CN113293393B - Bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode and preparation method and application thereof - Google Patents
Bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode and preparation method and application thereof Download PDFInfo
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- CN113293393B CN113293393B CN202011204109.9A CN202011204109A CN113293393B CN 113293393 B CN113293393 B CN 113293393B CN 202011204109 A CN202011204109 A CN 202011204109A CN 113293393 B CN113293393 B CN 113293393B
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- sodium phytate
- bismuth vanadate
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- 229940083982 sodium phytate Drugs 0.000 title claims abstract description 102
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 title claims abstract description 72
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 27
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 title claims abstract description 27
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 78
- 229910002588 FeOOH Inorganic materials 0.000 claims abstract description 45
- 239000011259 mixed solution Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002105 nanoparticle Substances 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001556 precipitation Methods 0.000 claims abstract description 14
- 239000012670 alkaline solution Substances 0.000 claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- 239000011258 core-shell material Substances 0.000 claims description 7
- 150000002505 iron Chemical class 0.000 claims description 7
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 7
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000008204 material by function Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 30
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 27
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 description 12
- QODWGQADHVWZQZ-UHFFFAOYSA-M [K+].[I-].[Bi+3].[O-][N+]([O-])=O Chemical compound [K+].[I-].[Bi+3].[O-][N+]([O-])=O QODWGQADHVWZQZ-UHFFFAOYSA-M 0.000 description 10
- 238000001354 calcination Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- OOIOHEBTXPTBBE-UHFFFAOYSA-N [Na].[Fe] Chemical compound [Na].[Fe] OOIOHEBTXPTBBE-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000008151 electrolyte solution Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 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 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- -1 iron ions Chemical class 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- MFWFDRBPQDXFRC-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;vanadium Chemical compound [V].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O MFWFDRBPQDXFRC-LNTINUHCSA-N 0.000 description 3
- 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 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- OSOVKCSKTAIGGF-UHFFFAOYSA-N [Ni].OOO Chemical compound [Ni].OOO OSOVKCSKTAIGGF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 229910000152 cobalt phosphate Inorganic materials 0.000 description 1
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- DMTIXTXDJGWVCO-UHFFFAOYSA-N iron(2+) nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Fe++].[Ni++] DMTIXTXDJGWVCO-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910000483 nickel oxide hydroxide Inorganic materials 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
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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
-
- 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)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention provides a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode and a preparation method and application thereof, belonging to the technical field of functional materials. The preparation method provided by the invention comprises the following steps: providing BiVO4Photoelectrode of said BiVO4The photoelectrode comprises a substrate and BiVO loaded on the surface of the substrate4Thin film, BiVO4The film is made of BiVO4Nanoparticle formation; mixing inorganic ferric salt, sodium phytate and water to obtain an inorganic ferric salt-sodium phytate mixed solution; dropping inorganic ferric salt-sodium phytate mixture on BiVO4And drying the surface of the photoelectrode, immersing the surface of the photoelectrode in an alkaline solution to perform precipitation reaction to obtain the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode. BiVO prepared by the method provided by the invention4The sodium phytate/FeOOH composite photoelectrode has better photoelectrocatalysis water decomposition performance.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode and a preparation method and application thereof.
Background
Semiconductor photoelectrocatalytic water oxidation, assisted by an applied bias, is considered one of the most promising methods for converting solar energy into hydrogen energy. Many semiconductor materials are used in the photoelectrocatalytic water oxidation technology, such as ZnO, CdS, Fe2O3、g-C3N4、TiO2、WO3、CuWO4Or BiVO4. Among these semiconductor materials, BiVO of monoclinic structure4The material has received extensive attention from researchers due to advantages of a suitable band gap (about 2.4eV), low cost, and ease of synthesis. However, BiVO results from slow water oxidation kinetics of photogenerated carriers at the electrode/electrolyte interface4Applications in the field of photoelectrocatalysis are still limited. Therefore, methods for improving the performance of photoelectrocatalysis have been proposed, wherein, the method of supporting oxygen evolution promoter (such as cobalt phosphate, nickel oxyhydroxide, nickel iron oxide or hydroxide) on the surface of photoelectrode has become a widely used modification method, and the supporting of oxygen evolution promoter can significantly reduce the activation energy of interfacial water oxidation, thereby reducing the overpotential of water decomposition to hydrogen and improving the current density of photoelectrode. However, in the method, the quality of the interface between the photoelectrode and the oxygen evolution promoter is poor, and the photoelectrode activity is influenced by uneven loading of the oxygen evolution promoter or gaps in the interface.
Disclosure of Invention
The invention aims to provide a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode and a preparation method and application thereof4The surface of the nano particles can obviously enhance BiVO4The interface quality with FeOOH ensures that the BiVO is obtained4the/FeOOH composite photoelectrode has better photoelectrocatalysis water decomposition performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode, which comprises the following steps:
providing BiVO4Photoelectrode of said BiVO4The photoelectrode comprises a substrate and BiVO loaded on the surface of the substrate4Film of said BiVO4The film is made of BiVO4Nanoparticle formation;
mixing inorganic ferric salt, sodium phytate and water to obtain an inorganic ferric salt-sodium phytate mixed solution;
dropwise coating the inorganic ferric salt-sodium phytate mixed solution on the BiVO4And drying the surface of the photoelectrode, immersing the surface of the photoelectrode in an alkaline solution to perform precipitation reaction to obtain the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode.
Preferably, the inorganic iron salt comprises one or more of ferric nitrate, ferric chloride and ferric sulfate.
Preferably, the concentration of the inorganic iron salt in the inorganic iron salt-sodium phytate mixed solution is 1-40 mmol/L, and the concentration of the sodium phytate is 5-40 mmol/L.
Preferably, the dripping amount of the inorganic ferric salt-sodium phytate mixed solution is 15-50 mu L/cm2。
Preferably, the alkaline solution comprises a potassium hydroxide solution or a sodium hydroxide solution, and the concentration of the alkaline solution is 0.8-1.2 mol/L.
Preferably, the drying temperature is 55-65 ℃ and the drying time is 3-8 min.
Preferably, the temperature of the precipitation reaction is 20-35 ℃ and the time is 5-60 min.
The invention provides a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode prepared by the preparation method in the technical scheme, which comprises a substrate and a bismuth vanadate/sodium phytate/iron oxyhydroxide composite film loaded on the surface of the substrate, wherein the bismuth vanadate/sodium phytate/iron oxyhydroxide composite film is formed by a core-shell structure material, and the core of the core-shell structure material is BiVO4Nanoparticles of said BiVO4The surface of the nano-particles is coated with an FeOOH shell layer after being modified by sodium phytate.
Preferably, the BiVO4The particle size of the nano particles is 100-200 nm; what is needed isThe thickness of the FeOOH shell layer is 3-10 nm.
The invention provides application of the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode in photoelectrocatalysis water oxidation reaction.
The invention provides a preparation method of a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode, which comprises the following steps: providing BiVO4Photoelectrode of said BiVO4The photoelectrode comprises a substrate and BiVO loaded on the surface of the substrate4Film of said BiVO4The film is made of BiVO4Nanoparticle formation; mixing inorganic ferric salt, sodium phytate and water to obtain an inorganic ferric salt-sodium phytate mixed solution; dropwise coating the inorganic ferric salt-sodium phytate mixed solution on the BiVO4And drying the surface of the photoelectrode, immersing the surface of the photoelectrode in an alkaline solution to perform precipitation reaction to obtain the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode. The invention uses sodium phytate with strong complexation with iron ions to uniformly load the iron-based oxygen evolution cocatalyst FeOOH on BiVO through simple dripping coating method and precipitation reaction4The photoelectrode surface can effectively improve BiVO4Integrity with FeOOH interface and simultaneously ensures BiVO4The nano particles and the FeOOH layer are tightly connected, so that a gap between the nano particles and the FeOOH layer is effectively avoided, the transfer resistance of a photogenerated hole and the recombination speed of a photogenerated carrier are reduced, the overpotential of water decomposition is reduced, the photocurrent density is increased, and the BiVO is obtained4The sodium phytate/FeOOH composite photoelectrode has better photoelectrocatalysis water decomposition performance.
In addition, the method provided by the invention is simple to operate, the Fe element is abundant in the natural world, and the BiVO can be effectively reduced by taking FeOOH as an oxygen evolution cocatalyst4And (4) modification cost.
Drawings
FIG. 1 is BiVO of example 14Photoelectrode and BiVO4XRD pattern of/sodium phytate/FeOOH composite photoelectrode;
FIG. 2 is BiVO in example 24Photoelectrode and BiVO4SEM image of/sodium phytate/FeOOH composite photoelectrode;
FIG. 3 is BiVO in example 24TEM image of/sodium phytate/FeOOH composite photoelectrode;
FIG. 4 is BiVO in example 34Photoelectrode and BiVO4Linear scanning voltammetry curve graphs of the/sodium phytate/FeOOH composite photoelectrode in a dark state and under illumination;
FIG. 5 is BiVO of comparative example 14Photoelectrode and BiVO4Linear sweep voltammogram of the/FeOOH composite photoelectrode in a dark state and under illumination.
Detailed Description
The invention provides a preparation method of a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode, which comprises the following steps:
providing BiVO4Photoelectrode of said BiVO4The photoelectrode comprises a substrate and BiVO loaded on the surface of the substrate4Film of said BiVO4The film is made of BiVO4Nanoparticle formation;
mixing inorganic ferric salt, sodium phytate and water to obtain an inorganic ferric salt-sodium phytate mixed solution;
dropwise coating the inorganic ferric salt-sodium phytate mixed solution on the BiVO4And drying the surface of the photoelectrode, immersing the surface of the photoelectrode in an alkaline solution to perform precipitation reaction to obtain the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode.
The invention provides BiVO4Photoelectrode of said BiVO4The photoelectrode comprises a substrate and BiVO loaded on the surface of the substrate4Film of said BiVO4The film is made of BiVO4And (4) forming nanoparticles. The substrate is not particularly limited in the invention, and may be any substrate known to those skilled in the art, and may specifically be FTO conductive glass. In the invention, the BiVO4The thickness of the film is preferably 500-1000 nm; the BiVO4The particle size of the nanoparticles is preferably 100 to 200 nm. The invention is to the BiVO4The source of the photoelectrode is not particularly limited, and the photoelectrode is prepared by adopting a method well known by the technical personnel in the field; in the invention, the BiVO4The preparation method of the photoelectrode preferably comprises the following steps:
adjusting the pH value of a potassium iodide aqueous solution to 1.7, and then mixing the potassium iodide aqueous solution with bismuth nitrate to obtain a potassium iodide-bismuth nitrate mixed solution; mixing p-benzoquinone with ethanol to obtain a p-benzoquinone solution;
mixing the potassium iodide-bismuth nitrate mixed solution with a p-benzoquinone solution to obtain an electrolyte solution; under the existence of the electrolyte solution, carrying out constant potential deposition by taking a substrate as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum mesh as a counter electrode to obtain a BiOI photoelectrode;
mixing vanadium acetylacetonate and dimethyl sulfoxide to obtain vanadyl acetylacetonate solution;
dropwise coating the vanadyl acetylacetonate solution on the surface of the BiOI electrode, and calcining to obtain BiVO4And a photoelectrode.
The pH value of the potassium iodide aqueous solution is adjusted to 1.7, and then the potassium iodide aqueous solution is mixed with bismuth nitrate to obtain a potassium iodide-bismuth nitrate mixed solution. In the invention, the concentration of the potassium iodide aqueous solution is preferably 0.45-0.55 mol/L, and more preferably 0.5 mol/L. In the present invention, the agent for adjusting the pH of the aqueous potassium iodide solution is preferably concentrated nitric acid, and the concentration of the concentrated nitric acid is preferably 68 wt%. In the invention, the concentration of bismuth nitrate in the potassium iodide-bismuth nitrate mixed solution is preferably 0.05-0.07 mol/L, and more preferably 0.06 mol/L.
The invention mixes p-benzoquinone with ethanol to obtain a p-benzoquinone solution. In the present invention, the concentration of p-benzoquinone in the p-benzoquinone solution is preferably 0.25 to 0.35mol/L, and more preferably 0.3 mol/L.
After a potassium iodide-bismuth nitrate mixed solution and a p-benzoquinone solution are obtained, the potassium iodide-bismuth nitrate mixed solution and the p-benzoquinone solution are mixed to obtain an electrolyte solution. In the present invention, the volume ratio of the potassium iodide-bismuth nitrate mixed solution to the p-benzoquinone solution is preferably 5: (1.8-2.2), more preferably 5: 2.
after the electrolyte solution is obtained, the invention preferably performs constant potential deposition in the presence of the electrolyte solution by using a substrate as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum mesh as a counter electrode to obtain the BiOI photoelectrode. In the invention, the potential of the constant potential deposition is preferably-0.05 to-0.2V, more preferably-0.1V, and the time is preferably 3 to 10min, more preferably 5 min.
After the constant potential deposition, the obtained sample is preferably cleaned to remove surface impurities; in the present invention, the cleaning agent preferably includes deionized water.
The invention mixes vanadium acetylacetonate and dimethyl sulfoxide to obtain vanadyl acetylacetonate solution. In the invention, the concentration of the vanadyl acetylacetonate solution is preferably 0.08-0.12 mol/L, and more preferably 0.1 mol/L.
After a BiOI photoelectrode and a vanadyl acetylacetonate solution are obtained, the method comprises the steps of dropwise coating the vanadyl acetylacetonate solution on the surface of the BiOI photoelectrode, and then calcining to obtain BiVO4And a photoelectrode. In the invention, the preferable dropping amount of the vanadyl acetylacetonate solution is 100-120 mu L/cm2(ii) a The calcination temperature is preferably 440-460 ℃, more preferably 450 ℃, and the time is preferably 1.5-2.5 h, more preferably 2 h; the calcination is preferably carried out in a muffle furnace. In the present invention, during the calcination, the BiOI is decomposed into Bi2O3Decomposition of vanadyl acetylacetonate to V2O5Said Bi2O3And V2O5High-temperature solid-phase reaction is carried out to generate BiVO4。
In the invention, the calcination preferably further comprises washing, specifically, the sample obtained after the calcination is placed in 1mol/L sodium hydroxide solution and soaked for 30min at room temperature to remove residual V2O5To obtain BiVO4And a photoelectrode.
The invention mixes inorganic molysite, sodium phytate and water to obtain the inorganic molysite-sodium phytate mixed solution. In the present invention, the inorganic iron salt preferably includes one or more of ferric nitrate, ferric chloride and ferric sulfate, and more preferably ferric nitrate, ferric chloride or ferric sulfate. In the invention, the concentration of the inorganic iron salt in the inorganic iron salt-sodium phytate mixed solution is preferably 1-40 mmol/L, and more preferably 5-10 mmol/L; the concentration of the sodium phytate in the inorganic ferric salt-sodium phytate mixed solution is preferably 5-40 mmol/L, and more preferably 20-30 mmol/L.
Obtaining BiVO4After photoelectrode and inorganic iron salt-sodium phytate mixed solution, the invention coats the inorganic iron salt-sodium phytate mixed solution on BiVO4And drying the surface of the photoelectrode, immersing the surface of the photoelectrode in an alkaline solution to perform precipitation reaction to obtain the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode. In the invention, the dripping amount of the inorganic ferric salt-sodium phytate mixed solution is preferably 15-50 mu L/cm2More preferably 25 to 30. mu.L/cm2. The dropping coating method of the inorganic iron salt-sodium phytate mixed solution is not particularly limited, and the dropping coating method known by the technical personnel in the field is adopted to ensure that the inorganic iron salt-sodium phytate mixed solution is uniformly coated. The drying method is not particularly limited, and a drying method known to those skilled in the art may be used. In the invention, the drying temperature is preferably 55-65 ℃, more preferably 60 ℃, and the drying time is preferably 3-8 min, more preferably 5 min; the drying is preferably carried out in an oven. In the invention, inorganic ferric salt-sodium phytate mixed liquid is dripped on the BiVO4After the surface of the photoelectrode, the phytate ion can be firmly adsorbed on BiVO4BiVO of photoelectrode4The surface of the nano-particles is then complexed with iron ions in the system, and the BiVO is subjected to subsequent precipitation reaction4The FeOOH shell layer is formed on the surface of the nano-particles.
In the invention, the alkaline solution preferably comprises a potassium hydroxide solution or a sodium hydroxide solution, and the concentration of the alkaline solution is preferably 0.8-1.2 mol/L, and more preferably 1 mol/L. In the invention, the temperature of the precipitation reaction is preferably 20-35 ℃, and more preferably 25-30 ℃; the time is preferably 5 to 60min, and more preferably 5 to 10 min. In the invention, in the precipitation reaction process, iron ions react in an alkaline environment to generate FeOOH, and the FeOOH is deposited on BiVO4The FeOOH shell layer is formed on the surface of the nano-particles.
In the present invention, it is preferable that the precipitation reaction is followed by washing, specifically, after the precipitation reaction, the obtained sample is taken out and washed with deionized water to remove impurities on the surface.
The invention provides any one of the technical schemesThe bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode prepared by the preparation method comprises a substrate and a bismuth vanadate/sodium phytate/iron oxyhydroxide composite film loaded on the surface of the substrate, wherein the bismuth vanadate/sodium phytate/iron oxyhydroxide composite film is formed by a core-shell structure material, and the core of the core-shell structure material is BiVO4Nanoparticles of said BiVO4The surface of the nano-particles is coated with an FeOOH shell layer after being modified by sodium phytate. In the invention, the BiVO4The particle size of the nano particles is preferably 100-200 nm; the thickness of the FeOOH shell layer is preferably 3-10 nm.
The invention provides the application of the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode in the technical scheme in the photoelectrocatalysis water oxidation reaction, and the application is not particularly limited and can be applied by adopting a mode known by a person skilled in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Mixing potassium iodide and ultrapure water, and adjusting the pH value to 1.7 by using concentrated nitric acid (the concentration is 68 wt%) to obtain a potassium iodide aqueous solution with the concentration of 0.5 mol/L; mixing bismuth nitrate with the potassium iodide aqueous solution, and dissolving by ultrasonic to obtain a potassium iodide-bismuth nitrate mixed solution, wherein the concentration of bismuth nitrate in the potassium iodide-bismuth nitrate mixed solution is 0.06 mol/L;
mixing p-benzoquinone with ethanol, and dissolving the mixture by ultrasonic waves to obtain a p-benzoquinone solution, wherein the concentration of the p-benzoquinone in the p-benzoquinone solution is 0.3 mol/L;
mixing the potassium iodide-bismuth nitrate mixed solution and a p-benzoquinone solution in a volume ratio of 5:2, uniformly stirring, taking the mixed solution as an electrolyte solution, adopting FTO conductive glass as a working electrode, an Ag/AgCl electrode as a reference electrode and a platinum mesh as a counter electrode, performing electrodeposition for 5min under the condition that the potential is-0.1V, and cleaning by using deionized water after the deposition is finished to remove surface impurities to obtain a BiOI photoelectrode;
mixing vanadium acetylacetonate with dimethyl sulfoxide to obtain 0.1mol/L vanadyl acetylacetonate solution, transferring 100 mu L of the vanadyl acetylacetonate solution by using a liquid transfer gun, and dropwise coating the vanadyl acetylacetonate solution on the surface of the BiOI electrode (the dropwise coating amount of the vanadyl acetylacetonate solution is 100 mu L/cm)2) Then calcining the mixture for 2 hours in a muffle furnace at the temperature of 450 ℃, naturally cooling the mixture to room temperature, taking out the photoelectrode, placing the photoelectrode into 1mol/L sodium hydroxide solution, and soaking the photoelectrode for 30 minutes at the room temperature (25 ℃) to remove residual V2O5To obtain BiVO4A photoelectrode;
mixing ferric nitrate, sodium phytate and water to obtain a ferric nitrate-sodium phytate mixed solution, wherein the concentration of the ferric nitrate in the ferric nitrate-sodium phytate mixed solution is 10mmol/L, and the concentration of the sodium phytate is 20 mmol/L; using a liquid transfer gun to transfer 20 mu L of the ferric nitrate-sodium phytate mixed liquid to be dripped on the BiVO4The surface of the photoelectrode (the dripping amount of the mixed solution of ferric nitrate and sodium phytate is 25 mu L/cm)2) Then drying in a 60 ℃ oven for 5min, naturally cooling to room temperature, taking out the photoelectrode, soaking in 1mol/L potassium hydroxide solution, reacting for 5min at 25 ℃, and washing away surface impurities by deionized water after the reaction is finished to obtain BiVO4The sodium phytate/FeOOH composite photoelectrode.
FIG. 1 is BiVO of example 14Photoelectrode and BiVO4The XRD pattern of the/sodium phytate/FeOOH composite photoelectrode is shown in figure 1, and BiVO is obtained in the modification process4The crystal form and the grain size of the crystal form are not changed by the load. In addition, no diffraction peak associated with FeOOH was observed, indicating that the supported FeOOH is amorphous.
Example 2
BiVO was prepared according to the method of example 14A photoelectrode;
mixing ferric chloride, sodium phytate and water to obtain a ferric chloride-sodium phytate mixed solution, wherein the concentration of ferric chloride in the ferric chloride-sodium phytate mixed solution is 5mmol/L, and the concentration of sodium phytate is 30 mmol/L; using a liquid transfer gun to transfer 25 μ L of the ferric chloride-The sodium phytate mixed liquid is dripped on the BiVO4The surface of the photoelectrode (the dripping amount of the mixed solution of ferric chloride and sodium phytate is 25 mu L/cm)2) Then drying in a 60 ℃ oven for 5min, naturally cooling to room temperature, taking out the photoelectrode, soaking in 1mol/L potassium hydroxide solution, reacting for 10min at 25 ℃, and washing away surface impurities by deionized water after the reaction is finished to obtain BiVO4The sodium phytate/FeOOH composite photoelectrode.
FIG. 2 is BiVO in example 24Photoelectrode and BiVO4Scanning electron microscope image of/sodium phytate/FeOOH composite photoelectrode, wherein (a) is BiVO4Photoelectrode, (b) is BiVO4The sodium phytate/FeOOH composite photoelectrode. As can be seen from FIG. 2, BiVO4Is nano-particles, and the surface is smooth; FeOOH is uniformly loaded on BiVO under the action of sodium phytate4The surface of the nano-particles forms a stable core-shell structure, which shows that sodium phytate can be used as a stable binding molecule to firmly adhere FeOOH to BiVO4A nanoparticle surface, wherein the BiVO4The particle size of the nano particles is 100-200 nm, and the thickness of the shell layer is 3-10 nm.
FIG. 3 is BiVO in example 24The transmission electron microscope image of the/sodium phytate/FeOOH composite photoelectrode can further prove BiVO from figure 34The surface of the nano-particles is uniformly loaded with a layer of FeOOH and BiVO4The nano particles are completely wrapped in FeOOH, and the surface has no gap.
Example 3
BiVO was prepared according to the method of example 14A photoelectrode;
mixing ferric sulfate, sodium phytate and water to obtain a ferric sulfate-sodium phytate mixed solution, wherein the concentration of ferric sulfate in the ferric sulfate-sodium phytate mixed solution is 5mmol/L, and the concentration of sodium phytate is 30 mmol/L; transferring 30 mu L of the ferric sulfate-sodium phytate mixed solution by using a liquid transfer gun, and coating the solution on the BiVO4The surface of the photoelectrode (the dripping amount of the mixed solution of ferric sulfate and sodium phytate is 30 mu L/cm)2) Then drying in a 60 ℃ oven for 5min, naturally cooling to room temperature, taking out the obtained photoelectrode, soaking in 1mol/L potassium hydroxide solution, reacting for 5min at 25 ℃, washing with deionized water after the reaction is finishedSurface impurities to obtain BiVO4The sodium phytate/FeOOH composite photoelectrode.
FIG. 4 is BiVO in example 34Photoelectrode and BiVO4Linear sweep voltammetry curve of/sodium phytate/FeOOH composite photoelectrode in dark state and illumination. As can be seen from FIG. 4, BiVO containing sodium phytate interface4BiVO (BiVO) with sodium phytate/FeOOH composite photoelectrode without modification4The photocurrent of the photoelectrode is obviously improved, which shows that BiVO4The interface charge transfer resistance of the/sodium phytate/FeOOH composite photoelectrode is reduced, which proves that BiVO can be improved by adopting sodium phytate4The interface quality of the sodium phytate/FeOOH composite photoelectrode can further promote interface hole transfer, and the photoelectrocatalysis efficiency is favorably improved.
Comparative example 1
A composite photoelectrode was prepared according to the method of example 3, except that sodium phytate was omitted and the final composite photoelectrode was BiVO4the/FeOOH composite photoelectrode.
FIG. 5 is BiVO of comparative example 14Photoelectrode and BiVO4Linear sweep voltammogram of the/FeOOH composite photoelectrode in a dark state and under illumination. As can be seen from FIG. 5, BiVO was observed in the absence of sodium phytate4The current density of the/FeOOH composite photoelectrode is higher than that of BiVO4The photoelectrode is only slightly improved, which indicates that the single FeOOH cocatalyst is difficult to realize effective water decomposition, and the existence of the sodium phytate is important to realize the effective water decomposition.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode comprises the following steps:
providing BiVO4Photoelectrode of said BiVO4The photoelectrode comprises a substrate and BiVO loaded on the surface of the substrate4Film of said BiVO4The film is made of BiVO4Nanoparticle formation;
mixing inorganic ferric salt, sodium phytate and water to obtain an inorganic ferric salt-sodium phytate mixed solution;
dropwise coating the inorganic ferric salt-sodium phytate mixed solution on the BiVO4And drying the surface of the photoelectrode, immersing the surface of the photoelectrode in an alkaline solution to perform precipitation reaction to obtain the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode.
2. The preparation method of claim 1, wherein the inorganic iron salt comprises one or more of ferric nitrate, ferric chloride and ferric sulfate.
3. The method according to claim 1 or 2, wherein the concentration of the inorganic iron salt in the mixed solution of the inorganic iron salt and the sodium phytate is 1 to 40mmol/L, and the concentration of the sodium phytate is 5 to 40 mmol/L.
4. The method according to claim 3, wherein the amount of the inorganic ferric salt-sodium phytate mixed solution is 15 to 50 μ L/cm2。
5. The preparation method according to claim 1, wherein the alkaline solution comprises a potassium hydroxide solution or a sodium hydroxide solution, and the concentration of the alkaline solution is 0.8-1.2 mol/L.
6. The method according to claim 1 or 5, wherein the drying is carried out at a temperature of 55 to 65 ℃ for 3 to 8 min.
7. The method according to claim 1 or 5, wherein the precipitation reaction is carried out at a temperature of 20 to 35 ℃ for 5 to 60 min.
8. The bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode prepared by the preparation method of any one of claims 1 to 7 comprises a substrate and a loadThe bismuth vanadate/sodium phytate/iron oxyhydroxide composite film is formed by a core-shell structure material, and the core of the core-shell structure material is BiVO4Nanoparticles of said BiVO4The surface of the nano-particles is coated with an FeOOH shell layer after being modified by sodium phytate.
9. The bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode of claim 8, wherein the BiVO is4The particle size of the nano particles is 100-200 nm; the thickness of the FeOOH shell layer is 3-10 nm.
10. The use of the bismuth vanadate/sodium phytate/iron oxyhydroxide composite photoelectrode according to claim 8 or 9 in photoelectrocatalytic water oxidation reactions.
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