CN104577139A - Photo-responsive titania nanotube-supported catalyst electrode and preparation method thereof - Google Patents
Photo-responsive titania nanotube-supported catalyst electrode and preparation method thereof Download PDFInfo
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- CN104577139A CN104577139A CN201510029999.7A CN201510029999A CN104577139A CN 104577139 A CN104577139 A CN 104577139A CN 201510029999 A CN201510029999 A CN 201510029999A CN 104577139 A CN104577139 A CN 104577139A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8853—Electrodeposition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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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
- Y02E60/50—Fuel cells
Abstract
The invention relates to a photo-responsive titania nanotube-supported catalyst electrode and a preparation method thereof, and belongs to a catalytic electrode material and preparation thereof in a fuel cell. A titania nanotube is adopted as a catalyst carrier of at least one noble metal in platinum, palladium, gold and silver; a photo-responsive semiconductor electrode is obtained by graphene modification, so that, on one hand, a titania nanotube array has good acidic and basic stability and excellent photoelectric property, and on the other hand, the electrical conductivity and the visible light response performance of the semiconductor electrode are enhanced by modification on the titania nanotube by graphene. By the preparation method provided by the invention, the dispersity of the catalyst and the visible light response of the electrode can be improved by the catalyst electrode, so that the catalysis efficiency of the noble metal catalyst is improved.
Description
Technical field
Titania nanotube supported catalyst electrode that the present invention relates to a kind of photoresponse and preparation method thereof, belongs to catalytic electrode material and preparation thereof in fuel cell.
Background technology
Fuel cell particularly direct methanol fuel cell is directly converted to the technology of electric energy as a kind of fuel chemical energy, have high efficiency, low emission, the plurality of advantages such as pollution-free, caused the great attention of scientific and technological circle and industrial circle.In a fuel cell, platinum serves as anodised the most frequently used catalyst always.But noble metal platinum is expensive, and pure platinum is easily poisoned by carbon monoxide, therefore needs the consumption reducing platinum, improves platinum utilization and anti-poisoning ability, to reach the object of commercializing fuel cells.
Because above-mentioned defect, the design people, actively in addition research and innovation, to founding a kind of titania nanotube supported catalyst electrode of photoresponse of new structure, make it have more value in industry.
Summary of the invention
For solving the problems of the technologies described above, the object of this invention is to provide a kind of titania nanotube supported catalyst electrode of photoresponse, it has higher dispersiveness and structural stability, and can strengthen the conductivity of semi-conducting electrode and visible light-responded performance.
The titania nanotube supported catalyst electrode of photoresponse of the present invention, is made up of base material and catalyst layer, and described base material is metal titanium sheet and carrier titania nanotube; Catalyst layer above base material is made up of at least one in catalyst platinum, palladium, gold, silver noble metal and redox graphene.
Further, the pattern of the catalyst of described load on base material is nano flower-like.
Present invention also offers a kind of preparation method of titania nanotube supported catalyst electrode of photoresponse, comprise the steps:
S1: generate titania nanotube at base material titanium plate surface by anode oxidation method;
S2: catalyst electro-deposition, by least one electro-deposition in platinum, palladium, gold, silver noble metal at titania nanotube on the surface, prepares titania nanotube supported catalyst electrode;
S3: at electrode face finish one deck redox Graphene, forms the titania nanotube supported catalyst electrode of the photoresponse of graphene modified.
Further, specifically comprise the steps: at described step S1
S11: electrochemical solution is prepared
Ammonium fluoride is dissolved in the mixed solution of ethylene glycol and water, makes the electrochemical solution that ammonium fluoride mass fraction is 0.5%;
S12: prepare titania nanotube
Being inserted by the electrochemical solution prepared and being provided with titanium sheet be anode and platinized platinum is in the electrochemical reaction appts of negative electrode, adopt anode oxidation method, to power on chemical preparation titania nanotube in base material titanium sheet, calcine in Muffle furnace after then obtained titania nanotube deionized water rinsing being dried.
Further, in described step S12, the current potential 60V of the anode oxidation method adopted, controls reaction time 2h-2.5h.
Further, in described step S12, titania nanotube 450 DEG C of calcining 2h in Muffle furnace after described oven dry.
Further; be specially at described step S2: titanium dioxide nanotube electrode is inserted in the aqueous solution of slaine of a kind of precious metal element at least had in platinum, palladium, gold, silver; under the protection of nitrogen; utilize potentiostatic method electro-deposition catalyst, prepare titania nanotube supported catalyst electrode.
Further, the concentration of aqueous solution of described slaine is 1-5mmol/L; The current potential of the potentiostatic method adopted is-0.2V, and reference electrode is saturated calomel electrode.
Further, specifically comprise the steps: at described step S3
S31: graphene oxide solution be slowly added drop-wise to titania nanotube supported catalyst electrode surface and dry;
S32: the titania nanotube supported catalyst electrode being coated with graphene oxide is inserted in PBS solution, with potentiostatic method, control the electrochemical reaction time at 1500s, electrochemical reduction oxidation Graphene, thus the titania nanotube supported catalyst electrode of obtained photoresponse.
Further, the current potential of the potentiostatic method adopted is-0.9V, and reference electrode is saturated calomel electrode.
By such scheme, the present invention at least has the following advantages: the present invention adopts titania nanotube as the catalyst carrier of at least one noble metal in platinum, palladium, gold, silver, and the semi-conducting electrode of photoelectric respone is obtained with graphene modified, thus make Nano tube array of titanium dioxide have good ph stability and excellent photoelectric properties, on the other hand, Graphene, to the modification of titania nanotube, enhances the conductivity of semi-conducting electrode and visible light-responded performance.The preparation method of the application of the invention, this catalyst electrode can improve the dispersiveness of catalyst and the response of electrode pair visible ray, thus improves the catalytic efficiency of noble metal catalyst.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of specification, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure of the titania nanotube Supported Pt Nanoparticles electrode of photoresponse.
Fig. 2 is the cyclic voltammogram of titania nanotube Supported Pt Nanoparticles electrode in 0.5mol/L potassium hydroxide solution of photoresponse;
Fig. 3 is the photoelectricity flow graph of titania nanotube Supported Pt Nanoparticles electrode in 1.0mol/L methyl alcohol+0.5mol/L potassium hydroxide solution of photoresponse under visible light conditions;
Fig. 4 is the cyclic voltammogram of titania nanotube Supported Pt Nanoparticles electrode in 1.0mol/L methyl alcohol+0.5mol/L potassium hydroxide solution of photoresponse under visible light conditions.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
The titania nanotube supported catalyst electrode of photoresponse of the present invention is made up of base material and catalyst layer, and described base material is metal titanium sheet and carrier titania nanotube; Catalyst layer above base material is made up of at least one in catalyst platinum, palladium, gold, silver noble metal and redox graphene.The pattern of the catalyst of described load on base material is nano flower-like.
Because titania nanotube is at the ordered arrangement of titanium plate surface, improve the transmission rate of photo-generated carrier, reduce the combined efficiency of photo-generate electron-hole, thus show excellent PhotoelectrocatalytiPerformance Performance, in addition, Nano tube array of titanium dioxide can prepare the combination electrode of photoelectric respone as precious metal catalyst agent carrier, can be applicable to photoelectrocatalysis organic molecule.And Graphene has a series of important photoelectric characteristics such as transparent, soft, conduction, electron mobility are high, so the hybrid being used for being formed after decorated nanometer titanium dioxide can strengthen the response of semiconductor at visible-range.
The preparation method of the titania nanotube supported catalyst electrode of above-mentioned photoresponse comprises step S1 to step S3.
S1: generate titania nanotube at base material titanium plate surface by anode oxidation method.This step specifically can comprise:
S11: electrochemical solution is prepared
Ammonium fluoride is dissolved in the mixed solution of ethylene glycol and water, makes the electrochemical solution that ammonium fluoride mass fraction is 0.5%;
S12: prepare titania nanotube
Being inserted by the electrochemical solution prepared and being provided with titanium sheet be anode and platinized platinum is in the electrochemical reaction appts of negative electrode, adopt anode oxidation method, current potential is 60V, control reaction time 2h-2.5h, to power on chemical preparation titania nanotube in base material titanium sheet, after then obtained titania nanotube being dried with deionized water rinsing in Muffle furnace 450 DEG C of calcining 2h.
S2: catalyst electro-deposition, by one or both Simultaneous Electrodepositions in platinum, palladium, gold, silver noble metal at titania nanotube on the surface, prepares titania nanotube supported catalyst electrode.This this step is specially: inserted by titanium dioxide nanotube electrode in the aqueous solution of slaine of a kind of precious metal element at least had in platinum, palladium, gold, silver; under the protection of nitrogen; utilize potentiostatic method electro-deposition catalyst; prepare titania nanotube supported catalyst electrode; wherein; the concentration of aqueous solution of described slaine is 1-5mmol/L, and the current potential of the potentiostatic method adopted is-0.2V, and reference electrode is saturated calomel electrode.In this step, the pattern of the catalyst of load on base material is nano flower-like.
S3: at electrode face finish one deck redox Graphene, forms the titania nanotube supported catalyst electrode of the photoresponse of graphene modified.This step can specifically comprise:
S31: graphene oxide solution be slowly added drop-wise to titania nanotube supported catalyst electrode surface and dry;
S32: the titania nanotube supported catalyst electrode being coated with graphene oxide is inserted in PBS solution, with potentiostatic method, (current potential is-0.9V, reference electrode is saturated calomel electrode), control the electrochemical reaction time at 1500s, electrochemical reduction oxidation Graphene, thus the titania nanotube supported catalyst electrode of obtained photoresponse.
Below by embodiment in detail the present invention is described in detail.
The preparation method of the titania nanotube load platinum catalyst electrode of photoresponse comprises the steps:
Step one: electrochemical solution is prepared
Ammonium fluoride is dissolved in the mixed solution of ethylene glycol and water (1.5V%), makes the electrochemical solution that ammonium fluoride mass fraction is 0.5%;
Step 2: prepare titania nanotube
Being inserted by the 30mL newly prepared ammonium fluoride/ethylene glycol solution and being provided with titanium sheet be anode and platinized platinum is in the electrochemical reaction appts of negative electrode, adopt anode oxidation method, the spacing of two electrodes is kept to be 1cm, controlling potential 60V, reaction time 2.5h, to power on chemical preparation Nano tube array of titanium dioxide in base material titanium sheet.The titania nanotube deionized water rinsing that obtains dry after in Muffle furnace 450 DEG C of calcining 2h;
Step 3: the electro-deposition of catalyst platinum
Titanium dioxide nanotube electrode is inserted containing in 3mmol/L chloroplatinic acid and 0.5mol/L sulphur aqueous acid; under the protection of nitrogen; utilize potentiostatic method (-0.2V; saturated calomel electrode) platinum electrodeposition nanotube; thus obtained titania nanotube supported platinum nano pipe electrode, wherein platinum catalyst carrying capacity is 0.5mg/cm
2.
Step 4: redox graphene is to the modification of catalyst surface
Graphene oxide solution (0.1mL, 1mg/mL) be slowly added drop-wise to the supporting platinum-based nanotube electrode surface of titania nanotube and dry.This electrode is inserted in Na-PBS cushioning liquid (1.0M, pH=4.2), with potentiostatic method (-0.9V, saturated calomel electrode) electrochemical reduction oxidation Graphene.
Respectively the titania nanotube Supported Pt Nanoparticles electrode of above-mentioned photoresponse and titania nanotube supported catalyst electrode are inserted in the potassium hydroxide solution of 0.5mol/L and 1.0mol/L methyl alcohol+0.5mol/L potassium hydroxide solution and scan, carry out the comparison of electrode performance.As can be seen from Figure 2, the effective area of the titania nanotube Supported Pt Nanoparticles electrode of photoresponse is obviously greater than the effective area of titania nanotube supported catalyst electrode.As can be seen from Figure 4, the titania nanotube Supported Pt Nanoparticles electrode of photoresponse in the basic conditions to the oxidation peak current of methyl alcohol and reduction peak current all larger, illustrate that the performance of this electrode is better than the electrode performance of titania nanotube supported catalyst electrode thus, as can be seen from Figure 3, under illumination condition, the electric current that the titania nanotube Supported Pt Nanoparticles electrode of photoresponse obtains obviously is greater than the electric current of titania nanotube supported catalyst electrode, illustrate that Graphene enhances the electric conductivity of electrode, the hybrid formed after graphene modified titanium dioxide can strengthen the electrochemical response of semiconductor in visible-range, in addition, prove further from Fig. 4, the electrode performance of the titania nanotube Supported Pt Nanoparticles electrode of photoresponse is optimum.
In sum, by adopting titania nanotube as the catalyst carrier of at least one noble metal in platinum, palladium, gold, silver, and the semi-conducting electrode of photoelectric respone is obtained with graphene modified, thus make Nano tube array of titanium dioxide have good ph stability and excellent photoelectric properties, the noble metal nano flower of load on its surface has higher dispersiveness and structural stability, on the other hand, Graphene, to the modification of titania nanotube, enhances the conductivity of semi-conducting electrode and visible light-responded performance.The preparation method of the application of the invention, this catalyst electrode can improve the dispersiveness of catalyst and the response of electrode pair visible ray, thus improves the catalytic efficiency of noble metal catalyst.
The above is only the preferred embodiment of the present invention; be not limited to the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (10)
1. a titania nanotube supported catalyst electrode for photoresponse, is made up of base material and catalyst layer, it is characterized in that: described base material is metal titanium sheet and carrier titania nanotube; Catalyst layer above base material is made up of at least one in catalyst platinum, palladium, gold, silver noble metal and redox graphene.
2. the titania nanotube supported catalyst electrode of photoresponse according to claim 1, is characterized in that: the pattern of the catalyst of described load on base material is nano flower-like.
3. a preparation method for the titania nanotube supported catalyst electrode of photoresponse, is characterized in that: comprise the steps:
S1: generate titania nanotube at base material titanium plate surface by anode oxidation method;
S2: catalyst electro-deposition, by least one electro-deposition in platinum, palladium, gold, silver noble metal at titania nanotube on the surface, prepares titania nanotube supported catalyst electrode;
S3: at electrode face finish one deck redox Graphene, forms the titania nanotube supported catalyst electrode of the photoresponse of graphene modified.
4. the preparation method of the titania nanotube supported catalyst electrode of photoresponse according to claim 3, is characterized in that: specifically comprise the steps: at described step S1
S11: electrochemical solution is prepared
Ammonium fluoride is dissolved in the mixed solution of ethylene glycol and water, makes the electrochemical solution that ammonium fluoride mass fraction is 0.5%;
S12: prepare titania nanotube
Being inserted by the electrochemical solution prepared and being provided with titanium sheet be anode and platinized platinum is in the electrochemical reaction appts of negative electrode, adopt anode oxidation method, to power on chemical preparation titania nanotube in base material titanium sheet, calcine in Muffle furnace after then obtained titania nanotube deionized water rinsing being dried.
5. the preparation method of the titania nanotube supported catalyst electrode of photoresponse according to claim 4, is characterized in that: in described step S12, the current potential 60V of the anode oxidation method adopted, and controls reaction time 2h-2.5h.
6. the preparation method of the titania nanotube supported catalyst electrode of photoresponse according to claim 4, is characterized in that: in described step S12, titania nanotube 450 DEG C of calcining 2h in Muffle furnace after described oven dry.
7. the preparation method of the titania nanotube supported catalyst electrode of photoresponse according to claim 3; it is characterized in that: be specially at described step S2: titanium dioxide nanotube electrode is inserted in the aqueous solution of slaine of a kind of precious metal element at least had in platinum, palladium, gold, silver; under the protection of nitrogen; utilize potentiostatic method electro-deposition catalyst, prepare titania nanotube supported catalyst electrode.
8. the preparation method of the titania nanotube supported catalyst electrode of photoresponse according to claim 7, is characterized in that: the concentration of aqueous solution of described slaine is 1-5mmol/L; The current potential of the potentiostatic method adopted is-0.2V, and reference electrode is saturated calomel electrode.
9. the preparation method of the titania nanotube supported catalyst electrode of photoresponse according to claim 3, is characterized in that: specifically comprise the steps: at described step S3
S31: graphene oxide solution be slowly added drop-wise to titania nanotube supported catalyst electrode surface and dry;
S32: the titania nanotube supported catalyst electrode being coated with graphene oxide is inserted in PBS solution, with potentiostatic method, control the electrochemical reaction time at 1500s, electrochemical reduction oxidation Graphene, thus the titania nanotube supported catalyst electrode of obtained photoresponse.
10. the preparation method of the titania nanotube supported catalyst electrode of photoresponse according to claim 9, is characterized in that: the current potential of the potentiostatic method adopted is-0.9V, and reference electrode is saturated calomel electrode.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105186009A (en) * | 2015-09-07 | 2015-12-23 | 武汉理工大学 | Fuel-cell catalyst with nano-graphite carbon rivet structure and preparation method of fuel-cell catalyst |
| CN106847666A (en) * | 2016-11-17 | 2017-06-13 | 中国船舶重工集团公司第七二五研究所 | A kind of TiO2/BaTiO3/ RGO tri compounds optoelectronic film, its quick in situ preparation method and application |
| CN108845004A (en) * | 2018-06-15 | 2018-11-20 | 浙江大学 | A kind of photoelectric current carbon dioxide sensor |
| WO2020164360A1 (en) * | 2019-02-12 | 2020-08-20 | 深圳市溢鑫科技研发有限公司 | Upright few-layer graphene-metal nanoparticle composite catalytic electrode |
| CN113070085A (en) * | 2021-03-22 | 2021-07-06 | 五邑大学 | Photoelectric catalyst and preparation method thereof |
| CN113972380A (en) * | 2020-07-24 | 2022-01-25 | 云南创能斐源金属燃料电池有限公司 | Fuel cell catalyst, preparation method and application thereof |
| CN115490304A (en) * | 2022-08-25 | 2022-12-20 | 南京师范大学 | Preparation method and application of cerium dioxide doped titanium nanotube electrode |
-
2015
- 2015-01-21 CN CN201510029999.7A patent/CN104577139A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105186009A (en) * | 2015-09-07 | 2015-12-23 | 武汉理工大学 | Fuel-cell catalyst with nano-graphite carbon rivet structure and preparation method of fuel-cell catalyst |
| CN106847666A (en) * | 2016-11-17 | 2017-06-13 | 中国船舶重工集团公司第七二五研究所 | A kind of TiO2/BaTiO3/ RGO tri compounds optoelectronic film, its quick in situ preparation method and application |
| CN106847666B (en) * | 2016-11-17 | 2019-10-11 | 中国船舶重工集团公司第七二五研究所 | A kind of TiO2/BaTiO3/ RGO tri compound optoelectronic film, its quick in situ preparation method and application |
| CN108845004A (en) * | 2018-06-15 | 2018-11-20 | 浙江大学 | A kind of photoelectric current carbon dioxide sensor |
| CN108845004B (en) * | 2018-06-15 | 2020-10-13 | 浙江大学 | Photocurrent carbon dioxide sensor |
| WO2020164360A1 (en) * | 2019-02-12 | 2020-08-20 | 深圳市溢鑫科技研发有限公司 | Upright few-layer graphene-metal nanoparticle composite catalytic electrode |
| CN113972380A (en) * | 2020-07-24 | 2022-01-25 | 云南创能斐源金属燃料电池有限公司 | Fuel cell catalyst, preparation method and application thereof |
| CN113070085A (en) * | 2021-03-22 | 2021-07-06 | 五邑大学 | Photoelectric catalyst and preparation method thereof |
| CN113070085B (en) * | 2021-03-22 | 2023-07-14 | 五邑大学 | Photoelectric catalyst and preparation method thereof |
| CN115490304A (en) * | 2022-08-25 | 2022-12-20 | 南京师范大学 | Preparation method and application of cerium dioxide doped titanium nanotube electrode |
| CN115490304B (en) * | 2022-08-25 | 2023-10-27 | 南京师范大学 | Preparation method and application of cerium dioxide doped titanium nanotube electrode |
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Application publication date: 20150429 |