CN103647088B - A kind of electrode of surface platinum electrodeposition nano flower and its preparation method and application - Google Patents

A kind of electrode of surface platinum electrodeposition nano flower and its preparation method and application Download PDF

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Publication number
CN103647088B
CN103647088B CN201310632782.6A CN201310632782A CN103647088B CN 103647088 B CN103647088 B CN 103647088B CN 201310632782 A CN201310632782 A CN 201310632782A CN 103647088 B CN103647088 B CN 103647088B
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cnt
electrode
glass
platinum
carbon
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CN103647088A (en
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杨海峰
叶平平
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Shanghai Normal University
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Shanghai Normal University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/8803—Supports for the deposition of the catalytic active composition
    • 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
    • H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Materials Engineering (AREA)
  • Inert Electrodes (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses the scattered multi-walled carbon nano-tubes of a kind of novel phytic acid for the method for platinum electrodeposition nanometer flowers and to methanol oxidation.The platinum nanometer flowers that the present invention provides can be used in catalysis methanol, prepares fuel cell, and the synthesis of nanometer flowers comprises the following steps: CNT is dissolved in plant acid solution by (1) so that the concentration of CNT is 0.5 3mg/mL；(2) scattered for phytic acid CNT independently being installed to glass-carbon electrode, the self assembly time is 10 90 minutes；(3) by above-mentioned glass-carbon electrode at 0.2mM H2PtCl6+0.5M H2SO4Solution deposits under 0.1V 0.3V, obtains platinum nanometer flowers.Preparation method of the present invention is simple, environmental protection；The platinum nanometer flowers prepared have good electrochemical catalysis performance to methyl alcohol, better to the catalytic performance of methyl alcohol than naked glass carbon and the scattered CNT of DMF self-assemble to glass-carbon electrode deposition platinum nanometer flowers.

Description

A kind of electrode of surface platinum electrodeposition nano flower and its preparation method and application
Technical field
The invention belongs to catalyst preparation technical field, be specifically related to a kind of by novel dispersing Nano carbon tubes For preparing the method for platinum electrodeposition nanometer flowers and using it for the application of the electrochemical catalysis to methyl alcohol.
Background technology
DMFC (DMFC) have fuel cheap, easily stored and carry, theoretical unit Energy is high, is close to the advantages such as non-pollution discharge, be various small portable power supply ideal power source it One.And the anode catalyst of actual DMFC is easily poisoned, and therefore prepares and finds highly active catalysis Agent is the important channel improving DMFC performance, also becomes the target that researchers constantly pursue.In order to The capability study personnel improving eelctro-catalyst catalysis Oxidation of Methanol mainly study in terms of following two: On the one hand utilize CNT, carbon fiber meso-porous carbon material, Graphene and compound thereof etc. various novel Material with carbon element replaces original conventional carbon material to provide excellent electric conductivity to be beneficial to electricity for carrier for catalyst Son conduction, and make catalyst at carrier surface height by regulation catalyst carrier material microstructure Dispersion improves the utilization rate of catalyst, and therefore the selection of catalyst carrier and preparation are to improve catalyst to urge Change the key of activity；On the other hand research people is by preparing the bianry alloy of platinum, ternary alloy three-partalloy and leading to Cross and mix the approach of transition metal oxide to improve the active and anti-Poisoning of catalyst.
CNT is " the cage type pipe " of the shape such as hollow cylindrical by the curling of graphite carbon source sublayer.? In numerous nano materials, CNT is generally had an optimistic view of by people, is referred to as " coal " of nano material. The special performance of CNT self determines it has tempting application at the numerous areas of new and high technology Prospect, it has also become international study hotspot.CNT is that nano material is managed again, belongs to one-dimensional Nano material, it is easy to reunite.The reason that CNT is reunited has two: be wound around and greatly than table The high apparent activation energy that area causes.In actual application, its reunion form often destroys list Excellent mechanics that root CNT is shown, electrology characteristic, thus limit CNT should With.The solution methods that CNT generally uses supersonic oscillations to be supplementary means is disperseed.Mesh Front conventional Carbon nano-tube dispersant has two classes: the first kind is by organic solvent such as chloroform, acetone The solution formed with water, though this kind solvent energy dispersing Nano carbon tubes, dispersion soln can only retain several Hour；The dispersant that Equations of The Second Kind is made up of surfactant, conventional has neopelex (SDS).
Phytic acid, i.e. phytic acid, be a kind of natural products, phytic acid as chelating agent, antioxidant, Antistaling agent, water correction agent, fermentation accelerant, anticorrosive metal agent etc., be widely used in food, Medicine, paint, daily-use chemical industry, intermetallic composite coating, textile industry, plastics industry and macromolecule work The industry fields such as industry.This patent finds that it will not destroying carbon nanometer tube the dispersing Nano carbon tubes when Structure, and the application of electrode surface, beneficially electrochemistry can be assembled into easily.Up to now, At home and abroad there is no and utilize phytic acid carry out dispersing Nano carbon tubes and be assembled into above electrode for preparing platinum nanometer The method of particle.So find a kind of method preparing simple electrode assembling CNT be one compel Be essential important technological problems to be solved.
Summary of the invention
It is an object of the invention to build and a kind of utilize phytic acid to be assembled into electrode as the CNT of dispersant Surface depositing platinum nanoparticles, improves methanol oxidation performance.
The object of the present invention is achieved like this:
The preparation method of the electrode of a kind of surface platinum electrodeposition nano flower, comprises the following steps:
(1) CNT is scattered in plant acid solution (PA), ultrasonic 3-5h, obtains PA-CNTs Nano composite material, solid-to-liquid ratio is 0.5-3mg/mL；
(2) PA-CNTs nano composite material being self-assembled to glass-carbon electrode, the self assembly time is 10-90 Minute, obtain depositing the glass-carbon electrode of PA-CNTs nano composite material, be designated as PA-CNTs/GCE；
(3) PA-CNTs/GCE step (2) obtained is at 0.1-2mM H2PtCl6+0.1-1M H2SO4Carrying out electro-deposition in solution, the electricity controlling electro-deposition is 6.3mC-50.4mC, sedimentation potential For 0.1V-0.3V.
The preferred 1mg/mL of solid-to-liquid ratio in step (1).
Self assembly time preferred 30min in step (2).
In step (3), preferred PA-CNTs/GCE is at 0.2mM H2PtCl6+0.5-M H2SO4Solution In carry out electro-deposition, deposition electricity is 37.8mC, and sedimentation potential is 0.15V.
The invention have the advantage that
1, preparation method is simple, low cost.
2, the phytic acid scattered CNT stable performance prepared, does not affect the structure of CNT.
3, the phytic acid dispersing Nano carbon tubes electrode deposition platinum nanometer flowers prepared have high electricity to methyl alcohol Chemical catalysis activity energy.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the platinum nanometer flowers of naked glass-carbon electrode deposition.
Fig. 2 is the SEM figure above glass-carbon electrode after autonomous dress CNT.
Fig. 3 be Different electrodes deposition platinum nanometer flowers after to methanol oxidation Performance comparision figure.
Above-mentioned electrochemistry experiment is in CHI660D type electrochemical workstation (the Shanghai occasion China limited public affairs of instrument Department) on carry out, use traditional three-electrode system, modified electrode is working electrode, wherein to electrode Using saturated calomel electrode, silver/silver chloride electrode is reference electrode.Ultraviolet-visible (UV-vis) spectrum Experiment uses 760CRT dual-beam ultraviolet specrophotometer (Shanghai Precision Scientific Apparatus Co., Ltd)； SK2200H Ultrasound Instrument (Shanghai High Kudos Science Instrument Co., Ltd.).
Detailed description of the invention
Below by detailed description of the invention, the present invention will be further described.
(1) CNT is dissolved in plant acid solution so that the concentration of CNT is 1mg/mL；
(2) scattered for phytic acid CNT independently being installed to glass-carbon electrode, autonomous ETL estimated time of loading is 30 points Clock；
(3) by above-mentioned glass-carbon electrode at 0.2mM H2PtCl6+0.5M H2SO4In electrolyte solution, Deposition electricity is 37.8mC, and sedimentation potential is 0.15V, obtains platinum nanometer flowers.
Fig. 1 is the SEM figure of the platinum nanometer flowers of naked glass-carbon electrode deposition, it can be seen that platinum The diameter of nanometer flowers is about 1 μm.
Fig. 2 is the SEM figure after independently loading onto CNT above glass-carbon electrode, and Fig. 2 A is that phytic acid divides The CNT dissipated, Fig. 2 B is the scattered CNT of DMF, is evident that, plants from figure The scattered CNT of acid is preferably assembled on electrode.
Fig. 3 be Different electrodes deposition platinum nanometer flowers after to methanol oxidation Performance comparision figure, from figure It can be seen that the scattered CNT of phytic acid self-assembles to deposit platinum nanometer flowers (Fig. 3 c) on electrode to first The catalytic performance of alcohol is substantially better than naked glass Carbon deposition platinum nanometer flowers (Fig. 3 a) and DMF scattered carbon nanometer Pipe self-assembles to deposit on electrode platinum nanometer flowers (Fig. 3 b).
The above is presently preferred embodiments of the present invention, but the present invention should not be limited to this enforcement Example disclosure of that.So it is every without departing from the equivalence completed under principles of this disclosure or repair Change, both fall within the scope of protection of the invention.

Claims (3)

1. the preparation method of the electrode of a surface platinum electrodeposition nano flower, it is characterised in that include with Lower step:
(1) CNT is scattered in plant acid solution (PA), ultrasonic 3-5h, obtains PA-CNTs Nano composite material, solid-to-liquid ratio is 1mg/mL；
(2) PA-CNTs nano composite material being self-assembled to glass-carbon electrode, the self assembly time is 30min minute, obtain depositing the glass-carbon electrode of PA-CNTs nano composite material, be designated as PA-CNTs/GCE；
(3) PA-CNTs/GCE step (2) obtained is at 0.2mM H2PtCl6+0.5M H2SO4 Carrying out electro-deposition in solution, deposition electricity is 37.8mC, and sedimentation potential is 0.15V.
2. the electrode of a surface platinum electrodeposition nano flower, it is characterised in that by described in claim 1 Prepared by method.
3. the electrode of the surface platinum electrodeposition nano flower described in claim 2 is for the electrochemistry to methyl alcohol Catalysis.
CN201310632782.6A 2013-12-02 2013-12-02 A kind of electrode of surface platinum electrodeposition nano flower and its preparation method and application Expired - Fee Related CN103647088B (en)

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CN108125677B (en) * 2017-11-16 2023-02-10 深圳先进技术研究院 Microelectrode and preparation method thereof
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Citations (1)

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CN101634038A (en) * 2009-09-01 2010-01-27 南京大学 Glassy carbon electrode (GCE) modified by conductive copolymer carbon nanotube composite, preparation method thereof and method for removing perchlorat from water

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JP2011044334A (en) * 2009-08-21 2011-03-03 Hitachi Ltd Pt based catalyst for fuel cell, method of manufacturing the same, membrane electrode assembly for fuel cell, and fuel cell

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101634038A (en) * 2009-09-01 2010-01-27 南京大学 Glassy carbon electrode (GCE) modified by conductive copolymer carbon nanotube composite, preparation method thereof and method for removing perchlorat from water

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Si Ra Bae等.The Determination of Dopamine in the Presence of Ascorbic Acid at the Modified Glassy Carbon Electrode with Phytic Acid and Single-Walled Carbon Nanotubes.《Bull. Korean Chem. Soc.》.2007,第28卷(第12期),2363-2368. *
Zekerya Dursun等.Simultaneous Determination of Ascorbic Acid, Dopamine and Uric Acid at Pt Nanoparticles Decorated Multiwall Carbon Nanotubes Modified GCE.《Electroanalysis》.2010,第22卷(第10期),1106–1114. *

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