CN106848330A - A kind of preparation method of oxygen reduction catalyst nano composite material - Google Patents
A kind of preparation method of oxygen reduction catalyst nano composite material Download PDFInfo
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- CN106848330A CN106848330A CN201611127395.7A CN201611127395A CN106848330A CN 106848330 A CN106848330 A CN 106848330A CN 201611127395 A CN201611127395 A CN 201611127395A CN 106848330 A CN106848330 A CN 106848330A
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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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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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
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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
- H01M4/96—Carbon-based electrodes
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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
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Abstract
The invention discloses a kind of preparation method of oxygen reduction catalyst nano composite material of technical field of nano material, the preparation method of the oxygen reduction catalyst nano composite material is comprised the following steps that：S1：Alumina formwork epoxy resin and curing agent are fixed on glassy carbon electrode surface；S2：Obtain nano line array electrode；S3：The surface of glass-carbon electrode is processed by mechanical lapping；S4：To be cleaned in ultrasonic water bath by the glass-carbon electrode after polishing；S5：Activated with cyclic voltammetry；S6：Nano particle is deposited with cyclic voltammetry, nano-particle electrode is prepared；S7：The nano-particle electrode that will be prepared in the nano line array electrode prepared in step S2 and step S6 prepares nano composite material using 25~30 circulations of cyclic voltammetry, preparation method of the present invention is simple, low cost, platinum catalyst is substituted using oxidation reduction catalyst, the nano composite material particle diameter distribution for obtaining is homogeneous, favorable reproducibility.
Description
Technical field
The present invention relates to technical field of nano material, specially a kind of preparation side of oxygen reduction catalyst nano composite material
Method.
Background technology
Proton Exchange Membrane Fuel Cells is a kind of fuel cell, in principle equivalent to " inverse " device of water electrolysis.Its list
Battery is made up of anode, negative electrode and PEM, and anode is the place that hydrogen fuel is aoxidized, and negative electrode is oxidant reduction
Place, all containing the catalyst for accelerating electrode electro Chemical reaction, PEM is used as electrolyte at the two poles of the earth.Equivalent to one during work
Dc source, its anode is power cathode, and negative electrode is positive source.Proton Exchange Membrane Fuel Cells has energy conversion efficiency
Height, specific energy, power density be high and room temperature quickly starts etc. it is many prominent the characteristics of, it is considered to be following main green energy resource
One of.The catalyst for being now widely used for cell cathode is platinum, but it is to restrict it commercially that the reserves of platinum are few and expensive
The main cause of application.
Therefore a kind of oxidation reduction catalyst that can substitute platinum as catalyst is needed, to adapt to the proton for developing increasingly
The development of exchange film fuel battery, therefore, we have proposed a kind of preparation method throwing of oxygen reduction catalyst nano composite material
Enter to use, to solve the above problems.
The content of the invention
It is above-mentioned to solve it is an object of the invention to provide a kind of preparation method of oxygen reduction catalyst nano composite material
The catalyst for being now widely used for cell cathode proposed in background technology is platinum, but the reserves of platinum are few and expensive is
Restrict the problem of the main cause of its business application.
To achieve the above object, the present invention provides following technical scheme：A kind of oxygen reduction catalyst nano composite material
Preparation method, the preparation method of the oxygen reduction catalyst nano composite material is comprised the following steps that：
S1：Alumina formwork epoxy resin and curing agent are fixed on glassy carbon electrode surface, and are stirred in room temperature and magnetic force
In the environment of mixing, plate constant potential -0.7~-0.9V in alkaline palladium and deposit 2~5h；
S2：Dissolved with 10~15% phosphoric acid solutions by post-depositional alumina formwork, obtained nano-wire array electricity
Pole；
S3：The surface of glass-carbon electrode is processed by mechanical lapping, minute surface degree is polished to its surface using diamond dust；
S4：To be cleaned in ultrasonic water bath by the glass-carbon electrode after polishing, every time 2~4min, wash cycles 3~
5 times；
S5：Glass-carbon electrode is used into cyclic voltammetric in the sulfuric acid solution of 0.5~1mol/L after thoroughly being washed using cleaning fluid
Method is activated；
S6：In by the modulation solution of pretreated glass-carbon electrode immersion nitrogen saturation, and redox is added to urge
Agent, under the system of three electrodes, nano particle is deposited with cyclic voltammetry, prepares nano-particle electrode, wherein scanning electricity
Position scope is 0.25~0.1V, and sweep speed is 0.013~0.015V/s；
S7：The nano-particle electrode that will be prepared in the nano line array electrode prepared in step S2 and step S6 is utilized
25~30 circulations of cyclic voltammetry prepare nano composite material.
Preferably, in the step S1, curing agent is the resol curing agent of high temperature modification, turning during magnetic agitation
Speed is 500~1800r/min.
Preferably, in the step S5, cleaning fluid is the mixture of ethanol, nitric acid and distilled water, wherein ethanol：Nitric acid：
Distilled water=1:1:3.5.
Preferably, in the step S5, when being activated using cyclic voltammetry, scanning potential range is -1~1V, instead
Multiple scanning is untill the cyclic voltammogram of stabilization is reached.
Preferably, in the step S6, modulation solution is 6~8mol/L platinum acid chloride solutions and 0.5~1mol/L hydrogen chloride
The mixed liquor of solution.
Preferably, in the step S6, it is working electrode that three-electrode system uses glass carbon, and saturation calomel is reference electrode,
Platinized platinum is electrode.
Preferably, in the step S6, oxidation reduction catalyst is catalytic hydrogenation class reducing catalyst.
Preferably, in the step S7, before volt-ampere experiment is circulated, the high pure nitrogen of 15~20min is first passed through,
To remove dissolved oxygen, with cyclic voltammetry activated electrode in nitrogen atmosphere, high-purity 15~20min of oxygen is then passed to,
Volt-ampere experiment is circulated in oxygen atmosphere.
Compared with prior art, the beneficial effects of the invention are as follows：Preparation method of the present invention is simple, low cost, using oxidation
Reducing catalyst substitutes platinum catalyst, and the nano composite material particle diameter distribution for obtaining is homogeneous, favorable reproducibility.
Brief description of the drawings
Fig. 1 is workflow diagram of the present invention；
Fig. 2 is the schematic diagram of the embodiment of the present invention one；
Fig. 3 is the schematic diagram of the embodiment of the present invention two；
Fig. 4 is the schematic diagram of the embodiment of the present invention three.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment one
A kind of preparation method of oxygen reduction catalyst nano composite material, the oxygen reduction catalyst nano composite material
Preparation method is comprised the following steps that：
S1：Alumina formwork epoxy resin and curing agent are fixed on glassy carbon electrode surface, and are stirred in room temperature and magnetic force
In the environment of mixing, in alkaline palladium plating constant potential -0.7V deposition 2h, curing agent is the resol curing agent of high temperature modification, magnetic
Rotating speed when power is stirred is 500r/min；
S2：Dissolved with 10% phosphoric acid solution by post-depositional alumina formwork, obtained nano line array electrode；
S3：The surface of glass-carbon electrode is processed by mechanical lapping, minute surface degree is polished to its surface using diamond dust；
S4：To be cleaned in ultrasonic water bath by the glass-carbon electrode after polishing, each 2min, wash cycles 3 times；
S5：Glass-carbon electrode is lived in the sulfuric acid solution of 0.5mol/L with cyclic voltammetry after thoroughly being washed using cleaning fluid
Change, cleaning fluid is the mixture of ethanol, nitric acid and distilled water, wherein ethanol：Nitric acid：Distilled water=1:1:3.5, lied prostrate using circulation
When peace method is activated, scanning potential range is -1V, is repeatedly scanned with untill the cyclic voltammogram of stabilization is reached；
S6：In by the modulation solution of pretreated glass-carbon electrode immersion nitrogen saturation, and redox is added to urge
Agent, under the system of three electrodes, nano particle is deposited with cyclic voltammetry, prepares nano-particle electrode, wherein scanning electricity
Position scope is 0.25V, and sweep speed is 0.013V/s, and modulation solution is that 6mol/L platinum acid chloride solutions and 0.5mol/L hydrogen chloride are molten
The mixed liquor of liquid, it is working electrode that three-electrode system uses glass carbon, and saturation calomel is reference electrode, and platinized platinum is electrode, and oxidation is also
Raw catalyst is catalytic hydrogenation class reducing catalyst；
S7：The nano-particle electrode that will be prepared in the nano line array electrode prepared in step S2 and step S6 is utilized
25 circulations of cyclic voltammetry prepare nano composite material, before volt-ampere experiment is circulated, are first passed through the High Purity Nitrogen of 15min
Gas, to remove dissolved oxygen, with cyclic voltammetry activated electrode in nitrogen atmosphere, then passes to high-purity oxygen 15min,
Volt-ampere experiment is circulated in oxygen atmosphere.Refer to Fig. 2 to learn, the cyclic voltammogram of nano line electrode has loaded nano wire
Glass-carbon electrode stronger redox peaks are observed near 0.2V in nitrogen atmosphere.
Embodiment two
A kind of preparation method of oxygen reduction catalyst nano composite material, the oxygen reduction catalyst nano composite material
Preparation method is comprised the following steps that：
S1：Alumina formwork epoxy resin and curing agent are fixed on glassy carbon electrode surface, and are stirred in room temperature and magnetic force
In the environment of mixing, in alkaline palladium plating constant potential -0.9V deposition 5h, curing agent is the resol curing agent of high temperature modification, magnetic
Rotating speed when power is stirred is 1800r/min；
S2：Dissolved with 15% phosphoric acid solution by post-depositional alumina formwork, obtained nano line array electrode；
S3：The surface of glass-carbon electrode is processed by mechanical lapping, minute surface degree is polished to its surface using diamond dust；
S4：To be cleaned in ultrasonic water bath by the glass-carbon electrode after polishing, each 4min, wash cycles 5 times；
S5：Glass-carbon electrode is lived in the sulfuric acid solution of 1mol/L with cyclic voltammetry after thoroughly being washed using cleaning fluid
Change, cleaning fluid is the mixture of ethanol, nitric acid and distilled water, wherein ethanol：Nitric acid：Distilled water=1:1:3.5, lied prostrate using circulation
When peace method is activated, scanning potential range is 1V, is repeatedly scanned with untill the cyclic voltammogram of stabilization is reached；
S6：In by the modulation solution of pretreated glass-carbon electrode immersion nitrogen saturation, and redox is added to urge
Agent, under the system of three electrodes, nano particle is deposited with cyclic voltammetry, prepares nano-particle electrode, wherein scanning electricity
Position scope is 0.1V, and sweep speed is 0.015V/s, and modulation solution is 8mol/L platinum acid chloride solutions and 1mol/L hydrogen chloride solutions
Mixed liquor, it is working electrode that three-electrode system uses glass carbon, and saturation calomel is reference electrode, and platinized platinum is electrode, redox
Catalyst is catalytic hydrogenation class reducing catalyst；
S7：The nano-particle electrode that will be prepared in the nano line array electrode prepared in step S2 and step S6 is utilized
30 circulations of cyclic voltammetry prepare nano composite material, before volt-ampere experiment is circulated, are first passed through the High Purity Nitrogen of 20min
Gas, to remove dissolved oxygen, with cyclic voltammetry activated electrode in nitrogen atmosphere, then passes to high-purity oxygen 20min,
Volt-ampere experiment is circulated in oxygen atmosphere.Fig. 3 is referred to, is the cyclic voltammogram that nano particle is loaded on glass-carbon electrode, oxygen
In 0.4V, maximum peak current is 0 μ A to a spike potential of reduction.
Embodiment three
A kind of preparation method of oxygen reduction catalyst nano composite material, the oxygen reduction catalyst nano composite material
Preparation method is comprised the following steps that：
S1：Alumina formwork epoxy resin and curing agent are fixed on glassy carbon electrode surface, and are stirred in room temperature and magnetic force
In the environment of mixing, in alkaline palladium plating constant potential -0.8V deposition 3.5h, curing agent is the resol curing agent of high temperature modification,
Rotating speed during magnetic agitation is 1000r/min；
S2：Dissolved with 13% phosphoric acid solution by post-depositional alumina formwork, obtained nano line array electrode；
S3：The surface of glass-carbon electrode is processed by mechanical lapping, minute surface degree is polished to its surface using diamond dust；
S4：To be cleaned in ultrasonic water bath by the glass-carbon electrode after polishing, each 3min, wash cycles 4 times；
S5：Glass-carbon electrode is lived in the sulfuric acid solution of 0.8mol/L with cyclic voltammetry after thoroughly being washed using cleaning fluid
Change, cleaning fluid is the mixture of ethanol, nitric acid and distilled water, wherein ethanol：Nitric acid：Distilled water=1:1:3.5, lied prostrate using circulation
When peace method is activated, scanning potential range is -0.5V, is repeatedly scanned with untill the cyclic voltammogram of stabilization is reached；
S6：In by the modulation solution of pretreated glass-carbon electrode immersion nitrogen saturation, and redox is added to urge
Agent, under the system of three electrodes, nano particle is deposited with cyclic voltammetry, prepares nano-particle electrode, wherein scanning electricity
Position scope is 0.75V, and sweep speed is 0.014V/s, and modulation solution is that 7mol/L platinum acid chloride solutions and 0.8mol/L hydrogen chloride are molten
The mixed liquor of liquid, it is working electrode that three-electrode system uses glass carbon, and saturation calomel is reference electrode, and platinized platinum is electrode, and oxidation is also
Raw catalyst is catalytic hydrogenation class reducing catalyst；
S7：The nano-particle electrode that will be prepared in the nano line array electrode prepared in step S2 and step S6 is utilized
28 circulations of cyclic voltammetry prepare nano composite material, before volt-ampere experiment is circulated, are first passed through the High Purity Nitrogen of 18min
Gas, to remove dissolved oxygen, with cyclic voltammetry activated electrode in nitrogen atmosphere, then passes to high-purity oxygen 18min,
Volt-ampere experiment is circulated in oxygen atmosphere.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (8)
1. a kind of preparation method of oxygen reduction catalyst nano composite material, it is characterised in that：The oxygen reduction catalyst nanometer
The preparation method of composite is comprised the following steps that：
S1：Alumina formwork epoxy resin and curing agent are fixed on glassy carbon electrode surface, and in room temperature and magnetic agitation
Under environment, plate constant potential -0.7~-0.9V in alkaline palladium and deposit 2~5h；
S2：Dissolved with 10~15% phosphoric acid solutions by post-depositional alumina formwork, obtained nano line array electrode；
S3：The surface of glass-carbon electrode is processed by mechanical lapping, minute surface degree is polished to its surface using diamond dust；
S4：To be cleaned in ultrasonic water bath by the glass-carbon electrode after polishing, every time 2~4min, wash cycles 3~5 times；
S5：Glass-carbon electrode is lived in the sulfuric acid solution of 0.5~1mol/L with cyclic voltammetry after thoroughly being washed using cleaning fluid
Change；
S6：In by the modulation solution of pretreated glass-carbon electrode immersion nitrogen saturation, and oxidation reduction catalyst is added,
Under the system of three electrodes, nano particle is deposited with cyclic voltammetry, nano-particle electrode is prepared, wherein scanning potential range
It is 0.25~0.1V, sweep speed is 0.013~0.015V/s；
S7：The nano-particle electrode that will be prepared in the nano line array electrode prepared in step S2 and step S6 is using circulation
25~30 circulations of voltammetry prepare nano composite material.
2. the preparation method of a kind of oxygen reduction catalyst nano composite material according to claim 1, it is characterised in that：Institute
State in step S1, curing agent is the resol curing agent of high temperature modification, rotating speed during magnetic agitation is 500~1800r/
min。
3. the preparation method of a kind of oxygen reduction catalyst nano composite material according to claim 1, it is characterised in that：Institute
State in step S5, cleaning fluid is the mixture of ethanol, nitric acid and distilled water, wherein ethanol：Nitric acid：Distilled water=1:1:3.5.
4. the preparation method of a kind of oxygen reduction catalyst nano composite material according to claim 1, it is characterised in that：Institute
State in step S5, when being activated using cyclic voltammetry, scanning potential range is -1~1V, be repeatedly scanned with until reaching stabilization
Cyclic voltammogram untill.
5. the preparation method of a kind of oxygen reduction catalyst nano composite material according to claim 1, it is characterised in that：Institute
State in step S6, modulation solution is the mixed liquor of 6~8mol/L platinum acid chloride solutions and 0.5~1mol/L hydrogen chloride solutions.
6. the preparation method of a kind of oxygen reduction catalyst nano composite material according to claim 1, it is characterised in that：Institute
State in step S6, it is working electrode that three-electrode system uses glass carbon, and saturation calomel is reference electrode, and platinized platinum is electrode.
7. the preparation method of a kind of oxygen reduction catalyst nano composite material according to claim 1, it is characterised in that：Institute
State in step S6, oxidation reduction catalyst is catalytic hydrogenation class reducing catalyst.
8. the preparation method of a kind of oxygen reduction catalyst nano composite material according to claim 1, it is characterised in that：Institute
State in step S7, before volt-ampere experiment is circulated, the high pure nitrogen of 15~20min is first passed through, to remove dissolved oxygen, in nitrogen
With cyclic voltammetry activated electrode in gas atmosphere, high-purity 15~20min of oxygen is then passed to, followed in oxygen atmosphere
Ring volt-ampere experiment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109962247A (en) * | 2017-12-22 | 2019-07-02 | 中国电子科技集团公司第十八研究所 | Preparation method of high-efficiency oxygen catalytic activity deposition platinum carbon fiber electrode |
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| CN109962247A (en) * | 2017-12-22 | 2019-07-02 | 中国电子科技集团公司第十八研究所 | Preparation method of high-efficiency oxygen catalytic activity deposition platinum carbon fiber electrode |
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Application publication date: 20170613 |