CN104499010B - The preparation technology of visible light-responded nanometer α-ferric oxide film electrode - Google Patents
The preparation technology of visible light-responded nanometer α-ferric oxide film electrode Download PDFInfo
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Abstract
A kind of visible light-responded nanometer α Fe2O3The preparation technology of membrane electrode, it includes following methods step: 1) by 2～8g FeSO4·7H2O is dissolved in 150mL deionized water, add the ammonia of 20～50mL 27% and be stirred vigorously and obtain electrolyte solution, with conductive substrates fluorine doped tin oxide electro-conductive glass as negative electrode, platinized platinum is anode, electro-deposition 15～60s under 1.5～2.5V voltages, to the Fe thin film deionized water rinsing obtained on the cathode, and it is dried more than 1h at about 50 DEG C；2) in air atmosphere, by dry Fe thin film in 400～700 DEG C of heat treatments 1～6h, described nanometer α Fe after natural cooling, is i.e. obtained2O3Membrane electrode.The present invention has simplicity, gentleness, efficient feature, prepared nanometer α Fe2O3Membrane electrode has good visible absorption performance and good stability, and photoelectric efficiency is high, and photoelectric catalysis degrading organic is effective, it is possible to is applied to photoelectrocatalysis and produces hydrogen and degradation of organic substances field, obtains more preferable effect.
Description
Technical field
The present invention relates to photoelectrocatalysielectrode electrode material, be specifically related to a kind of visible light-responded nanometer α-iron sesquioxide (i.e.
α-Fe2O3) preparation technology of film photoelectric catalysis electrode, belong to field of nanometer material technology.
Background technology
Sunlight degradation of organic substances based on photo-electrocatalytic technology and hydrogen manufacturing, be a kind of new technique with application prospect.In this skill
In art, the performance of photochemical catalyst electrode directly affects the effect of photoelectrocatalytioxidation oxidation system.Therefore, the preparation of photochemical catalyst electrode material is
The focus of photoelectrocatalysis area research.
At present, generally believe that the feature that excellent photochemical catalyst electrode should possess mainly has: good visible absorption performance, water
In solution stable, nontoxic, easily prepared and inexpensive etc..In existing photoelectrocatalysimaterial material, α-iron sesquioxide (chemical formula
For α-Fe2O3) because having good visible absorption performance (band gap～2.1eV, absorbable wavelength < the visible and ultraviolet of 600nm
Light), good under the conditions of neutral and alkalescence stability, the advantage such as nontoxic and cheap, and be considered most potential photoelectricity and urge
Formed material.(following unified presentation is α-Fe to use electrochemical deposition method to prepare nanometer α-iron sesquioxide2O3) thin film has simply,
The feature of convenient easy-adjustable control, becomes α-Fe in recent years2O3The main stream approach of film preparation.Existing electrochemical method is divided into again sun
Pole sedimentation (Chem.Mater., 2009,21,3701 3709) and cathodic deposition (Chem.Mater., 2008,20,
3803 3805), wherein anodic deposition method is by Fe in solution2+It is oxidized to Fe3+, Fe3+FeOOH is obtained in anode surface precipitation
Thin film, then obtain α-Fe through the calcining of FeOOH thin film2O3Thin film；Cathodic deposition is to utilize the H in solution2O2At the moon
Pole reduction forms local OH-Concentration increases and makes Fe in solution3+Obtain FeOOH thin film in anode surface precipitation, then pass through
The calcining of FeOOH thin film obtains α-Fe2O3Thin film.In the above-mentioned methods, due to Fe2+And Fe3+Can be formed in aqueous
Such as multiple uppity complex compounds such as polyol, polynuclear complex, abutment compounds, therefore in deposition
There is a large amount of fault of construction in FeOOH thin film, this will be incorporated into α-Fe in calcination process2O3In thin film (Chem.Mater.,
1994,6,858 863) α-Fe, is affected2O3The PhotoelectrocatalytiPerformance Performance of thin film.
Prior art also reports and utilizes iron plate direct sintering to obtain α-Fe2O3The method of thin film (Nanotechnology, 2012,
23,194009).Iron plate thermal oxidation method is by iron plate thermal oxide in oxygen-containing atmosphere is formed iron-based α-Fe2O3Membrane electrode,
It is a kind of original position and simple α-Fe2O3Thin film preparation process.But oxide layer forms speed soon in the method preparation process, oxygen
Change layer thickness to be not easy to control, and be easily formed such as FeO and Fe in contact portion at the bottom of oxide layer with iron-based3O4Transition zone
(Electrochem.Commun., 2012,23,59 62.), this will have a strong impact on prepared α-Fe2O3The photoelectricity of membrane electrode
Catalytic performance.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that easy, the most visible light-responded a kind of nanometer α-three
Aoxidize two ferrum (i.e. α-Fe2O3) preparation technology of film photoelectric catalysis electrode, make prepared nanometer α-Fe2O3Thin-film electro is great
There are good visible absorption performance, good stability and high photoelectric efficiency, to obtain α-Fe2O3Electrode produces at photoelectrocatalysis
Hydrogen and degradation of organic substances aspect preferably apply effect.
The present invention is achieved by the following technical solutions:
A kind of visible light-responded nanometer α-Fe2O3The preparation technology of membrane electrode, it includes following methods step:
1) by 2～8g FeSO4·7H2O is dissolved in 150mL deionized water, adds the ammonia of 20～50mL 27% and acutely stirs
Mixing and obtain electrolyte solution, with conductive substrates fluorine doped tin oxide electro-conductive glass as negative electrode, platinized platinum is anode, at 1.5～2.5V voltages
Lower electro-deposition 15～60s, to the Fe thin film deionized water rinsing obtained on the cathode, and is dried 1h at about 50 DEG C
Above；
2) in air atmosphere, by dry Fe thin film in 400～700 DEG C of heat treatments 1～6h, i.e. obtain after natural cooling
Described nanometer α-Fe2O3Membrane electrode.
Visible light-responded nanometer α-Fe of the present invention2O3The process of preparing of membrane electrode has simplicity, gentleness, height
The feature of effect, lot of experimental data shows, prepared nanometer α-Fe2O3Membrane electrode has good visible absorption performance,
Good stability and high photoelectric efficiency, photoelectric catalysis degrading organic is effective.Compared with the conventional method, achieve good
Technique effect, is embodied in:
(1) present invention uses the mode of electro-deposition under ammonia-water systems to prepare Fe thin film, thus overcomes prior art in acidity
In system, electrodeposition of Fe dissolves once again and causes the inhomogenous problem of Fe thin film.
(2) ammonia-water systems that the present invention uses, NH4 +Fe (OH) can be adsorbed in2Isocolloid and fluorine doped tin oxide electro-conductive glass
(FTO) cathode surface, NH4 +Existence promote the carrying out of following reaction, thus be conducive to obtaining the Fe thin film of uniformity
Formed, overcome and tradition electrodeposition process preparation process exists a large amount of fault of construction in FeOOH thin film be incorporated into α-Fe2O3Thin film
In deficiency.
FeOH++NH4 ++2e-→Fe+NH3·H2O (3)
Fe(OH)2+2NH4 ++2e-→Fe+2NH3·H2O (4)
Fe2++2e-→Fe (5)
(3) the electrodeposition of Fe thin film that the present invention obtains, prepares α-Fe through in-situ thermal oxidation2O3Thin film, it is possible to achieve Fe
Thin film is fully converted to α-Fe2O3Thin film, overcomes in tradition iron plate thermal oxidation method preparation process and FeO and Fe occurs3O4Transition
The deficiency of layer.
(4) the Fe thin film that in the present invention prepared by electro-deposition, its thickness can be adjusted by sedimentation time, thus controls institute
Preparation α-Fe2O3The thickness of thin film, overcomes oxidation rate at the bottom of iron-based in tradition iron plate thermal oxidation method preparation process too fast and cause
The unmanageable deficiency of oxidated layer thickness.
(5) α-Fe that the present invention obtains2O3The PhotoelectrocatalytiPerformance Performance of thin film is better than tradition electrodeposition process and iron plate thermal oxide legal system
Standby α-the Fe obtained2O3Thin film.
Accompanying drawing explanation
Fig. 1 is the preparation technology schematic diagram of the present invention.
Fig. 2 is the Fe thin film and α-Fe obtained in embodiment 12O3The surface Electronic Speculum figure of thin film；
In figure, A is the surface electromicroscopic photograph of gained Fe thin film；B is the α-Fe obtained after thermal oxide2O3The surface electricity of thin film
Mirror photo.
Fig. 3 is the α-Fe obtained in embodiment 12O3The cross section Electronic Speculum figure of thin film.
Fig. 4 is the Fe thin film and α-Fe obtained in embodiment 12O3The XRD figure spectrum of thin film；
In figure, curve A is the XRD figure spectrum of gained Fe thin film, it is shown that the characteristic peak in (110) face in Emission in Cubic Fe crystal formation；
Curve B is the α-Fe obtained after thermal oxide2O3The XRD figure spectrum of thin film, it is shown that α-Fe2O3In crystal formation (012), (104)
(110) characteristic peak in face.
Fig. 5 is the α-Fe obtained in embodiment 12O3The xps energy spectrum figure of thin film.
Fig. 6 is the α-Fe obtained in embodiment 12O3The core level spectra of Fe 2p in thin film.
Fig. 7 is the α-Fe obtained in embodiment 12O3Raman (Raman) spectrogram of thin film.
Fig. 8 is the α-Fe obtained in embodiment 12O3The uv-visible absorption spectrum of thin film.
Fig. 9 is the α-Fe obtained in embodiment 42O3The volt-ampere curve that thin film obtains under intermittent light source.
Figure 10 is the α-Fe obtained in embodiment 42O3The photocurrent-time curve of thin film.
Figure 11 is the α-Fe obtained in embodiment 42O3Photoelectric transformation efficiency (IPCE) curve of thin film.
Figure 12 is the α-Fe obtained in embodiment 52O3α-the Fe that thin film and Conventional electrochemical sedimentation obtain2O3The modulation of thin film
The comparison diagram of photoelectric current collection of illustrative plates (IMPS).
Figure 13 is the α-Fe obtained in embodiment 62O3Thin film is in the degradation kinetics curve of difference degraded system.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is elaborated, but should not limit the scope of the invention with this.
First referring to Fig. 1, Fig. 1 is visible light-responded nanometer α-Fe of the present invention2O3The preparation technology signal of membrane electrode
Figure, it specifically includes following steps:
1) by 2～8g FeSO4·7H2O is dissolved in 150mL deionized water, adds the ammonia of 20～50mL 27% and acutely stirs
Mixing and obtain electrolyte solution, be negative electrode with conductive substrates, such as fluorine doped tin oxide electro-conductive glass (FTO), platinized platinum is anode,
Electro-deposition 15～60s under 1.5～2.5V voltages, to the Fe thin film deionized water rinsing obtained on the cathode, and at 50 DEG C
Left and right is dried more than 1h；
2) in air atmosphere, by dry Fe thin film in 400～700 DEG C of heat treatments 1～6h, i.e. obtain after natural cooling
Described nanometer α-Fe2O3Membrane electrode.
Present disclosure is illustrated below with embodiment.
Embodiment 1
First by 5g FeSO4·7H2O is dissolved in 150mL deionized water, then is added thereto to ammonia the play of 30mL 27%
Strong stirring obtains electrolyte solution, is placed in this electrolyte solution by clean fluorine doped tin oxide electro-conductive glass (FTO), and surely
The negative electrode of voltage source is connected, and with platinum electrode for electrode, regulation voltage is 2V, electro-deposition 30s, by the FTO of deposition Fe thin film
Take out, after deionized water rinsing, be placed in about 50 DEG C and be dried 1h and i.e. obtain Fe thin film；Then by described Fe thin film
It is placed in Muffle furnace and naturally cools to room temperature after 500 DEG C of high temperature sintering 2h, obtain nanometer α-Fe2O3Membrane electrode.
In Fig. 2, A shows the surface microscopic topographic of described Fe thin film, and its surface is single-size shape, and B shows described
Nanometer α-Fe2O3Film surface is more smooth than described Fe thin film, with a small amount of granule.
Fig. 3 gives described α-Fe2O3The cross section electromicroscopic photograph of thin film, shows described α-Fe in figure2O3Film thickness is about
230nm。
In Fig. 4, curve A gives the XRD figure spectrum of described Fe thin film, shows that the crystal formation of described Fe thin film is Emission in Cubic；
B gives described α-Fe2O3The XRD figure spectrum of thin film, shows described α-Fe2O3The composition of thin film is pure α-Fe2O3。
Fig. 5 gives described α-Fe2O3The xps energy spectrum figure of thin film, it shows described α-Fe2O3Except Fe and O in thin film
Outside element, without other impurity elements, (in figure, C element derives from the CO of film surface absorption2)。
Fig. 6 gives described α-Fe2O3The core level spectra of Fe 2p in thin film, its α-Fe described in display2O3Fe 2p in thin film
Corresponding peak～724.1eV and～710.8eV be typical α-Fe2O3The combination energy of middle Fe, shows described α-Fe2O3Thin film
For pure α-Fe2O3。
Fig. 7 gives described α-Fe2O3The Raman spectrogram of thin film, it is shown that α-Fe2O3Characteristic peak positions respectively 212,
271,384,484,579 and 1282cm-1Place, further demonstrates that described α-Fe2O3Thin film is pure α-Fe2O3, do not contain
The Fe oxide of other forms.
Fig. 8 gives described α-Fe2O3The ultraviolet-visible absorption spectroscopy of thin film, it shows described α-Fe2O3Thin film is for ripple
The long visible and ultraviolet light less than 600nm all has good absorbent properties.
Embodiment 2
First by 2g FeSO4·7H2O is dissolved in 150mL deionized water, then is added thereto to ammonia the play of 20mL 27%
Strong stirring obtains electrolyte solution, is placed in this electrolyte solution by clean fluorine doped tin oxide electro-conductive glass (FTO), and surely
The negative electrode of voltage source is connected, and with platinum electrode for electrode, regulation voltage is 2.5V, and electro-deposition 60s will deposited Fe thin film
FTO take out, after deionized water rinsing, be placed in about 50 DEG C and be dried 1h and i.e. obtain Fe thin film, then by described
Fe thin film is placed in Muffle furnace and naturally cools to room temperature after 700 DEG C of high temperature sintering 1.5h, obtains nanometer α-Fe2O3Membrane electrode.
Described α-Fe2O3Thin film is pure α-Fe2O3, thickness is about 410nm.
Embodiment 3
First by 8g FeSO4·7H2O is dissolved in 150mL deionized water, then is added thereto to ammonia the play of 50mL 27%
Strong stirring obtains electrolyte solution, is placed in this electrolyte solution by clean FTO, is connected with the negative electrode of regulated power supply, with platinum
Electrode is to electrode, and regulation voltage is 1.5V, electro-deposition 15s, is taken out by the FTO that deposited Fe thin film, uses deionized water
After flushing, it is placed in about 50 DEG C and is dried 1h and i.e. obtains Fe thin film, then described Fe thin film is placed in warp in Muffle furnace
Naturally cool to room temperature after 400 DEG C of high temperature sintering 6h, obtain nanometer α-Fe2O3Membrane electrode.Described α-Fe2O3Thin film is
Pure α-Fe2O3, thickness is about 180nm.
Embodiment 4
First by 5g FeSO4·7H2O is dissolved in 150mL deionized water, then is added thereto to ammonia the play of 30mL 27%
Strong stirring obtains electrolyte solution, is placed in this electrolyte solution by clean FTO, is connected with the negative electrode of regulated power supply, with platinum
Electrode is to electrode, and regulation voltage is 2V, electro-deposition 30s, is taken out by the FTO that deposited Fe thin film, rushes with deionized water
After washing, it is placed in about 50 DEG C and is dried more than 1h and i.e. obtains Fe thin film, then described Fe thin film is placed in warp in Muffle furnace
Naturally cool to room temperature after 500 DEG C of high temperature sintering 2h, obtain nanometer α-Fe2O3Membrane electrode.
By described α-Fe2O3Membrane electrode is as working electrode, with platinum electrode for electrode, with saturated calomel electrode (SCE)
For reference electrode, with the KOH solution of 1M as electrolyte, at simulated solar irradiation AM1.5 (100mW/cm2) irradiate condition
Under, scanning speed 0.005V/s, by electrochemical workstation test described in α-Fe2O3The photocatalytic water performance of membrane electrode.
Fig. 9 gives described α-Fe2O3The volt-ampere curve that membrane electrode obtains under intermittent light source, it shows described α-Fe2O3
Membrane electrode, when bias-voltage is higher than 0.75V (vs.RHE), has good photoresponse, and photocatalytic water current value is along with bias-voltage
Raise and persistently increase.
Figure 10 gives described α-Fe2O3Membrane electrode photocurrent-time curve under 1.23V (vs.RHE) biases,
Optical Electro-Chemistry test condition: electrolyte is 1M KOH solution, light intensity is AM1.5 (100mW/cm2), bias-voltage is 1.23
V (relative to standard hydrogen electrode, vs.RHE), testing time 2h；Figure showing, photocatalytic water electric current density is about 1.34mA/cm2,
Significantly reducing does not occurs in prolongation over time, and shows described α-Fe2O3It is steady that membrane electrode has good photoelectrocatalysis
Qualitative.After measured, in the present embodiment, hydrogen generation rate is 40.6 μm ol h-1cm-2。
Figure 11 gives described α-Fe2O3Membrane electrode photoelectric transformation efficiency curve under 1.23V (vs.RHE) biases,
Optical Electro-Chemistry test condition: electrolyte is 1M KOH solution, bias-voltage is 1.23V (vs.RHE)；Figure show described
α-Fe2O3Membrane electrode has response to wavelength at the light of below 600nm, to wavelength in the opto-electronic conversion of the light of below 400nm
Efficiency is higher than 14%.
Embodiment 5
First by 5g FeSO4·7H2O is dissolved in 150mL deionized water, then is added thereto to ammonia the play of 30mL 27%
Strong stirring obtains electrolyte solution, is placed in this electrolyte solution by clean fluorine doped tin oxide electro-conductive glass (FTO), and surely
The negative electrode of voltage source be connected, with platinum electrode for electrode regulating voltage as 2V, electro-deposition 60s, the FTO of Fe thin film will be deposited
Take out, after deionized water rinsing, be placed in about 50 DEG C and be dried 1h and i.e. obtain Fe thin film, then by described Fe thin film
It is placed in Muffle furnace and naturally cools to room temperature after 500 DEG C of high temperature sintering 2h, obtain nanometer α-Fe2O3Membrane electrode, its thin film
Thickness is about 410nm.
By described α-Fe2O3Membrane electrode is as working electrode, with platinum electrode for electrode, with saturated calomel electrode (SCE)
For reference electrode, with the KOH solution of 1M as electrolyte, bias-voltage is 1.23V (vs.RHE), the α-Fe described in test2O3
The modulated photocurrent collection of illustrative plates (IMPS) of membrane electrode.
As comparison, according to reporting document (Chem.Mater., 2009,21,3,701 3709) described Conventional electrochemical sedimentation
α-Fe described in preparation2O3Thin film, specific as follows: clean FTO is placed in the 0.02M FeCl of 75 DEG C2In aqueous solution,
Connecting the anode of regulated power supply, with platinum electrode for electrode, regulation voltage is 1.2V, electro-deposition 8min, gained FeOOH
Thin film is washed with deionized water only, is dried 1h in about 50 DEG C, then naturally cools to room temperature after 500 DEG C of high temperature sintering 2h,
Obtain the α-Fe described in Conventional electrochemical sedimentation2O3Thin film, its film thickness is about 410nm.Enter under the conditions of as described above
Row test.
Figure 12 gives the α-Fe obtained in the present embodiment2O3α-the Fe that thin film and Conventional electrochemical sedimentation obtain2O3Thin film
The comparison figure of IMPS.In figure, curve A is the α-Fe of the present invention2O3The IMPS test curve of thin film, curve minimum point correspondence frequency
Rate is 133Hz, according to formula τd=(2 π fmin(IMPS))-1(wherein τdBy being tested (the electricity of majority carrier in photochemical catalyst electrode
Son) arrive conductive substrates the average mobility time, fmin(IMPS) it is frequency values corresponding to minimum point in IMPS curve), calculate
To described α-Fe2O3In thin film, the average mobility time of light induced electron is 1.197ms；Curve B is Conventional electrochemical sedimentation
α-the Fe obtained2O3The IMPS test curve of thin film, curve minimum point respective frequencies is 53Hz, is calculated light in this thin film
The average mobility time of raw electronics is 3.004ms.Figure is shown the α-Fe obtained by the present invention2O3Photo-generated carrier in thin film
Migration rate is higher than the α-Fe that Conventional electrochemical sedimentation obtains2O3The migration rate of photo-generated carrier in thin film.Due to the two
Film thickness is identical, then α-the Fe that the present invention obtains2O3Fault of construction Conventional electrochemical to be less than sedimentation in thin film obtains
α-Fe2O3Thin film.
Embodiment 6
First by 5g FeSO4·7H2O is dissolved in 150mL deionized water, then is added thereto to ammonia the play of 30mL 27%
Strong stirring obtains electrolyte solution, is placed in this electrolyte solution by clean fluorine doped tin oxide electro-conductive glass (FTO), and surely
The negative electrode of voltage source is connected, and with platinum electrode for electrode, regulation voltage is 2V, and electro-deposition 30s will deposited Fe thin film
FTO takes out, and after deionized water rinsing, is placed in about 50 DEG C and is dried 1h and i.e. obtains Fe thin film, then by described Fe
Thin film is placed in Muffle furnace and naturally cools to room temperature after 500 DEG C of high temperature sintering 2h, obtains nanometer α-Fe2O3Membrane electrode.With
Containing 0.01M Na2SO4It is simulative organic wastewater with methylene blue (MB) aqueous solution of 5mg/L, with described nanometer α-Fe2O3
Membrane electrode is working electrode, with platinum electrode for electrode, at simulated solar irradiation AM1.5 (100mW/cm2) irradiate, 0.6V
Under bias condition, measure MB concentration over time.
In Figure 13, " photoelectrocatalysis " curve is the degradation kinetics curve of MB in the present embodiment, and it shows MB in the present embodiment
Speed constant be 0.9372h-1。
The effect of embodiment 6 is described with 2 reference examples below.
Reference examples 1
As comparison, with simulated solar irradiation AM1.5 (100mW/cm2) the MB solution described in direct irradiation embodiment 6,
Measure MB concentration over time.In Figure 13, the kinetic curve corresponding to " direct photolysis " shows MB in this reference examples
Degradation rate constant only has 0.1028h-1。
Reference examples 2
As comparison, in the case of other condition of embodiment 6 is constant, to described α-Fe2O3Membrane electrode adds 0V bias,
At simulated solar irradiation AM1.5 (100mW/cm2) irradiate lower mensuration MB concentration over time.In Figure 13 " photocatalysis "
Corresponding kinetic curve shows that in this reference examples, the degradation rate constant of MB only has 0.1851h-1。
Visible light-responded nanometer α-Fe of the present invention2O3The preparation technology of membrane electrode has simplicity, gentleness, efficient
Feature, prepared nanometer α-Fe2O3Membrane electrode has good visible absorption performance, good stability, and photoelectricity is imitated
Rate is high, and photoelectric catalysis degrading organic is effective.Compared with the prior art, achieve good technique effect, photoelectricity is urged
The development of change technology is significant.
Claims (1)
1. a visible light-responded nanometer α-Fe2O3The preparation technology of membrane electrode, it is characterised in that include that following methods walks
Rapid:
1) by 2～8g FeSO4·7H2O is dissolved in 150mL deionized water, adds the ammonia of 20～50mL 27% and acutely stirs
Mixing and obtain electrolyte solution, with conductive substrates fluorine doped tin oxide electro-conductive glass as negative electrode, platinized platinum is anode, at 1.5～2.5V voltages
Lower electro-deposition 15～60s, to the Fe thin film deionized water rinsing obtained on the cathode, and is dried 1h at about 50 DEG C
Above；
2) in air atmosphere, by dry Fe thin film in 400～700 DEG C of heat treatments 1～6h, i.e. obtain after natural cooling
Described nanometer α-Fe2O3Membrane electrode.
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| CN107326385B (en) * | 2017-06-16 | 2019-01-22 | 中国科学院化学研究所 | A kind of preparation method of boron doping di-iron trioxide optoelectronic pole |
| CN110438526A (en) * | 2019-07-17 | 2019-11-12 | 福建师范大学 | A kind of preparation method of nanogold codope iron oxide composite catalyzing electrode, catalysis electrode and electrolysis wetting system |
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