CN104383950A - Bi2O3-BiOI heterojunction visible-light response photocatalyst and preparation method thereof - Google Patents
Bi2O3-BiOI heterojunction visible-light response photocatalyst and preparation method thereof Download PDFInfo
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- CN104383950A CN104383950A CN201410586341.1A CN201410586341A CN104383950A CN 104383950 A CN104383950 A CN 104383950A CN 201410586341 A CN201410586341 A CN 201410586341A CN 104383950 A CN104383950 A CN 104383950A
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Abstract
The invention discloses a Bi2O3-BiOI heterojunction visible-light response photocatalyst and a preparation method thereof. The photocatalyst is of a film structure, and comprises a conductive substrate and a Bi2O3-BiOI heterojunction film positioned on the conductive substrate. The preparation method comprises the following steps: firstly, preparing a Bi2O3 film on the conductive substrate, then putting the Bi2O3 film in an iodide ion solution for ion exchange so as to obtain the Bi2O3-BiOI heterojunction visible-light response photocatalyst. Under the irradiation of sunlight, the photocatalyst disclosed by the invention shows relatively high visible light catalytic activity, and the photoelectrocatalysis degradation effect is relatively good; moreover, photoproduction electron-hole pair compounding is inhibited while transferring of electrons is promoted, and the Bi2O3-BiOI heterojunction visible-light response photocatalyst and the preparation method thereof can be used for degrading environment pollutants by photoelectrocatalysis, photoelectrocatalysis synthesis and hydrogen production through water photolysis.
Description
Technical field
The present invention relates to photocatalyst technology field, particularly a kind of Bi
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst and preparation method thereof.
Background technology
Along with the energy and environmental problem increase the weight of day by day, the eco-friendly pollutant abatement technology seeking effective, harmless has become mankind's problem urgently to be resolved hurrily.Photocatalysis technology arises at the historic moment, and presents its superior application prospect, and a lot of novel photochemical catalyst is developed and shows high photocatalytic activity.
Nineteen eighty-three Pruden and Ollis finds TiO
2the photic mineralization of halogenated organic (as trichloro-ethylene, carrene etc.) in sensitization system, people are clearly realized that TiO
2to the photocatalytic degradation function of organic pollution, start the frontier of optically catalytic TiO 2 research.In recent years, along with the development of technology, TiO
2photocatalysis technology shows wide application prospect especially in improvement air pollution and purification of water quality.
Band gap wider (anatase type tio2, Eg=3.2eV), can only be less than the ultraviolet light response of 387nm to wavelength, and ultraviolet light only accounts for and reaches 4 ~ 6% of surface solar radiation energy, but visible ray accounts for 45% of solar radiation energy, causes TiO
2photochemical catalyst is very low to the utilization rate of sunshine.Therefore, the visible-light-responsive photocatalyst that development of new is efficient, stable is one of the key issue in photocatalysis technology field.
At present, bismuth based semiconductor photochemical catalyst obtains and pays close attention to because having good catalytic activity widely and study.Typical bismuth oxide (Bi
2o
3), energy gap band is 2.8eV, and absorbing wavelength is longer, and the utilization rate of visible ray is higher.In addition, BiOX also has good conduction and optical property, and band-gap energy is 1.7 ~ 3.2eV, can be excited under the irradiation of visible ray, is also the high performance visible light catalyst of a class.
Active for improving visible light catalyst, generally can take the methods such as modification doping and semiconductors coupling.Wherein semiconductors coupling is that the different photochemical catalyst of two kinds of two kinds of band gap mutually being mated carries out compound, forms the composite photo-catalyst of heterojunction structure.Under illumination condition, the electronics that this composite photo-catalyst is excited, hole can realize effective mobility, thus greatly reduce the recombination rate of electron hole pair, and then effectively can improve the photocatalytic activity of semiconductor.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of Bi
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst and preparation method thereof.This preparation method is simple, and the heterojunction photocatalyst light induced electron prepared and hole good separating effect, show higher photocatalytic activity, photoelectric catalysis degrading pollutant Be very effective.
Bi of the present invention
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, described photochemical catalyst is membrane structure, comprises conductive substrates and is positioned at the Bi in conductive substrates
2o
3-BiOI hetero-junction thin-film.
Wherein, Bi
2o
3-BiOI hetero-junction thin-film comprises the Bi be positioned in conductive substrates from the bottom to top successively
2o
3film and be positioned at Bi
2o
3biOI film on film.
Conductive substrates mostly is electro-conductive glass (FTO) material.
The present invention is by Bi
2o
3carry out compound with BiOI semi-conducting material and be prepared into Bi
2o
3-BiOI heterojunction photocatalyst, effectively can improve visible light-responded property photoelectric current and the photocatalytic activity of catalyst.Bi
2o
3be respectively+0.33V and 0.56V with the conduction band of BiOI, valence band is respectively+3.13V and+2.42V.So BiOI has less band-gap energy, and the semiconductor possessing narrow band-gap energy is easily activated generation hole and electronics by visible ray.While BiOI is activated, the absorbable high photon energy of BiOI can make the electronics in its valence band be excited to a higher energy of position band (-0.68V).
The position of energy band of restructuring makes the conduction band of BiOI compare Bi
2o
3conduction band more active.Therefore, the electronics produced on BiOI surface can transfer to Bi easily
2o
3conduction band get on, only leave hole in the valence band of BiOI.In addition, Bi
2o
3also Absorbable rod some visible light is activated, and the hole stayed in valence band can be transferred in the BiOI valence band lower than oneself valence band.By the matching way of this valence band, the light induced electron produced at two kinds of semiconductor surfaces just reaches with hole the effect be efficiently separated.The light induced electron of high separation and hole avoid the probability of compound, make its each self energy carry out better being oxidized and reduction reaction.Therefore, the Bi of formation
2o
3-BiOI heterojunction photocatalyst is relative to single Bi
2o
3or BiOI catalyst has shown better photocatalysis performance in degradation of contaminant.
Bi of the present invention
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst is membrane structure, considerably increases the specific area of photochemical catalyst, and then substantially increases photocatalysis efficiency.
Described Bi
2o
3the thickness of-BiOI hetero-junction thin-film is 1 ~ 3 μm.This thickness range can be expanded according to the actual requirements.Bi
2o
3the light that when-BiOI hetero-junction thin-film thickness is too thin, film absorbs is few; The easy compound of the too thick photo-generate electron-hole of thickness.Preferably, described Bi
2o
3the thickness of-BiOI hetero-junction thin-film is 2 ~ 3 μm.
The thickness of described BiOI film is 0.5 ~ 2 μm.And the thickness of BiOI film is less than Bi
2o
3-BiOI hetero-junction thin-film.
Described Bi
2o
3the surface structure in the form of sheets of-BiOI hetero-junction thin-film, described laminated structure is of a size of 0.5 μm × 0.5 μm ~ 5 μm × 5 μm.。
Present invention also offers a kind of Bi
2o
3the preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, first prepares Bi in conductive substrates
2o
3film, then by described Bi
2o
3film is placed in iodide ion solution and carries out ion-exchange, namely obtains described Bi
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst.Specifically comprise the steps:
(S1) conductive substrates cleaning will containing Bi after drying
3+with HNO
3ethylene glycol solution slowly drop to described conductive substrates conducting surface on (HNO
3be acid for regulating ethylene glycol solution), vacuum drying, calcining, obtains Bi
2o
3film;
Preferably, Bi described in this step
3+with HNO
3ethylene glycol solution for containing Bi (NO
3)
3with HNO
3the ethylene glycol solution of (68.0% ~ 70%).
Preferably, Bi (NO in ethylene glycol solution described in this step
3)
3be 2 ~ 6g:20ml, HNO with the mass volume ratio of ethylene glycol solution
3amount of substance be 0.01 ~ 0.03mol.
Further preferably, vacuum drying temperature described in this step is 50 ~ 100 DEG C, and calcining heat is 300 ~ 700 DEG C, and calcination time is 1 ~ 6h.
Most preferably, Bi (NO
3)
3be 4g:20ml, HNO with the mass volume ratio of ethylene glycol solution
3amount of substance be 0.02mol, vacuum drying temperature is 80 DEG C, and the temperature of calcining is 500 DEG C, and calcination time is 3h.
(S2) be dissolved in distilled water by KI, regulate the pH of solution according to the needs preparing different-shape sample, the adjustable interval of pH value is 1 ~ 13, by the Bi obtained in step one
2o
3film is immersed in this iodide ion solution, obtains Bi
2o
3-BiOI hetero-junction thin-film.
Adopt the H of 1mol/L
2sO
4or the NaOH of 1mol/L regulates the pH value of iodide ion solution, preferably, pH is adjusted to 2 ~ 10, and soak time is 0 ~ 24h.
Further preferably, the H of 1mol/L is adopted
2sO
4being adjusted to pH is 3 ~ 5, and soak time is 1 ~ 4h.
Most preferably, the H of 1mol/L is adopted
2sO
4being adjusted to pH is 3, and soak time is 2h.
Bi in the present invention
2o
3the photoelectric catalytically active of-BiOI heterojunction photocatalysis film and Bi
2o
3the time of soaking in iodide ion solution about time of: immersion the I-in solution can be made too for a long time to exchange too much, cause the BiOI of generation to account for the component of film excessive, affect Bi
2o
3and the synergy between BiOI semiconductor, cause the photo-generate electron-hole separative efficiency produced to be cut down.The time of soaking is too short, and the BiOI generated is very few, affects the synergy between two kinds of semiconductors equally.Therefore, under this preferred soak time, the Bi contained by film
2o
3fit mutually with BiOI component, the synergy of hetero-junctions can be promoted, reach and promote that photo-generate electron-hole efficiently shifts the object of separation, and then improve the photocatalytic activity of film.
In the present invention, iodide ion solution is interpreted as the solution containing iodide ion, is generally the alkali metal salt of iodine, as KI or NaI solution.
Compared with prior art, beneficial effect of the present invention:
(1) the present invention has prepared a kind of Bi
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst, two kinds of photochemical catalysts with different band structure are utilized to combine, the light induced electron that two kinds of material surfaces are produced effectively is separated with hole, and the synergy of formation substantially increases the organic performance of photocatalyst for degrading.
(2) Bi of the present invention
2o
3-BiOI heterojunction photocatalyst has good visible ray photoelectrochemical behaviour, under visible light illumination, and the Bi prepared in the process of the present invention
2o
3the photoelectric current of-BiOI composite photo-catalyst is relative to Bi
2o
3improve about 7 times;
(3) Bi of the present invention
2o
3-BiOI heterojunction photocatalyst is membrane structure, considerably increase the specific area of photochemical catalyst, greatly improve catalytic efficiency, under sunlight, show good visible photoelectricity degradation of contaminant performance, can be used for the field such as photoelectric catalysis degrading environmental contaminants, photoelectrocatalysis synthesis;
(4) Bi of the present invention
2o
3the preparation technology of-BiOI heterojunction photocatalyst is simple, by the time-controllable to dip time, forms the Bi of different single Component molar content
2o
3-BiOI heterojunction photocatalysis film.
Accompanying drawing explanation
Fig. 1 is Bi
2o
3the SEM figure of film surface appearance;
The Bi that Fig. 2 is 2h for dipping duration (ion-exchange time)
2o
3the SEM figure of-BiOI film surface appearance;
Fig. 3 is dipping duration is the Bi of 2h
2o
3the SEM figure of-BiOI thin-membrane section pattern;
Fig. 4 is Bi
2o
3film and Bi
2o
3the XRD figure of-BiOI film;
Fig. 5 a is Bi
2o
3film and Bi
2o
3-BiOI film is at 0.1M Na
2sO
4with 0.1M Na
2sO
3mixed solution in, the linear sweep voltammetry curve under radiation of visible light;
Fig. 5 b is Bi
2o
3and Bi
2o
3-BiOI film is at 0.1M Na
2sO
4with 0.1M Na
2sO
3mixed solution in, ultraviolet-visible irradiate under linear sweep voltammetry curve;
Fig. 6 is Bi
2o
3and Bi
2o
3the UV-Vis absorption spectrum of-BiOI film;
Fig. 7 is Bi
2o
3and Bi
2o
3-BiOI film is at 0.1M Na
2sO
4solution in, respectively in the dark with the EIS collection of illustrative plates under visible light conditions;
Fig. 8 is Bi
2o
3film and Bi
2o
3the electricity conversion comparison diagram of-BiOI film;
Fig. 9 is Bi
2o
3film and Bi
2o
3the clearance comparison diagram of-BiOI film degradation of phenol under visible photoelectricity condition;
Figure 10 is dipping duration is the Bi of 24h
2o
3the SEM figure of-BiOI film surface appearance.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.Do not make specified otherwise, raw materials usedly in following embodiment be commercially available prod.Employing flies to receive desk-top ESEM (Phenom G2 Pro) and characterizes the surface texture of film and fractions distribution.Electron gun: 1500 hours CeB6 filaments, the pumpdown time: 10 seconds.
Embodiment 1
The Bi of the present embodiment
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst prepares as follows:
(1) by 4g Bi (NO
3)
35H
2o is dissolved in 20ml ethylene glycol solution, adds 0.02molHNO
3(68.0% ~ 70%), magnetic agitation 20min forms homogeneous transparent solution, get this solution 20 μ l, be coated with the conducting surface (10mm × 10mm) dropping in conductive substrates, put into vacuum drying chamber to dry, be warmed up to 500 DEG C with 5 DEG C/min in Muffle furnace after, cycle annealing process 3h, obtains Bi
2o
3film.
The conductive substrates of this enforcement is FTO glass (Fluorin doped tin-oxide, fluorine-doped tinoxide).Specification is 10mm × 50mm × 2mm.Preparation Bi
2o
3first FTO glass is carried out ultrasonic cleaning 5min by acetone, absolute ethyl alcohol and deionized water successively during film, then take out and dry.
The Bi prepared
2o
3as shown in Figure 1, surface has intensive cavernous structure to the surface texture of film.This structure is conducive to the ion-exchange between solution and film, and then promotes the generation of BiOI film.
(2) by Bi
2o
3film is placed in ligand solution and soaks 2h and carry out ion-exchange, after taking-up in distilled water soaking flushing naturally drying in air, obtain Bi
2o
3-BiOI film is Bi
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst.
The ligand solution of the present embodiment is KI solution.Concrete configuration method is as follows:
1.66g KI is dissolved in 50ml distilled water, stirs, then use 1M (i.e. 1mol/L) H
2sO
4solution B being adjusted to pH is 3.
Bi in the present embodiment
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst is membrane structure, comprises conductive substrates and is positioned at the Bi in conductive substrates
2o
3-BiOI hetero-junction thin-film.Fig. 2 is the SEM image of the surface texture of the photochemical catalyst of the present embodiment.Can observe and work as Bi
2o
3after film immerses KI solution, BiOI is that obvious random laminated structure growth is at Bi
2o
3the top of film, and the position generated is at Bi
2o
3near the cavernous structure of film.Laminated structure is of a size of 1 μm × 1 μm, and thickness is 240nm.Random laminated structure surface is conducive to Bi
2o
3combine closely with BiOI, the staggered laminated structure of formation considerably increases the specific area of material.
Fig. 3 is the Bi of the present embodiment
2o
3the SEM image of the section of-BiOI hetero-junctions visible-light-responsive photocatalyst, can find out that the photochemical catalyst obtained comprises conductive substrates, the Bi be positioned in conductive substrates
2o
3film and be positioned at Bi
2o
3biOI film on film.Bi
2o
3the thickness of-BiOI hetero-junction thin-film is 2.5 μm, and the thickness of BiOI film is 1 μm.
Fig. 4 is the Bi that the present embodiment prepares
2o
3film and Bi
2o
3the XRD collection of illustrative plates contrast of-BiOI film.Bi can be found out
2o
3the collection of illustrative plates of-BiOI film is at Bi
2o
3the collection of illustrative plates basis of film has obviously had more the diffractive features peak of BiOI material, this illustrates at Bi
2o
3film successfully generates BiOI, and two kinds of materials combine well.
Fig. 5 a is the Bi that the present embodiment prepares
2o
3film and Bi
2o
3-BiOI film linear sweep voltammetry curve under visible light illumination; Fig. 5 b is the Bi that this embodiment prepares
2o
3and Bi
2o
3the linear sweep voltammetry curve of-BiOI film under ultraviolet-visible irradiates.From Fig. 5 a and 5b, relative to Bi
2o
3film, Bi
2o
3the photoelectric current of-BiOI film, under visible ray and ultraviolet-visible irradiate, improves 7 times and 8.5 times, visible Bi respectively
2o
3the photoelectric catalytically active of material greatly can be improved with the compound of BiOI material.
Fig. 6 is Bi
2o
3film and Bi
2o
3the UV-Vis absorption spectrum of-BiOI film.Can be observed by figure, Bi
2o
3the visible light-responded point of-BiOI film is about 650nm place, and Bi
2o
3the visible light-responded point of film, about 500nm place, this shows Bi
2o
3the visible absorption district of-BiOI film has and significantly widens.In addition, in whole absorption POP, Bi
2o
3-BiOI film is relative to Bi
2o
3the absorbance of film all has significantly improved.Therefore, Bi
2o
3the formation of-BiOI laminated film improves the visible light-responded performance of photochemical catalyst greatly.
Fig. 7 is the Bi that this embodiment prepares
2o
3film and Bi
2o
3-BiOI film is at 0.1MNa
2sO
4solution in, respectively in the dark with the EIS collection of illustrative plates under visible light conditions.As seen from the figure, in the dark with under visible illumination condition, Bi
2o
3film and Bi
2o
3the arc radius of the EIS spectrogram of-BiOI film is reduction trend, and Bi is described
2o
3film and Bi
2o
3the compound of-BiOI material reduces the compound of photo-generate electron-hole, and improves the transfer rate of carrier.
Fig. 8 is the Bi that this embodiment prepares
2o
3film and Bi
2o
3the electricity conversion comparison diagram of-BiOI film.As seen from the figure, Bi
2o
3-BiOI film in whole wavelength absorption section, electricity conversion is all significantly improved.
Fig. 9 is the Bi that this embodiment prepares
2o
3film and Bi
2o
3the clearance comparison diagram of-BiOI film degradation of phenol under visible photoelectricity condition.As seen from the figure, Bi
2o
3the phenol clearance of film is about 50%, and Bi
2o
3the phenol clearance of-BiOI film is about 90%, visible, relative to independent Bi
2o
3film, Bi
2o
3the efficiency of-BiOI compound film optoelectronic Synergistic degradation organic pollution is greatly improved.
Embodiment 2
Identical with embodiment 1, difference is Bi
2o
3the time (i.e. the time of ion-exchange) of flooding in solution B in the preparation process of-BiOI film is reduced to 30min.
The Bi prepared under the condition of the present embodiment
2o
3the phenol clearance of-BiOI film is 60%.
Embodiment 3
Identical with embodiment 1, difference is Bi
2o
3the time of flooding in solution B in the preparation process of-BiOI film is reduced to 60min.
The Bi prepared under the condition of the present embodiment
2o
3the phenol clearance of-BiOI film is 75%.
Embodiment 4
Identical with embodiment 1, difference is Bi
2o
3the time of flooding in solution B in the preparation process of-BiOI film is increased to 240min.
The Bi prepared under the condition of the present embodiment
2o
3the phenol clearance of-BiOI film is 66%.
Embodiment 5
Identical with embodiment 1, difference is Bi
2o
3the time of flooding in solution B in the preparation process of-BiOI film is increased to 24h.Figure 10 is Bi under this condition
2o
3the SEM collection of illustrative plates of-BiOI, can observe, and through flooding for a long time, the laminated structure area of BiOI has to be increased very significantly, and its size is about 5 μm × 5 μm, and significantly cannot observe Bi due to the content increase of BiOI
2o
3substrate film.
The Bi prepared under the condition of the present embodiment
2o
3the phenol clearance of-BiOI film is 57%.
Embodiment 6
Identical with embodiment 1, difference is Bi
2o
3in the preparation process of-BiOI film, the pH 1mol/L H of solution B
2sO
4be adjusted to 5.
The Bi prepared under the condition of the present embodiment
2o
3the phenol clearance of-BiOI film is 55%.
Embodiment 7
Identical with embodiment 1, difference is Bi
2o
3in the preparation process of-BiOI film, the pH 1mol/L NaOH of solution B is adjusted to 9.
The Bi prepared under the condition of the present embodiment
2o
3the phenol clearance of-BiOI film is 53%.
Can be found out by above embodiment, the Bi prepared under embodiment 1 condition
2o
3the photocatalytic activity of-BiOI hetero-junction thin-film is the strongest.
Above-described detailed description of the invention has been described in detail technical scheme of the present invention and beneficial effect; be understood that and the foregoing is only most preferred embodiment of the present invention; be not limited to the present invention; all make in spirit of the present invention any amendment, supplement and equivalent to replace, all should be included within protection scope of the present invention.
Claims (10)
1. a Bi
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, described photochemical catalyst is membrane structure, comprises conductive substrates and is positioned at the Bi in conductive substrates
2o
3-BiOI hetero-junction thin-film.
2. Bi as claimed in claim 1
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, described Bi
2o
3-BiOI hetero-junction thin-film comprises the Bi be positioned in conductive substrates from the bottom to top successively
2o
3film and be positioned at Bi
2o
3biOI film on film.
3. Bi as claimed in claim 2
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, described Bi
2o
3the thickness of-BiOI hetero-junction thin-film is 1 μm ~ 3 μm.
4. Bi as claimed in claim 3
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, the thickness of described BiOI film is 0.5 μm ~ 2 μm.
5. as the Bi in Claims 1 to 4 as described in any one
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, described Bi
2o
3the surface of-BiOI hetero-junction thin-film is random laminated structure, and described laminated structure is of a size of 0.5 μm × 0.5 μm ~ 5 μm × 5 μm.
6. one kind as the Bi in Claims 1 to 5 as described in any one
2o
3the preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, conductive substrates prepares Bi
2o
3film, then by described Bi
2o
3film is placed in iodide ion solution and carries out ion-exchange, namely obtains described Bi
2o
3-BiOI hetero-junctions visible-light-responsive photocatalyst.
7. the Bi as described in right 6
2o
3the preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, the pH value of described iodide ion solution is 1 ~ 13.
8. the Bi as described in right 6
2o
3the preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, the pH value of described iodide ion solution is 3 ~ 5.
9. the Bi as described in right 6
2o
3the preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, the time of described ion-exchange is 0 ~ 24h.
10. the Bi as described in right 6
2o
3the preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, is characterized in that, the time of described ion-exchange is 1 ~ 4h.
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CN110280278B (en) * | 2019-06-05 | 2022-07-26 | 常州大学 | Iodine vacancy BiO 1.2 I 0.6 /Bi 2 O 3 Photocatalytic composite material and preparation method thereof |
CN113571717A (en) * | 2021-07-23 | 2021-10-29 | 中国人民解放军军事科学院军事医学研究院 | High-efficiency photoelectrode and preparation method and application thereof |
CN113571717B (en) * | 2021-07-23 | 2024-03-19 | 中国人民解放军军事科学院军事医学研究院 | Efficient photoelectrode and preparation method and application thereof |
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