CN108355688A - A kind of photoelectrocatalysis water decomposition BiVO4/Ag3PO4The preparation method of film - Google Patents
A kind of photoelectrocatalysis water decomposition BiVO4/Ag3PO4The preparation method of film Download PDFInfo
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- CN108355688A CN108355688A CN201810043714.9A CN201810043714A CN108355688A CN 108355688 A CN108355688 A CN 108355688A CN 201810043714 A CN201810043714 A CN 201810043714A CN 108355688 A CN108355688 A CN 108355688A
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- film
- bivo
- solution
- conductive glass
- pucherite
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 30
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000010408 film Substances 0.000 claims abstract description 66
- 229910000161 silver phosphate Inorganic materials 0.000 claims abstract description 33
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000010409 thin film Substances 0.000 claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 10
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 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 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 19
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 18
- 238000004528 spin coating Methods 0.000 claims description 18
- 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 14
- 238000004070 electrodeposition Methods 0.000 claims description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 229960001484 edetic acid Drugs 0.000 claims description 8
- 239000001488 sodium phosphate Substances 0.000 claims description 8
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 8
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000003792 electrolyte Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 206010013786 Dry skin Diseases 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 238000007539 photo-oxidation reaction Methods 0.000 abstract description 4
- 230000005611 electricity Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000000034 method Methods 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
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 18
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 15
- FRTNIYVUDIHXPG-UHFFFAOYSA-N acetic acid;ethane-1,2-diamine Chemical class CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCN FRTNIYVUDIHXPG-UHFFFAOYSA-N 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 5
- 230000004044 response Effects 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229940075397 calomel Drugs 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 210000000720 eyelash Anatomy 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- VQYORFXOSQZHEF-UHFFFAOYSA-K trisodium azane phosphate Chemical compound N.P(=O)([O-])([O-])[O-].[Na+].[Na+].[Na+] VQYORFXOSQZHEF-UHFFFAOYSA-K 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000004832 voltammetry 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
Classifications
-
- 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
-
- 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
- B01J35/39—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
-
- 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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- 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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of photoelectrocatalysis water decomposition BiVO4/Ag3PO4The preparation method of film, belongs to field of inorganic nonmetallic material；It comprises the steps of：Step 1：Prepare pucherite seed layer precursor liquid；Step 2：Prepare pucherite seed layer；Step 3：Prepare vanadic acid bismuth thin film；Step 4：Ag is deposited using three-electrode system3PO4；The BiVO prepared by the method for the invention4/Ag3PO4Film；Electricity conversion is high, and photooxidation water take-off potential is low, has broad application prospects in fields such as photocatalytic degradation, photoelectrocatalysis water decomposition, artificial photosynthesis, light auxiliary energy storage batteries.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, are related to the vanadium using phosphoric acid modified by silver of photoelectrocatalysis water decomposition
The preparation method of sour bismuth thin film, in particular to a kind of photoelectrocatalysis water decomposition BiVO4/Ag3PO4The preparation method of film.
Background technology
Since 21st century, environmental pollution constantly aggravates with problem of energy crisis, is faced at human society
Urgent problem.For the sustainable development of human society, the free of contamination new energy source technology of research and development is compeled
The eyebrows and eyelashes.Solar energy has the features such as pollution-free, nexhaustible, therefore carry out trans-utilization to solar energy as a kind of new energy
Become current one of research hotspot.Since Japanese scholars in 1972 report for the first time light is carried out using titanium dioxide photo anode
Electrolysis water, it is proposed that solar energy is converted into new way [the A. Fujishima and K. Honda. of chemical energy
Photolysis/decomposition of water at the surface of an irradiated
Semiconductor. Nature, 1972,238,37/38.], greatly pushed the research of solar energy transformation technology.So
And titanium dioxide energy gap is wider, is only capable of absorbing the 5% of solar spectrum energy, limits its answering in photoelectric conversion field
With.Thus, a large amount of novel narrow bandgap semiconductor materials with high catalytic activity of researchers' developmental research, such as three oxygen
Change tungsten, di-iron trioxide, pucherite etc..
Wherein, pucherite as a kind of emerging semi-conducting material by the extensive concern of researchers.Due to its band gap
It is relatively narrow（Monoclinic phase pucherite is 2.4eV）, thus the visible light part in solar spectrum can be absorbed, it more fully utilizes too
Sunlight spectrum energy.And its valence band location is about 2.4eV, and water oxygen effectively can be turned to oxygen by the photohole of generation.
Also, pucherite physics and chemical stability are good, cheap, non-toxic, before photoelectric conversion field has prodigious application
Scape.However, pucherite as photo cathode use still there are many insufficient, as photohole and electronics are easy compound, surface
The problems such as water oxidation kinetics is slower.
Therefore, the electricity conversion for improving pucherite light anode is always this field researchers strategic point technology to be solved
One of problem.
Invention content
The present invention is directed to problems of the prior art, it is proposed that a kind of photoelectrocatalysis water decomposition BiVO4/Ag3PO4
The preparation method of film builds the separation that rational hetero-junctions promotes photo-generate electron-hole pair by silver orthophosphate and pucherite,
The vanadic acid bismuth thin film of high-crystallinity is prepared by hydro-thermal and builds hetero-junctions in its surface modification silver orthophosphate, overcomes pucherite surface
The easily compound defect in electron hole.
The invention is realized in this way：
A kind of photoelectrocatalysis water decomposition BiVO4/Ag3PO4The preparation method of film, which is characterized in that steps are as follows：
Step 1：Prepare pucherite seed layer precursor liquid；
1.1, it is 1 to weigh molar ratio：1.5 bismuth nitrate and ethylenediamine tetra-acetic acid is dissolved in the water and adjusts PH to 10, stirring
Form colourless transparent solution；
1.2, it is 1 to weigh molar ratio：0.5 ammonium metavanadate and edta solution, be dissolved in the water and adjust PH to
10, stirring forms yellow transparent solution；It is uniformly mixed with the colourless transparent solution of step 1.1；Pucherite kind is obtained after mixing
Sublayer precursor liquid；
Step 2：Prepare pucherite seed layer；
2.1, pretreated FTO electro-conductive glass is placed on sol evenning machine, pucherite seed layer precursor liquid is taken to carry out spin coating, spin coating
3 times, 10 drip every time, and each spin coating, which is placed in 500 DEG C, keeps the temperature 15 min；
2.2, the FTO electro-conductive glass after spin coating is placed in air atmosphere, is warming up to 500 DEG C, 1h is kept the temperature, obtains BiVO4Seed
Layer；
Step 3：Prepare vanadic acid bismuth thin film；
3.1, it is 1 to weigh molar ratio：1.5 bismuth nitrate and edta solution adjusts pH=9.2, stirring to water white transparency
The ammonium metavanadate with bismuth nitrate equimolar amounts is added afterwards, stirring is transferred to yellow transparent solution is formed in autoclave；
3.2, contain BiVO by prepared by step 24The FTO electro-conductive glass oblique cuttings of seed layer enter in reaction kettle, will be covered with seed layer
Side downward and be immersed in the yellow transparent solution of step 3.1；
3.3, reaction kettle is placed in 180 DEG C of environment and reacts 3h, is cooled to room temperature, the FTO electro-conductive glass after hydro-thermal is taken out, spends
100 DEG C of dryings after ion water washing；
3.4, the electro-conductive glass after 3.3 dryings is placed in 500 DEG C, 4h is heat-treated under air atmosphere, obtaining growth has BiVO4Film
FTO electro-conductive glass；
Step 4：Deposit Ag3PO4；
4.1, prepare the silver ammino solution of sodium phosphate；
4.2, using three-electrode system, with BiVO4The FTO electro-conductive glass of film is working electrode, the silver containing sodium phosphate
Ammonia solution is electrolyte, in BiVO4Film surface potentiostatic electrodeposition Ag3PO4, apply constant potential 0.2V（vs. SCE）, electro-deposition
30/120s obtains BiVO4/Ag3PO4Film.
Further, the mass concentration of the bismuth nitrate in the step 1.1 is 0.0263 g/ml；The ethylenediamine tetraacetic
The mass concentration of acetic 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 ethylenediamine
Tetraacethyl concentration of polymer solution is 0.0094 g/ml.
Further, pH value of solution is adjusted to 10 using concentrated ammonia liquor in the step one.
Further, the pretreatment in the step two is：Electro-conductive glass is cut into the small pieces of 3 cm x, 1.5 cm,
Acetone, deionized water, absolute ethyl alcohol is used to be cleaned by ultrasonic 30 min, and cleaned electro-conductive glass is placed in absolute ethyl alcohol respectively
It preserves, using preceding with 60 DEG C of drying of air dry oven.
Further, the mass concentration of the bismuth nitrate in the step 3.1 is 0.0040 g/ml；The ethylenediamine tetraacetic
Acetic acid solution mass concentration is 0.0044 g/ml；The ammonium metavanadate mass concentration is 0.0012 g/ml.
Further, pH value of solution=9.2 are adjusted using sodium hydroxide solution in the step 3.1.
Further, the silver ammino solution of the step 4.1 sodium phosphate is：By the nitric acid that mass concentration is 0.00034 g/ml
Silver-colored solution, is added dropwise concentrated ammonia liquor and adjusts pH to 9, and the sodium phosphate that mass concentration is 0.00152 g/ml is then added.
Further, three-electrode system is with BiVO in the step 4.24The FTO electro-conductive glass of film is work
Electrode, it is that reference electrode is formed by system that Pt pieces, which are to electrode, saturated calomel electrode,.
The advantageous effect of the present invention compared to the prior art is：
The principle that the present invention promotes the separation of photo-generate electron-hole pair using rational hetero-junctions is built, using silver orthophosphate energy level with
Pucherite level-density parameter, structure hetero-junctions forms built in field and promotes electron hole separation, to improve electricity conversion.It is logical
Cross the BiVO of the method for the present invention preparation4/Ag3PO4Film has the low advantage of photooxidation water take-off potential, in photocatalytic degradation, light
The fields such as electro-catalysis water decomposition, artificial photosynthesis, light auxiliary energy storage battery have broad application prospects.
Description of the drawings
Fig. 1 is BiVO prepared by the embodiment of the present invention 14/Ag3PO4The scanning electron microscope diagram piece of film.
Fig. 2 is BiVO prepared by the embodiment of the present invention 14/Ag3PO4The high resolution transmission electron microscopy piece of film.
Fig. 3 is BiVO prepared by embodiment 54The scanning electron microscope diagram piece of film.
Fig. 4 is BiVO prepared by embodiment 54The X-ray diffraction spectrogram of film.
Fig. 5 is BiVO in the embodiment of the present invention 14/Ag3PO4Film and BiVO4The x-ray photoelectron spectroscopy of film.
Fig. 6 is BiVO prepared by the present invention4/Ag3PO4Film and BiVO4The photocurrent curve of film.
Specific implementation mode
It is clear to keep the purpose of the present invention, technical solution and effect clearer, referring to the drawings and give an actual example to this
Invention is further described.It should be understood that specific implementation described herein is not used to limit only to explain the present invention
The present invention.
Embodiment 1
1）The ethylenediamine tetra-acetic acid of the bismuth nitrate and 0.438 g that weigh 0.395 g is dissolved in 15ml water, and solution is adjusted with concentrated ammonia liquor
PH=10, until forming colourless transparent solution, ammonium metavanadate and the 0.141 g ethylenediamine tetra-acetic acids for separately weighing 0.117 g are molten for stirring
In 15ml water, pH value of solution=10 are adjusted with concentrated ammonia liquor, stirring mixes two solution until forming yellow transparent solution, and stirring is equal
It is even, pucherite seed layer precursor liquid is made；
2）Pucherite precursor solution is spun on FTO electro-conductive glass, it is complete per spin coating that 15min, rotation are once heat-treated at 500 DEG C
It applies 3 times, 10 drop, is then heat-treated 1h at 500 DEG C, obtains pucherite seed layer every time；
3）The bismuth nitrate and 0.132 g ethylenediamine tetra-acetic acids for weighing 0.12 g are dissolved in 30ml water, with the NaOH solution of 2 mol/L
PH value of solution=9.2 are adjusted, then until forming colourless transparent solution the ammonium metavanadate of 0.036g is added, stirring is until forming in stirring
Solution is transferred in the polytetrafluoroethyllining lining of 50ml autoclaves by yellow transparent solution later；
4）There are the FTO electro-conductive glass oblique cuttings of pucherite seed layer to enter inside inner liner of reaction kettle spin coating, makes have pucherite seed layer
One down；
5）It is put into after reaction kettle is sealed in baking oven and carries out hydro-thermal reaction, 180 DEG C of thermal response 3h, cooled to room temperature is taken out
It is rinsed afterwards with deionized water, obtains the film of yellow；
6）By 500 DEG C of heat treatments of electro-conductive glass with film of gained, 4h is kept the temperature, the vanadic acid bismuth thin film of yellow is obtained.
7）It weighs 0.034g silver nitrates to be added in 100ml water, ammonium hydroxide is added dropwise and adjusts pH=9,0.152g phosphoric acid is then added
Sodium obtains silver orthophosphate precursor liquid, the i.e. silver ammino solution of sodium phosphate.
8）Using three-electrode system, as working electrode, platinized platinum is used as to electrode the FTO electro-conductive glass with pucherite,
Saturated calomel electrode is reference electrode, and electrolyte is silver orthophosphate precursor liquid, in pucherite film surface with relative to saturation calomel
The current potential of electrode 0.2V carries out potentiostatic electrodeposition silver orthophosphate, and it is thin finally to obtain phosphoric acid modified by silver pucherite by electrodeposition time 30s
Film.
As shown in FIG. 1, FIG. 1 is the BiVO that the present embodiment obtains4/Ag3PO4Film scanning electromicroscopic photograph, it is seen that preparation
BiVO4/Ag3PO4Film by nano-sheet BiVO4With the granular Ag for being deposited on surface3PO4Composition
As shown in Fig. 2, Fig. 2 is the thin film transmission electron microscope, as shown in Figure 2, the product of synthesis is to crystallize good BiVO4And particle
The Ag of shape3PO4Composition.
Embodiment 2
1）The ethylenediamine tetra-acetic acid of the bismuth nitrate and 0.438 g that weigh 0.395 g is dissolved in 15ml water, and solution is adjusted with concentrated ammonia liquor
PH=10, until forming colourless transparent solution, ammonium metavanadate and the 0.141 g ethylenediamine tetra-acetic acids for separately weighing 0.117 g are molten for stirring
In 15ml water, pH value of solution=10 are adjusted with concentrated ammonia liquor, stirring mixes two solution until forming yellow transparent solution, and stirring is equal
It is even, pucherite seed layer precursor liquid is made；
2）Pucherite precursor solution is spun on FTO electro-conductive glass, it is complete per spin coating that 15min, rotation are once heat-treated at 500 DEG C
It applies 3 times, 10 drop, is then heat-treated 1h at 500 DEG C, obtains pucherite seed layer every time；
3）The bismuth nitrate and 0.132 g ethylenediamine tetra-acetic acids for weighing 0.12 g are dissolved in 30ml water, with the NaOH solution of 2 mol/L
PH value of solution=9.2 are adjusted, then until forming colourless transparent solution the ammonium metavanadate of 0.036g is added, stirring is until forming in stirring
Solution is transferred in the polytetrafluoroethyllining lining of 50ml autoclaves by yellow transparent solution later；
4）There are the FTO electro-conductive glass oblique cuttings of pucherite seed layer to enter inside inner liner of reaction kettle spin coating, makes have pucherite seed layer
One down；
5）It is put into after reaction kettle is sealed in baking oven and carries out hydro-thermal reaction, 180 DEG C of thermal response 3h, cooled to room temperature is taken out
It is rinsed afterwards with deionized water, obtains the film of yellow；
6）By 500 DEG C of heat treatments of electro-conductive glass with film of gained, 4h is kept the temperature, the vanadic acid bismuth thin film of yellow is obtained.
7）It weighs 0.034g silver nitrates to be added in 100ml water, ammonium hydroxide is added dropwise and adjusts pH=9,0.152g phosphoric acid is then added
Sodium obtains silver orthophosphate precursor liquid.
8）Using three-electrode system, as working electrode, platinized platinum is used as to electrode the FTO electro-conductive glass with pucherite,
Saturated calomel electrode is reference electrode, and electrolyte is silver orthophosphate precursor liquid, in pucherite film surface with relative to saturation calomel
The current potential of electrode 0.2V carries out potentiostatic electrodeposition silver orthophosphate, and it is thin finally to obtain phosphoric acid modified by silver pucherite by electrodeposition time 60s
Film.
Embodiment 3
1）The ethylenediamine tetra-acetic acid of the bismuth nitrate and 0.438 g that weigh 0.395 g is dissolved in 15ml water, and solution is adjusted with concentrated ammonia liquor
PH=10, until forming colourless transparent solution, ammonium metavanadate and the 0.141 g ethylenediamine tetra-acetic acids for separately weighing 0.117 g are molten for stirring
In 15ml water, pH value of solution=10 are adjusted with concentrated ammonia liquor, stirring mixes two solution until forming yellow transparent solution, and stirring is equal
It is even, pucherite seed layer precursor liquid is made；
2）Pucherite precursor solution is spun on FTO electro-conductive glass, it is complete per spin coating that 15min, rotation are once heat-treated at 500 DEG C
It applies 3 times, 10 drop, is then heat-treated 1h at 500 DEG C, obtains pucherite seed layer every time；
3）The bismuth nitrate and 0.132 g ethylenediamine tetra-acetic acids for weighing 0.12 g are dissolved in 30ml water, with the NaOH solution of 2 mol/L
PH value of solution=9.2 are adjusted, then until forming colourless transparent solution the ammonium metavanadate of 0.036g is added, stirring is until forming in stirring
Solution is transferred in the polytetrafluoroethyllining lining of 50ml autoclaves by yellow transparent solution later；
4）There are the FTO electro-conductive glass oblique cuttings of pucherite seed layer to enter inside inner liner of reaction kettle spin coating, makes have pucherite seed layer
One down；
5）It is put into after reaction kettle is sealed in baking oven and carries out hydro-thermal reaction, 180 DEG C of thermal response 3h, cooled to room temperature is taken out
It is rinsed afterwards with deionized water, obtains the film of yellow；
6）By 500 DEG C of heat treatments of electro-conductive glass with film of gained, 4h is kept the temperature, the vanadic acid bismuth thin film of yellow is obtained.
7）It weighs 0.034g silver nitrates to be added in 100ml water, ammonium hydroxide is added dropwise and adjusts pH=9,0.152g phosphoric acid is then added
Sodium obtains silver orthophosphate precursor liquid.
8）Using three-electrode system, as working electrode, platinized platinum is used as to electrode the FTO electro-conductive glass with pucherite,
Saturated calomel electrode is reference electrode, and electrolyte is silver orthophosphate precursor liquid, in pucherite film surface with relative to saturation calomel
The current potential of electrode 0.2V carries out potentiostatic electrodeposition silver orthophosphate, and it is thin finally to obtain phosphoric acid modified by silver pucherite by electrodeposition time 90s
Film.
Embodiment 4
1）The ethylenediamine tetra-acetic acid of the bismuth nitrate and 0.438 g that weigh 0.395 g is dissolved in 15ml water, and solution is adjusted with concentrated ammonia liquor
PH=10, until forming colourless transparent solution, ammonium metavanadate and the 0.141 g ethylenediamine tetra-acetic acids for separately weighing 0.117 g are molten for stirring
In 15ml water, pH value of solution=10 are adjusted with concentrated ammonia liquor, stirring mixes two solution until forming yellow transparent solution, and stirring is equal
It is even, pucherite seed layer precursor liquid is made；
2）Pucherite precursor solution is spun on FTO electro-conductive glass, it is complete per spin coating that 15min, rotation are once heat-treated at 500 DEG C
It applies 3 times, 10 drop, is then heat-treated 1h at 500 DEG C, obtains pucherite seed layer every time；
3）The bismuth nitrate and 0.132 g ethylenediamine tetra-acetic acids for weighing 0.12 g are dissolved in 30ml water, with the NaOH solution of 2 mol/L
PH value of solution=9.2 are adjusted, then until forming colourless transparent solution the ammonium metavanadate of 0.036g is added, stirring is until forming in stirring
Solution is transferred in the polytetrafluoroethyllining lining of 50ml autoclaves by yellow transparent solution later；
4）There are the FTO electro-conductive glass oblique cuttings of pucherite seed layer to enter inside inner liner of reaction kettle spin coating, makes have pucherite seed layer
One down；
5）It is put into after reaction kettle is sealed in baking oven and carries out hydro-thermal reaction, 180 DEG C of thermal response 3h, cooled to room temperature is taken out
It is rinsed afterwards with deionized water, obtains the film of yellow；
6）By 500 DEG C of heat treatments of electro-conductive glass with film of gained, 4h is kept the temperature, the vanadic acid bismuth thin film of yellow is obtained.
7）It weighs 0.034g silver nitrates to be added in 100ml water, ammonium hydroxide is added dropwise and adjusts pH=9,0.152g phosphoric acid is then added
Sodium obtains silver orthophosphate precursor liquid.
8）Using three-electrode system, as working electrode, platinized platinum is used as to electrode the FTO electro-conductive glass with pucherite,
Saturated calomel electrode is reference electrode, and electrolyte is silver orthophosphate precursor liquid, in pucherite film surface with relative to saturation calomel
The current potential of electrode 0.2V carries out potentiostatic electrodeposition silver orthophosphate, and electrodeposition time 120s is final to obtain phosphoric acid modified by silver pucherite
Film.
Embodiment 5
1）The ethylenediamine tetra-acetic acid of the bismuth nitrate and 0.438 g that weigh 0.395 g is dissolved in 15ml water, and solution is adjusted with concentrated ammonia liquor
PH=10, until forming colourless transparent solution, ammonium metavanadate and the 0.141 g ethylenediamine tetra-acetic acids for separately weighing 0.117 g are molten for stirring
In 15ml water, pH value of solution=10 are adjusted with concentrated ammonia liquor, stirring mixes two solution until forming yellow transparent solution, and stirring is equal
It is even, pucherite seed layer precursor liquid is made；
2）Pucherite precursor solution is spun on FTO electro-conductive glass, it is complete per spin coating that 15min, rotation are once heat-treated at 500 DEG C
It applies 3 times, 10 drop, is then heat-treated 1h at 500 DEG C, obtains pucherite seed layer every time；
3）The bismuth nitrate and 0.132 g ethylenediamine tetra-acetic acids for weighing 0.12 g are dissolved in 30ml water, with the NaOH solution of 2 mol/L
PH value of solution=9.2 are adjusted, then until forming colourless transparent solution the ammonium metavanadate of 0.036g is added, stirring is until forming in stirring
Solution is transferred in the polytetrafluoroethyllining lining of 50ml autoclaves by yellow transparent solution later；
4）There are the FTO electro-conductive glass oblique cuttings of pucherite seed layer to enter inside inner liner of reaction kettle spin coating, makes have pucherite seed layer
One down；
5）It is put into after reaction kettle is sealed in baking oven and carries out hydro-thermal reaction, 180 DEG C of thermal response 3h, cooled to room temperature is taken out
It is rinsed afterwards with deionized water, obtains the film of yellow；
6）By 500 DEG C of heat treatments of electro-conductive glass with film of gained, 4h is kept the temperature, the vanadic acid bismuth thin film of yellow is obtained.
The BiVO that the present embodiment 5 is obtained4Film（Ag is not deposited3PO4Pure BiVO4Film）It is as a comparison sample, not
Deposit Ag3PO4Pure BiVO4The scanning electron microscopic picture of film is as shown in figure 3, the BiVO prepared as seen from Figure 34Film is by nanometer
Sheet BiVO4Composition.Fig. 4 is the BiVO that the present embodiment obtains4The X ray diffracting spectrum of film, as can be seen from Figure film object
It is mutually the BiVO of monoclinic form4。
The BiVO that embodiment 1 obtains4/Ag3PO4Film（Embodiment 1）The BiVO obtained with embodiment 54The XPS of film schemes
Spectrum is as shown in figure 5, as seen from Figure 5,1 product BiVO of embodiment4There are Ag on surface3PO4, the valence state composition of 5 product of embodiment is really
It is BiVO4。
The photoelectric current of test product, test specific method are：Test equipment is CHI660A electrochemical workstations, three electrodes
Test system is using Pt pieces as to electrode, saturated calomel electrode（SCE）As reference electrode, with BiVO4And BiVO4/
Ag3PO4The FTO glass of film is working electrode, and light passes through electrolytic cell quartz window, vertically shone from one sides of the FTO with semiconductor
It penetrates, all test areas are fixed on 1cm2, select linear surface sweeping voltammetry, 0.5 ~ 1.5 V of sweep interval（vs. RHE）.Electrolysis
Liquid is the kaliumphosphate buffer of 0.2 mol/L, and pH value 7, logical nitrogen half an hour, removes the dissolved oxygen in electrolyte before testing.
Light source uses 300 W xenon lamps of Perfect companies, additional filter plate（AM 1.5 G）.Fig. 6 is the light of embodiment 1,2,3,4 and 5
Current curve, with pure BiVO4（Embodiment 5）It compares, BiVO4/Ag3PO4Film（Embodiment 1,2,3,4）Photooxidation water decomposition
Current density is all higher than the former, and it is lower to analyse oxygen take-off potential.Compare the BiVO of different sedimentation times4/Ag3PO4Film（Implement
Example 1,2,3,4）As can be seen that the BiVO of 90 s of deposition4/Ag3PO4Film（Embodiment 3）Show maximum photooxidation water decomposition
Current density and minimum analysis oxygen take-off potential show preferable application prospect.
It is described above to be only used as presently preferred embodiments of the present invention and application, the limitation of the present invention is should not be construed as, it is all
The invention for being modification, replacement and the change in the other forms made of technological thought based on the present invention and realizing belongs to this hair
Bright protection domain.Can several change can be cooked the present invention under the premise of not departing from the present invention for those skilled in the art
Into and modification, these improvement and modification are also considered as protection scope of the present invention.
Claims (9)
1. a kind of photoelectrocatalysis water decomposition BiVO4/Ag3PO4The preparation method of film, which is characterized in that steps are as follows：
Step 1：Prepare pucherite seed layer precursor liquid；
1.1, it is 1 to weigh molar ratio：1.5 bismuth nitrate and ethylenediamine tetra-acetic acid is dissolved in the water and adjusts PH to 10, stirring
Form colourless transparent solution；
1.2, it is 1 to weigh molar ratio：0.5 ammonium metavanadate and edta solution, be dissolved in the water and adjust PH to
10, stirring forms yellow transparent solution；It is uniformly mixed with the colourless transparent solution of step 1.1；Pucherite kind is obtained after mixing
Sublayer precursor liquid；
Step 2：Prepare pucherite seed layer；
2.1, pretreated FTO electro-conductive glass is placed on sol evenning machine, pucherite seed layer precursor liquid is taken to carry out spin coating, spin coating
3 times, 10 drip every time, and each spin coating, which is placed in 500 DEG C, keeps the temperature 15 min；
2.2, the FTO electro-conductive glass after spin coating is placed in air atmosphere, is warming up to 500 DEG C, 1h is kept the temperature, obtains BiVO4Seed
Layer；
Step 3：Prepare vanadic acid bismuth thin film；
3.1, it is 1 to weigh molar ratio：1.5 bismuth nitrate and edta solution adjusts pH=9.2, stirring to water white transparency
The ammonium metavanadate with bismuth nitrate equimolar amounts is added afterwards, stirring is transferred to yellow transparent solution is formed in autoclave；
3.2, contain BiVO by prepared by step 24The FTO electro-conductive glass oblique cuttings of seed layer enter in reaction kettle, will be covered with seed layer
Side downward and be immersed in the yellow transparent solution of step 3.1；
3.3, reaction kettle is placed in 180 DEG C of environment and reacts 3h, is cooled to room temperature, the FTO electro-conductive glass after hydro-thermal is taken out, spends
100 DEG C of dryings after ion water washing；
3.4, the electro-conductive glass after 3.3 dryings is placed in 500 DEG C, 4h is heat-treated under air atmosphere, obtaining growth has BiVO4Film
FTO electro-conductive glass；
Step 4：Deposit Ag3PO4；
4.1, prepare the silver ammino solution of sodium phosphate；
4.2, using three-electrode system, with BiVO4The FTO electro-conductive glass of film is working electrode, the silver-colored ammonia containing sodium phosphate
Solution is electrolyte, in BiVO4Film surface potentiostatic electrodeposition Ag3PO4, apply constant potential 0.2V（vs. SCE）, electro-deposition 30/
120s obtains BiVO4/Ag3PO4Film.
2. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, the mass concentration of the bismuth nitrate in the step 1.1 is 0.0263 g/ml；The quality of the ethylenediamine tetra-acetic acid
A concentration of 0.0292 g/ml.
3. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, the mass concentration of the ammonium metavanadate in the step 1.2 is 0.0078 g/ml；The edta solution
Mass concentration is 0.0094 g/ml.
4. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, pH value of solution is adjusted to 10 using concentrated ammonia liquor in the step one.
5. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, the pretreatment in the step two is：Electro-conductive glass is cut into the small pieces of 3 cm x, 1.5 cm, respectively use acetone,
Deionized water, absolute ethyl alcohol are cleaned by ultrasonic 30 min, and cleaned electro-conductive glass are placed in absolute ethyl alcohol and is preserved, before use
With 60 DEG C of drying of air dry oven.
6. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, the mass concentration of the bismuth nitrate in the step 3.1 is 0.0040 g/ml；The edta solution matter
Measure a concentration of 0.0044 g/ml；The ammonium metavanadate mass concentration is 0.0012 g/ml.
7. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, pH value of solution=9.2 is adjusted using sodium hydroxide solution in the step 3.1.
8. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, the silver ammino solution of the step 4.1 sodium phosphate is：By the silver nitrate solution that mass concentration is 0.00034 g/ml, drop
Enriching ammonium hydroxide adjusts pH to 9, and the sodium phosphate that mass concentration is 0.00152 g/ml is then added.
9. a kind of photoelectrocatalysis water decomposition BiVO according to claim 14/Ag3PO4The preparation method of film, feature
It is, three-electrode system is with BiVO in the step 4.24The FTO electro-conductive glass of film is working electrode, and Pt pieces are
It is that reference electrode is formed by system to electrode, saturated calomel electrode.
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