Preparation method of carbon-coated transition metal nano hollow particle

A transition metal, carbon coating technology, applied in structural parts, electrical components, battery electrodes, etc., can solve the problems of being easily oxidized and not stable, and achieve good commercial application prospects, rich raw material sources, and mild reaction conditions. Effect

Inactive Publication Date: 2011-10-05
BEIJING UNIV OF CHEM TECH
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  • Abstract
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  • Application Information

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Problems solved by technology

Nam et al. through face-centered cubic cobalt oxide (CoO) in oleamide (C 18 h 35 NH 2 ) in pyrolysis synthesized face-centered cubic cobalt single substance hollow nanoparticles [Nam.K.M et al, Single-crystalline hollowface-centered-cubic cobalt nanoparticles from solid face-centered-cubic cobalt oxidenanoparticles, Angew.Chem.Int. Ed.2008: 47: 9504], since the hollow nano-cobalt particles prepared by this method are not coated with carbon shells, they are easily oxidized and cannot exist stably in the air
At present, there is no report on the preparation of carbon-coated transition metal nano-hollow structure composites

Method used

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  • Preparation method of carbon-coated transition metal nano hollow particle
  • Preparation method of carbon-coated transition metal nano hollow particle
  • Preparation method of carbon-coated transition metal nano hollow particle

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh 10g of resorcinol and 20g of ferrocene in a weight ratio of 1:2 and dissolve them in acetone, mechanically stir until the acetone is completely volatilized, then place the resulting solid in a high-pressure reactor, and add 60ml of high-temperature silicone oil as a reaction medium , under continuous uniform mechanical stirring and nitrogen protection, the temperature was gradually raised to 420 ° C and slowly lowered, and kept at 400 ° C for 6 hours to obtain co-pyrolysis products.

[0024] The reaction product was subjected to repeated thermal extraction with petroleum ether and pyridine as solvents until the filtrate was colorless and clear. After suction filtration and drying, the carbon-coated iron nanometer hollow particle material is obtained.

[0025] as attached figure 1 X-ray diffraction (XRD) analysis shows that the metal shell of the obtained product is composed of iron (α-Fe), and the carbon shell has a high density and orderly arrangement; as shown ...

Embodiment 2

[0027] The operation method is the same as in Example 1, except that 10g of phloroglucinol and 30g of cobaltocene are weighed in a weight ratio of 1:3 and dissolved in acetone, and 100ml of high-temperature-resistant simethicone oil is added as a reaction medium. Under protection, the temperature was gradually raised from room temperature to 540°C for pyrolysis reaction, and then the temperature was lowered to 400°C for 8 hours. Finally, carbon-coated cobalt nano hollow particle materials were obtained, and there were metal element particles with smaller particle sizes in some shell nanoparticles. According to X-ray diffraction and transmission electron microscope (TEM) photos, the average thickness of the carbon-coated metal shell is about 2.2nm, the metal component is mainly cobalt, and the smaller particle size distribution of the core part is 35-50nm.

Embodiment 3

[0029] The operation method is the same as in Example 1, except that 20 g of phenol and 10 g of palladium acetylacetonate are weighed and dissolved in acetone at a weight ratio of 1:0.5, and 80 ml of high-temperature-resistant simethicone oil is added. The temperature is raised to 500° C. for pyrolysis reaction, and then the temperature is lowered to 400° C. for 4 hours to obtain a carbon-coated palladium nano hollow particle material with significantly increased amorphous carbon content. According to X-ray diffraction and transmission electron microscope (TEM) photos, the average thickness of the carbon-coated metal shell is about 4.3nm, the diameter of the nanoparticles ranges from 25nm to 40nm, and the metal component is mainly elemental palladium.

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Abstract

The invention provides a preparation method of a carbon-coated transition metal nano hollow particle. The method comprises the following steps: based on a Kirkendall effect, carrying out dissolving and mixing, high temperature co-pyrolysis and insulation in-situ reduction on an aromatic hydrocarbon compound with oxygen-containing groups and a transition metal compound so as to obtain the carbon coated metal nano hollow particle. The hollow structure shell layer prepared by the method consists of carbon and a nano metal composite material; and the nano particles are evenly distributed, the diameter range of the nano particle is 20nm-80nm, and the thickness of the carbon-coated layer is 2.2nm-4.3nm.

Description

technical field [0001] The invention relates to a carbon-coated material, in particular to a preparation method of carbon-coated transition metal simple nanometer hollow particles. Background technique [0002] Carbon-coated transition metal nano-hollow particles are a new class of hollow-structured nanocomposites. Since the nano-metal material is covered by the carbon shell, it can avoid the problem that the nano-hollow metal particles cannot exist stably in the air; in addition, due to the existence of the carbon coating, the recycling performance of the composite material can be improved, so in the lithium ion secondary Battery anode materials have broad application prospects. [0003] At present, the preparation methods of hollow nanomaterials mainly include template method and non-template method. Wherein template method (comprising soft template method and hard template method) follow-up processing needs to remove template, if template is not removed clean, may cause...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1393H01M4/134
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 宋怀河郭晓丰陈晓红
Owner BEIJING UNIV OF CHEM TECH
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