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Preparation method of metal and alloy nanocrystalline

An alloy nanocrystal and metal technology, applied in the field of metal and alloy nanocrystal preparation, can solve problems such as restricting the large-scale production and practical application of nano-alloys, difficulty in separation and purification of nanomaterials, poor homogeneity in the same batch, etc. In industrial production, good catalytic performance and stability, high production efficiency

Active Publication Date: 2019-12-17
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the controllable preparation of nano-alloys, especially the regulation of size and composition, still faces great challenges.
First of all, in the synthesis method, it is usually necessary to add surfactants or polymers to inhibit the growth and agglomeration of nanocrystals to achieve the purpose of regulating the size of nanocrystals. However, these viscous substances are very easy to adsorb on the surface of alloy nanocrystals, giving nanomaterials In addition, the synthesis process usually faces problems such as high temperature or hydrothermal / solvothermal process, long synthesis cycle, complicated control conditions, and poor uniformity in the same batch.
These have restricted the large-scale production and practical application of nano-alloys.
Secondly, the nucleation-growth of alloy nanocrystals is different from the synthesis of single metal nanocrystals, because different metal elements have different electrochemical reduction potentials, which will cause differences in the precipitation time of different metal atoms in nanoalloys. Therefore, Alloy nanoparticles are more difficult to synthesize than single metal nanoparticles

Method used

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  • Preparation method of metal and alloy nanocrystalline
  • Preparation method of metal and alloy nanocrystalline
  • Preparation method of metal and alloy nanocrystalline

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Preparation steps of Pt-Cu-vxc72:

[0030] (1) Take 13 mg of copper acetylacetonate powder and 20 mg of chloroplatinic acid as raw materials, and 51.6 mg of conductive carbon black of the model vxc72 as a carrier, add it to 80 ml of ethylene glycol dimethyl ether, stir well and ultrasonically for 5 minutes obtain its dispersion;

[0031] (2) 0.1 gram of metal sodium and 0.3 gram of metal potassium are cut into small pieces and added into ethylene glycol dimethyl ether and pressed into potassium-sodium alloy droplets respectively, and 160 microliters of potassium-sodium alloy droplets are added to the step ( 1) In the obtained dispersion liquid, the dispersion liquid is then subjected to high-speed shearing with a high-speed shear emulsifier at 25° C. and under the protection of argon, with a shear rate of 10,000 rpm and a shear time of 1 minute;

[0032] (3) The crude product of step (2) was washed 3 times with absolute ethanol, and then the washed product was washed 5...

Embodiment 2

[0040] Preparation steps of Pt-Cu-Fe-vxc72:

[0041] (1) With 35.4 milligrams of iron acetylacetonate powder, 26 milligrams of copper acetylacetonate and 40 milligrams of chloroplatinic acid as raw materials, with 125.6 milligrams of models as the conductive carbon black of vxc72 as a carrier, join in 80 milliliters of ethylene glycol dimethyl ether, Stir evenly and ultrasonically for 5 minutes to obtain its dispersion;

[0042] (2) Cut 0.1 gram of metal sodium and 0.3 gram of metal potassium into small pieces and add them to ethylene glycol dimethyl ether and press them into droplets. Take 160 microliters of alloy droplets and add them to the dispersed mixture obtained in step (1). liquid, and then carry out high-speed shearing on the dispersion liquid with a high-speed shear emulsifier at 25°C and under the protection of argon, the shear rate is 10000rpm, and the shear time is 1 minute;

[0043] (3) Wash the crude product of step (2) 3 times with absolute ethanol, then wash...

Embodiment 3

[0045] Preparation steps of Pt-Fe-vxc72:

[0046] (1) With 17.7 mg of iron acetylacetonate powder and 20 mg of chloroplatinic acid as raw materials, 51.2 mg of conductive carbon black with a type of vxc72 as a carrier, added to 80 ml of ethylene glycol dimethyl ether, stirred evenly and ultrasonicated for 5 minutes obtain its dispersion;

[0047] (2) Cut 0.1 gram of metal sodium and 0.1 gram of metal potassium into small pieces and add them to ethylene glycol dimethyl ether and press them into droplets. Take 160 microliters of alloy droplets and add them to the dispersed mixture obtained in step (1). liquid, and then carry out high-speed shearing on the dispersion liquid with a high-speed shear emulsifier at 25°C and under the protection of argon, the shear rate is 10000rpm, and the shear time is 1 minute;

[0048] (3) The crude product of step (2) was washed 3 times with absolute ethanol, and then the washed product was washed 5 times with deionized water, and the obtained p...

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Abstract

The invention relates to a preparation method of metal and alloy nanocrystalline, and belongs to the field of inorganic nano materials. A metal precursor is taken as a raw material, and under the condition that no surfactant is added, alloy nanocrystalline with ultra-small (less than 3 nm) and uniform size is rapidly (less than 2 min) prepared at room temperature by means of shearing assistance, the metal and alloy nanocrystalline with different compositions and a controllable size can be obtained by controlling the volume of a reducing agent, a reactant molar ratio, a concentration, reactiontime and other parameters, and the prepared carbon-supported nanocrystalline is used as a hydrogen evolution electrocatalyst and has excellent performance. The method has the characteristics of high reaction speed, simple operation, recyclable solvent, low cost, easy industrial amplification production and the like.

Description

technical field [0001] The invention relates to a method for preparing metal and alloy nanocrystals, belonging to the technical field of nanomaterial preparation. Background technique [0002] In recent years, the synthesis of metal and alloy nanocrystals has been a hot spot in nanomaterials research. This is because nanoalloys have tunable size, surface structure and composition, and the resulting synergistic effects, which make them have broad application prospects in catalysis, electronics, and biomedicine. However, the controllable preparation of nanoalloys, especially the regulation of size and composition, still faces great challenges. First of all, in the synthesis method, it is usually necessary to add surfactants or polymers to inhibit the growth and agglomeration of nanocrystals to achieve the purpose of regulating the size of nanocrystals. However, these viscous substances are very easy to adsorb on the surface of alloy nanocrystals, giving nanomaterials In addi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C5/04B22F9/24B22F1/00C25B11/08C25B1/04B82Y30/00B82Y40/00
CPCC22C5/04B22F9/24C25B1/04B82Y30/00B82Y40/00C22C2200/04C25B11/091B22F1/07B22F1/054Y02E60/36
Inventor 冯红彬
Owner QINGDAO UNIV
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