CN104451782B - A kind of octahedral structure nano platinum particle and its synthetic method and application - Google Patents
A kind of octahedral structure nano platinum particle and its synthetic method and application Download PDFInfo
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- CN104451782B CN104451782B CN201410719673.2A CN201410719673A CN104451782B CN 104451782 B CN104451782 B CN 104451782B CN 201410719673 A CN201410719673 A CN 201410719673A CN 104451782 B CN104451782 B CN 104451782B
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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
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- 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 discloses a kind of electrochemical techniques method of the nano platinum particle of synthesizing octahedral structure, using CHI660D electrochemical workstations, working electrode is used as using glass-carbon electrode, Ag/AgCl electrodes are used as reference electrode, platinum electrode is as to electrode, with ampere I t curve methods, with sedimentation potential 0.2V and sedimentation time 500s condition, electrochemical deposition chloroplatinic acid mixed solution is carried out, octahedral structure nano platinum particle has been synthesized.It is an advantage of the invention that simple to operate, favorable reproducibility, the nanoparticles stable of preparation is high to methanol oxidation activity.
Description
Technical field
It is specifically that one kind uses simple to operate, the high electrochemical techniques side of reappearance the invention belongs to fuel cell field
The nano platinum particle of method synthesizing octahedral structure, for catalysis methanol oxidation reaction.
Background technology
Fuel cell has the features such as energy transformation ratio is high, pollution is small, applied widely, load responding is fast, as vapour
Car electrical source of power, communication base station power supply, stand-by power supply and laptop computer field of power supplies have good development prospect.
In fuel cell, platinum catalyst is the electrocatalyst materials being most widely used.But its high cost and money
The scarcity in source is generally considered as the biggest obstacle of commercializing fuel cells.Therefore, need badly research novel high-performance, low cost
Elctro-catalyst.Performance is constituted with electrocatalysis material and decentralization is closely related, and in past 10 years, people are in nanocatalyst material
Impressive progress is achieved in terms of material composition and size controlling.In addition, catalytic performance also with the pattern of particle (i.e. surface crystal face or table
Face atomic arrangement) it is closely related.Recent years, design and develop the elctro-catalyst and its related basic research of new special appearance
Become the research emphasis of fuel cell electro-catalyst.Catalysis of the nano platinum particle of octahedral structure to methanol has very high
Activity.
The preparation of metal platinum nano material in terms of big for can be divided into physical preparation method and chemical preparation process.
Physical preparation method is material is evaporated in vacuum or inert atmosphere using technologies such as light, electricity, then makes atom or molecule shape
Into the ultramicro powder of nanoscale.Chemical preparation process is by the nucleation of metallic atom, grows and to prepare metal nanoparticle.
For example, chemical reduction method, electrochemical reducing, thermal decomposition method, photochemical breakdown method, phonochemistry decomposition method, Organometallic compounds
The part reduction of thing and displacement method etc..The Size Distribution for the metal nanoparticle that usual physical preparation method is obtained is relatively wide, and
Chemical preparation process then can by the species of the molar ratio, reducing agent and surfactant for changing reducing agent and metal salt,
The conditions such as reaction temperature, the pH value of solution relatively efficiently control the size and dimension of metal nanoparticle.Therefore chemistry is made
Preparation Method is the main method for preparing metal nanoparticle.
So far, it at home and abroad there is no using simple to operate, the electrochemical techniques method synthesizing octahedral of favorable reproducibility
The nano platinum particle of structure.So invention is a kind of to have simple to operate, favorable reproducibility, the nano platinum particle system of nanoparticles stable
Preparation Method is an important technological problems in the urgent need to address.
The content of the invention
The purpose of the present invention is that by simple to operate, the electrochemical techniques of favorable reproducibility prepare nanoparticles stable, to first
The nano platinum particle of the high octahedral structure of alcohol catalysis activity.
The object of the present invention is achieved like this：
A kind of octahedral structure nano platinum particle electrochemical method for synthesizing and its methanol oxidation application, comprise the following steps:
(1) chloroplatinic acid mixed solution is prepared：Take 18.0~20.0mmol/L chloroplatinic acids (H2PtCl6), chlorination is added thereto
Potassium (KCl) solid, makes chloroplatinic acid mixed solution concentration reach 19.0~25.0mmol/L, adds Brij58 surfactants extremely
Its mass fraction is 0.7%~1.2%, is stirred, and is stood, and is put into 4 DEG C of preservations in refrigerator；
(2) glass-carbon electrode is successively subjected to sanding and polishing with the alumina powder of 0.3 micron and 0.05 micron respectively, then
Deionized water is used respectively, and ethanol and deionized water are cleaned to glass-carbon electrode；
(3) electrochemical deposition synthesis nano platinum particle is carried out using CHI660D electrochemical workstations and three-electrode system：With
Glass-carbon electrode is as working electrode, and Ag/AgCl electrodes are as reference electrode, and platinum electrode is bent using ampere i-t as to electrode
Line method, with sedimentation potential -0.2V and sedimentation time 500s condition, carries out the above-mentioned chloroplatinic acid mixed solution of electrochemical deposition,
Nano platinum particle is synthesized, 10 microlitres of 1% Nafion solution is then added dropwise, dries at room temperature standby.
Catalysis of the nano platinum particle of octahedral structure to methanol and formic acid has higher activity.Using simple to operate,
Reproducible electrochemical techniques prepare nanoparticles stable, the octahedral structure nano platinum particle high to methanol oxidation activity.
The pattern of nano-particle under the conditions of differential responses is observed by field emission scanning electron microscope (SEM), and has investigated the platinum of different-shape
Catalytic activity of the nano-particle to methanol.Test result indicates that, using I-t curve electrochemical methods, in sedimentation potential -0.2V,
Under the conditions of sedimentation time 500s, obtain the nano platinum particle of octahedral structure, and with the nano platinum particle that is prepared under other conditions
Compare, to the catalytic activity highest of methanol.
Brief description of the drawings
The nano platinum particle modified electrode of Fig. 1 difference sedimentation time synthesis is in 0.5M H2SO4, following in 1.0M methanol solutions
Ring volt-ampere curve figure.
The SEM figures of the nano platinum particle of Fig. 2 difference sedimentation time synthesis, A-100s, B-200s, C-300s, D-400s, E-
500s, F-600s (sedimentation time).
The nano platinum particle modified electrode of Fig. 3 difference sedimentation potential synthesis is in 0.5M H2SO4, following in 1.0M methanol solutions
Ring volt-ampere curve figure.
Fig. 4 octahedral structures modified glassy carbon electrode and commercial nano platinum particle modified glassy carbon electrode are in 0.5M H2SO4, 1.0M
Cyclic voltammetry curve figure in methanol solution.
Fig. 5 octahedral structures modified glassy carbon electrode and commercial nano platinum particle modified glassy carbon electrode are in 0.5M H2SO4Solution
In cyclic voltammetry curve figure.
Embodiment
Present invention experiment is enterprising in electrochemistry CHI 660D types electrochemical workstation (Shanghai Chen Hua Instrument Ltd.)
OK；Field emission scanning electron microscope spectrum uses Hitachi S -4800 (Tokyo, Japan) field emission scanning electron microscope,
SK2200H Ultrasound Instruments (Shanghai High Kudos Science Instrument Co., Ltd.).
Below by embodiment, the present invention will be further described.
Measure 18.0~20.0mmol/L chloroplatinic acids (H2PtCl6) 3.0~5.0mL, add potassium chloride into platinum acid chloride solution
(KCl) solid, makes its concentration reach 19.0~25.0mmol/L.Into this mixed solution add Brij58 surfactants to its
Mass fraction is 0.7%~1.2%, and stirring makes it uniform, then stands certain time, is then placed within 4 DEG C of refrigerators and preserves,
It is standby.A diameter of 3 millimeters of glass-carbon electrode is successively subjected to polishing throwing with the alumina powder of 0.3 micron and 0.05 micron respectively
Light, then uses deionized water, ethanol and deionized water are cleaned to glass-carbon electrode respectively.Using CHI660D electrochemical operations
Stand and three-electrode system carries out electrochemical deposition synthesis nano platinum particle.Using glass-carbon electrode as working electrode, Ag/AgCl electrodes
As reference electrode, platinum electrode is as to electrode.Using ampere i-t curve methods, with sedimentation potential -0.2V and sedimentation time
500s condition, carries out the above-mentioned chloroplatinic acid mixed solution of electrochemical deposition, synthesizing octahedral structure nano platinum particle.Then it is added dropwise
10 microlitres of 1% Nafion solution, dries standby at room temperature.
Influence of the nano platinum particle synthesized under the conditions of different sedimentation times to the catalytic performance of methanol：
Fig. 1 is the H in 0.5M2SO4, in 1.0M methanol, the platinum synthesized in sedimentation potential -0.2V and different sedimentation times is received
Catalytic cycle volt-ampere curve figure of the rice corpuscles modified glassy carbon electrode to methanol.By Fig. 1, it is apparent that depositing electricity in -0.2V
Under position, catalytic performance highest of the nano platinum particle that sedimentation time 500s is synthesized to methanol.Meanwhile, in order to observe during not synsedimentary
Between the influence of the pattern of nano platinum particle that synthesizes to methanol oxidation performance, in experimentation, using field emission scanning electron microscope
(SEM) morphology characterization is carried out to nano platinum particle modified electrode.
Fig. 2 A-F are the nano platinum particle SEM morphology characterization figures synthesized under the conditions of different sedimentation times, can from figure
Go out, when deposited between when being 100s, the shape of nano-particle is largely ball-shaped and particle size is smaller, there is fraction
Nano-particle is octahedral structure, but the octahedra volume formed is larger (diameter is about 1 μm).Sedimentation time from 100s~
400s, most of nanostructured of formation is all spheroidal, and octahedral just only occurs under the conditions of 100s and 300s sedimentation times
The nano platinum particle of body structure.It is that the Nanoparticle shape of synthesis is almost octahedral under the conditions of 500s and 600s between when deposited
Body structure, and particle diameter about 500nm.The nano platinum particle surface synthesized under the conditions of 500s is relatively rough, and edge has
Defect.The nano platinum particle synthesized under the conditions of 600s has some particles to be stacked, and may reduce active surface area.
By Fig. 1 data it may be speculated that surface is rougher, the nano platinum particle of the defective octahedral structure in edge is shown pair
The catalytic performance of methanol is higher.Experimental data shows, the nano platinum particle of octahedral structure is than spherical nano platinum particle to methanol
Catalytic performance it is higher.
Influence of the nano platinum particle of different sedimentation potential synthesis to methanol oxidation performance：
Ampere I-t curve methods are a kind of methods that constant potential reduces metal ions.
Fig. 3 is the H in 0.5M2SO4, in 1.0M methanol, the nano platinum particle modified glassy carbon electrode of different sedimentation potentials synthesis
To the catalytic cycle volt-ampere curve figure of methanol, clearly showed that from Fig. 3, under the conditions of sedimentation potential -0.2V, the platinum nanometer of synthesis
Catalytic performance highest of the particle modified electrode to methanol.
Fig. 4 and Fig. 5 is contrast experiment.
Fig. 4 is that octahedral structure nano platinum particle modified glassy carbon electrode and commercial nano platinum particle modified glassy carbon electrode exist
0.5M H2SO4, cyclic voltammetry experiment is carried out in 1.0M methanol, hence it is evident that found out, the nano platinum particle of octahedral structure is to methanol
The high nano platinum particle with commercialization of catalytic activity.
Fig. 5 is two kinds of different modifying electrodes in 0.5M H2SO4Carry out cyclic voltammetry experiment, from experimental result as can be seen that
The active surface area of the glass-carbon electrode of octahedral structure nano platinum particle modification is higher than the glass carbon of commercial nano platinum particle modification
Electrode.
Claims (1)
1. a kind of octahedral structure nano platinum particle electrochemical deposition synthetic method, it is characterised in that comprise the following steps:
(1) chloroplatinic acid mixed solution is prepared：18.0~20.0mmol/L chloroplatinic acids are taken, solid potassium chloride is added thereto, make chlorine
Platinic acid mixed solution concentration reaches 19.0~25.0mmol/L, adds Brij58 surfactants to its mass fraction and is
0.7%~1.2%, stir, stand, be put into 4 DEG C of preservations in refrigerator；
(2) glass-carbon electrode is successively subjected to sanding and polishing with the alumina powder of 0.3 micron and 0.05 micron respectively, then distinguished
With deionized water, ethanol and deionized water are cleaned to glass-carbon electrode；
(3) electrochemical deposition synthesis nano platinum particle is carried out using CHI660D electrochemical workstations and three-electrode system：With glass carbon
Electrode is as working electrode, and Ag/AgCl electrodes are as reference electrode, and platinum electrode is as to electrode, using ampere i-t curve sides
Method, with sedimentation potential -0.2V and sedimentation time 500s condition, chloroplatinic acid mixed solution obtained by electrochemical-deposition step (1) is closed
Into nano platinum particle.
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| CN107482231A (en) * | 2017-08-01 | 2017-12-15 | 江苏理工学院 | A kind of spherical Pt/ charings stalk compound material of fine and close three-dimensional manometer and preparation method thereof |
| CN107845815B (en) * | 2017-10-23 | 2019-08-09 | 济南大学 | It is a kind of for improving the implementation method of methanol fuel cell electrooxidation activity |
| CN107845817B (en) * | 2017-10-23 | 2019-06-21 | 济南大学 | A method of using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidation formic acid electrochemistry |
| CN107845816B (en) * | 2017-10-23 | 2019-08-09 | 济南大学 | A kind of coarse shape of octahedron PtCoFe alloy particle and preparation method thereof |
| CN113224324B (en) * | 2021-07-08 | 2021-09-07 | 成都大学 | Palladium-doped aluminum-cobalt-chromium-iron-nickel high-entropy alloy composite electrode and preparation method thereof |
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| CN102189267B (en) * | 2011-04-26 | 2013-04-10 | 浙江理工大学 | Method for preparing highly-dispersed regular octahedral platinum nano particles |
| CN102290257B (en) * | 2011-05-19 | 2012-10-03 | 内蒙古大学 | Method for preparing dye sensitized solar cell with selective light transmission |
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