Method for treating organic ligands on surfaces of gold clusters

A technology of organic ligands and atomic clusters, applied in the field of nanomaterials, can solve the problems of inapplicable excision, etc., and achieve the effect of improving catalytic activity, improving catalytic activity, and simple operation steps

Active Publication Date: 2019-08-13
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

However, this method is not suitable for removing strong covalent bonds like Au-S

Method used

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  • Method for treating organic ligands on surfaces of gold clusters
  • Method for treating organic ligands on surfaces of gold clusters
  • Method for treating organic ligands on surfaces of gold clusters

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Au 25 (SR) 18 Synthesis

[0029] Weigh 60 mg of HAuCl 4 4H 2 O was added to a 50mL three-necked flask, and 15mL THF was added, and the solution was golden yellow. Add TOAB 92 mg (TOAB: Au = 1.16 mol: 1 mol), and the solution gradually turns from golden yellow to orange red. After stirring for 30 min, add C 12 h 25 SH 177μL (C 12 h 25 SH: Au=5mol:1mol), when the color of the solution gradually becomes lighter to colorless, add NaBH 4 (4mL ice water) 55mg (NaBH 4 : Au=10mol:1mol). Stir overnight to stop the reaction. Wash the product with n-hexane and methanol, dissolve the precipitate with acetone, remove the insoluble matter, and obtain Au after drying 25 (SR) 18 .

[0030] Such as figure 1 The scanning transmission electron microscope image of the gold cluster prepared in Example 1, the size is about 1.5nm.

[0031] Such as figure 2 The ultraviolet-visible spectrum of the gold cluster prepared in Example 1 has a relatively strong absorption ...

Embodiment 2

[0033] Example 2 Au 25 (SR) 18 / CeO 2 Catalyst Synthesis

[0034] Dissolve 10 mg of Au in 10 mL of dichloromethane at room temperature 25 (C 12 h 25 S) 18 , added to CeO dispersed in 40 and mL dichloromethane 2 (2 g), stirred overnight and dried by centrifugation to obtain an untreated sample.

[0035] Such as Figure 4 , 5 , 6 are the Fourier transform infrared spectrum, X-ray photoelectron energy spectrum and Raman spectrum of the untreated sample respectively

Embodiment 3

[0036] Embodiment 3 sample heat treatment in reaction gas

[0037] 50mg Au 25 (SR) 18 / CeO 2 The catalyst is placed in a fixed bed reaction tube, and a gas mixture of 1.67CO / 3.33O is introduced 2 / He 12.5mL. Raise the temperature to 100°C, 120°C, 140°C, and 200°C for 1 hour respectively.

[0038] Such as Figure 4 The FTIR spectra of the samples treated at different temperatures are shown in the middle.

[0039] Such as Figure 7 The middle is the catalytic performance of CO oxidation of samples with different treatment temperatures.

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Abstract

The invention relates to a method for treating organic ligands on the surfaces of gold clusters. According to the method, the surface stabilizer ligands of gold nanoparticles can be simply and efficiently treated in an environment-friendly manner, so that unsaturated coordination atoms on the surface stabilizer ligands of the gold nanoparticles are exposed, and the catalytic activity is greatly improved. The method mainly comprises the following steps of introducing water into a reactive atmosphere to activate Au-S bonds, and removing the organic ligands under a mild condition. The changes ofvibration peaks and absorption peaks before and after water treatment can be observed visibly in a Fourier infrared spectrum and an X-ray photoelectron spectrum, and these changes are matched with a result of DFT calculation.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, in particular to a new method for removing organic ligands on the surface of gold atom clusters. Background technique [0002] In recent years, the unique optical, electrical, and catalytic properties of noble metal nanomaterials and their applications in new energy research, photoelectric information storage, and biomedicine have attracted extensive attention in related research fields. Noble metal clusters exhibit unique properties in catalysis due to their precise atomic composition and energy quantization. However, the synthesis of noble metal clusters often requires certain organic ligands for protection. These stabilizer ligands play an important role in preventing the irreversible aggregation of interactions between noble metal atoms. However, once the noble metal nanoparticles are deposited on the substrate, these coordination-saturated metal particles seriously reduce their...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/66B01J37/10
CPCB01J23/66B01J35/0046B01J35/006B01J37/0018
Inventor 李杲李志敏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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