CN107845815A - A kind of implementation method for being used to improve methanol fuel cell electrooxidation activity - Google Patents
A kind of implementation method for being used to improve methanol fuel cell electrooxidation activity Download PDFInfo
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- CN107845815A CN107845815A CN201710990589.8A CN201710990589A CN107845815A CN 107845815 A CN107845815 A CN 107845815A CN 201710990589 A CN201710990589 A CN 201710990589A CN 107845815 A CN107845815 A CN 107845815A
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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
- H01M4/921—Alloys or mixtures with metallic elements
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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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 present invention relates to a kind of implementation method for being used to improve methanol fuel cell electrooxidation activity.Methanol electro-oxidizing test is in 0.5M H2SO4+2M CH3Cyclic voltammetry is carried out in OH electrolyte; using the coarse octahedra PtCoFe being prepared as methanol fuel cell electro-oxidizing-catalyzing agent; catalyst preparation is with chloroplatinic acid; cobalt chloride and ferric trichloride are raw material; using glycine as reducing agent and protective agent; the SDS and NaI of certain content are added, the higher coarse shape of octahedron PtCoFe alloy nano particles of selectivity, preparation method green cleaning is prepared.The coarse octahedra PtCoFe alloy nano particles step atom obtained is more, and active site density is high, shows excellent electro catalytic activity in the experiment of methanol fuel cell electro-oxidizing-catalyzing, is with a wide range of applications.
Description
Technical field
The invention belongs to methanol fuel cell performance study field.Specifically, the present invention is to use the coarse octahedral bodily form
Looks PtCoFe alloy nano particles improve catalysis oxidation methanol fuel cell electroxidation performance.
Background technology
Precious metals pt nano-structured calalyst is widely used in work due to its excellent catalytic performance and heat endurance
Industry is catalyzed, bionic, the field such as electro-catalysis.But due to some restraining factors in actual applications, such as easily poisoning, life-span
Short and price is high so that this excellent nanocatalyst can not further genralrlization and application.Research worker is understanding
Certainly these problems, substitute Pt, formation Pt bases binary/polynary frequently with by cheap 3d transition metals part at present
Alloy catalyst, and controlled by condition, probe into its pattern, composition and the relation of stable in catalytic performance.
In numerous transition metals, Co and Fe respectively as on the earth compared with one of transition metal of horn of plenty,
It is that Pt base bianry alloys preferably select.It is less that the report of PtCoFe alloy nanoparticle submethods is prepared at present, and these methods
All it is that organic solvent macromolecular is wrapped up as most of solvent, the PtCoFe alloy nano particles being synthesized by organic matter, it is living
Property position can not expose, and can not be in contact with reactant.Therefore design and the exploitation aqueous solution prepares PtCoFe alloy nano particles tool
There is important meaning.A kind of method for preparing coarse octahedra PtCoFe alloy nano particles that the present invention develops, is greatly improved
Pt step atomicity, add the active site density of PtCoFe alloys.
Fuel cell is considered as the important power set of traditional internal combustion engine alternative in the near future.Proton is handed over
Change another important feature of membrane cell and be that it both can be using clean energy resource such as hydrogen etc. as fuel, also can be with renewable
Small organic molecule such as formic acid, ethanol, methanol etc. be fuel.Shown according to research before, Pt catalyst is proton exchange
The best catalyst of catalytic performance in membrane cell, but the high cost of Pt catalyst and utilization rate are to a certain extent
The application prospect of fuel cell is limited, therefore prepares the catalyst that electrocatalysis characteristic is improved for improving as current urgent
Cut urgent problem.
The content of the invention
For above-mentioned technical problem, the present invention solves current Pt nano-structured calalysts and is poisoned in the presence of easy, short life,
The technical problems such as price is high and the methanol fuel cell catalyst catalytic activity of prior art is low, prepare a kind of high density
The coarse shape of octahedron PtCoFe alloy nano particles of active sites, improve the methanol electro-catalysis of Pt base nano-structured calalysts
Performance.
To achieve the above object, the present invention is achieved by the following technical solutions:
Methanol fuel cell electrooxidation activity method of testing:Anodic oxidation performance test is using three conventional electrode bodies
System, carries out on CHI650D type electrochemical workstations, is a platinum filament to electrode using saturated calomel electrode as reference electrode,
And working electrode is a diameter of 3mm glass-carbon electrode, a certain amount of coarse shape of octahedron PtCoFe alloy nano catalyst is taken to hang
Supernatant liquid is dripped on the surface of glass-carbon electrode electrode and dried under infrared lamp, then has one end of sample opposite working electrode drop
UV ozone lamp is separated by 5mm and irradiates 12h to remove the organic molecule of sample surfaces, then in the drop of the surface of working electrode
The Nafion solution of 1.5 μ L 0.5wt% ethanol dilution, catalyst electrochemical activation area are tested with 0.5M H2SO4Solution is made
For electrolyte, first logical 30min high-purity N before experiment2To electrolyte deoxygenation, cyclic voltammetric is then carried out with 50mV/s speed and swept
Retouch, the scanning range of setting is -0.24~1.0V, and it is N that superjacent is kept in experimentation2Atmosphere, methanol electro-oxidizing are surveyed
Examination is in 0.5M H2SO4+2M CH3Carried out in OH electrolyte, before cyclic voltammetry, lead to high-purity N2Purging 30min is used for
The dissolved oxygen in electrolyte is removed, for the scanning range set as -0.2~1.0V, it is 50mV/s to determine sweep speed, and electric current is close
Degree represents that each working electrode is with 50mV/s speed with the electric current on working electrode on unit catalyst electrochemical activation area
The cyclic voltammetry curve for the stabilization that the circle of rate scan round processing 50 obtains, and a kind of coarse octahedra PtCoFe alloy nanoparticles
The experimental procedure of sub- preparation method is as follows:
The chloroplatinic acid aqueous solution that 1.0mL concentration is 19.3mmol/L is measured, 4.0mL concentration is 1.66mmol/L chlorination
The cobalt aqueous solution and 3.0mL concentration be 1.66mmol/L ferric chloride aqueous solutionses in 30ml reactors, be subsequently added into glycine
With lauryl sodium sulfate SDS and NaI, dissolving is stirred with magnetic stirring apparatus, then with empty in oxygen discharge reactor
After gas, 1.0MPa oxygen is passed through into reactor, then heating is reacted, reaction terminate after by ethanol centrifuge washing, cold
The processing step such as dry is freezed, obtains coarse octahedra PtCoFe alloy nano particles.
Preferably, SDS amount ranges are 200-250mg, preferably 220mg.
Preferably, the amount ranges of glycine are 100-130mg, preferably 120mg.
Wherein:Glycine plays a part of reducing agent and Morphological control agent, and SDS effect is mainly pattern protective agent, and
Na+Ion and I-Formation of the ratio of ion to PtCoFe crystal topologies has guide effect, the only addition as NaI
In the case of for SDS addition half, the coarse octahedra PtCoFe alloy nano particles of the present invention can be just obtained, synthesis exists
Reach unexpected technique effect together.
Preferably, the temperature range of heating response is 200-210 DEG C.
Further, it should be noted that 1.0MPa hydrogen atmosphere is also the coarse octahedron of the synthesis present invention under primary condition
The essential factor of PtCoFe alloy nano particles, because oxygen has oxidisability, the present invention forms gaseous oxidation-liquid
Phase reduction system, it is used for synthesizing PtCoFe alloys first, and gaseous oxidation is tended to preferentially reduce metal on octahedral structure face
So as to form coarse structure, the specific atmosphere of the present invention forms the entirety of a mutual cooperation, association with other experiment parameters
With the coarse octahedra PtCoFe alloys that can just obtain the present invention together.
Beneficial effects of the present invention:The coarse octahedra PtCoFe nanocatalysts being prepared, with chloroplatinic acid, chlorination
Cobalt and ferric trichloride are raw material, using glycine as reducing agent and protective agent, using specific SDS and NaI additions, in oxygen
The higher coarse shape of octahedron PtCoFe alloy nano particles of selectivity, method green cleaning are prepared under atmosphere.
And the catalyst step atom of synthesis is more, active site density is high, and methanol electro-oxidizing test is in 0.5M 0.5M H2SO4+2M
CH3Cyclic voltammetry is carried out in OH electrolyte, shows that excellent electricity is urged in the experiment of methanol fuel cell electro-oxidizing-catalyzing
Change activity, be with a wide range of applications.
Brief description of the drawings
Fig. 1 is the TEM collection of illustrative plates for the coarse octahedra PtCoFe alloy nano particles that embodiment 1 is prepared;
Fig. 2 is that the first vegetarian noodles for the coarse octahedra PtCoFe alloy nano particles that embodiment 1 is prepared sweeps collection of illustrative plates;
Fig. 3 is the coarse octahedra PtCoFe alloy nano particles that embodiment 1 is prepared and business Pt/C as methanol
The cyclic voltammetry curve comparison diagram of electro-oxidizing-catalyzing agent;
Fig. 4 is the TEM collection of illustrative plates for the PtCoFe alloy nano particles that comparative example 1 is prepared.
Fig. 5 is the TEM collection of illustrative plates for the PtCoFe alloy nano particles that comparative example 2 is prepared.
Embodiment
The implementation of technical solution of the present invention and possessed beneficial effect are described in detail below by way of specific embodiment, but
It cannot be assumed that for the present invention can practical range any restriction.
Embodiment 1
Measure 1.0mL chloroplatinic acids (19.3mmol/L), cobalt chloride solution that 4.0mL concentration is 1.66mmol/L and
3.0mL concentration be 1.66mmol/L ferric chloride aqueous solutionses in 30ml reactors, be subsequently added into glycine and dodecyl
Sodium sulphate SDS and NaI, dissolving is stirred with magnetic stirring apparatus, then with oxygen discharge reactor after air, to anti-
Answer and 1.0MPa oxygen be passed through in kettle, then heat and reacted at 210 DEG C, reaction terminate after by ethanol centrifuge washing, cold
The processing step such as dry is freezed, obtains coarse octahedra PtCoFe alloy nano particles (as shown in Figure 1-2), wherein, glycine
Dosage is 120mg, and SDS amount ranges are 220mg, and NaI addition is 110mg.
Methanol electro-oxidizing is tested:Anodic oxidation performance test is using conventional three-electrode system, in CHI650D types electricity
Carried out on chem workstation.It is a platinum filament to electrode with saturated calomel electrode (SCE) for reference electrode, and working electrode is
A diameter of 3mm glass-carbon electrode (GC).A certain amount of catalyst suspension (holding metal quality is 4 μ g) is taken to drip to GC electrodes
Dried on surface under infrared lamp, working electrode drop then is had into one end of sample, and against UV ozone lamp, (launch wavelength is
185nm and 254nm, power 10W) it is separated by 5mm irradiation 12h to remove the organic molecule of sample surfaces.Then in work electricity
Drip upper 1.5 μ L 0.5wt%Nafion solution (ethanol dilution) in the surface of pole.Catalyst electrochemical activation area test with
0.5M H2SO4Solution is as electrolyte, first logical 30min high-purity N before experiment2To electrolyte deoxygenation, then with 50 mV/s speed
Cyclic voltammetric (CV) scanning is carried out, the scanning range of setting is -0.24~1.0V.It is N that superjacent is kept in experimentation2
Atmosphere.Methanol electro-oxidizing test is in 0.5M H2SO4Carried out in+2M CH3OH electrolyte, before CV tests, lead to high-purity N2Blow
Sweep 30min to be used for removing the dissolved oxygen in electrolyte, the scanning range set determines that sweep speed is as -0.2~1.0V
50mV/s.Current density is with unit catalyst electrochemical activation area (cm on working electrode2) on electric current represent.Each work
Make the CV curves that electrode encloses obtained stabilization with 50mV/s rate loop scan process 50.Coarse eight are prepared for embodiment 1
Face body PtCoFe nano-particles, its current density that peak is normalized on electrochemical surface area ECSA of just sweeping represent catalysis
The size of the latent active of agent, from figure 3, it can be seen that coarse octahedra PtCoFe nano-particles in methanol electro-oxidizing most
High current density is 3.85mA cm-2, the methanol highest current density far above commercial Pt/C is 0.47mA cm-2。
Comparative example 1
Measure 1.0mL chloroplatinic acids (19.3mmol/L), cobalt chloride solution that 4.0mL concentration is 1.66mmol/L and
3.0mL concentration be 1.66mmol/L ferric chloride aqueous solutionses in 30ml reactors, be subsequently added into 120mg glycine and
220mg lauryl sodium sulfate SDS and 100mgNaI, dissolving is stirred with magnetic stirring apparatus, is then discharged with oxygen anti-
Answer in kettle after air, 1.0MPa oxygen is passed through into reactor, then heat and reacted at 210 DEG C, reaction passes through after terminating
Cross the processing steps such as ethanol centrifuge washing, freeze-drying, obtain PtCoFe alloy nano particles (as shown in Figure 5), and using with
The identical test condition of embodiment 1, it is 1.59mA cm to obtain its highest current density in methanol electro-oxidizing-2。
Comparative example 2
Measure 1.0mL chloroplatinic acids (19.3mmol/L), cobalt chloride solution that 4.0mL concentration is 1.66mmol/L and
3.0mL concentration be 1.66mmol/L ferric chloride aqueous solutionses in 30ml reactors, be subsequently added into 120mg glycine and
220mg lauryl sodium sulfate SDS and 110mgNaI, dissolving is stirred with magnetic stirring apparatus, is then discharged with hydrogen anti-
Answer in kettle after air, 1.0MPa hydrogen is passed through into reactor, then heat and reacted at 210 DEG C, reaction passes through after terminating
Cross the processing steps such as ethanol centrifuge washing, freeze-drying, obtain PtCoFe alloy nano particles (as shown in Figure 5), and using with
The identical test condition of embodiment 1, it is 1.68mA cm to obtain its highest current density in methanol electro-oxidizing-2。
Moreover, it relates to arrive multigroup comparative example, in view of length will not enumerate, embodiment 1 is respectively relative to
Change one or more parametric variables, be as a result shown in the case of changing one or more variable and cannot get this
Invention coarse shape of octahedron PtCoFe alloy nano particles, show the application each technical characteristic of technical scheme it
Between have synergy, and methanol electro-oxidizing-catalyzing activity be respectively less than 2.2mA cm-2, far below the catalysis of the embodiment of the present invention 1
Activity, shows no matter the technical scheme of the application has reached unexpected skill for alloy pattern or catalytic activity
Art effect.
Claims (5)
1. a kind of implementation method for being used to improve methanol fuel cell electrooxidation activity, is concretely comprised the following steps:
Methanol fuel cell electrooxidation activity method of testing:Anodic oxidation performance test uses conventional three-electrode system,
Carried out on CHI650D type electrochemical workstations, be a platinum filament to electrode using saturated calomel electrode as reference electrode, and worked
Electrode is a diameter of 3mm glass-carbon electrode, takes a certain amount of coarse shape of octahedron PtCoFe alloy nanos catalyst suspension drop
Dried on to the surface of glass-carbon electrode under infrared lamp, working electrode drop is then had into one end of sample against UV ozone lamp phase
12h is irradiated to remove the organic molecule of sample surfaces every 5mm, and 1.5 μ L 0.5wt% is then dripped on the surface of working electrode
The Nafion solution of ethanol dilution, catalyst electrochemical activation area are tested with 0.5M H2SO4Solution is as electrolyte, before experiment
First lead to 30min high-purity N2To electrolyte deoxygenation, cyclic voltammetry scan, the scanning range of setting are then carried out with 50mV/s speed
It is -0.24~1.0V, it is N that superjacent is kept in experimentation2Atmosphere, methanol electro-oxidizing test is in 0.5M H2SO4+2M
CH3Carried out in OH electrolyte, before cyclic voltammetry, lead to high-purity N2Purging 30min is used for removing the dissolved oxygen in electrolyte,
For the scanning range set as -0.2~1.0V, it is 50mV/s to determine sweep speed, and current density is catalyzed with unit on working electrode
Electric current on agent electrochemical activation area represents that each working electrode encloses what is obtained with 50mV/s rate loop scan process 50
Stable cyclic voltammetry curve, it is characterised in that:The preparation method of the coarse PtCoFe alloy nanos catalyst is:Measure
1.0mL concentration be 19.3mmol/L chloroplatinic acid aqueous solution, 4.0mL concentration be 1.66mmol/L cobalt chloride solution and
3.0mL concentration be 1.66mmol/L ferric chloride aqueous solutionses in 30ml reactors, be subsequently added into glycine and dodecyl
Sodium sulphate SDS and NaI, dissolving is stirred with magnetic stirring apparatus, is then discharged with oxygen in reactor after air, to reaction
1.0MPa oxygen is passed through in kettle, then heating is reacted, and reaction is handled after terminating by ethanol centrifuge washing, freeze-drying etc.
Step, obtain coarse octahedra PtCoFe alloy nano particles.
A kind of 2. implementation method for being used to improve methanol fuel cell electrooxidation activity described in claim 1, it is characterised in that:
SDS amount ranges are 200-250mg, preferably 220mg.
3. a kind of implementation method for being used to improve methanol fuel cell electrooxidation activity described in claim 1-2, its feature exist
In:The amount ranges of glycine are 100-130mg, preferably 120mg.
4. a kind of implementation method for being used to improve methanol fuel cell electrooxidation activity described in claim 1-3, its feature exist
In:NaI addition is SDS half dosage.
5. a kind of implementation method for being used to improve methanol fuel cell electrooxidation activity described in claim 1-4, its feature exist
In:The temperature range of heating response is 200-210 DEG C.
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Cited By (1)
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