A kind of graphene-supported nitrogen-doped carbon nanotube composite material and its preparation and application

A technology of nitrogen-doped carbon and composite materials, applied in fuel cell half-cells and primary battery half-cells, structural parts, electrical components, etc., can solve problems such as poor cycle stability and achieve excellent catalytic performance , Improve the conductivity and stability, and the effect of high cycle stability

Active Publication Date: 2022-08-02
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the above defects or improvement needs of the prior art, the present invention provides a graphene-supported nitrogen-doped carbon nanotube composite material and its preparation and application, which is achieved by in-situ growth of graphene and nitrogen-doped carbon nanotubes Connected, the resulting large continuous two-dimensional layered multi-level structure composite material, when used as an electrode active material for a rechargeable zinc-air battery, exhibits an ultra-long (up to 3000 hours) battery life, thus solving the problem of The technical problem of poor cycle stability when the existing graphene-supported nitrogen-doped carbon nanotube composites are used as battery electrode active materials

Method used

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  • A kind of graphene-supported nitrogen-doped carbon nanotube composite material and its preparation and application
  • A kind of graphene-supported nitrogen-doped carbon nanotube composite material and its preparation and application
  • A kind of graphene-supported nitrogen-doped carbon nanotube composite material and its preparation and application

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preparation example Construction

[0043] The invention provides a method for preparing a graphene-loaded nitrogen-doped carbon nanotube composite material, which is characterized in that it includes the following steps:

[0044] (1) with graphene oxide solution, the organic solution of transition metal salt and the organic solution of organic ligand, mix and stir for several hours, solid-liquid separation obtains solid, it is the precursor of graphene oxide supported metal organic framework material; Described The organic solution of the organic ligand also includes a nucleation promoter, and the nucleation promoter is used to promote the crystallization, nucleation and uniform dispersion of the metal-organic framework material on the graphene oxide surface;

[0045] (2) annealing the precursor obtained in step (1) in a reducing atmosphere to convert transition metal ions in the precursor into metal nanoparticles, and catalyze the conversion of organic ligands into nitrogen-doped carbon nanotubes, Obtain the s...

Embodiment 1

[0090] Example 1: Preparation of ZIF-67@GO-4

[0091] First, 2 ml of graphene oxide was ultrasonically dispersed in 10 ml of methanol, and then 291 mg of Co(NO 3 ) 2 ·6H 2 O and 657 mg of 2-methylimidazole were dissolved in 20 ml of methanol. After adding 10 μl of triethylamine to the 2-methylimidazole solution, the Co(NO 3 ) 2 ·6H 2 O and the 2-methylimidazole solution containing triethylamine were poured into the GO solution in turn, magnetically stirred at room temperature for 3 h, centrifuged and dried, and the obtained product was redispersed into 10 ml of methanol solution, and Co(NO) was added again. 3 ) 2 ·6H 2 O and 2-methylimidazole solution containing triethylamine, magnetic stirring for 3 h, repeated four times to obtain the ZIF-67@GO-4 precursor. figure 1 (b) and figure 1 (c) is the scanning electron microscope image of ZIF-67@GO-4, it can be seen from the figure that ZIF-67 is evenly distributed on both sides of GO.

Embodiment 2

[0092] Example 2: Preparation of GNCNTs-4

[0093] The ZIF-67@GO-4 in Example 1 was placed in the tube furnace, and the H 2 / Ar mixture (H 2 The volume percentage of the mixture is 5%), heated to 700°C at a rate of 2°C / min, kept at this temperature for 3h, cooled naturally, placed in 0.5M H 2 SO 4 48h, centrifugal drying to obtain GNCNTs-4 material. figure 1 (d) is the scanning electron microscope photo of GNCNTs-4. It can be seen from the figure that the CNTs are distributed on both sides of the graphene in a layered and multi-level structure. figure 1 (e), figure 1 (f) and figure 1 (g) is the transmission electron micrograph of GNCNTs-4, showing the successful preparation of CNTs. figure 1 (h), figure 1 (i), figure 1 (j) andfigure 1 (k) is the mapping characterization map of GNCNTs-4, showing the presence of C, N, and Co.

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Abstract

The invention belongs to the field of energy storage nanomaterials, and more particularly relates to a graphene-supported nitrogen-doped carbon nanotube composite material and its preparation and application. It first grows metal-organic framework materials on graphene oxide sheets, and uses nucleation promoters to promote the protonation of organic ligands to accelerate the nucleation and dispersion of metal-organic frameworks on graphene oxide, resulting in uniform loading of graphene oxide. The precursor of the metal-organic framework is then annealed at high temperature to obtain the graphene-supported nitrogen-doped carbon nanotube material. Integrating this material into an air electrode for zinc-air batteries at 5 mA cm ‑2 Under the condition of charge and discharge, ultra-high stability performance of 3000h can be achieved.

Description

technical field [0001] The invention belongs to the field of energy storage nanomaterials, and more particularly relates to a graphene-supported nitrogen-doped carbon nanotube composite material and its preparation and application. Background technique [0002] Rechargeable zinc-air batteries have the advantages of low cost, high voltage, high theoretical energy density, and environmental protection, and are considered to be one of the most promising batteries. However, their poor energy conversion efficiency and low lifetime are the main bottlenecks limiting their wide application, these disadvantages mainly stem from the inherently slow kinetics of oxygen reduction (ORR) and oxygen evolution (OER) reactions, and their use in harsh bases limited stability in volatile electrolytes. To address the above problems, considerable effort has been devoted to exploring bifunctional oxygen electrocatalysts with high activity and durability. Although noble metal catalysts, such as p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88H01M4/90H01M12/06
CPCH01M4/8825H01M4/9083H01M12/06
Inventor 夏宝玉徐洋洋
Owner HUAZHONG UNIV OF SCI & TECH
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