CN107845815B - It is a kind of for improving the implementation method of methanol fuel cell electrooxidation activity - Google Patents
It is a kind of for improving the implementation method of methanol fuel cell electrooxidation activity Download PDFInfo
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Abstract
The present invention relates to a kind of for improving the implementation method of 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 octahedron 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 is added, the higher coarse shape of octahedron PtCoFe alloy nano particle of selectivity, the cleaning of preparation method green is prepared.The coarse octahedron PtCoFe alloy nano particle 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 fields.Specifically, the present invention is using the coarse octahedral bodily form
Looks PtCoFe alloy nano particle improves catalysis oxidation methanol fuel cell electroxidation performance.
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 report for preparing PtCoFe alloy nanoparticle submethod at present is less, and these 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
The technical problems such as lattice are high and the methanol fuel cell catalyst catalytic activity of the prior art is low, prepare a kind of high density active
The coarse shape of octahedron PtCoFe alloy nano particle of position improves the methanol electrocatalysis characteristic of Pt base nano-structured calalyst.
To achieve the above object, the present invention is achieved by the following technical solutions:
Methanol fuel cell electrooxidation activity test method: anodic oxidation performance test is using three conventional electrode bodies
System, carries out on CHI650D type electrochemical workstation, is a platinum filament to electrode using saturated calomel electrode as reference electrode, and
Working electrode is the glass-carbon electrode that diameter is 3mm, and a certain amount of coarse shape of octahedron PtCoFe alloy nano catalyst is taken to suspend
It is dry under infrared lamp on drop to the surface of glass-carbon electrode electrode, working electrode drop then there is into one end of sample against ultraviolet
Ozone lamp is separated by 5mm irradiation 12h to remove the organic molecule of sample surfaces, then drips upper 1.5 μ L on the surface of working electrode
The diluted Nafion solution of 0.5wt% ethyl alcohol, catalyst electrochemical activation area test with 0.5M H2SO4Solution is as electrolysis
Matter first leads to the high-purity N of 30min before experiment2To electrolyte deoxygenation, cyclic voltammetry scan, setting are then carried out with 50mV/s rate
Scanning range be -0.24~1.0V, it is N that superjacent is kept in experimentation2Atmosphere, methanol electro-oxidizing test is in 0.5M
H2SO4+2M CH3It is carried out in OH electrolyte, before cyclic voltammetry, leads to high-purity N2Purging 30min is used to remove in electrolyte
Dissolved oxygen, the scanning range set as -0.2~1.0V, determine scanning speed be 50mV/s, current density is on working electrode
Electric current on unit catalyst electrochemical activation area indicates that each working electrode is with the rate loop scan process 50 of 50mV/s
Obtained stable cyclic voltammetry curve is enclosed, and a kind of experiment of coarse octahedron PtCoFe alloy nano particle preparation method walks
It is rapid 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+The ratio of ion and I- 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: the coarse octahedron PtCoFe nanocatalyst being prepared, with chloroplatinic acid, cobalt chloride
It is raw material with ferric trichloride, using glycine as reducing agent and protective agent, using specific SDS and NaI additional amount, in oxygen atmosphere
The higher coarse shape of octahedron PtCoFe alloy nano particle of selectivity, the cleaning of method green are prepared under environment.And it closes
At catalyst step atom it is more, active site density is high, and methanol electro-oxidizing test is in 0.5M 0.5M H2SO4+2M CH3OH electricity
Xie Zhizhong carries out cyclic voltammetry, shows excellent electro catalytic activity in the experiment of methanol fuel cell electro-oxidizing-catalyzing,
It 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 methanol
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 the ferric chloride aqueous solutions of 1.66mmol/L in 30ml reaction kettle, is subsequently added into glycine and dodecyl
Sodium sulphate SDS and NaI are stirred dissolution with magnetic stirring apparatus, are then discharged in reaction kettle after air with oxygen, Xiang Fanying
It is passed through 1.0MPa oxygen in kettle, then heats and is reacted at 210 DEG C, after reaction by ethyl alcohol centrifuge washing, freezing
The processing steps such as dry, obtain coarse octahedron PtCoFe alloy nano particle (as shown in Figs. 1-2), wherein the use of glycine
Amount is 120mg, and the amount ranges of SDS are 220mg, and the additional amount of NaI is 110mg.
Methanol electro-oxidizing test: 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 surface of GC electrode
On it is dry under infrared lamp, then by working electrode drop have one end of sample against UV ozone lamp (launch wavelength be 185nm and
254nm, power 10W) it is separated by 5mm irradiation 12h to remove the organic molecule of sample surfaces.Then on the surface of working electrode
Drip the 0.5wt%Nafion solution (ethyl alcohol dilution) of upper 1.5 μ L.Catalyst electrochemical activation area is tested with 0.5M H2SO4It is molten
Liquid first leads to the high-purity N of 30min as electrolyte before experiment2To electrolyte deoxygenation, cyclic voltammetric is then carried out with 50mV/s rate
(CV) it scans, the scanning range of setting is -0.24~1.0V.It is N that superjacent is kept in experimentation2Atmosphere.Methanol electricity oxygen
Changing test is in 0.5M H2SO4It is carried out in+2M CH3OH electrolyte, before CV test, leads to high-purity N2Purging 30min is used to remove
Dissolved oxygen in electrolyte, the scanning range set determine that scanning speed is 50mV/s as -0.2~1.0V.Current density is with work
Make unit catalyst electrochemical activation area (cm on electrode2) on electric current indicate.Each working electrode is with the rate of 50mV/s
The stable CV curve that 50 circle of scan round processing obtains.Prepared by coarse octahedron PtCoFe nanoparticle for embodiment 1, it
The size just swept the current density that peak is normalized on electrochemical surface area ECSA and represent the latent active of catalyst, from figure
3 as can be seen that highest current density of the coarse octahedron PtCoFe nanoparticle in methanol electro-oxidizing is 3.85mA cm-2, far
Methanol highest current density higher than commercial Pt/C is 0.47mA 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 Figure 4), and using with
The identical test condition of embodiment 1, obtaining its highest current density in methanol electro-oxidizing is 1.59mA 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 Figure 5), and using with
The identical test condition of embodiment 1, obtaining its highest current density in methanol electro-oxidizing is 1.68mA 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 and has
There is synergistic effect, and methanol electro-oxidizing-catalyzing activity is respectively less than 2.2mA cm-2, far below the catalytic activity of the embodiment of the present invention 1,
Show no matter the technical solution of the application has reached unexpected technical effect for alloy pattern or catalytic activity.
Claims (4)
1. a kind of for improving the implementation method of methanol fuel cell electrooxidation activity, specific steps are as follows:
Methanol fuel cell electrooxidation activity test method: anodic oxidation performance test uses conventional three-electrode system,
It is carried out on CHI650D type electrochemical workstation, is a platinum filament to electrode using saturated calomel electrode as reference electrode, and worked
Electrode is the glass-carbon electrode that diameter is 3mm, takes a certain amount of coarse shape of octahedron PtCoFe alloy nano catalyst suspension drop
It is dry under infrared lamp on to the surface of glass-carbon electrode, then there is one end of sample against UV ozone lamp phase working electrode drop
12h is irradiated to remove the organic molecule of sample surfaces every 5mm, and the 0.5wt% of upper 1.5 μ L is then dripped on the surface of working electrode
The diluted Nafion solution of ethyl alcohol, catalyst electrochemical activation area are tested with 0.5M H2SO4Solution is as electrolyte, before experiment
First lead to the high-purity N of 30min2To electrolyte deoxygenation, cyclic voltammetry scan, the scanning range of setting are then carried out with 50mV/s rate
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
CH3It is carried out in OH 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, it is characterised in that: the preparation method of the coarse octahedron PtCoFe alloy nano catalyst exists
In: the chloroplatinic acid aqueous solution that 1.0mL concentration is 19.3mmol/L is measured, 4.0mL concentration is that the cobalt chloride of 1.66mmol/L is water-soluble
The ferric chloride aqueous solutions that liquid and 3.0mL concentration are 1.66mmol/L are subsequently added into the sweet ammonia of 100-130mg in 30ml reaction kettle
Acid and 200-250mg lauryl sodium sulfate SDS and NaI, the additional amount of NaI are the half dosage of SDS, use magnetic stirring apparatus
Be stirred dissolution, then with after air, 1.0MPa oxygen is passed through into reaction kettle in oxygen discharge reaction kettle, then heat into
Row reaction, passes through ethyl alcohol centrifuge washing, freeze-drying process step after reaction, obtains coarse octahedron PtCoFe alloy and receive
Rice corpuscles.
2. according to claim 1 a kind of for improving the implementation method of methanol fuel cell electrooxidation activity, feature
Be: the dosage of SDS is 220mg.
3. it is according to claim 1 or 2 a kind of for improving the implementation method of methanol fuel cell electrooxidation activity, it is special
Sign is: the dosage of glycine is 120mg.
4. it is according to claim 1 or 2 a kind of for improving the implementation method of methanol fuel cell electrooxidation activity, it is special
Sign is: the temperature range for heating reaction is 200-210 DEG C.
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Granted publication date: 20190809 Termination date: 20211023 |