Preparation method of palladium nano-clusters with sizes controllable

A palladium nano-size technology, applied in the field of preparation of palladium metal nano-clusters, can solve the problems of preparation of different sizes, complex operation, cumbersome steps, etc., and achieve the effect of easy control and simple operation

Inactive Publication Date: 2018-06-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the synthesis process, it is found that each nanocluster is carried out under different reaction conditions, and it is difficult to prepare nanoclusters of different sizes in the same system; for some nanocluster synthesis methods, the steps are cumbersome and the operation is complicated

Method used

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  • Preparation method of palladium nano-clusters with sizes controllable
  • Preparation method of palladium nano-clusters with sizes controllable
  • Preparation method of palladium nano-clusters with sizes controllable

Examples

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Effect test

example 1

[0017] Example 1: Synthesis of 0.6-0.9nm Palladium Nanoparticles

[0018] First dissolve 20mg of palladium chloride in 0.5mL of concentrated hydrochloric acid, then add 20mL of methanol solvent and stir for 40 minutes, then add a thiol ligand with a molar ratio of 3:1 for reaction, wait for one hour to react, and add a molar ratio of 5:1 Sodium borohydride reduction yields zero-valent palladium nanoparticles. The obtained palladium nanocluster solution was spin-dried, and then washed 3 times with a large amount of methanol. Finally, the palladium nanoparticles were dissolved in dichloromethane, centrifuged at 9000 r / min, and spin-dried.

[0019] Such as figure 1 , Embodiment 1 prepares the transmission electron micrograph of palladium nanoparticle, and the size of its palladium atom is 0.6-0.9nm.

example 2

[0020] Example 2: Synthesis of 1.0-1.3nm palladium nanoclusters

[0021] First dissolve 20mg of palladium chloride in 0.5mL of concentrated hydrochloric acid, then add 20mL of methanol solvent and stir for 40 minutes, then add a thiol ligand with a molar ratio of 2:1 for reaction, wait for one hour to react, and add a molar ratio of 5:1 Sodium borohydride reduction yields zero-valent palladium nanoparticles. The obtained palladium nanocluster solution was spin-dried, and then washed 3 times with a large amount of methanol. Finally, the palladium nanoparticles were dissolved in dichloromethane, centrifuged at 9000 r / min, and spin-dried.

[0022] Such as figure 2 , Embodiment 2 prepares the transmission electron micrograph of palladium nanoparticle, and the size of its palladium atom is 1.0-1.3nm.

example 3

[0023] Example 3: Synthesis of 1.4-1.7nm Palladium Nanoparticles

[0024] First dissolve 20mg of palladium chloride in 0.5mL of concentrated hydrochloric acid, then add 20mL of methanol solvent and stir for 40 minutes, then add a thiol ligand with a molar ratio of 1:1 for reaction, wait for one hour to react, and add a molar ratio of 5:1 Sodium borohydride reduction yields zero-valent palladium nanoparticles. The obtained palladium nanocluster solution was spin-dried, and then washed 3 times with a large amount of methanol. Finally, the palladium nanoparticles were dissolved in dichloromethane, centrifuged at 9000 r / min, and spin-dried.

[0025] Such as image 3 , Embodiment 3 prepares the transmission electron micrograph of palladium nanoparticle, and the size of its palladium atom is 1.4-1.7nm.

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Abstract

The invention discloses a preparation method of palladium nano-clusters with the sizes being controllable. The method can be used for preparing the palladium nano-clusters of different sizes on a large scale. The method specifically comprises the steps that firstly, palladium chloride is dissolved into a trace amount of concentrated hydrochloric acid; secondly, an obtained mixture is added into anorganic solvent and stirred for a period of time; and thirdly, mercaptan ligands with different mole ratios are added for reaction, after one hour of reaction, sodium borohydride is added for reduction, and non-valent palladium nano particles are obtained. The sizes of the nano-clusters are controlled by changing the ratios of the ligands. The preparation method related by the invention is feasible and easy to operate, and the palladium nano particles of different sizes can be obtained by adjusting and controlling the ligands with the different mole ratios.

Description

Technical field: [0001] The invention belongs to the preparation of palladium metal nanoclusters, and the invention illustrates the simple preparation of palladium nanoclusters with different sizes and controllable sizes. Background technique: [0002] Transition metal thiolates play an important role in biological reactions and coordination chemistry, and thiolate ligands can bond to metal atoms in different coordination ways. Various thiolated transition metal clusters have been synthesized and characterized, such as iron, cobalt, nickel, copper, zinc, palladium, silver, platinum, and gold. Due to the high specific surface area and special surface properties of nano-metal-thiolate clusters, metal nano-clusters have broad application prospects in the fields of new energy, optoelectronic information storage, and biomedicine. As an important member of the family of catalytic materials, Pd nanomaterials have many characteristics that make them irreplaceable advantages and pot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00B22F9/24B22F1/054
Inventor 黄家辉刘超任秀清
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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