CN109273731A - A kind of 3D porous network structure Pd3Pb alloy and preparation method and applications - Google Patents

A kind of 3D porous network structure Pd3Pb alloy and preparation method and applications Download PDF

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Publication number
CN109273731A
CN109273731A CN201811098657.0A CN201811098657A CN109273731A CN 109273731 A CN109273731 A CN 109273731A CN 201811098657 A CN201811098657 A CN 201811098657A CN 109273731 A CN109273731 A CN 109273731A
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alloy
preparation
added
network structure
porous network
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石乃恩
杨瑞
王涛
韩敏
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Nanjing Post and Telecommunication University
Nanjing University of Posts and Telecommunications
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Nanjing Post and Telecommunication University
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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
    • 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
    • H01M4/928—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
    • 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

Present invention discloses a kind of 3D porous network structure Pd3The preparation method of Pb alloy, comprising the following steps: be surfactant B rij-58 to be dissolved in the solution for being made into that concentration is 0.15-0.3 mol/l in the solvent of DMPU, ultrasonic 2-10 min, then carry out magneton stirring 20-40 min first, form uniform dispersion liquid；Followed by 1-3 mL octadecylene will be added in dispersion liquid, continues to stir 2-10 min, form micella；It is first to be dispersed in palladium source and lead source in 5-10 mL distilled water according to the ratio that molar ratio is 3:1 later, ultrasonic 2-10 min forms uniform mixed solution；Followed by mixed solution is added in micella, 20-40 min is stirred, uniform micellar solution is formed；It is finally tetrabutyl ammonia borine to be added in micellar solution, and be packed into reaction kettle, heat up and react 8-12 h, after room temperature, is centrifugated, washs, being dried to obtain the Pd of 3D porous network structure3Pb alloy.Preparation method of the invention is simple, has excellent performance, and stability is good, and the Pd according to obtained by hydro-thermal method3Pb alloy shows excellent electro-catalysis ORR performance.

Description

A kind of 3D porous network structure Pd3Pb alloy and preparation method and applications
Technical field
The present invention relates to a kind of alloy and preparation method and application more particularly to a kind of 3D porous network structure Pd3Pb is closed The preparation method and application of gold belongs to nano material synthesis field.
Background technique
For a long time, fuel cell has always been considered as being most potential one of the generator of various energy conversion devices, because Has many advantages, such as the discharge of high-energy density low pollution object for it.Oxygen reduction reaction (ORR) is the key that fuel cell half-reaction, so And it usually has slow dynamics and needs effective elctro-catalyst to drive.Although platinum (Pt) base catalyst has Excellent electrocatalysis characteristic, but its scarcity and high cost seriously hinder commercialized development.
Sabatier principle show palladium be catalyzed ORR the second largest active metal, and its activity by with transition metal M(M=Co, Ni, Fe etc.) alloying can further enhance.Meanwhile the adjusting of elctro-catalyst dimension also affects catalysis and lives Property.3D structure has biggish specific surface area, is easily formed conductive network, is conducive to the transmission of electronics, and porous structure is mentioning The transmission of electrolyte is also helped while high surface area.
In conclusion how to provide a kind of Pd and 3D porous network structure is prepared in cheap transition metal Pb alloying Elctro-catalyst, and this material is applied in electro-catalysis ORR, just become those skilled in the art's urgent problem to be solved.
Summary of the invention
The object of the present invention is to provide a kind of 3D porous network structure Pd3The synthetic method of Pb alloy material, passes through Simple and easy additional reducing agent hydro-thermal method synthetic mesh structure Pd3Pb alloy, this method simple process, repeatability are strong；Separately Outside, the present invention can pass through the temperature of change hydro-thermal reaction, controllable adjustment Pd3The growth of Pb alloy and pattern produce different differences Different ORR performance, and the Pd that optimum condition obtains is provided3Application of the Pb alloy material as elctro-catalyst in ORR.
The technical solution of the invention is as follows:
A kind of 3D porous network structure Pd3The preparation method of Pb alloy, comprising the following steps:
Surfactant B rij-58: being dissolved in the solution for being made into that concentration is 0.15-0.3 mol/l in the solvent of DMPU by S1, Ultrasonic 2-10 min, then magneton stirring 20-40 min is carried out, form uniform dispersion liquid；
S2: being added the octadecylene of 1-3 mL in step sl in resulting dispersion liquid, continue to stir 2-10 min, form micella；
S3: palladium source and lead source are dispersed in 5-10 mL distilled water according to the ratio that molar ratio is 3:1, ultrasonic 2-10 min, shape At uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 20-40 min, is formed equal Even micellar solution；
S5: reducing agent tetrabutyl ammonia borine being added in micellar solution obtained in step S4, and is quickly charged with reaction kettle, is risen Temperature simultaneously reacts 8-12 h, after room temperature, is centrifugated, washs, being dried to obtain the Pd of 3D porous network structure3Pb Alloy.
Preferably, warming temperature is 90-150 DEG C in the step S5.
Preferably, the palladium source in the step S3 is palladium acetate, and lead source is lead acetate.
Preferably, a kind of 3D porous network structure Pd3The preparation method of Pb alloy, includes the following steps
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6g reducing agent tetrabutyl ammonia borine is added in micellar solution obtained in step S4, and is quickly charged with reaction Kettle is warming up to 120 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D porous web after room temperature The Pd of shape structure3Pb alloy.
Preferably, a kind of 3D porous network structure Pd3The preparation method of Pb alloy, comprising the following steps:
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6 g reducing agent tetrabutyl ammonia borines are added in micellar solution obtained in step S4, and are quickly charged with reaction Kettle is warming up to 90 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D holey after room temperature The Pd of structure3Pb alloy.
Preferably, a kind of 3D porous network structure Pd3The preparation method of Pb alloy, comprising the following steps:
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6g reducing agent tetrabutyl ammonia borine is added in micellar solution obtained in step S4, and is quickly charged with reaction Kettle is warming up to 150 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D porous web after room temperature The Pd of shape structure3Pb alloy.
It is a kind of to use 3D porous network structure Pd3The Pd of the preparation method preparation of Pb alloy3Pb alloy, the Pd3Pb alloy Crystal structure be in cubic phase, and the spacing between lattice be 2.02-2.32 nm.
It is a kind of to use 3D porous network structure Pd3The Pd of the preparation method preparation of Pb alloy3Pb alloy, the Pd3Pb alloy Structure be in granular form, and the diameter of the particle be 5-20 nm.
It is a kind of to use 3D porous network structure Pd3The Pd of the preparation method preparation of Pb alloy3The purposes of Pb alloy, by Pd3Pb Alloy is used for electrocatalytic oxidation reduction reaction as elctro-catalyst.
The present invention provides a kind of 3D porous network structure Pd3Pb alloy and preparation method and application, the main body of advantage It is present:
(1) Pd of 3D porous network structure is prepared using reduction hydro-thermal method by the present invention3Pb alloy, wherein surfactant The addition of Brij-58 can not only provide soft template, and the hole configurations and size of adjustable product；Meanwhile ODE Addition be not only advantageous to form micella A, and ensure that the uniformity of nucleation；In addition, the adjusting for passing through hydrothermal temperature Control Pd3The growth of Pb alloy, to influence Pd3Performance of the Pb alloy catalyst in ORR, preparation method is simple, and performance is excellent Different, stability is good.
(2) present invention Pd according to obtained by hydro-thermal method3Pb alloy shows excellent electro-catalysis ORR performance, wherein Under 120 DEG C of reaction temperatures, obtained Pd3Pb alloy has the take-off potential and bigger Limited diffusion current density of corrigendum, Its ORR activity is close to business Pt/C catalyst.
(3) additions in the source Pb reduces the cost of catalyst in the present invention, and the use of surfactant is expected to substitute quotient Industry Pt catalyst is in alkaline fuel cell.
Just attached drawing in conjunction with the embodiments below, the embodiment of the present invention is described in further detail, so that of the invention Technical solution is more readily understood, grasps.
Detailed description of the invention
Fig. 1 is 3D porous network structure Pd in the present invention3The preparation method flow chart of Pb alloy；
Fig. 2 is the Pd of 3D porous network structure in the present invention3The EDS map of Pb alloy；
Fig. 3 is the Pd of 3D porous network structure in the present invention3The XRD map of Pb alloy；
Fig. 4 A is the Pd of 3D porous network structure in the present invention3The TEM of Pb alloy schemes；
Fig. 4 B is the Pd of 3D porous network structure in the present invention3The HRTEM of Pb alloy schemes；
Fig. 5 A is the Pd of 3D porous network structure in the present invention3The HAADF-STEM of Pb alloy schemes；
Fig. 5 B is the Pd distribution diagram of element of corresponding region in Fig. 5 A；
Fig. 5 C is corresponding region Pb distribution diagram of element in Fig. 5 A；
Fig. 6 A is the TEM figure of 90 DEG C of hydrothermal temperature obtained Pd-Pb alloys in the present invention；
Fig. 6 B is the XRD diagram of 90 DEG C of hydrothermal temperature obtained Pd-Pb alloys in the present invention；
Fig. 6 C is the TEM figure of 150 DEG C of hydrothermal temperature obtained Pd-Pb alloys in the present invention；
Fig. 6 D is the XRD diagram of 150 DEG C of hydrothermal temperature obtained Pd-Pb alloys in the present invention；
Fig. 7 is the Pd of 3D porous network structure in the present invention3The ORR performance test figure of Pb alloy；
Fig. 8 is to obtain Pd under different temperatures in the present invention3ORR performance comparison figure of the Pb alloy in the case where revolving speed is 1600 rpm.
Specific embodiment
A kind of preparation method of 3D porous network structure Pd3Pb alloy, as shown in Figure 1, comprising the following steps:
Surfactant B rij-58: being dissolved in the solution for being made into that concentration is 0.15-0.3 mol/l in the solvent of DMPU by S1, Ultrasonic 2-10 min, then magneton stirring 20-40 min is carried out, form uniform dispersion liquid；
S2: being added the octadecylene of 1-3 mL in step sl in resulting dispersion liquid, continue to stir 2-10 min, form micella；
S3: palladium source and lead source are dispersed in 5-10 mL distilled water according to the ratio that molar ratio is 3:1, ultrasonic 2-10 min, shape At uniform mixed solution；Wherein, palladium source is palladium acetate, and lead source is lead acetate；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 20-40 min, is formed equal Even micellar solution；
S5: reducing agent tetrabutyl ammonia borine being added in micellar solution obtained in step S4, and is quickly charged with reaction kettle, is risen Temperature simultaneously reacts 8-12 h, after room temperature, is centrifugated, washs, being dried to obtain the Pd of 3D porous network structure3Pb Alloy, wherein warming temperature is 90-150 DEG C.
Technical solutions according to the invention are further described in detail below by way of specific embodiment:
The Pd of 1 3D porous network structure of embodiment3The preparation of Pb alloy
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6g reducing agent tetrabutyl ammonia borine is added in micellar solution obtained in step S4, and is quickly charged with reaction Kettle is warming up to 120 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D porous web after room temperature The Pd of shape structure3Pb alloy.
Using EDS, XRD and element M apping test the Pd to obtained 3D porous network structure3Pb alloy compositions carry out Analysis, such as Fig. 2, Fig. 3, from the organic capping reagent and air that are adsorbed on surface, remaining is at the peak of C and O in Fig. 2 The peak of bis- kinds of elements of Pd, Pb, atom number ratio show that resulting materials may be Pd close to 3:13Pb alloy.Diffraction in Fig. 3 Peak and standard card correspond, it was demonstrated that obtained product is Pd3Pb alloy.From Pd3The HAADF-STEM of Pb alloy schemes and phase The distribution diagram of element in region is answered it is found that again demonstrating two kinds of elements of Pd, Pb as shown in Fig. 5 A, Fig. 5 B, Fig. 5 C and being evenly distributed on Pd3In Pb alloy.
Schemed using TEM and HRTEM, as shown in Fig. 4 A, Fig. 4 B, to obtained Pd3Pb alloy pattern is analyzed, can be with See Pd of the invention3Pb alloy is 3D porous network structure.It can be seen that clearly lattice item from the HRTEM figure of Fig. 4 B Line shows Pd of the invention3Pb alloy crystallinity is good.By measurement, the spacing of lattice of plane is 2.02 nm-2.32 nm, It can determine that the present invention obtains the Pd for cubic phase3Pb alloy (JCPDS-50-1631).
The Pd of 2 nanoparticle structure of embodiment3The preparation of Pb alloy
A kind of 3D porous network structure Pd3The preparation method of Pb alloy, comprising the following steps:
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6 g reducing agent tetrabutyl ammonia borines are added in micellar solution obtained in step S4, and are quickly charged with reaction Kettle is warming up to 90 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D holey after room temperature The Pd of structure3Pb alloy.
Using TEM to Pd3Pb alloy pattern is analyzed, and as shown in Figure 6A, obtains granular structure, diameter about exists 5-20 nm, size are uniform.XRD diffraction maximum and standard card in Fig. 6 B correspond, it was demonstrated that have obtained cubic phase Pd3Pb alloy (JCPDS-50-1631).
The preparation of the Pd3Pb alloy of 3 3D porous network structure of embodiment
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6g reducing agent tetrabutyl ammonia borine is added in micellar solution obtained in step S4, and is quickly charged with reaction Kettle is warming up to 150 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D porous web after room temperature The Pd of shape structure3Pb alloy.
Using TEM to Pd3Pb alloy pattern is analyzed, and such as Fig. 6 C, obtains three-dimensional porous reticular structure, but size is big It is small inhomogenous, there is clustering phenomena.XRD diffraction maximum and standard card in Fig. 6 D correspond, it was demonstrated that have obtained cubic phase Pd3Pb alloy (JCPDS-50-1631).
It is a kind of to use 3D porous network structure Pd3The Pd of the preparation method preparation of Pb alloy3The purposes of Pb alloy is will Pd3Pb alloy is used for electrocatalytic oxidation reduction reaction as elctro-catalyst.
It is a kind of to use 3D porous network structure Pd3The Pd of the preparation method preparation of Pb alloy3The purposes of Pb alloy passes through following Embodiment illustrates Pd3Pb alloy is used for electrocatalytic oxidation reduction reaction as elctro-catalyst.
Pd3Pb alloy is as follows as test method of the elctro-catalyst in electrocatalytic oxidation reduction reaction: weighing 2.5 mg's Pd3Pb alloy material is dissolved in the mixed solution of 0.5 mL deionized water, 0.5 mL dehydrated alcohol and 40 μ L naphthols, the mixing The concentration of solution is 2.5 mg/mL, ultrasonic disperse most homogeneous mixture solotion.
It takes 16 μ L homogeneous mixture solotions and is added dropwise on clean Rotation ring disk electrode glass-carbon electrode, after dry, repetition takes 16 The μ L homogeneous mixture solotion is simultaneously added dropwise on clean Rotation ring disk electrode glass-carbon electrode, can be used to electro-chemical test after dry.
For electrocatalytic oxidation reduction reaction, first in N2Cyclic voltammetry is carried out in the solution of 0.1 M KOH of saturation. After it is stablized, gas is changed into O2And be passed through in the mixed solution, cyclic voltammetry is equally carried out, is carried out after it is stablized The measurement of polarization curve under different rotating speeds.
As a result as shown in Figure 7, Figure 8, the Pd that different hydrothermal temperatures obtain3In Pb alloy material, at 120 DEG C of reaction temperature When, the Pd of obtained 3D porous network structure3Pb alloy has most excellent electrocatalytic oxidation reduction reaction performance, take-off potential It is respectively 0.95 V vs. RHE and 0.83 V vs. RHE with half wave potential, catalytic performance is better than the Pd of other temperature3Pb is closed Gold.
In conclusion having investigated gained 3D porous network structure using electrocatalytic oxidation reduction reaction as probe reaction Pd3Pb alloy electrocatalysis characteristic.The result shows that Pd obtained by hydro-thermal method3Pb alloy shows excellent electro-catalysis electrocatalytic oxidation Reduction reaction performance, wherein under 120 DEG C of reaction temperatures, obtained Pd3Pb alloy is with the take-off potential corrected and bigger Limited diffusion current density, electrocatalytic oxidation reduction reaction activity close to business Pt/C catalyst, thus we conclude that should The activity of catalyst, which reacts with it temperature, close association.The addition in the source Pb reduces the cost and its preparation of catalyst The advantages that method is simple, has excellent performance, and stability is good is expected to substitution business Pt catalyst in alkaline fuel cell.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and this Field technical staff can be designed alternative embodiment without departing from the scope of the appended claims.

Claims (9)

1. a kind of 3D porous network structure Pd3The preparation method of Pb alloy, which comprises the following steps:
Surfactant B rij-58: being dissolved in the solution for being made into that concentration is 0.15-0.3 mol/l in the solvent of DMPU by S1, Ultrasonic 2-10 min, then magneton stirring 20-40 min is carried out, form uniform dispersion liquid；
S2: being added the octadecylene of 1-3 mL in step sl in resulting dispersion liquid, continue to stir 2-10 min, form micella；
S3: palladium source and lead source are dispersed in 5-10 mL distilled water according to the ratio that molar ratio is 3:1, ultrasonic 2-10 min, shape At uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 20-40 min, is formed equal Even micellar solution；
S5: reducing agent tetrabutyl ammonia borine being added in micellar solution obtained in step S4, and is quickly charged with reaction kettle, is risen Temperature simultaneously reacts 8-12 h, after room temperature, is centrifugated, washs, being dried to obtain the Pd of 3D porous network structure3Pb Alloy.
2. a kind of 3D porous network structure Pd according to claim 13The preparation method of Pb alloy, it is characterised in that: described Warming temperature is 90-150 DEG C in step S5.
3. a kind of 3D porous network structure Pd according to claim 13The preparation method of Pb alloy, it is characterised in that: described Palladium source in step S3 is palladium acetate, and lead source is lead acetate.
4. a kind of 3D porous network structure Pd according to claim 23The preparation method of Pb alloy, it is characterised in that: including Following steps:
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6g reducing agent tetrabutyl ammonia borine is added in micellar solution obtained in step S4, and is quickly charged with reaction Kettle is warming up to 120 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D porous web after room temperature The Pd of shape structure3Pb alloy.
5. a kind of 3D porous network structure Pd according to claim 23The preparation method of Pb alloy, it is characterised in that: including Following steps:
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6 g reducing agent tetrabutyl ammonia borines are added in micellar solution obtained in step S4, and are quickly charged with reaction Kettle is warming up to 90 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D holey after room temperature The Pd of structure3Pb alloy.
6. a kind of 3D porous network structure Pd according to claim 23The preparation method of Pb alloy, it is characterised in that: including Following steps:
S1: being dissolved in wiring solution-forming in the solvent of 20 ml DMPU for the surfactant B rij-58 of 5.0 g, 5 min of ultrasound, Magneton is carried out again and stirs 30 min, forms uniform dispersion liquid；
S2: being added the octadecylene of 1 mL in step sl in resulting dispersion liquid, continue to stir 5 min, form micella；
S3: palladium acetate and lead acetate are dispersed in 8 mL distilled water according to the ratio that molar ratio is 3:1,7 min of ultrasound are formed Uniform mixed solution；
Mixed solution obtained in step S3: being added to the micella formed in step S2 by S4, stirs 30 min, is formed uniform Micellar solution；
S5: 1.6g reducing agent tetrabutyl ammonia borine is added in micellar solution obtained in step S4, and is quickly charged with reaction Kettle is warming up to 150 DEG C, and reacts 10 h and be centrifugated, wash, being dried to obtain 3D porous web after room temperature The Pd of shape structure3Pb alloy.
7. a kind of 3D porous network structure Pd according to claim 43The Pd of the preparation method preparation of Pb alloy3Pb alloy, It is characterized by: the Pd3The crystal structure of Pb alloy is in cubic phase, and the spacing between lattice is 2.02-2.32 nm.
8. a kind of 3D porous network structure Pd according to claim 53The Pd of the preparation method preparation of Pb alloy3Pb alloy, It is characterized by: the Pd3The structure of Pb alloy is in granular form, and the diameter of the particle is 5-20 nm.
9. a kind of use 3D porous network structure Pd a method according to any one of claims 1-33The preparation method preparation of Pb alloy Pd3The purposes of Pb alloy, it is characterised in that: by Pd3Pb alloy is used for electrocatalytic oxidation reduction reaction as elctro-catalyst.
CN201811098657.0A 2018-09-20 2018-09-20 A kind of 3D porous network structure Pd3Pb alloy and preparation method and applications Pending CN109273731A (en)

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