Method for preparing spheroidal graphene

A technology of spherical graphite and graphene, which is applied in the field of preparing graphene powder materials, can solve the problems of taking up a lot of space during transportation and storage, weakening the excellent properties of graphene sheets, and limiting the scope of application, so as to achieve controllable processing capacity. Adjustable, suitable for large-scale production, high safety performance

Active Publication Date: 2012-06-27
BTR NEW MATERIAL GRP CO LTD
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Problems solved by technology

In the above methods, self-assembly is used to form three-dimensional graphene materials through chemical reactions. In practical applications, even if they can be well dispersed, they are dispersed in spherical form. Graphene balls or graphene flowers are not easy to disperse into monomer graphene. This weakens the excellent properties of graphene sheets and limits its application range.
Moreover, the prepared graphene has a small density and a large volume, which will take up a lot of space during transportation and storage, resulting in a waste of resources.

Method used

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  • Method for preparing spheroidal graphene
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  • Method for preparing spheroidal graphene

Examples

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Effect test

Embodiment 1

[0027] In the first step, graphene is prepared according to Example 1 of the redox method disclosed in Chinese Patent Publication No. CN101997120A to obtain graphene powder. The tap density of graphene is 0.09 g / mL.

[0028] The second step is to disperse the graphene powder in water, the concentration is 3mg / mL, the frequency is 28kHz, and the power is 1800W / cm 2 , sonicated for 10 min, granulated and dried to obtain spherical graphene powder.

[0029] like figure 1 As shown, the microscopic morphology of graphene is spherical, the diameter is distributed in the range of 5-15 μm, and the tap density of spherical graphene is 0.25 g / mL. like figure 2 and 3 As shown, the graphene sheets are distributed between 1-10, and the thin-layer graphene sheets exist stably in the form of microspheres with uniform size.

Embodiment 2

[0031] The first step is graphene prepared by epitaxial growth method. References: 1. Berger, C.; Song, Z.; Li, T.; Li, X.; Ogbazghi, A.Y.; Feng, R.; Dai, Z.T.; Marchenkov, A.N.; Conrad, E.H.; de Heer, W.A.J.Phys.Chem.B, 2004, 108(52):19912; 2, Berger, C.; Song, Z.; Li, X.; Wu, X.; Brown, N.; Naud, C. ; Mayou, D.; Li, T.; Hass, J.; Marchenkov, A.N.; Conrad, E.H.; Clean the surface of the SiC single crystal first, and the process is as follows: 1. Use analytically pure carbon tetrafluoride, acetone, ethanol, and deionized water to ultrasonically clean it several times to remove the organic matter adsorbed on the surface; 2. Use a mixture of concentrated sulfuric acid and hydrogen peroxide (Volume ratio 1: 1) Rinse with deionized water after soaking for 5 minutes to remove oxides, metals and organic impurities on the surface; 3. Etch the surface for 3 minutes with 5% hydrofluoric acid solution to remove the oxide layer on the surface; 4. Finally, rinse with deionized water sev...

Embodiment 3

[0034] The first step is to prepare graphene by chemical vapor deposition. For graphene prepared by chemical vapor deposition, refer to the literature: Obraztsov, A.N.Nat.Nanotechnol., 2009, 4:212. The specific operation steps are as follows: 1. A uniform nickel layer with a thickness of 400 nm is plated on the surface of a single crystal silicon wafer with a thickness of 0.7 mm by sputtering method, and this is used as a plane substrate. 2. Carry out high-temperature annealing treatment in a tube furnace, heat the flat substrate to 1000°C at a heating rate of 5°C / min, and then introduce a high-temperature decomposable precursor ethylene atmosphere, and carbon atoms will grow and deposit on the surface of the nickel layer. The time is 30 minutes. Cool to room temperature in the air; 3. Put the substrate with graphene on the surface into ferric chloride solution with a concentration of 1mol / L for chemical corrosion, and the soaking time is 24h. Graphene will float on the surfa...

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Abstract

The invention discloses a method for preparing spheroidal graphene, and a technical problem to be solved is to increase the density of graphene and make the transportation and storage convenient. The method comprises the following steps: dispersing graphene in water or alcohol, carrying out ultrasonic processing or ball milling, and carrying out granulation and drying to obtain the spheroidal graphene; or dispersing graphene in water with stirring, carrying out decentralized processing, and carrying out granulation and drying to obtain the spheroidal graphene. Compared with the prior art, by high temperature granulation or low temperature refrigeration granulation processing, the obtained graphene has uniform structure, small volume, large density, good electrical conductivity, and convenience in transportation, and can be applied in catalyst carrier, drug delivery, lithium ion battery and super capacitor as a carbosphere; by ultrasonic processing, the spheroidal graphene is dispersedinto graphene monomers with less than 10 layers, and the excellent properties of the graphene are kept, the obtained spheroidal graphene can be convenient for being applied in various fields, the safety performance is high, the continuous preparation production can be realized, the processing capacity can be controllable and adjustable, and the invention is suitable for large scale production.

Description

technical field [0001] The invention relates to a method for preparing nanometer materials, in particular to a method for preparing graphene powder materials. technical background [0002] In 2004, Geim's group at the University of Manchester used mechanical exfoliation for the first time to obtain a single-layer two-dimensional atomic crystal - graphene. The discovery of graphene has enriched the family of carbon materials, forming a complete system from zero-dimensional fullerenes, one-dimensional carbon nanotubes (CNTs), two-dimensional graphene to three-dimensional diamond and graphite. Single-layer graphene is composed of carbon atoms with sp 2 It is composed of monoatomic layers connected by hybridization, and its basic structural unit is the most stable benzene six-membered ring in organic materials. Its theoretical thickness is only 0.335nm, which is the thinnest two-dimensional material found so far. Graphene, the building block of other graphitic materials, can b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y40/00C01B32/184
Inventor 梁奇梅佳时浩丁世云吕雪孔东亮
Owner BTR NEW MATERIAL GRP CO LTD
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