CN106654299B - A kind of metasable state is nanocrystalline and its preparation method and application - Google Patents
A kind of metasable state is nanocrystalline and its preparation method and application Download PDFInfo
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- CN106654299B CN106654299B CN201611000124.5A CN201611000124A CN106654299B CN 106654299 B CN106654299 B CN 106654299B CN 201611000124 A CN201611000124 A CN 201611000124A CN 106654299 B CN106654299 B CN 106654299B
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- nanocrystalline
- acac
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- metasable state
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
-
- 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
- H01M4/9041—Metals or alloys
- H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
- H01M4/9058—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC of noble metals or noble-metal based alloys
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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 belongs to nm regime, specifically disclose that a kind of metasable state is nanocrystalline and its preparation method and application, and nanocrystalline metasable state disclosed in this invention is Pd2MAg is nanocrystalline, and wherein M is Fe, Co, Cu or Mn.It is with excellent ORR performances, ORR that can be in efficient catalytic fuel cell.Simple for process simultaneously, reaction temperature is low, and the time is short, is suitable for producing in batches, meets industrialization production requirements.
Description
Technical field
It is nanocrystalline and its preparation method and application the invention discloses a kind of metasable state, belong to nm regime.
Background technology
As world energy sources need the increasingly increase with environmental problem, renewable H2-O2Fuel cell is in new energy system
In hold the balance, still, cathode O2Reduction reaction (oxygenreductionreaction, ORR) dynamics is slow, is to influence
Its performance and the main bottleneck of application.Although Pt bases catalyst can be catalyzed ORR well, due to Pt reserves on earth
It is limited, cause catalyst cost very high and be difficult to large-scale use, which greatly limits H2-O2Fuel cell it is big
Scale commercial process.Therefore, low cost, high-performance, the elctro-catalyst of long-life are designed and prepare to improve ORR dynamics mistakes
Journey is most important.Literature research shows that Pd- base nanometer crystals are considered as that can substitute the Pt catalysis most effective catalyst of ORR.Together
When significantly, since the increase of component and the abundant adjustability of electronic structure so that polynary Pd- base nanometer crystals are shown
Go out with catalytic performance similar in Pt- base nanometer crystals, thus cause extensive concern recently.Meanwhile the hair of current nanometer technology
It opens up to novel renewable H2-O2The design of fuel cell electro-catalyst brings new opportunity.Especially there is identical chemical composition not
Isostructural metasable state Pd- base nanometer crystals, because of the difference of its special surface atom number, arrangement mode and density of electronic states,
Its performance can be had an important influence on (for example, twin polyhedral structure or metastable phase with more defect are because its is special
Structure generally all has the performance of specificity).In recent years, researcher is to controlledly synthesis high activity metasable state Pd- base nanometers
Crystalline substance produces great interest.For example, Ying seminars in non-aqueous system using multiple twin Ag nano-particles as predecessor,
PdCl is restored in oleyl amine system2With Pt (acac)2, the AgPd@Pt core-shell nanos for being successfully prepared multiple twin structure are brilliant.With ORR
For probe reaction, the results showed that the AgPd@Pt core-shell nanos crystalline substances of multiple twin structure than stable structure there is excellent ORR to live
Property.Therefore, it is one of hot spot studied at present to research and develop efficient high activity metasable state Pd- base nanometer crystal catalyst, renewable
In the evolution of energy technology, the metasable state Pd- base nanometer crystal elctro-catalysts for seeking efficient special construction are of great significance
And huge challenge.
Invention content
The present invention is directed to develop a kind of novel, efficient metasable state Pd- base nanometer crystal catalyst.
For the purpose of it, the invention discloses a kind of metasable state is nanocrystalline, the nanocrystalline Pd of metasable state2MAg nanometers
Crystalline substance, wherein M are Fe, Co, Cu or Mn.The metasable state is nanocrystalline to have preferable hydrogen reduction performance.
Further, it is by Pd (NO that it is nanocrystalline, which to disclose the metasable state, for we3)2·2H2O、Fe(acac)2Or Co
(acac)2Or Cu (acac)2Or Mn (ac)2、AgNO3Reaction generation.
Further, our Pd preferably wherein：M：The molar ratio of Ag is 2:1:1.
The invention also discloses the nanocrystalline preparation methods of this metasable state simultaneously to be：By Pd (NO3)2·2H2O, Fe
(acac)2Or Co (acac)2Or Cu (acac)2Or Mn (ac)2, AgNO3, oleyl amine (OLA) and octadecene (ODE) solution mixing,
250-300 DEG C is gradually warming up to, and is obtained by the reaction at this temperature containing Pd2Product nanocrystalline MAg, be dispersed through sedimentation,
It is centrifugally separating to obtain Pd2MAg is nanocrystalline, and wherein M is Fe, Co, Cu or Mn.
Preferably, we are according to 5 DEG C of -8 DEG C of min-1Heating rate gradually heat up.
Further, we more preferably mode is that reaction process is divided into two stages, first by Pd (NO3)2·
2H2O, Fe (acac)2Or Co (acac)2Or Cu (acac)2Or Mn (ac)2It heats up with oleyl amine (OLA) and octadecene (ODE) solution
To 250-300 DEG C, reaction a period of time, AgNO is added thereafter3Solution, and continue after reacting a period of time at this temperature
Obtain metasable state Pd2Product nanocrystalline MAg, wherein M are Fe, Co, Cu or Mn.
Wherein, the mixed solution dispersing and settling of product normal heptane and absolute ethyl alcohol after preferably reacting.
Preferably, it is Pd (NO the invention also discloses the adding proportion of each component3)2·2H2O 1mmol-0.5mmol, Fe
(acac)2Or Co (acac)2Or Cu (acac)2Or Mn (ac)20.5mmol-0.25mmol, AgNO30.5mmol-0.25mmol,
OLA 6-10mL, ODE 10-20mL.
Further, we give the preferred reaction time as 20-60min.This reaction time is total reaction time,
When reaction is made of two stages, the reaction time summation in two stages is 20-60min.
Metasable state Pd is claimed in the present invention simultaneously2MAg (M=Fe, Co, Cu and Mn) is nanocrystalline in fuel-cell catalyst
In application.Particularly this metasable state Pd2The nanocrystalline applications in ORR is catalyzed of MAg (M=Fe, Co, Cu and Mn).
Pd obtained by the present invention2MAg (M=Fe, Co, Cu and Mn) is nanocrystalline to be penetrated using X-ray energy spectrometer (EDS) and X
Line diffractometer (XRD) characterizes its component and structure；With transmission electron microscope (TEM) and high-resolution perspective electron microscope
(HRTEM) its size, pattern and micro-structure etc. are analyzed.
Pd obtained by the present invention2MAg (M=Fe, Co, Cu and Mn) is nanocrystalline to have excellent ORR performances.After testing certain
A little metasable state Pd2CoAg performances are better than presently commercially available Pt-C, anticipate for renewable energy technologies development with important guidance
Justice.
Involved Pd in the present invention2It is prepared by nanocrystalline chemically reacted by solid liquid phase of MAg (M=Fe, Co, Cu and Mn),
Obtain that there is unique metasable state structure by the way of " treating different things alike " simultaneously, simple for process, reaction temperature is low, and the time is short, is suitble to
In batch production.
Description of the drawings
Fig. 1 is the Pd that the present invention synthesizes2(a) EDS figures nanocrystalline FeAg；(b) XRD diagram；(c) TEM schemes；(d) HREM schemes.
Fig. 2 is the Pd that the present invention synthesizes2(a) EDS figures nanocrystalline CoAg；(b) XRD diagram；(c) TEM schemes；(d) HREM schemes.
Fig. 3 is the Pd that the present invention synthesizes2(a) EDS figures nanocrystalline CuAg；(b) XRD diagram；(c) TEM schemes；(d) HREM schemes.
Fig. 4 is the Pd that the present invention synthesizes2(a) EDS figures nanocrystalline MnAg；(b) XRD diagram；(c) TEM schemes；(d) HREM schemes.
Fig. 5 is the metasable state Pd that the present invention synthesizes2ORR performance test figures nanocrystalline MAg (M=Fe, Co, Cu and Mn).
Specific embodiment
Technical solutions according to the invention are further described in detail below by specific embodiment, but it is necessary to
It points out that following embodiment is served only for the description to invention content, does not form limiting the scope of the invention.
Embodiment 1
At room temperature, 0.5mmol Pd (NO are weighed3)2·2H2O, 0.25mmol Fe (acac)2Or Co (acac)2Or Cu
(acac)2Or Mn (ac)2Be added to dry capacity be 250mL three neck round bottom in, then with graduated cylinder measure 8mL OLA and
10mL ODE are added in three neck round bottom, and three neck round bottom is transferred in sand-bath, with 7 DEG C/min's under temperature programmed control
Rate is warming up at 280 DEG C after heat preservation 20min, adds in 0.25mmol AgNO3Solution continues to keep the temperature 40min, until reaction terminates.
It treats reactor cooled to room temperature, adds in appropriate normal heptane and absolute ethyl alcohol dispersion, centrifuge solid.After solid is washed
Black product is obtained, after being dried in vacuum overnight in vacuum drying chamber, for being analyzed and characterized.
Product is analyzed respectively using EDS, XRD, TEM and HREM test, as a result as shown in Figures 1 to 4.In Fig. 1
EDS shows that sample main component is Pd, Fe and Ag, and XRD shows that the crystalline phase of sample is face-centered cubic phase.TEM shows to obtain nanometer
Crystalline substance is polyhedral structure, and grain size is about 10nm.Further microstructure analysis by HRTEM figures it can be seen that sample exist compared with
Multidigit is wrong, this may have a major impact electrocatalytic reaction.EDS shows that sample main component is Pd, Co and Ag in Fig. 2, and XRD is shown
The crystalline phase of sample product is face-centered cubic phase.It is multiway shape structure that TEM, which shows to obtain nanocrystalline, and the size of each foot is about 5nm.Into
The microstructure analysis of one step is by HRTEM figures it can be seen that multiway shape Pd2CoAg is that have many little particles to merge, particle with
There is fusion dislocation between particle.Literature research shows that multiway shape structure has and increases nanocrystalline specific surface area, provides more
More active sites and Twin Defects, this has a major impact catalytic performance.EDS shows that sample main component is Pd, Cu in Fig. 3
And Ag, XRD show that the crystalline phase of sample is face-centered cubic phase.It is torispherical structure that TEM, which shows to obtain nanocrystalline, and size is about
10nm.Further microstructure analysis is by HRTEM figures it can be seen that torispherical Pd2CuAg is that have apparent Twin Defects.Text
Offer research shows that, Twin Defects increase nanocrystalline active site, this has a major impact catalytic performance.EDS is shown in Fig. 4
Sample main component is Pd, Mn and Ag, and XRD shows that the crystalline phase of sample is face-centered cubic phase.TEM shows to obtain nanocrystalline for spherical shape
Structure, size are about 10nm.Further microstructure analysis is by HRTEM figures it can be seen that spherical shape Pd2MnAg be have it is very complete
Beautiful lattice structure.Equally there are rearrangements in microcell domain discovery particle.Literature research shows that nanocrystalline interior atoms reset production
Raw lattice defect, this has a major impact catalytic performance.
Embodiment 2
Pass through cyclic voltammetry and method of polarization curve, the electrochemical properties of test sample, specific mistake in three-electrode system
Journey is as follows：
Electrochemistry experiment carries out on CHI760e type electrochemical workstations, using three electrode test systems of standard, accordingly
Glass-carbon electrode of the working electrode for the sample modification acquired in this paper, be platinized platinum to electrode, reference electrode is silver/silver chlorate
(Ag/AgCl).All potentials are both with respect to Ag/AgCl herein.Electrolyte is the KOH solution of 0.1M.All electrochemistry are surveyed
Examination carries out at 30 DEG C.Every time during experiment, all modified electrodes are tested in 0.1M KOH solutions.
The preparation method of sample modified electrode is as follows：
Every time before experiment, by the rotating disk electrode (r.d.e) of a diameter of 5mm successively with 1.0 μm, 0.3 μm and 0.05 μm of Al2O3Powder
Minute surface is milled to, is then cleaned by ultrasonic, it is finally clean with second distillation water wash, in room temperature N2Dried for standby under atmosphere.By 2mg's
Pd2MAg (M=Fe, Co, Cu and Mn) is nanocrystalline to be distributed in 1mL water, obtains 2mg mL-1Pd2MAg (M=Fe, Co, Cu and
Mn) nanocrystalline suspension.This suspension of 20 μ L and 5 μ L, 1% naphthol solutions, are successively dispersed in rotating circular disk
Electrode surface N2It is dry in atmosphere, obtain Pd2MAg (M=Fe, Co, Cu and Mn) nanocrystalline modified electrode.
Before ORR tests, high-purity O is first passed through into solution230min, and continue logical O during the experiment2To keep solution
O2Atmosphere.The linear scan polarization curve (LSV) that difference sweeps under speed is also in O2It is carried out in atmosphere, corresponding Electrochemical Scanning speed
Rate is 10mV/s, and scanning range is -0.80V-0.20V.
Testing result is referring to Fig. 5.Test result shows：Each catalyst all has catalytic activity to ORR, catalyst
Catalysis ORR take-off potential be：Pd2Ag ＜ Pd2CuAg ＜ Pd2FeAg ＜ Pd2MnAg ＜ 20%Pt/C ＜ Pd2CoAg.Compared to
Other ternary metals synthesized in same reaction system are nanocrystalline, Pd2The nanocrystalline catalytic oxidation-reductions for showing enhancing of CoAg
Performance.Further analysis reason is it is found that Pd2The nanocrystalline patterns of CoAg are multiway shape structure, and all there are twinning dislocation, so as to increase
Add the active site of catalyst, and then improve ORR performances.
Claims (6)
1. a kind of nanocrystalline preparation method of metasable state, which is characterized in that the metasable state is nanocrystalline nanocrystalline for Pd2MAg,
Middle M is Fe, Co, Cu or Mn, and the nanocrystalline metasable state is by 1. Pd (NO3) 2.2H2O, 2. Fe (acac) 2 or Co (acac)
2 or Cu (acac) 2 or Mn (ac) 2,3. AgNO3 reactions generation, preparation method is, by Pd (NO3) 2.2H2O, Fe (acac) 2
Or Co (acac) 2 or Cu (acac) 2 or Mn (ac) 2, AgNO3, oleyl amine（OLA）And octadecene（ODE）Solution mixes, and gradually rises
Temperature is obtained by the reaction at this temperature to 250-300 °C containing product nanocrystalline Pd2MAg, is dispersed through settling, is centrifuged and divide
Nanocrystalline from Pd2MAg is obtained, wherein M is Fe, Co, Cu or Mn.
2. preparation method according to claim 1, which is characterized in that gradually risen according to the heating rate of 5 DEG C of -8 DEG C of min-1
Temperature.
3. the preparation method according to claim 1 or 2, which is characterized in that reaction process is divided into two stages, first will
Pd (NO3) 2.2H2O, Fe (acac) 2 or Co (acac) 2 or Cu (acac) 2 or Mn (ac) 2 and oleyl amine（OLA）And octadecene
（ODE）Solution is warming up to 250-300 °C, and reaction a period of time adds AgNO3 solution, and continues at this temperature thereafter
The nanocrystalline products of metasable state Pd2MAg are obtained after reaction a period of time, wherein M is Fe, Co, Cu or Mn.
4. preparation method according to claim 1, which is characterized in that the production nanocrystalline containing Pd2MAg obtained after reaction
Object normal heptane and absolute ethyl alcohol mixed solution dispersing and settling.
5. preparation method according to claim 1, which is characterized in that the adding proportion of each component is Pd (NO3) 2.2H2O
1mmol-0.5mmol, Fe (acac) 2 or Co (acac) 2 or Cu (acac) 2 or Mn (ac) 20.5mmol-0.25mmol,
AgNO30.5mmol-0.25mmol, OLA6-10mL, ODE10-20mL.
6. preparation method according to claim 1, which is characterized in that reaction time 20-60min.
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