CN108311691A - A method of the no hot method of templating solvent synthesizes PtCu nanometers of frame materials of dodecahedron - Google Patents

A method of the no hot method of templating solvent synthesizes PtCu nanometers of frame materials of dodecahedron Download PDF

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CN108311691A
CN108311691A CN201810122216.3A CN201810122216A CN108311691A CN 108311691 A CN108311691 A CN 108311691A CN 201810122216 A CN201810122216 A CN 201810122216A CN 108311691 A CN108311691 A CN 108311691A
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ptcu
dodecahedron
nanometers
frame
reaction
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CN108311691B (en
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王爱军
张小芳
冯九菊
黄先燕
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Zhejiang Normal University CJNU
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0549—Hollow particles, including tubes and shells
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • 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

Abstract

The invention discloses a kind of methods that the no hot method of templating solvent synthesizes PtCu nanometers of frame materials of dodecahedron, belong to the synthesis technical field of dodecahedron nanometer frame material.Technical scheme of the present invention main points are：Regulatory molecule hexadecyltrimethylammonium chloride is added in solvent oleyl amine and is uniformly mixed, metal precursor acetylacetone,2,4-pentanedione platinum and copper chloride CuCl is added until completely dissolved in stirring, ultrasound2·2H2O and reducing agent allantoin, mixed solution is added in reaction kettle, in 180 DEG C of fully reaction 10h, is discharged and is washed for several times with the mixed solution of ethyl alcohol and hexamethylene, drying to PtCu nanometers of frame materials of dodecahedron.PtCu dodecahedrons nanometer frame material produced by the present invention can significantly improve it to evolving hydrogen reaction in acid and alkaline medium（HER）Catalytic activity.

Description

A method of the no hot method of templating solvent synthesizes PtCu nanometers of frame materials of dodecahedron
Technical field
The invention belongs to the synthesis technical fields of dodecahedron nanometer frame material, and in particular to a kind of no hot method of templating solvent Synthesize PtCu nanometers of frames of dodecahedron（PtCu DNFs）The method of material.
Background technology
A series of problems that the energy consumes and combustion of fossil fuel causes has received widespread attention, and develops reproducible Green energy resource is the grand strategy route solved these problems.It is well known that Pt nano materials are that most have in many important applications The catalyst of effect, but Pt catalyst is at high price, kinetics process is slow and stability is poor.Therefore, for a long time, make The problem of standby nanocatalyst is how to improve the catalytic activity and rate of metal of Pt base catalyst.
Currently, solution primarily rests on the following aspects：1）With transition metal alloy, precious metals pt is reduced Usage amount improves its catalytic performance simultaneously；2）The pattern and structure for regulating and controlling Pt base catalyst, improve the active site on surface； 3）The nanostructure for building inner hollow, increases the utilization ratio of noble metal.However, catalyst tends to gather during the reaction Collection or sintering, lead to the significant reduction of catalyst activity, therefore, how the steady of catalyst are improved while ensureing catalyst activity Qualitative is still the problem for needing to solve at present.And there is the exploitation of the nanometer frame material of the three-dimensional structure of high opening and set It is calculated as capturing this problem and brings new opportunity, this nanometer frame material with unique texture not only remains big ratio Surface area, while can effectively mitigate aggregation and sintering, improve the catalytic activity and stability of catalyst.
The synthesis strategy of nanometer frame material can be divided into two major classes：Site selection deposition and etching and nanocrystal go to close Aurification, these hollow out mechanism are mostly derived from displacement reaction, oxide etch, the multiple action of atoms permeating or their combinations in particle Under synergistic mechanism.Synthetic method described above is mainly examined from the factors such as oxidation-reduction potential, stability of metal between metal Consider, designs the three-dimensional Pt based alloys nanometer frame structure of morphology controllable.However nanometer frame is highly prone in forming process The influence of element composition, temperature, regulatory molecule and reducing agent, therefore, the nanocrystalline adjusting and controlling growth system of Development of Novel frame is adjusted Element composition, surface texture, pattern and the physical size of nanometer frame, to optimize its catalytic performance, this nanometer of frame of further investigated Application of the frame in energy catalysis.
Invention content
The present invention is avoids the use of template in the prior art and etchant from providing a kind of simple for process and is easy to real The existing method for synthesizing PtCu nanometers of frame materials of dodecahedron without the hot method of templating solvent.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, and a kind of no hot method of templating solvent synthesizes 12 faces The method of PtCu nanometers of frame materials of body, it is characterised in that the specific steps are：Regulatory molecule hexadecyltrimethylammonium chloride is added Enter into solvent oleyl amine and be uniformly mixed, metal precursor acetylacetone,2,4-pentanedione platinum and chlorination is added until completely dissolved in stirring, ultrasound Copper CuCl2·2H2O and reducing agent allantoin, the wherein molar concentration of hexadecyltrimethylammonium chloride are 25mM, acetylacetone,2,4-pentanedione The molar concentration of platinum is 2mM, and the molar concentration of copper chloride is 2mM, and the molar concentration of allantoin is 25mM, and mixed solution is added Into reaction kettle, in 180 DEG C of fully reaction 10h, discharges and washed for several times with the mixed solution of ethyl alcohol and hexamethylene, drying To PtCu nanometers of frame materials of dodecahedron.
Further preferably, the cube in PtCu nanometers of frame material obtained is evenly dispersed dodecahedron nanometer frame, The dodecahedron nanometer mount structure formed detailed process be：Metal precursor copper chloride is reduced into Cu atoms, metal precursor The experience displacement reaction of acetylacetone,2,4-pentanedione platinum ultimately forms PtCu cores, in the presence of regulatory molecule hexadecyltrimethylammonium chloride, shape At PtCu cores selectivity along the vertex of { 110 } crystal face and edge precipitation dissolving, formed after the reaction time for undergoing 2h solid Rich in the nanocrystalline of Cu, as time went on to 6h, solid pattern gradually forms hollow-core construction under metathesis, with the time 10h is extended to, hollow intermediate undergoes bimetallic displacement reaction, ultimately forms dodecahedron frame structure.
Compared with the prior art, the present invention has the following advantages：The PtCu DNFs materials of the present invention are using no templating solvent Hot method is prepared, and preparation method is simple, black compared to business Pt/C and Pt, dodecahedron PtCu nanometers of frames produced by the present invention Material can significantly improve it to evolving hydrogen reaction in acid and alkaline medium（HER）Catalytic activity.
Description of the drawings
Fig. 1 is the transmission electron microscope picture under PtCu DNFs material different multiplyings, and wherein C, D, the illustration in E is corresponding Structural model, the illustration in a, b is Fast Fourier Transform（FFT）Figure；
Fig. 2 is PtCu DNFs material formation process schematic diagrames；
A is PtCu DNFs, Pt/C and the black polarization curves in 0.5M KOH solutions of Pt in Fig. 3, and B is Tafel slope, C It is -0.05V for HER polarization curves before and after the 1000 circle loop tests in the 0.5M KOH solutions that nitrogen is saturated and Dvs. Chronoa mperometric plot figure under NHE current potentials；
A is that PtCu DNFs, Pt/C and Pt are black in 0.5M H in Fig. 42SO4HER figures in solution, B is Tafel slope, C be The 0.5M H of nitrogen saturation2SO4HER polarization curves and D are -0.03V before and after 1000 circle loop tests in solutionvs.NHE electricity Chronoa mperometric plot figure under position.
Specific implementation mode
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on the above of the present invention belong to this hair Bright range.
Embodiment 1
Reagent and instrument
Hexadecyltrimethylammonium chloride, acetylacetone,2,4-pentanedione platinum, copper chloride（CuCl2·2H2O）, ethanol amine, oleyl amine, dimethyl-silicon Oil, ethyl alcohol, hexamethylene buy Shanghai Chemical Plant, and all reagents are that analysis is pure.Scanning electron microscope（SEM, JSM- 6390LV, JEOL, Japan）, transmission electron microscope（TEM, JEM-2100, JEOL, Japan）, accelerating potential 200kV, The chemical composition of PtCu DNFs materials is by energy disperse spectroscopy（EDX, Oxford）, X-ray diffraction（XRD）To determine.
By regulatory molecule hexadecyltrimethylammonium chloride（CTAC 25mM）It is added to solvent oleyl amine（20mL）Middle mixing is equal It is even, stirring, ultrasound, after dissolving after, metal precursor acetylacetone,2,4-pentanedione platinum and copper chloride CuCl is added2·2H2O and reducing agent urine Bursin, the wherein molar concentration of acetylacetone,2,4-pentanedione platinum are 2mM, and the molar concentration of copper chloride is 2mM, and the molar concentration of allantoin is Mixed solution is added in reaction kettle by 25mM, in 180 DEG C of fully reaction 10h, is discharged and molten with the mixing of ethyl alcohol and hexamethylene Liquid washs for several times, drying to PtCu nanometers of frame materials of dodecahedron.
Fig. 1 is the transmission electron microscope picture Fast Fourier Transform figure of PtCu DNFs materials.As seen from the figure, prepared nanometer Material is made of evenly dispersed hollow cube, and single nanostructure shows that this hollow cube is dodecahedron nanometer Frame, nanometer mount structure surface are conducive to improve surface-active and then enhance its catalytic performance there are twin.The quick Fourier of Fig. 1 Leaf transformation figure confirms its good crystalline structure.
Fig. 2 is the growth mechanism of PtCu DNFs materials, and the formation of dodecahedron nanometer mount structure can be divided into two steps：Before Drive the reduction of body copper chloride, the displacement between copper and platinum ion.According to pertinent literature, Cu ratios Pt is first restored, metal precursor chlorination Copper reduction is at Cu atoms, and the experience displacement reaction of metal precursor acetylacetone,2,4-pentanedione platinum ultimately forms PtCu cores, in regulatory molecule 16 In the presence of alkyl trimethyl ammonium chloride, the PtCu cores selectivity of formation is along the vertex of { 110 } crystal face and edge precipitation dissolving, warp After going through the reaction time of 2h, formation is solid nanocrystalline rich in Cu, as time went on to 6h, the solid pattern under metathesis Hollow-core construction is gradually formed, as time went on to 10h, hollow intermediate undergoes bimetallic displacement reaction, ultimately generates ten Dihedron nanometer mount structure.
Fig. 3 is PtCu DNFs materials under alkaline condition to evolving hydrogen reaction（HER）Catalytic applications.A in Fig. 3 is PtCu DNFs, Pt/C and the black polarization curves in 0.5M KOH solutions of Pt, PtCu DNFs' plays spike potential（-25mV）It wants Than business Pt/C（-28mV）It is black with Pt（-58mV）Corrigendum, and Tafel slope（55mV dec–1）It is less than control material Pt/ C（64mV dec–1）And Pt is black（81mV dec–1）, this demonstrate that PtCu DNFs catalyst in alkaline medium to HER have compared with Good catalytic activity.C and D is that HER polarization is bent before and after 1000 circle loop tests in the 0.5M KOH solutions that nitrogen is saturated in Fig. 3 Line chart and chronoa mperometric plot figure, by scheming C it is found that before and after loop test, polarization curve essentially coincides, and it is preferable steady to illustrate it Qualitative, in scheming D, PtCu DNFs materials are in -0.05VvsCurrent density fall under NHE current potentials（16%）It is less than Pt/C（47.2%）It is black with Pt（73.8%）, the result further demonstrate PtCu DNFs materials with superior catalytic performance and Stability.
Fig. 4 is PtCu DNFs materials in acid condition to evolving hydrogen reaction（HER）Catalytic applications.A in Fig. 4 is PtCu DNFs, Pt/C and Pt are black in 0.5M H2SO4Polarization curve in solution, PtCu DNFs' plays spike potential（-27mV） Than business Pt/C（-32mV）It is black with Pt（-63mV）Corrigendum, and Tafel slope（34mV dec–1）It is suitable with Pt/C's, but It is more black than Pt（45mV dec–1）It is much smaller, this demonstrate that PtCu DNFs catalyst in acid medium to HER have it is superior Catalytic activity.C and D is the 0.5M H being saturated in nitrogen in Fig. 32SO4HER polarization curves before and after 1000 circle loop tests in solution Figure and chronoa mperometric plot figure, by scheming C it is found that before and after loop test, polarization curve essentially coincides, and it is preferable stable to illustrate it Property, figure D stability test in, PtCu DNFs materials in -0.03VvsCurrent density fall under NHE current potentials （8.4%）It is less than Pt/C（10.3%）It is black with Pt（44.7%）, the result further demonstrate PtCu DNFs materials have it is superior Catalytic performance and stability.
Embodiment 2
In this example, regulatory molecule CTAC concentration changes（10mM, 35mM）, other experiment conditions are with reference to embodiment 1, guarantor Hold constant, the PtCu NPs materials being prepared are shown in the body of the email, and when reducing the concentration of regulatory molecule, hollow-core construction is endless Entirely, when increasing regulatory molecule concentration to 35mM, agglomeration is than more serious.
Embodiment 3
In the present embodiment, it is used for substituting allantoin with another reducing agent 6- amino-uracils, other experiment conditions are with reference to real Example 1 is applied, is remained unchanged, the PtCu NPs materials being prepared show that pattern is no longer hollow cube knot in backing material Structure.
According to example 1-3 it is found that reaction time, regulatory molecule in the construction process of dodecahedron nanometer frame（CTAC）Concentration And the control of the type of reducing agent is vital.
Embodiment above describes the basic principles and main features and advantage of the present invention, and the technical staff of the industry should Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within In the scope of protection of the invention.

Claims (2)

1. a kind of method of the hot method synthesis PtCu nanometers of frame materials of dodecahedron of no templating solvent, it is characterised in that specific steps For：Regulatory molecule hexadecyltrimethylammonium chloride is added in solvent oleyl amine and is uniformly mixed, stirring, ultrasound wait for completely molten Metal precursor acetylacetone,2,4-pentanedione platinum and copper chloride CuCl is added in Xie Hou2·2H2O and reducing agent allantoin, wherein cetyl three The molar concentration of ammonio methacrylate is 25mM, and the molar concentration of acetylacetone,2,4-pentanedione platinum is 2mM, and the molar concentration of copper chloride is 2mM, urine The molar concentration of Bursin is 25mM, and mixed solution is added in reaction kettle, in 180 DEG C of fully reaction 10h, discharges and uses ethyl alcohol And the mixed solution washing of hexamethylene is for several times, drying to PtCu nanometers of frame materials of dodecahedron.
2. the method for the hot method synthesis PtCu nanometers of frame materials of dodecahedron of no templating solvent according to claim 1, special Sign is：Cube in PtCu nanometers of frame material obtained is evenly dispersed dodecahedron nanometer frame, which receives Rice mount structure formed detailed process be：Metal precursor copper chloride is reduced into Cu atoms, metal precursor acetylacetone,2,4-pentanedione platinum warp It goes through displacement reaction and ultimately forms PtCu cores, in the presence of regulatory molecule hexadecyltrimethylammonium chloride, the PtCu cores of formation select Selecting property forms the solid nanometer rich in Cu along the vertex of { 110 } crystal face and edge precipitation dissolving after the reaction time for undergoing 2h Crystalline substance, as time went on to 6h, solid pattern gradually forms hollow-core construction under metathesis, empty as time went on to 10h Mesosome undergoes bimetallic displacement reaction in the heart, ultimately forms dodecahedron frame structure.
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