CN107638881A - A kind of preparation method for photoelectrocatalysis production hydrogen ZnO CuO FeOOH laminated films - Google Patents
A kind of preparation method for photoelectrocatalysis production hydrogen ZnO CuO FeOOH laminated films Download PDFInfo
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a kind of preparation method for photoelectrocatalysis production hydrogen ZnO CuO FeOOH laminated films, configures ZnO colloidal sols first and prepares ZnO Seed Layers using dip-coating method, using Hydrothermal Growth ZnO nanorod film.Then copper based film is prepared on ZnO nanorod film using electrodeposition process, CuO films is obtained by thermal oxide.FeOOH films are finally prepared on ZnO CuO films using electrodeposition process and obtain ZnO CuO FeOOH films.The ZnO CuO FeOOH films that are obtained of the present invention, after various tests, it is found that ZnO light absorbs make moderate progress and photoelectrocatalysis H2-producing capacity increases.Preparation method provided by the invention is simple to operation, has actual feasibility, and the ZnO CuO FeOOH film costs prepared are low, and pollution-free, photoelectrocatalysis H2-producing capacity is good.
Description
Technical field
The invention belongs to technical field of material, and in particular to one kind is used for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH
The preparation method of laminated film.
Background technology
For realize society sustainable development, Hydrogen Energy because its clean environment firendly, easily store the advantages that, as energy quilt of future generation
Development, it is intended to solve extremely urgent energy problem and environmental problem.It is worth noting that, photoelectrocatalysis decomposition water produces hydrogen
It is the optimization approach for producing hydrogen.Solar energy is inexhaustible, has become the widely studied energy source object being used.Half
Conductor catalysis material absorbs solar photon energy, and light induced electron transition occurs, and reaches semiconductor material surface and is contacted with water, is started
Decomposition water reaction produces hydrogen.Hydrogen is unique water using rear product as the energy, and this process realizes contamination-free
The utilization of solar energy and water.Therefore carrying out photoelectrocatalysis production hydrogen using semi-conducting material turns into study hotspot.
Semi-conducting material, which must simultaneously meet three key factors, could realize effective photoelectrocatalysis production hydrogen：(1) extensively
Photoresponse and absorption region, make full use of solar energy；(2) separation and transport of effective photo-generate electron-hole pair；(3) it is high
Semi-conducting material durability.From semi-conducting material TiO in 19722Be used as photoelectrocatalysis production hydrogen investigation of materials start, ZnO by
In with TiO2Property feature is similar, is used as TiO2Substitute and it is widely studied.ZnO energy gap is about 3.2eV, and its is right
Absorbing for sunshine is only limitted to ultraviolet light, and energy needed for electron transition is larger, and photo-generate electron-hole is to easily compound.Therefore
It is necessary targetedly to be modified it to lift its photoelectrocatalysis H2-producing capacity.CuO energy gaps are about 1.7eV, can
Good visible absorption is realized, therefore performance can be absorbed to sunshine to be modified ZnO with it.FeOOH is because of its water
The hole capture of iron ore and storage capacity can promote the separation and transport of photo-generate electron-hole pair.Therefore can be changed with it
Property ZnO photo-generate electron-holes are to easy composite performance.
At present for ZnO study on the modification mainly to construct based on hetero-junctions, for ZnO different performance functional layer study on the modification
Less, the photoelectrocatalysis production hydrogen report about ZnO-CuO-FeOOH ternary function coating systems is then relatively fewer.Therefore at present on
The photoelectrocatalysis production hydrogen of ZnO-CuO-FeOOH ternary function coating systems, which is one, to be worth inquiring into and having the research class of very big potentiality
Topic.
The content of the invention
For the performance for improving ZnO, further strengthen the utilizability of ZnO photoelectrocatalysis production hydrogen, it is of the invention to propose
It is used for the preparation method of the ternary functional layer ZnO-CuO-FeOOH films of photoelectrocatalysis production hydrogen.
The technical scheme is that：
A kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films, comprise the following steps：
Step 1：Prepare ZnO film
(1) ZnO colloidal sols are prepared；
(2) ZnO Seed Layers are prepared using dip-coating method；
(3) Hydrothermal Growth ZnO nanorod film is used；
Step 2：Prepare ZnO-CuO films
(1) CuO films are prepared on ZnO film using electrodeposition process；
(2) ZnO-CuO films are made by thermal oxide in the CuO films in (1)；
Step 3：Prepare ZnO-CuO-FeOOH films
(1) FeOOH films are prepared on ZnO-CuO films using electrodeposition process；
(2) ZnO-CuO-FeOOH films are made by thermal oxide in the FeOOH films prepared in (1).
Further, the technological parameter of (1) in the step 1 is：
1. configure 0.3-0.5molL-1ZnO colloidal sols：3-11g zinc acetates are added to 50-100mL ethylene glycol monomethyl ethers
In, 45-55 DEG C of magnetic agitation 20-30min, 2-6mL liquid simple substance MEAs are then added dropwise, continue to obtain after stirring 1.5-2h
Shallow yellow transparent solution, as ZnO colloidal sols；
2. the ZnO colloidal sols described in 1. are stood into 6-8 days, light yellow clear ZnO gels are obtained.
Further, the technological parameter of (2) in the step 1 is：
Obtained ZnO colloidal sols in (1) of the step 1 are prepared into ZnO Seed Layers using dip-coating method, then with 2
DEG C/min is warming up to 200 DEG C of insulation 30min, then proceed to be warming up to 450 DEG C of insulation 1-2h and obtain ZnO Seed Layers.
Further, the technological parameter of (3) in the step 1 is：ZnO seeds prepared by (2) in the step 1
Layer in growth solution, reacts 3-4h, 80-90 DEG C of drying obtains ZnO nanorod film using hydro-thermal method under the conditions of 90-100 DEG C.
Further, the growth solution is the mixed liquor of zinc nitrate and hexamethylenetetramine, the concentration of the mixed liquor
For 0.04-0.05molL-1, the mol ratio of the zinc nitrate and the hexamethylenetetramine is 1：1.
Further, the technological parameter of (1) in the step 2 is：ZnO film prepared by the step 1 is as work
Make electrode, Pt is used as to electrode, and Ag/AgCl is as reference electrode, electrolyte 0.4-0.5molL-1Copper sulphate and 2.5-
3mol·L-1The mixed liquor of lactic acid, uses 10molL-1Sodium hydroxide solution pH is adjusted to 8-10, applied voltage is -0.4
~-0.65V vs.Ag/AgCl, electrodeposition time 60-600s.
Further, the technological parameter of (2) in the step 2 is：(1) electro-deposition in the step 2 is obtained
CuO films be placed in Muffle furnace 500 DEG C of oxidation processes 1-2h of progress, obtain ZnO/CuO films.
Further, the technological parameter of (1) is in the step 3：ZnO-CuO films conduct made from the step 2
Working electrode, Pt are used as to electrode, and Ag/AgCl is as reference electrode, electrolyte 0.1-0.3molL-1Solution of ferrous chloride,
Applied voltage is 1.15-1.3V vs.Ag/AgCl, electrodeposition time 60-600s.
Further, the technological parameter of (2) is in the step 3：(1) electro-deposition in the step 3 is obtained
ZnO-CuO film deionized water rinsings, 80 DEG C of drying obtain ZnO-CuO-FeOOH films.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) the ZnO-CuO-FeOOH films that the present invention is obtained, after various tests, it is found that ZnO light absorbs have changed
Kind and photoelectrocatalysis H2-producing capacity increases.
(2) preparation method provided by the invention is simple to operation, has actual feasibility, and the ZnO-CuO- prepared
FeOOH film costs are low, pollution-free, and photoelectrocatalysis H2-producing capacity is good.
Brief description of the drawings
Fig. 1 is the electron-microscope scanning figure of the ternary functional layer ZnO-CuO-FeOOH films of the present invention.
Embodiment
The following examples can make those skilled in the art that the present invention be more completely understood, but not limit in any way
The present invention.
Embodiment 1
Step 1：Prepare ZnO film
By 11g zinc acetate [Zn (CH3COO)2·2H2O] it is added to 100ml ethylene glycol monomethyl ether [CH3OCH2CH2OH]
In, 45 DEG C of magnetic agitation 30min, 6ml MEAs [HO (CH are then added dropwise2)2NH2], continue stir 1.5h after obtain it is light yellow
Clear solution, as 0.5molL-1ZnO colloidal sols, ZnO colloidal sols are stood 7 days, obtain light yellow clear ZnO gels；
ZnO Seed Layers are prepared using dip-coating method, i.e.,：ZnO Seed Layers are plated on electro-conductive glass with 2mm/s speed,
60 DEG C of drying, 60 DEG C of dry 2h after plating two layers in the same way；By the ZnO Seed Layers on electro-conductive glass with 2 DEG C/min liters
Temperature then proceedes to be warming up to 450 DEG C of insulation 1h and obtains ZnO Seed Layers to 200 DEG C of insulation 30min；
Using hydro-thermal method, in growth solution, (growth solution is 0.04molL-1Zinc nitrate and hexamethylenetetramine mixing
Liquid, the two mol ratio are 1:1) in, 3h is reacted under the conditions of 100 DEG C, 80 DEG C of drying obtain ZnO nanorod film.
Step 2：Prepare ZnO-CuO films
ZnO film is used as to electrode as working electrode, Pt, and Ag/AgCl is as reference electrode, electrolyte 0.4mol
L-1Copper sulphate and 2.5molL-1The mixed liquor of lactic acid, 10molL-1Sodium hydroxide solution pH is adjusted to 10, using electricity
Press as -0.4V vs.Ag/AgCl, electrodeposition time 600s；
The film that electro-deposition is obtained is placed in Muffle furnace, 500 DEG C of oxidation processes 2h, obtains ZnO-CuO films.
Step 2：Prepare ZnO-CuO-FeOOH films
As working electrode, Pt is used as is ZnO-CuO films as reference electrode, electrolyte to electrode, Ag/AgCl
0.3mol·L-1Solution of ferrous chloride, applied voltage are 1.3V vs.Ag/AgCl, electrodeposition time 600s；
The film deionized water rinsing that electro-deposition is obtained, 80 DEG C of drying obtain ZnO-CuO-FeOOH films.
Embodiment 2
Step 1：Prepare ZnO film
By 3.3g zinc acetate [Zn (CH3COO)2·2H2O] it is added to 50ml ethylene glycol monomethyl ether [CH3OCH2CH2OH]
In, 50 DEG C of magnetic agitation 20min, 2ml MEAs [HO (CH are then added dropwise2)2NH2], continue stir 2h after obtain it is light yellow
Bright solution, as 0.3molL-1ZnO colloidal sols, ZnO colloidal sols are stood 7 days, obtain light yellow clear ZnO gels；
ZnO Seed Layers are prepared using dip-coating method, i.e.,：ZnO Seed Layers are plated on electro-conductive glass with 1mm/s speed,
80 DEG C of drying, 80 DEG C of dry 1h after plating two layers in the same way；ZnO Seed Layers on electro-conductive glass are heated up with 2 DEG C/min
To 200 DEG C of insulation 30min, then proceed to be warming up to 450 DEG C of insulation 1h and obtain ZnO Seed Layers；
Using hydro-thermal method, in growth solution, (growth solution is 0.05molL-1Zinc nitrate and hexamethylenetetramine mixing
Liquid, the two mol ratio are 1:1) in, 4h is reacted under the conditions of 90 DEG C, 80 DEG C of drying obtain ZnO nanorod film.
Step 2：Prepare ZnO-CuO films
ZnO film is used as to electrode as working electrode, Pt, and Ag/AgCl is as reference electrode, electrolyte 0.5mol
L-1Copper sulphate and 3molL-1The mixed liquor of lactic acid, 10molL-1Sodium hydroxide solution pH is adjusted to 8, applied voltage
For -0.5V vs.Ag/AgCl, electrodeposition time 60s；
The film that electro-deposition is obtained is placed in Muffle furnace, 500 DEG C of oxidation processes 1h, obtains ZnO-CuO films.
Step 2：Prepare ZnO-CuO-FeOOH films
As working electrode, Pt is used as is ZnO-CuO films as reference electrode, electrolyte to electrode, Ag/AgCl
0.1mol·L-1Solution of ferrous chloride, applied voltage are 1.2V vs.Ag/AgCl, electrodeposition time 60s；
The film deionized water rinsing that electro-deposition is obtained, 80 DEG C of drying obtain ZnO-CuO-FeOOH films.
The present invention the mechanism of action be：The photon energy absorbed after ZnO and CuO is by illumination is equal to or more than its each
Energy gap when, its electrons each in valence band, which is excited, to be transitted on its respective conduction band, so as in former electronics
Photohole is left on position, produces electron-hole pair.ZnO and CuO electron hole can be captured by FeOOH, so as to promote
The separation of photo-generate electron-hole pair.Light induced electron has very strong reducing power, and water can be promoted by reaching semiconductor catalyst surface
Decompose and produce hydrogen.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (9)
1. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films, it is characterised in that including as follows
Step：
Step 1：Prepare ZnO film
(1) ZnO colloidal sols are prepared；
(2) ZnO Seed Layers are prepared using dip-coating method；
(3) Hydrothermal Growth ZnO nanorod film is used；
Step 2：Prepare ZnO-CuO films
(1) CuO films are prepared on ZnO film using electrodeposition process；
(2) ZnO-CuO films are made by thermal oxide in the CuO films in (1)；
Step 3：Prepare ZnO-CuO-FeOOH films
(1) FeOOH films are prepared on ZnO-CuO films using electrodeposition process；
(2) ZnO-CuO-FeOOH films are made by thermal oxide in the FeOOH films prepared in (1).
2. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 1, its
It is characterised by, the technological parameter of (1) in the step 1 is：
1. configure 0.3-0.5molL-1ZnO colloidal sols：3-11g zinc acetates are added in 50-100mL ethylene glycol monomethyl ethers, 45-
55 DEG C of magnetic agitation 20-30min, 2-6mL MEAs are then added dropwise, continue to stir after 1.5-2h that to obtain light yellow clear molten
Liquid, as ZnO colloidal sols；
2. the ZnO colloidal sols described in 1. are stood into 6-8 days, light yellow clear ZnO gels are obtained.
3. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 1, its
It is characterised by, the technological parameter of (2) in the step 1 is：
Obtained ZnO colloidal sols in (1) of the step 1 are prepared into ZnO Seed Layers using dip-coating method, then with 2 DEG C/min
200 DEG C of insulation 30min are warming up to, then proceedes to be warming up to 450 DEG C of insulation 1-2h and obtains ZnO Seed Layers.
4. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 1, its
It is characterised by, the technological parameter of (3) in the step 1 is：ZnO Seed Layers prepared by (2) in the step 1 are used into water
Hot method reacts 3-4h in growth solution under the conditions of 90-100 DEG C, 80-90 DEG C of drying obtains ZnO nanorod film.
5. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 4, its
It is characterised by, the growth solution is the mixed liquor of zinc nitrate and hexamethylenetetramine, and the concentration of the mixed liquor is 0.04-
0.05mol·L-1, the mol ratio of the zinc nitrate and the hexamethylenetetramine is 1：1.
6. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 1, its
It is characterised by, the technological parameter of (1) in the step 2 is：ZnO film prepared by the step 1 is as working electrode, Pt
As to electrode, Ag/AgCl is as reference electrode, electrolyte 0.4-0.5molL-1Copper sulphate and 2.5-3molL-1Breast
The mixed liquor of acid, uses 10molL-1Sodium hydroxide solution pH is adjusted to 8-10, applied voltage is -0.4~-0.65V
Vs.Ag/AgCl, electrodeposition time 60-600s.
7. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 1, its
It is characterised by, the technological parameter of (2) in the step 2 is：The CuO films that (1) electro-deposition in the step 2 is obtained
500 DEG C of oxidation processes 1-2h of progress in Muffle furnace are placed in, obtain ZnO/CuO films.
8. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 1, its
It is characterised by, the technological parameter of (1) is in the step 3：ZnO-CuO films made from the step 2 as working electrode,
Pt is used as to electrode, and Ag/AgCl is as reference electrode, electrolyte 0.1-0.3molL-1Solution of ferrous chloride, applied voltage
For 1.15-1.3V vs.Ag/AgCl, electrodeposition time 60-600s.
9. a kind of preparation method for photoelectrocatalysis production hydrogen ZnO-CuO-FeOOH laminated films as claimed in claim 1, its
It is characterised by, the technological parameter of (2) is in the step 3：By the ZnO-CuO films that (1) electro-deposition obtains in the step 3
With deionized water rinsing, 80 DEG C of drying obtain ZnO-CuO-FeOOH films.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109794264A (en) * | 2019-02-02 | 2019-05-24 | 河北工业大学 | A kind of micron of flower ball-shaped high-performance complete solution water bifunctional electrocatalyst FeOOH/Ni3S2Preparation method |
| CN109987856A (en) * | 2019-03-21 | 2019-07-09 | 天津城建大学 | One kind having hydrophilic TiO2The preparation method of/FeOOH laminated film |
| CN110484951A (en) * | 2019-08-12 | 2019-11-22 | 浙江大学 | Reduce the method for electro-deposition CuO electrode band gap using high-temperature calcination in a nitrogen atmosphere |
| CN111774057A (en) * | 2020-07-02 | 2020-10-16 | 辽宁大学 | High-performance heterojunction material Fe2O3/CuO photoelectrode film and preparation method and application thereof |
| CN112108156A (en) * | 2019-06-20 | 2020-12-22 | 天津城建大学 | Ag nano particle modified MgFe2O4Method for preparing nano-rod composite film |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109794264A (en) * | 2019-02-02 | 2019-05-24 | 河北工业大学 | A kind of micron of flower ball-shaped high-performance complete solution water bifunctional electrocatalyst FeOOH/Ni3S2Preparation method |
| CN109794264B (en) * | 2019-02-02 | 2022-02-08 | 河北工业大学 | Micro-popcorn-shaped high-performance full-hydrolysis bifunctional electrocatalyst FeOOH/Ni3S2Preparation method of (1) |
| CN109987856A (en) * | 2019-03-21 | 2019-07-09 | 天津城建大学 | One kind having hydrophilic TiO2The preparation method of/FeOOH laminated film |
| CN112108156A (en) * | 2019-06-20 | 2020-12-22 | 天津城建大学 | Ag nano particle modified MgFe2O4Method for preparing nano-rod composite film |
| CN112108156B (en) * | 2019-06-20 | 2023-05-02 | 天津城建大学 | Ag nanoparticle modified MgFe 2 O 4 Preparation method of nanorod composite film |
| CN110484951A (en) * | 2019-08-12 | 2019-11-22 | 浙江大学 | Reduce the method for electro-deposition CuO electrode band gap using high-temperature calcination in a nitrogen atmosphere |
| CN111774057A (en) * | 2020-07-02 | 2020-10-16 | 辽宁大学 | High-performance heterojunction material Fe2O3/CuO photoelectrode film and preparation method and application thereof |
| CN111774057B (en) * | 2020-07-02 | 2022-06-14 | 辽宁大学 | High-performance heterojunction material Fe2O3/CuO photoelectrode film and preparation method and application thereof |
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