CN107845817A - A kind of method using coarse shape of octahedron PtCoFe nanocatalysts catalysis oxidation formic acid electrochemistry - Google Patents
A kind of method using coarse shape of octahedron PtCoFe nanocatalysts catalysis oxidation formic acid electrochemistry Download PDFInfo
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- CN107845817A CN107845817A CN201710990652.8A CN201710990652A CN107845817A CN 107845817 A CN107845817 A CN 107845817A CN 201710990652 A CN201710990652 A CN 201710990652A CN 107845817 A CN107845817 A CN 107845817A
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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; add the CTAB and NaBr of certain content; the higher coarse shape of octahedron PtCoFe nanocatalysts of selectivity, preparation method green cleaning are prepared under oxygen atmosphere.The coarse shape of octahedron PtCoFe alloy catalysts 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 field.Specifically, the present invention is to prepare one kind slightly using hydrothermal synthesis method
Rough shape of octahedron PtCoFe alloy nano particles.
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.The method for preparing PtCoFe alloy nano particles at present is less, and these preparation 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,
Price is high and the more low technical problem of the catalyst activity of prior art, prepares a kind of the thick of high density active position
Rough shape of octahedron PtCoFe alloy nano particles, improve the catalytic performance of the formic acid electroxidation of Pt base nano-structured calalysts.
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
Carried out on type electrochemical workstation, be 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 suspensions are taken to drip to glass carbon
Dried on the surface of electrode under infrared lamp, one end that working electrode drop has sample is then separated by 5mm against UV ozone lamp
12h is irradiated to remove the organic molecule of sample surfaces, and 1.5 μ L 0.5wt% ethanol is then dripped on the surface of working electrode
The Nafion solution of dilution, catalyst electrochemical activation area are tested with 0.5M H2SO4Solution is first before experiment as electrolyte
Logical 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, the test of formic acid electroxidation is in 0.5M H2SO4+
Carried out in 0.25M HCOOH electrolyte, before cyclic voltammetry, lead to high-purity N230 min are purged to be used for removing in electrolyte
Dissolved oxygen, the scanning range set is -0.2~1.0V, and it is 50mV/s to determine sweep speed, and current density is with working electrode
Electric current on unit catalyst electrochemical activation area represents that each working electrode is with 50mV/s rate loop scan process
The cyclic voltammetry curve for the stabilization that 50 circles obtain, and a kind of reality of coarse octahedra PtCoFe alloy nano particles preparation method
It is as follows to test step：
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：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, add certain content CTAB and
NaBr, the higher coarse shape of octahedron PtCoFe nanocatalysts of selectivity, preparation method are prepared under oxygen atmosphere
Green cleaning.The coarse shape of octahedron PtCoFe alloy catalysts 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+0.25 M HCOOH electrolyte, is urged in formic acid electroxidation
Change in experiment and show excellent electro catalytic 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 formic acid
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 is in 1.66mmol/L ferric chloride aqueous solutionses 30ml reactors, is subsequently added into glycine and dodecyl sulphur
Sour sodium 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 heats and is reacted at 210 DEG C, is reacted after terminating by ethanol centrifuge washing, freezing
The processing step such as dry, obtains coarse octahedra PtCoFe alloy nano particles (as shown in Figure 1-2), wherein, the use of glycine
Measure as 120mg, SDS amount ranges are 220mg, and NaI addition is 110mg.
Formic acid electroxidation 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.The test of formic acid electroxidation is in 0.5M H2SO4Carried out in+0.25M HCOOH electrolyte, before CV tests, lead to high-purity N2
Purging 30min is used for removing the dissolved oxygen in electrolyte, and 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.Prepared for embodiment 1 coarse
Octahedra PtCoFe nano-particles, its current density that peak is normalized on electrochemical surface area ECSA of just sweeping are represented and urged
The size of the latent active of agent, from figs. 3 and 4 it can be seen that coarse octahedra PtCoFe nano-particles are in formic acid electroxidation
Highest current density in experiment is 0.83mA cm-2, the formic acid highest current density far above commercial Pt/C is 0.24mA
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 0.44mA cm to obtain it in the highest current density in the experiment of formic acid electroxidation-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 0.35mA cm to obtain its highest current density in the experiment of formic acid electroxidation-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 formic acid electro-oxidizing-catalyzing activity be respectively less than 0.5mA 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 method using coarse shape of octahedron PtCoFe nanocatalysts catalysis oxidation formic acid electrochemistry, specific steps
For：
Formic acid electrochemical test method：Anodic oxidation performance test is using conventional three-electrode system, in CHI650D types electrification
Learn and carried out on work station, be 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 suspensions are taken to drip to glass-carbon electrode
Dried on surface under infrared lamp, one end that working electrode drop is then had to sample is separated by 5mm irradiations 12h against UV ozone lamp
To remove the organic molecule of sample surfaces, the then 1.5 μ L 0.5wt% ethanol dilution in the drop of the surface of working electrode
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 speed, 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 for removing the dissolved oxygen in electrolyte, setting
Scanning range is -0.2~1.0V, and it is 50mV/s to determine sweep speed, and current density is with unit catalyst electrification on working electrode
The electric current learned on active area represents that each working electrode encloses obtained stabilization with 50mV/s rate loop scan process 50
Cyclic voltammetry curve, it is characterised in that：The preparation method of the coarse shape of octahedron PtCoFe alloy nano catalyst 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 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.
2. one kind described in claim 1 uses coarse shape of octahedron PtCoFe nanocatalysts catalysis oxidation formic acid electrochemistry
Method, it is characterised in that：SDS amount ranges are 200-250mg, preferably 220mg.
3. one kind described in claim 1-2 is using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidations formic acid electrification
Method, it is characterised in that：The amount ranges of glycine are 100-130mg, preferably 120mg.
4. one kind described in claim 1-3 is using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidations formic acid electrification
Method, it is characterised in that：NaI addition is SDS half dosage.
5. one kind described in claim 1-4 is using coarse shape of octahedron PtCoFe nanocatalyst catalysis oxidations formic acid electrification
Method, it is characterised in that：The temperature range of heating response 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 |
| CN111230141A (en) * | 2020-03-04 | 2020-06-05 | 王冲 | Preparation method of PtRuCoS alloy nanocrystalline with floccule morphology |
| CN111318720A (en) * | 2020-03-04 | 2020-06-23 | 王冲 | Cubic PtCoS alloy nano-particles and preparation method thereof |
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| CN111318720A (en) * | 2020-03-04 | 2020-06-23 | 王冲 | Cubic PtCoS alloy nano-particles and preparation method thereof |
| CN111230141B (en) * | 2020-03-04 | 2022-10-25 | 王冲 | Preparation method of PtRuCoS alloy nanocrystalline with floccule morphology |
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| CN107845817B (en) | 2019-06-21 |
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