Preparation method of size controllable rhotanium nano particles

A nanoparticle, gold-palladium alloy technology, applied in nanotechnology, metal processing equipment, transportation and packaging, etc., to achieve the effect of simple operation, uniform dispersion and easy control

Inactive Publication Date: 2017-06-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But how to control small-sized

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  • Preparation method of size controllable rhotanium nano particles
  • Preparation method of size controllable rhotanium nano particles
  • Preparation method of size controllable rhotanium nano particles

Examples

Experimental program
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Embodiment 1

[0024] Synthesis of about 3nm gold-palladium alloy of embodiment 1

[0025] Dissolve the gold organic complex and palladium chloride in tetrahydrofuran, methanol or ethanol solvent, the molar ratio of the gold organic complex to palladium chloride is 1:1, the molar concentration of the gold organic complex in the organic solvent is 3mg / ml, stirred at room temperature for 30 minutes, then added phenethanethiol ligand and stirred for one hour until a large amount of orange precipitate was formed, the molar ratio of the sum of thiol ligand to gold organic complex and palladium chloride is 0.25:1. Finally, an aqueous sodium borohydride solution with a molar ratio of 15:1 to the sum of the gold organic complex and palladium chloride was added to the above reaction, and a black precipitate was formed immediately. After the reaction was carried out for 20 hours, the thiol ligand was washed 4 times with a large amount of methanol, the product was extracted 2 times with dichlorometha...

Embodiment 2

[0027] The synthesis of embodiment 2 2-2.5nm gold-palladium alloy

[0028] Dissolve the gold organic complex and palladium chloride in tetrahydrofuran, methanol or ethanol solvent, the molar ratio of the organic gold source to palladium chloride is 1:1, the molar concentration of the gold organic complex in the organic solvent is 3mg / ml , stirred at room temperature for 30 minutes, then added phenylethyl thiol ligand and stirred for one hour until a large amount of orange precipitate was formed, wherein the molar ratio of thiol ligand to metal source was 0.5:1. Finally, an aqueous sodium borohydride solution with a molar ratio of 15:1 to the sum of the gold organic complex and palladium chloride was added to the above reaction, and a black precipitate was formed immediately. After the reaction was carried out for 20 hours, the thiol ligand was washed 4 times with a large amount of methanol, the product was extracted 2 times with dichloromethane, and the product dissolved in di...

Embodiment 31

[0030] The synthesis of embodiment 3 1.7-2nm gold-palladium alloy

[0031] Dissolve the gold organic complex and palladium chloride in tetrahydrofuran, methanol or ethanol solvent, the molar ratio of the organic gold source to palladium chloride is 1:1, the molar concentration of the gold organic complex in the organic solvent is 3mg / ml , stirred at room temperature for 30 minutes, then added phenylethyl thiol ligand and stirred for one hour until a large amount of orange precipitate was formed, wherein the molar ratio of thiol ligand to metal source was 1:1. Finally, an aqueous sodium borohydride solution with a molar ratio of 15:1 to the sum of the gold organic complex and palladium chloride was added to the above reaction to immediately generate a black precipitate. After the reaction was carried out for 20 hours, the thiol ligand was washed 4 times with a large amount of methanol, the product was extracted 2 times with dichloromethane, and the product dissolved in dichloro...

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Abstract

The invention discloses a preparation method of size controllable rhotanium nano particles. The method can adjust and control the size of the nano particles through changing proportion of a ligand and comprises the following steps in specific: dissolving gold organic complex and palladium salt in an organic solvent, stirring, adding certain proportion of mercaptan ligand, stirring for a while until a large amount of saffron yellow sediment in the solvent, and adding sodium borohydride for reduction to generate black substance immediately; washing the black substance with a large amount of methyl alcohol, and removing mercaptan not reacting; and finally, extracting the nano particles with dichloromethane, and drying the nano particles in a vacuum drying box. Through adjusting the proportion of the mercaptan ligand, nano particles of different sizes are obtained, and the size distribution range comprises 1-1.5 nm, 1.7-2 nm, 2-2.5 nm and 3 nm. The preparation method, disclosed by the invention, is feasible and simple to operate; and nano particles of different sizes can be obtained through adjusting and controlling the proportion of the ligand.

Description

[0001] Technical field: [0002] The invention belongs to the preparation of metal alloy nanoparticles, and the invention describes a simple method for preparing size-controllable alloy nanoparticles. [0003] Background technique: [0004] Gold nanoparticles have good catalytic effect and are mainly used in hydrogenation reaction, oxidation reaction and electrochemical catalytic reaction. However, for some catalytic reactions, the catalytic activity and selectivity of gold nanoparticles are very low. Therefore, gold-based alloys have been extensively studied, for example, Au-Pd alloys, Au-Pt alloys, Au-Fe alloys and so on. Its main applications are in catalysis, magnetism, medicine and so on. [0005] The preparation of alloy nanoparticles is mainly divided into physical and chemical methods, among which chemical methods include chemical reduction method, co-precipitation method, ion substitution method, ultrasonic method and so on. The size distribution of alloy nanopartic...

Claims

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Application Information

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IPC IPC(8): B22F9/24B82Y40/00
CPCB82Y40/00B22F9/24B22F1/054
Inventor 李杲刘超林计志
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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