, J.; Tosine, H. M. Bull. Environ. Contam. Toxieol. 1976, 16(6): 697-701.
[3] Hodes, G.; Cahen, D.; Manassen, J.; Nature,1976, 260(5549): 312 -313.
[4] Elzovic, N. R.; Babic, B. M.; Ercius, P.; et al. Appl. Catal. B-Environmental, 2012, 125: 390-397.
[5] Arait, T.; Horiguchi, M.; Yamagoda, M.; et al. J. Phys. Chem. C, 2009, 113(16): 6602-6609.
Summary of the invention
The object of the invention is to the shortcoming and defect for prior art, a kind of preparation method of Zinc modified tungstic oxide optoelectronic pole is provided.
The preparation method of Zinc modified tungstic oxide optoelectronic pole comprises the steps:
1) with the Na of 0.0025 ~ 0.0100mol 2WO 4Be dissolved in the distilled water of 50mL, adding 0.25 ~ 1.00mL mass percent concentration is 30% H 2O 2Solution stirred 3 ~ 5 minutes, obtained containing W 2O 7 2-Solution, add the ethylene glycol of 30mL, stir 1 ~ 3min, obtain mixing solutions, regulate pH value to 1.10 ~ 1.30 with perchloric acid or the nitric acid of 2mol/L, add distilled water to make the volume of mixing solutions reach 100mL, the electrolytic solution that obtains clarifying; Take the ITO conductive glass as working electrode, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, be placed in electrolytic solution and carry out galvanic deposit, cathode potential with respect to saturated calomel electrode is-0.4V ~-0.6V, depositing time is 60 minutes, dries, obtain amorphous oxidation W film, standby;
2) amorphous oxidation W film is placed in the Zn (NO of 0.005mol/L 3) 2Flooded in solution 20 ~ 40 minutes, and used distilled water flushing 1 ~ 2 minute, naturally dry in air, obtain Zinc modified tungsten oxide film;
3) Zinc modified tungsten oxide film is placed in retort furnace, 450 oUnder C, high-temperature heat treatment is 3 hours, and is cooling, obtains Zinc modified WO 3 film optoelectronic pole.
The method of the invention utilizes zinc nitrate to be starting material, adopts pickling process that zinc is dispersed on tungsten oxide film, through Overheating Treatment, obtains at last ZnO/WO 3The compound film optoelectronic pole material.This kind method is simple, easy to operate, and with low cost, and parameter is easy to control.Zn modifies WO 3Afterwards at WO 3The surface formed the layer of ZnO film, due to valence band location and the WO of ZnO 3Compare more negative, when illumination is mapped to membrane electrode, WO 3Photohole on valence band can flow in the valence band of ZnO under the effect of electrical forces, thereby has suppressed WO 3Light induced electron and hole compound reached the purpose that improves photoelectric transformation efficiency and photoelectrocatalysis ability.The present invention adopts electrochemical deposition method to prepare tungsten oxide film, and experimental installation is simple, carry out under normal temperature and pressure, parameter is easy to control, cost is low, green, high repeatability and other advantages, is expected to realize suitability for industrialized production.
The Zinc modified WO 3 film optoelectronic pole of gained is compared with pure tungstic oxide, and its photoelectric current and photoelectrocatalysis efficient all increase significantly.
Description of drawings
Fig. 1 is the embodiment 4 Zinc modified tungstic oxides of gained (a) and pure tungstic oxide (WO 3) X-ray diffracting spectrum of film photoelectric electrode;
Fig. 2 is the embodiment 4 Zinc modified tungstic oxides of gained (a) and pure tungstic oxide (WO 3) the steady-state light current density comparison diagram of film photoelectric electrode under impressed voltage 0.8V vs. SCE;
Fig. 3 is the embodiment 4 Zinc modified tungstic oxides of gained (a) and pure tungstic oxide (WO 3) the PhotoelectrocatalytiPerformance Performance comparison diagram of film photoelectric electrode;
Fig. 4 is the photoelectrochemistry mechanism figure of Zinc modified tungstic oxide and pure WO 3 film optoelectronic pole.
Embodiment
Embodiment 1
1) with the Na of 0.0025mol 2WO 4Be dissolved in the distilled water of 50mL, adding the 0.25mL mass percent concentration is 30% H 2O 2Solution stirred 3 minutes, obtained containing W 2O 7 2-Solution, add the ethylene glycol of 30mL, stir 1min, obtain mixing solutions, regulate pH value to 1.10 with the perchloric acid of 2mol/L, add distilled water to make the volume of mixing solutions reach 100mL, the electrolytic solution that obtains clarifying; Take the ITO conductive glass as working electrode, platinum plate electrode is to electrode, and saturated calomel electrode is reference electrode, being placed in electrolytic solution and carrying out galvanic deposit, is-0.4V that depositing time is 60 minutes with respect to the cathode potential of saturated calomel electrode, dry, obtain amorphous oxidation W film, standby;
2) amorphous oxidation W film is placed in the Zn (NO of 0.005mol/L 3) 2In solution, dipping is 20 minutes, uses distilled water flushing 1 minute, naturally dries in air, obtains Zinc modified tungsten oxide film;
3) Zinc modified tungsten oxide film is placed in retort furnace, 450 oUnder C, high-temperature heat treatment is 3 hours, and is cooling, obtains Zinc modified WO 3 film optoelectronic pole.
Embodiment 2
1) with the Na of 0.0100mol 2WO 4Be dissolved in the distilled water of 50mL, adding the 1.00mL mass percent concentration is 30% H 2O 2Solution stirred 5 minutes, obtained containing W 2O 7 2-Solution, add the ethylene glycol of 30mL, stir 1 ~ 3min, obtain mixing solutions, regulate pH value to 1.30 with the nitric acid of 2mol/L, add distilled water to make the volume of mixing solutions reach 100mL, the electrolytic solution that obtains clarifying; Take the ITO conductive glass as working electrode, platinum plate electrode is to electrode, and saturated calomel electrode is reference electrode, being placed in electrolytic solution and carrying out galvanic deposit, is-0.6V that depositing time is 60 minutes with respect to the cathode potential of saturated calomel electrode, dry, obtain amorphous oxidation W film, standby;
2) amorphous oxidation W film is placed in the Zn (NO of 0.005mol/L 3) 2In solution, dipping is 40 minutes, uses distilled water flushing 2 minutes, naturally dries in air, obtains Zinc modified tungsten oxide film;
3) Zinc modified tungsten oxide film is placed in retort furnace, 450 oUnder C, high-temperature heat treatment is 3 hours, and is cooling, obtains Zinc modified WO 3 film optoelectronic pole.
Embodiment 3
1) with the Na of 0.0050mol 2WO 4Be dissolved in the distilled water of 50mL, adding the 0.25mL mass percent concentration is 30% H 2O 2Solution stirred 4 minutes, obtained containing W 2O 7 2-Solution, add the ethylene glycol of 30mL, stir 1min, obtain mixing solutions, regulate pH value to 1.20 with perchloric acid or the nitric acid of 2mol/L, add distilled water to make the volume of mixing solutions reach 100mL, the electrolytic solution that obtains clarifying; Take the ITO conductive glass as working electrode, platinum plate electrode is to electrode, and saturated calomel electrode is reference electrode, being placed in electrolytic solution and carrying out galvanic deposit, is-0.5V that depositing time is 60 minutes with respect to the cathode potential of saturated calomel electrode, dry, obtain amorphous oxidation W film, standby;
2) amorphous oxidation W film is placed in the Zn (NO of 0.005mol/L 3) 2In solution, dipping is 30 minutes, uses distilled water flushing 1 minute, naturally dries in air, obtains Zinc modified tungsten oxide film;
3) Zinc modified tungsten oxide film is placed in retort furnace, 450 oUnder C, high-temperature heat treatment is 3 hours, and is cooling, obtains Zinc modified WO 3 film optoelectronic pole.
Embodiment 4
1) with the Na of 0.0025mol 2WO 4Be dissolved in the distilled water of 50mL, adding the 0.25mL mass percent concentration is 30% H 2O 2Solution stirred 3 minutes, obtained containing W 2O 7 2-Solution, add the ethylene glycol of 30mL, stir 2min, obtain mixing solutions, regulate pH value to 1.20 with the nitric acid of 2mol/L, add distilled water to make the volume of mixing solutions reach 100mL, the electrolytic solution that obtains clarifying; Take the ITO conductive glass as working electrode, platinum plate electrode is to electrode, and saturated calomel electrode is reference electrode, being placed in electrolytic solution and carrying out galvanic deposit, is-0.6V that depositing time is 60 minutes with respect to the cathode potential of saturated calomel electrode, dry, obtain amorphous oxidation W film, standby;
2) amorphous oxidation W film is placed in the Zn (NO of 0.005mol/L 3) 2In solution, dipping is 30 minutes, uses distilled water flushing 1 minute, naturally dries in air, obtains Zinc modified tungsten oxide film;
3) Zinc modified tungsten oxide film is placed in retort furnace, 450 oUnder C, high-temperature heat treatment is 3 hours, and is cooling, obtains Zinc modified WO 3 film optoelectronic pole.
Embodiment 5
1) with the Na of 0.075mol 2WO 4Be dissolved in the distilled water of 50mL, adding the 0.75mL mass percent concentration is 30% H 2O 2Solution stirred 4 minutes, obtained containing W 2O 7 2-Solution, add the ethylene glycol of 30mL, stir 1min, obtain mixing solutions, regulate pH value to 1.20 with the perchloric acid of 2mol/L, add distilled water to make the volume of mixing solutions reach 100mL, the electrolytic solution that obtains clarifying; Take the ITO conductive glass as working electrode, platinum plate electrode is to electrode, and saturated calomel electrode is reference electrode, being placed in electrolytic solution and carrying out galvanic deposit, is-0.5V that depositing time is 60 minutes with respect to the cathode potential of saturated calomel electrode, dry, obtain amorphous oxidation W film, standby;
2) amorphous oxidation W film is placed in the Zn (NO of 0.005mol/L 3) 2In solution, dipping is 30 minutes, uses distilled water flushing 1 minute, naturally dries in air, obtains Zinc modified tungsten oxide film;
3) Zinc modified tungsten oxide film is placed in retort furnace, 450 oUnder C, high-temperature heat treatment is 3 hours, and is cooling, obtains Zinc modified WO 3 film optoelectronic pole.
Photoelectric current test experiments of the present invention: improve a lot in order to prove the photoelectric current after Zinc modified WO 3 film optoelectronic pole, the present invention has carried out under simulated solar irradiation, adds as the experiment of testing transient photoelectric current under 0.8V vs. SCE voltage outward.Experiment is carried out in the threeway electrolyzer, and light source is 500W xenon lamp (Science and Technology Ltd. is freely opened up in Beijing), and the intensity of light source is 4.0mw/cm 2, the electrochemical workstation model is CHI650(Shanghai occasion China instrument company).By the density of photocurrent value that records with the reflection photoelectric transformation efficiency, in Fig. 3, sample is respectively Zinc modified tungstic oxide optoelectronic pole in pure tungstic oxide and embodiment 4, can be found out by transient current density value in figure: the density of photocurrent value of the tungstic oxide after Zinc modified is 3.5 times of pure tungstic oxide.
Photoelectrocatalysis experiment of the present invention: improve a lot in order to prove the photoelectric catalytically active after Zinc modified WO 3 film optoelectronic pole, the present invention has carried out under simulated solar irradiation, the photoelectrocatalysis experiment of the Victoria Green WPB (MG) of degraded 10mg/L under impressed voltage 0.8V vs. SCE, light source is 500W xenon lamp (Science and Technology Ltd. is freely opened up in Beijing), and the electrochemical workstation model is CHI650(Shanghai occasion China instrument company).The variation of the uv-vis spectra absorption value by MG characterizes its degradation rate, and to degradation time T mapping, the slope that obtains degrading comes photoelectrocatalysis efficient more both with ln (Co/C).In Fig. 3, sample is respectively Zinc modified WO 3 film optoelectronic pole in pure tungstic oxide and embodiment 4, and as can be seen from the figure: the degradation effect to MG that Zinc modified WO 3 film optoelectronic pole reaches (slope is 0.0214) is 2 times of the degradation effect to MG (slope is 0.0111) that reaches of pure tungstic oxide.
Photoelectric current and the PhotoelectrocatalytiPerformance Performance that can prove the WO 3 film optoelectronic pole after Zinc modified all increase significantly, and efficiently solve the photoelectric properties of tungstic oxide and to light utilization efficiency problem on the low side all.

Claims (1)

1. the preparation method of a Zinc modified tungstic oxide optoelectronic pole, is characterized in that comprising the steps:
1) with the Na of 0.0025 ~ 0.0100mol 2WO 4Be dissolved in the distilled water of 50mL, adding 0.25 ~ 1.00mL mass percent concentration is 30% H 2O 2Solution stirred 3 ~ 5 minutes, obtained containing W 2O 7 2-Solution, add the ethylene glycol of 30mL, stir 1 ~ 3min, obtain mixing solutions, regulate pH value to 1.10 ~ 1.30 with perchloric acid or the nitric acid of 2mol/L, add distilled water to make the volume of mixing solutions reach 100mL, the electrolytic solution that obtains clarifying; Take the ITO conductive glass as working electrode, platinum plate electrode is to electrode, saturated calomel electrode is reference electrode, be placed in electrolytic solution and carry out galvanic deposit, cathode potential with respect to saturated calomel electrode is-0.4V ~-0.6V, depositing time is 60 minutes, dries, obtain amorphous oxidation W film, standby;
2) amorphous oxidation W film is placed in the Zn (NO of 0.005mol/L 3) 2Flooded in solution 20 ~ 40 minutes, and used distilled water flushing 1 ~ 2 minute, naturally dry in air, obtain Zinc modified tungsten oxide film;
3) Zinc modified tungsten oxide film is placed in retort furnace, 450 oUnder C, high-temperature heat treatment is 3 hours, and is cooling, obtains Zinc modified WO 3 film optoelectronic pole.
CN2013100334597A 2013-01-29 2013-01-29 Preparation method of zinc-modified tungsten trioxide thin film photoelectrode Pending CN103088381A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103774196A (en) * 2014-01-14 2014-05-07 浙江大学 Tungsten trioxide photoelectrode with surface modified by europium and preparation method thereof
CN105107519A (en) * 2015-09-11 2015-12-02 辽宁石油化工大学 Method for synthetizing tungstate/tungsten oxide heterojunction photocatalyst in situ
CN106757123A (en) * 2016-12-23 2017-05-31 温州大学 A kind of WO of bipyridyl cobalt modification3The preparation method of nanometer sheet optoelectronic pole
CN106881078A (en) * 2017-01-22 2017-06-23 天津大学 Z-type junction ZnO-WO3Electrode, preparation method thereof and application thereof in photoelectrocatalysis

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CN101162780B (en) * 2007-11-22 2010-05-19 华南师范大学 Direct methanol fuel battery anode catalyst and method for producing the same
CN102691071A (en) * 2012-06-01 2012-09-26 浙江大学 Preparation method for iron-doped tungsten trioxide photoelectrode

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103774196A (en) * 2014-01-14 2014-05-07 浙江大学 Tungsten trioxide photoelectrode with surface modified by europium and preparation method thereof
CN105107519A (en) * 2015-09-11 2015-12-02 辽宁石油化工大学 Method for synthetizing tungstate/tungsten oxide heterojunction photocatalyst in situ
CN106757123A (en) * 2016-12-23 2017-05-31 温州大学 A kind of WO of bipyridyl cobalt modification3The preparation method of nanometer sheet optoelectronic pole
CN106757123B (en) * 2016-12-23 2018-10-02 温州大学 A kind of WO of bipyridyl-cobalt modification3The preparation method of nanometer sheet optoelectronic pole
CN106881078A (en) * 2017-01-22 2017-06-23 天津大学 Z-type junction ZnO-WO3Electrode, preparation method thereof and application thereof in photoelectrocatalysis
CN106881078B (en) * 2017-01-22 2019-07-26 天津大学 Z-type junction ZnO-WO3Electrode, preparation method thereof and application thereof in photoelectrocatalysis

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Application publication date: 20130508