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Method for preparing graphene

A graphene and metal technology, applied in the field of preparation of nanomaterials, can solve the problem that graphite oxide is not easy to redisperse, etc., and achieve the effects of high yield and simple operation.

Inactive Publication Date: 2011-05-04
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the direct reduction of graphene oxide with hydrogen as a reducing agent usually requires very high temperatures (for example, above 400 °C), and the graphite oxide obtained by reduction at high temperature may aggregate and is not easy to redisperse in the solution, thus limiting its application.

Method used

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  • Method for preparing graphene

Examples

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Embodiment 1

[0047] Example 1 : Palladium chloride as a catalyst to catalyze the hydrogenation of graphene oxide to prepare graphene

[0048] (1) Preparation of graphene oxide: Preparation of graphene oxide: Take about 1 g of natural flake graphite, add 20 g of concentrated sulfuric acid, stir overnight in an ice bath, add 0.15 g of potassium permanganate to prevent the temperature from rising, and stir after adding 30 minutes, then add 3 grams of potassium permanganate, control the temperature below 20 degrees, raise the temperature to 35 degrees, and keep this temperature for 30 minutes, during this process the solution becomes viscous, add 45 milliliters of water and prevent bubbling, And raise the temperature to 90-95 ° C, maintain this temperature for 15 minutes, then add 30 ml of 30% hydrogen peroxide, add 26 ml of water after stirring for 30 minutes, filter while it is hot, wash 3 times with 50 ml of 3% hydrochloric acid, and filter cake Sonicate 400 ml of water for 1 hour, centri...

Embodiment 2

[0050] Example 2 : Palladium chloride as a catalyst to catalyze the hydrogenation of graphene oxide to prepare graphene

[0051] (1) Preparation of graphene oxide: refer to embodiment 1 step (1);

[0052] (2) Preparation of Graphene: Get 60 milliliters of the above-mentioned graphene oxide solution (which contains about 60 mg of graphene oxide), add 1 milliliter of palladium chloride aqueous solution (2g / l, calculated as palladium), and place under high pressure at 25°C React for 20 hours under 5MPa hydrogen pressure in the kettle to obtain graphene. The electron micrograph of this example gained graphene (see Figure 4 ) shows that the obtained graphene exists independently, and electron diffraction photos show that it is a single-layer graphene structure (see Figure 5 ). Among them, the evaluation standard of single-layer graphene is that the brightness of the outer ring is the same as the brightness of the inner ring in the electron diffraction photo. If the brightness...

Embodiment 3

[0054] Example 3 : Palladium chloride as a catalyst to catalyze the hydrogenation of graphene oxide to prepare graphene

[0055] (1) Preparation of graphene oxide: refer to embodiment 1 step (1);

[0056] (2) Preparation of graphene: get 60 milliliters of the solution of above-mentioned graphene oxide (wherein approximately contain 60 milligrams of graphene oxide), micropipette gun takes palladium chloride aqueous solution (2g / l, counts as palladium) 0.05 milliliters and joins in The above solution was reacted for 10,000 h in an autoclave under 0.2 MPa hydrogen pressure at 200° C. to obtain graphene. The ratio of metal atoms to carbon atoms in this example is about 0.0001.

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Abstract

The invention provides a method for preparing graphene, which comprises that: a supported metal catalyst containing metals, metallic colloid particles or metal salts are used, and graphene oxide and hydrogen are reacted in a solvent to prepare the graphene at the temperature of between -50 and 200 DEG C, preferably 20 to 120 DEG C. In the method, the temperature of hydrogen reduction is reduced by utilizing the catalyst, the method is easy to operate, and high-quality graphene capable of being dissolved in solution can be prepared massively. The prepared graphene has a few impurities, high yield and the characteristics of the graphene, and can be widely applied to preparing membrane electrode materials, lithium ion battery electrode materials, super capacitor electrode materials and the like.

Description

technical field [0001] The invention relates to a preparation method of nanomaterials, in particular to a preparation method of graphene. Background technique [0002] Graphene is composed of hexagonally arranged sp 2 A two-dimensional sheet of carbon atoms with a thickness of one atom, which is the building block of graphite. It has been found that graphene has many properties that graphite does not have, such as room temperature quantum Hall effect, massless transport properties, optical properties, thermoelectric transport properties, light transmittance and extremely high Young's modulus. Due to these characteristics of graphene, graphene and graphene-based materials have potential applications in many aspects, such as display films, solar cell electrodes, lithium ion battery electrodes, field effect transistors, sensors, etc. [0003] The large-scale preparation of graphene is an important basis for its wide application and performance research, so it is very importan...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 梁明会智林杰
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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