CN107845817B - A method of using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidation formic acid electrochemistry - Google Patents
A method of using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidation formic acid electrochemistry Download PDFInfo
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- CN107845817B CN107845817B CN201710990652.8A CN201710990652A CN107845817B CN 107845817 B CN107845817 B CN 107845817B CN 201710990652 A CN201710990652 A CN 201710990652A CN 107845817 B CN107845817 B CN 107845817B
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- 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
- H01M4/928—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
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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 coarse shape of octahedron PtCoFe nanocatalysts and its formic acid electrocatalysis characteristic to study.Using the coarse shape of octahedron PtCoFe being prepared as catalyst; catalyst preparation is with chloroplatinic acid; cobalt chloride and ferric trichloride are raw material; using PVP as reducing agent and protective agent; the CTAB and NaBr of certain content is added; the higher coarse shape of octahedron PtCoFe nanocatalyst of selectivity, the cleaning of preparation method green are prepared under oxygen atmosphere.The coarse shape of octahedron PtCoFe alloy catalyst particle step atom obtained is more, and active site density is high, and the test of formic acid electroxidation is in 0.5M H2SO4Cyclic voltammetry is carried out in+0.25M HCOOH electrolyte, excellent electro catalytic activity is shown in the experiment of formic acid electro-oxidizing-catalyzing, is with a wide range of applications.
Description
Technical field
The invention belongs to function nano alloy fields.Specifically, the present invention is that one kind is prepared using hydrothermal synthesis method slightly
Rough shape of octahedron PtCoFe alloy nano particle.
Background technique
Precious metals pt nano-structured calalyst is widely used in industry due to its excellent catalytic performance and thermal stability
Catalysis, bionic, the fields such as electro-catalysis.But due to some restraining factors in practical applications, such as easily poisoning, the service life it is short with
And it is at high price, so that this excellent nanocatalyst can not further genralrlization and application.Research worker is in order to solve this
A little problems substitute Pt frequently with by cheap 3d transition metal element part at present, form Pt base binary/multicomponent alloy and urge
Agent, and controlled by condition, probe into its pattern, the relationship of composition and stable in catalytic performance.
In numerous transition metal elements, Co and Fe respectively as one of transition metal element more abundant on the earth,
It is that Pt base bianry alloy preferably selects.The method for preparing PtCoFe alloy nano particle at present is less, and these preparation methods
It is all organic solvent macromolecular as solvent, most of PtCoFe alloy nano particle being synthesized is wrapped up by organic matter, living
Property position cannot expose, and can not be in contact with reactant.Therefore it designs and exploitation aqueous solution preparation PtCoFe alloy nano particle has
There is important meaning.A kind of method for preparing coarse octahedron PtCoFe alloy nano particle that the present invention develops, greatly improves
The step atomicity of Pt, increases the active site density of PtCoFe alloy.
Fuel cell is considered as the important power device of traditional internal combustion engine alternative in the near future.Proton exchange
Another important feature of membrane cell is that it both can be using clean energy resource such as hydrogen etc. as fuel, also can be with reproducible small
Molecular organic such as formic acid, ethyl alcohol, methanol etc. is fuel.According to before studies have shown that Pt catalyst is proton exchange membrane combustion
Expect the best catalyst of catalytic performance in battery, but the high cost and utilization rate of Pt catalyst limits to a certain extent
The application prospect of fuel cell, therefore prepare to be used to improve the catalyst for improving electrocatalysis characteristic and have become and be currently urgently badly in need of solving
Certainly the problem of.
Summary of the invention
In view of the above technical problems, the present invention solves current Pt nano-structured calalyst and there is easily poisoning, and the service life is short, valence
Lattice are high and the more low technical problem of catalyst activity of the prior art, prepare coarse the eight of a kind of high density active position
Face bodily form looks PtCoFe alloy nano particle improves the catalytic performance of the formic acid electroxidation of Pt base nano-structured calalyst.
To achieve the above object, the present invention is achieved by the following technical solutions:
Formic acid electrochemical test method: anodic oxidation performance test is using conventional three-electrode system, in CHI650D type
It is carried out on electrochemical workstation, is a platinum filament to electrode using saturated calomel electrode as reference electrode, and working electrode is diameter
For the glass-carbon electrode of 3mm, a certain amount of coarse shape of octahedron PtCoFe alloy nano catalyst suspension is taken to drip to glass-carbon electrode
Surface on it is dry under infrared lamp, then there is one end of sample to be separated by 5mm irradiation against UV ozone lamp working electrode drop
Then 12h is diluted with removing the organic molecules of sample surfaces in the 0.5wt% ethyl alcohol that upper 1.5 μ L is dripped on the surface of working electrode
Nafion solution, catalyst electrochemical activation area test with 0.5M H2SO4Solution first leads to before experiment as electrolyte
The high-purity N of 30min2To electrolyte deoxygenation, cyclic voltammetry scan is then carried out with 50mV/s rate, the scanning range of setting is-
0.24~1.0V, it is N that superjacent is kept in experimentation2Atmosphere, the test of formic acid electroxidation is in 0.5M H2SO4+0.25M
It is carried out in HCOOH electrolyte, before cyclic voltammetry, leads to high-purity N2Purging 30min is used to remove the dissolved oxygen in electrolyte,
The scanning range set determines that scanning speed is 50mV/s, current density is catalyzed with unit on working electrode as -0.2~1.0V
Electric current on agent electrochemical activation area indicates that each working electrode is obtained with the circle of rate loop scan process 50 of 50mV/s
Stable cyclic voltammetry curve, and a kind of experimental procedure of coarse octahedron PtCoFe alloy nano particle preparation method is as follows:
The chloroplatinic acid aqueous solution that 1.0mL concentration is 19.3mmol/L is measured, 4.0mL concentration is the cobalt chloride of 1.66mmol/L
Aqueous solution and 3.0mL concentration are the ferric chloride aqueous solutions of 1.66mmol/L in 30ml reaction kettle, be subsequently added into glycine and
Lauryl sodium sulfate SDS and NaI are stirred dissolution with magnetic stirring apparatus, then with air in oxygen discharge reaction kettle
Afterwards, 1.0MPa oxygen is passed through into reaction kettle, then heating is reacted, after reaction by ethyl alcohol centrifuge washing, freezing
The processing steps such as dry, obtain coarse octahedron PtCoFe alloy nano particle.
Preferably, the amount ranges of SDS are 200-250mg, preferably 220mg.
Preferably, the amount ranges of glycine are 100-130mg, preferably 120mg.
Wherein: glycine plays the role of reducing agent and Morphological control agent, and SDS is mainly pattern protective agent, and
Na+Ion and I-The ratio of ion has guiding role to the formation of PtCoFe crystal topology, only when the additional amount of NaI
In the case where for SDS additional amount half, coarse octahedron PtCoFe alloy nano particle of the invention can be just obtained, it is comprehensive one
It rises and reaches unexpected technical effect.
Preferably, the temperature range for heating reaction is 200-210 DEG C.
Further, it should be noted that the oxygen atmosphere of 1.0MPa is also the coarse octahedron of the synthesis present invention under primary condition
The essential factor of PtCoFe alloy nano particle, since oxygen has oxidisability, the present invention constitutes gaseous oxidation-liquid phase
Reduction system is used to synthesize PtCoFe alloy for the first time, and gaseous oxidation tend to preferentially restore on octahedral structure face metal from
And coarse structure is formed, the specific atmosphere of the present invention and other experiment parameters constitute a mutually matched entirety, collaboration
Coarse octahedron PtCoFe alloy of the invention can be just obtained together.
Beneficial effects of the present invention: using the coarse shape of octahedron PtCoFe being prepared as catalyst, catalyst preparation
With chloroplatinic acid, cobalt chloride and ferric trichloride are raw material, using PVP as reducing agent and protective agent, be added the CTAB of certain content with
The higher coarse shape of octahedron PtCoFe nanocatalyst of selectivity, preparation method is prepared in NaBr under oxygen atmosphere
Green cleaning.The coarse shape of octahedron PtCoFe alloy catalyst particle step atom obtained is more, and active site density is high, first
Sour electroxidation test is in 0.5M H2SO4Cyclic voltammetry is carried out in+0.25M HCOOH electrolyte, is urged in formic acid electroxidation
Change in experiment and show excellent electro catalytic activity, is with a wide range of applications.
Detailed description of the invention
Fig. 1 is the TEM map for the coarse octahedron PtCoFe alloy nano particle that embodiment 1 is prepared；
Fig. 2 is that the first vegetarian noodles for the coarse octahedron PtCoFe alloy nano particle that embodiment 1 is prepared sweeps map；
Fig. 3 is the coarse octahedron PtCoFe alloy nano particle that embodiment 1 is prepared and business Pt/C as formic acid
The cyclic voltammetry curve comparison diagram of electro-oxidizing-catalyzing agent；
Fig. 4 is the TEM map for the PtCoFe alloy nano particle that comparative example 1 is prepared.
Fig. 5 is the TEM map for the PtCoFe alloy nano particle that comparative example 2 is prepared.
Specific embodiment
Below by way of the implementation and possessed beneficial effect of specific embodiment the present invention will be described in detail technical solution, but not
It can regard as any restriction to enforceable range of the invention.
Embodiment 1
Measure 1.0mL chloroplatinic acid (19.3mmol/L), 4.0mL concentration be 1.66mmol/L cobalt chloride solution and
3.0mL concentration is to be subsequently added into glycine and dodecyl sulphur in the ferric chloride aqueous solutions 30ml reaction kettle of 1.66mmol/L
Sour sodium SDS and NaI is stirred dissolution with magnetic stirring apparatus, is then discharged with oxygen in reaction kettle after air, to reaction kettle
In be passed through 1.0MPa oxygen, then heat and reacted at 210 DEG C, it is dry by ethyl alcohol centrifuge washing, freezing after reaction
The processing steps such as dry obtain coarse octahedron PtCoFe alloy nano particle (as shown in Figs. 1-2), wherein the dosage of glycine
For 120mg, the amount ranges of SDS are 220mg, and the additional amount of NaI is 110mg.
The test of formic acid electroxidation: anodic oxidation performance test is using conventional three-electrode system, in CHI650D type electrification
It learns and is carried out on work station.It is a platinum filament to electrode with saturated calomel electrode (SCE) for reference electrode, and working electrode is straight
Diameter is the glass-carbon electrode (GC) of 3mm.A certain amount of catalyst suspension (holding metal quality is 4 μ g) is taken to drip to the table of GC electrode
It is dry under infrared lamp on face, then there is one end of sample against UV ozone lamp (launch wavelength 185nm working electrode drop
And 254nm, power 10W) it is separated by 5mm irradiation 12h to remove the organic molecule of sample surfaces.Then in working electrode
Drip the 0.5wt%Nafion solution (ethyl alcohol dilution) of upper 1.5 μ L in surface.Catalyst electrochemical activation area is tested with 0.5M
H2SO4Solution first leads to the high-purity N of 30min as electrolyte before experiment2To electrolyte deoxygenation, then followed with 50mV/s rate
Ring volt-ampere (CV) scanning, the scanning range of setting is -0.24~1.0V.It is N that superjacent is kept in experimentation2Atmosphere.First
Sour electroxidation test is in 0.5M H2SO4It is carried out in+0.25M HCOOH electrolyte, before CV test, leads to high-purity N2Purging
30min is used to remove the dissolved oxygen in electrolyte, and the scanning range set determines that scanning speed is 50mV/ as -0.2~1.0V
s.Current density is with unit catalyst electrochemical activation area (cm on working electrode2) on electric current indicate.Each working electrode
Obtained stable CV curve is enclosed with the rate loop scan process 50 of 50mV/s.Prepared by coarse octahedron for embodiment 1
PtCoFe nanoparticle, its current density that peak is normalized on electrochemical surface area ECSA of just sweeping represent the sheet of catalyst
Active size is levied, from figure 3, it can be seen that highest electricity of the coarse octahedron PtCoFe nanoparticle in the experiment of formic acid electroxidation
Current density is 0.83mA cm-2, the formic acid highest current density much higher than commercial Pt/C is 0.24mA cm-2。
Comparative example 1
Measure 1.0mL chloroplatinic acid (19.3mmol/L), 4.0mL concentration be 1.66mmol/L cobalt chloride solution and
3.0mL concentration be 1.66mmol/L ferric chloride aqueous solutions in 30ml reaction kettle, be subsequently added into 120mg glycine and
220mg lauryl sodium sulfate SDS and 100mgNaI, are stirred dissolution with magnetic stirring apparatus, are then discharged with oxygen anti-
It answers in kettle after air, 1.0MPa oxygen is passed through into reaction kettle, then heat and reacted at 210 DEG C, passed through after reaction
Cross the processing steps such as ethyl alcohol centrifuge washing, freeze-drying, obtain PtCoFe alloy nano particle (as shown in Fig. 4), and using with
The identical test condition of embodiment 1, obtaining it in the highest current density in the experiment of formic acid electroxidation is 0.44mA cm-2。
Comparative example 2
Measure 1.0mL chloroplatinic acid (19.3mmol/L), 4.0mL concentration be 1.66mmol/L cobalt chloride solution and
3.0mL concentration be 1.66mmol/L ferric chloride aqueous solutions in 30ml reaction kettle, be subsequently added into 120mg glycine and
220mg lauryl sodium sulfate SDS and 110mgNaI, are stirred dissolution with magnetic stirring apparatus, are then discharged with hydrogen anti-
It answers in kettle after air, 1.0MPa hydrogen is passed through into reaction kettle, then heat and reacted at 210 DEG C, passed through after reaction
Cross the processing steps such as ethyl alcohol centrifuge washing, freeze-drying, obtain PtCoFe alloy nano particle (as shown in Fig. 5), and using with
The identical test condition of embodiment 1, obtaining its highest current density in the experiment of formic acid electroxidation is 0.35mA cm-2。
Moreover, it relates to arrive multiple groups comparative example, it will not enumerate in view of length, be respectively relative to embodiment 1
Change one or more parametric variables, cannot get this hair in the case where changing one or more variable as the result is shown
Bright coarse shape of octahedron PtCoFe alloy nano particle, shows between each technical characteristic of the technical solution of the application
With synergistic effect, and formic acid electro-oxidizing-catalyzing activity is respectively less than 0.5mA cm-2, living far below the catalysis of the embodiment of the present invention 1
Property, show no matter the technical solution of the application has reached unexpected technology effect for alloy pattern or catalytic activity
Fruit.
Claims (4)
1. a kind of method using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidation formic acid electrochemistry, specific steps
Are as follows:
Formic acid electrochemical test method: anodic oxidation performance test is using conventional three-electrode system, in CHI650D type electrification
It learns and is carried out on work station, be a platinum filament to electrode using saturated calomel electrode as reference electrode, and working electrode is that diameter is
The glass-carbon electrode of 3mm takes a certain amount of coarse shape of octahedron PtCoFe alloy nano catalyst suspension to drip to glass-carbon electrode
It is dry under infrared lamp on surface, then there is one end of sample to be separated by 5mm irradiation 12h against UV ozone lamp working electrode drop
To remove the organic molecule of sample surfaces, the 0.5wt% ethyl alcohol for then dripping upper 1.5 μ L on the surface of working electrode is diluted
Nafion solution, catalyst electrochemical activation area are tested with 0.5M H2SO4Solution first leads to 30min as electrolyte before experiment
High-purity N2To electrolyte deoxygenation, cyclic voltammetry scan is then carried out with 50mV/s rate, the scanning range of setting is -0.24~
1.0V, it is N that superjacent is kept in experimentation2Atmosphere, the test of formic acid electroxidation is in 0.5M H2SO4+ 0.25M HCOOH electricity
Xie Zhizhong is carried out, and before cyclic voltammetry, leads to high-purity N2Purging 30min is used to remove the dissolved oxygen in electrolyte, setting
Scanning range is -0.2~1.0V, determines that scanning speed is 50mV/s, current density is with unit catalyst electrification on working electrode
The electric current learned on active area indicates that each working electrode obtains stable with the circle of rate loop scan process 50 of 50mV/s
Cyclic voltammetry curve, it is characterised in that: the coarse shape of octahedron PtCoFe alloy nano catalyst the preparation method is as follows:
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 solutions in 30ml reaction kettle, be subsequently added into 100-130mg glycine and
200-250mg lauryl sodium sulfate SDS and NaI, the additional amount of NaI are the half dosage of SDS, are carried out with magnetic stirring apparatus
Stirring and dissolving is passed through 1.0MPa oxygen into reaction kettle, then heating carries out anti-then with after air in oxygen discharge reaction kettle
It answers, passes through ethyl alcohol centrifuge washing, freeze-drying process step after reaction, obtain coarse octahedron PtCoFe alloy nanoparticle
Son.
2. described in claim 1 a kind of using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidation formic acid electrochemistry
Method, it is characterised in that: the dosage of SDS be 220mg.
3. of any of claims 1 or 2 a kind of using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidation formic acid electricity
The method of chemistry, it is characterised in that: the dosage of glycine is 120mg.
4. of any of claims 1 or 2 a kind of using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidation formic acid electricity
The method of chemistry, it is characterised in that: the temperature range for heating reaction is 200-210 DEG C.
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| CN110364744A (en) * | 2019-07-23 | 2019-10-22 | 济南大学 | A kind of preparation method of the extra small Pt-Ni-Cu alloy nanoparticle with high miller index surface |
| CN111230141B (en) * | 2020-03-04 | 2022-10-25 | 王冲 | Preparation method of PtRuCoS alloy nanocrystalline with floccule morphology |
| CN111318720B (en) * | 2020-03-04 | 2022-10-25 | 王冲 | Cubic PtCoS alloy nano-particles and preparation method thereof |
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Granted publication date: 20190621 Termination date: 20191023 |