CN107313065B - Iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode and its preparation method and application - Google Patents
Iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to iron phosphide modified alpha type iron oxide vermiform nano-structure array light anodes and its preparation method and application, belong to novel energy resource material technology field, pass through hydro-thermal reaction and heat treatment, α type iron oxide is grown in conductive substrates in a manner of vermiform nano-structure array, and the superficial layer of α type iron oxide is converted into FeP with the mode of low temperature phosphor, it effectively inhibits the compound of electron-hole pair and accelerates oxygen evolution reaction dynamics, to substantially increase the efficiency of photoelectrolysis water.In addition, the present invention is during preparing iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode, material therefor is cheap, advantageously reduces production cost, realizes large-scale production.
Description
Technical field
The invention belongs to novel energy resource material technology fields, and in particular to iron phosphide modified alpha type iron oxide vermiform nano junction
Structure array photo-anode and its preparation method and application.
Background technique
Hydrogen has high energy density, and will not generate any pollutant and greenhouse effects as fuel, thus is
A kind of energy carrier of great potential.On the other hand, solar energy is a kind of inexhaustible clean energy resource, and water is on earth
Reserves it is extremely abundant.Therefore, solar energy is stored in hydrogen by way of photoelectrolysis water is to solve current fossil fuel
Face the exhausted method with a kind of great potential of the deterioration of the ecological environment.However due to the oxidation of water be four electronic processes and
It needs that molecular rearrangement occurs, leads to serious limitation of the performance of photoelectrolysis water by anode.Bloodstone di-iron trioxide (α-
Fe2O3) it is used as a kind of n-type semiconductor, there is relatively narrow energy band (Eg=2.2eV), ultraviolet light and visible light are shown preferably
Photoresponse, while its content in the earth's crust is also relatively abundant, has the characteristics that stablize nontoxic, thus is a kind of very promising
Optical anode material.But it there is also oxygen evolution reaction dynamic process is slow, electric conductivity is poor, hole diffusion length it is short with
And electron-hole pair it is easily compound the disadvantages of.Therefore, how to accelerate α-Fe2O3Oxygen evolution reaction dynamic process, inhibit photocatalysis
Electron-hole pair is compound in the process, and improving its electric conductivity is the key that can preferably become optical anode material.
Summary of the invention
In view of this, the present invention is to α-Fe2O3It can be improved on the basis of keeping its ontological property by being surface modified
Oxygen evolution reaction dynamics, promotes the separation of electronics and hole, and then improves its photoelectrocatalysis efficiency.Wherein, base metal phosphatization
Object is used to modified alpha-Fe due to its excellent analysis oxygen catalytic activity, by it2O3, it is remarkably improved it and analyses oxygen catalytic efficiency, to mentions
The performance of bloom electrolysis water.Therefore, it is an object of the invention to: (1) provide iron phosphide modified alpha type iron oxide vermiform nano junction
The preparation method of structure array photo-anode；(2) iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode is provided；(3)
Application of the iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode in photoelectrolysis water is provided.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, the preparation method of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode, includes the following steps:
(1) after conductive substrates being carried out surface clean, it is immersed in FeCl3·6H2Hydro-thermal reaction is carried out in O solution, then through two
After step annealing, cooling obtains the conductive substrates that load has α type iron oxide, and the α type iron oxide is in vermiform nano-structure array；
(2) conductive substrates of α type iron oxide and sodium hypophosphite are respectively placed in two porcelain boats load in step (1),
There is the porcelain boat of many lacunary masking foil pack accommodating sodium hypophosphites with thorn first, then with not piercing the masking foil of aperture for two porcelain
It is placed in tube furnace together after boat package, is warming up to 200~400 DEG C under protection of argon gas with the heating rate of 1~5 DEG C/min and forges
10~30min of annealing is burnt, iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode is obtained.
Further, in step (1), the conductive substrates are FTO glass；The surface clean specifically: first super with acetone
10~15min of sound, is eluted with water；10~15min of dehydrated alcohol ultrasound is used again, is eluted with water；Finally use deionized water ultrasound 10
~15min.
Further, in step (1), the hydro-thermal reaction specifically: under conditions of 100~120 DEG C hydro-thermal reaction 3~
6h；The double annealing specifically: be warming up to 550 DEG C of holding 1h first, be then warming up to 700~730 DEG C of holding 15min again.
Further, in step (1), the FeCl3·6H2O solution concentration is 0.1~0.15M.
Further, in step (1), FeCl3·6H2O solution concentration is 0.15M.
Further, in step (2), the weight ratio of α type iron oxide and sodium hypophosphite is 1~3:20.
Further, in step (2), the weight ratio of α type iron oxide and sodium hypophosphite is 1:20.
Further, in step (2), 300 DEG C of calcining annealing are warming up to the heating rate of 2 DEG C/min under protection of argon gas
15min。
2, the iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode prepared by the method.
3, iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode the answering in photoelectrolysis water
With.
The beneficial effects of the present invention are: the present invention provides iron phosphide modified alpha type iron oxide vermiform nano-structure array
Light anode and its preparation method and application, by hydro-thermal reaction and heat treatment, by α type iron oxide with vermiform nano-structure array
Mode grow in conductive substrates, and the superficial layer of α type iron oxide is converted into FeP with the mode of low temperature phosphor, effectively inhibited
Electron-hole pair compound and oxygen evolution reaction dynamics is accelerated, to substantially increase the efficiency of photoelectrolysis water.Separately
Outside, the present invention is during preparing iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode, material therefor price
It is cheap, production cost is advantageously reduced, realizes large-scale production.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is the FTO glass and iron phosphide modified alpha type iron oxide vermiform nanometer that load has α type iron oxide in embodiment 1
The field emission scanning electron microscope figure of array of structures light anode；
Fig. 2 is the FTO glass and iron phosphide modified alpha type iron oxide vermiform nanometer that load has α type iron oxide in embodiment 1
The XRD diagram of array of structures light anode；
Fig. 3 is the XPS figure of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode in embodiment 1；
Fig. 4 is the FTO glass and iron phosphide modified alpha type iron oxide vermiform nanometer that load has α type iron oxide in embodiment 1
The UV-visible absorption spectrum of array of structures light anode；
Fig. 5 is the FTO glass and iron phosphide modified alpha type iron oxide vermiform nanometer that load has α type iron oxide in embodiment 1
The LSV curve graph of array of structures light anode.
Specific embodiment
Below by a preferred embodiment of the present invention will be described in detail.
Embodiment 1
Prepare iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode
(1) FTO glass is first used into acetone ultrasound 15min, be eluted with water；Dehydrated alcohol ultrasound 15min is used again, is washed with water
Only；After finally using deionized water ultrasound 15min, it is immersed in the FeCl that concentration is 0.15M3·6H2In O solution under conditions of 100 DEG C
The hydro-thermal reaction for carrying out 4h, is then first warming up to 550 DEG C of holding 1h, then be warming up to 700 DEG C of holding 15min in Muffle furnace, drops
Temperature obtains the FTO glass that load has α type iron oxide, and the α type iron oxide is in vermiform nano-structure array；
(2) load in step (1) is had the conduction of α type iron oxide by the weight ratio 1:20 for pressing α type iron oxide and sodium hypophosphite
Substrate and sodium hypophosphite are respectively placed in two porcelain boats, have many lacunary masking foil pack accommodating sodium hypophosphites with thorn first
Porcelain boat, then will be placed in tube furnace together after two porcelain boats package with the masking foil for not piercing aperture, under protection of argon gas with 2 DEG C/
The heating rate of min is warming up to 300 DEG C of calcining annealing 15min, obtains iron phosphide modified alpha type iron oxide vermiform nanostructure battle array
Column light anode.
Embodiment 2
Prepare iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode
(1) FTO glass is first used into acetone ultrasound 12min, be eluted with water；Dehydrated alcohol ultrasound 12min is used again, is washed with water
Only；After finally using deionized water ultrasound 12min, it is immersed in the FeCl that concentration is 0.1M3·6H2In O solution under conditions of 120 DEG C
The hydro-thermal reaction for carrying out 3h, is then first warming up to 550 DEG C of holding 1h, then be warming up to 715 DEG C of holding 15min in Muffle furnace, drops
Temperature obtains the FTO glass that load has α type iron oxide, and the α type iron oxide is in vermiform nano-structure array；
(2) load in step (1) is had the conduction of α type iron oxide by the weight ratio 3:20 for pressing α type iron oxide and sodium hypophosphite
Substrate and sodium hypophosphite are respectively placed in two porcelain boats, have many lacunary masking foil pack accommodating sodium hypophosphites with thorn first
Porcelain boat, then will be placed in tube furnace together after two porcelain boats package with the masking foil for not piercing aperture, under protection of argon gas with 5 DEG C/
The heating rate of min is warming up to 400 DEG C of calcining annealing 10min, obtains iron phosphide modified alpha type iron oxide vermiform nanostructure battle array
Column light anode.
Embodiment 3
Prepare iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode
(1) FTO glass is first used into acetone ultrasound 10min, be eluted with water；Dehydrated alcohol ultrasound 10min is used again, is washed with water
Only；After finally using deionized water ultrasound 10min, it is immersed in the FeCl that concentration is 0.12M3·6H2In O solution under conditions of 110 DEG C
The hydro-thermal reaction for carrying out 6h, is then first warming up to 550 DEG C of holding 1h, then be warming up to 730 DEG C of holding 15min in Muffle furnace, drops
Temperature obtains the FTO glass that load has α type iron oxide, and the α type iron oxide is in vermiform nano-structure array；
(2) load in step (1) is had the conduction of α type iron oxide by the weight ratio 2:20 for pressing α type iron oxide and sodium hypophosphite
Substrate and sodium hypophosphite are respectively placed in two porcelain boats, have many lacunary masking foil pack accommodating sodium hypophosphites with thorn first
Porcelain boat, then will be placed in tube furnace together after two porcelain boats package with the masking foil for not piercing aperture, under protection of argon gas with 1 DEG C/
The heating rate of min is warming up to 200 DEG C of calcining annealing 30min, obtains iron phosphide modified alpha type iron oxide vermiform nanostructure battle array
Column light anode.
Figure 1A is the Flied emission scanning that the load prepared in embodiment 1 has the FTO glass of α type iron oxide to amplify 50000 times
Electron microscope, Figure 1B are that the Flied emission of 50000 times of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode amplification is swept
Electron microscope is retouched, by A, B in Fig. 1 it is found that α type iron oxide is in vermiform nano-structure array, vermiform nanostructure in Figure 1B
Diameter is greater than the diameter of vermiform nanostructure in Figure 1A, and some are merged between structure, implies α-Fe2O3It has sent out
Raw phosphatization.
Fig. 2 is the FTO glass and iron phosphide modified alpha type iron oxide vermiform nanometer that load has α type iron oxide in embodiment 1
The XRD diagram of array of structures light anode, as seen from the figure, iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode
Do not occur new characteristic peak in XRD diagram, display crystal form is there is no changing significantly, thus the main body after phosphatization is still α-
Fe2O3。
Fig. 3 is the XPS figure of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode in embodiment 1, Fig. 3 A
In, Fe 2p3/2There are two peaks, wherein derives from Fe at the peak of 712.1eV2O3, and phosphatization is then derived from the peak of 707.1eV
Iron；In Fig. 3 B, there are three peaks by P 2p, wherein two peaks 130.2 and 129.5eV are the P 2p of iron phosphide1/2With P 2p3/2Peak, and
This peak 133.8eV then derives from the oxide of P caused by phosphatization iron surface is oxidized, and above data illustrates α-Fe2O3Surface quilt
Success phosphatization generates iron phosphide.
Fig. 4 is the FTO glass and iron phosphide modified alpha type iron oxide vermiform nanometer that load has α type iron oxide in embodiment 1
The UV-visible absorption spectrum of array of structures light anode, as seen from the figure, load have the FTO glass of α type iron oxide to light absorption
Range is wider, and after iron phosphide is modified, absorption region is basically unchanged, and other than ultra-violet (UV) band intensity has larger decline,
The absorption in other sections is basically unchanged, and illustrates that iron phosphide blocks absorption of the α type iron oxide to ultraviolet light to a certain extent, but
It is that as shown in Figure 5, the photocatalysis electric current of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode is that load has α
4.1 times at 1.23V (vs.RHE) of the FTO glass of type iron oxide, photocatalysis electric current is not only because of the ultraviolet light of absorption
It reduces and becomes smaller, have photocatalysis electric current caused by the FTO glass of α type iron oxide big than load instead, illustrate iron phosphide modified alpha
The promotion of type iron oxide vermiform nano-structure array light anode PhotoelectrocatalytiPerformance Performance does not lie in the enhancing of light absorption, but because
The analysis oxygen catalytic activity for the iron phosphide modified thereon enhances light absorption with passing through in the prior art to improve PhotoelectrocatalytiPerformance Performance
In the presence of the difference of essence.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. the preparation method of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode, which is characterized in that including such as
Lower step:
(1) after conductive substrates being carried out surface clean, it is immersed in FeCl3·6H2Hydro-thermal reaction is carried out in O solution, is then moved back through two steps
After fire, cooling obtains the conductive substrates that load has α type iron oxide, and the α type iron oxide is in vermiform nano-structure array；
(2) conductive substrates of α type iron oxide and sodium hypophosphite are respectively placed in two porcelain boats load in step (1), first
There is the porcelain boat of many lacunary masking foil pack accommodating sodium hypophosphites with thorn, then with not piercing the masking foil of aperture for two porcelain boat packets
It is placed in tube furnace together after wrapping up in, 200~400 DEG C of calcinings is warming up to the heating rate of 1~5 DEG C/min under protection of argon gas and are moved back
10~30min of fire obtains iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode.
2. the preparation method of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as described in claim 1,
It is characterized in that, the conductive substrates are FTO glass in step (1)；The surface clean specifically: first use acetone ultrasound 10
~15min, is eluted with water；10~15min of dehydrated alcohol ultrasound is used again, is eluted with water；Finally with deionized water ultrasound 10~
15min。
3. the preparation method of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as described in claim 1,
It is characterized in that, in step (1), the hydro-thermal reaction specifically: 3~6h of hydro-thermal reaction under conditions of 100~120 DEG C；Institute
State double annealing specifically: be warming up to 550 DEG C of holding 1h first, be then warming up to 700~730 DEG C of holding 15min again.
4. the preparation method of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as described in claim 1,
It is characterized in that, in step (1), the FeCl3·6H2O solution concentration is 0.1~0.15M.
5. the preparation method of iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as described in claim 1,
It is characterized in that, in step (1), FeCl3·6H2O solution concentration is 0.15M.
6. iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as claimed in any one of claims 1 to 5
Preparation method, which is characterized in that in step (2), the weight ratio of α type iron oxide and sodium hypophosphite is 1~3:20.
7. iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as claimed in any one of claims 1 to 5
Preparation method, which is characterized in that in step (2), the weight ratio of α type iron oxide and sodium hypophosphite is 1:20.
8. iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as claimed in any one of claims 1 to 5
Preparation method, which is characterized in that in step (2), 300 DEG C of calcinings are warming up to the heating rate of 2 DEG C/min under protection of argon gas
Anneal 15min.
9. the iron phosphide modified alpha type iron oxide vermiform nanostructure battle array prepared by method according to any one of claims 1 to 8
Column light anode.
10. iron phosphide modified alpha type iron oxide vermiform nano-structure array light anode as claimed in claim 9 is in photoelectrolysis water
Application.
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