CN110791777B - Bismuth vanadate electrode rich in surface oxygen vacancies and preparation method and application thereof - Google Patents

Bismuth vanadate electrode rich in surface oxygen vacancies and preparation method and application thereof Download PDF

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CN110791777B
CN110791777B CN201911036370.XA CN201911036370A CN110791777B CN 110791777 B CN110791777 B CN 110791777B CN 201911036370 A CN201911036370 A CN 201911036370A CN 110791777 B CN110791777 B CN 110791777B
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bismuth vanadate
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oxygen vacancies
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巩金龙
冯时佳
王拓
刘斌
胡聪玲
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Tianjin University
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Abstract

The invention belongs to the technical field of photoelectrochemical cell semiconductor electrodes, and discloses a bismuth vanadate electrode rich in surface oxygen vacancies, a preparation method and application thereof, wherein the electrode comprises a conductive substrate layer and a bismuth vanadate layer, and the bismuth vanadate layer is obtained by modification through photoetching; firstly, growing bismuth vanadate particles on a conductive substrate by adopting a metallorganic decomposition method, then immersing the bismuth vanadate particles in an alkaline buffer solution containing sulfite, and simultaneously applying illumination with certain time, certain wavelength and certain intensity to finish the preparation of the whole electrode; the electrode can be assembled into a photoelectrochemical cell for hydrogen production by water photolysis of the photoelectrochemical cell. The oxygen vacancy is introduced into the surface layer of the bismuth vanadate electrode, so that the charge separation efficiency of a solid-liquid interface is effectively improved, the photoelectric conversion efficiency of the photoelectrochemical cell is improved, the operation is simple, the oxygen vacancy introduction efficiency is high, and meanwhile, vacuum equipment is not needed, so that the operation cost is extremely low, and the large-scale production is facilitated.

Description

Bismuth vanadate electrode rich in surface oxygen vacancies and preparation method and application thereof
Technical Field
The invention belongs to the technical field of photoelectrochemical cell semiconductor electrodes, and particularly relates to a bismuth vanadate electrode and a preparation method and application thereof.
Background
Energy and environment become the focus of global attention, and the photoelectrochemical cell photolysis water to produce hydrogen can convert solar energy into hydrogen energy to be stored1And hydrogen as a clean energy can effectively alleviate environmental problems. Therefore, the function of the photoelectrochemical cell for photolyzing water to produce hydrogen cannot be ignored2
In the research of hydrogen production by photolysis of water in a photoelectrochemical cell, monoclinic bismuth vanadate is the most widely used semiconductor anode material with visible light response at present3-4. However, the photocurrent of bismuth vanadate still has a large gap from the theoretical value, mainly due to poor charge transport and carrier separation capability5. Bulk doping of impurity elements can effectively increase the majority carrier concentration of bismuth vanadate, thereby improving charge transport capability, but this approach inevitably introduces new recombination centers6. Similar effects can be obtained by bulk phase introduction of oxygen vacancies, however, the bulk phase oxygen vacancy content is not easily controlled. Proper oxygen vacancy content can improve the performance of the bismuth vanadate, but too many oxygen vacancies can become recombination centers7. The oxygen vacancy of the surface layer or the sub-surface layer can effectively improve the photoelectric property of the semiconductor anode and simultaneously can avoid the generation of a bulk phase recombination center8. For bismuth vanadate, the introduction of surface oxygen vacancies is minimal.
Therefore, the introduction of surface oxygen vacancies is a critical scientific and technical problem which needs to be solved urgently in the existing bismuth vanadate thin film electrode.
(1)Chang,X.X.;Wang,T.;Gong,J.L.,CO2 photo-reduction:insights into CO2activation and reaction on surfaces of photocatalysts.Energy Environ.Sci.2016,9(7),2177-2196.
(2)Kobayashi,H.;Sato,N.;Orita,M.;Kuang,Y.;Kaneko,H.;Minegishi,T.;Yamada,T.;Domen,K.,Development of highly efficient CuIn0.5Ga0.5Se2-based photocathode and application to overall solar driven water splitting.Energy Environ.Sci.2018,11(10),3003-3009.
(3)Wang,S.;Chen,P.;Bai,Y.;Yun,J.H.;Liu,G.;Wang,L.,New BiVO4 Dual Photoanodes with Enriched Oxygen Vacancies for Efficient Solar-Driven Water Splitting.Adv.Mater.2018,30(20),1800486.
(4)Han,H.S.;Shin,S.;Kim,D.H.;Park,I.J.;Kim,J.S.;Huang,P.S.;Lee,J.K.;Cho,I.S.;Zheng,X.L.,Boosting the solar water oxidation performance of a BiVO4photoanode by crystallographic orientation control.Energy Environ.Sci.2018,11(5),1299-1306.
(5)Park,Y.;McDonald,K.J.;Choi,K.S.,Progress in bismuth vanadate photoanodes for use in solar water oxidation.Chem.Soc.Rev.2013,42(6),2321-37.
(6)Luo,W.J.;Li,Z.S.;Yu,T.;Zou,Z.G.,Effects of Surface Electrochemical Pretreatment on the Photoelectrochemical Performance of Mo-Doped BiVO4.J.Phys.Chem.C 2012,116(8),5076-5081.
(7)Zhang,J.J.;Chang,X.X.;Li,C.C.;Li,A.;Liu,S.S.;Wang,T.;Gong,J.L.,WO3photoanodes with controllable bulk and surface oxygen vacancies for photoelectrochemical water oxidation.J.Mater.Chem.A2018,6(8),3350-3354.
(8)Li,L.;Yan,J.;Wang,T.;Zhao,Z.;Zhang,J.;Gong,J.;Guan,N.,Sub-10nm rutile titanium dioxide nanoparticles for efficient visible-light-driven photocatalytic hydrogen production.Nat.Commun.2015,6,5881.
Disclosure of Invention
The invention aims to solve the technical problem of introducing oxygen vacancies into the surface layer of a bismuth vanadate film electrode, and provides a bismuth vanadate electrode rich in surface layer oxygen vacancies, a preparation method and application thereof in photocatalysis.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a bismuth vanadate electrode rich in surface oxygen vacancies comprises a conductive substrate layer and a bismuth vanadate layer; the electrode is obtained by growing bismuth vanadate particles on a conductive substrate to obtain a bismuth vanadate electrode, and then immersing the bismuth vanadate electrode in an alkaline buffer solution containing sulfite for photoetching modification.
Further, the conductive substrate layer is FTO conductive glass or ITO conductive glass.
Further, the sulfite is potassium sulfite or sodium sulfite.
Further, the concentration of the sulfite is 0.05-0.5 mol/L.
Further, the photoetching modification adopts a wavelength of 200-1000nm and an intensity of 10-100mW/cm2The illumination time of the light source is 1-30 min.
The preparation method of the bismuth vanadate electrode rich in surface oxygen vacancies comprises the steps of immersing the bismuth vanadate electrode in a buffer solution which contains 0.05-0.5mol/L of sulfite and has the pH value of 9-10, and simultaneously applying a solution with the wavelength of 200-1000nm and the intensity of 10-100mW/cm2The illumination time is 1-30min, and the target product can be obtained.
Further, the bismuth vanadate electrode is prepared by adopting a metallorganic decomposition method, and the method specifically comprises the following steps:
(1) dropwise adding the precursor solution onto a conductive substrate which is preheated to 25-60 ℃, and uniformly coating the surface of the conductive substrate with the precursor solution; the precursor is a mixed solution of bismuth nitrate and vanadium oxide acetylacetonate, the solvent is dimethyl sulfoxide, and the molar concentrations of the bismuth nitrate and the vanadium oxide acetylacetonate are the same and are both 0.1-1 mol/L;
(2) and (2) sintering the sample obtained in the step (1) at a high temperature in the air or oxygen atmosphere, and then cooling to room temperature to obtain the bismuth vanadate electrode.
Further, the temperature of the high-temperature sintering in the step (2) is 450-500 ℃.
The bismuth vanadate electrode rich in the surface oxygen vacancies is used as a working electrode, a platinum sheet electrode is used as a counter electrode, and a silver/silver chloride electrode is used as a reference electrode, so that a photoelectrochemical cell is assembled.
The invention has the beneficial effects that:
according to the invention, the oxygen vacancy is successfully introduced into the surface layer of the bismuth vanadate electrode by a photoetching method, and the bismuth vanadate thin film electrode rich in the oxygen vacancy of the surface layer has higher majority carrier concentration and higher charge separation efficiency of a solid-liquid interface, so that the bismuth vanadate thin film electrode has higher photoelectric conversion efficiency and photocurrent density in a photoelectrochemical cell. In addition, the invention only introduces oxygen vacancy on the surface layer of the bismuth vanadate electrode, thereby effectively avoiding the generation of bulk phase defect sites. This facilitates increased interfacial charge separation by the introduction of surface oxygen vacancies, while avoiding bulk oxygen vacancies from introducing new bulk recombination centers.
Compared with the prior art (such as a plasma etching method) for introducing oxygen vacancies, the method has the advantages of simple and easy operation, low cost because no vacuum equipment is needed, and contribution to industrial production. Meanwhile, the operation condition of the invention is mild, and only oxygen vacancy is introduced into the surface layer of the bismuth vanadate, so that the conductive substrate is not substantially damaged.
The bismuth vanadate electrode obtained by the invention is used for an anode for hydrogen production by photolysis of water, can efficiently carry out the reaction of photolysis of water, and has better application prospect.
Drawings
FIG. 1 is a sectional view of a scanning electron microscope of a bismuth vanadate electrode prepared in example 1, with a scale of 500 nm;
FIG. 2 is a plan view of a scanning electron microscope of a bismuth vanadate electrode prepared in example 1, with a scale of 500 nm;
FIGS. 3 to 4 are comparative graphs of X-ray photoelectron spectra of the bismuth vanadate electrode prepared in example 1 before and after modification by photolithography;
FIG. 5 is a comparison graph of the model-Schottky curves of the bismuth vanadate electrode prepared in example 1 before and after modification by photolithography;
fig. 6 is a graph comparing photocurrent-voltage curves of the bismuth vanadate electrode prepared in example 1 before and after modification by photolithography under simulated sunlight irradiation.
Detailed Description
The present invention is further described in detail below by way of specific examples, which will enable one skilled in the art to more fully understand the present invention, but which are not intended to limit the invention in any way.
Example 1
(1) Preparing a precursor solution: 0.2425g of bismuth nitrate and 0.1325g of vanadium oxide acetylacetonate are weighed and dissolved in 500 mu L of dimethyl sulfoxide to obtain 1mol/L precursor solution;
(2) 75 μ L of the precursor solution was applied dropwise to 2X 2cm preheated to 60 deg.C2On FTO conductive glass;
(3) uniformly coating the precursor solution on FTO (fluorine-doped tin oxide) by a spin coater according to certain spin coating parameters, wherein the spin coating parameters are that the spin coating parameters are kept at 1000rpm for 20s, the spin coating parameters are kept at 4000rpm for 40s, and the acceleration is 1000 rpm/s;
(4) placing the sample in a tubular furnace in an air atmosphere for sintering, wherein the sintering system is that the temperature is kept for 2h at 500 ℃ and the heating rate is 5 ℃/min, and then cooling to the room temperature to obtain a bismuth vanadate thin film electrode (marked as BVO);
(5) immersing the bismuth vanadate film electrode in 1mol/L potassium borate solution containing 0.5mol/L sodium sulfite and having pH of 9.2, and simultaneously applying light with wavelength range of 200-1000nm and illumination intensity of 100mW/cm2The illumination time is 10min, and the photoetching modified bismuth vanadate thin film electrode (marked as PE-BVO) is obtained.
(6) And assembling the obtained electrode as a working electrode, a platinum sheet electrode as a counter electrode and a silver/silver chloride electrode as a reference electrode into a photoelectrochemical cell for photoelectric performance test. The photoelectric property test condition is that the electrolyte is 1mol/L boric acid buffer solution with pH of 9.0 and containing 0.2mol/L sodium sulfite; the illumination area of the working electrode is 0.5cm2(ii) a The light source is simulated sunlight obtained by matching a 300W xenon lamp with an AM 1.5G optical filter, and the light intensity at the working electrode of the photoelectrochemical cell is 10 after being tested by an radiometer0mW/cm2
Example 2:
the reaction was carried out by the method of example 1, except that step (5) was not included.
Example 3:
the reaction was carried out by the method of example 1, except that the substrate in the step (2) was ITO conductive glass.
Example 4:
the reaction was carried out by the method of example 2, except that the substrate in the step (2) was ITO conductive glass.
Example 5:
the reaction was carried out using the method of example 1, except that the sulfite of step (5) was potassium sulfite.
Example 6:
the reaction was carried out by the method of example 1 except that the sodium sulfite concentration in step (5) was 0.05 mol/L.
Example 7:
the reaction was carried out by the method of example 1 except that the sodium sulfite concentration in step (5) was 0.25 mol/L.
Example 8:
the reaction was carried out by the method of example 1 except that the light source intensity of step (5) was 10mW/cm2
Example 9:
the reaction was carried out by the method of example 1 except that the light source intensity of step (5) was 50mW/cm2
Example 10:
the reaction was carried out by the method of example 1 except that the light irradiation time of step (5) was 1 min.
Example 11:
the reaction was carried out by the method of example 1 except that the light irradiation time in step (5) was 30 min.
Example 12:
the reaction was carried out by the method of example 1, except that the FTO temperature in step (2) was 25 ℃.
Example 13:
the reaction was carried out by the method of example 1, except that the FTO temperature in step (2) was 40 ℃.
Example 14:
the reaction was carried out by the method of example 1 except that the precursor concentration in step (2) was 0.1 mol/L.
Example 15:
the reaction was carried out by the method of example 1, except that the precursor concentration in step (2) was 0.5 mol/L.
The electrodes obtained in examples 1 to 15 were subjected to a photoelectric property test, and the photoelectric properties were measured as photocurrents (mA/cm) of 0.6V (relative to a reversible hydrogen electrode) in a voltage-photocurrent curve2) Is used as an index.
Figure BDA0002251612090000061
As can be seen from the table, the photoelectric performance of the bismuth vanadate electrode in the photoelectrochemical cell is effectively improved by the photoetching method. Specifically, under the voltage of 0.6V (relative to the reversible hydrogen electrode), the photocurrent density of the bismuth vanadate electrode is improved after the photoetching treatment. Therefore, the invention proves that the oxygen vacancy is successfully introduced into the surface layer of the bismuth vanadate electrode, and the bismuth vanadate thin-film electrode rich in the oxygen vacancy of the surface layer has higher majority carrier concentration and higher charge separation efficiency of a solid-liquid interface, thereby showing higher photoelectric conversion efficiency and photocurrent density in a photoelectric cell. Compared with the prior art, the bismuth vanadate electrode prepared by the method has stronger competitive power on the aspects of simplicity of operation and photoelectric property.
As shown in FIG. 1, it can be seen from the cross-sectional view of the scanning electron microscope that the PE-BVO thin film is regularly grown on the FTO substrate, and the thickness of the thin film is 200-210 nm.
As shown in the attached figure 2, the PE-BVO film has a nano-porous structure and a particle size of 50-150nm as seen from a scanning electron microscope top view.
As shown in the attached figures 3-4, it can be seen from the comparison graphs of X-ray photoelectron spectra that Bi and V both shift to low binding energy after the bismuth vanadate film is modified by photoetching, which indicates that the photoetching promotes the generation of surface oxygen vacancies.
As shown in fig. 5, it can be seen from the comparison graph of the model-schottky curves that the carrier concentration of the bismuth vanadate film is effectively increased after the photo-etching modification.
As shown in fig. 6, it can be seen from the photo-current-potential comparison graph that after the bismuth vanadate film is modified by photo-etching, the photo-current is significantly improved, and the advantage of photo-etching modification in the aspect of photo-electric performance is reflected.
As can be seen from the results of comparing examples 1 and 2, the photo-etching effectively improved the photocurrent of the bismuth vanadate electrode from 1.35mA/cm2Lifting the mixture to 3.53mA/cm2
It can be seen from the results of comparing examples 3 and 4 that the photo-etching still effectively improves the photocurrent of the bismuth vanadate electrode. Meanwhile, comparing the results of examples 1 and 2 with those of examples 3 and 4, it is understood that the effect of the photo etching is applicable to both FTO and ITO substrates.
It can be seen from the results of comparative examples 1 and 5 that the effect of photo-etching on the photocurrent of the bismuth vanadate electrode is maintained even when sodium sulfite is replaced with potassium sulfite.
The results of comparative examples 1, 6 and 7 show that the higher the concentration of sodium sulfite, the better the effect of the photolithography on enhancing the bismuth vanadate electrode.
The results of comparative examples 1, 8 and 9 show that the higher the illumination intensity, the better the promotion effect of the photoetching on the bismuth vanadate electrode.
It can be seen from the results of comparative examples 1, 10 and 11 that the longer the illumination time, the better the promotion effect of the photolithography on the bismuth vanadate electrode, but the illumination time of 10min is enough to promote the photocurrent to the maximum value.
It can be seen from the results of comparative examples 1, 12 and 13 that the higher the substrate temperature, the higher the photocurrent of the resulting bismuth vanadate electrode, because increasing the substrate temperature can increase the thickness of the bismuth vanadate film, thereby increasing the light absorption of the bismuth vanadate electrode.
It can be seen from the results of comparative examples 1, 14 and 15 that the higher the precursor concentration is, the higher the photocurrent of the obtained bismuth vanadate electrode is, because the precursor concentration can increase the thickness of the bismuth vanadate film, thereby improving the light absorption of the bismuth vanadate electrode.
Although the preferred embodiments of the present invention have been described above with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and those skilled in the art can make various changes and modifications within the spirit and scope of the present invention without departing from the spirit and scope of the appended claims.

Claims (9)

1. A bismuth vanadate electrode rich in surface oxygen vacancies is characterized by comprising a conductive substrate layer and a bismuth vanadate layer; the electrode is obtained by growing bismuth vanadate particles on a conductive substrate to obtain a bismuth vanadate electrode, and then immersing the bismuth vanadate electrode in an alkaline buffer solution containing sulfite for photoetching modification;
the content of sulfite in the alkaline buffer solution is 0.05-0.5mol/L, and the pH value of the alkaline buffer solution is 9-10; the light wavelength applied by the photoetching is 200-1000nm, and the light intensity is 10-100mW/cm2The illumination time is 1-30 min.
2. The bismuth vanadate electrode rich in surface oxygen vacancies according to claim 1, wherein the conductive substrate layer is FTO conductive glass or ITO conductive glass.
3. The bismuth vanadate electrode rich in epilayer oxygen vacancies according to claim 1, wherein the sulfite is potassium sulfite or sodium sulfite.
4. The bismuth vanadate electrode rich in epilayer oxygen vacancies according to claim 1, wherein the concentration of sulfite is 0.05-0.5 mol/L.
5. The bismuth vanadate electrode rich in surface oxygen vacancies as claimed in claim 1, wherein the modification by photolithography employs a wavelength of 200-1000nm and an intensity of 10-100mW/cm2The illumination time of the light source is 1-30 min.
6. A method for preparing the bismuth vanadate electrode rich in oxygen vacancies on the surface layer according to any one of claims 1 to 5, wherein the bismuth vanadate electrode is immersed in a buffer solution containing 0.05 to 0.5mol/L of sulfite and having a pH of 9 to 10 while applying a solution having a wavelength of 200-1000nm and an intensity of 10 to 100mW/cm2The illumination time is 1-30min, and the target product can be obtained.
7. The method for preparing a bismuth vanadate electrode rich in oxygen vacancies on the surface layer according to claim 6, wherein the bismuth vanadate electrode is prepared by a metallorganic decomposition method, and the method comprises the following steps:
(1) dropwise adding the precursor solution onto a conductive substrate which is preheated to 25-60 ℃, and uniformly coating the surface of the conductive substrate with the precursor solution; the precursor is a mixed solution of bismuth nitrate and vanadium oxide acetylacetonate, the solvent is dimethyl sulfoxide, and the molar concentrations of the bismuth nitrate and the vanadium oxide acetylacetonate are the same and are both 0.1-1 mol/L;
(2) and (2) sintering the sample obtained in the step (1) at a high temperature in the air or oxygen atmosphere, and then cooling to room temperature to obtain the bismuth vanadate electrode.
8. The method as claimed in claim 7, wherein the temperature of the high temperature sintering in step (2) is 450-500 ℃.
9. The application of the bismuth vanadate electrode rich in surface oxygen vacancies as claimed in any one of claims 1 to 5 in photocatalysis, which is characterized in that a photoelectrochemical cell is assembled by taking the bismuth vanadate electrode rich in surface oxygen vacancies as a working electrode, a platinum sheet electrode as a counter electrode and a silver/silver chloride electrode as a reference electrode.
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