CN106238081A - Preparation has the WO of high activity photoelectrocatalysis decomposition water performance3the method of nanometer thorn/CoPi complex light anode - Google Patents
Preparation has the WO of high activity photoelectrocatalysis decomposition water performance3the method of nanometer thorn/CoPi complex light anode Download PDFInfo
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- CN106238081A CN106238081A CN201511004800.1A CN201511004800A CN106238081A CN 106238081 A CN106238081 A CN 106238081A CN 201511004800 A CN201511004800 A CN 201511004800A CN 106238081 A CN106238081 A CN 106238081A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000000694 effects Effects 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 17
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- 229910003893 H2WO4 Inorganic materials 0.000 claims description 12
- 238000004062 sedimentation Methods 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 230000004044 response Effects 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 7
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 6
- 239000007836 KH2PO4 Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 22
- 239000003054 catalyst Substances 0.000 abstract description 13
- 239000010941 cobalt Substances 0.000 abstract description 9
- 229910017052 cobalt Inorganic materials 0.000 abstract description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 9
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000007423 decrease Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 150000004972 metal peroxides Chemical class 0.000 abstract description 2
- 238000007539 photo-oxidation reaction Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 238000000627 alternating current impedance spectroscopy Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 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
- 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
- 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
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
Preparation has the WO of high activity photoelectrocatalysis decomposition water performance3The method of nanometer thorn/CoPi complex light anode, its its preparation method is: (1) WO3Nanosized seeds synthesizes；(2) WO is prepared3Nanometer is stung；(3) WO is prepared3Nanometer thorn/CoPi complex light anode.Advantage: (1) uses semi-conducting material and cobalt-based to produce VPO catalysts and is combined, and improves the photoelectric catalytically active of semi-conducting material, reduces the overpotential of photooxidation reaction, save energy consumption；(2) WO3Semi-conducting material, by producing the compound of VPO catalysts with cobalt-based, decreases the photoetch reaction of semi-conducting material, and the formation and the semiconductor oxide that eliminate surface metal peroxide are dissolved, and effectively protects the photochemical catalyzing activity of light anode.
Description
Technical field
The present invention is open based on WO3The highly active photoelectrocatalysis for preparing of nanometer thorn/CoPi complex light anode decomposes
The method of aqueous energy, is particularly well-suited to photoelectrocatalysis decomposition water and converts the solar into the method that chemical energy stores.
Background technology
The excessive exploitation of chemical energy source and application, not only make non-renewable energy resources the most exhausted, also bring serious ring
Border problem and social problem.Under this background, the demand finding green alternative energy source is more and more urgent.Photochemical catalyzing is
The focus of field of solar energy utilization, can convert solar energy into chemical energy.Within 1972, first Fujishima and Honda find
TiO2Under ultraviolet light irradiates, photoelectrocatalysis decomposition water produces O2, open solar energy and be converted into the new approaches of chemical energy, recognized
For being that photocatalysis converts at solar energy and utilizes the ground-breaking achievement in research of aspect, become from this photochemical catalyzing and receive much attention
Research direction.In many semi-conducting materials, WO3Energy gap be 2.7eV, energy gap is less, it is possible to part inhale
Receiving visible ray, oxidation reaction driving force is relatively big, enjoys researcher to favor.But from the point of view of the effect utilizing sunlight, there is also
Some defects: one is that its light absorption wavelength is limited in scope, and can only partly utilize visible ray；Two is the recombination rate of semiconductor carriers
Higher, quantum efficiency is low.Therefore to WO3The study on the modification of photocatalyst is also always one of focus of photocatalysis research.At present
The modification technology of quasiconductor is had following two aspect:
(1), design has visible light-responded photocatalyst.In solar spectrum, ultraviolet light only accounts for the 4% of sunlight, it is seen that light accounts for
The 43% of sunlight, major part quasiconductor energy gap is relatively big, can only absorb ultraviolet light, the utilization rate of solar energy to be improved, design
Having visible light-responded semiconductor light-catalyst is to improve one of effective way utilizing solar energy.Concrete means include:
Metal cation doping, nonmetal doping, variable valency metal element compound sensitization.
(2) the efficiently separating of photocarrier.In light-catalyzed reaction, light induced electron and photohole life-span are shorter, big portion
Occurring compound after light splitting carrier produces and in inside, part photocarrier transits to catalyst surface and comes in contact, the fewest
The photocarrier of number comes in contact with external agency, and redox reaction occurs, it is therefore necessary to eliminate answering of photocarrier as far as possible
Close, photocatalysis efficiency could be improved.Concrete means include: supported co-catalyst, semi-conducting material are compound, nanostructured material
Material, heterojunction structure material.
Additionally, Nocera Daniel G. etc. report a kind of cobalt-based phosphate catalyst on the Science of 2008,
This catalyst can produce oxygen with relatively low overpotential electrochemical decomposition water in neutral conditions.CoPi catalyst can
With the realization " self-regeneration " of appraising at the current rate of cobalt, and utilize Co4+Drive the oxidation of water, it is achieved thereby that the recycling of catalyst.Permitted
Many reports show, CoPi is deposited on ZnO, Fe2O3、BiVO4Surface formation complex light anode Deng semi-conducting material, it is possible to press down
Being combined of semi-conducting material photocarrier processed, thus significantly improve its photoelectrocatalysis decomposition water and form the performance of oxygen, but civilian
Offer report
Semi-conducting material be layer structure, limited with CoPi contact area, layer structure also limit itself and electrolyte solution
Exposure level, the utilization to light is the most insufficient simultaneously.Therefore, by CoPi and WO3Photocatalyst is compound must solve above all
Many shortcomings could improve conductor photocatalysis decomposition water activity.
Summary of the invention
It is an object of the invention to avoid the weak point in above-mentioned background technology and provide one to prepare and there is high activity
The WO of photoelectrocatalysis decomposition water performance3The method of nanometer thorn/CoPi complex light anode.
Preparation method of the present invention is:
(1) WO3Nanosized seeds synthesizes, by H2WO4Powder and polyvinyl alcohol are dissolved in 30%H2O2In solution, mixed solution
It is transferred in water heating kettle, FTO electro-conductive glass base conductive is faced down and hangs by the feet in this solution, under 240-2-60 DEG C of hot conditions
React 0.8-1.2 hour, obtained WO3Nanosized seeds electrode；
(2) WO is prepared3Nanometer is stung: by WO3Nanosized seeds electrode is hung by the feet in H2WO4Solution, oxalic acid, H2O, HCl and acetonitrile
Mixed solution in, under 170-190 ° of C hot conditions react 1.5-2.5 hour, obtained the WO with space structure3Receive
Rice thorn, carrys out controllable growth WO by concentration of composition each in solution and the change in response time3Nanometer is stung；
(3) WO is prepared3Nanometer thorn/CoPi complex light anode: be electrochemically-deposited on electrochemical workstation and carry out, use routine
Three-electrode system, WO3Nanometer thorn electrode is working electrode, and saturated calomel electrode (SCE) is reference electrode, and Pt sheet is as to electricity
Pole, with CoCl2And KH2PO4Mixed solution be electrolyte, electrolyte pH6.8-7.2, sedimentation potential is 9-1.1 V, during deposition
Between be 1700-1900 s, obtained the WO with heterojunction structure3Nanometer thorn/CoPi complex light anode.
Concrete preparation method is:
(1) WO3Nanosized seeds synthesizes, and weighs 0. 3-0.4g H2WO4Powder and 0.1-0.5g polyvinyl alcohol are dissolved in 8-
12mL 30%H2O2In solution, mixed solution is transferred in water heating kettle, is faced down by FTO electro-conductive glass base conductive and hangs by the feet in this
In solution, react 0.8-1.2 hour under 240-2-60 DEG C of hot conditions, obtained WO3Nanosized seeds electrode；
(2) WO is prepared3Nanometer is stung: by WO3Nanosized seeds electrode hang by the feet in 2-4 mL concentration be 0.03-0.07 M H2WO4Molten
Liquid, 0.01-0.03 g oxalic acid, 7-8 mL H2O, 0.4-0.6 mL concentration is 5-7M HCl and 2-3 mL acetonitrile
In mixed solution, react 1.5-2.5 hour under 170-190 ° of C hot conditions, obtained the WO with space structure3Nanometer
Thorn, carrys out controllable growth WO by concentration of composition each in solution and the change in response time3Nanometer is stung；
(3) WO is prepared3Nanometer thorn/CoPi complex light anode: be electrochemically-deposited on CHI750c electrochemical workstation and carry out, make
With conventional three-electrode system, WO3Nanometer thorn electrode is working electrode, and saturated calomel electrode (SCE) is reference electrode, and Pt sheet is made
For to electrode, with 0.4-0.6 mmol L-1CoCl2With 0.08-0.12 mol L-1 KH2PO4Mixed solution for electrolysis
Matter, electrolyte pH6.8-7.2, sedimentation potential is 9-1.1 V, and sedimentation time is 1700-1900 s, has obtained having hetero-junctions knot
The WO of structure3Nanometer thorn/CoPi complex light anode.
Optimum concrete preparation method is:
(1) WO3Nanosized seeds synthesizes, and weighs 0.3125g H2WO4Powder and 0.125g polyvinyl alcohol are dissolved in 10mL
30%H2O2In solution, mixed solution is transferred in water heating kettle, is faced down by FTO electro-conductive glass base conductive and hangs by the feet in this solution
In, react 1. hours under 250 DEG C of hot conditionss, obtained WO3Nanosized seeds electrode；
(2) WO is prepared3Nanometer is stung: by WO3Nanosized seeds electrode hang by the feet in 3 mL concentration be 0.05 M H2WO4Solution,
0.02 g oxalic acid, 7.5 mL H2O, 0.5 mL concentration is in the mixed solution of 6M HCl and 2.5 mL acetonitriles, 180
React 2 hours under ° C hot conditions, obtained the WO with space structure3Nanometer is stung, by the concentration of composition each in solution
Change with the response time carrys out controllable growth WO3Nanometer is stung；
(3) WO is prepared3Nanometer thorn/CoPi complex light anode: be electrochemically-deposited on CHI750c electrochemical workstation and carry out, make
With conventional three-electrode system, WO3Nanometer thorn electrode is working electrode, and saturated calomel electrode (SCE) is reference electrode, and Pt sheet is made
For to electrode, with 0.5 mmol L-1CoCl2With 0.1 mol L-1 KH2PO4Mixed solution be electrolyte, electrolyte
PH6.8-7.2, sedimentation potential is 1.0 V, and sedimentation time is 1800 s, has obtained the WO with heterojunction structure3Nanometer thorn/
CoPi complex light anode.
The present invention has the advantage that than background technology
(1) use semi-conducting material and cobalt-based to produce VPO catalysts to be combined, improve the photoelectric catalytically active of semi-conducting material, reduce
The overpotential of photooxidation reaction, saves energy consumption；
(2) WO3Semi-conducting material, by producing the compound of VPO catalysts with cobalt-based, decreases the photoetch reaction of semi-conducting material,
The formation and the semiconductor oxide that eliminate surface metal peroxide are dissolved, and effectively protect the photochemical catalyzing of light anode
Activity；
(3) WO3Semi-conducting material and cobalt-based produce and define heterojunction structure between VPO catalysts, and the two is anti-to photochemical catalyzing
Should have a synergism, cobalt-based produces VPO catalysts and is effectively utilized the photohole that semiconductor optical anode produces, it is to avoid current-carrying
Being combined of son, improves the utilization rate of photocarrier；
(4) semi-conducting material being prepared as have space-filling model, electrochemical deposition CoPi can fully and semi-conducting material
In conjunction with, beneficially the carrying out of electrochemical-deposition step；
(5) WO of space structure3Nanometer thorn/CoPi complex light anode can be fully contacted electrolyte solution, beneficially photocatalysis
Effectively carrying out of decomposition water reaction；
(6) WO of space structure3Nanometer thorn/CoPi complex light anode makes incident illumination reflect at semiconductor material surface,
Can farthest absorb incident illumination；
Prove through Optical Electro-Chemistry test experiments, WO3Nanometer thorn photoanode surface deposited catalytic decomposition water and prepares the cobalt of oxygen
Based phosphates catalyst, significantly improves photoelectrocatalysis decomposition water and prepares the efficiency of oxygen.The electric current obtained with cyclic voltammetry
Compare as a example by density, under the given current potential of 1.2V, WO3Electric current under nanometer thorn/CoPi complex light anode illumination condition is close
Degree is 4.3 mA cm-2, it is 2 times of electric current density under dark condition；Under identical potential condition, WO3Nanometer thorn/CoPi is combined
Electric current density under light anode illumination condition is for having reached WO3Nanometer thorn light anode under illumination condition nearly 3 times of electric current density.
Detailed description of the invention
The concrete technology step of the present invention is:
1, FTO electro-conductive glass is respectively at 0.5 mol.L-1Ultrasonic cleaning 10 min and 15 min in KOH and acetone, and with high-purity
N2Dry up standby；
2,1.25g H is weighed2WO4Powder is mixed in 30mL H2In O, add 10mL 30%H2O2Solution, stirs under the conditions of 95 DEG C
Reacting 1 hour, the completely rear constant volume of question response, in the volumetric flask of 100mL, has obtained 0.05 M H2WO4Precursor solution；
3,0.3125g H is weighed2WO4Powder and 0.125g polyvinyl alcohol are dissolved in 10mL 30%H2O2In solution, mixing
Solution is transferred in water heating kettle, is faced down by above-mentioned clean FTO electro-conductive glass base conductive and hangs by the feet in this solution, 250 DEG C
React 2 hours under hot conditions, take out reactor after question response and naturally cool to room temperature, take out the FTO conduction wherein hung by the feet
Substrate of glass, rinses with high purity water, obtains WO3Nanosized seeds electrode；
4, by WO obtained above3Nanosized seeds electrode hang by the feet in 3 mL concentration be 0.05 M H2WO4Solution, 0.02 g grass
Acid, 7.5 mL H2O, 0.5 mL concentration is in the mixed solution of 6M HCl and 2.5 mL acetonitriles, 180 ° of C high temperature bars
React 2 hours under part, take out reactor after question response and naturally cool to room temperature, take out the FTO electro-conductive glass wherein hung by the feet
Substrate, rinses with high purity water, has obtained the WO with space structure3Nanometer thorn electrode；
5, electrochemical deposition CoPi is in the WO of above-mentioned preparation3On nanometer thorn electrode, this step is on CHI750c electrochemical workstation
Carry out, use the three-electrode system of routine, WO3Nanometer thorn electrode is working electrode, and saturated calomel electrode (SCE) is reference electricity
Pole, Pt sheet is as to electrode, with 0.5 mmol L-1CoCl2With 0.1 mol L-1 KH2PO4Mixed solution (pH ≈ 7)
For electrolyte, sedimentation potential is 1.0 V, and sedimentation time is 1800 s, has obtained the WO with heterojunction structure3Nanometer thorn/
CoPi complex light anode, cleans with high purity water, and sealing is kept in Dark Place；
6, utilization has prepared WO3Nanometer thorn/CoPi complex light anode, carries out photoelectrocatalysis decomposition water performance test, specifically
Means of testing includes cyclic voltammetry curve, photocurrent response, transient current, ac impedance spectroscopy etc., and wherein cyclic voltammetry is swept
Retouching speed is 50 mV.s-1, and photocurrent response is divided into 5 opening and closing light cycle to test under given current potential is 1.0 V,
The test frequency of ac impedance spectroscopy is 10000-0.01 Hz, and given current potential is 1.0 V.
It is as follows that described high activity light anode prepares committed step:
First, FTO electro-conductive glass conducting surface is hung by the feet in solution, and particle grows naturally；
Second, WO3The preparation of nanometer thorn electrode is to realize controllable growth by change reactant concentration and reaction temperature；
3rd, CoPi are deposited on WO3On nanometer thorn electrode, use the sedimentation potential being suitable for.
Claims (2)
1. preparation has the WO of high activity photoelectrocatalysis decomposition water performance3The method of nanometer thorn/CoPi complex light anode, its feature
It is that its preparation method is:
(1) WO3Nanosized seeds synthesizes, by H2WO4Powder and polyvinyl alcohol are dissolved in 30%H2O2In solution, mixed solution turns
Move in water heating kettle, FTO electro-conductive glass base conductive is faced down and hangs by the feet in this solution, anti-under 240-2-60 DEG C of hot conditions
Answer 0.8-1.2 hour, obtained WO3Nanosized seeds electrode；
(2) WO is prepared3Nanometer is stung: by WO3Nanosized seeds electrode is hung by the feet in H2WO4Solution, oxalic acid, H2O, HCl and acetonitrile
Mixed solution in, under 170-190 ° of C hot conditions react 1.5-2.5 hour, obtained the WO with space structure3Receive
Rice thorn, carrys out controllable growth WO by concentration of composition each in solution and the change in response time3Nanometer is stung；
(3) WO is prepared3Nanometer thorn/CoPi complex light anode: be electrochemically-deposited on electrochemical workstation and carry out, uses routine
Three-electrode system, WO3Nanometer thorn electrode is working electrode, and saturated calomel electrode (SCE) is reference electrode, and Pt sheet is as to electricity
Pole, with CoCl2And KH2PO4Mixed solution be electrolyte, electrolyte pH6.8-7.2, sedimentation potential is 9-1.1 V, during deposition
Between be 1700-1900 s, obtained the WO with heterojunction structure3Nanometer thorn/CoPi complex light anode.
Preparation the most according to claim 1 has the WO of high activity photoelectrocatalysis decomposition water performance3Nanometer thorn/CoPi is combined
The method of light anode, it is characterised in that its preparation method is:
(1) WO3Nanosized seeds synthesizes, and weighs 0.3125g H2WO4Powder and 0.125g polyvinyl alcohol are dissolved in 10mL
30%H2O2In solution, mixed solution is transferred in water heating kettle, is faced down by FTO electro-conductive glass base conductive and hangs by the feet in this solution
In, react 1. hours under 250 DEG C of hot conditionss, obtained WO3Nanosized seeds electrode；
(2) WO is prepared3Nanometer is stung: by WO3Nanosized seeds electrode hang by the feet in 3 mL concentration be 0.05 M H2WO4Solution, 0.02
G oxalic acid, 7.5 mL H2O, 0.5 mL concentration is in the mixed solution of 6M HCl and 2.5 mL acetonitriles, 180 ° of C height
React 2 hours under the conditions of temperature, obtained the WO with space structure3Nanometer is stung, by the concentration of composition each in solution with anti-
Change between Ying Shi carrys out controllable growth WO3Nanometer is stung；
(3) WO is prepared3Nanometer thorn/CoPi complex light anode: be electrochemically-deposited on CHI750c electrochemical workstation and carry out, make
With conventional three-electrode system, WO3Nanometer thorn electrode is working electrode, and saturated calomel electrode (SCE) is reference electrode, and Pt sheet is made
For to electrode, with 0.5 mmol L-1CoCl2With 0.1 mol L-1 KH2PO4Mixed solution be electrolyte, electrolyte
PH6.8-7.2, sedimentation potential is 1.0 V, and sedimentation time is 1800 s, has obtained the WO with heterojunction structure3Nanometer thorn/
CoPi complex light anode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511004800.1A CN106238081A (en) | 2015-12-29 | 2015-12-29 | Preparation has the WO of high activity photoelectrocatalysis decomposition water performance3the method of nanometer thorn/CoPi complex light anode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511004800.1A CN106238081A (en) | 2015-12-29 | 2015-12-29 | Preparation has the WO of high activity photoelectrocatalysis decomposition water performance3the method of nanometer thorn/CoPi complex light anode |
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| Publication Number | Publication Date |
|---|---|
| CN106238081A true CN106238081A (en) | 2016-12-21 |
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| CN201511004800.1A Pending CN106238081A (en) | 2015-12-29 | 2015-12-29 | Preparation has the WO of high activity photoelectrocatalysis decomposition water performance3the method of nanometer thorn/CoPi complex light anode |
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