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Solid-liquid interface self-assembly preparation method for graphene oxide film

A technology of graphene film and liquid interface, which is applied in the field of graphene oxide film preparation, can solve the problems of slow film forming speed, complex process and equipment, and limit the large-scale preparation of graphene film, and achieve fast film forming speed, thickness and Effects of controllable geometric area, adjustable film thickness and size

Active Publication Date: 2010-02-24
SHENZHEN CTRUST TESTING TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the processes and equipment required by the above methods are relatively complicated, and the film formation speed is relatively slow, which limits the large-scale preparation of graphene films.

Method used

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  • Solid-liquid interface self-assembly preparation method for graphene oxide film
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Examples

Experimental program
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preparation example Construction

[0031] 1. Preparation of soluble graphite oxide sheet solution: the preparation of graphite oxide solution refers to literature (Chen C M, Yang Q H, Yang Y G, et al. Self-assembled free-standing graphite oxide membrane [J]. Adv. Mater., 2009 , DOI: 10.1002 / adma.200803726.). The ratio of graphite oxide to solvent is: 1-30:1 (mg / mL), ultrasonic for 0.5-10h, ultrasonic power is 20-300W, and a well-dispersed graphite oxide solution is obtained.

[0032] In this embodiment, in addition to the water used in the literature, the graphite oxide solution solvent can also use other solvents, such as absolute ethanol, acetone, ether or methylamine, etc.

[0033]2. Preparation of anodic aluminum oxide film: After annealing, mechanical polishing, alkaline solution immersion to remove natural oxide layer, electrochemical polishing and other pretreatments, the aluminum or aluminum alloy is placed in an acidic electrolyte, and a voltage of 8235V is applied for the first time. Anodizing treatm...

Embodiment 1

[0038] Graphite oxide powder materials were prepared by Hummers method.

[0039] Weigh 10 mg of graphite oxide powder material into a 20 ml small beaker, add 10 ml of water, and ultrasonically disperse in an ice-water bath for 6 h with an ultrasonic power of 20 W to obtain a well-dispersed graphite oxide solution.

[0040] The metal aluminum foil with a size of 1.5 × 5 cm was sequentially subjected to annealing (at 400 °C, 4 h), mechanical polishing, lye immersion to remove the natural oxide layer (1 mol / L, 5 min), electrochemical polishing (perchloric acid and ethanol mixed solution, After pretreatment such as 12V, 5min), it was placed in a sulfuric acid solution with a concentration of 1.2mol / L and a temperature of 5°C, and a DC voltage of 25V was applied for anodic oxidation for 2 hours. 1.8% and 6%, respectively) for 1 h to remove the primary anodic oxide film, and then perform secondary anodic oxidation for 2 h under the same conditions to obtain an anodic aluminum oxide ...

Embodiment 2

[0043] Weigh 100 mg of graphite oxide powder material into a 20 ml small beaker, add 10 ml of absolute ethanol, and ultrasonically disperse in an ice-water bath for 4 hours with an ultrasonic power of 100 W to obtain a well-dispersed graphite oxide solution.

[0044] The preparation of the porous anodic aluminum oxide film was the same as that of Example 1.

[0045] The prepared porous anodic aluminum oxide film was immersed in the prepared graphite oxide solution with a concentration of 10 mg / ml, left standing for 2 h, taken out, and dried at 50 °C for 2 h to obtain a graphene oxide film on its surface. Using SEM measurement, the thickness of this graphene oxide film was 1 μm. The size is 1.5×4cm 2 , which is the same as the area of ​​the porous anodic aluminum oxide film substrate immersed in the solution.

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Abstract

The invention relates to a solid-liquid interface self-assembly preparation method for a graphene oxide film, which comprises the following steps: adding graphite oxide into solvent to carry out ultrasound with the ultrasonic power of 20-300W; after aluminum or aluminum alloy is carried out natural oxidation layer removal preprocessing, placing the aluminum or the aluminum alloy into acid electrolyte; applying voltage to carry out first anodic oxidation processing; soaking in a mixing solution of phosphoric acid and chromic acid to remove a first anodic oxidation film so as to retain a highlysequential shell-shaped convex-concave structure on the surface of the metal aluminum; carrying out second anodic oxidation under the same condition with the first anodic oxidation; adopting a concaveposition as an initial forming locus of a hole and forming a highly sequential hole array so as to acquire a porous anodic aluminum oxide solid film attached to a matrix of the aluminum; soaking theanodic aluminum oxide film into a prepared soluble graphene oxide film solution; standing and then taking out to air or dry to obtain the graphene oxide film. The preparation method for the graphene oxide film has simple operation, high film forming speed and adjustable thickness and size of the film.

Description

technical field [0001] The invention relates to a solid-liquid interface self-assembly preparation method of graphene oxide film, and belongs to the technical field of graphene oxide film preparation. Background technique [0002] Graphene was discovered in 2004 by a research group at the University of Manchester (Science, 306, DOI: 10.1126 / science1102896 http: / / dx.doi.org / 10.1126 / science.1102896), this two-dimensional carbon atomic crystal is a zero-dimensional structure fullerenes, one-dimensional carbon nanotubes, [0003] 3D bulk graphite etc. sp 2 The basic structural unit of hybrid carbon is one of the research hotspots in the field of carbonaceous materials and condensed matter physics. Graphene has very broad application prospects. Its peculiar properties provide a good physical experiment platform. It is also the best material for the manufacture of nanoelectronic devices, high-frequency transistors and single-electron transistors. It also has great applications i...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 杨全红张少波郭敏吕伟吴思达
Owner SHENZHEN CTRUST TESTING TECH CO LTD
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