CN104928648A - Zinc oxide photo-anode film and preparation method and application thereof - Google Patents
Zinc oxide photo-anode film and preparation method and application thereof Download PDFInfo
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- CN104928648A CN104928648A CN201510404103.9A CN201510404103A CN104928648A CN 104928648 A CN104928648 A CN 104928648A CN 201510404103 A CN201510404103 A CN 201510404103A CN 104928648 A CN104928648 A CN 104928648A
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- 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
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Abstract
Disclosed is a zinc oxide photo-anode film. A zinc oxide photo-anode is manufactured on a substrate with a deposited FTO by means of the organometallic chemistry gas deposition technology, the photoelectrochemical properties of the photo-anode are improved by changing the deposition time and the B2H6 doping flow, and the MOCVD-ZnO is used as the photo-anode for electrolysis of water to obtain the higher photocurrent density. The zinc oxide photo-anode film has the advantages that the preparation method is simple in technology, the deposition temperature is low, the preparation time is short, implementation is easy and repeatability is good; the obtained ZnO photo-anode film has the pyramid-like appearance, incident light absorption of the ZnO photo-anode can be improved, and then incident light utilization of the photo-anode is improved; the zinc oxide photo-anode film is used as the photo-anode of a photoelectrochemical cell, the universality of the ZnO photo-anode can be improved, and industrial production is facilitated.
Description
Technical field
The present invention relates to the method for photoelectrochemistry water decomposition hydrogen manufacturing, particularly a kind of zinc oxide photo-anode film and its preparation method and application.
Background technology
Sun power is utilized to be considered to solve a kind of effective way of future source of energy crisis.The core component of photoelectrochemistry (PEC) battery is semiconductor photoelectrode, is mainly divided into light anode and photocathode.Both all exist as light absorbing zone, and the oxygenizement utilizing photohole to carry out water unlike the former generates oxygen, and the reductive action that the latter utilizes light induced electron to carry out water generates hydrogen.TiO
2, ZnO, FeO
3and WO
3exist mainly as light anode in PEC structure Deng metal oxide.By means of favourable band gap locations, high photochemical activity, large reserves, low cost and the advantage such as nontoxic, ZnO film has been widely used in light anode.
But current zinc oxide technology of preparing is mainly limited to chemical solution method.Comprise the method etc. utilizing hydrothermal method, Best-Effort request method and electroless plating inculating crystal layer to combine with electrochemically aided deposition.Although these methods all improve the PEC performance of ZnO, its preparation method is more loaded down with trivial details, and cost is higher and be unfavorable for the extensive deposition of film, so have considerable influence for the universality of ZnO photo-anode material.Therefore, we are badly in need of a kind of method finding new making ZnO light anode material.
Summary of the invention
Object of the present invention is exactly for above-mentioned Problems existing, a kind of zinc oxide photo-anode film and its preparation method and application is provided, this preparation method utilizes Metalorganic Chemical Vapor Deposition (MOCVD) on FTO substrate, prepare zinc oxide light anode, have on the basis of better photoelectrochemical cell performance in guarantee, triviality prepared by reduction zinc oxide light anode and production cost, realize the extensive deposition of zinc oxide light anode, its preparation method technique be simple, depositing temperature is low, preparation time is short, easy to implement and better repeated.
Technical scheme of the present invention:
A kind of zinc oxide photo-anode film, utilize MOCVD technology in the FTO substrate surface deposition preparation of matte, wherein the thickness of FTO layer is 600nm, and centimetre resistance is 20 Ω, optical band gap is 2eV; The thickness of zinc oxide photo-anode film is that 1.5-7.5 μm, centimetre resistance is 500 Ω, optical band gap width is 3.2eV.
A preparation method for described zinc oxide photo-anode film, with zinc class source liquid for zinc ethyl (DEZn) ﹑ oxygen class source liquid is that water ﹑ doped source gas is for B
2h
6, carrier gas carries gas and is Ar gas, comprises the following steps:
1) FTO substrate is placed in the container ultrasonic cleaning 30min that purity is the dehydrated alcohol of 99.7%, utilizes high-purity N afterwards
2dry up, and on FTO substrate, reserve the electric transmission electrode not depositing ZnO with high temperature gummed tape;
2) by above process after FTO sample be positioned over deposit film in the chamber of single chamber MOCVD depositing system, the base vacuum of chamber is 0.03Torr, the vacuum tightness of chamber is 1Torr, depositing temperature is 155 DEG C, zinc ethyl (DEZn) flow is 180sccm, H
2o flow is 110sccm, impurity gas B
2h
6original dilution ratio be 1%, diluent gas is H
2, B
2h
6flow is 0-7sccm, depositing time is 25-175min, ZnO film thickness is 1.5-7.5 μm, obtained " pyramid-like " shape zinc oxide photo-anode film on matte FTO substrate.
A kind of application of described zinc oxide photo-anode film, light anode as photoelectrochemical cell the is used for light anode PEC brine electrolysis that is substrate with matte FTO, time of photoelectrochemical cell very platinum filament, reference electrode be Ag/AgCl solution, the NaSO of electrolytic solution to be concentration be 0.5M
4solution and utilize the NaOH solution of 0.01M its pH to be adjusted to 7, test area is 0.2826cm
2, light intensity is 100mW/cm
2.
Advantage of the present invention and positively effect are:
This preparation method's technique is simple, depositing temperature is low, preparation time is short, easy to implement and better repeated; The ZnO photo-anode film of preparation has " pyramid-like " shape pattern and can improve the absorption of ZnO photo-anode to incident light, and then increases light anode to the utilization of incident light; Its light anode as photoelectrochemical cell is used for light anode electrolysis water, can improve the universality of ZnO photo-anode.
Accompanying drawing explanation
Fig. 1 is the surface topography of zinc oxide light anode prepared by the method.
Fig. 2 is the process schematic that the method prepares zinc oxide light anode light PEC brine electrolysis.
Fig. 3 is the density of photocurrent curve that the method prepares zinc oxide light anode.
Embodiment
Embodiment 1:
A kind of zinc oxide photo-anode film, utilize MOCVD technology in the FTO substrate surface deposition preparation of matte, wherein the thickness of FTO layer is 600nm, and centimetre resistance is 20 Ω, optical band gap is 2eV; The thickness of ZnO photo-anode film is that 1.5-7.5 μm, centimetre resistance is 500 Ω, optical band gap width is 3.2eV; Its preparation method is for zinc ethyl (DEZn) ﹑ oxygen class source liquid is that water ﹑ doped source gas is for B with zinc class source liquid
2h
6, carrier gas carries gas and is Ar gas, comprises the following steps:
1) FTO substrate is placed in the container ultrasonic cleaning 30min that purity is the dehydrated alcohol of 99.7%, utilizes high-purity N afterwards
2dry up, and on FTO substrate, reserve the electric transmission electrode not depositing ZnO with high temperature gummed tape;
2) by above process after FTO sample be positioned over deposit film in the chamber of single chamber MOCVD depositing system, the base vacuum of chamber is 0.03Torr, the vacuum tightness of chamber is 1Torr, depositing temperature is 155 DEG C, zinc ethyl (DEZn) flow is 180sccm, H
2o flow is 110sccm, depositing time is 25min, ZnO film thickness is 1.5 μm, obtained " pyramid-like " shape zinc oxide (ZnO) photo-anode film on matte FTO substrate.
Fig. 1 is the surface topography of zinc oxide light anode prepared by the method, shows in figure: MOCVD is sharp-pointed pyramid shape at the surface topography of FTO deposited on substrates zinc oxide sample.
The application of prepared zinc oxide photo-anode film, light anode as photoelectrochemical cell the is used for light anode PEC brine electrolysis that is substrate with matte FTO, time of photoelectrochemical cell very platinum filament, reference electrode be Ag/AgCl solution, the NaSO of electrolytic solution to be concentration be 0.5M
4solution and utilize the NaOH solution of 0.01M its pH to be adjusted to 7, test area is 0.2826cm
2, light intensity is 100mW/cm
2.
Fig. 2 is the process schematic that the method prepares zinc oxide light anode light PEC brine electrolysis, show in figure: solar energy converting can be Hydrogen Energy by zinc oxide light anode under low impressed voltage, the products of combustion of hydrogen is water, thus make up the region limitation of sun power, meet the strategic decision of ground, world sustainable development source.
The method prepares the density of photocurrent curve of zinc oxide light anode as shown in Figure 3, shows in figure: it is 0.30mA/cm that MOCVD-ZnO is used for photoelectrochemical cell at the density of photocurrent that 0.62V vs.Ag/AgCl obtains as light anode
2.
Embodiment 2:
A kind of preparation method of zinc oxide photo-anode film, substantially the same manner as Example 1, difference is: step 2) in depositing time be 75min, ZnO film thickness is 2.5 μm, obtained " pyramid-like " shape zinc oxide (ZnO) photo-anode film on matte FTO substrate.
The surface topography of zinc oxide light anode prepared by the method is identical with embodiment 1.
The application method of prepared zinc oxide photo-anode film is identical with embodiment 1, the method prepares the density of photocurrent curve of zinc oxide light anode as shown in Figure 3, shows in figure: the density of photocurrent that MOCVD-ZnO obtains for photoelectrochemical cell as light anode under 0.62V vs.Ag/AgCl is 0.37mA/cm
2.
Embodiment 3:
A kind of preparation method of zinc oxide photo-anode film, substantially the same manner as Example 1, difference is: step 2) in depositing time be 125min, ZnO film thickness is 5.5 μm, obtained " pyramid-like " shape zinc oxide (ZnO) photo-anode film on matte FTO substrate.
The surface topography of zinc oxide light anode prepared by the method is identical with embodiment 1.
The application method of prepared zinc oxide photo-anode film is identical with embodiment 1, the method prepares the density of photocurrent curve of zinc oxide light anode as shown in Figure 3, shows in figure: the density of photocurrent that MOCVD-ZnO obtains for photoelectrochemical cell as light anode under 0.62V vs.Ag/AgCl is 0.71mA/cm
2.
Embodiment 4:
A kind of preparation method of zinc oxide photo-anode film, substantially the same manner as Example 1, difference is: step 2) in depositing time be 175min, ZnO film thickness is 7.5 μm, obtained " pyramid-like " shape zinc oxide (ZnO) photo-anode film on matte FTO substrate.
The surface topography of zinc oxide light anode prepared by the method is identical with embodiment 1.
The application method of prepared zinc oxide photo-anode film is identical with embodiment 1, the method prepares the density of photocurrent curve of zinc oxide light anode as shown in Figure 3, shows in figure: the density of photocurrent that MOCVD-ZnO obtains for photoelectrochemical cell as light anode under 0.62V vs.Ag/AgCl is 0.81mA/cm
2.
Embodiment 5:
A preparation method for zinc oxide photo-anode film, substantially the same manner as Example 1, difference is step 2) be:
2) by above process after FTO sample be positioned over deposit film in the chamber of single chamber MOCVD depositing system, the base vacuum of chamber is 0.03Torr, the reaction vacuum of chamber is 1Torr, depositing temperature is 155 DEG C, zinc ethyl (DEZn) flow is 180sccm, H
2o flow is 110sccm, impurity gas B
2h
6original dilution ratio be 1%, diluent gas is H
2, B
2h
6flow is 5sccm, and depositing time is 15min, obtained ZnO:B film, and ZnO:B film thickness is 700nm; And then depositing ZnO film, the reaction vacuum of chamber is 1Torr, depositing temperature is 155 DEG C, DEZn flow is 180sccm, H
2o flow is 110sccm, impurity gas B
2h
6flow is 0, and depositing time is 60min, and ZnO film thickness is 1.7 μm, can obtain " pyramid-like " shape zinc oxide (ZnO:B-ZnO bilayer film) double-deck light anode on matte FTO substrate.
The application method of prepared zinc oxide photo-anode film is identical with embodiment 1, the method prepares the density of photocurrent curve of zinc oxide light anode as shown in Figure 3, shows in figure: the density of photocurrent that the double-deck light anode of ZnO:B and ZnO obtains under 0.62V vs.Ag/AgCl for photoelectrochemical cell is 0.49mA/cm
2.
Embodiment 6:
A preparation method for zinc oxide photo-anode film, substantially the same manner as Example 1, difference is step 2) be:
2) by above process after FTO sample be positioned over deposit film in the chamber of single chamber MOCVD depositing system, the base vacuum of chamber is 0.03Torr, the reaction vacuum of chamber is 1Torr, depositing temperature is 155 DEG C, zinc ethyl (DEZn) flow is 180sccm, H
2o flow is 110sccm, impurity gas B
2h
6original dilution ratio be 1%, diluent gas is H
2, B
2h
6flow is 7sccm, and depositing time is 15min, obtained ZnO:B film, and ZnO:B film thickness is 600nm; And then depositing ZnO film, the reaction vacuum of chamber is 1Torr, depositing temperature is 155 DEG C, DEZn flow is 180sccm, H
2o flow is 110sccm, impurity gas B
2h
6flow is 0, and depositing time is 60min, and ZnO film thickness is 1.7 μm, can obtain " pyramid-like " shape zinc oxide (ZnO:B-ZnO bilayer film) double-deck light anode on matte FTO substrate.
The application method of prepared zinc oxide photo-anode film is identical with embodiment 1, the method prepares the density of photocurrent curve of zinc oxide light anode as shown in Figure 3, shows in figure: the density of photocurrent that the double-deck light anode of ZnO:B and ZnO obtains under 0.62V vs.Ag/AgCl for photoelectrochemical cell is 0.59mA/cm
2.
To sum up, the invention provides the novel processing step of zinc oxide light anode, this preparation method can prepare the light anode material of high photoelectrochemical behaviour, in addition, the method operation is more simple, and preparation time is shorter, can extensive deposition, be beneficial to its suitability for industrialized production, directly can prepare the light anode material of matte in deposition substrate.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (3)
1. a zinc oxide photo-anode film, is characterized in that: utilize MOCVD technology in the FTO substrate surface deposition preparation of matte, wherein the thickness of FTO layer is 600nm, and centimetre resistance is 20 Ω, optical band gap is 2eV; The thickness of zinc oxide photo-anode film is that 1.5-7.5 μm, centimetre resistance is 500 Ω, optical band gap width is 3.2eV.
2. a preparation method for zinc oxide photo-anode film as claimed in claim 1, with zinc class source liquid for zinc ethyl (DEZn) ﹑ oxygen class source liquid is that water ﹑ doped source gas is for B
2h
6, to carry gas be Ar gas in carrier gas, it is characterized in that comprising the following steps:
1) FTO substrate is placed in the container ultrasonic cleaning 30min that purity is the dehydrated alcohol of 99.7%, utilizes high-purity N afterwards
2dry up, and on FTO substrate, reserve the electric transmission electrode not depositing ZnO with high temperature gummed tape;
2) by above process after FTO sample be positioned over deposit film in the chamber of single chamber MOCVD depositing system, the base vacuum of chamber is 0.03Torr, the vacuum tightness of chamber is 1Torr, depositing temperature is 155 DEG C, zinc ethyl (DEZn) flow is 180sccm, H
2o flow is 110sccm, impurity gas B
2h
6original dilution ratio be 1%, diluent gas is H
2, B
2h
6flow is 0-7sccm, depositing time is 25-175min, ZnO film thickness is 1.5-7.5 μm, obtained " pyramid-like " shape zinc oxide photo-anode film on matte FTO substrate.
3. the application of a zinc oxide photo-anode film as claimed in claim 1, it is characterized in that: the light anode as photoelectrochemical cell the is used for light anode PEC brine electrolysis that is substrate with matte FTO, time of photoelectrochemical cell very platinum filament, reference electrode be Ag/AgCl solution, the NaSO of electrolytic solution to be concentration be 0.5M
4solution and utilize the NaOH solution of 0.01M its pH to be adjusted to 7, test area is 0.2826cm
2, light intensity is 100mW/cm
2.
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| CN106384669A (en) * | 2016-10-27 | 2017-02-08 | 常州大学 | Preparation method of photoelectric response carbon quantum dot modified zinc oxide photo anode |
| CN106544693A (en) * | 2016-11-28 | 2017-03-29 | 北京工业大学 | A kind of preparation of multilevel hierarchy ZnO@CoS membrane electrodes and its application in photoelectric decomposition water |
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