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Preparation method for controllable duplex metal alloy nano particle

A technology of alloy nanoparticles and bimetal, which is applied in the field of preparation of Pt/Pd-M bimetal alloy nanoparticles, can solve problems such as difficulty in obtaining alloy nanoparticles, and achieve uniform and controllable size and simple and controllable preparation process

Active Publication Date: 2013-07-10
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a method for preparing controllable bimetallic alloy nanoparticles, using n-butyl as a strong reducing agent, which solves the problem that when the reduction potential of two metal precursors is too different, one metal is Preferential reduction, it is difficult to obtain alloy nanoparticles. The prepared bimetallic alloy nanoparticles are uniform and have no concentration gradient, uniform and controllable size, and have a face-centered cubic structure.

Method used

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  • Preparation method for controllable duplex metal alloy nano particle
  • Preparation method for controllable duplex metal alloy nano particle
  • Preparation method for controllable duplex metal alloy nano particle

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Put 20ml of octadecene in a 50ml three-necked flask, fill it with nitrogen, heat the above solvent to 75°C under magnetic stirring and nitrogen protection, and inject 2ml of n-butyllithium n-hexane with a concentration of 2.2mol / L into the above solvent Solution, after about two minutes, 0.065mmolH dissolved in protective agent A (4ml oleylamine) 2 PtCl 6 ·6H 2 O(chloroplatinic acid hexahydrate) and 0.065mmolCo(CH 3 COO) 2 (Cobalt acetate) solution is injected into the above-mentioned solvent, and the solution in the three-necked flask turns brown-black instantly, and is kept at this temperature for 30 minutes, then heated up to 260°C and kept for 2 hours, and then begins to cool down, and when it drops to about 120°C, Inject 1.5ml of protective agent B (tri-n-octylphosphine) into the reaction product and wait for it to cool down to room temperature. Move the reaction product into a 50ml centrifuge tube, take 5ml and put it into another centrifuge tube, add about 40...

Embodiment 2

[0032] Put 20ml of octadecene in a 50ml three-necked flask, fill it with nitrogen, heat the above solvent to 75°C under magnetic stirring and nitrogen protection, and inject 2ml of n-butyllithium n-hexane with a concentration of 2.2mol / L into the above solvent Solution, after about two minutes, 0.065mmolH dissolved in protective agent A (4ml oleylamine) 2 PtCl 6 6H2O (chloroplatinic acid hexahydrate) and 0.065mmol Fe(acac) 3 The (iron acetylacetonate) solution is injected into the above solvent, and the solution in the three-necked flask instantly turns brown-black, and is kept at this temperature for 30 minutes. Inject 1.5ml of protective agent B (tri-n-octylphosphine) into the reaction product and wait for it to cool down to room temperature. Move the reaction product into a 50ml centrifuge tube, take 5ml and put it into another centrifuge tube, add about 40ml of ethanol and centrifuge at 8000 rpm, disperse the centrifuged precipitate with 2ml of toluene each time, and the...

Embodiment 3

[0036] Put 20ml of octadecene in a 50ml three-necked flask, fill it with nitrogen, heat the above solvent to 75°C under magnetic stirring and nitrogen protection, and inject 1ml of n-butyllithium n-hexane with a concentration of 2.2mol / L into the above solvent Solution, after about two minutes, 0.13mmolH dissolved in protective agent A (2ml oleylamine) 2 PtCl 6 ·6H 2 O(chloroplatinic acid hexahydrate) and 0.13mmol Ni(acac) 2 (Nickel acetylacetonate) solution is injected into the above solvent, and the solution in the three-necked flask turns brown-black instantly, and is kept at this temperature for 30 minutes, then heated up to 260°C and kept for 2 hours, and then begins to cool down, and when it drops to about 120°C Inject 1.5ml of protective agent B (tri-n-octylphosphine) into the reaction product and wait for it to cool down to room temperature. Move the reaction product into a 50ml centrifuge tube, take 5ml and put it into another centrifuge tube, add about 40ml of eth...

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Abstract

The invention relates to a preparation method for a controllable duplex metal alloy nano particle. The metal alloy nano particles is a Pt / Pd-M alloy nano particle, wherein the M is selected from Ni, Fe, Co, Mn, Pd, Zn, Cu and Mo; during preparation, n-butyllithium is used as a strong reducing agent and oleylamine and tri-n-octylphosphine are used as protective agents to reduce acetylacetone, chlorate or acetate of the Pt / Pd-M (M= Ni, Fe, Co, Mn, Pd, Zn, Cu,Mo) at the same time so as to form the uniform and size-controllable Pt / Pd-M alloy nano particle without a concentration gradient. The preparation method is simple and controllable in preparation technology, and can solve the problem that when precursor reduction potentials of two metals are greatly different, one metal can be reduced in prior, so that the alloy nano particle can not be obtained easily, provides a better and universal synthetic method for the preparation of the duplex metal alloy nano particle, and provides a key precursor for the preparation of a new generation of metal-oxide nano hybridization body catalyst used for selective hydrogenation reaction.

Description

technical field [0001] The invention relates to a method for preparing controllable bimetallic alloy nanoparticles, specifically a Pt / Pd-M (M=Ni, Fe, Co, Mn, Pd, Zn, Cu, Mo) bimetallic alloy nanoparticles method of preparation. Background technique [0002] It is well known that in many cases the properties of alloying are enhanced under synergistic effects. Metal alloys are widely used in electronics, engineering and catalysis due to their diversity in composition, structure and properties. [0003] The mechanism of the reduction of metal precursors to form bimetallic alloy nanoparticles by liquid phase reduction is very complicated. The matching of metal precursors plays a key role in simultaneous rapid reduction, and metal precursors with large reduction potentials will cause differences in the reduction rates of the two metal precursors, making it difficult to obtain alloy nanoparticles. The synthesis of bimetallic alloy nanoparticles is not a simple technique, requir...

Claims

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Application Information

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IPC IPC(8): B22F9/24B82Y40/00
Inventor 周生虎王向东
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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