CN105633425B - A kind of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts and preparation method thereof - Google Patents
A kind of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts and preparation method thereof Download PDFInfo
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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
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a kind of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts and preparation method thereof, include the following steps：1）Palladium presoma and conductive carrier are added to N, in N dimethylformamides or ethyl alcohol, borine N is added after ultrasonic mixing, N diethylanilines or sodium borohydride, after reacting 0.5 1.5 hours at room temperature, carbon supported Pd catalyst, i.e. Pd/C are obtained after centrifuge washing, vacuum drying；2）It is 1 by the atomic ratio of Pt and Pd by Pd/C ultrasonic disperses made from upper step in the formic acid solution of a concentration of 1 5ml formic acid/20ml water:1、1:2 or 1:3 are added the aqueous solution of platinum compounds, react 2 ~ 6 hours at room temperature, centrifuge washing, and vacuum drying is to get to product.Present invention employs the catalyst that galvanic interaction principle is prepared for having high catalytic activity and stability, and the relatively pure Pt catalyst of cost is cheap, it is preparation method simplicity, mild condition, easily operated, solve the problems, such as that conventional chemical reduction method prepares catalyst with core-casing structure and needs high temperature, surfactant.
Description
Technical field
The invention belongs to fuel-cell catalyst field more particularly to a kind of Pdx@Pt/C nucleocapsid fuel battery negative poles
Catalyst and preparation method thereof.
Background technology
Precious metals pt is best one of the catalyst of current fuel battery negative pole oxygen reduction reaction, however, being made using pure Pt
There is a problem of that performance is low and stability is poor for fuel battery cathod catalyst.In addition, most dilute as one of which on the earth
Some elements, high cost also significantly limit its commercial applications.Although Pt and 3dTransition-metal Fe, Co, Ni, Cu etc.
The alloy of formation can improve fuel battery negative pole performance to a certain extent, but these 3dMetal in acid condition easy
Dissolubility results in the bad stability of catalyst entirety.If being prepared into nucleocapsid M@Pt（M represents monometallic or conjunction
Gold）Catalyst can then improve the utilization rate of Pt simultaneously, moreover it is possible to improve the stability of catalyst.Studies have shown that Pd is to oxygen
Most suitable substrate is restored, it and Pt not only have face-centred cubic structure, but also anti-with similar lattice constant and chemistry
Ying Xing.By the slight compression strain of Pt shells caused by Pd cores, its catalytic activity can be improved, in addition, Pd cores there are energy
Enough improve the stability of catalyst.The synthetic method of common catalyst with core-casing structure includes electronation and underpotential deposition.
Electronation generally requires higher temperature and ensures uniform cladding and the surfactant of Pt to prevent the Pt particles generated hair
Raw aggregation；The method that underpotential deposition Cu single layers carry out Pt displacements again cannot achieve the cladding of full single layer, and the amount prepared is non-
It is often few, it is difficult to realize large-scale prepare.
Invention content
In view of the problems of the existing technology, the present invention with improve fuel battery negative pole performance, increase catalyst stability,
For the purpose of reducing Pt dosages, a kind of Pdx@Pt (x=1,1.4,2) nucleocapsid fuel battery cathod catalysts and its system are provided
Preparation Method.
A kind of preparation method of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts, comprises the steps of：
1）Palladium presoma and conductive carrier are added in n,N-Dimethylformamide or ethyl alcohol, boron is added after ultrasonic mixing
Alkane N, N- diethylaniline or sodium borohydride obtain after reacting 0.5-1.5 hours at room temperature after centrifuge washing, vacuum drying
Carbon supported Pd catalyst, i.e. Pd/C；
2）By Pd/C ultrasonic disperses made from upper step in the formic acid solution of a concentration of 1-5ml formic acid/20ml water, by Pt with
The atomic ratio of Pd is 1:1、1:2 or 1:3 are added the aqueous solution of platinum compounds, react 2 ~ 6 hours at room temperature, centrifuge washing, very
Sky is dry to get to product.
Preferred embodiment as said program：
The palladium presoma is palladium acetylacetonate.
The conductive carrier is high specific area carbon.
The conductive carrier is one or more of conductive black, activated carbon, carbon nanotube and graphene.
The aqueous solution of the platinum compounds is the aqueous solution of chloroplatinic acid, potassium chloroplatinate, potassium chloroplatinite or sodium chloroplatinite.
The present invention also provides Pdx@Pt/C nucleocapsid fuel battery cathod catalysts prepared by the above method, are carried by conduction
Body and Pdx@Pt/C Core-shell Structure Nanoparticles composition, the mass percentage content of Pt is 19 ~ 40% in catalyst, the Pd with
The molar ratio of Pt is 1 ~ 2.
The Pdx@Pt/C nucleocapsids are nanoscale.
The particle size range of the Pdx@Pt/C nucleocapsids is 3 ~ 6nm.
Compared with prior art, the present invention has the following advantages that and advantageous effect：
1) preparation method of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts of the invention is simple, does not need height
Mild surfactant is suitble to large-scale production；The oxygen reduction activity for the Pd@Pt catalyst that Pt mass fractions are 25.9% is super
Cross 60% business Pt/C, hence it is evident that the content of platinum in catalyst is reduced, and the resource of Pd is relatively abundant, so as to solve
The catalyst resource problem that fuel cell is faced at present；
2) Pdx@Pt/C nucleocapsid fuel battery cathod catalysts of the invention have Cathodic oxygen reduction non-
Often good catalytic activity, compared with commercially available 20wt.% Pt/C catalyst, the area activated of catalyst Pt of the present invention improves 3
Times, the mass activity of Pt improves 3 ~ 4 times so that fuel battery negative pole performance is greatly improved；
4) Pdx@Pt/C nucleocapsid fuel battery cathod catalysts of the invention, are urged with the pure Pt/C of commercially available 20wt.%
Agent is compared, and stability significantly improves；After accelerated stability test, the mass activity of catalyst obtains slight improvement,
And area activated 1.5 times be increased to before test；
5) of the invention Pdx@Pt/C nucleocapsid fuel battery cathod catalysts are prepared by Pd particle surfaces
Galvanic interaction and the Pd and Pt catalytic efficiencies different to formic acid, solve the catalyst surface of general chemistry reduction method preparation
The problem of Pt homogeneous nucleations, hence it is evident that the uniformity and utilization rate for improving catalyst surface Pt are conducive to the face for improving catalyst
Product activity and mass activity；In addition, take full advantage of Pd removes reduction Pt presomas to the catalysis of formic acid that is cheap, being easy to get, greatly
The cost for reducing reducing agent；
6）The preparation method of the Pdx@Pt/C nucleocapsid fuel battery cathod catalysts of the present invention solves common deficient electricity
The coverage of catalyst surface Pt prepared by position deposition displacement method is low, and the problem of be difficult to mass produce.
Description of the drawings
Fig. 1 is Pd1.4Hydrogen reduction polarization when@Pt/C are initial, after the 10000th circle and the 20000th circle cyclic voltammetry scan is bent
Line；
Fig. 2 is Pd1.4Cyclic voltammetric when@Pt/C are initial, after the 10000th circle and the 20000th circle cyclic voltammetry scan is bent
Line；
Cyclic voltammetry curve when Fig. 3 is Pt/C initial and after the 10000th circle cyclic voltammetry scan；
Polarization curves of oxygen reduction when Fig. 4 is Pt/C initial and after the 10000th circle cyclic voltammetry scan；
Fig. 5 is to prepare Pd-Pt/C, Pd1.4The polarization curves of oxygen reduction of@Pt/C, Pt/C and Pd/C catalyst.
Specific implementation mode
In order to better understand the present invention, with reference to embodiment, the present invention is described further.
The Pt/C catalyst of commercially available 20wt.% is chosen in the embodiment of the present invention（Hereinafter referred to as Pt/C）As a comparison
Catalyst, by itself and Pd obtained by the embodiment of the present inventionxThe chemical property of@Pt/C catalyst with core-casing structure is compared.
Preparation method includes step：
1）Palladium presoma and conductive carrier are added in n,N-Dimethylformamide or ethyl alcohol, boron is added after ultrasonic mixing
Alkane N, N- diethylaniline or sodium borohydride obtain after reacting 0.5-1.5 hours at room temperature after centrifuge washing, vacuum drying
Carbon supported Pd catalyst, i.e. Pd/C；
2）By Pd/C ultrasonic disperses made from upper step in the formic acid solution of a concentration of 1-5ml formic acid/20ml water, by Pt with
The atomic ratio of Pd is 1:1、1:2 or 1:3 are added the aqueous solution of platinum compounds, react 2 ~ 6 hours at room temperature, centrifuge washing, very
Sky is dry to get to Pdx@Pt/C catalyst with core-casing structure.
Embodiment 1
1）PdxThe preparation of@Pt/C catalyst with core-casing structure
Palladium presoma and conductive carrier are added in n,N-Dimethylformamide, borine N, N- are added after ultrasonic mixing
After reacting 1 hour at room temperature, carbon supported Pd catalyst, i.e. Pd/C are obtained after centrifugation, vacuum drying for diethylaniline；By upper step
Pd/C ultrasonic disperses obtained are in extremely low concentration formic acid solution（1-5ml formic acid/20ml water）In, the atomic ratio of Pt and Pd is pressed respectively
It is 1:1,1:2,1:3 are added the aqueous solution of potassium chloroplatinite, react 3 hours at room temperature, centrifuge washing, vacuum drying divides
Pd@Pt/C, Pd are not obtained1.4@Pt/C, Pd2@Pt/C catalyst.Wherein, Pd@Pt/C, Pd1.4@Pt/C, Pd2@Pt/C nucleocapsids
The Pt contents of nanocatalyst are about the 35.8wt% of catalyst, 25.9wt%, 19.5wt%.Gained catalyst PdxThe grain of@Pt/C
Diameter ranging from 3 ~ 6nm.
2）Test PdxThe cathode performance and stability of@Pt/C catalyst with core-casing structure
Pd is contained on surfacexThe electrode of@Pt/C catalyst is inserted into electrolyte, as working electrode.Using three electrode bodies
System tests catalyst Pd@Pt/C, Pd respectively1.4@Pt/C, Pd2The chemical property of@Pt/C and Pt/C, specific test are as follows：With
The perchloric acid of 0.1mol/L is electrolyte, and 30 °C of water-bath temperature controls are used as to electrode using big platinized platinum, are made using saturated calomel electrode
For reference electrode, reference electrode is placed in salt bridge, the salt bridge other end is inserted into electrolytic cell and by capillary tip close to work
Electrode.It is saturated 50mV/s sweep speeds test Pd@Pt/C, Pd in electrolyte in Ar1.4@Pt/C, Pd2The cycle of@Pt/C and Pt/C
Volt-ampere curve, in O2It is saturated 5mV/s sweep speed electrode rotating speeds 1600rpm test catalyst Pd@Pt/C, Pd in electrolyte1.4@
Pt/C, Pd2Catalytic activity of the@Pt/C and Pt/C to oxygen reduction reaction.Test result is shown in 0.9V (vs reversible hydrogen electrodes)
When the area activated of Pt/C be 0.12 mA/cm2, mass activity is 96 mA/mg；Pd@Pt/C, Pd1.4@Pt/C, Pd2@Pt/C's
Area activated is respectively 0.31,0.341,0.273 mA/cm2, mass activity is respectively 276,338,199 mA/mg；Compared to Pt/
C, Pd1.4The area activated of@Pt/C improves nearly 3 times, and mass activity improves nearly 4 times.
In O220,000 circle cyclic voltammetric of scanning in 0.6V-1.1V (vs reversible hydrogen electrodes) potential range is saturated in electrolyte,
Catalyst stability is tested, test result shows：Pd prepared by embodiment 11.4@Pt/C catalyst is after 10,000 circle cyclic voltammetrics
Electrochemical surface area decaying 32%, the half wave potential of oxygen reduction reaction polarization curve is than initial oxygen reduction reaction polarization curve
Half wave potential has slight improvement；At second 10,000 after circle scanning, electrochemical surface area only decays 5%, and hydrogen reduction is anti-
The half wave potential of polarization curve is answered, almost without changing, to show this than the half wave potential of initial oxygen reduction reaction polarization curve
Catalyst with core-casing structure has good stability, as depicted in figs. 1 and 2；And Pt/C catalyst is after 10,000 circle cyclic voltammetrics
Electrochemical surface area decaying 52%, oxygen reduction reaction polarization curve half wave potential is negative to move 34mV, as shown in Figure 3 and Figure 4, Pt/C
Activity occur acutely decaying.
Palladium presoma used is palladium acetylacetonate in embodiment 1, and conductive carrier used is that conductive black, activated carbon, carbon are received
One or more of mitron and graphene, n,N-Dimethylformamide used can be replaced by ethyl alcohol, borine N used, N- diethyls
Base aniline can be replaced by sodium borohydride, and potassium chloroplatinite used can be replaced by chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinite, and
Gained catalyst Pd@Pt/C, Pd are not influenced1.4@Pt/C, Pd2The properties of@Pt/C；And a concentration of 1-5ml first of formic acid
Acid/20ml water, first set reaction time are 0.5-1.5 hours, gained catalysis when second of reaction time is 2-6 hours arbitrary values
Agent Pd@Pt/C, Pd1.4@Pt/C, Pd2The properties of@Pt/C are same as Example 1.
Embodiment 2
1）The preparation of the non-catalyst with core-casing structure of Pd-Pt/C
Palladium presoma and conductive carrier are added in n,N-Dimethylformamide, borine N, N- are added after ultrasonic mixing
After reacting 1 hour at room temperature, carbon supported Pd catalyst, i.e. Pd/C are obtained after centrifugation, vacuum drying for diethylaniline；By upper step
Pd/C ultrasonic disperses obtained are in intermediate concentration formic acid solution（8-15ml formic acid/20ml water）In, chloroplatinous acid potassium solution is added,
It reacts 3 hours at room temperature, centrifuge washing, vacuum drying is to get to Pd-Pt/C catalyst.Wherein, Pd-Pt/C nano-catalytics
The Pt contents of agent are about the 26wt% of catalyst.
2）Test the cathode performance of the non-catalyst with core-casing structure of Pd-Pt/C
The electrode that Pd-Pt/C catalyst is contained on surface is inserted into electrolyte, as working electrode.Using three-electrode system
The chemical property of test catalyst Pd-Pt/C and Pt/C respectively, specific test are as follows：It is electrolysis with the perchloric acid of 0.1mol/L
Liquid, 30 °C of water-bath temperature controls are used as using big platinized platinum to electrode, using saturated calomel electrode as reference electrode, by reference electrode
It is placed in salt bridge, the salt bridge other end is inserted into electrolytic cell and by capillary tip close to working electrode.It is saturated in electrolyte in Ar
50mV/s sweep speeds test the cyclic voltammetry curve of Pd-Pt/C and Pt/C, in O2It is saturated 5mV/s sweep speeds electricity in electrolyte
Pole rotating speed 1600rpm tests catalytic activity of the catalyst Pd-Pt/C and Pt/C to oxygen reduction reaction.Test result is shown in 0.9V
The area activated of Pt/C is 0.12 mA/cm when (vs reversible hydrogen electrodes)2, mass activity is 96 mA/mg, the face of Pd-Pt/C
0.135 mA/cm of product activity2, mass activity is 132 mA/mg, compared to the catalyst with core-casing structure prepared, since surface layer Pt goes out
Existing dendritic growth causes a large amount of Pd to be exposed to outer, causes its expression activitiy poor.
Palladium presoma used is palladium acetylacetonate in the present embodiment, and conductive carrier used is that conductive black, activated carbon, carbon are received
One or more of mitron and graphene, n,N-Dimethylformamide used can be replaced by ethyl alcohol, borine N used, N- diethyls
Base aniline can be replaced by sodium borohydride, and potassium chloroplatinite used can be replaced by chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinite, and first
The secondary response time is 0.5-1.5 hours arbitrary values, and second of reaction time is 2-6 hours arbitrary values and does not influence gained Pd-
The properties of the non-catalyst with core-casing structure of Pt/C.
The Pd below prepared by embodiment 11.4@Pt/C catalyst, business Pt/C catalyst, pure Pd/C catalyst and reality
The polarization curves of oxygen reduction for applying the Pd-Pt/C catalyst of the preparation of example 2 makees further comparative illustration：
As shown in figure 5, polarization curves of oxygen reduction test result shows that the half wave potential of business Pt/C is 0.89V, pure Pd/C
Catalyst half wave potential is 0.829V, and the Pd-Pt/C catalyst half wave potentials of non-nucleocapsid are 0.889V, and according to the present invention
Pd prepared by method1.4@Pt/C catalyst half wave potentials are 0.913V.Pd manufactured in the present embodiment1.4@Pt/C catalyst half-wave electricity
Gesture is moved to positive potential direction respectively than the half wave potential of business Pt/C, pure Pd/C and the Pd-Pt/C catalyst of non-nucleocapsid
About 24mV, 84mV and 24.1mV show that catalyst prepared by the present invention has very outstanding cathode performance.
Claims (8)
1. a kind of preparation method of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts, it is characterised in that include following step
Suddenly：
1) palladium presoma and conductive carrier are added in n,N-Dimethylformamide or ethyl alcohol, borine is added after ultrasonic mixing
N, N- diethylaniline or sodium borohydride obtain carbon after reacting 0.5-1.5 hours at room temperature after centrifuge washing, vacuum drying
Carry Pd catalyst, i.e. Pd/C；
2) by Pd/C ultrasonic disperses made from upper step in the formic acid solution of a concentration of 1-5ml formic acid/20ml water, by Pt's and Pd
Atomic ratio is 1:1、1:2 or 1:3 are added the aqueous solution of platinum compounds, react 2~6 hours at room temperature, centrifuge washing, and vacuum is dry
It is dry to get to product.
2. the preparation method of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts as described in claim 1, feature exist
In：The palladium presoma is palladium acetylacetonate.
3. the preparation method of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts as described in claim 1, feature exist
In：The conductive carrier is high specific area carbon.
4. the preparation method of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts as claimed in claim 3, feature exist
In：The conductive carrier is one or more of conductive black, activated carbon, carbon nanotube and graphene.
5. the preparation method of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts as described in claim 1, feature exist
In：The aqueous solution of the platinum compounds is the aqueous solution of chloroplatinic acid, potassium chloroplatinate, potassium chloroplatinite or sodium chloroplatinite.
6. a kind of Pdx@Pt/C nucleocapsid fuel battery cathod catalysts prepared based on claim 1 the method, special
Sign is：It is made of conductive carrier and Pdx@Pt/C Core-shell Structure Nanoparticles, the mass percentage content of Pt is in catalyst
The molar ratio of 19~40%, the Pd and Pt are 1~2.
7. Pdx@Pt/C nucleocapsid fuel battery cathod catalysts as claimed in claim 6, it is characterised in that：The Pdx@
Pt/C nucleocapsids are nanoscale.
8. Pdx@Pt/C nucleocapsid fuel battery cathod catalysts as claimed in claim 6, it is characterised in that：The Pdx@
The particle size range of Pt/C nucleocapsids is 3~6nm.
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| CN106169587A (en) * | 2016-08-15 | 2016-11-30 | 陈隽 | A kind of new fuel cell of high alcohol-rejecting ability and preparation method thereof |
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| CN109378492B (en) * | 2018-11-27 | 2021-09-21 | 上海交通大学 | Core-shell structure Pd @ Pt/C or PdM @ Pt/C catalyst and preparation thereof |
| CN109830702A (en) * | 2019-02-13 | 2019-05-31 | 深圳市雄韬电源科技股份有限公司 | A kind of fuel-cell catalyst and its preparation method and application |
| CN112510220B (en) * | 2020-11-19 | 2022-02-01 | 武汉大学 | Core-shell type platinum-based alloy electrocatalyst with high oxygen reduction performance and preparation method thereof |
| CN112695223B (en) * | 2020-12-07 | 2022-03-04 | 青岛大学 | Method for synthesizing small-particle-size platinum-rhodium nanocrystals |
| CN113270601B (en) * | 2021-05-06 | 2022-04-01 | 燕山大学 | Preparation method of double-element Pt/PdPt/Pt interlayer tube wall porous nanotube and porous nanotube |
| CN114335577B (en) * | 2021-12-30 | 2024-03-08 | 全球能源互联网研究院有限公司 | Modified catalyst, membrane electrode, preparation method of modified catalyst and membrane electrode, and fuel cell |
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