CN109119640A - The preparation and its hydrogen reduction catalytic applications of palladium platinum nickel icosahedron alloy nanoparticle - Google Patents
The preparation and its hydrogen reduction catalytic applications of palladium platinum nickel icosahedron alloy nanoparticle Download PDFInfo
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- CN109119640A CN109119640A CN201810504422.0A CN201810504422A CN109119640A CN 109119640 A CN109119640 A CN 109119640A CN 201810504422 A CN201810504422 A CN 201810504422A CN 109119640 A CN109119640 A CN 109119640A
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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
- H01M4/8825—Methods for deposition of the catalytic active composition
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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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- 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
- H01M4/9041—Metals or alloys
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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
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- H01M4/90—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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- 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
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Abstract
The application being catalyzed the invention discloses a kind of palladium platinum nickel regular dodecahedron alloy nanoparticle prepared by one-step method and its in a fuel cell as hydrogen reduction, by being constituted by main component peak catalyst carrier and the catalyst metals supported in said catalyst carrier of carbon.The invention has the advantages that: (1) preparation method of the material simple, does not need additional step and carries out load support material, is not related to toxic chemical spills, environmentally friendly and energy saving；(2) the regular dodecahedron alloy nanoparticle structure novel of this method preparation, predominantly face centered cubic FCC(111) crystal face；(3) there is efficient electrocatalysis characteristic by palladium platinum nickel ternary regular dodecahedron alloy nanoparticle prepared by one-step method in this research, its take-off potential, half wave potential and reduction spike potential are much higher than business platinum carbon, limiting current density also far super business platinum carbon, a kind of new cathode catalyst material is provided for fuel cell, is had a good application prospect.
Description
Technical field
The present invention is reacted using alloy nano-material applied to efficient catalytic oxidation-reduction, and catalyst and new energy materials are belonged to
Technical field.Specifically related to the preparation of used in proton exchange membrane fuel cell alloy nano-material catalyst, and in fuel electricity
Application in terms of pool cathode material.
Background technique
Fuel cell is a kind of novel power generation device, and possessing the conventional fossil fuels such as natural gas, coal, petroleum energy can not look forward to
And advantage, it can be achieved that expeditiously converting electric energy for the chemical energy in fuel cell, and energy conversion process basically reaches
Zero-emission, to solving that the global warming that global village faces, conventional fossil fuel development difficulty be big and ecological pollution etc. is most important,
The always research and development focus in clean energy resource field in the world.
Because Cathodic oxygen reduction (oxygen reduction reaction, be abbreviated as ORR) is that fuel cell electricity is urged
The committed step for changing reaction is talked when common catalyst and carries platinum, and wherein platinum reserves are rare and expensive, leads to proton exchange
The cost of membrane cell is high, greatly limits the development of Proton Exchange Membrane Fuel Cells.Therefore, it improves
Platinum utilization, developing cheap, high activity oxygen reduction catalyst is the pass for realizing the application of fuel cell large-scale commercial applications
Key.In recent years, with the development of nanometer synthetic technology, the research of more metal nano catalyst has attracted the note of numerous researchers
Meaning.Through the retrieval discovery to existing associated materials, the alloy nano particle with { 111 } exposure crystal face has significant catalytic
Energy.As the patent of application number 201710148367.1 disclose a kind of icosahedron shape Pd PdFe metal nano catalyst and its
Preparation and application；The patent of application number 201710223096.1 discloses a kind of platinum palladium vermiform alloy by mildly preparing and receives
Rice grain and its hydrogen reduction catalytic applications.Since the two has all used relatively relatively inexpensive metal completely or partially instead of your gold
Belong to Pt, thus greatly reduces the synthesis cost of catalyst.
Summary of the invention
Technical problems based on background technology the invention proposes icosahedron shape PdPtNi/C nanocrystal and are urged
Agent preparation, application carry out alloying to Pt using price less expensive Ni and Pd, can both reduce the synthesis of catalyst at
This, and particular crystal plane and twin boundaries can be made it have using crystal face grain boundary effect, the special twin structure of metal
PdPtNi/C nanocrystal catalytic performance with higher.
Icosahedron nanocrystal proposed by the present invention, average grain diameter are the regular dodecahedron of 20nm, have twin knot
Structure, surface layer exposed area are { 111 } crystal face.
Preferably, wherein Pd element and Pt element precursor molar ratio are 0.5 ~ 1.5, Pt element and Ni element precursor
Ratio is 2.5 ~ 3.5.
The present invention also proposes above-mentioned icosahedron PdPtNi/C nanocrystal peak preparation method, includes the following steps: room temperature
Under, by sodium tetrachloropallate, two (acetylacetone,2,4-pentanedione) platinum (II), four hydration nickel acetates, diallyl dimethyl ammoniumchloride aqueous solution
It is added in ethylene glycol solution with carbon dust, is passed through argon gas, stirred, be put into high temperature oil bath pan and carry out pyroreaction, be cooled to room
Temperature, cleaning, is dried to obtain icosahedron PdPtNi/C nanocrystal.
Preferably, diallyl dimethyl ammoniumchloride concentration of aqueous solution is 30 ~ 40%, and additional amount is 150 ~ 200 μ l.
Preferably, load carbon black mass is 20 ~ 25mg.
Preferably, ethylene glycol additional amount is 13 ~ 18 ml.
Preferably, the temperature of pyroreaction is 185 ~ 195 DEG C, and the pyroreaction time is 1.5 ~ 2.5h.
Preferably, the concrete operations of cleaning are as follows: material is centrifuged after will be cooled to room temperature, and centrifugation gained is produced
The mixed liquor of object deionized water and polar solvent carries out supersound washing, repeats above-mentioned centrifuge separation and supersound washing step 3 time.
Preferably, the revolving speed of centrifuge separation is 9000 ~ 11000 revs/min, and the time of centrifuge separation is 3 ~ 5min.
Preferably, the supersound washing time is 3 ~ 5min.
Preferably, polar solvent is acetone and ethyl alcohol.
Preferably, drying temperature is 70 DEG C, drying time 3h.
The above-mentioned PdPtNi/C nanocrystal catalyst that the present invention also proposes fuel battery cathode with proton exchange film oxygen also
As the application of catalyst in former reaction process.
Agitating mode in the present invention is magnetic agitation.
Gained catalyst of the invention has in the Cathodic oxygen reduction of fuel cell to have great advantage, unit mass Mars
The commercial Pt/C catalytic performance of Johnson Mattney company of coin U.S. production promotes nearly 40 times, and unit area activity is than commercial
Pt/C catalyst improves 43 times, sufficiently shows significant advantage of the structure in catalysis reaction.Therefore, of the invention
PdPtNi/C metal nano catalyst has wide application prospect in Proton Exchange Membrane Fuel Cells catalysis technical field.
Detailed description of the invention
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with attached drawing to the present invention make into
The detailed description of one step, in which:
Fig. 1 is the XRD diagram for the catalyst that embodiment 1 is prepared；
Fig. 2 is EDX, TEM and HRTEM figure for the catalyst that embodiment 1 is prepared；
The catalyst that Fig. 3 is embodiment 1, comparative example 1 is prepared is in 0.1M HClO4CV figure in electrolyte；
The catalyst that Fig. 4 is embodiment 1, comparative example 1 is prepared is in 0.1M HClO4LSV Fig. 5 in electrolyte is to implement
The catalyst that example 1, comparative example 1 are prepared is in 0.85 VRHEUnder area specific activity and mass ratio activity histogram.
Specific embodiment
Embodiment 1
The method of feeling oneself inferior of above-mentioned PdPtNi/C metal nano catalyst proposed by the present invention, comprising the following steps:
1) 44.88mg sodium tetrachloropallate (NaPdCl is weighed4), 60mg bis- (acetylacetone,2,4-pentanedione) platinum (II) (Pt (acac)2、12.65mg
Four hydration nickel acetate (Ni (CH3COO)2·4H2O)), the diallyl dimethyl ammoniumchloride of 150 μ l mass concentrations 35%
(PDDA) aqueous solution, 23.5mg carbon dust are added to excessive 15ml ethylene glycol (C in three hole flasks2H6O2) in solution, shake manually
Dynamic mixing.
2) mixed solution in three hole flasks is subjected to ultrasound procedure 3min；
3) mixed solution in three hole flasks is transferred in oil bath pan, the logical protective gas in condensing unit, it is anti-at 190 DEG C
2h is answered, PdPtNi/C mixed solution is prepared.
4) mixed solution is placed in centrifuge tube centrifugally operated, 10000 revs/min, is centrifuged 3min, obtains hybrid solid product；
5) hybrid solid product is successively cleaned with deionized water, ethyl alcohol, acetone: first ultrasound procedure dispersion, then be collected by centrifugation
It is centrifuged product.
6) centrifugation product is placed in 70 DEG C of baking oven drying process, obtains PdPtNi/C ternary alloy catalyst powder；
Comparative example 1
The oxygen reduction catalyst of comparative example 1 uses business Pt/C catalyst.
Hereinafter reference will be made to the drawings, and a preferred embodiment of the present invention will be described in detail.It can be demonstrate,proved by above-mentioned experiment
PdPtNi/C oxygen reduction catalyst bright, that embodiment 1 is prepared by reduction method has good crystallinity, and partial size
It is evenly distributed with more prominent latent active site, area specific activity is higher.PdPtNi/C current potential is shuffled, than comparative example 1
Electrochemical oxygen reduction performance has more superiority.In the present invention, the PdPtNi/C oxygen reduction catalyst that is prepared with reduction method
Performance is more preferable in oxygen reduction reaction.
Fig. 1 is the XRD diagram for the PdPtNi/C catalyst material that embodiment 1 is prepared, as shown in Figure 1.Because having in figure
There is sharp diffraction maximum, therefore prepared PdPtNi/C catalyst is crystal structure.Peak 1 is PdPtNi(111 in figure) crystal face
Corresponding diffraction maximum.Peak 2 is PdPtNi(200 in figure) diffraction maximum corresponding to crystal face.Peak 3 is PdPtNi(111 in figure) it is brilliant
Diffraction maximum corresponding to face.Peak 1 is PdPtNi/C(220 in figure) diffraction maximum corresponding to crystal face.Peak 4 is PdPtNi in figure
(311) diffraction maximum corresponding to.Therefore by XRD diagram it is found that the ternary alloy catalyst PdPtNi/C of preparation has face-centered cubic
(FCC) crystal structure.The position of PdPtNi/C diffraction maximum and there is deviation with the diffraction maximum peak position position of monometallic Pd, Pt, Ni,
The material for showing that we prepare belongs to alloy.
Fig. 2 is EDX, TEM and HRTEM figure for the PdPtNi/C catalyst material that embodiment 1 is prepared, such as Fig. 2 institute
Show.Contain Pd, Pt and Ni element in catalyst material from can be seen that in Fig. 2 (a), it is determined that the shape of PdPtNi ternary alloy three-partalloy
At.It is successfully carried on carbon material from can be seen that PdPtNi catalyst nano-particles in Fig. 2 (b).It can be with from Fig. 2 (c)
Find out, PdPtNi catalyst nano-particles are relatively uniform, about 20 nm of average grain diameter.It is found that PdPtNi from Fig. 2 (d) HRTEM
Catalyst nano-particles belong to regular dodecahedron there are apparent fivefold symmetry twin boundary, have 20 { 111 } crystal faces.
PdPtNi interplanar distance has following four: 0.225nm, 0.196nm, 0.135nm and 0.123nm, be respectively belonging to { 111 },
{ 200 }, { 220 } and { 311 } crystal face.PdPtNi catalyst nano-particles interplanar distance proves that its structure is face-centred cubic crystal
Structure.
The PdPtNi/C catalyst material and business Pt/C catalyst that embodiment 1 is prepared respectively are coated in rotation
As working electrode, platinum filament is used as to electrode glassy carbon electrode surface, and for saturated calomel electrode as reference electrode, concentration is 0.1 M
HClO4Solution is electrolyte, is prepared into oxygen reduction reaction electro-chemical test group.
Fig. 3 is the 0.1M HClO of 1 two kinds of embodiment 1, comparative example catalyst when Ar is saturated4Rotational circle in electrolyte
CV figure when the revolving speed of disc electrode is 1600 rpm, as shown in Figure 3.It can be seen from the figure that two kinds of catalyst are in hydrogen adsorption desorption
The feature in area is different, and the adsorption desorption region for the PdPtNi/C catalyst that embodiment 1 is prepared is smaller.
The catalyst that Fig. 4 is embodiment 1, comparative example 1 is prepared is in 0.1M HClO4Rotating circular disk electricity in electrolyte
LSV figure when the revolving speed of pole is 1600 rpm, as shown in Figure 4.Test of the activity of catalyst in terms of the electroreduction of oxygen can
With with hydrodynamics rotating disk electrode (r.d.e) technology.Show that the polarization measured in terms of hydrogen reduction with rotating disk electrode (r.d.e) is bent in figure
The position of line, it can be seen from the figure that PdPtNi/C nanoparticle catalyst is dynamic under same current potential in rotating disk electrode (r.d.e)
Mechanics current density is bigger, plays spike potential and half wave potential corrigendum, shows that the PdPtNi/C nanoparticle catalyst of preparation has
Better electro-chemical activity.
By above-mentioned experiment it can be proved that the PdPtNi/C oxygen reduction catalyst that embodiment 1 is prepared by hydro-thermal method,
With good crystallinity, and particle size is small, is evenly distributed.PdPtNi/C oxygen reduction catalyst electrochemical surface area compared with
It is small, illustrate the negligible amounts of active site, and active site latent active is preferable, and current potential is shuffled, than other alloy types electrification
It learns hydrogen reduction performance and has more superiority.So PdPtNi/C nanometer oxygen reduction catalyst prepared by embodiment 1 is in 0.1M
HClO4There is good oxygen reduction catalytic activity in electrolyte.Therefore, it in the present invention, is prepared with hydro-thermal method
PdPtNi/C oxygen reduction catalyst performance in oxygen reduction reaction is more preferable.
In the present invention, ultrasound, which goes out parameter, to be conventional ultrasonic treatment parameter, the equipment of certain other agitating solutions
It can be used for the present invention, ultrasonic time and ultrasonic power can be with STOCHASTIC CONTROLs.Palladium source, platinum source, nickel source are only limitted to sodium tetrachloropallate, two
(acetylacetone,2,4-pentanedione) platinum (II), four hydration nickel acetates.Solvent is ethylene glycol, ultrasound procedure can according to material therefor and feedstock property into
Row adjustment.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although passing through ginseng
According to the preferred embodiment of the present invention, invention has been described, it should be appreciated by those of ordinary skill in the art that can
To make various changes to it in the form and details, without departing from the present invention defined by the appended claims
Spirit and scope.
Claims (5)
1. a kind of preparation method of PdPtNi/C nanometers of oxygen reduction catalyst, it is characterised in that: the following steps are included:
(1) diallyl dimethyl ammoniumchloride of 15 ml ethylene glycol and 150 μ l mass concentrations 35% is measured with liquid-transfering gun
(PDDA) it is fitted into 30ml round bottom three hole flasks；
It (2) is 3:3:1 according to palladium element, platinum element and nickel element molar ratio, control platinum element mole is 0.015 mmol, will
Sodium tetrachloropallate (NaPdCl4), two (acetylacetone,2,4-pentanedione) platinum (II) (Pt (acac) 2, four be hydrated nickel acetate (Ni (CH3COO)2·
4H2O it)) is added in above-mentioned 30ml round bottom three hole flasks with carbon dust, seals ultrasound 1h；
(3) solution for being completely dissolved precursor after ultrasound is put into oil bath pan, 180 ~ 190 DEG C of heating under argon gas (Ar) protection
Stirring, continues 2 ~ 3h；
(4) it is restored with the palladium platinum nickel ternary nano alloy particle of preparation applied to electrocatalytic oxidation, it is efficient to obtain fuel battery negative pole
Catalyst.
2. the preparation method of PdPtNi/C nanometers of oxygen reduction catalyst according to claim 1, it is characterised in that:
PDDA used by step (1) adjusts the appearance structure of catalyst nano-particles, ethylene glycol conduct as surfactant
Reducing agent and solvent occur redox reaction with metallic precursor as the temperature rises, are reduced into metallic state palladium, platinum
And nickel, form palladium platinum nickel icosahedron Nanoalloy.Using the method for ultrasound, ultrasonic power 80%, the suspension partial size of preparation
Size, form can control, and ultrasonic dispersibility is also preferable.
3. the preparation method of PdPtNi/C nanometers of oxygen reduction catalyst according to claim 1, it is characterised in that:
Step (2) the sodium tetrachloropallate sodium tetrachloropallate, two (acetylacetone,2,4-pentanedione) platinum (II), four hydration nickel acetates and carbon dust are according to this
It is added in round-bottomed flask, a kind of substance under isodynamic adds again after mixing evenly, after being all added, needs to seal ultrasound 60
Min, solid powder are completely dissolved.
4. the preparation method of PdPtNi/C nanometers of oxygen reduction catalyst according to claim 1, it is characterised in that:
Round-bottomed flask after step (3) ultrasound is placed directly in the oil bath pan for having been heated to 180 ~ 190 DEG C, is opened simultaneously
Magnetic agitation is opened, 2 ~ 3h is kept the temperature.
5. the preparation method of PdPtNi/C nanometers of oxygen reduction catalyst according to claim 1, it is characterised in that:
Step (4) resulting catalyst is coated onto progress electrocatalytic oxidation reduction reaction on glass carbon working electrode, unified to load
Amount is 80 μ g/cm2。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109709172A (en) * | 2019-01-30 | 2019-05-03 | 中国科学院重庆绿色智能技术研究院 | A kind of electrochemical analysis method and system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109709172A (en) * | 2019-01-30 | 2019-05-03 | 中国科学院重庆绿色智能技术研究院 | A kind of electrochemical analysis method and system |
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