Method capable of preparing few-layer graphene powder in batches

A technology of few-layer graphene and graphene powder, which is applied in the energy field, can solve the problems of poor electrical conductivity and easy agglomeration of graphene, and achieve the effects of good crystallinity, preventing a large amount of agglomeration, and facilitating rapid washing

Active Publication Date: 2015-07-15
SHANDONG YUHUANG NEW ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to make up for the deficiencies of the prior art, the present invention provides a simple, rapid, and batch-ready method for preparing few-layer (less than 10 layers) graphene powder, which solves the problem of graphene powder in the preparation process existing in the prior art. Problems such as easy agglomeration and poor conductivity

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  • Method capable of preparing few-layer graphene powder in batches
  • Method capable of preparing few-layer graphene powder in batches
  • Method capable of preparing few-layer graphene powder in batches

Examples

Experimental program
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Embodiment 1

[0031] The preparation process of few-layer graphene powder:

[0032] (1) Graphene oxide: Using the Hummers method, mix 50g of natural graphite with 25g of sodium nitrate in an ice bath, add 1.15L of concentrated sulfuric acid, then add 150g of potassium permanganate, react for 2 hours, heat up to 35°C for 50 minutes , then add 0.75L of deionized water, keep at 90-100°C for 20-30 minutes, then add 0.15L of hydrogen peroxide and 7L of deionized water to obtain a bright yellow graphite oxide solution; after that, use 5% sulfuric acid solution and deionized The water is alternately centrifuged until there is no sulfate ion, pH=5-6, and a pure graphite oxide solution is obtained; finally, graphite oxide is ultrasonically treated to prepare a graphene oxide solution with a certain concentration.

[0033] (2) Hydrazine hydrate reduction: Using hydrazine hydrate reduction method, add 2L deionized water to 2L 0.5mg / mL graphene oxide solution, add 1.4 mL hydrazine hydrate (mass fractio...

Embodiment 2

[0037] The preparation process of few-layer graphene powder:

[0038] (1) Graphene oxide: Same as Embodiment 1.

[0039] (2) Reduction of hydrazine hydrate: same as embodiment one.

[0040] (3) Flocculation floating suction filtration: use 5% hydrochloric acid solution by mass fraction as the flocculation floating agent, mix 1 volume of graphene colloid solution with 2 volumes of 5% hydrochloric acid solution, and let stand at room temperature (-25°C) for 1 Hours, graphene slowly gathers, floats above the solution, washes with deionized suction filtration water, removes chloride ions, and then washes and freeze-dries to obtain graphene powder reduced by hydrazine hydrate, with a specific surface area of ​​about 346.1 m 2 / g, the conductivity is about 370.7 S / m.

[0041] (4) Thermal reduction treatment: Put the dried graphene reduced by hydrazine hydrate into a tube furnace, raise the temperature at a rate of 10°C / min under the protection of nitrogen, keep it at 1050°C for 1 ...

Embodiment 3

[0043] The preparation process of few-layer graphene powder:

[0044] (1) Graphene oxide: Same as Embodiment 1.

[0045] (2) Reduction of hydrazine hydrate: same as embodiment one.

[0046] (3) Flocculation floating suction filtration: use 5% sodium hydroxide solution as the flocculation floating agent, mix 1 volume of graphene colloid solution with 2 volumes of 5% sodium hydroxide solution, room temperature (-25°C ) to stand still for 1 hour, graphene slowly aggregated and floated above the solution, washed with deionized suction filtration water until pH = 7, and then freeze-dried to obtain graphene powder reduced by hydrazine hydrate, with a specific surface area of ​​about 270.1 m 2 / g, the conductivity is about 168.1 S / m.

[0047] (4) Thermal reduction treatment: Put the dried graphene reduced by hydrazine hydrate into a tube furnace, raise the temperature at a rate of 10°C / min under the protection of nitrogen, keep it at 1050°C for 3 hours, and cool to room temperature...

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Abstract

The invention particularly relates to a method capable of preparing few-layer graphene powder in batches. By using various electrolytes as a flocculent floating agent of a graphene colloidal solution, the graphene quickly floats on the upper side of the solution to prepare the graphene powder. According to the method provided by the invention, a diluted graphene oxide solution is reduced by virtue of hydrazine hydrate to form the graphene colloidal solution, so that the reductive graphene is prevented from being agglomerated in a large quantity. By using the flocculent floating agents of electrolyte solutions of acids, bases and alkalis, the graphene is quick to wash, so that the method is simple to operate and beneficial for quantity production and has a wide prospect of large-scaled industrialized application. The diluted solution is used in the method, so that the whole reaction process is less in influence on the environment. Moreover, the waste liquid contains few ions, so that the treatment cost is low.

Description

(1) Technical field [0001] The invention belongs to the preparation technology of micro-nano materials in the field of energy, and in particular relates to a method for preparing few-layer graphene powder in batches. (2) Background technology [0002] Graphene is a carbon atom with sp 2 The single-layer planar film composed of hexagonal and honeycomb lattice arrangement composed of hybridized orbitals is a two-dimensional material with a thickness of only one carbon atom. The basic unit of graphite). Graphene has excellent physical and chemical properties, and has been gradually used in transparent conductive films, nanoelectronic devices (transistors, transistor circuit interconnection memory semiconductors), conductive inks, solar cells, lithium batteries, supercapacitors, sensors and biomedicine and other fields. [0003] One of the current methods that may realize large-scale production of graphene powder is the method of combining the Hummers method (Preparation of gr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
Inventor 陈欣肖双王胜伟王瑛赵成龙董贺存张兵
Owner SHANDONG YUHUANG NEW ENERGY TECH
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