CN109103467A - A kind of preparation method and application of the graphene-based metallic catalyst of electrochemical stripping - Google Patents
A kind of preparation method and application of the graphene-based metallic catalyst of electrochemical stripping Download PDFInfo
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- CN109103467A CN109103467A CN201810937955.8A CN201810937955A CN109103467A CN 109103467 A CN109103467 A CN 109103467A CN 201810937955 A CN201810937955 A CN 201810937955A CN 109103467 A CN109103467 A CN 109103467A
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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
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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
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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 embodiment of the invention discloses a kind of graphene-based metallic catalyst of electrochemical stripping, preparation method and applications, wherein the graphene-based metallic catalyst is made of electrochemical stripping graphene with the metal nanoparticle for being distributed in graphene surface.The graphene-based metallic catalyst of electrochemical stripping provided by the invention, since the few surface defects of electrochemical stripping graphene, oxygen-containing functional group are few, so that the mechanical performance of the material and electric conductivity increase substantially.Therefore, a kind of graphene-based metallic catalyst with outstanding catalytic performance is obtained.
Description
Technical field
The present invention relates to electro-catalysis field, in particular to the graphene-based metallic catalyst of a kind of electrochemical stripping, its preparation
Method and application.
Background technique
Catalyst material can be improved reaction rate, determine reaction path, reduce the activation energy of reaction so as to reduce
The consumption of external energy, catalyst is but also many energy and materials are able to industrialization, commercialization, so that many new energy obtain
To promote and apply.
Fuel cell has many advantages, such as that small in size, energy conversion efficiency is high, theoretical energy is than high and environmental clean, in machine
Motor-car, mobile device, residential households are widely used in field, and the future fuel cell of miniaturization can be used as notebook
The power supply of the portable electronic products such as computer, video recorder, camera.However the raising of electrode catalyst material property and cost
Decline largely determines the promotion of fuel battery performance and widening for application range.Therefore, electrocatalysis characteristic is developed
Excellent catalyst material is the focus and emphasis of current fuel cell studies.
Graphene is a kind of ultra-thin two-dimension carbon material of only one atomic thickness.Studies have shown that graphene is with excellent
Electric conductivity and high theoretical specific surface area (2630m2g-1).Compared to traditional graphene oxide, the graphite of electrochemical stripping
Alkene has the advantages that oxygen-containing functional group is few, defect is small, makes it have the high advantage of good mechanical property, electric conductivity, and which dictates that
Its great potential in fuel cell field.The electrode material that electrochemical stripping graphene introduces fuel cell is expected to promote electricity
The performance in pond.But electrochemical stripping graphene is easy to reunite in water, while its surface lacks functional group, is not easy gold-supported
Metal catalyst.Therefore, it finds a kind of solution graphene to reunite and in the method for its area load metallic catalyst, just seem outstanding
It is important.
Summary of the invention
The embodiment of the invention discloses a kind of graphene-based metallic catalyst of electrochemical stripping, preparation method and application,
For improving the catalytic performance of catalyst.Technical solution is as follows:
Present invention firstly provides a kind of graphene-based metallic catalysts of electrochemical stripping, by electrochemical stripping graphene
And it is distributed in the metal nanoparticle composition of graphene surface.
In the preferred embodiment of the present invention, the partial size 5-10nm of the metal nanoparticle.
The present invention also provides the preparation methods of the graphene-based metallic catalyst of above-mentioned electrochemical stripping, comprising:
By the graphene ultrasonic disperse of electrochemical stripping in polar non-solute, corresponding metal is added into solution
Presoma stirs 2 hours at room temperature；
Solution is heated to 70~90 DEG C under nitrogen flowing, is then added thereto sodium borohydride, quickly stirs 0.5~1
Hour.Centrifuge washing, drying are later to get the graphene-based metallic catalyst of the electrochemical stripping.
In the preferred embodiment of the present invention, the polar solvent is selected from n,N-Dimethylformamide.
In the preferred embodiment of the present invention, the metal precursor is selected from chloroplatinic acid, palladium chloride, chlorine gold
Acid.
In the preferred embodiment of the present invention, electrochemical stripping graphene and the mass ratio of metal precursor are
1:1。
In the preferred embodiment of the present invention, oil bath temperature is 70 DEG C, and the reaction time is 30 minutes.
The present invention also provides a kind of electrode materials of fuel cell, with the graphene-based metal catalytic of above-mentioned electrochemical stripping
Agent is as anode active material.
Through the above technical solution it is found that the present invention provides a kind of graphene-based metallic catalyst of electrochemical stripping,
It is made of electrochemical stripping graphene and the metal nanoparticle for being distributed in graphene surface, electrochemical stripping graphene can divide
It is dispersed in polar non-solute, is conducive to the preparation of the graphene-based metallic catalyst of electrochemical stripping, electrochemistry of the invention
Removing graphene-based metallic catalyst can be used as the electrode material of fuel cell, can also be used as hydrogenation reaction, dehydrogenation reaction, two
The catalyst of carbon oxide conversion reaction, due to the high conductivity and metal nanoparticle and graphene of electrochemical stripping graphene
Between synergistic effect, the catalytic performance of catalyst can be promoted.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the X-ray diffractogram of the graphene-based metal platinum of electrochemical stripping prepared in embodiment 1；
Fig. 2 is the transmission electron microscope figure of the graphene-based metal platinum of electrochemical stripping prepared in embodiment 1；
Fig. 3 is the electrocatalysis characteristic of the graphene-based metal platinum of electrochemical stripping prepared in embodiment 1；
Fig. 4 is the electro-catalysis stability of the graphene-based metal platinum of electrochemical stripping prepared in embodiment 1.
Specific embodiment
The present invention provides a kind of graphene-based metallic catalysts of electrochemical stripping, by electrochemical stripping graphene and distribution
It is formed in the metal nanoparticle of graphene surface, the partial size of the metallic particles is 5-10nm.The electrochemical stripping graphene
Based metal catalysts can be made by following methods:
0.5~1.5g ammonium sulfate is weighed, is dissolved in 100mL water as electrolyte, uses platinum filament as cathode, graphite foil conduct
Anode, connection DC power supply are electrolysed, gained suspension are filtered, is cleaned 3 times or more, after drying with deionized water and ethyl alcohol
Product mixed with n,N-Dimethylformamide, ultrasound discards bottom sediment after standing, by upper layer dispersion liquid polytetrafluoroethyl-ne
Alkene filter membrane filters, dry, and electrochemical stripping graphene is made；
By the graphene ultrasonic disperse of electrochemical stripping in polar non-solute, metal precursor is added to solution
In, it stirs 2 hours at room temperature, reducing agent is added in solution, nitrogen stream protection, 70 DEG C of heating are quickly stirred 0.5 hour,
Centrifuge washing, it is dry to get the graphene-based metallic catalyst of the electrochemical stripping.
In the preferred embodiment of the present invention, polar non-solute described in scheme is selected from N, N- dimethyl methyl
Amide；As long as polar solvent described in scheme guarantees that it can be by electrochemical stripping graphene dispersion, it is preferable that the non-matter of polarity
The ratio of sub- solvent and electrochemical stripping graphene is 1000-2000:1mL/g；The metal precursor is selected from chloroplatinic acid, chlorine
Change palladium, gold chloride；Electrochemical stripping graphene and the mass ratio of metal precursor are 3:1~5, preferably 3:2；Described is lazy
Property gas can be the common gas, preferably nitrogen such as argon gas, nitrogen；The reducing agent can be sodium citrate, boron hydrogen
Change the common reducing agents, preferably sodium borohydride such as sodium, ascorbic acid.
The present invention also provides a kind of graphene-based metallic catalysts of application electrochemical stripping as anode catalyst
Fuel cell, following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Intrinsic graphene used in the present invention is prepared by the method for electrochemical stripping, abbreviation electrochemical stripping stone
Black alkene (EEG), the specific method is as follows:
The ammonium sulfate of 1.32g is dissolved in the deionized water of 100ml, using the solution as electrolyte.Use platinum (Pt) silk as
Cathode, graphite foil are anode, and connection DC power supply is electrolysed.In electrolytic process, voltage is first risen into 3V, is electrolysed 5min, then
5V is risen to, 5min is electrolysed, 10V is finally risen to, until electrolysis finishes.Resulting suspended mixture is filtered, with deionized water and second
Alcohol cleans several times.The graphene after being removed is dried, the product after drying is mixed with n,N-Dimethylformamide (DMF),
Ultrasound 3h again discards bottom sediment, then obtains the dispersion liquid of high-quality electrochemical stripping graphene (EEG) after standing 8h,
This dispersion liquid is filtered with teflon membrane filter (PTFE), it is dry then obtain electrochemical stripping graphene (EEG).
Embodiment 1:
By the EEG ultrasonic disperse of 0.03g in the DMF of 60ml, the chloroplatinic acid (H of 0.02g is added into solution2PtCl6·
6H2O), at room temperature stirring 2h to evenly dispersed.Mixed liquor is transferred in 100mL round-bottomed flask, mixed liquor is in N2It flows down and is added
Heat is to 70 DEG C, the then NaBH of 0.1g4It is added thereto, quickly stirs 30min.Be centrifuged after being then cooled to room temperature (10000 turns/
Minute) separation, ethanol washing three times, after removing supernatant liquid, 60 DEG C of vacuum are dried overnight, be made electrochemical stripping it is graphene-based
Metal platinum.
Embodiment 2:
By the EEG ultrasonic disperse of 0.02g in the DMF of 60ml, the palladium chloride (PdCl of 0.02g is added into solution2), room
The lower stirring 2h of temperature is to evenly dispersed.Mixed liquor is transferred in 100mL round-bottomed flask, mixed liquor is in N2It flows down and is heated to 70
DEG C, the then KBH of 0.1g4It is added thereto, quickly stirs 30min.(10000 revs/min) points are centrifuged after being then cooled to room temperature
Three times from, ethanol washing, after removing supernatant liquid, 60 DEG C of vacuum are dried overnight, and the graphene-based Metal Palladium of electrochemical stripping is made.
Embodiment 3:
By GO (graphene oxide) ultrasonic disperse of 0.02g in the DMF of 60ml, the chlorine platinum of 0.02g is added into solution
Acid (H2PtCl6·6H2O), at room temperature stirring 2h to evenly dispersed.Mixed liquor is transferred in 100mL round-bottomed flask, mixed liquor
In N2It flows down and is heated to 70 DEG C, then the NaBH of 0.1g4It is added thereto, quickly stirs 30min.After being then cooled to room temperature from
Three times, after removing supernatant liquid, 60 DEG C of vacuum are dried overnight for (10000 revs/min) of the heart separation, ethanol washings, and reduction is made
Graphene oxide Base Metal platinum.
Performance and test
1, X-ray diffraction (XRD) is analyzed
Using the x-ray powder diffraction instrument (model: X Pert PRO MPD) of Dutch Panaco company production to the present invention
The graphene-based metal platinum of the electrochemical stripping prepared in embodiment 1 carries out X-ray diffraction analysis, and analysis result is as shown in Figure 1；Point
Radioactive source during analysis is Cu-Ka, and measurement step-length is 0.017 °, and sweep time is 10 seconds/step.
As can be seen that the graphene-based metal of electrochemical stripping from the comparison of the standard card of the XRD and Pt of sample in Fig. 1
The base peak of platinum is fitted very much in the diffraction maximum of platinum, with standard PDF card, it was demonstrated that has successfully been loaded on the surface of graphene
Metal Pt nanoparticle.
2, transmission electron microscope (TEM) is analyzed
It is graphene-based to the electrochemical stripping prepared in embodiment 1 using transmission electron microscope (JEOL JEM-2010)
Metal platinum is scanned analysis, as a result as shown in Fig. 2, can clearly find out that metal Pt nanoparticle is dispersed in electricity in Fig. 2
The surface of chemical stripping graphene, the partial size of particle is about in 3~8nm.
Embodiment 4
Handle glass-carbon electrode
By diameter be 3mm glass-carbon electrode on the lens wiping paper soaked with isopropanol rounded grinding 0.5min, spend from
Sub- water washes surface contaminants, then successively in HNO3、CH3CH2OH、H22~3min of ultrasound is distinguished in O, finally uses deionized water
Rinse electrode surface.Glass-carbon electrode is successively used to the Al of 1.0 μm, 0.3 μm again2O3Slurry is polished to mirror surface on deerskin, polishes every time
Surface contaminants are first washed away afterwards, according still further to sequence ultrasound as above, are rinsed again with deionized water again after ultrasound.Thoroughly washing
Afterwards, in the KNO of 0.20mol/L3Middle record 1 × 10-3The K of mol/L3Fe(CN)6The cyclic voltammetry curve of solution, to test electrode
Performance, scanning speed 50mV/s, scanning range -0.6~0.8V.Spike potential under laboratory condition in gained cyclic voltammogram is poor
In 80mV hereinafter, and as close possible to 64mV, electrode can use, and electrode otherwise be handled again, until meeting the requirements.Then
Satisfactory electrode is rinsed well with deionized water rear spare.
Embodiment 5
Sample preparation work electrode is applied with glass-carbon electrode prepared by embodiment 4
By prepared sample according to sample: Nafion:CH3OH tests institute at CV for the proportional arrangement of 3mg:3 μ L:500 μ L
Sample is needed, adds it in 5ml sample cell after ultrasound 30min, the glass-carbon electrode handled well is coated in micro syringe
Mirror surface point, dripping sample amount every time is 1uL, amounts to 5uL.It is stand-by after the working electrode prepared is dried.
Comparative example 1
By sample prepared by embodiment 1 according to sample (EEG-Pt): Nafion:CH3OH is the ratio of 3mg:3 μ L:500 μ L
It is configured to sample needed for CV is tested, is added it in 5ml sample cell after ultrasound 30min, is coated in and has been handled with micro syringe
On the mirror surface of good glass-carbon electrode, dripping sample amount every time is 1uL, amounts to 5uL.It is stand-by after the working electrode prepared is dried.It should
Electrode is known as No. 1 electrode.
Comparative example 2
With the graphene oxide Base Metal platinum (rGO-Pt) of reduction prepared by embodiment 3 for catalyst, preparation work electricity
Pole.The difference of the preparation process of comparative example 2 and comparative example 1, which is only that, is substituted for the catalyst (EEG-Pt) in comparative example 1
RGO-Pt is other identical as comparative example 1.The electrode is known as No. 2 electrodes.
Fuel battery performance test
No. 1 electrode and No. 2 electrodes are tested on electrochemical workstation respectively, test result is respectively such as Fig. 3 and Fig. 4 institute
Show, this experiment is to carry out cyclic voltammetry, sampling interval 0.001V, voltage range 0- in the case where sweeping speed and being 0.05V/S
1.0V。
Fig. 3 is the electrocatalysis characteristic test result of No. 1 electrode and No. 2 electrodes, as can be seen from the figure electrochemical stripping stone
The peak current density of black alkene Supported Pt Nanoparticles is 1.50mA/cm2, the peak current density of the graphene oxide-loaded platinum of reduction is
1.16mA/cm2；As it can be seen that No. 1 electrode is compared with No. 2 electrodes, electrocatalysis characteristic is greatly improved.Fig. 4 is No. 1 electrode and 2
The stability test of number electrode is as a result, it can be seen from the figure that after carrying out 200 CV loop tests, electrochemical stripping graphene
The peak current density of Supported Pt Nanoparticles is 1.28mA/cm2, remain the 85% of initial current density；No. 2 electrodes carry out 200 CV and follow
After ring test, the peak current density of the graphene oxide-loaded platinum of reduction is 0.77mA/cm2, remain initial current density
66%；As it can be seen that No. 1 electrode is compared with No. 2 electrodes, stability is greatly improved.
It can be seen that by above-mentioned test using the graphene-based metallic catalyst of electrochemical stripping provided by the present invention,
As fuel battery anode catalyst, performance compared with the graphene oxide-loaded metallic catalyst using reduction, urge by electricity
It is obviously high to change performance, and cyclical stability significantly improves.
Above to a kind of graphene-based metallic catalyst of electrochemical stripping provided by the present invention, preparation method and application
It is described in detail.Principle and implementation of the present invention are described for specific embodiment used herein, above
The explanation of embodiment is merely used to help understand method and its central idea of the invention.It should be pointed out that for the general of this field
, without departing from the principle of the present invention, can be with several improvements and modifications are made to the present invention for logical technical staff, this
A little improvement and modification also fall into the protection of the claims in the present invention.
Claims (12)
1. a kind of graphene-based metallic catalyst, which is characterized in that by electrochemical stripping graphene and be distributed in graphene table
The metal nanoparticle in face forms.
2. the preparation method of graphene-based metallic catalyst as described in claim 1, it is characterised in that the following steps are included:
0.5~1.5g ammonium sulfate is weighed, is dissolved in 100mL water as electrolyte, uses platinum filament as cathode, graphite foil is as just
Pole, connection DC power supply are electrolysed, gained suspension are filtered, is cleaned 3 times or more, after drying with deionized water and ethyl alcohol
Product is mixed with n,N-Dimethylformamide, ultrasound, bottom sediment is discarded after standing, by upper layer dispersion liquid polytetrafluoroethylene (PTFE)
Filter membrane filters, dry, and electrochemical stripping graphene is made；
By the graphene ultrasonic disperse of electrochemical stripping in polar non-solute, metal precursor is added in solution,
It stirs 2 hours at room temperature, reducing agent is added in solution, it is small quickly to stir 0.5~1 for nitrogen stream protection, 70~90 DEG C of heating
When, centrifuge washing is dry, and graphene-based metallic catalyst is made.
3. the method as described in claim 1, which is characterized in that the metal nanoparticle include platinum, palladium, gold, silver, iron, cobalt,
The alloy that nickel, copper, tin, zinc and above-mentioned any two kinds of metals form.
4. the method as described in claim 1, which is characterized in that the size of the metal nanoparticle is in 2~20nm.
5. method according to claim 1 or 2, which is characterized in that the graphene is the graphene of electrochemical process removing, is contained
There are considerably less defect and oxygen-containing functional group.
6. method according to claim 2, which is characterized in that the voltage range is 3~15V.
7. method according to claim 2, which is characterized in that the metal precursor includes metal described in claim 3
Chloride, nitrate, sulfate, acetate, alkoxide.
8. method according to claim 2, which is characterized in that the polar non-solute includes acetonitrile, N, N- dimethyl
Formamide, dimethyl sulfoxide, hexamethylphosphoramide, 1,3-Dimethyl-2-imidazolidinone.
9. method according to claim 2, which is characterized in that the reducing agent includes sodium citrate, sodium borohydride, hydroboration
Potassium, lithium aluminium hydride reduction, hydrazine hydrate, vitamin C, ascorbic acid.
10. method according to claim 2, which is characterized in that the mass ratio of electrochemical stripping graphene and metal precursor
Example is 3:1~5, preferably 1:1.
11. graphene-based metallic catalyst according to claim 1, main application is the electrode material of fuel cell,
Peak current density is in 1.5mA/cm2More than, the active conservation rate after 200 circulations is 85% or more.
12. graphene-based metallic catalyst according to claim 1, is also used as hydrogenation reaction, dehydrogenation reaction, dioxy
Change the catalyst of carbon conversion reaction.
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| CN112430828A (en) * | 2020-09-23 | 2021-03-02 | 浙江大学衢州研究院 | Preparation method of transition metal doped nickel-based metal organic framework three-dimensional electrode material, product and application thereof |
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| CN112430828A (en) * | 2020-09-23 | 2021-03-02 | 浙江大学衢州研究院 | Preparation method of transition metal doped nickel-based metal organic framework three-dimensional electrode material, product and application thereof |
| CN112430828B (en) * | 2020-09-23 | 2021-11-09 | 浙江大学衢州研究院 | Preparation method of transition metal doped nickel-based metal organic framework three-dimensional electrode material, product and application thereof |
| CN113046777A (en) * | 2021-03-03 | 2021-06-29 | 厦门大学 | Preparation of graphene composite material and application of graphene composite material in energy storage and conversion |
| CN114477152A (en) * | 2021-12-30 | 2022-05-13 | 杭州电子科技大学 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
| CN114477152B (en) * | 2021-12-30 | 2023-08-15 | 杭州电子科技大学 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
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