Method for preparing grapheme through organic amine solvothermal method
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An organic solvent and organic amine technology, which is applied in the field of preparing large sheets of high-quality graphene by organic amine solvothermal method, can solve the problems that graphene cannot take into account the output, graphene quality, poor quality of graphene, etc., and achieves good application prospects and oxidation degree. Light, low-cost effects
Inactive Publication Date: 2010-06-23
INST OF CHEM CHINESE ACAD OF SCI
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This method can prepare a large amount of graphene, but due to the damage of the oxidant to the graphite layer, the graphene quality is very poor and there are many defects
Other liquid-phase methods for preparing graphene cannot balance yield and graphene quality
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Embodiment 1
[0044] Embodiment 1, prepare graphene
[0045] 1) Preparation of expanded graphite
[0046] Under the condition of water bath at 20°C, add 15ml of sulfuric acid with a mass fraction of 95% and 5ml of concentrated nitric acid with a mass fraction of 65% into a 50ml three-neck flask, add 1g of graphite and 0.01g of potassium dichromate to the above mixed acid solution, and keep stirring at 30°C 40 minutes. After the reaction was completed, the mixture was poured into 200ml of water, vacuum filtered, the filter residue was rinsed with double distilled water, and the filter residue was dried at 50°C for 12 hours to obtain a large amount of black solid, namely expanded graphite.
[0047] 2) Preparation of graphene semi-dispersion
[0048] Add 30 mg of expanded graphite to 10 ml of oleylamine. Sealed in an autoclave under a nitrogen-protected environment, reacted at 170°C for 72h, and cooled to room temperature to obtain pasty semi-dispersed graphene.
[0049] 3) Preparation of ...
Embodiment 2
[0069] Embodiment 2, prepare graphene
[0070] The preparation method of graphene is basically the same as embodiment 1. The difference is: when preparing expanded graphite, 0.01 gram of potassium dichromate in Example 1 was replaced with 0.01 gram of potassium permanganate. Single-layer graphene can also be obtained with this method (see Figure 9 ).
Embodiment 3
[0071] Embodiment 3, prepare graphene
[0072] The preparation method of graphene is basically the same as embodiment 1. The difference is that when the graphene semi-dispersion is prepared, the reaction temperature is changed to 150°C, and graphene can also be obtained, but the concentration of the graphene dispersion is as low as 0.05mg / ml.
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Abstract
The invention discloses a method for preparing grapheme through organic amine solvothermal method, which comprises the following steps: 1) adopting the solvothermal method to lead expanded graphite to react with organic amine or organic amine solvent to obtain the semi-discrete liquid of grapheme; 2) implementing ultrasonic dispersion and then implementing centrifugation on the semi-discrete liquid of grapheme obtained from the step 1), and then collecting supernate, thus obtaining the grapheme. The invention obtains the grapheme by taking solvent thermal spalling as a means. A scanning electron microscope, a transmission electron microscope, and an atomic force microscope are adopted to represent the topogram of the grapheme; a Raman spectrum and an X-ray photoelectron spectroscopy are used to represent the density of imperfection and oxidation situation of the grapheme. The result shows that the grapheme synthesized by the method of the invention has the advantages of small size, high quality, less defects, light oxidation degree, etc. besides, the method for preparing grapheme through organic amine solvothermal method also has the advantages of simple synthetic route, low cost, high concentration and uneasy accumulation of the synthesized discrete liquid of grapheme, and excellent application prospect on the aspect of discrete liquid of grapheme materials.
Description
technical field [0001] The invention relates to a method for preparing large sheets of high-quality graphene by an organic amine solvothermal method. Background technique [0002] Graphene is another new carbon element structure discovered by scientists after fullerene and carbon nanotubes. 2 Hybridized carbon atoms are bonded and have a single layer of planar graphite with a hexagonal lattice honeycomb two-dimensional structure. In 2004, scientists successfully exfoliated graphene for the first time (Science 2004, 306, 666-669), which broke the theory of condensed matter physics and overturned the previously generally accepted scientific prediction that strict two-dimensional crystals cannot exist at a limited temperature , may have a significant impact on the development of condensed matter physics. In addition, graphene exhibits a series of peculiar electronic and physical properties, which have important application prospects in molecular electronics, micro-nano device...
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