CN106058277B - A kind of fuel cell PdAu elctro-catalyst and preparation method thereof - Google Patents
A kind of fuel cell PdAu elctro-catalyst and preparation method thereof Download PDFInfo
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- CN106058277B CN106058277B CN201610661170.3A CN201610661170A CN106058277B CN 106058277 B CN106058277 B CN 106058277B CN 201610661170 A CN201610661170 A CN 201610661170A CN 106058277 B CN106058277 B CN 106058277B
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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
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Abstract
The present invention relates to a kind of fuel cell PdAu elctro-catalysts and preparation method thereof.Synthetic method uses continuous reduction technique, and synthetic method includes the following steps: that triblock copolymer P123 is taken to be dissolved in secondary distilled water, potassium chloropalladate solution is slowly added dropwise into P123 solution and is stirred continuously, and reaction temperature is controlled at 20-60 DEG C；After 30-90 minutes, then to six hydration gold chlorides are slowly added dropwise in reaction solution；The reaction was continued 60-240 minutes after dripping；Reaction solution centrifugation, washing three to five times are obtained into fuel-cell catalyst PdAu.Triblock copolymer P123 serves as protective agent and reducing agent; using Pd as seed; reduction potential using Pd and Au is poor; carry out potential replacement reaction; the catalyst PdAu of core-shell structure is made; its dispersibility is preferably and size, shape are uniform, has excellent Electrocatalytic Oxidation of Methanol performance, is a kind of fuel-cell catalyst of great development prospect.
Description
Technical field
The invention belongs to field of fuel cell technology, are related to the preparation method of catalyst, more particularly, to a kind of fuel
The preparation method of cell catalyst PdAu.
Background technique
As social progress and population increase, energy crisis is got worse.Fossil energy extensive use not only aggravates the energy
Crisis, and also result in environmental pollution and global warming.Therefore, seek efficiently, cleaning, sustainable development new energy obtain with
Transformation technology has become one of the top priority for solving energy problem.Fuel cell is a kind of chemical energy by fuel and 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,
Have many advantages, such as that clean fuel diversification, exhaust, low noise, environmental pollution are small, is a kind of environmentally protective energy.Due to reaction
Process is not related to burning, and therefore, energy conversion efficiency is not limited by Carnot cycle, and up to 60% ~ 80%, efficiency of actual
It is 2 ~ 3 times of ordinary internal combustion engine.
Proton Exchange Membrane Fuel Cells (PEMFC) is one of main candidate power supply of the following electric car, wherein direct alcohol
The advantages that types of fuel cells (DAFC) is due to its high power density, fuel source is abundant and easily stored and supply becomes commercialization
First choice, cost, Performance And Reliability are largely limited by elctro-catalyst, understand, research fuel cell electro catalytic mechanism,
Especially Study of Catalyst structure composition and the relationship between the battery performance service life have great science and realistic meaning.Pd
Price and reserves have very big advantage relative to Pt.The catalytic activity and stability of Pd can be by forming with Au, Cu etc.
Alloy improves.Due to difunctional mechanism, the introducing of Au can play promoting catalysis, enhance the antitoxinization performance of catalyst, mention
The activity and stability of high catalysis oxidation alcohol.By the different incorporation ways of Au, the PdAu binary of different-shape can be prepared
Alloy catalyst.
Present invention introduces Au, and using simple continuous reduction synthesis process, triblock copolymer P123 is as protective agent and also
Former agent, prepare it is dispersed preferably, regular appearance is uniform, with core-shell structure and has the PdAu catalysis of preferable electrocatalysis characteristic
Agent.
Summary of the invention
It is an object of the invention to react to introduce another more stable metal Au by potential replacement, being formed has core
The bianry alloy catalyst PdAu of shell structure further increases urging for catalyst by difunctional mechanism and its special structure
Change activity and stability.
To realize the above purposes, the technical scheme adopted is as follows:
A kind of preparation of fuel-cell catalyst PdAu uses continuous reduction synthesis process, passes through and introduces metal Au, three block
Copolymer p 123 is used as protective agent and reducing agent, prepare it is dispersed preferably, pattern is uniform and has excellent electro catalytic activity
PdAu catalyst.Method includes the following steps:
(1) take triblock copolymer P123 ultrasonic dissolution in secondary distilled water；Potassium chloroplatinate is added into P123 solution
Solution, magnetic agitation, temperature control triblock copolymer P123 concentration in 20-60 DEG C, mixed solution is 10-50 mg/mL.
Potassium chloropalladate is slowly added dropwise, wherein potassium chloropalladate concentration is 0.01-0.05 mmol/L；After reaction 30 minutes, six water are slowly added dropwise
Close gold chloride, wherein six hydration gold chloride concentration be 0.01-0.05 mmol/L, drip after the reaction was continued 60-240 minutes, instead
Liquid is answered to ultimately become black suspension.
(3) reaction solution is centrifugated at the r/min of 3000 r/min ~ 10000, with water and dehydrated alcohol wash three to
Five times, dehydrated alcohol dispersion protection finally is added in the product after washes clean and obtains fuel cell PdAu catalyst.
Further 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 is slowly added to dropwise with constant pressure funnel, drips speed control in 5-10 s/ drop.
In step (2), in centrifugal separation processes, first uses second distillation water washing 2-3 times, then wash 2- with dehydrated alcohol
3 times, guarantee that unreacted complete triblock copolymer P123 and presoma are completely removed from catalyst surface.
Preferably, pattern size is uniform, and average grain diameter is in 3-15nm for the fuel-cell catalyst PdAu dispersibility.
The fuel-cell catalyst PdAu electrochemical surface area (ECSA) is 1-100 m2/gPd
The atomic percentage content of Pd is 40%-80% in the fuel-cell catalyst PdAu.
A kind of fuel cell according to the present invention has following outstanding feature with PdAu catalyst and preparation method thereof:
(1) preparation method is continuous reduction, and process is simple, easy to operate.
(2) triblock copolymer P123 is used as protective agent and reducing agent simultaneously, green and pollution-free.
(3) it is reacted using potential replacement, using the difference of two kinds of metal master oxidation-reduction potentials, the two is spontaneously sent out
Raw redox reaction, can be made with core-shell structure and the uniform catalyst of pattern.
(4) by introducing metal Au, the dosage of precious metals pd had both been reduced, the alloy catalytic activity and stabilization being formed simultaneously
Property is more preferable.
(5) due to difunctional mechanism, lattice deformability effect and surface ligand effect, the introducing of Au can play co-catalysis work
With, enhance catalyst antitoxinization performance, improve catalysis oxidation alcohol activity and stability.
(6) catalyst prepared by has excellent electrocatalytic oxidation alcohols performance, has in direct alcohol fuel cell
Biggish application and development prospect.
Detailed description of the invention
Fig. 1: for transmission electron microscope Fig. 1 of fuel-cell catalyst PdAu prepared by embodiment 1.
Fig. 2: for transmission electron microscope Fig. 2 of fuel-cell catalyst PdAu prepared by embodiment 1.
Fig. 3: for the cyclic voltammetry curve figure of fuel-cell catalyst PdAu prepared by embodiment 1.
Fig. 4: for the cyclic voltammetry curve of fuel-cell catalyst PdAu Electrocatalytic Oxidation of Methanol prepared by embodiment 1
Figure.
Fig. 5: for the cyclic voltammetry curve comparison diagram of fuel-cell catalyst PdAu prepared by embodiment 2 and 3.
Fig. 6: bent for the cyclic voltammetric of fuel-cell catalyst PdAu Electrocatalytic Oxidation of Methanol prepared by embodiment 2 and 3
Line comparison diagram.
Specific embodiment
It is arranged with reference to the accompanying drawing with specific implementation case, the present invention is further explained, it should be understood that these embodiments are only used for
It is bright the present invention rather than limit the scope of the invention, after the present invention has been read, those skilled in the art are to of the invention
The modification of various equivalent forms falls within the application range as defined in the appended claims.
Embodiment 1
(1) take 1.0 g triblock copolymer P123s stirring ultrasonic dissolution in 50 mL secondary distilled waters；Magnetic agitation,
Temperature is controlled at 30 DEG C, and 10 mL potassium chloropalladate solution (1.192 mg/mL) are added dropwise with the speed of 5s/ drop into P123 solution.
After (2) 30 minutes, 10mL is added dropwise with the speed of 5s/ drop into mixed solution and is hydrated gold chloride (1.179 mg/
ML), until mixed solution becomes black and generates precipitating.
(3) black suspension obtained after reaction is centrifugated at 10000 r/min, is first washed with second distillation
It washs 3 times, then with dehydrated alcohol 3 times, dehydrated alcohol dispersion protection finally is added in the product after washes clean and obtains fuel electricity
Pond PdAu catalyst.
Fig. 1 and Fig. 2 show transmission electron microscope (TEM) figure of the present embodiment preparation gained fuel cell PdAu catalyst,
Prepared it can be seen from Fig. 1 and Fig. 2 resulting catalyst be it is well dispersed, pattern size is uniform, substantially without agglomeration,
The average grain diameter of particle is about 7 nm.
The present embodiment is prepared into resulting catalyst PdAu and is coated in the obtained working electrode of modification on glass-carbon electrode, after modification
The content of electrode surface Pd is 0.027 mg, and electrochemical surface area ECAS is 47.62 m2/gPd, cyclic voltammetric survey is carried out to it
Examination, test one: scanning range is -0.9-0.5 V (vs SCE), and scanning speed is 100 mV/s, and solution is the 1 of nitrogen saturation
Mol/L NaOH solution；Test two: scanning range is -0.8-0.4 V (vs SCE), and scanning speed is 50 mV/s, and solution is
1 mol/L NaOH+1 mol/LCH of nitrogen saturation3OH solution；Test result is as shown in Fig. 3 and Fig. 4.
As seen from Figure 3, there is the reduction peak of Pd under the current potential of -0.18 V in preparation-obtained catalyst PdAu,
Occurs the reduction peak of Au under the current potential of 0.15 V.
As seen from Figure 4, there is maximum methanol oxidation under the current potential of -0.1 V in preparation-obtained catalyst PdAu
Peak current density, about 1.94 mA/cm2, show preferable Electrocatalytic Oxidation of Methanol activity.
Embodiment 2
(1) take 1.0 g triblock copolymer P123s stirring ultrasonic dissolution in 50 mL secondary distilled waters；Magnetic agitation,
Temperature is controlled at 30 DEG C, and 10 mL potassium chloropalladate solution (1.192 mg/mL) are added dropwise with the speed of 5s/ drop into P123 solution.
After (2) 30 minutes, 10mL hydration gold chloride (2.360 mg/mL) is slowly added dropwise into mixed solution, until mixing
Until solution becomes black and generates precipitating.
(3) black suspension obtained after reaction is centrifugated at 10000 r/min, is first washed with second distillation
It washs 3 times, then with dehydrated alcohol 3 times, dehydrated alcohol dispersion protection finally is added in the product after washes clean and obtains fuel electricity
Pond PdAu catalyst.
By the present embodiment prepare resulting catalyst PdAu be coated on glass-carbon electrode modify be made working electrode, to its into
Row cyclic voltammetry, test one: scanning range is -0.9-0.5 V (vs SCE), and scanning speed is 100 mV/s, and solution is
1 mol/L NaOH solution of nitrogen saturation；Test two: scanning range is -0.8-0.4 V (vs SCE), scanning speed 50
MV/s, solution are 1 mol/L NaOH+1 mol/LCH of nitrogen saturation3OH solution；Test result is as shown in Fig. 5 and Fig. 6.
There is maximum first under the current potential of -0.1 V in preparation-obtained catalyst PdAu it can be seen from Fig. 5 and Fig. 6
Alcohol oxidation peak current density, about 2.70 mA/cm2, show preferable Electrocatalytic Oxidation of Methanol activity.
Embodiment 3
(1) take 1.0 g triblock copolymer P123s stirring ultrasonic dissolution in 50 mL secondary distilled waters；Magnetic agitation,
Temperature is controlled at 30 DEG C, and 10 mL potassium chloropalladate solution (1.192 mg/mL) are added dropwise with the speed of 5s/ drop into P123 solution.
After (2) 30 minutes, 10mL hydration gold chloride (0.561 mg/mL) is slowly added dropwise into mixed solution, until mixing
Until solution becomes black and generates precipitating.
(3) black suspension obtained after reaction is centrifugated at 10000 r/min, is first washed with second distillation
It washs 3 times, then with dehydrated alcohol 3 times, dehydrated alcohol dispersion protection finally is added in the product after washes clean and obtains fuel electricity
Pond PdAu catalyst.
By the present embodiment prepare resulting catalyst PdAu be coated on glass-carbon electrode modify be made working electrode, to its into
Row cyclic voltammetry, test one: scanning range is -0.9-0.5 V (vs SCE), and scanning speed is 100 mV/s, and solution is
1 mol/L NaOH solution of nitrogen saturation；Test two: scanning range is -0.8-0.4 V (vs SCE), scanning speed 50
MV/s, solution are 1 mol/L NaOH+1 mol/LCH of nitrogen saturation3OH solution；Test result is as shown in Fig. 5 and Fig. 6.
There is maximum under the current potential of -0.15 V in preparation-obtained catalyst PdAu it can be seen from Fig. 5 and Fig. 6
Methanol oxidation peak current density, about 1.07 mA/cm2, show preferable Electrocatalytic Oxidation of Methanol activity.
Fig. 5 and Fig. 6, which show embodiment 1,2,3 and prepares resulting three kinds of different proportion fuel-cell catalysts PdAu, to be urged
Change the cyclic voltammetric comparison diagram of Oxidation of Methanol.It is found that 2 resulting fuel-cell catalyst (Pd:Au=1:2) of embodiment is catalyzed oxygen
Change methanol spike potential is smaller and peak current density peak performance is best, possesses optimal catalysis oxidation methanol ability, has extensive
Development space and application value.
Embodiment 4
(1) take 0.5 g triblock copolymer P123 stirring ultrasonic dissolution in 50 mL secondary distilled waters；Magnetic agitation,
Temperature is controlled at 30 DEG C, and 10 mL potassium chloropalladate solution (1.192 mg/mL) are added dropwise with the speed of 5s/ drop into P123 solution.
After (2) 30 minutes, 10mL is added dropwise with the speed of 5s/ drop into mixed solution and is hydrated gold chloride (1.179 mg/
ML), until mixed solution becomes black and generates precipitating.
(3) black suspension obtained after reaction is centrifugated at 10000 r/min, is first washed with second distillation
It washs 3 times, then with dehydrated alcohol 3 times, dehydrated alcohol dispersion protection finally is added in the product after washes clean and obtains fuel electricity
Pond PdAu catalyst.
Claims (5)
1. a kind of 1 mol/L NaOH+1 mol/LCH in nitrogen saturation3The PdAu electricity of Electrocatalytic Oxidation of Methanol is urged in OH solution
Agent, which is characterized in that for PdAu elctro-catalyst average grain diameter in 3nm-15nm, electrochemical surface area (ECSA) is 1-100
m2The atomic percentage content of/gPd, Pd are 40%-80%, and steps are as follows for specific method:
(1) take triblock copolymer P123 ultrasonic dissolution in secondary distilled water；Temperature control is at 20-60 DEG C, magnetic agitation,
Potassium chloropalladate solution is added dropwise into P123 solution；After reaction 30-90 minutes, six hydration gold chlorides are added dropwise into mixed reaction solution,
The reaction was continued 60-240 minutes after dripping, and reaction solution ultimately becomes black suspension；
(2) black suspension is centrifugated at the r/min of 3000 r/min ~ 10000, with water and dehydrated alcohol wash three to
Five times, fuel cell PdAu catalyst can be obtained.
2. the 1 mol/L NaOH+1 mol/LCH according to claim 1 in nitrogen saturation3Electrocatalytic oxidation in OH solution
The PdAu elctro-catalyst of methanol, which is characterized in that in the mixed reaction solution of step (1), triblock copolymer P123 concentration is 10-
50 mg/mL, potassium chloropalladate concentration are 0.01-0.05 mmol/L, and hydration gold chloride concentration is 0.01-0.05 mmol/L.
3. the 1 mol/L NaOH+1 mol/LCH according to claim 1 in nitrogen saturation3Electrocatalytic oxidation in OH solution
The PdAu elctro-catalyst of methanol, which is characterized in that in the mixed reaction solution of step (1), triblock copolymer P123 concentration is 20
Mg/mL, potassium chloropalladate concentration are 0.03 mmol/L, and hydration gold chloride concentration is 0.03 mmol/L.
4. the 1 mol/L NaOH+1 mol/LCH according to claim 1 in nitrogen saturation3Electrocatalytic oxidation in OH solution
The PdAu elctro-catalyst of methanol, which is characterized in that in step (1), rate of addition is controlled in 5-10 s/ drop.
5. the 1 mol/L NaOH+1 mol/LCH according to claim 1 in nitrogen saturation3Electrocatalytic oxidation in OH solution
The PdAu elctro-catalyst of methanol, which is characterized in that in step (2), in centrifugal separation processes, first use second distillation water washing 2-3
It is secondary, it is then washed 2-3 times with dehydrated alcohol, guarantees unreacted complete triblock copolymer P123 and presoma from catalyst surface
It completely removes.
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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 |
| 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 |
| CN108598501B (en) * | 2018-06-12 | 2020-11-13 | 三峡大学 | Preparation method and application of PdRh catalyst for fuel cell |
| 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 |
| CN109802143B (en) * | 2019-01-18 | 2021-05-18 | 三峡大学 | Preparation method and application of PdRh alloy electrocatalyst with 3D mesh structure of fuel cell |
| 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 |
| CN114361487B (en) * | 2021-12-20 | 2024-03-15 | 三峡大学 | Fuel cell PdAG/AgCl alloy electrocatalyst and application |
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| CN103658672A (en) * | 2012-09-11 | 2014-03-26 | 中国科学院大连化学物理研究所 | Aqueous phase preparation method for metal nanoparticles |
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