CN104383950B - A kind of Bi2o3-BiOI hetero-junctions visible-light-responsive photocatalyst and preparation method thereof - Google Patents
A kind of Bi2o3-BiOI hetero-junctions visible-light-responsive photocatalyst and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of Bi2O3BiOI hetero-junctions visible-light-responsive photocatalyst and preparation method thereof, this photocatalyst is membrane structure, including conductive substrates and the Bi being positioned in conductive substrates2O3BiOI hetero-junction thin-film.First in conductive substrates, Bi is prepared during preparation2O3Thin film, then by described Bi2O3Thin film is placed in iodide ion solution and carries out ion exchange, i.e. obtains described Bi2O3BiOI hetero-junctions visible-light-responsive photocatalyst.The photocatalyst of the present invention, under sunlight, shows higher visible light catalysis activity, and photoelectric catalysis degrading effect is preferable.And while promoting electronics to shift, it is suppressed that photo-generate electron-hole, to compound, can be used for photoelectric catalysis degrading environmental contaminants, photoelectrocatalysis synthesis and photodissociation Aquatic product hydrogen field.
Description
Technical field
The present invention relates to photocatalyst technology field, particularly to a kind of Bi2O3-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 the problem that the mankind are urgently to be resolved hurrily.Photocatalysis technology arises at the historic moment, and presents its superior application prospect, and a lot of novel photocatalysts are developed and show high photocatalytic activity.
Nineteen eighty-three Pruden and Ollis finds TiO2In sensitization system, the photic mineralization of halogenated organic (such as trichloro ethylene, dichloromethane etc.), makes people clearly realize that TiO2Photocatalytic degradation function to organic pollution, has started the frontier of optically catalytic TiO 2 research.In recent years, along with the development of technology, TiO2Photocatalysis technology shows wide application prospect in terms of administering air pollution and purification of water quality especially.
Band gap wider (anatase type tio2, Eg=3.2eV), can only be less than the ultraviolet light response of 387nm, and ultraviolet light only accounts for reaching the 4～6% of surface solar radiation energy, but visible ray accounts for the 45% of solar radiation energy, causes TiO wavelength2Photocatalyst is the lowest to the utilization rate of sunlight.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 photocatalyst has obtained paying close attention to widely and studying because having good catalysis activity.Typical bismuth oxide (Bi2O3), energy gap band is 2.8eV, and absorbing wavelength is longer, it is seen that the utilization rate of light is higher.Additionally, BiOX also has good conduction and optical property, band-gap energy is 1.7～3.2eV, it is possible to be excited under the irradiation of visible ray, is also a high performance visible light catalyst of class.
For improving visible light catalyst activity, the methods such as modified doping and semiconductors coupling typically can be taked.Wherein semiconductors coupling is that the two kinds of different photocatalysts two kinds of band gap being mutually matched are combined, and forms the composite photo-catalyst of heterojunction structure.Under illumination condition, electronics, hole that this composite photo-catalyst is excited can realize effective mobility, thus greatly reduce the recombination rate of electron hole pair, and then can be effectively improved the photocatalytic activity of quasiconductor.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of Bi2O3-BiOI hetero-junctions visible-light-responsive photocatalyst and preparation method thereof.This preparation method is simple, the heterojunction photocatalyst light induced electron prepared and hole good separating effect, shows higher photocatalytic activity, and photoelectric catalysis degrading pollutant effect is notable.
The Bi of the present invention2O3-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that described photocatalyst is membrane structure, including conductive substrates and the Bi being positioned in conductive substrates2O3-BiOI hetero-junction thin-film.
Wherein, Bi2O3-BiOI hetero-junction thin-film includes the Bi being positioned in conductive substrates the most successively2O3Thin film and be positioned at Bi2O3BiOI thin film on thin film.
Conductive substrates mostly is electro-conductive glass (FTO) material.
The present invention is by Bi2O3Carry out being combined with BiOI semi-conducting material and be prepared as Bi2O3-BiOI heterojunction photocatalyst, can be effectively improved visible light-responded property photoelectric current and the photocatalytic activity of catalyst.Bi2O3Being 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 quasiconductor possessing narrow band-gap energy is easily activated by visible ray and produces hole and electronics.While BiOI is activated, the absorbable high photon energy of BiOI can make the electronics in its valence band be excited to higher electric potential energy band (-0.68V).
The position of energy band of restructuring makes the conduction band of BiOI compare Bi2O3Conduction band more active.Therefore, the electronics produced on BiOI surface can transfer to Bi easily2O3Conduction band up, only stay hole in the valence band of BiOI.Additionally, Bi2O3Also it can absorb some visible light to be activated, stay the hole in valence band and can transfer 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 and hole have just reached the effect of high efficiency separation.The light induced electron of high separation and hole avoid compound probability so that it is each self energy preferably carries out aoxidizing and reduction reaction.Therefore, the Bi of formation2O3-BiOI heterojunction photocatalyst is relative to single Bi2O3Or BiOI catalyst has shown more preferable photocatalysis performance in terms of degradation of contaminant.
The Bi of the present invention2O3-BiOI hetero-junctions visible-light-responsive photocatalyst is membrane structure, considerably increases the specific surface area of photocatalyst, and then substantially increases photocatalysis efficiency.
Described Bi2O3The thickness of-BiOI hetero-junction thin-film is 1～3 μm.This thickness range can be expanded according to the actual requirements.Bi2O3The light that when-BiOI hetero-junction thin-film thickness is the thinnest, film absorbs is few；The thickest photo-generate electron-hole of thickness is easily combined.Preferably, described Bi2O3The thickness of-BiOI hetero-junction thin-film is 2～3 μm.
The thickness of described BiOI thin film is 0.5～2 μm.And the thickness of BiOI thin film is less than Bi2O3-BiOI hetero-junction thin-film.
Described Bi2O3The surface of-BiOI hetero-junction thin-film structure in the form of sheets, the size of described laminated structure is 0.5 μ m 0.5 μm～5 μ m 5 μm..
Present invention also offers a kind of Bi2O3The preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, first prepares Bi in conductive substrates2O3Thin film, then by described Bi2O3Thin film is placed in iodide ion solution and carries out ion exchange, i.e. obtains described Bi2O3-BiOI hetero-junctions visible-light-responsive photocatalyst.Specifically include following steps:
(S1) conductive substrates will contain Bi after cleaning and drying3+With HNO3Ethylene glycol solution slowly drop to (HNO on the conducting surface of described conductive substrates3It is acidity for regulating ethylene glycol solution), vacuum drying, calcining, obtain Bi2O3Thin film；
Preferably, Bi described in this step3+With HNO3Ethylene glycol solution be containing Bi (NO3)3With HNO3The ethylene glycol solution of (68.0%～70%).
Preferably, Bi (NO in ethylene glycol solution described in this step3)3It is 2～6g:20ml with the mass volume ratio of ethylene glycol solution, HNO3The amount of material be 0.01～0.03mol.
It is further preferred that vacuum drying temperature described in this step is 50～100 DEG C, calcining heat is 300～700 DEG C, and calcination time is 1～6h.
Most preferably, Bi (NO3)3It is 4g:20ml, HNO with the mass volume ratio of ethylene glycol solution3The amount of material 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) being dissolved in distilled water by KI, regulate the pH of solution according to the needs preparing different-shape sample, pH value scalable interval is 1～13, the Bi that will obtain in step one2O3Thin film is immersed in this iodide ion solution, obtains Bi2O3-BiOI hetero-junction thin-film.
Use the H of 1mol/L2SO4Or the pH value of the NaOH regulation iodide ion solution of 1mol/L, it is preferable that pH is adjusted to 2～10, and soak time is 0～24h.
It is further preferred that use the H of 1mol/L2SO4Being adjusted to pH is 3～5, and soak time is 1～4h.
Most preferably, the H of 1mol/L is used2SO4Being adjusted to pH is 3, and soak time is 2h.
Bi in the present invention2O3The photoelectric catalytically active of-BiOI heterojunction photocatalysis thin film and Bi2O3The time soaked in iodide ion solution about: time of immersion can make that the I-in solution exchanges the most for a long time too much, cause the BiOI of generation to account for the component of thin film excessive, affect Bi2O3And the synergism between BiOI quasiconductor, the photo-generate electron-hole separation efficiency resulted in is cut down.The time soaked is the shortest, and the BiOI generated is very few, affects the synergism between two kinds of quasiconductors equally.Therefore, under this preferred soak time, the Bi contained by thin film2O3Fit mutually with BiOI component, the synergism of hetero-junctions can be promoted, reach to promote the purpose that photo-generate electron-hole efficiently shifts separation, and then improve the photocatalytic activity of thin film.
In the present invention, iodide ion solution is interpreted as the solution containing iodide ion, the usually alkali metal salt of iodine, such as KI or NaI solution.
Compared with prior art, beneficial effects of the present invention:
(1) present invention is prepared for a kind of Bi2O3-BiOI hetero-junctions visible-light-responsive photocatalyst, two kinds of photocatalysts with different band structure are utilized to combine, the light induced electron and the hole that make two kinds of material surfaces generations efficiently separate, and the synergism of formation substantially increases the organic performance of photocatalyst for degrading.
(2) Bi of the present invention2O3-BiOI heterojunction photocatalyst has good visible ray photoelectrochemical behaviour, under visible light illumination, the Bi prepared in the process of the present invention2O3The photoelectric current of-BiOI composite photo-catalyst is relative to Bi2O3Improve about 7 times；
(3) Bi of the present invention2O3-BiOI heterojunction photocatalyst is membrane structure, considerably increase the specific surface area of photocatalyst, be greatly improved catalytic efficiency, under sunlight, show good visible ray electrically-degradable pollutant performance, can be used for the field such as photoelectric catalysis degrading environmental contaminants, photoelectrocatalysis synthesis；
(4) Bi of the present invention2O3The preparation technology of-BiOI heterojunction photocatalyst is simple, by the time-controllable to dip time, forms the Bi of different single Component molar content2O3-BiOI heterojunction photocatalysis thin film.
Accompanying drawing explanation
Fig. 1 is Bi2O3The SEM figure of film surface appearance；
Fig. 2 is the Bi of 2h for dipping duration (ion-exchange time)2O3The SEM figure of-BiOI film surface appearance；
The Bi of a length of 2h when Fig. 3 is dipping2O3The SEM figure of-BiOI thin-membrane section pattern；
Fig. 4 is Bi2O3Thin film and Bi2O3The XRD figure of-BiOI thin film；
Fig. 5 a is Bi2O3Thin film and Bi2O3-BiOI thin film is at 0.1M Na2SO4With 0.1M Na2SO3Mixed solution in, it is seen that light irradiate under linear sweep voltammetry curve；
Fig. 5 b is Bi2O3And Bi2O3-BiOI thin film is at 0.1M Na2SO4With 0.1M Na2SO3Mixed solution in, ultraviolet-visible irradiate under linear sweep voltammetry curve；
Fig. 6 is Bi2O3And Bi2O3The UV-Vis absorption spectrum of-BiOI thin film；
Fig. 7 is Bi2O3And Bi2O3-BiOI thin film is at 0.1M Na2SO4Solution in, respectively the most in the dark with the EIS collection of illustrative plates under visible light conditions；
Fig. 8 is Bi2O3Thin film and Bi2O3The electricity conversion comparison diagram of-BiOI thin film；
Fig. 9 is Bi2O3Thin film and Bi2O3-BiOI thin film is the clearance comparison diagram of degradation of phenol under the conditions of visible photoelectricity；
The Bi of a length of 24h when Figure 10 is dipping2O3The 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 used in following embodiment be commercially available prod.Employing flies to receive desk-top scanning electron microscope (Phenom G2 Pro) and characterizes surface texture and the fractions distribution of thin film.Electron gun: 1500 hours CeB6 filaments, the pumpdown time: 10 seconds.
Embodiment 1
The Bi of the present embodiment2O3-BiOI hetero-junctions visible-light-responsive photocatalyst is made by the steps and obtains:
(1) by 4g Bi (NO3)3·5H2O is dissolved in 20ml ethylene glycol solution, adds 0.02molHNO3(68.0%～70%), magnetic agitation 20min forms homogeneous transparent solution, take this solution 20 μ l, it is coated with the conducting surface (10mm × 10mm) dropping in conductive substrates, put in vacuum drying oven and dry, after being warmed up to 500 DEG C with 5 DEG C/min in Muffle furnace, cycle annealing processes 3h, obtains Bi2O3Thin film.
The conductive substrates of this enforcement is FTO glass (Fluorin doped tin-oxide, fluorine-doped tin oxide).Specification is 10mm × 50mm × 2mm.Preparation Bi2O3First FTO glass is carried out ultrasonic cleaning 5min with acetone, dehydrated alcohol and deionized water successively during thin film, then take out and dry.
The Bi prepared2O3The surface texture of thin film is as it is shown in figure 1, surface has intensive cavernous structure.This structure is conducive to the ion between solution and thin film to exchange, and then promotes the generation of BiOI thin film.
(2) by Bi2O3Thin film is placed in ligand solution immersion 2h and carries out ion exchange, naturally dries, obtain Bi after taking-up in distilled water in soaking flushing air2O3-BiOI thin film is Bi2O3-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 with 1M (i.e. 1mol/L) H2SO4It is 3 that solution B is adjusted to pH.
Bi in the present embodiment2O3-BiOI hetero-junctions visible-light-responsive photocatalyst, for membrane structure, including conductive substrates and the Bi that is positioned in conductive substrates2O3-BiOI hetero-junction thin-film.Fig. 2 is the SEM image of the surface texture of the photocatalyst of the present embodiment.It is observed that work as Bi2O3After thin film immerses KI solution, BiOI is that obvious random laminated structure is grown in Bi2O3The top of thin film, and the position generated is at Bi2O3Near the cavernous structure of thin film.The size of laminated structure is 1 μ m 1 μm, and thickness is 240nm.Random laminated structure surface is conducive to Bi2O3Combining closely with BiOI, the staggered laminated structure of formation considerably increases the specific surface area of material.
Fig. 3 is the Bi of the present embodiment2O3The SEM image of the section of-BiOI hetero-junctions visible-light-responsive photocatalyst, it can be seen that the photocatalyst obtained includes conductive substrates, the Bi being positioned in conductive substrates2O3Thin film and be positioned at Bi2O3BiOI thin film on thin film.Bi2O3The thickness of-BiOI hetero-junction thin-film is 2.5 μm, and the thickness of BiOI thin film is 1 μm.
Fig. 4 is the Bi that the present embodiment prepares2O3Thin film and Bi2O3The XRD figure spectrum contrast of-BiOI thin film.Can be seen that Bi2O3The collection of illustrative plates of-BiOI thin film is at Bi2O3Substantially having had more the diffractive features peak of BiOI material on the basis of the collection of illustrative plates of thin film, this explanation is at Bi2O3It is successfully generated BiOI on thin film, and two kinds of materials have combined well.
Fig. 5 a is the Bi that the present embodiment prepares2O3Thin film and Bi2O3-BiOI thin film linear sweep voltammetry curve under visible light illumination；Fig. 5 b is the Bi that this embodiment prepares2O3And Bi2O3-BiOI thin film linear sweep voltammetry curve under ultraviolet-visible irradiates.From Fig. 5 a and 5b, relative to Bi2O3Thin film, Bi2O3The photoelectric current of-BiOI thin film, under visible ray and ultraviolet-visible irradiate, has been respectively increased 7 times and 8.5 times, it is seen that Bi2O3The compound photoelectric catalytically active being greatly improved material with BiOI material.
Fig. 6 is Bi2O3Thin film and Bi2O3The UV-Vis absorption spectrum of-BiOI thin film.By figure it is observed that Bi2O3The visible light-responded point of-BiOI thin film is about at 650nm, and Bi2O3The visible light-responded point of thin film, about at 500nm, this shows Bi2O3The visible absorption district of-BiOI thin film has and significantly widens.Additionally, in whole absorption POP, Bi2O3-BiOI thin film is relative to Bi2O3The absorbance of thin film suffers from significantly improving.Therefore, Bi2O3The formation of-BiOI laminated film is greatly improved the visible light-responded performance of photocatalyst.
Fig. 7 is the Bi that this embodiment prepares2O3Thin film and Bi2O3-BiOI thin film is at 0.1MNa2SO4Solution in, respectively the most in the dark with the EIS collection of illustrative plates under visible light conditions.As seen from the figure, under the conditions of in the dark shining with visible ray, Bi2O3Thin film and Bi2O3The arc radius of the EIS spectrogram of-BiOI thin film, in reducing trend, illustrates Bi2O3Thin film and Bi2O3The 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 prepares2O3Thin film and Bi2O3The electricity conversion comparison diagram of-BiOI thin film.As seen from the figure, Bi2O3-BiOI thin film in whole wavelength absorption section, electricity conversion is all significantly improved.
Fig. 9 is the Bi that this embodiment prepares2O3Thin film and Bi2O3-BiOI thin film is the clearance comparison diagram of degradation of phenol under the conditions of visible photoelectricity.As seen from the figure, Bi2O3The phenol clearance of thin film is about 50%, and Bi2O3The phenol clearance of-BiOI thin film is about 90%, it is seen then that relative to single Bi2O3For thin film, Bi2O3The efficiency of-BiOI compound film optoelectronic Synergistic degradation organic pollution is greatly improved.
Embodiment 2
Same as in Example 1, difference is Bi2O3In the preparation process of-BiOI thin film, in solution B, the time (i.e. the time of ion exchange) of dipping is reduced to 30min.
The Bi of preparation under conditions of the present embodiment2O3The phenol clearance of-BiOI thin film is 60%.
Embodiment 3
Same as in Example 1, difference is Bi2O3In the preparation process of-BiOI thin film, in solution B, the time of dipping is reduced to 60min.
The Bi of preparation under conditions of the present embodiment2O3The phenol clearance of-BiOI thin film is 75%.
Embodiment 4
Same as in Example 1, difference is Bi2O3In the preparation process of-BiOI thin film, in solution B, the time of dipping increases to 240min.
The Bi of preparation under conditions of the present embodiment2O3The phenol clearance of-BiOI thin film is 66%.
Embodiment 5
Same as in Example 1, difference is Bi2O3In the preparation process of-BiOI thin film, in solution B, the time of dipping increases to 24h.Figure 10 is Bi under this condition2O3The SEM collection of illustrative plates of-BiOI, it can be observed that, through dipping for a long time, the laminated structure area of BiOI has significant increase, and its size is about 5 μ m 5 μm, and owing to Bi cannot have significantly been observed in the content increase of BiOI2O3Substrate film.
The Bi of preparation under conditions of the present embodiment2O3The phenol clearance of-BiOI thin film is 57%.
Embodiment 6
Same as in Example 1, difference is Bi2O3In the preparation process of-BiOI thin film, the pH of solution B 1mol/L H2SO4It is adjusted to 5.
The Bi of preparation under conditions of the present embodiment2O3The phenol clearance of-BiOI thin film is 55%.
Embodiment 7
Same as in Example 1, difference is Bi2O3In the preparation process of-BiOI thin film, the pH 1mol/L NaOH of solution B is adjusted to 9.
The Bi of preparation under conditions of the present embodiment2O3The phenol clearance of-BiOI thin film is 53%.
Be can be seen that by above example, the Bi of preparation under the conditions of embodiment 12O3The photocatalytic activity of-BiOI hetero-junction thin-film is the strongest.
Technical scheme and beneficial effect have been described in detail by above-described detailed description of the invention; it it should be understood that and the foregoing is only presently most preferred embodiment of the invention; it is not limited to the present invention; all made in the spirit of the present invention any amendment, supplement and equivalent etc., should be included within the scope of the present invention.
Claims (9)
1. a Bi2O3-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that described photocatalyst is membrane structure, including conductive substrates and the Bi being positioned in conductive substrates2O3-BiOI hetero-junction thin-film；Described Bi2O3-BiOI hetero-junction thin-film includes the Bi being positioned in conductive substrates the most successively2O3Thin film and be positioned at Bi2O3BiOI thin film on thin film.
2. Bi as claimed in claim 12O3-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that described Bi2O3The thickness of-BiOI hetero-junction thin-film is 1 μm～3 μm.
3. Bi as claimed in claim 22O3-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that the thickness of described BiOI thin film is 0.5 μm～2 μm.
4. the Bi as described in any one in claims 1 to 32O3-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that described Bi2O3The surface of-BiOI hetero-junction thin-film is random laminated structure, and the size of described laminated structure is 0.5 μ m 0.5 μm～5 μ m 5 μm.
5. the Bi as described in any one in Claims 1 to 42O3The preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that prepare Bi in conductive substrates2O3Thin film, then by described Bi2O3Thin film is placed in iodide ion solution and carries out ion exchange, i.e. obtains described Bi2O3-BiOI hetero-junctions visible-light-responsive photocatalyst.
6. Bi as claimed in claim 52O3The preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that the pH value of described iodide ion solution is 1～13.
7. Bi as claimed in claim 52O3The preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that the pH value of described iodide ion solution is 3～5.
8. Bi as claimed in claim 52O3The preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that the time of described ion exchange is 0～24h.
9. Bi as claimed in claim 52O3The preparation method of-BiOI hetero-junctions visible-light-responsive photocatalyst, it is characterised in that the time of described ion exchange is 1～4h.
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| CN107754837B (en) * | 2017-09-21 | 2020-10-13 | 浙江工商大学 | Single-layer carbon nitride nanosheet and bismuth plasma combined modified bismuth oxide-based electrode and preparation and application thereof |
| CN108187699B (en) * | 2018-01-31 | 2021-01-05 | 安徽师范大学 | BiOX-Bi4O5X2Heterojunction and preparation method and application thereof |
| 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 |
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