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A method, device and application of batch and controllable preparation of graphitic carbon-coated metal/metal oxide nanoparticles

A nanoparticle and oxide technology, applied in the direction of carbon compounds, chemical instruments and methods, ferrous oxides, etc., can solve the problems of difficult to control product structure, low degree of graphitization, poor thermal stability and chemical stability, etc. , to achieve the effect of easy large-scale production, simple operation method and universality

Active Publication Date: 2022-02-11
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Among them, the arc discharge method is the earliest and commonly used method. It is a method of preparing a mixed anode composed of graphite and target-coated metal element or metal oxide by arc discharge evaporation under vacuum or inert atmosphere. The reaction conditions are relatively harsh, the yield is low, it is difficult to control the structure of the product, and there are many by-products that are difficult to avoid
Methods such as chemical vapor deposition, pyrolysis, and high-temperature carbonization are similar in nature. They all carbonize and deposit carbon-containing substances on the surface of metal particles at high temperatures to complete the coating process. The difference is the type and type of metal source and carbon source. state, the preparation process is greatly constrained by raw materials and reaction conditions, and the product is inevitably accompanied by a large number of by-products (such as carbon nanotubes, carbon nanocages, and carbon atom cluster impurities such as amorphous carbon), which cannot achieve large-scale production
The sol-gel method and the hydrothermal method have outstanding advantages in improving product yield and purity, regulating particle size and morphology, and the preparation process also has the characteristics of relatively simple equipment, mild reaction conditions, and easy control, but the inventors found that: Due to the low reaction temperature, the carbon shell is mainly composed of amorphous carbon, with a low degree of graphitization and poor thermal and chemical stability.

Method used

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  • A method, device and application of batch and controllable preparation of graphitic carbon-coated metal/metal oxide nanoparticles
  • A method, device and application of batch and controllable preparation of graphitic carbon-coated metal/metal oxide nanoparticles
  • A method, device and application of batch and controllable preparation of graphitic carbon-coated metal/metal oxide nanoparticles

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[0032] As introduced in the background technology, the carbon-coated nano-metal / metal oxide carbon prepared by the existing method has the problems of low degree of graphitization, poor thermal stability and chemical stability. Therefore, the present invention proposes a batch, controllable preparation method for preparing graphitic carbon-coated metal / metal oxide nanoparticles, comprising the steps of:

[0033] 1. Stir and dissolve Tris in deionized water, configure Tris buffer solution, and adjust the pH with concentrated hydrochloric acid;

[0034] 2. Disperse the ratio of metal / metal oxide nanoparticles and dopamine hydrochloride in the Tris buffer solution prepared in the first step, then stir at room temperature, centrifuge, and vacuum dry;

[0035] 3. The above-prepared dopamine-coated metal / metal oxide nanoparticles are heated in a microwave fluidized bed under nitrogen atmosphere to prepare graphitic carbon-coated metal / metal oxide nanoparticles.

[0036] In some embod...

Embodiment 1

[0043] A batch and controllable preparation of graphitic carbon-coated Fe 3 o 4 The method for nanoparticles, comprising the steps of:

[0044] (1) Stir and dissolve 1.2114g Tris in 1L deionized water, prepare a Tris buffer solution, and adjust the pH to 8.5 with concentrated hydrochloric acid;

[0045] (2) Add 2.0g of Fe 3 o 4 and 2.0 g of dopamine hydrochloride were dispersed in the Tris buffer solution prepared in the first step according to a ratio of 1:1, then continuously stirred at room temperature for 10 hours, centrifuged, and vacuum-dried at 50° C. for 12 hours;

[0046] (3) Coating Fe with 1.0 g of dopamine prepared above 3 o 4 , heated at 1500W solid-state microwave source for 15min in a nitrogen atmosphere to prepare graphite carbon-coated Fe 3 o 4 nanoparticles.

[0047] Depend on Figure 1 to Figure 3 It can be seen that the present invention achieves fluidized uniform heating of materials under microwaves by simulating a fluidized bed, and prevents mat...

Embodiment 2

[0051] A batch and controllable preparation of graphitic carbon-coated Fe 3 o 4 The method for nanoparticles, comprising the steps of:

[0052] (1) Stir and dissolve 1.2114g Tris in 1L deionized water, prepare a Tris buffer solution, and adjust the pH to 8.5 with concentrated hydrochloric acid;

[0053] (2) Add 2.0g of Fe 3 o 4 and 4.0 g of dopamine hydrochloride were dispersed in the Tris buffer solution prepared in the first step according to a ratio of 1:2, then continuously stirred at room temperature for 24 hours, centrifuged, and vacuum-dried at 60° C. for 12 hours;

[0054] (3) Coating Fe with 1.0 g of dopamine prepared above 3 o 4 , heated at 1000W solid-state microwave source for 15min in a nitrogen atmosphere to prepare graphitic carbon-coated Fe 3 o 4 nanoparticles.

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Abstract

The present invention relates to a batch and controllable method, device and application for preparing graphite carbon-coated metal / metal oxide nanoparticles. The method uses dopamine hydrochloride dispersed in Tris buffer solution to process metal / metal oxide nanoparticles Coating by polymerization, followed by centrifugation and vacuum drying to prepare dopamine-coated metal / metal oxide nanomaterials; The carbon-coated metal / metal oxide prepared above is subjected to targeted heating to catalyze the graphitization conversion of the carbon layer in a fluidized bed to obtain graphitic carbon-coated metal / metal oxide nanomaterials. The graphitic carbon-coated metal / metal oxide nanomaterial obtained in the present invention has uniform appearance, high purity, and good monodispersity; high yield and efficiency, relatively low cost, relatively simple reaction device; and can realize large-scale preparation , with industrial prospects.

Description

technical field [0001] The invention belongs to a method for preparing graphite carbon-coated metal / metal oxide nanoparticles, and particularly relates to a controllable shape and size that can be applied to the fields of catalytic materials, biomedicine, magnetic recording materials, electrode materials, etc. A series of methods for preparing carbon-coated metal / metal oxide nanoparticles. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Carbon-coated nanometer metal / metal oxide is a new type of functional composite material with a core-shell structure. The cladding shell layer is an amorphous carbon structure or a multilayer graphite layer structure, and the inner core i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08C01B32/205B82Y30/00
CPCC01G49/08C01B32/205B82Y30/00C01P2004/80C01P2004/03C01P2004/04C01P2002/82C01P2006/40
Inventor 孙静于冠群江镇宇王文龙宋占龙赵希强毛岩鹏
Owner SHANDONG UNIV