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Preparation method and application of porous graphene-based composite film material

A technology of porous graphene and composite film, which is applied in the manufacture of hybrid/electric double layer capacitors, hybrid capacitor electrodes, etc. Achieve high energy/power density, long cycle life, good application prospects

Inactive Publication Date: 2019-12-20
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, graphene sheets are prone to agglomeration, which affects its application as a substrate for flexible electrodes.
Researchers at home and abroad proposed to introduce supports between graphene sheets. For example, YamingWang et al. self-assembled carbon black particles and graphene nanosheets into graphene / carbon black composite film flexible electrode materials (J.Power Sources, 2014, 271,269-277), the carbon black particles play the role of spacer graphene nanosheets, and show excellent rate characteristics; but due to the limitation of the electric double layer energy storage mechanism, the specific capacity of the graphene / carbon black composite film is only 112F g -1
Pooi See Lee et al. introduced pseudocapacitive materials between graphene sheets, which effectively suppressed the agglomeration of graphene and improved the specific capacity of flexible electrode materials (Adv.Mater.,2013,25(20):2809-2815); However, for pseudocapacitive materials, especially metal oxides, the addition of graphene-based flexible electrode materials tends to destroy the conductive network of graphene.
In order to solve this problem, Jie Liu et al. introduced third-phase carbon nanotubes into graphene / manganese dioxide powder to improve the conductivity and flexibility of the composite material, and prepared graphene / manganese dioxide / carbon nanotube composite films (Nano Lett.,2012,12(8):4206-4211), the composite thin film shows a high specific capacity of 372F g as a flexible monolithic electrode material -1 ; but because most of the electrolyte ions transport and diffuse in the direction between graphene layers, and the ion transport ability in the radial direction is poor, resulting in a rapid decline in the specific capacity in the case of high-current charge and discharge, the rate characteristics of the electrode material are poor Poor, its specific capacity retention rate is only 45%

Method used

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  • Preparation method and application of porous graphene-based composite film material
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  • Preparation method and application of porous graphene-based composite film material

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Experimental program
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Embodiment 1

[0047] (1) Preparation of porous graphene dispersion: the graphite oxide dispersion was prepared by the Hummers method, and the concentration of graphite oxide in the aqueous dispersion was 0.5mg mL -1 , take 100mL of graphite oxide dispersion and ultrasonically treat it for 1h to make it evenly dispersed; add 0.0606g of KMnO in the state of continuous stirring 4 , 1000W microwave heating for 5min; when the temperature drops to room temperature, add 50mL deionized water, 100μL hydrazine hydrate and 350μL ammonia water in sequence; after mixing evenly, heat in a water bath at 100°C for 20min, cool to room temperature, add 2g of oxalic acid and stir At least 12h; filter with suction, wash the final product with deionized water to neutrality, and prepare a concentration of 0.33mg mL -1 porous graphene dispersion.

[0048] (2) Carbon nanotubes@MnO 2 Preparation of the dispersion: Take 20mg of carbon nanotubes and disperse them in 200mL of deionized water, add 160mg of KMnO 4 , ...

Embodiment 2

[0056] (1) Preparation of porous graphene dispersion: the graphite oxide dispersion was prepared by the Hummers method, and the concentration of graphite oxide in the aqueous dispersion was 0.2mg mL -1 , take 100mL of graphene oxide suspension and ultrasonically treat it for 1h to make it evenly dispersed; add 0.0545g of KMnO 4 , 800W microwave heating for 10min; when the temperature drops to room temperature, add 50mL deionized water, 200μL hydrazine hydrate and 500μL ammonia water in sequence; after mixing evenly, heat in a water bath at 95°C for 40min, cool to room temperature, add 2g oxalic acid and stir for at least 12h; Suction filtration, the final product was washed with deionized water until neutral, and prepared into 0.2mg mL -1 porous graphene dispersion.

[0057] (2) Carbon nanotubes@Fe 2 o 3 Preparation of dispersion: take 280mg FeCl 3 ·6H 2 O was added to 160mL deionized water, stirred evenly, added 20mg carbon nanotubes, ultrasonically treated to disperse t...

Embodiment 3

[0062] (1) Preparation of porous graphene dispersion: the graphite oxide dispersion was prepared by the Hummers method, and the concentration of graphite oxide in the aqueous dispersion was 1mg mL -1 , take 100mL of graphene oxide suspension and ultrasonically treat it for 1h to make it evenly dispersed; add 0.7271g of KMnO 4 , 1200W microwave heating for 8min; when the temperature drops to room temperature, add 50mL deionized water, 500μL hydrazine hydrate and 700μL ammonia water in sequence; after mixing evenly, heat in a water bath at 98°C for 30min, cool to room temperature, add 2g oxalic acid and stir for at least 12h; Suction filtration, the final product was washed with deionized water until neutral, and prepared into 0.8mg mL -1 porous graphene dispersion.

[0063] (2) Carbon nanotubes@Ni(OH) 2 Preparation of the dispersion: 20 mg of carbon nanotubes were ultrasonically dispersed in 40 mL of deionized water, and 4 mmol of NiCl was added 2 ·6H 2 O, after stirring ev...

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Abstract

The invention discloses a preparation method of a porous graphene-based composite film material. The preparation method comprises the following steps of: (1) preparing porous graphene dispersion liquid; (2) preparing a carbon nanotube and pseudocapacitor material dispersion liquid; (3) preparation of a composite film material: mixing the porous graphene dispersion liquid and the carbon nanotube and pseudocapacitor material dispersion liquid, and performing ultrasonic treatment, carrying out vacuum filtration, naturally drying a filter cake, and performing stripping to obtain a porous graphene / carbon nanotube and pseudocapacitor material composite film material. The porous graphene-based composite film material prepared by the invention can be directly used as a flexible electrode materialin the absence of a conductive agent and a binder; the material has the advantages of excellent rate capability, high energy / power density, long cycle service life, low raw material cost, simple process and environmental friendliness, and has a good application prospect in the field of electrode materials of flexible supercapacitors.

Description

technical field [0001] The invention relates to the structural design and preparation of flexible composite electrode materials, and belongs to the fields of material science and electrochemical technology, and more specifically relates to a preparation method and application of a porous graphene-based composite thin film material. Background technique [0002] With the rapid development of electronic technology, mobile electronic devices are gradually becoming more flexible, thinner and wearable. However, traditional energy storage devices (such as batteries) are rigid products, and when folded or bent, it is easy to cause separation of electrode materials and current collectors, degrade electrochemical performance, and even cause short circuits, posing a huge safety hazard. Therefore, in order to adapt to the development of a new generation of flexible electronic devices, new thin and flexible electrochemical energy storage devices have become a research hotspot today. ...

Claims

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Application Information

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IPC IPC(8): H01G11/32H01G11/36H01G11/26H01G11/86
CPCH01G11/26H01G11/32H01G11/36H01G11/86Y02E60/13
Inventor 江丽丽侯宝权盛利志
Owner JILIN INST OF CHEM TECH
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