Preparation method of grapheme three-dimensional entity

A technology of three-dimensional solids and graphene, which is applied in the field of preparation of three-dimensional graphene solids, can solve problems such as low density and rough solid surface, and achieve the effects of convenient operation, improved mechanical properties and electrical properties

Inactive Publication Date: 2011-08-10
SOUTHEAST UNIV
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  • Claims
  • Application Information

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Problems solved by technology

Some researchers used the hydrothermal reduction method to prepare three-dimensional graphene solids (Xu, Y.X., Sheng, K.X., Li, C. et al. ACS NANO 2010, 4, 4324), and their mechanical and electrical properties are relatively better than those previously used The properties of the entities obtained by colloidal self-assembly have been greatly improved, but these entities are obtained without adding alkaline solution, resulting in the rough surface of these entities, and the low density, which makes it unable to meet many requirements. field requirements

Method used

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  • Preparation method of grapheme three-dimensional entity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: The first step, weigh 55mg of graphene oxide sheets, place in a beaker, add 33ml of deionized water in the beaker, then carry out ultrasonic dispersion (40KHz, 15min), make the solution without obvious particles, then add ammonia water Make the pH of the solution 10;

[0019] In the second step, pour the solution in the beaker into the inner cup of the hydrothermal reaction kettle (volume 50ml), tighten the lid of the outer cup, put it upright in the drying oven, set the heating rate to 50°C / min, and the reaction temperature to 180°C. The reaction time is 15 hours, and it is naturally cooled after the reaction is completed. Scanning electron micrographs of the three-dimensional solids of graphene as figure 2 As shown, it can be observed that the surface is smooth;

[0020] The third step is to dry the prepared entity at 45°C and normal pressure for 15h; the scanning electron micrograph of the dried product is as follows: image 3 with Figure 4 shown....

Embodiment 2

[0024] Embodiment 2: The preparation method is basically the same as in Example 1, the difference is: the dispersion of graphene oxide is achieved by stirring, and less ammonia water is added to make the solution pH=8, Figure 5 It is a scanning electron micrograph of the obtained three-dimensional graphene solid, and it can be seen that the surface of the obtained solid is also very smooth. Table 2 is a comparison of the relative properties of the graphene three-dimensional entity and the three-dimensional entity obtained without ammonia water.

[0025] sample

[0026] Table 2

Embodiment 3

[0027] Embodiment 3: The preparation method is basically the same as that of Embodiment 1, the difference is: the heating rate of the drying oven is set to 5°C / min, and the following figure 2 Similar results are shown, see Table 3 for performance comparison.

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Abstract

The invention discloses a method for preparing a grapheme three-dimensional entity with a hydrothermal reduction method. The method comprises the following steps of: mixing oxidized grapheme with water; stirring or ultrasonically dispersing to form an oxidized grapheme solution with the mass volume concentration between 1 mg/ml and 10 mg/ml; adding an alkali solution to adjust the pH value of the solution to 8-13; pouring the solution into a hydrothermal reaction kettle; putting the reaction kettle into a drying oven and raising the temperature to 100-400 DEG C for reacting for 3-48 hours; cooling; and taking the product out and drying to obtain the grapheme three-dimensional entity. The grapheme entity prepared with the method has a smooth surface, high density and high electric conductivity. The preparation method is convenient to operate, and is simple and practical.

Description

technical field [0001] The invention relates to a method for preparing a graphene three-dimensional entity. Background technique [0002] Along with the discovery of graphene, its excellent electrical property, mechanical property, thermal property and magnetic property have caused people's widespread concern, and the method for preparing graphene also emerges in endlessly simultaneously, mainly contains micromechanical exfoliation method (Novoselov, K.S., Geim , A.K., Morozov, S.V., Jiang, D., Zhang Y., Dubonos, S.V. et al. Science 2004, 306, 666), chemical method (Stankovich, S., Dikin, D.A. et al. Carbon 2007, 45, 1558 ) and epitaxial growth method (Kim, K.S., Zhao, Y.et al.Nature 2009, 457, 706), researchers have studied the properties of graphene prepared by these methods, but most of the research objects are thickness It is a graphene film below the micron level. The graphene three-dimensional entity is formed by the chaotic agglomeration of graphene sheets, with a l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 孙立涛毕恒昌尹奎波万能徐峰
Owner SOUTHEAST UNIV
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