CN108355688B - BiVO for photoelectrocatalysis water decomposition4/Ag3PO4Method for producing thin film - Google Patents
BiVO for photoelectrocatalysis water decomposition4/Ag3PO4Method for producing thin film Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000010409 thin film Substances 0.000 title claims description 12
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 63
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 11
- 238000000151 deposition Methods 0.000 claims abstract description 10
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 239000010408 film Substances 0.000 claims description 66
- 239000011521 glass Substances 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 33
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 32
- 229960001484 edetic acid Drugs 0.000 claims description 32
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 25
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 23
- 229910002915 BiVO4 Inorganic materials 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 21
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 18
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 17
- 238000004528 spin coating Methods 0.000 claims description 16
- 239000001488 sodium phosphate Substances 0.000 claims description 13
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 13
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 13
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 7
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000010335 hydrothermal treatment Methods 0.000 claims description 2
- 238000005342 ion exchange Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000001360 synchronised effect Effects 0.000 claims description 2
- 238000007539 photo-oxidation reaction Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000004577 artificial photosynthesis Methods 0.000 abstract description 2
- 238000004146 energy storage Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 103
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 20
- 229940019931 silver phosphate Drugs 0.000 description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 11
- 238000001027 hydrothermal synthesis Methods 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 150000001621 bismuth Chemical class 0.000 description 4
- 238000004070 electrodeposition Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 2
- QIVUCLWGARAQIO-OLIXTKCUSA-N (3s)-n-[(3s,5s,6r)-6-methyl-2-oxo-1-(2,2,2-trifluoroethyl)-5-(2,3,6-trifluorophenyl)piperidin-3-yl]-2-oxospiro[1h-pyrrolo[2,3-b]pyridine-3,6'-5,7-dihydrocyclopenta[b]pyridine]-3'-carboxamide Chemical class C1([C@H]2[C@H](N(C(=O)[C@@H](NC(=O)C=3C=C4C[C@]5(CC4=NC=3)C3=CC=CN=C3NC5=O)C2)CC(F)(F)F)C)=C(F)C=CC(F)=C1F QIVUCLWGARAQIO-OLIXTKCUSA-N 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000008057 potassium phosphate buffer Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
- B01J35/59—Membranes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a BiVO for photoelectrocatalysis water decomposition4/Ag3PO4A preparation method of a film, belonging to the field of inorganic nonmetallic materials; comprises the following steps: the method comprises the following steps: preparing a bismuth vanadate seed layer precursor solution; step two: preparing a bismuth vanadate seed layer; step three: preparing a bismuth vanadate film; step four: deposition of Ag using a three-electrode system3PO4(ii) a BiVO prepared by the method of the invention4/Ag3PO4A film; the photoelectric conversion efficiency is high, the initial potential of the photooxidation water is low, and the method has wide application prospects in the fields of photocatalytic degradation, photocatalytic water decomposition, artificial photosynthesis, photo-assisted energy storage batteries and the like.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, relates to a preparation method of a bismuth vanadate film modified by silver phosphate for photoelectrocatalytic water decomposition, and particularly relates to BiVO for photoelectrocatalytic water decomposition4/Ag3PO4A method for preparing a film.
Background
Since the twenty-first century, the problems of environmental pollution and energy crisis are continuously aggravated, and the problems are urgently needed to be solved in the human society. For the sustainable development of human society, research and development of novel energy technologies without pollution are urgently needed. Solar energy is used as a new energy source, has the characteristics of no pollution, inexhaustible use and the like, and therefore, the conversion and utilization of the solar energy becomes one of the current research hotspots. Since the first report of the photoelectric decomposition of water by using titanium dioxide photoanode in 1972, a new approach to the conversion of solar energy into chemical energy was proposed [ a. Fujishima and k. honda. photolysis/decomposition of water at the surface of an irradiateds electrochemical reactor. Nature, 1972, 238, 37/38 ], which greatly promoted the research on solar energy conversion technology. However, the titanium dioxide has a wide forbidden band width, and can only absorb solar spectrum energy by 5%, so that the application of the titanium dioxide in the field of photoelectric conversion is limited. Therefore, researchers have developed and researched a large number of novel narrow bandgap semiconductor materials with high catalytic activity, such as tungsten trioxide, ferric oxide, bismuth vanadate, etc.
Among them, bismuth vanadate has attracted much attention as an emerging semiconductor material. Because the band gap is narrow (the monoclinic phase bismuth vanadate is 2.4 eV), the visible light part in the solar spectrum can be absorbed, and the solar spectrum energy is more fully utilized. And the valence band position is about 2.4eV, the generated photogenerated holes can effectively oxidize water into oxygen. And the bismuth vanadate has good physical and chemical stability, low price and no toxicity, and has great application prospect in the field of photoelectric conversion. However, the use of bismuth vanadate as a photo-anode still has many disadvantages, such as easy recombination of photo-generated holes and electrons, and slow surface hydro-oxidation kinetics.
Therefore, improving the photoelectric conversion efficiency of the bismuth vanadate photo-anode has been one of the technical problems to be solved by researchers in the field.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a photoelectrocatalysis water decomposition methodWith BiVO4/Ag3PO4According to the preparation method of the film, a reasonable heterojunction is constructed through silver phosphate and bismuth vanadate to promote separation of photo-generated electron hole pairs, the bismuth vanadate film with high crystallinity is prepared through hydrothermal, the silver phosphate is modified on the surface of the bismuth vanadate film to construct the heterojunction, and the defect that electron holes on the surface of the bismuth vanadate are easy to compound is overcome.
The invention is realized by the following steps:
BiVO for photoelectrocatalysis water decomposition4/Ag3PO4The preparation method of the film is characterized by comprising the following steps:
the method comprises the following steps: preparing a bismuth vanadate seed layer precursor solution;
1.1, weighing the mixture with the molar ratio of 1: 1.5 of bismuth nitrate and ethylene diamine tetraacetic acid, dissolving in water, adjusting the pH value to 10, and stirring to form a colorless transparent solution;
1.2, weighing the mixture with the molar ratio of 1: 0.5 of ammonium metavanadate and ethylene diamine tetraacetic acid solution are dissolved in water, the PH value is adjusted to 10, and a yellow transparent solution is formed by stirring; uniformly mixing the colorless transparent solution obtained in the synchronous step 1.1; mixing to obtain bismuth vanadate seed layer precursor solution;
step two: preparing a bismuth vanadate seed layer;
2.1, placing the pretreated FTO conductive glass on a spin coater, spin-coating the bismuth vanadate seed layer precursor solution for 3 times (10 drops each time), and placing the mixture at 500 ℃ for heat preservation for 15min after each spin-coating;
2.2, placing the FTO conductive glass after spin coating in an air atmosphere, heating to 500 ℃, and preserving heat for 1h to obtain BiVO4A seed layer;
step three: preparing a bismuth vanadate film;
3.1, weighing the mixture with the molar ratio of 1: 1.5, adjusting the pH value of a bismuth nitrate and ethylene diamine tetraacetic acid solution to be =9.2, stirring until the solution is colorless and transparent, adding ammonium metavanadate with the same molar quantity as the bismuth nitrate, stirring until a yellow transparent solution is formed, and transferring the solution to a high-pressure reaction kettle;
3.2 preparation of BiVO containing step two4The FTO conductive glass of the seed layer is obliquely inserted into the reaction kettle, and the side covered with the seed layer is downwards immersed in the reaction kettleStep 3.1, in the yellow transparent solution;
3.3, placing the reaction kettle in an environment of 180 ℃ for reaction for 3h, cooling to room temperature, taking out the FTO conductive glass after hydrothermal treatment, washing with deionized water, and drying at 100 ℃;
3.4, placing the conductive glass after 3.3 drying at 500 ℃ and carrying out heat treatment for 4h in the air atmosphere to obtain the BiVO4Thin film FTO conductive glass;
step four: deposition of Ag3PO4；
4.1, preparing a silver ammonia solution of sodium phosphate;
4.2, using three-electrode system to grow BiVO4The FTO conductive glass of the film is used as a working electrode, silver ammonia solution containing sodium phosphate is used as electrolyte, and the film is subjected to ion exchange in BiVO4Constant potential deposition of Ag on the surface of thin film3PO4Applying constant potential 0.2V (vs. SCE), and electrodepositing 30/120s to obtain BiVO4/Ag3PO4A film.
Further, the mass concentration of the bismuth nitrate in the step 1.1 is 0.0263 g/ml; the mass concentration of the ethylene diamine tetraacetic acid is 0.0292 g/ml.
Further, the mass concentration of the ammonium metavanadate in the step 1.2 is 0.0078 g/ml; the mass concentration of the ethylene diamine tetraacetic acid solution is 0.0094 g/ml.
Further, in the first step, strong ammonia water is used for adjusting the pH value of the solution to 10.
Further, the pretreatment in the second step is as follows: cutting the conductive glass into pieces of 3 cm x 1.5 cm, respectively ultrasonically cleaning with acetone, deionized water and absolute ethyl alcohol for 30 min, storing the cleaned conductive glass in absolute ethyl alcohol, and drying with an air-blast drying oven at 60 ℃ before use.
Further, the mass concentration of the bismuth nitrate in the step 3.1 is 0.0040 g/ml; the mass concentration of the ethylene diamine tetraacetic acid solution is 0.0044 g/ml; the mass concentration of the ammonium metavanadate is 0.0012 g/ml.
Further, in step 3.1, a sodium hydroxide solution is used to adjust the solution pH = 9.2.
Further, the silver ammonia solution of sodium phosphate in step 4.1 is: adding 0.00034 g/ml silver nitrate solution dropwise into concentrated ammonia water to adjust the pH to 9, and then adding 0.00152 g/ml sodium phosphate.
Furthermore, the three-electrode system in step 4.2 is a long-lived BiVO4The FTO conductive glass of the film is a working electrode, the Pt sheet is a counter electrode, and the saturated calomel electrode is a system formed by a reference electrode.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, by utilizing the principle of constructing a reasonable heterojunction to promote the separation of photo-generated electron hole pairs and utilizing the matching of the silver phosphate energy level and the bismuth vanadate energy level, the heterojunction is constructed to form a built-in electric field to promote the separation of electron holes, so that the photoelectric conversion efficiency is improved. BiVO prepared by the method of the invention4/Ag3PO4The film has the advantage of low initial potential of photooxidation water, and has wide application prospect in the fields of photocatalytic degradation, photoelectrocatalysis water decomposition, artificial photosynthesis, photo-assisted energy storage batteries and the like.
Drawings
FIG. 1 shows BiVO prepared in example 1 of the present invention4/Ag3PO4Scanning electron microscope pictures of the films.
FIG. 2 shows BiVO prepared in example 1 of the present invention4/Ag3PO4High resolution transmission electron microscopy pictures of the thin film.
FIG. 3 is BiVO prepared in example 54Scanning electron microscope pictures of the films.
FIG. 4 is BiVO prepared in example 54X-ray diffraction pattern of the film.
FIG. 5 shows BiVO in example 1 of the present invention4/Ag3PO4Film and BiVO4X-ray photoelectron spectroscopy of thin films.
FIG. 6 shows BiVO prepared by the present invention4/Ag3PO4Film and BiVO4Photocurrent curve of the thin film.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be noted that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
1) Weighing 0.395 g of bismuth nitrate and 0.438 g of ethylenediamine tetraacetic acid, dissolving the bismuth nitrate and the ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a colorless transparent solution is formed, weighing 0.117 g of ammonium metavanadate and 0.141 g of ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a yellow transparent solution is formed, mixing the two solutions, and uniformly stirring the two solutions to prepare a bismuth vanadate seed layer precursor solution;
2) spin-coating a bismuth vanadate precursor solution on FTO conductive glass, performing heat treatment at 500 ℃ for 15min every time the FTO conductive glass is spin-coated, performing spin-coating for 3 times, performing heat treatment for 10 drops every time, and performing heat treatment at 500 ℃ for 1h to obtain a bismuth vanadate seed layer;
3) weighing 0.12 g of bismuth nitrate and 0.132 g of ethylenediamine tetraacetic acid, dissolving in 30ml of water, adjusting the pH =9.2 of the solution with 2 mol/L of NaOH solution, stirring until a colorless transparent solution is formed, then adding 0.036g of ammonium metavanadate, stirring until a yellow transparent solution is formed, and then transferring the solution to a polytetrafluoroethylene liner of a 50ml high-pressure reaction kettle;
4) inserting FTO conductive glass spin-coated with a bismuth vanadate seed layer into the inner liner of the reaction kettle in an inclined manner, so that the side with the bismuth vanadate seed layer faces downwards;
5) sealing the reaction kettle, putting the reaction kettle into an oven for hydrothermal reaction, carrying out hydrothermal reaction for 3h at 180 ℃, naturally cooling to room temperature, taking out, and washing with deionized water to obtain a yellow film;
6) and (3) carrying out heat treatment on the obtained conductive glass with the film at 500 ℃, and keeping the temperature for 4 hours to obtain a yellow bismuth vanadate film.
7) 0.034g of silver nitrate was weighed into 100ml of water, ammonia was added dropwise to adjust pH =9, and then 0.152g of sodium phosphate was added to obtain a silver phosphate precursor solution, i.e., a silver-ammonia solution of sodium phosphate.
8) The method comprises the steps of adopting a three-electrode system, using FTO conductive glass grown with bismuth vanadate as a working electrode, using a platinum sheet as a counter electrode, using a saturated calomel electrode as a reference electrode, using an electrolyte as a silver phosphate precursor solution, carrying out constant potential deposition on silver phosphate on the surface of a bismuth vanadate film at a potential of 0.2V relative to the saturated calomel electrode, and finally obtaining the silver phosphate modified bismuth vanadate film, wherein the electrodeposition time is 30 s.
As shown in FIG. 1, FIG. 1 shows BiVO obtained in this example4/Ag3PO4Film scanning electron micrograph, showing the prepared BiVO4/Ag3PO4The film is made of nano-flaky BiVO4And granular Ag deposited on the surface3PO4Composition of
As shown in FIG. 2, FIG. 2 is a transmission electron microscope of the thin film, and it can be seen from FIG. 2 that the synthesized product is BiVO with good crystallinity4And granular Ag3PO4And (4) forming.
Example 2
1) Weighing 0.395 g of bismuth nitrate and 0.438 g of ethylenediamine tetraacetic acid, dissolving the bismuth nitrate and the ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a colorless transparent solution is formed, weighing 0.117 g of ammonium metavanadate and 0.141 g of ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a yellow transparent solution is formed, mixing the two solutions, and uniformly stirring the two solutions to prepare a bismuth vanadate seed layer precursor solution;
2) spin-coating a bismuth vanadate precursor solution on FTO conductive glass, performing heat treatment at 500 ℃ for 15min every time the FTO conductive glass is spin-coated, performing spin-coating for 3 times, performing heat treatment for 10 drops every time, and performing heat treatment at 500 ℃ for 1h to obtain a bismuth vanadate seed layer;
3) weighing 0.12 g of bismuth nitrate and 0.132 g of ethylenediamine tetraacetic acid, dissolving in 30ml of water, adjusting the pH =9.2 of the solution with 2 mol/L of NaOH solution, stirring until a colorless transparent solution is formed, then adding 0.036g of ammonium metavanadate, stirring until a yellow transparent solution is formed, and then transferring the solution to a polytetrafluoroethylene liner of a 50ml high-pressure reaction kettle;
4) inserting FTO conductive glass spin-coated with a bismuth vanadate seed layer into the inner liner of the reaction kettle in an inclined manner, so that the side with the bismuth vanadate seed layer faces downwards;
5) sealing the reaction kettle, putting the reaction kettle into an oven for hydrothermal reaction, carrying out hydrothermal reaction for 3h at 180 ℃, naturally cooling to room temperature, taking out, and washing with deionized water to obtain a yellow film;
6) and (3) carrying out heat treatment on the obtained conductive glass with the film at 500 ℃, and keeping the temperature for 4 hours to obtain a yellow bismuth vanadate film.
7) 0.034g of silver nitrate is weighed and added into 100ml of water, ammonia water is added dropwise to adjust the pH =9, and then 0.152g of sodium phosphate is added, so that the silver phosphate precursor solution is obtained.
8) The method comprises the steps of adopting a three-electrode system, using FTO conductive glass grown with bismuth vanadate as a working electrode, using a platinum sheet as a counter electrode, using a saturated calomel electrode as a reference electrode, using an electrolyte as a silver phosphate precursor solution, carrying out constant potential deposition on silver phosphate on the surface of a bismuth vanadate film at a potential of 0.2V relative to the saturated calomel electrode, wherein the electrodeposition time is 60s, and finally obtaining the silver phosphate modified bismuth vanadate film.
Example 3
1) Weighing 0.395 g of bismuth nitrate and 0.438 g of ethylenediamine tetraacetic acid, dissolving the bismuth nitrate and the ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a colorless transparent solution is formed, weighing 0.117 g of ammonium metavanadate and 0.141 g of ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a yellow transparent solution is formed, mixing the two solutions, and uniformly stirring the two solutions to prepare a bismuth vanadate seed layer precursor solution;
2) spin-coating a bismuth vanadate precursor solution on FTO conductive glass, performing heat treatment at 500 ℃ for 15min every time the FTO conductive glass is spin-coated, performing spin-coating for 3 times, performing heat treatment for 10 drops every time, and performing heat treatment at 500 ℃ for 1h to obtain a bismuth vanadate seed layer;
3) weighing 0.12 g of bismuth nitrate and 0.132 g of ethylenediamine tetraacetic acid, dissolving in 30ml of water, adjusting the pH =9.2 of the solution with 2 mol/L of NaOH solution, stirring until a colorless transparent solution is formed, then adding 0.036g of ammonium metavanadate, stirring until a yellow transparent solution is formed, and then transferring the solution to a polytetrafluoroethylene liner of a 50ml high-pressure reaction kettle;
4) inserting FTO conductive glass spin-coated with a bismuth vanadate seed layer into the inner liner of the reaction kettle in an inclined manner, so that the side with the bismuth vanadate seed layer faces downwards;
5) sealing the reaction kettle, putting the reaction kettle into an oven for hydrothermal reaction, carrying out hydrothermal reaction for 3h at 180 ℃, naturally cooling to room temperature, taking out, and washing with deionized water to obtain a yellow film;
6) and (3) carrying out heat treatment on the obtained conductive glass with the film at 500 ℃, and keeping the temperature for 4 hours to obtain a yellow bismuth vanadate film.
7) 0.034g of silver nitrate is weighed and added into 100ml of water, ammonia water is added dropwise to adjust the pH =9, and then 0.152g of sodium phosphate is added, so that the silver phosphate precursor solution is obtained.
8) The method comprises the steps of adopting a three-electrode system, using FTO conductive glass grown with bismuth vanadate as a working electrode, using a platinum sheet as a counter electrode, using a saturated calomel electrode as a reference electrode, using an electrolyte as a silver phosphate precursor solution, carrying out constant potential deposition on silver phosphate on the surface of a bismuth vanadate film at a potential of 0.2V relative to the saturated calomel electrode, wherein the electrodeposition time is 90s, and finally obtaining the silver phosphate modified bismuth vanadate film.
Example 4
1) Weighing 0.395 g of bismuth nitrate and 0.438 g of ethylenediamine tetraacetic acid, dissolving the bismuth nitrate and the ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a colorless transparent solution is formed, weighing 0.117 g of ammonium metavanadate and 0.141 g of ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a yellow transparent solution is formed, mixing the two solutions, and uniformly stirring the two solutions to prepare a bismuth vanadate seed layer precursor solution;
2) spin-coating a bismuth vanadate precursor solution on FTO conductive glass, performing heat treatment at 500 ℃ for 15min every time the FTO conductive glass is spin-coated, performing spin-coating for 3 times, performing heat treatment for 10 drops every time, and performing heat treatment at 500 ℃ for 1h to obtain a bismuth vanadate seed layer;
3) weighing 0.12 g of bismuth nitrate and 0.132 g of ethylenediamine tetraacetic acid, dissolving in 30ml of water, adjusting the pH =9.2 of the solution with 2 mol/L of NaOH solution, stirring until a colorless transparent solution is formed, then adding 0.036g of ammonium metavanadate, stirring until a yellow transparent solution is formed, and then transferring the solution to a polytetrafluoroethylene liner of a 50ml high-pressure reaction kettle;
4) inserting FTO conductive glass spin-coated with a bismuth vanadate seed layer into the inner liner of the reaction kettle in an inclined manner, so that the side with the bismuth vanadate seed layer faces downwards;
5) sealing the reaction kettle, putting the reaction kettle into an oven for hydrothermal reaction, carrying out hydrothermal reaction for 3h at 180 ℃, naturally cooling to room temperature, taking out, and washing with deionized water to obtain a yellow film;
6) and (3) carrying out heat treatment on the obtained conductive glass with the film at 500 ℃, and keeping the temperature for 4 hours to obtain a yellow bismuth vanadate film.
7) 0.034g of silver nitrate is weighed and added into 100ml of water, ammonia water is added dropwise to adjust the pH =9, and then 0.152g of sodium phosphate is added, so that the silver phosphate precursor solution is obtained.
8) The method comprises the steps of adopting a three-electrode system, using FTO conductive glass grown with bismuth vanadate as a working electrode, using a platinum sheet as a counter electrode, using a saturated calomel electrode as a reference electrode, using an electrolyte as a silver phosphate precursor solution, carrying out constant potential deposition on silver phosphate on the surface of a bismuth vanadate film at a potential of 0.2V relative to the saturated calomel electrode, and finally obtaining the silver phosphate modified bismuth vanadate film, wherein the electrodeposition time is 120 s.
Example 5
1) Weighing 0.395 g of bismuth nitrate and 0.438 g of ethylenediamine tetraacetic acid, dissolving the bismuth nitrate and the ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a colorless transparent solution is formed, weighing 0.117 g of ammonium metavanadate and 0.141 g of ethylenediamine tetraacetic acid in 15ml of water, adjusting the pH =10 of the solution with strong ammonia water, stirring the solution until a yellow transparent solution is formed, mixing the two solutions, and uniformly stirring the two solutions to prepare a bismuth vanadate seed layer precursor solution;
2) spin-coating a bismuth vanadate precursor solution on FTO conductive glass, performing heat treatment at 500 ℃ for 15min every time the FTO conductive glass is spin-coated, performing spin-coating for 3 times, performing heat treatment for 10 drops every time, and performing heat treatment at 500 ℃ for 1h to obtain a bismuth vanadate seed layer;
3) weighing 0.12 g of bismuth nitrate and 0.132 g of ethylenediamine tetraacetic acid, dissolving in 30ml of water, adjusting the pH =9.2 of the solution with 2 mol/L of NaOH solution, stirring until a colorless transparent solution is formed, then adding 0.036g of ammonium metavanadate, stirring until a yellow transparent solution is formed, and then transferring the solution to a polytetrafluoroethylene liner of a 50ml high-pressure reaction kettle;
4) inserting FTO conductive glass spin-coated with a bismuth vanadate seed layer into the inner liner of the reaction kettle in an inclined manner, so that the side with the bismuth vanadate seed layer faces downwards;
5) sealing the reaction kettle, putting the reaction kettle into an oven for hydrothermal reaction, carrying out hydrothermal reaction for 3h at 180 ℃, naturally cooling to room temperature, taking out, and washing with deionized water to obtain a yellow film;
6) and (3) carrying out heat treatment on the obtained conductive glass with the film at 500 ℃, and keeping the temperature for 4 hours to obtain a yellow bismuth vanadate film.
BiVO obtained in example 54Film (non-deposited Ag)3PO4Pure BiVO of4Thin film) as a comparative sample, which had no Ag deposited3PO4Pure BiVO of4The scanning electron microscope picture of the film is shown in FIG. 3, and the BiVO prepared by the method can be seen from FIG. 34The film is made of nano-sheet BiVO4And (4) forming. FIG. 4 shows BiVO obtained in this example4The X-ray diffraction pattern of the film can show that the phase of the film is monoclinic BiVO4。
BiVO obtained in example 14/Ag3PO4BiVO obtained from the thin film (example 1) and example 54The XPS spectrum of the film is shown in FIG. 5, and the BiVO of the product of example 1 can be seen from FIG. 54Surface of Ag3PO4The valence composition of the product of example 5 is indeed BiVO4。
Testing the photocurrent of the product, wherein the specific testing method comprises the following steps: the test instrument is an electrochemical workstation CHI660A, and the three-electrode test system is characterized in that a Pt sheet is used as a counter electrode, a Saturated Calomel Electrode (SCE) is used as a reference electrode, and BiVO is grown on the Pt sheet4And BiVO4/Ag3PO4The FTO glass of the film is used as a working electrode, light passes through a quartz window of the electrolytic cell and vertically irradiates from one surface of the FTO where the semiconductor is grown, and all test areas are fixed at 1cm2And selecting a linear sweep voltammetry, wherein the sweep interval is 0.5-1.5V (vs. RHE). The electrolyte is 0.2 mol/L potassium phosphate buffer solution, the pH value is 7, nitrogen is introduced for half an hour before testing, and dissolved oxygen in the electrolyte is removed. The light source used was a 300W xenon lamp from Perfect corporation, with the addition of a filter (AM 1.5G). FIG. 6 is a plot of photocurrent versus pure BiVO for examples 1, 2, 3, 4 and 54Example 5 BiVO in comparison4/Ag3PO4The film (examples 1, 2, 3 and 4) had a higher photooxidation water decomposition current density than the former and a lower oxygen evolution initiation potential. BiVO comparing different deposition times4/Ag3PO4As can be seen from the films (examples 1, 2, 3 and 4), 90s of BiVO was deposited4/Ag3PO4The film (example 3) shows the maximum photooxidation water splitting current density and the lowest oxygen evolution initial potential shows better application prospect.
The above description is only for the purpose of illustrating preferred embodiments and applications of the present invention, and should not be construed as limiting the present invention, and all modifications, substitutions and alterations based on the technical spirit of the present invention are intended to be included in the scope of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the invention, and these changes and modifications are to be considered as within the scope of the invention.
Claims (9)
1. BiVO for photoelectrocatalysis water decomposition4/Ag3PO4The preparation method of the film is characterized by comprising the following steps:
the method comprises the following steps: preparing a bismuth vanadate seed layer precursor solution;
1.1, weighing the mixture with the molar ratio of 1: 1.5 of bismuth nitrate and ethylene diamine tetraacetic acid, dissolving in water, adjusting the pH value to 10, and stirring to form a colorless transparent solution;
1.2, weighing the mixture with the molar ratio of 1: 0.5 of ammonium metavanadate and ethylene diamine tetraacetic acid solution are dissolved in water, the pH value is adjusted to 10, and a yellow transparent solution is formed by stirring; uniformly mixing the colorless transparent solution obtained in the synchronous step 1.1; mixing to obtain bismuth vanadate seed layer precursor solution;
step two: preparing a bismuth vanadate seed layer;
2.1, placing the pretreated FTO conductive glass on a spin coater, spin-coating the bismuth vanadate seed layer precursor solution for 3 times (10 drops each time), and placing the mixture at 500 ℃ for heat preservation for 15min after each spin-coating;
2.2, placing the FTO conductive glass after spin coating in an air atmosphere and raisingHeating to 500 ℃, and preserving heat for 1h to obtain BiVO4A seed layer;
step three: preparing a bismuth vanadate film;
3.1, weighing the mixture with the molar ratio of 1: 1.5, adjusting the pH value of a bismuth nitrate and ethylene diamine tetraacetic acid solution to be =9.2, stirring until the solution is colorless and transparent, adding ammonium metavanadate with the same molar quantity as the bismuth nitrate, stirring until a yellow transparent solution is formed, and transferring the solution to a high-pressure reaction kettle;
3.2 preparation of BiVO containing step two4Inserting the FTO conductive glass of the seed layer into a reaction kettle in an inclined manner, and immersing the side covered with the seed layer downwards into the yellow transparent solution in the step 3.1;
3.3, placing the reaction kettle in an environment of 180 ℃ for reaction for 3h, cooling to room temperature, taking out the FTO conductive glass after hydrothermal treatment, washing with deionized water, and drying at 100 ℃;
3.4, placing the conductive glass after 3.3 drying at 500 ℃ and carrying out heat treatment for 4h in the air atmosphere to obtain the BiVO4Thin film FTO conductive glass;
step four: deposition of Ag3PO4；
4.1, preparing a silver ammonia solution of sodium phosphate;
4.2, using three-electrode system to grow BiVO4The FTO conductive glass of the film is used as a working electrode, silver ammonia solution containing sodium phosphate is used as electrolyte, and the film is subjected to ion exchange in BiVO4Constant potential deposition of Ag on the surface of thin film3PO4Applying constant potential 0.2V vs. SCE, and electrodepositing for 30s, 60s, 90s or 120s to obtain BiVO4/Ag3PO4A film.
2. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4The preparation method of the film is characterized in that the mass concentration of the bismuth nitrate in the step 1.1 is 0.0263 g/mL; the mass concentration of the ethylene diamine tetraacetic acid is 0.0292 g/mL.
3. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4Film(s)The preparation method is characterized in that the mass concentration of the ammonium metavanadate in the step 1.2 is 0.0078 g/mL; the mass concentration of the ethylene diamine tetraacetic acid solution is 0.0094 g/mL.
4. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4The preparation method of the film is characterized in that in the first step, strong ammonia water is used for adjusting the pH value of the solution to 10.
5. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4The preparation method of the film is characterized in that the pretreatment in the second step is as follows: cutting the conductive glass into pieces of 3 cm x 1.5 cm, respectively ultrasonically cleaning with acetone, deionized water and absolute ethyl alcohol for 30 min, storing the cleaned conductive glass in absolute ethyl alcohol, and drying with an air-blast drying oven at 60 ℃ before use.
6. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4The preparation method of the film is characterized in that the mass concentration of the bismuth nitrate in the step 3.1 is 0.0040 g/mL; the mass concentration of the ethylene diamine tetraacetic acid solution is 0.0044 g/mL; the mass concentration of the ammonium metavanadate is 0.0012 g/mL.
7. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4The preparation method of the film is characterized in that in the step 3.1, the solution pH =9.2 is adjusted by using a sodium hydroxide solution.
8. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4The preparation method of the film is characterized in that the silver ammonia solution of the sodium phosphate in the step 4.1 is as follows: adding 0.00034 g/mL silver nitrate solution into the solution, dropwise adding concentrated ammonia water to adjust the pH to 9, and then adding 0.00152 g/mL sodium phosphate.
9. BiVO for photoelectrocatalytic water splitting according to claim 14/Ag3PO4The preparation method of the film is characterized in that the three-electrode system in the step 4.2 is a long BiVO4The FTO conductive glass of the film is a working electrode, the Pt sheet is a counter electrode, and the saturated calomel electrode is a system formed by a reference electrode.
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| CN110172708B (en) * | 2019-05-05 | 2021-05-25 | 南京航空航天大学 | Polyimide-protected bismuth vanadate composite photo-anode and preparation method thereof |
| CN111705333A (en) * | 2020-05-19 | 2020-09-25 | 江苏大学 | Ag-Pi/BiVO4Heterogeneous combination method and application thereof in photoelectrolysis water |
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