CN110438526A - A kind of preparation method of nanogold codope iron oxide composite catalyzing electrode, catalysis electrode and electrolysis wetting system - Google Patents
A kind of preparation method of nanogold codope iron oxide composite catalyzing electrode, catalysis electrode and electrolysis wetting system Download PDFInfo
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- CN110438526A CN110438526A CN201910644056.3A CN201910644056A CN110438526A CN 110438526 A CN110438526 A CN 110438526A CN 201910644056 A CN201910644056 A CN 201910644056A CN 110438526 A CN110438526 A CN 110438526A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- 238000005868 electrolysis reaction Methods 0.000 title claims description 15
- 238000009736 wetting Methods 0.000 title claims description 7
- 239000000758 substrate Substances 0.000 claims abstract description 42
- 239000010936 titanium Substances 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001354 calcination Methods 0.000 claims abstract description 37
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 31
- 229910052802 copper Inorganic materials 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 18
- 239000010941 cobalt Substances 0.000 claims abstract description 18
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011135 tin Substances 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 229910052718 tin Inorganic materials 0.000 claims abstract description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 5
- 239000001509 sodium citrate Substances 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 39
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 27
- 239000012498 ultrapure water Substances 0.000 claims description 27
- 239000002243 precursor Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 238000007598 dipping method Methods 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 33
- 229910002588 FeOOH Inorganic materials 0.000 description 24
- 239000010931 gold Substances 0.000 description 19
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 14
- 238000012360 testing method Methods 0.000 description 13
- 238000002156 mixing Methods 0.000 description 10
- 238000007789 sealing Methods 0.000 description 9
- 238000001035 drying Methods 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000006424 Flood reaction Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- GTKRFUAGOKINCA-UHFFFAOYSA-M chlorosilver;silver Chemical group [Ag].[Ag]Cl GTKRFUAGOKINCA-UHFFFAOYSA-M 0.000 description 4
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 4
- 239000006193 liquid solution Substances 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 230000001052 transient effect Effects 0.000 description 4
- 229910017827 Cu—Fe Inorganic materials 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XTLNYNMNUCLWEZ-UHFFFAOYSA-N ethanol;propan-2-one Chemical compound CCO.CC(C)=O XTLNYNMNUCLWEZ-UHFFFAOYSA-N 0.000 description 2
- 229910001922 gold oxide Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- 229910020598 Co Fe Inorganic materials 0.000 description 1
- 229910002519 Co-Fe Inorganic materials 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229910052721 tungsten Inorganic materials 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8913—Cobalt and noble metals
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8966—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
-
- 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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- 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
-
- 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
- C25B1/50—Processes
- C25B1/55—Photoelectrolysis
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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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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- 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)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Catalysts (AREA)
Abstract
Inventor provide a kind of preparation method of nanogold codope iron oxide composite catalyzing electrode, the following steps are included: the first metal-calcining iron oxide-conductive substrates compound is impregnated with the solution containing nanogold, nanogold codope iron oxide composite catalyzing electrode is obtained；The solution containing nanogold is prepared using reduction of sodium citrate method, first metal, is selected from one or more of cobalt, titanium, tin, copper.The first metal-calcining iron oxide-conductive substrates compound is impregnated using nano-Au solution in above-mentioned technical proposal, this method makes nanogold be deposited on the first metal-calcining iron oxide-conductive substrates compound surface, nanogold can effectively facilitate the light absorption of iron oxide, expand ABSORPTION EDGE.Compound chemical property with higher, can get higher photoelectric current, while stability is preferable, can effectively catalysis electrode water reaction.
Description
Technical field
The present invention relates to catalyst technical fields, especially with regard to a kind of nanogold codope iron oxide composite catalyzing electrode
Preparation method, catalysis electrode and electrolysis wetting system.
Background technique
Recently as the fast development of nanosecond science and technology, people, which largely concentrate on research, has good crystal form and pattern,
Excellent physical and chemical performance nano structural material, and it is applied to catalytic field.Compared to other materials, nanometer materials tool
There is bigger specific surface area, to increase the contact of catalyst with reactant and solution, provides more reactivity sites, because
This improves photo-generated carrier density to increase the photoelectric conversion efficiency of material, to improve the catalytic efficiency of catalyst.Nano oxygen
Change iron as a kind of nontoxic photoelectric material, rich content, unglazed corrosion phenomenon.
Iron oxide is a kind of n-type semiconductor, has relatively narrow band gap width, and can be absorbed nearly 50% in solar energy
Energy.One or two kinds of metallic element is mixed in iron oxide, its electric conductivity can be improved, and reduces electron-hole pair
It is compound, improve the catalytic activity of iron oxide.Chinese patent CN105780087A uses Electric oxidative synthesis 1-dimention nano oxide,
Organic matter is needed to make electrolyte, it is also necessary to which pattern assists liquid, cumbersome；Chinese patent CN103880091A is closed using hydro-thermal method
At the ferric oxide particles of nanometer hexagon, electric conductivity is poor；Chinese patent CN104815668A using electro-deposition synthesis Ta,
The iron oxide of Al codope, film thickness are difficult to control.
Summary of the invention
In order to solve iron oxide, for hole expansion from short, oxidation reaction kinetics are poor, and pass through atom in practical applications
Uneven, the cumbersome problem of the material morphology of layer sedimentation, electrochemical deposition method and supersonic spraying preparation, it is desirable to provide
Simply, with the ferric oxide catalyst of stronger electrochemical catalysis performance.
The first aspect of the present invention provides a kind of preparation method of nanogold codope iron oxide composite catalyzing electrode,
The following steps are included:
First metal-calcining iron oxide-conductive substrates compound is impregnated with the solution containing nanogold, obtains nanometer
Golden codope iron oxide composite catalyzing electrode；The solution containing nanogold is prepared using reduction of sodium citrate method, and described first
Metal is selected from one or more of cobalt, titanium, tin, copper.
Preferably, the concentration of the nano-Au solution is 0.97-1.94mmol/L, dip time 10-15h.
Preferably, the first metal-calcining iron oxide-conductive substrates compound preparation the following steps are included:
Pretreatment: first conductive substrates are successively cleaned by ultrasonic with organic solvent and ultrapure water, the organic solvent is
Ethyl alcohol, acetone or its mixed liquor；
Hydro-thermal: pretreated conductive substrates being put into after precursor solution and carry out hydro-thermal reaction, the hydro-thermal reaction
Temperature is 80-120 DEG C, time 1-12h；Contain the Fe of 0.001-0.4mol/L in the precursor solution3+Ion；
Calcining: by conductive substrates cooled to room temperature, after being cleaned with ultrapure water, by room temperature to 500-800
DEG C calcining 1-4h, cooled to room temperature；
First is metal-doped:
Before calcination, conductive substrates are impregnated in the dipping solution of the first metal ion containing 0.001-0.4mol/L
In；
With or
After firing, conductive substrates are impregnated in the dipping solution of the first metal ion containing 0.001-0.4mol/L
In.
Preferably, the precursor solution also the first metal ion containing 0.001-0.4mol/L.
Preferably, in the calcining step, heating rate is 2~10 DEG C/min.
Preferably, in the calcining step, the atmosphere that when calcining uses include air and or nitrogen.
Preferably, the conductive substrates include titanium, electro-conductive glass and foamed material.
The second aspect of the present invention provides a kind of nanogold codope iron oxide composite catalyzing electrode, the catalysis electricity
It is prepared by the preparation method of pole first aspect present invention.
Preferably, the catalysis electrode is used for electrolysis water.
The third aspect of the present invention, provides a kind of electrolysis wetting system, and the electrolysis wetting system uses the present invention second
Catalysis electrode described in aspect is anode.
It is different from the prior art, is led in above-mentioned technical proposal using nano-Au solution dipping the first metal-calcining iron oxide-
Electric substrate composite, this method make nanogold be deposited on the first metal-calcining iron oxide-conductive substrates compound surface,
Nanogold can effectively facilitate the light absorption of iron oxide, expand ABSORPTION EDGE.Compound chemical property with higher can get
Higher photoelectric current, while stability is preferable, it can effectively catalysis electrode water reaction.
Detailed description of the invention
Fig. 1 is optical electro-chemistry test schematic diagram, comprising to electrode Pt piece (CE), working electrode (WE), reference electrode (RE).
It is platinized platinum to electrode, working electrode is the iron oxide electrode of preparation, and reference electrode is silver-silver chloride electrode.
Fig. 2 is Co-Fe prepared by embodiment 12O3、(Co,Ti)-Fe2O3、(Co,Ti)-Fe2O3The density of photocurrent of/Au
(j-V) curve.
Fig. 3 is Fe prepared by embodiment 22O3、(Co,Cu)-Fe2O3、(Co,Cu)-Fe2O3The density of photocurrent (j-V) of/Au
Curve.
Fig. 4 is Fe prepared by embodiment 32O3Transient state photoelectric respone curve (current density-time).
Fig. 5 is (Co, Cu)-Fe prepared by embodiment 32O3Transient state photoelectric respone curve (current density-time).
Fig. 6 is (Co, Cu)-Fe prepared by embodiment 32O3The transient state photoelectric respone curve (current density-time) of/Au.
Specific embodiment
Technology contents, construction feature, the objects and the effects for detailed description technical solution, below in conjunction with specific reality
It applies example and attached drawing is cooperated to be explained in detail.
In present embodiment, conductive substrates include titanium, electro-conductive glass and foamed material.Conductive glass surface resistance be >=
Tin indium oxide (ITO) conduction specifically can be used in 100 Ω/sq, electro-conductive glass thickness >=2mm, surface conductive layer thickness >=200nm
The fin oxide condutire glass (FTO) of glass or fluorine doped；Titanium includes titanium net and titanium sheet, and the thickness of titanium sheet is generally 0.05mm；Titanium net
Specification be 100 mesh；Foamed material includes titanium foam, foam nickel chromium triangle and nickel foam, and thickness is 1.5mm.
In present embodiment, reduction of sodium citrate method prepares the solution containing nanogold, the specific steps are as follows: is taken with liquid-transfering gun
2.0mL aqueous solution of chloraurate (0.01912g/mL), which is added in 100mL ultrapure water, to be heated to boiling, and is rapidly added while stirring
10mL sodium citrate solution (10%W/V) then makes the mixed liquor boil 2 minutes, is finally cooled to room temperature in cold water.
In present embodiment, hydro-thermal reaction carries out in water heating kettle, is put into baking oven and reacts after the completion of water heating kettle sealing, instead
Water heating kettle cooled to room temperature after the completion of answering.Sealing is sealed using the high pressure resistant medium that insulate, and after hydro-thermal reaction
Sealing medium is removed, the sealing medium used is high voltage bearing insulating tape or the epoxy resin of insulating.
In present embodiment；Fe is provided in the precursor solution3+Ion includes FeCl3、Fe(NO3)3, provide first
Metal ion includes cobalt nitrate, butyl titanate, stannic chloride, copper nitrate.
The performance test methods that the present invention uses are as described below:
1) photoelectricity current test:
Test condition: voltage range is -1.1-1.0VAg/AgCl, sweeping speed is 0.01V/S, the irradiation of 300W xenon lamp.
Voltage conversion equation: ERHE=EAg/AgCl+0.197V+0.059pH。
2) transient current responds:
Test condition: voltage E=0.4VRHE, sweep time is 400 seconds, and manual chopping the light, 300W xenon lamp first irradiates 10 seconds, so
It light-blocking 10 seconds afterwards, circuits sequentially until 400 seconds.
A kind of preparation of the catalysis electrode of embodiment 1
Use nickel foam (1cm × 3cm) as conductive substrates, which is pre-processed.Successively use acetone-ethanol
After (volume ratio 1:1) and ultrapure water are successively cleaned by ultrasonic, it is put into 60 DEG C of dryings in air dry oven；
Pretreated conductive substrates nickel foam is placed in water heating kettle liner, it is molten that presoma is added into water heating kettle liner
Liquid makes precursor solution just flood the part conductive substrates (1cm × 1cm)；Precursor solution: with ultrapure water as solvent, contain
Ferric nitrate, 0.02mol/L cobalt nitrate, 0.1mol/L ammonium fluoride, the 0.16mol/L urea of 0.01mol/L；
100 DEG C of heating 2h in baking oven will be put into after the completion of water heating kettle sealing；After the reaction was completed by water heating kettle with furnace in 10min
Inside it is cooled to room temperature；Substrate is taken out from water heating kettle, is placed on after ultrapure water cleans in air dry oven and is dried at 60 DEG C, obtains
Mix the FeOOH (Co-FeOOH) of cobalt；
Co-FeOOH is immersed in the ethanol solution of 0.1mol/L butyl titanate, dip time is 12 hours, takes out and uses
Ultrapure water gently rinses, and obtains FeOOH (Co, the Ti)-FeOOH for mixing cobalt and titanium；
(Co, Ti)-FeOOH is placed on temperature programming in tube furnace, rises to 500 from room temperature with the heating rate of 5 DEG C/min
It is heated 2 hours after DEG C, cooled to room temperature, obtains calcining iron oxide (Co, the Ti)-Fe for mixing cobalt and titanium2O3；
Calcining iron oxide (Co, Ti)-Fe of cobalt and titanium will be mixed2O3；It is immersed in the solution containing nanogold (0.97mmol/L)
In, dip time is 12 hours, then takes out sample ultrapure water, naturally dry obtains the cobalt and titanium of decorated by nano-gold
Iron oxide (Co, Ti)-Fe of codope2O3/ Au catalysis electrode.
For the catalysis electrode obtained using embodiment 1 as anode (working electrode), Pt is cathode to electrode, and reference electrode is silver-
Silver chloride electrode.Electrolyte: 26 DEG C of 1M KOH, test temperature carry out electricity hydrolysis test.Test results are shown in figure 2.Wherein, E
=1.62VRHEWhen, the cobalt and Ti doped calcining iron oxide of decorated by nano-gold prepared by embodiment 1, (Co, Ti)-Fe2O3/Au
Obtain 14.28mA/cm2Density of photocurrent.
Show that the catalyst of preparation is applied to density of photocurrent with higher when electrolysis water process.Illustrate embodiment system
Standby catalysis electrode chemical property with higher, can effectively catalytic electrolysis water reaction.
Embodiment 2
Use titanium sheet (1cm × 3cm) as conductive substrates, which is pre-processed.Successively use acetone-ethanol (body
Product is than 1:1) and after ultrapure water is successively cleaned by ultrasonic, it is put into 60 DEG C of dryings in air dry oven；
Pretreated conductive substrates are placed in water heating kettle liner, precursor solution are added into water heating kettle liner, before making
It drives liquid solution and floods the part conductive substrates (1cm × 1cm)；Precursor solution: dehydrated alcohol, ultrapure water as solvent (volume ratio are used
For 3:7), the iron chloride containing 0.01mol/L, 0.1mol/L sodium nitrate, it is 1 that concentrated hydrochloric acid, which adjusts pH value,；
100 DEG C of heating 4h in baking oven will be put into after the completion of water heating kettle sealing；Water heating kettle is cooled to the furnace after the reaction was completed
Room temperature；Conductive substrates are taken out from water heating kettle, are placed on after ultrapure water cleans in air dry oven and are dried at 40 DEG C, obtain hydroxyl
Base iron oxide FeOOH；
FeOOH FeOOH is placed on temperature programming in tube furnace, is risen to from room temperature with the heating rate of 5 DEG C/min
It is heated 2 hours after 500 DEG C, cooled to room temperature obtains calcining iron oxide Fe2O3；
By calcining iron oxide Fe2O3It is immersed in the aqueous solution of copper nitrate containing 0.01mol/L and 0.01mol/L cobalt nitrate, soaks
It stain 12 hours, takes out and uses ultrapure water, the drying at 40 DEG C is obtained, to calcining iron oxide (Co, the Cu)-Fe for mixing cobalt and copper2O3；
Calcining iron oxide (Co, Cu)-Fe of cobalt and copper will be mixed2O3It is immersed in the solution containing nanogold (0.97mmol/L),
Dip time is 12 hours, then takes out sample ultrapure water, naturally dry, the cobalt and copper for obtaining decorated by nano-gold are co-doped with
Miscellaneous iron oxide (Co, Cu)-Fe2O3/Au。
For the catalysis electrode obtained using embodiment 2 as anode (working electrode), Pt is cathode to electrode, and reference electrode is silver-
Silver chloride electrode.Electrolyte: 25 DEG C of 1M KOH, test temperature carry out electricity hydrolysis test.Test results are shown in figure 3, E=
1.60VRHEWhen, the cobalt of decorated by nano-gold and iron oxide (Co, Cu)-Fe of copper codope prepared by embodiment 22O3/ Au is obtained
4.304mA/cm2Density of photocurrent, in 2.0VRHEPlace obtains maximum photoelectric current, that is, 178.4mA/cm2.Show the catalysis of preparation
Agent is applied to density of photocurrent with higher when electrolysis water process.Illustrate the catalysis electrode electricity with higher of embodiment preparation
Chemical property, can effectively catalytic electrolysis water reaction.
Embodiment 3
Use titanium net (1cm × 3cm) as conductive substrates, which is pre-processed.Successively use ethyl alcohol and ultrapure water
After carrying out 30min ultrasonic cleaning, it is put into 40 DEG C of dryings in air dry oven；
Precursor solution: making solvent with ethanol water, and (volume ratio of dehydrated alcohol and ultrapure water is 3:7) is contained
Iron chloride, the 0.1mol/L sodium nitrate of 0.01mol/L, it is 1 that concentrated hydrochloric acid, which adjusts pH value,；
Pretreated conductive substrates are placed in water heating kettle liner, precursor solution are added into water heating kettle liner, before making
It drives liquid solution and floods conductive substrates；
100 DEG C of heating 4h in baking oven will be put into after the completion of water heating kettle sealing；Water heating kettle is cooled to the furnace after the reaction was completed
Room temperature；Conductive substrates are taken out from water heating kettle, are placed on after ultrapure water cleans in air dry oven and are dried at 40 DEG C, obtain hydroxyl
Base iron oxide FeOOH；
FeOOH FeOOH is immersed in the aqueous solution of copper nitrate containing 0.01mol/L and 0.01mol/L cobalt nitrate,
Dipping 12 hours takes out and uses ultrapure water, dry at 40 DEG C, obtains the FeOOH (Co, Cu)-for mixing cobalt and copper
FeOOH；
FeOOH (Co, the Cu)-FeOOH for mixing cobalt and copper is placed on temperature programming in tube furnace, from room temperature with 5 DEG C/
The heating rate of min heats 2 hours after rising to 500 DEG C, and cooled to room temperature obtains the calcining iron oxide for mixing cobalt and copper
(Co,Cu)-Fe2O3；
Calcining iron oxide (Co, Cu)-Fe of cobalt and copper will be mixed2O3；It is immersed in the solution containing nanogold (1.94mmol/L)
In, dip time is 12 hours, sample ultrapure water then taken out, is calcined 30 minutes at 350 DEG C after natural drying,
350 DEG C of calcinings can be such that transient current increases, and obtain the cobalt of decorated by nano-gold and iron oxide (Co, Cu)-Fe of copper codope2O3/
Au。
For the catalysis electrode obtained using embodiment 3 as anode (working electrode), Pt is cathode to electrode, and reference electrode is silver-
Silver chloride electrode.Electrolyte: 28 DEG C of 1M KOH, test temperature carry out electricity hydrolysis test.Test results are shown in figure 6.Fig. 5 is
Comparative example when calcining iron oxide is as working electrode.
Wherein, anode transient photocurrents density are as follows:
Fe2O3: I=0.038mA/cm2
(Co,Cu)-Fe2O3: I=0.068mA/cm2
(Co,Cu)-Fe2O3/ Au:I=0.08mA/cm2
Show that the catalyst of preparation is applied to density of photocurrent with higher when electrolysis water process.Illustrate prepared by embodiment
Catalysis electrode chemical property with higher, can effectively catalytic electrolysis water reaction.
Embodiment 4
Use electro-conductive glass as conductive substrates, which is pre-processed.Successively carried out with acetone and ultrapure water
After 30min ultrasonic cleaning, it is put into 40 DEG C of dryings in air dry oven；
Precursor solution: making solvent with propanol solution, the iron chloride containing 0.4mol/L, 0.4mol/L Titanium Nitrate, dense salt
Acid for adjusting pH value is 1；
Pretreated conductive substrates are placed in water heating kettle liner, precursor solution are added into water heating kettle liner, before making
It drives liquid solution and floods conductive substrates；
120 DEG C of heating 1h in baking oven will be put into after the completion of water heating kettle sealing；Water heating kettle is cooled to the furnace after the reaction was completed
Room temperature；Conductive substrates are taken out from water heating kettle, are placed on after ultrapure water cleans in air dry oven and are dried at 40 DEG C, are mixed
The FeOOH (Ti-FeOOH) of titanium；
Doped titanium FeOOH (Ti-FeOOH) is immersed in the aqueous solution of the tin of nitric acid containing 0.4mol/L, dipping 12 is small
When, it takes out and uses ultrapure water, it is dry at 40 DEG C, obtain FeOOH (Sn, the Ti)-FeOOH for mixing tin and titanium；
FeOOH (Sn, the Ti)-FeOOH for mixing tin and titanium is placed on temperature programming in tube furnace, from room temperature with 2 DEG C/
The heating rate of min heats 1 hour after rising to 800 DEG C, cooled to room temperature, obtain tin and titanium calcining iron oxide (Sn,
Ti)-Fe2O3；
Calcining iron oxide (Sn, Ti)-Fe of tin and titanium will be mixed2O3；It is immersed in the solution containing nanogold (1.1mmol/L),
Dip time is 12 hours, then takes out sample ultrapure water, obtains the tin of decorated by nano-gold and the calcining iron oxide of titanium
(Sn,Ti)-Fe2O3/Au。
Embodiment 5
Use electro-conductive glass as conductive substrates, which is pre-processed.Successively carried out with ethyl alcohol and ultrapure water
After 30min ultrasonic cleaning, it is put into 60 DEG C of dryings in air dry oven；
Precursor solution: making solvent with propanol solution, the iron chloride containing 0.01mol/L, 0.001mol/L copper nitrate, dense
Sulphur acid for adjusting pH value is 1；
Pretreated conductive substrates are placed in water heating kettle liner, precursor solution are added into water heating kettle liner, before making
It drives liquid solution and floods conductive substrates；
120 DEG C of heating 1h in baking oven will be put into after the completion of water heating kettle sealing；Water heating kettle is cooled to the furnace after the reaction was completed
Room temperature；Conductive substrates are taken out from water heating kettle, are placed on after ultrapure water cleans in air dry oven and are dried at 40 DEG C, are mixed
The FeOOH (Cu-FeOOH) of copper；
The FeOOH (Cu-FeOOH) for mixing copper is placed on temperature programming in tube furnace, from room temperature with the liter of 10 DEG C/min
Warm rate heats 1 hour after rising to 800 DEG C, and cooled to room temperature obtains the calcining iron oxide Cu-Fe for mixing copper2O3；
The calcining iron oxide Cu-Fe of copper will be mixed2O3；It is immersed in the solution containing nanogold (1.36mmol/L), dip time
It is 10 hours, then takes out sample ultrapure water, obtains the calcining iron oxide Cu-Fe of the Copper-cladding Aluminum Bar of decorated by nano-gold2O3/
Au。
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or the terminal device that include a series of elements not only include those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or end
The intrinsic element of end equipment.In the absence of more restrictions, being limited by sentence " including ... " or " including ... "
Element, it is not excluded that there is also other elements in process, method, article or the terminal device for including the element.This
Outside, herein, " being greater than ", " being less than ", " being more than " etc. are interpreted as not including this number；" more than ", " following ", " within " etc. understand
Being includes this number.
It should be noted that being not intended to limit although the various embodiments described above have been described herein
Scope of patent protection of the invention.Therefore, it based on innovative idea of the invention, change that embodiment described herein is carried out and is repaired
Change, or using equivalent structure or equivalent flow shift made by description of the invention and accompanying drawing content, it directly or indirectly will be with
Upper technical solution is used in other related technical areas, is included within scope of patent protection of the invention.
Claims (10)
1. a kind of preparation method of nanogold codope iron oxide composite catalyzing electrode, which comprises the following steps:
First metal-calcining iron oxide-conductive substrates compound is impregnated with the solution containing nanogold, it is total to obtain nanogold
Doped ferric oxide composite catalyzing electrode；
The solution containing nanogold is prepared using reduction of sodium citrate method,
First metal is selected from one or more of cobalt, titanium, tin, copper.
2. preparation method according to claim 1, which is characterized in that the concentration of the nano-Au solution is 0.97-
1.94mmol/L, dip time 10-15h.
3. preparation method according to claim 1, which is characterized in that the first metal-calcining iron oxide-conductive substrates
The preparation of compound the following steps are included:
Pretreatment: first conductive substrates are successively cleaned by ultrasonic with organic solvent and ultrapure water, the organic solvent be ethyl alcohol,
Acetone or its mixed liquor；
Hydro-thermal: pretreated conductive substrates being put into after precursor solution and carry out hydro-thermal reaction, the temperature of the hydro-thermal reaction
It is 80-120 DEG C, time 1-12h；Contain the Fe of 0.001-0.4mol/L in the precursor solution3+Ion；
Calcining: conductive substrates cooled to room temperature after being cleaned with ultrapure water, is forged by room temperature to 500-800 DEG C
Burn 1-4h, cooled to room temperature；
First is metal-doped:
Before calcination, conductive substrates are impregnated in the dipping solution of the first metal ion containing 0.001-0.4mol/L；
With or
After firing, conductive substrates are impregnated in the dipping solution of the first metal ion containing 0.001-0.4mol/L.
4. preparation method according to claim 3, which is characterized in that the precursor solution also contains 0.001-
The first metal ion of 0.4mol/L.
5. preparation method according to claim 3 or 4, which is characterized in that in the calcining step, heating rate be 2~
10℃/min。
6. preparation method according to claim 3 or 4, which is characterized in that in the calcining step, gas that when calcining uses
Atmosphere include air and or nitrogen.
7. -6 any preparation method according to claim 1, which is characterized in that the conductive substrates include titanium, conductive glass
Glass and foamed material.
8. a kind of nanogold codope iron oxide composite catalyzing electrode, which is characterized in that the catalysis electrode is by claim 1-7
Any preparation method preparation.
9. catalysis electrode according to claim 7, which is characterized in that the catalysis electrode is used for electrolysis water.
10. a kind of electrolysis wetting system, which is characterized in that the electrolysis wetting system is using any catalysis of claim 8-9
Electrode is anode.
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