CN107012480A - Polyacid and the eight co-modified Nano tube array of titanium dioxide optical electro-chemistry of nine cobalts of vulcanization analyse the preparation method of oxygen electrode - Google Patents
Polyacid and the eight co-modified Nano tube array of titanium dioxide optical electro-chemistry of nine cobalts of vulcanization analyse the preparation method of oxygen electrode Download PDFInfo
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- CN107012480A CN107012480A CN201710190524.5A CN201710190524A CN107012480A CN 107012480 A CN107012480 A CN 107012480A CN 201710190524 A CN201710190524 A CN 201710190524A CN 107012480 A CN107012480 A CN 107012480A
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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
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract
The present invention provides a kind of preparation method for the Nano tube array of titanium dioxide optical electro-chemistry analysis oxygen electrode that polyacid and eight nine cobalts of vulcanization are modified jointly.The Nano tube array of titanium dioxide composite film photo-anode that preparation-obtained polyacid and eight nine cobalts of vulcanization are modified jointly can be used for optical electro-chemistry to decompose elutriation oxygen.The composite film photo-anode is that the formed titanium dioxide eight of modification vulcanizes nine cobalt polyacid composite film photo-anodes jointly based on Nano tube array of titanium dioxide, and with eight nine cobalts of vulcanization and a kind of Keggin-type phosphotungstic acid.Under the irradiation of room temperature environment and xenon lamp, the composite film photo-anode has good optical electro-chemistry decomposition water performance.It is simple that the titanium dioxide eight that the present invention is provided vulcanizes nine cobalt polyacid compound film electrode preparation methods; cost is very low; need not sacrifice reagent, protective layer and cushioning liquid can efficient stable photoelectric decomposition water; realize that the high efficiency of luminous energy to chemical energy is changed, it is adaptable to the exploitation and production of novel photoelectric chemical breakdown elutriation oxygen electrode.
Description
Technical field
The invention belongs to PhotoelectrochemicalTechnique Technique field, it is related to the titanium dioxide that a kind of polyacid and eight vulcanization nine cobalts collaborations promote
Nano-tube array optical electro-chemistry decomposes the preparation method of elutriation oxygen electrode.
Background technology
Be made the energy that hydrogen and oxygen can be used as the mankind by decomposition water, and using solar energy and electric energy come
Obtain the solution route that these energy are an ideal and environmental protection.From thermodynamics and kineticses angle analysis, direct light decomposition water
There is larger obstruction so that this process is difficult to realize in practice, and the emphasis captured as numerous scientific research personnel.Electrochemistry
The dynamics that the introducing of catalyst or photochemical catalyst can substantially reduce light decomposition water hinders.Titanium dioxide (TiO2) it is a kind of
Important conductor photocatalysis material, can be prepared into having the nano material of different-shape, wherein nano titania
Pipe array due to regular, directional profile, possess larger ratio surface thus with preferable electron transport ability and electronics-
Hole separating capacity, photoelectrocatalysis decomposition water oxygen can be effectively carried out as light anode.But titanium dioxide is under light illumination, light
Raw electron transition is to after conduction band, and electronics and hole are easily combined, so as to influence the transmission of electronics, cause optical electro-chemistry decomposition water energy
Power weakens.If by introducing other compounds and titanium dioxide formation nano composite material, and then improving electrode photoelectric chemistry
Decomposition water performance, it will promote application of the titanic oxide material in optical electro-chemistry decomposition water.
In recent years, many seminars were directed to the non-noble of exploitation is made up of earth's crust high abundance element high catalytic activity
Metal elctro-catalyst, some of transient metal chalcogenide compounds, including Mo bases or Co base amorphous sulphur compounds also show compared with
The property of good electrocatalytic decomposition water.Eight nine cobalt (Co of vulcanization9S8) as one of them, with outstanding electro catalytic activity.Cause
This, is supported on Nano tube array of titanium dioxide, helps to reduce the compound of light induced electron and hole, and then lift photoelectricity
The performance of chemical breakdown water.
Polyoxometallate (i.e. polyacid, Polyoxometalates, POMs) is a class polynuclear complex, there is nearly two so far
Century-old developing history, it has also become the important research direction in inorganic chemistry.Polyoxometallate (abbreviation polyacid) is that a class is good
Good electron acceptor, can suppress the compound of photo-generated carrier by capturing the light induced electron of semiconductor conduction band and promote light
The migration of raw carrier, is conducive to electron transmission.
Therefore, eight nine cobalts of vulcanization and polyacid are collectively incorporated into titania nanotube material by we, form semiconductor
Photoelectric nano-composite material, so as to significantly improve titanium dioxide electrodes optical electro-chemistry decomposition water performance.
The content of the invention
It is an object of the invention to provide a kind of composite film photo-anode, it need not sacrifice reagent, protective layer and cushioning liquid i.e.
Can efficient stable photoelectric decomposition water, realize luminous energy to the conversion of chemical energy, and the electrode has and prepares simple, efficiency high, again
Renaturation is good, it is cheap the advantages of.
The vulcanization of titanium dioxide-eight nine cobalts-polyacid composite film photo-anode that the present invention is provided can be prepared via a method which：
(1) preparation of film of Nano tube array of titanium dioxide light anode：
Titanium foil is cut into the rectangle that size is 25 × 15mm first, successively with detergent, distilled water flushing, then used respectively
After acetone, ethanol solution ultrasonic wave are cleaned 10 minutes, as anode after drying, negative electrode is made with platinized platinum, two electrodes are apart
2.5cm, is immersed in the ethylene glycol electrolyte of the ammonium fluoride containing 1.0wt%, and constant temperature is at 25 DEG C, in 60V voltage anodic oxygens
Change after 90min, take out titanium foil and rinsed well with deionized water, dried up, with 5 DEG C of min in Muffle furnace-1It is warming up at 400 DEG C
Calcining at constant temperature 2h, naturally cools to room temperature, you can obtain film of Nano tube array of titanium dioxide electrode.
(2) titanium dioxide-eight vulcanizes the preparation of nine cobalt composite film photo-anodes：
5mmol cobalt acetate and 5mmol thiocarbamides are added in 30mL ethylene glycol, magnetic agitation loads 40mL to clarifying
Ptfe autoclave in.Then, the titanium dioxide membrane electrode previously prepared is fitted into reactor, is placed in baking oven, it is permanent
200 DEG C of reaction 8h of temperature.Naturally cool to after room temperature, obtained electrode is respectively washed 3 times, 60 DEG C with deionized water, absolute ethyl alcohol
Lower dry 3h, you can obtain titanium dioxide-eight and vulcanize nine cobalt compound film electrodes.
(3) titanium dioxide-eight vulcanizes the preparation of nine cobalts-polyacid composite film photo-anode：
The titanium dioxide-eight prepared is vulcanized into nine cobalt compound film electrodes and immerses many acid solutions of 1mmol and 3mmol tetra- respectively
1 minute in butylammonium bromide solution, while carrying out ultrasonic wave added.After each layer adsorbs, by membrane electrode deionized water rinsing,
And rush dry with nitrogen.Aforesaid operations are repeated until 10 circulations, you can obtain titanium dioxide-eight and vulcanize nine cobalts-polyacid composite membrane electricity
Pole.
The structure of the vulcanization of titanium dioxide-eight nine cobalts-polyacid compound film electrode is spread out by x-ray powder made from the above method
Penetrate measure (XRD is shown in accompanying drawing 2) and energy spectrum analysis figure (EDS is shown in accompanying drawing 3) is characterized.It can be found that in XRD spectra, institute
The material of preparation is consistent with titanium dioxide, the main peak position of eight nine cobalts of vulcanization and peak intensity, this demonstrate that using above-mentioned side
Material prepared by method contains titanium dioxide and eight nine cobalts of vulcanization.Because many acid contents are less, it can not be observed in XRD spectra
To the presence of polyacid, but polyacid is introduced, do not influence the crystal formation of titanium dioxide and eight nine cobalts of vulcanization.In x-ray photoelectron spectroscopy
In, it can substantially observe phosphorus, the characteristic peak of wolfram element, it was demonstrated that the presence of polyacid in material.Meanwhile, it is aobvious by scanning electron
Micro mirror image (see accompanying drawing 4) is it was determined that nano-tube array appearance and size is homogeneous made from the above method, and eight vulcanize nine cobalts and many
Acid is evenly distributed on nanotube surface.
The vulcanization nine cobalts-polyacid compound film electrode of titanium dioxide-eight the answering in optical electro-chemistry decomposition water that the present invention is provided
With its condition of work is as follows：
Experiment is carried out using three-electrode system in quartz beaker, and titanium dioxide-eight vulcanizes nine cobalts-polyacid composite membrane light sun
Extremely working electrode, platinum filament is as to electrode, and Ag/AgCl electrodes are used as reference electrode.Supporting electrolyte is metabisulfite solution.With
Xenon lamp is used as light source.When illumination, the light induced electron that titanium dioxide is produced can be delivered separately to the cobalt of eight vulcanization nine and polyacid, so that
Remaining more photoholes are by OH—Oxidation generation oxygen.
According to above-mentioned principle, with the continuous increase of voltage, the vulcanization nine cobalts-polyacid composite film photo-anode of titanium dioxide-eight
Surface has a certain amount of bubble to occur, it was demonstrated that have oxygen generation.
The vulcanization of titanium dioxide-eight nine cobalts-polyacid composite film photo-anode provided in the present invention has the characteristics that：
1st, the vulcanization of titanium dioxide-eight nine cobalts-polyacid composite film photo-anode main body is made up of Nano tube array of titanium dioxide, and eight
Vulcanize nine cobalts and polyacid is evenly distributed on titanic oxide material surface, the optical electro-chemistry decomposition water performance to titanium dioxide plays rush
Enter effect.
2nd, the vulcanization of titanium dioxide-eight nine cobalts-polyacid composite film photo-anode optical electro-chemistry decomposition water condition of work is gentle, in room
It can be reacted under temperature and reagent, protective layer and cushioning liquid need not be sacrificed.
3rd, the vulcanization of titanium dioxide-eight nine cobalts-polyacid composite film photo-anode can be stabilized in the solution, can be existed for a long time
Decomposition water under the conditions of photoelectricity.
Brief description of the drawings
Fig. 1 is the crystal structure of polyacid (Keggin-type phosphotungstic acid).
Fig. 2 is the X-ray powder diffraction figure that titanium dioxide-eight vulcanizes nine cobalts-polyacid composite film photo-anode.
Fig. 3 is the energy spectrum analysis figure that titanium dioxide-eight vulcanizes nine cobalts-polyacid composite film photo-anode.
Fig. 4 is the scanning electron microscope (SEM) photograph that titanium dioxide-eight vulcanizes nine cobalts-polyacid composite film photo-anode.
Fig. 5 is that the current-voltage of the vulcanization nine cobalts-polyacid composite film photo-anode optical electro-chemistry decomposition water of titanium dioxide-eight is bent
Line chart.
Embodiment
In order to further illustrate the present invention, following embodiment is enumerated, but it is not intended to limit each accessory claim and determined
The invention scope of justice.
Specific embodiment 1：
Experiment is carried out using three-electrode system in quartz beaker, and titanium dioxide photo anode and titanium dioxide-eight are vulcanized
Nine cobalts-polyacid composite film photo-anode is respectively as working electrode, and effective area is 1 × 1cm2, platinum filament is as to electrode, Ag/
AgCl electrodes are used as reference electrode.Supporting electrolyte is 0.5M metabisulfite solutions.Light source, irradiation intensity are used as with 300W xenon lamp
For 100mWcm-2.Voltage range is 0.2~1.6V (compared to standard hydrogen electrode).It will be evident that introducing eight sulphur from figure
Change after nine cobalts and polyacid, the composite film photo-anode photoelectric current is obviously improved (see accompanying drawing 5).
Claims (5)
1. a kind of titanium dioxide-eight vulcanizes nine cobalts-polyacid compound film electrode, it is characterised in that：Elutriation oxygen is decomposed to optical electro-chemistry
With good performance.
2. vulcanize nine cobalts-polyacid compound film electrode according to the titanium dioxide-eight described in claim 1, it is characterised in that：Titanium dioxide
The pattern of titanium is nano-tube array, and its chemical formula is TiO2；Eight nine cobalt patterns of vulcanization are nanometer sheet, and its chemical formula is Co9S8；It is many
Acid is Keggin-type phosphotungstic acid, and its chemical formula is H3[PW12O40]·nH2O。
3. vulcanize nine cobalts-polyacid compound film electrode according to the titanium dioxide-eight described in claim 1, it is characterised in that：Titanium dioxide
Titanium nano-tube array can be obtained titanium dioxide-eight using hydro-thermal method afterwards and vulcanized nine cobalt composite membranes using anodizing synthesis
Electrode, finally obtains the vulcanization nine cobalts-polyacid compound film electrode of titanium dioxide-eight using chemical bath deposition method.
4. vulcanize nine cobalts-polyacid compound film electrode according to the titanium dioxide-eight described in claim 1, it is characterised in that：Can be
Under conditions of room temperature and optical electro-chemistry, using independent Nano tube array of titanium dioxide as contrast, using the change of electrochemical signals come
Compare the performance that its optical electro-chemistry decomposes elutriation oxygen.
5. vulcanize nine cobalts-polyacid compound film electrode according to the titanium dioxide-eight described in claim 1, it is characterised in that：Main body is
Nano tube array of titanium dioxide structure, eight nine cobalts of vulcanization and polyacid are evenly distributed in Nano tube array of titanium dioxide surface.This
Plant material stably can be present on titanium foil in the form of a film, and its preparation method is simple, with low cost, and performance is stable, real
Mild condition is tested, reclaims complete.
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| CN201710190524.5A CN107012480B (en) | 2017-03-27 | 2017-03-27 | The preparation method of polyacid and the co-modified Nano tube array of titanium dioxide optical electro-chemistry analysis oxygen electrode of eight nine cobalts of vulcanization |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110023542A (en) * | 2017-01-26 | 2019-07-16 | 旭化成株式会社 | Bipolar electrolyzer, buck electrolysis bipolar electrolyzer and hydrogen manufacturing method |
| CN112403503A (en) * | 2020-11-27 | 2021-02-26 | 电子科技大学 | Preparation method of nitrogen-doped MOF structure modified two-phase sulfide material |
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2017
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110023542A (en) * | 2017-01-26 | 2019-07-16 | 旭化成株式会社 | Bipolar electrolyzer, buck electrolysis bipolar electrolyzer and hydrogen manufacturing method |
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| CN112403503A (en) * | 2020-11-27 | 2021-02-26 | 电子科技大学 | Preparation method of nitrogen-doped MOF structure modified two-phase sulfide material |
| CN112403503B (en) * | 2020-11-27 | 2021-08-03 | 电子科技大学 | Preparation method of nitrogen-doped MOF structure modified two-phase sulfide material |
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