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Preparation method of high-conductivity hydroxyl/epoxy group externally modified graphene transparent conductive film

A technology of transparent conductive film and high conductivity, which is applied in the direction of graphene, chemical instruments and methods, and bulk chemical production, etc. It can solve the problems of graphene materials that are difficult to handle, have large structural damage, and high oxygen content, and achieve easy reduction Treatment, the effect of less damage to the sheet structure, and high conductivity

Active Publication Date: 2018-07-24
广州金穗芯能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the shortcomings of the existing technology, a new method for the preparation of graphene-based transparent conductive films is proposed to solve the problems of difficult handling of graphene materials, poor conductivity, high oxygen content, and large structural damage
The soluble graphene prepared by the present invention has little damage to the sheet structure of graphene, overcomes the problem that graphene is difficult to handle and easy to pile up, thus endows graphene with further processing performance and handleability, and realizes the performance of graphene Better retention, high conductivity graphene transparent conductive film can be obtained

Method used

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  • Preparation method of high-conductivity hydroxyl/epoxy group externally modified graphene transparent conductive film
  • Preparation method of high-conductivity hydroxyl/epoxy group externally modified graphene transparent conductive film
  • Preparation method of high-conductivity hydroxyl/epoxy group externally modified graphene transparent conductive film

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Mix 30g of iodine bromide and 50mg of expanded graphite evenly, fill it with protective gas Ar, seal it in a 50mL glass bottle, place it in an oil bath environment at 100°C, and heat it for 12h to prepare a third-order graphite intercalation compound.

[0026] (2) The graphite intercalation compound was quickly taken out from the glass bottle and filtered.

[0027] (3) Put the intercalation compound into a hydrothermal kettle with a volume of 50 mL rapidly.

[0028] (4) Add 10 mL of aqueous solution into the hydrothermal kettle, and quickly fix the hydrothermal kettle equipment.

[0029] (5) Heat the hydrothermal kettle to 180° C. and keep it for 1 hour. After the reaction is completed, take out the sample and clean the sample to obtain a three-atom layer high-quality graphene powder aggregate.

[0030] (6) 20mL H 2 SO 4 Maintained in ice water (0°C) for 0.5 hours.

[0031] (7) Add 30 mg of the original graphene material into concentrated sulfuric acid, and stir...

Embodiment 2

[0041] (1) Mix 30g of iodine bromide and 50mg of expanded graphite evenly, fill it with protective gas Ar, seal it in a 50mL glass bottle, place it in an oil bath environment at 100°C, and heat it for 12h to prepare a third-order graphite intercalation compound.

[0042] (2) The graphite intercalation compound was quickly taken out from the glass bottle and filtered.

[0043] (3) Put the intercalation compound quickly into a supercritical water device with a volume of 50 mL.

[0044] (4) Add 2 mL of aqueous solution to the supercritical water device, and quickly fix the device.

[0045](5) Heat the hypersupercritical water device to 180° C., raise the pressure to 22.1 Mpa, and keep it for 1 hour. After the reaction is completed, take out the sample and clean the sample to obtain graphene powder aggregates.

[0046] (6) 20mL H 2 SO 4 Maintained in ice water (0°C) for 0.5 hours.

[0047] (7) Add 30 mg of the original graphene material into concentrated sulfuric acid, and sti...

Embodiment 3

[0054] (1) 0.3g anhydrous FeCl 3 Mix with 0.05g of expanded graphite, seal in vacuum, heat up to 380°C for 1h, and maintain for 12h to prepare a third-order graphite intercalation compound.

[0055] (2) Dissolve the graphite intercalation compound in dilute hydrochloric acid solution, filter and dry with suction, and set aside.

[0056] (3) Put the graphite intercalation compound into supercritical CO with a volume of 50mL rapidly 2 device.

[0057] (4) to supercritical CO 2 Add 5mL of 30% hydrogen peroxide solution into the device, and quickly fix the device.

[0058] (5) the high supercritical CO 2 The device is heated to 38°C, the pressure is increased to 75atm, and kept for 1 hour. After the reaction is completed, the sample is taken out, and the sample is cleaned to obtain graphene powder aggregates.

[0059] (6) 20mL H 2 SO 4 Maintained in ice water (0°C) for 0.5 hours.

[0060] (7) Add 30 mg of the original graphene material into concentrated sulfuric acid, and ...

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Abstract

The invention provides a preparation method of a high-conductivity hydroxyl / epoxy group externally modified graphene transparent conductive film. The preparation method comprises the following steps:performing oxidative modification on the two outer layers of a three-atomic layer high-quality graphene by adopting a specific oxidant to obtain a hydroxyl / epoxy group externally modified three-atomiclayer graphene material which can be dispersed in a common solvent; preparing a film with three-atomic thickness by utilizing a winding bar film coating method, a spin-coating method and the like, and reducing to obtain a high-conductivity transparent conductive film. An intermediate graphene flake layer of an externally modified three-atomic layer graphene material prepared by the method provided by the invention is not oxidized, so that good conductivity is still maintained; the external two flake layers are modified with a hydroxyl / an epoxy group, so that the problems that graphene is difficult to treat and is easy to accumulate are solved. The hydroxyl / epoxy group modified three-atomic layer graphene material endows the graphene with further machinability and processability, meanwhile, maintains the performance of the graphene better, and can be applied to the fields such as photoelectric devices and energy storage.

Description

technical field [0001] The invention relates to the field of preparation of graphene-based transparent conductive films. A specific oxidant and concentrated acid system are used to oxidize the outer two layers of high-quality three-atom-layer graphene to obtain dispersible hydroxyl / epoxylated graphene with low oxygen content. Then prepare transparent conductive film. Background technique [0002] Since its discovery in 2004, graphene has attracted much attention as a new type of carbon material. Graphene is a quasi-two-dimensional crystal material composed entirely of sp2 hybridized carbon atoms with a thickness of only one atomic layer or several single atomic layers. It is almost completely transparent, has high thermal conductivity, and has high electron mobility at room temperature. It is the material with the smallest resistivity in the world, and it is also the thinnest but hardest nanomaterial in the world. Graphene materials can be widely used in high-performance n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19C01B32/194
CPCC01B2204/22Y02P20/54
Inventor 苗中正刘亚兵
Owner 广州金穗芯能科技有限公司
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