CN110212206A - A kind of recessed shape of octahedron PtCuNi alloy nanoparticle and preparation method thereof - Google Patents
A kind of recessed shape of octahedron PtCuNi alloy nanoparticle and preparation method thereof Download PDFInfo
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- CN110212206A CN110212206A CN201910401100.8A CN201910401100A CN110212206A CN 110212206 A CN110212206 A CN 110212206A CN 201910401100 A CN201910401100 A CN 201910401100A CN 110212206 A CN110212206 A CN 110212206A
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- H01M4/90—Selection of catalytic material
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- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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Abstract
The present invention relates to PtCuNi alloy nanoparticles of a kind of concave surface shape of octahedron and preparation method thereof.The present invention is with chloroplatinic acid, copper chloride and nickel chloride are raw material, it is Morphological control agent by reducing agent, glycine and NaI of PVP, and the ethanol amine of certain content is added, the higher concave surface shape of octahedron PtCuNi alloy nano particle of selectivity is prepared in a short time under microwave heating condition, reduces energy consumption and preparation method green cleans.The PtCuNi alloy nano particle of the concave surface shape of octahedron of acquisition not only shows good chemical property and good activity stability, is with a wide range of applications.
Description
Technical field
The invention belongs to function nano alloy fields.Specifically, the present invention be prepared using microwave irradiation it is a kind of recessed
Shape of octahedron PtCuNi alloy nano particle.
Background technique
Precious metals pt nano-structured calalyst is widely used in industry due to its excellent catalytic performance and thermal stability
Catalysis, bionic, the fields such as electro-catalysis.But due to some restraining factors in practical applications, such as easily poisoning, the service life it is short with
And it is at high price, so that this excellent nanocatalyst can not further genralrlization and application.Research worker is in order to solve this
A little problems substitute Pt frequently with by cheap 3d transition metal element part at present, form Pt base binary/multicomponent alloy and urge
Agent, and controlled by condition, probe into its pattern, the relationship of composition and stable in catalytic performance.
In numerous transition metal elements, Cu and Ni respectively as one of transition metal element more abundant on the earth,
It is that Pt base bianry alloy preferably selects.The report for preparing PtCuNi alloy nanoparticle submethod at present is less, and these methods
It is all organic solvent macromolecular as solvent, most of PtCuNi alloy nano particle being synthesized is wrapped up by organic matter, living
Property position cannot expose, can not be in contact with reactant, and hydrothermal synthesis generate Sample crystals nucleation mostly first along chamber wall shape
At further growing, cause inevitable energy dissipation and inefficiency.A kind of microwave heating preparation that the present invention develops
The method of concave surface octahedron PtCuNi alloy nano particle, not only substantially increases the step atomicity of Pt, increases PtCuNi
The active site density of alloy can more promote crystal fast nucleation, reduce energy consumption and have a good application prospect.
Fuel cell is considered as the important power device of traditional internal combustion engine alternative in the near future.Proton exchange
Another important feature of membrane cell is that it both can be using clean energy resource such as hydrogen etc. as fuel, also can be with reproducible small
Molecular organic such as formic acid, ethyl alcohol, methanol etc. is fuel.According to before studies have shown that Pt catalyst is proton exchange membrane combustion
Expect the best catalyst of catalytic performance in battery, but the high cost and utilization rate of Pt catalyst limits to a certain extent
The application prospect of fuel cell, therefore prepare and have become current compel for improving raising electrocatalysis characteristic and stability catalyst
Cut urgent problem.
Summary of the invention
In view of the above technical problems, the present invention solve current Pt nano-structured calalyst there are the service life it is short it is at high price with
And the technical problems such as preparation cost height, a kind of recessed shape of octahedron PtCuNi alloy nano particle of high density active position is prepared,
Improve the performance of Pt nano-structured calalyst.
To achieve the above object, the present invention is achieved by the following technical solutions:
A kind of experimental procedure of recessed octahedron PtCuNi alloy nano particle preparation method is as follows:
(1) 303.4mg glycine is successively weighed, 200mg PVP and 300mg NaI are added in the beaker of 50mL；
(2) 2mL 19.3mM H successively then is pipetted with liquid-transfering gun again2PtCl6Aqueous solution, 1mL 20mM CuCl2It is water-soluble
Liquid, 1mL 20mM NiCl2Aqueous solution and 0.7mL ethanol amine are added in above-mentioned beaker, are stirred by ultrasonic 30 minutes or so, until
Solution becomes clear；
(3) secondly solution is transferred in micro-wave digestion kettle, maintains after forty minutes, to keep it naturally cold for 200 DEG C in microwave
But room temperature is arrived；
(4) finally the solution for being cooled to room temperature is centrifuged, 10000r/min, 15 minutes, then with ethyl alcohol: water=1:1
Mixed liquor washs three times, is then freeze-dried.
It should be noted that different with traditional heating mode, microwave heating is very rapid, as long as usually there is microwave spoke
It penetrates, substance just can be heated rapidly.Due to the preheating of traditional heating needs and there are high-temperature medium heat loss, radiation heat loss
Etc. a series of energy losses, inevitable energy dissipation and inefficiency are caused；The sample that traditional hydrothermal synthesis generates is brilliant
Body nucleation is mostly first formed along chamber wall, is further grown；The mechanism of action of the two is different, thus the effect to crystal growth
It is usually the lesser spherical morphology of size that mechanism difference, which causes the nanocrystalline of microwave irradiation synthesis, and the active sites of surface catalyst are close
Spend low, and I-Additional amount it is embodied in nucleating process to the control of pattern there is stronger suction to { 100 } crystal face
Attached selectivity, to make to grow crystal towards the crystal face of { 111 } and tend to form octahedron
Pattern it is nanocrystalline, and the controllable formation concave structure of addition of glycine has had been reported that in the article delivered before, and
Ethanol amine then facilitate under the conditions of microwave radiation by metal precursor chelating achieve the purpose that simultaneously restore three kinds of metals thus
Ternary alloy three-partalloy is formed, the molar percent ratio by the ICP-OES Pt/Cu/Ni measured is 26.2/72.5/1.3.
Beneficial effects of the present invention: for the present invention with chloroplatinic acid, copper chloride and nickel chloride are raw material, using PVP as reducing agent, sweet
Propylhomoserin and NaI are Morphological control agent, and the ethanol amine that certain content is added can be prepared under microwave heating condition in the short time
The higher concave surface shape of octahedron PtCuNi alloy nano particle of selectivity is obtained, energy consumption is reduced and preparation method green cleans.
The PtCuNi alloy nano particle of the concave surface shape of octahedron of acquisition not only shows good chemical property and good
Activity stability more has wide practical use.
Detailed description of the invention
Fig. 1 is the TEM map for the PtCuNi alloy nano particle that embodiment 1 is prepared；
Fig. 2 is the TEM amplification map for the PtCuNi alloy nano particle that embodiment 1 is prepared；
Fig. 3 is TEM enlarged drawing of the PtCuNi alloy nano particle that is prepared of embodiment 1 under different transmission angles
Spectrum；
Fig. 4 is that the cyclic voltammetric for the PtCuNi alloy nano particle methanol electro-oxidizing-catalyzing agent that embodiment 1 is prepared is bent
Line chart；
Fig. 5 is the PtCuNi alloy nano particle that is prepared of embodiment 1 methanol fuel electricity when constant potential is 0.4V
The chronoa mperometric plot figure in pond.
Specific embodiment
Below by way of the implementation and possessed beneficial effect of specific embodiment the present invention will be described in detail technical solution, but not
It can regard as any restriction to enforceable range of the invention.
Embodiment 1
A kind of experimental procedure of recessed octahedron PtCuNi alloy nano particle preparation method is as follows:
(1) 303.4mg glycine is successively weighed, 200mg PVP and 300mg NaI are added in the beaker of 50mL；
(2) 2mL 19.3mM H successively then is pipetted with liquid-transfering gun again2PtCl6Aqueous solution, 1mL 20mM CuCl2It is water-soluble
Liquid, 1mL 20mM NiCl2Aqueous solution and 0.7mL ethanol amine are added in above-mentioned beaker, are stirred by ultrasonic 30 minutes or so, until
Solution becomes clear；
(3) secondly solution is transferred in micro-wave digestion kettle, maintains after forty minutes, to keep it naturally cold for 200 DEG C in microwave
But room temperature is arrived；
(4) finally the solution for being cooled to room temperature is centrifuged, 10000r/min, 15 minutes.Ethyl alcohol: water=1:1 is used again
Mixed liquor washs three times, is then freeze-dried.
We carry out electrochemical catalysis test using three-electrode system on CHI760e type electrochemical workstation.With saturation
Calomel electrode (SCE, in saturation KCl solution) is reference electrode；Pt electrodes are to electrode, and glass-carbon electrode (GC) is used as work
Electrode.
The application method of GC electrode: the Al2O3 powder for being respectively before every use 1 μm, 0.3 μm and 0.05 μm with diameter
It is polished to mirror surface, then washs two to three times with EtOH Sonicate, is dried with infrared drying oven.
GC electrode is added dropwise: pipetting the catalyst suspension of 6 μ L under being dried under infrared lamp, drips to the surface of GC electrode
On, the 0.5wt%Nafion solution of upper 2 μ L is dripped then at the surface of working electrode, makes GC electrode surface dry under infra-red drying.
Electrochemical activation area test: with 0.5M H2SO4Solution does electrolyte solution, leads to high-purity N 2 to electrolyte except dissolution
Oxygen, then carries out cyclic voltammetric (CV) scanning, sweep speed 50mV/s, and scanning range is -0.24~1.0V.In experimentation
Holding superjacent is inert gas.Until to the last a circle is overlapped with circle second from the bottom.
Methanol electro-oxidizing test: being 2M CH in concentration3OH+0.5M H2SO4It is carried out under electrolyte, logical high-purity N 2 removes electricity
Xie Zhizhong dissolved oxygen, then does CV scanning, sweep speed 50mV/s, and scanning range is -0.24~1.0V.It keeps in the process molten
It is inert gas above liquid, to the last two circles are overlapped and terminate, and the methanol electro catalytic activity for measuring the catalyst is up to 5.06mA
cm-2, much higher than commercial platinum catalyst.
Chronoa mperometric plot: in 2M CH3OH+0.5M H2SO4Voltage is respectively 0.4V when sweeping chronoa mperometric plot, test
Time is 1000s, and the stability of the catalyst is better than commercial platinum series catalyst as shown in Figure 5.
Comparative example 1
On the basis of embodiment 1, NaI is not added, obtained nanotopography is general category spherical polyhedron, and electro-catalysis
Methanol activity is 2.15mA cm-2。
Comparative example 2
On the basis of documents 1, ethanol amine is not added, then what is obtained is nanocrystalline for PtCu bianry alloy, passes through
The molar percent ratio for the Pt/Cu that ICP-OES is measured is 32.6/67.4.And electro-catalysis methanol activity is 1.79mA cm-2。
Comparative example 3
On the basis of documents 1, conventional hydrothermal synthesis is carried out at 200 DEG C, then what is obtained is nanocrystalline for PtCu bis-
First alloy and part be concave surface cube pattern, be partially irregular pattern.
Moreover, it relates to arrive multiple groups comparative example, it will not enumerate in view of length, be respectively relative to embodiment 1
Change one or more parametric variables, cannot get this hair in the case where changing one or more variable as the result is shown
Bright recessed shape of octahedron PtCuNi alloy nano particle, showing between each technical characteristic of the technical solution of the application has
Synergistic effect, shows no matter the technical solution of the application for alloy pattern or catalytic activity has reached unexpected
Technical effect.
Claims (1)
1. a kind of recessed shape of octahedron PtCuNi alloy nanoparticle and preparation method thereof, specific steps are as follows:
(1) 303.4mg glycine is successively weighed, 200mg PVP and 300mg NaI are added in the beaker of 50mL；
(2) 2mL 19.3mM H successively then is pipetted with liquid-transfering gun again2PtCl6Aqueous solution, 1mL 20mM CuCl2Aqueous solution, 1mL
20mM NiCl2Aqueous solution and 0.7mL ethanol amine are added in above-mentioned beaker, are stirred by ultrasonic 30 minutes or so, until solution becomes clear
It is clear bright；
(3) secondly solution is transferred in micro-wave digestion kettle, maintains after forty minutes, to naturally cool to it for 200 DEG C in microwave
Room temperature；
(4) finally the solution for being cooled to room temperature is centrifuged, 10000r/min, 15 minutes.Ethyl alcohol: water=1:1 mixing is used again
Liquid washs three times, is then freeze-dried.
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Cited By (6)
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| CN111063899A (en) * | 2020-01-08 | 2020-04-24 | 济南大学 | Method for improving CO resistance of formic acid fuel cell electrooxidation |
| CN111230141A (en) * | 2020-03-04 | 2020-06-05 | 王冲 | Preparation method of PtRuCoS alloy nanocrystalline with floccule morphology |
| CN112974832A (en) * | 2021-04-07 | 2021-06-18 | 南京师范大学 | Preparation method of Pt concave cubic nanocrystal, and nanocrystal and application thereof |
| CN113488670A (en) * | 2021-07-07 | 2021-10-08 | 内蒙古科技大学 | Pt-Ni alloy and preparation method and application thereof |
| CN113603603A (en) * | 2021-08-05 | 2021-11-05 | 西北大学 | Method for preparing beta-glycine by solution freezing and anti-solvent washing |
| CN114182290A (en) * | 2021-12-22 | 2022-03-15 | 北京科技大学 | Noble metal-two-dimensional transition metal chalcogenide heterostructure, preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111063899A (en) * | 2020-01-08 | 2020-04-24 | 济南大学 | Method for improving CO resistance of formic acid fuel cell electrooxidation |
| CN111230141A (en) * | 2020-03-04 | 2020-06-05 | 王冲 | Preparation method of PtRuCoS alloy nanocrystalline with floccule morphology |
| CN111230141B (en) * | 2020-03-04 | 2022-10-25 | 王冲 | Preparation method of PtRuCoS alloy nanocrystalline with floccule morphology |
| CN112974832A (en) * | 2021-04-07 | 2021-06-18 | 南京师范大学 | Preparation method of Pt concave cubic nanocrystal, and nanocrystal and application thereof |
| CN113488670A (en) * | 2021-07-07 | 2021-10-08 | 内蒙古科技大学 | Pt-Ni alloy and preparation method and application thereof |
| CN113603603A (en) * | 2021-08-05 | 2021-11-05 | 西北大学 | Method for preparing beta-glycine by solution freezing and anti-solvent washing |
| CN113603603B (en) * | 2021-08-05 | 2023-09-15 | 西北大学 | Method for preparing beta glycine by solution freezing and antisolvent washing |
| CN114182290A (en) * | 2021-12-22 | 2022-03-15 | 北京科技大学 | Noble metal-two-dimensional transition metal chalcogenide heterostructure, preparation method and application thereof |
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