CN106058277A - PdAu electrocatalyst for fuel cell and preparation method thereof - Google Patents
PdAu electrocatalyst for fuel cell and preparation method thereof Download PDFInfo
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- CN106058277A CN106058277A CN201610661170.3A CN201610661170A CN106058277A CN 106058277 A CN106058277 A CN 106058277A CN 201610661170 A CN201610661170 A CN 201610661170A CN 106058277 A CN106058277 A CN 106058277A
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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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- 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
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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
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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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 invention relates to a PdAu electrocatalyst for a fuel cell and a preparation method thereof. The preparation method employs continuous reduction technology and comprises the following steps: dissolving a three-block copolymer P123 in redistilled water, slowly adding a potassium chloropalladate solution into the obtained P123 solution drop by drop while stirring continuously, and carrying out a reaction with temperature controlled to be 20 to 60 DEG C; in 30 to 90 minutes, slowly adding chloroauric acid hexahydrate into a reaction solution drop by drop; after completion of the addition, continuing the reaction for 60 to 240 minutes; and subjecting the reaction solution to centrifugation and washing three to five times so as to obtain the catalyst PdAu for the fuel cell. The three-block copolymer P123 is used as a protective agent and reducing agent; Pd is used as a seed; in virtue of difference between the reduction potential of Pd and Au, a potential replacement reaction is carried out so as to prepare the core-shell-structured catalyst PdAu; and the prepared catalyst has good dispersity, uniform size and shape and excellent electrocatalytic oxidation of methanol, and is a promising catalyst for fuel cells.
Description
Technical field
The invention belongs to field of fuel cell technology, relate to the preparation method of catalyst, especially relate to a kind of fuel
The preparation method of cell catalyst PdAu.
Background technology
Along with social progress and population increase, energy crisis is the most serious.Fossil energy is extensively applied and is not only aggravated the energy
Crisis, but also cause environmental pollution and global warming.Therefore, seek efficiently, cleaning, the new forms of energy of sustainable development obtain with
Transformation technology has become one of top priority solving energy problem.Fuel cell is a kind of by fuel with the chemical energy of oxidant
It is directly changed into the device of electric energy by electrode reaction, is the 4th class generation technology after waterpower, firepower and nuclear energy power generation,
There is the advantages such as fuel variation, aerofluxus is clean, noise is low, environmental pollution is little, be a kind of environmental protection energy.Due to reaction
Process is not related to burning, and therefore, its energy conversion efficiency is not limited by Carnot cycle, and up to 60% ~ 80%, efficiency of actual
It it is 2 ~ 3 times of ordinary internal combustion engine.
Proton Exchange Membrane Fuel Cells (PEMFC) is one of following electric automobile main candidate power supply, wherein direct alcohol
Types of fuel cells (DAFC) is owing to its high power density, fuel source are abundant and easily stored and the advantage such as supply becomes commercialization
First-selection, its cost, Performance And Reliability be largely limited by eelctro-catalyst, understand, study fuel cell electro catalytic mechanism,
Particularly Study of Catalyst structure composition and the relation between the battery performance life-span, have great science and realistic meaning.Pd
Price and reserves all have the biggest advantage relative to Pt.The catalysis activity of Pd and stability can be by being formed with Au, Cu etc.
Alloy improves.Due to difunctional mechanism, the introducing of Au can play promoting catalysis, strengthens the antitoxinization performance of catalyst, carries
The activity of high catalysis oxidation alcohol and stability.By the different incorporation way of Au, the PdAu binary of different-shape can be prepared
Alloy catalyst.
Present invention introduces Au, use simple reduction synthesis process continuously, triblock copolymer P123 is as protective agent and goes back
Former dose, prepare that dispersibility is preferable, regular appearance is homogeneous, there is nucleocapsid structure and possess the PdAu catalysis of preferable electrocatalysis characteristic
Agent.
Summary of the invention
It is an object of the invention to introduce another more stable metal Au by current potential displacement reaction, formed and there is core
The bianry alloy catalyst PdAu of shell structure, by difunctional mechanism and its special structure, improves urging of catalyst further
Change activity and stability.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose used:
The preparation of a kind of fuel-cell catalyst PdAu uses continuous reduction synthesis process, by introducing metal Au, triblock copolymer
Thing P123 as protective agent and reducing agent, prepares that dispersibility is preferable, pattern is homogeneous and possesses the electro catalytic activity of excellence
PdAu catalyst.The method comprises the following steps:
(1) triblock copolymer P123 ultrasonic dissolution is taken in redistilled water；Potassium chloroplatinate is added molten in P123 solution
Liquid, magnetic agitation, temperature controls at 20-60 DEG C, and in mixed solution, triblock copolymer P123 concentration is 10-50 mg/mL.Slow
Slowly dripping potassium chloropalladate, wherein potassium chloropalladate concentration is 0.01-0.05 mmol/L；After reacting 30 minutes, it is slowly added dropwise six hydrations
Gold chloride, wherein six hydration gold chloride concentration are 0.01-0.05 mmol/L, continue reaction 60-240 minute, reaction after dripping
Liquid ultimately becomes black suspension.
(3) by reactant liquor centrifugation under 3000 r/min ~ 10000 r/min, with water and absolute ethanol washing three to
Five times, finally the product after washes clean is added dehydrated alcohol dispersion protection and i.e. obtains fuel cell PdAu catalyst.
More preferably, in the mixed reaction solution of step (1), triblock copolymer P123 concentration is 20 mg/mL, chlorine
Palladium acid potassium concn is 0.03 mmol/L, and hydration gold chloride concentration is 0.03 mmol/L.
In step (1), metal front liquid solution constant pressure funnel is dropwise slowly added to, and drips speed and controls to drip at 5-10 s/.
In step (2), in centrifugal separation processes, first wash 2-3 time with redistilled water, then use absolute ethanol washing 2-
3 times, it is ensured that triblock copolymer P123 and presoma that unreacted is complete completely remove from catalyst surface.
Described fuel-cell catalyst PdAu dispersibility is preferable, and pattern size is homogeneous, and its mean diameter is at 3-15nm.
Described fuel-cell catalyst PdAu electrochemical surface area (ECSA) is 1-100 m2/gPd
In described fuel-cell catalyst PdAu, the atomic percentage conc of Pd is 40%-80%.
A kind of fuel cell PdAu catalyst involved in the present invention and preparation method thereof has a following outstanding feature:
(1) preparation method is continuous reduction, and flow process is simple, easy and simple to handle.
(2) triblock copolymer P123 is simultaneously as protective agent and reducing agent, and environmental protection is pollution-free.
(3) using current potential displacement reaction, utilize the difference of two kinds of metal master oxidation-reduction potentials, both spontaneously send out
Raw redox reaction, can prepare and have nucleocapsid structure and the uniform catalyst of pattern.
(4) by introducing metal Au, both having reduced the consumption of precious metals pd, the alloy as catalyst activity concurrently formed is with stable
Property is more preferable.
(5) due to difunctional mechanism, lattice deformability effect and surface ligand effect, the introducing of Au can be played co-catalysis and make
With, strengthen the antitoxinization performance of catalyst, the activity improving catalysis oxidation alcohol and stability.
(6) catalyst prepared by possesses the electrocatalytic oxidation alcohols performance of excellence, has in direct alcohol fuel cell
Bigger application and development prospect.
Accompanying drawing explanation
Fig. 1: transmission electron microscope Fig. 1 of the fuel-cell catalyst PdAu prepared by embodiment 1.
Fig. 2: transmission electron microscope Fig. 2 of the fuel-cell catalyst PdAu prepared by embodiment 1.
Fig. 3: the cyclic voltammetry curve figure of the fuel-cell catalyst PdAu prepared by embodiment 1.
Fig. 4: the cyclic voltammetry curve of the fuel-cell catalyst PdAu Electrocatalytic Oxidation of Methanol prepared by embodiment 1
Figure.
Fig. 5: the cyclic voltammetry curve comparison diagram of the fuel-cell catalyst PdAu prepared by embodiment 2 and 3.
The cyclic voltammetric of Fig. 6: the fuel-cell catalyst PdAu Electrocatalytic Oxidation of Methanol prepared by embodiment 2 and 3 is bent
Line comparison diagram.
Detailed description of the invention
Below in conjunction with the accompanying drawings and be embodied as case row, the present invention is expanded on further, it should be understood that these embodiments are only used for
The bright present invention rather than restriction the scope of the present invention, after having read the present invention, those skilled in the art are to the present invention's
The amendment of the various equivalent form of values all falls within the application claims limited range.
Embodiment 1
(1) 1.0 g triblock copolymer P123 stirring ultrasonic dissolutions are taken in 50 mL redistilled waters；Magnetic agitation, temperature
Controlling at 30 DEG C, the speed dripped with 5s/ in P123 solution drips 10 mL potassium chloropalladate solution (1.192 mg/mL).
After (2) 30 minutes, the speed dropping 10mL dripped with 5s/ in mixed solution is hydrated gold chloride (1.179 mg/
ML), until mixed solution becomes black and generates precipitation.
(3) the black suspension centrifugation under 10000 r/min that will obtain after reaction, first washes with second distillation
Wash 3 times, then with dehydrated alcohol 3 times, finally the product after washes clean is added dehydrated alcohol dispersion protection and i.e. obtains fuel electricity
Pond PdAu catalyst.
Fig. 1 and Fig. 2 show the present embodiment and prepares transmission electron microscope (TEM) figure of gained fuel cell PdAu catalyst,
By Fig. 1 and Fig. 2 it can be seen that the catalyst preparing gained is good dispersion, pattern size is homogeneous, does not substantially have agglomeration,
The mean diameter of granule is about 7 nm.
The catalyst PdAu that the present embodiment is prepared gained is coated on glass-carbon electrode the prepared working electrode of modification, after modification
The content of electrode surface Pd is 0.027 mg, and electrochemical surface area ECAS is 47.62 m2/gPd, it is circulated volt-ampere and surveys
Examination, tests one: sweep limits is-0.9-0.5 V (vs SCE), and scanning speed is 100 mV/s, and solution is 1 that nitrogen is saturated
Mol/L NaOH solution；Test two: sweep limits is-0.8-0.4 V (vs SCE), and scanning speed is 50 mV/s, and solution is
The 1 mol/L NaOH+1 mol/LCH that nitrogen is saturated3OH solution；Test result is as shown in Fig. 3 and Fig. 4.
As seen from Figure 3, preparation-obtained catalyst PdAu occurs the reduction peak of Pd under the current potential of-0.18 V,
The reduction peak of Au occurs under the current potential of 0.15 V.
As seen from Figure 4, preparation-obtained catalyst PdAu occurs that under the current potential of-0.1 V maximum methanol aoxidizes
Peak current density, about 1.94 mA/cm2, show preferable Electrocatalytic Oxidation of Methanol activity.
Embodiment 2
(1) 1.0 g triblock copolymer P123 stirring ultrasonic dissolutions are taken in 50 mL redistilled waters；Magnetic agitation, temperature
Controlling at 30 DEG C, the speed dripped with 5s/ in P123 solution drips 10 mL potassium chloropalladate solution (1.192 mg/mL).
After (2) 30 minutes, in mixed solution, it is slowly added dropwise 10mL hydration gold chloride (2.360 mg/mL), until mixing
Till solution becomes black and generates precipitation.
(3) the black suspension centrifugation under 10000 r/min that will obtain after reaction, first washes with second distillation
Wash 3 times, then with dehydrated alcohol 3 times, finally the product after washes clean is added dehydrated alcohol dispersion protection and i.e. obtains fuel electricity
Pond PdAu catalyst.
The catalyst PdAu that the present embodiment is prepared gained is coated on glass-carbon electrode the prepared working electrode of modification, enters it
Row cyclic voltammetry, tests one: sweep limits is-0.9-0.5 V (vs SCE), and scanning speed is 100 mV/s, and solution is
The 1 mol/L NaOH solution that nitrogen is saturated；Test two: sweep limits is-0.8-0.4 V (vs SCE), and scanning speed is 50
MV/s, solution is the 1 mol/L NaOH+1 mol/LCH that nitrogen is saturated3OH solution；Test result is as shown in Fig. 5 and Fig. 6.
By Fig. 5 and Fig. 6 it can be seen that preparation-obtained catalyst PdAu occurs maximum first under the current potential of-0.1 V
Alcohol oxidation peak current density, about 2.70 mA/cm2, show preferable Electrocatalytic Oxidation of Methanol activity.
Embodiment 3
(1) 1.0 g triblock copolymer P123 stirring ultrasonic dissolutions are taken in 50 mL redistilled waters；Magnetic agitation, temperature
Controlling at 30 DEG C, the speed dripped with 5s/ in P123 solution drips 10 mL potassium chloropalladate solution (1.192 mg/mL).
After (2) 30 minutes, in mixed solution, it is slowly added dropwise 10mL hydration gold chloride (0.561 mg/mL), until mixing
Till solution becomes black and generates precipitation.
(3) the black suspension centrifugation under 10000 r/min that will obtain after reaction, first washes with second distillation
Wash 3 times, then with dehydrated alcohol 3 times, finally the product after washes clean is added dehydrated alcohol dispersion protection and i.e. obtains fuel electricity
Pond PdAu catalyst.
The catalyst PdAu that the present embodiment is prepared gained is coated on glass-carbon electrode the prepared working electrode of modification, enters it
Row cyclic voltammetry, tests one: sweep limits is-0.9-0.5 V (vs SCE), and scanning speed is 100 mV/s, and solution is
The 1 mol/L NaOH solution that nitrogen is saturated；Test two: sweep limits is-0.8-0.4 V (vs SCE), and scanning speed is 50
MV/s, solution is the 1 mol/L NaOH+1 mol/LCH that nitrogen is saturated3OH solution；Test result is as shown in Fig. 5 and Fig. 6.
By Fig. 5 and Fig. 6 it can be seen that preparation-obtained catalyst PdAu occurs maximum under the current potential of-0.15 V
Methanol oxidation peak current density, about 1.07 mA/cm2, show preferable Electrocatalytic Oxidation of Methanol activity.
Fig. 5 and Fig. 6 show embodiment 1,2,3 to be prepared three kinds of different proportion fuel-cell catalyst PdAu of gained and urges
Change the cyclic voltammetric comparison diagram of Oxidation of Methanol.Understand, fuel-cell catalyst (Pd:Au=1:2) the catalysis oxygen of embodiment 2 gained
Change methanol spike potential is less and peak current density peak performance best, has optimal catalysis Oxidation of Methanol ability, has extensively
Development space and using value.
Embodiment 4
(1) 0.5 g triblock copolymer P123 stirring ultrasonic dissolution is taken in 50 mL redistilled waters；Magnetic agitation, temperature
Controlling at 30 DEG C, the speed dripped with 5s/ in P123 solution drips 10 mL potassium chloropalladate solution (1.192 mg/mL).
After (2) 30 minutes, the speed dropping 10mL dripped with 5s/ in mixed solution is hydrated gold chloride (1.179 mg/
ML), until mixed solution becomes black and generates precipitation.
(3) the black suspension centrifugation under 10000 r/min that will obtain after reaction, first washes with second distillation
Wash 3 times, then with dehydrated alcohol 3 times, finally the product after washes clean is added dehydrated alcohol dispersion protection and i.e. obtains fuel electricity
Pond PdAu catalyst.
Claims (7)
1. a DMFC catalyst PdAu, it is characterised in that described fuel-cell catalyst PdAu average particle
Footpath is 1-100 m at 3nm-15nm, electrochemical surface area (ECSA)2/gPd, the atomic percentage conc of Pd is 40%-80%.
2. the preparation method of the fuel-cell catalyst PdAu described in claim 1, it is characterised in that its preparation method is continuous
Reduction synthesis technology, concrete grammar step is as follows:
(1) triblock copolymer P123 ultrasonic dissolution is taken in redistilled water；Temperature controls at 20-60 DEG C, magnetic agitation,
Potassium chloropalladate solution is dripped in P123 solution；After reacting 30-90 minute, in mixed reaction solution, drip six hydration gold chlorides,
Continuing reaction 60-240 minute after dripping, reactant liquor ultimately becomes black suspension；
(2) by black suspension centrifugation under 3000 r/min ~ 10000 r/min, with water and absolute ethanol washing three to
Five times, i.e. can get fuel cell PdAu catalyst.
The preparation method of fuel-cell catalyst PdAu the most according to claim 1, it is characterised in that the mixing of step (1)
In reactant liquor, triblock copolymer P123 concentration is 10-50 mg/mL, potassium chloropalladate concentration is 0.01-0.05 mmol/L, water
Closing gold chloride concentration is 0.01-0.05 mmol/L.
The preparation method of fuel-cell catalyst PdAu the most according to claim 3, it is characterised in that the mixing of step (1)
In reactant liquor, triblock copolymer P123 concentration is 20 mg/mL, potassium chloropalladate concentration is 0.03 mmol/L, is hydrated gold chloride
Concentration is 0.03 mmol/L.
The most according to claim 1, the fuel cell preparation method of PdAu catalyst, it is characterised in that in step (1), drip
Acceleration Control is dripped at 5-10 s/.
The fuel cell preparation method of PdAu catalyst the most according to claim 1, it is characterised in that in step (2), from
In heart separation process, first wash 2-3 time with redistilled water, then use absolute ethanol washing 2-3 time, it is ensured that unreacted complete three
Block copolymer P123 and presoma completely remove from catalyst surface.
7. the fuel-cell catalyst PdAu described in any one of claim 1-6 is at Electrocatalytic Oxidation of Methanol, ethanol and ethylene glycol
On application.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784902A (en) * | 2016-12-27 | 2017-05-31 | 南京大学昆山创新研究院 | Load type platinum porpezite ternary alloy nano catalyst and its preparation method and application |
| CN107195917A (en) * | 2017-06-02 | 2017-09-22 | 浙江大学台州研究院 | A kind of AuPdNWs superfine nano forest elctro-catalysts of the vertical-growth on FTO glass and preparation method thereof |
| CN108565476A (en) * | 2018-02-05 | 2018-09-21 | 三峡大学 | A kind of fuel cell ternary CoAuPd catalyst, preparation method and applications |
| CN108598499A (en) * | 2018-05-28 | 2018-09-28 | 东莞众创新能源科技有限公司 | A kind of preparation method of hydrogen fuel cell catalyst |
| CN108598501A (en) * | 2018-06-12 | 2018-09-28 | 三峡大学 | A kind of fuel cell PdRh method for preparing catalyst and its application |
| CN109148904A (en) * | 2018-09-20 | 2019-01-04 | 宁波高新区诠宝绶新材料科技有限公司 | A kind of preparation method of proton exchange membrane direct methanoic acid fuel cell catalyst |
| CN109167078A (en) * | 2018-08-13 | 2019-01-08 | 三峡大学 | The preparation method and applications of catalyst for fuel cell |
| CN109802143A (en) * | 2019-01-18 | 2019-05-24 | 三峡大学 | A kind of preparation method and application of fuel cell 3D reticular structure PdRh alloy elctro-catalyst |
| CN110931813A (en) * | 2020-01-08 | 2020-03-27 | 西北师范大学 | Au @ N-CQDs @ Pd core-shell structure nano composite material, preparation thereof and application of nano composite material in electrocatalytic oxidation of methanol |
| CN114361487A (en) * | 2021-12-20 | 2022-04-15 | 三峡大学 | PdAg/AgCl alloy electrocatalyst for fuel cell and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106784902A (en) * | 2016-12-27 | 2017-05-31 | 南京大学昆山创新研究院 | Load type platinum porpezite ternary alloy nano catalyst and its preparation method and application |
| CN107195917A (en) * | 2017-06-02 | 2017-09-22 | 浙江大学台州研究院 | A kind of AuPdNWs superfine nano forest elctro-catalysts of the vertical-growth on FTO glass and preparation method thereof |
| CN108565476A (en) * | 2018-02-05 | 2018-09-21 | 三峡大学 | A kind of fuel cell ternary CoAuPd catalyst, preparation method and applications |
| CN108565476B (en) * | 2018-02-05 | 2021-02-19 | 三峡大学 | Preparation method and application of ternary CoAuPd @ AuPd core-shell catalyst for fuel cell |
| CN108598499A (en) * | 2018-05-28 | 2018-09-28 | 东莞众创新能源科技有限公司 | A kind of preparation method of hydrogen fuel cell catalyst |
| CN108598501A (en) * | 2018-06-12 | 2018-09-28 | 三峡大学 | A kind of fuel cell PdRh method for preparing catalyst and its application |
| CN109167078A (en) * | 2018-08-13 | 2019-01-08 | 三峡大学 | The preparation method and applications of catalyst for fuel cell |
| CN109148904A (en) * | 2018-09-20 | 2019-01-04 | 宁波高新区诠宝绶新材料科技有限公司 | A kind of preparation method of proton exchange membrane direct methanoic acid fuel cell catalyst |
| CN109802143A (en) * | 2019-01-18 | 2019-05-24 | 三峡大学 | A kind of preparation method and application of fuel cell 3D reticular structure PdRh alloy elctro-catalyst |
| CN110931813A (en) * | 2020-01-08 | 2020-03-27 | 西北师范大学 | Au @ N-CQDs @ Pd core-shell structure nano composite material, preparation thereof and application of nano composite material in electrocatalytic oxidation of methanol |
| CN114361487A (en) * | 2021-12-20 | 2022-04-15 | 三峡大学 | PdAg/AgCl alloy electrocatalyst for fuel cell and application thereof |
| CN114361487B (en) * | 2021-12-20 | 2024-03-15 | 三峡大学 | Fuel cell PdAG/AgCl alloy electrocatalyst and application |
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