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Preparation method of three-dimensional mesoporous NiCo2O4/nitrogen-doped graphene composite electrode material

A technology of nitrogen-doped graphene and composite electrodes, which is applied in hybrid capacitor electrodes, hybrid/electric double-layer capacitor manufacturing, nanotechnology for materials and surface science, etc., and can solve problems such as fast attenuation and small actual capacity

Inactive Publication Date: 2016-11-30
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the literature shows that the actual capacity of graphene is less than the theoretical capacity and decays faster, which requires nitrogen doping to adjust the electronic structure of graphene

Method used

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  • Preparation method of three-dimensional mesoporous NiCo2O4/nitrogen-doped graphene composite electrode material
  • Preparation method of three-dimensional mesoporous NiCo2O4/nitrogen-doped graphene composite electrode material
  • Preparation method of three-dimensional mesoporous NiCo2O4/nitrogen-doped graphene composite electrode material

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Experimental program
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Effect test

Embodiment 1

[0029] Weigh 50 mg of graphene oxide, place it in 60 mL of acetonitrile for ultrasonic dispersion for 30 min to obtain a uniform graphene oxide acetonitrile solution, transfer the solution to a hydrothermal kettle, and react at 180°C for 24 h. After the reaction was completed, it was naturally cooled to room temperature, and the obtained product was suction-filtered with a No. 6 sand core funnel, washed alternately with absolute ethanol and deionized water for five times, and then dried in a vacuum oven at 60°C for 12 hours to obtain the nitrogen-doped modified product. permanent graphene (NG). The product is analyzed by X-ray photoelectron spectroscopy (XPS), and the nitrogen exists in the form of carbon-nitrogen bond, pyridine nitrogen, and pyrrole nitrogen.

Embodiment 2

[0031] 2.9107g Co(NO 3 ) 2 ·6H 2 O(0.01mol), 1.4590g Ni(NO 3 ) 2 ·6H 2 O (0.005mol), 2.1029g of hexamethylenetetramine (0.015mol) were ultrasonically dispersed in 70ml of deionized water, and the uniformly mixed solution was transferred to a polytetrafluoroethylene hydrothermal kettle, and hydrothermally reacted at 180°C for 24h. Obtain nickel cobalt oxide precursor. After the precursor was filtered and dried, it was calcined in a tube furnace at 350 °C for 3 h under air atmosphere to obtain the product mesoporous nickel cobaltate nanomaterial NiCo 2 o 4 , mesoporous NiCo 2 o 4 It has a larger specific surface, increases the number of active sites, and is conducive to the reaction of electrolyte ions and active substances. The loose lamellar NiCo 2 o 4 It has a good skeleton support effect, provides a strong transmission channel for electrons, and is conducive to the transmission process of electrons, such as figure 2 . The nickel cobalt oxide nanomaterial prepar...

Embodiment 3

[0033] 2.9107g Co(NO 3 ) 2 ·6H 2 O(0.01mol), 1.4590g Ni(NO 3 ) 2 ·6H 2O (0.005mol), 0.1000g GO, 2.1029g hexamethylenetetramine (0.015mol) were ultrasonically dispersed in 70ml deionized water. After thermal reaction for 24h, nickel cobaltate graphene precursor was obtained. After the precursor was filtered and dried, it was calcined in a tube furnace at 350 °C for 3 h under air atmosphere to obtain the product NiCo 2 o 4 / GO, the sample has X-ray diffraction peaks at 2θ of 18.9°, 31.1°, 36.7°, 38.4°, 44.5°, 55.3°, 59.2° and 65.0°, which can be compared with NiCo 2 The standard spectra of (111), (220), (311), (222), (400), (422), (511) and (440) crystal planes of O4 crystals correspond to each other, such as figure 1 . The above-prepared NiCo 2 o 4 / GO for charge and discharge experiments with a current density of 1A g -1 , the specific capacity value reached 1800F g -1 ; After 2000 charge and discharge tests, the specific capacity remains above 87%. Figure 4 The...

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Abstract

The invention provides a preparation method of a three-dimensional mesoporous NiCo2O4 / nitrogen-doped graphene composite electrode material. The preparation method comprises the following steps: step 1, implementing ultrasonic dispersion on graphene oxide in an acetonitrile system to obtain a uniform graphene oxide solution A; step 2, transferring the solution A to a polytetrafluoroethylene hydrothermal reactor to implement constant-temperature thermal reaction, and completing the reaction to obtain mixed liquid B; step 3, implementing extraction filtration, washing and drying on the mixed liquid B to obtain a product C; step 4, implementing uniform ultrasonic dispersion on the product C, cobalt nitrate hexahydrate, nickel nitrate hexahydrate and hexamethylenetetramine to obtain mixed liquid D; step 5, transferring the mixed liquid D to the polytetrafluoroethylene hydrothermal reactor to implement constant-temperature thermal reaction, and filtering and washing the liquid to obtain a nickel cobaltate precursor E; and step 6, putting the precursor E into a tubular furnace, and implementing calcination at an air atmosphere to obtain a reaction product namely the three-dimensional mesoporous NiCo2O4 / nitrogen-doped graphene composite electrode material. The preparation method provided by the invention is mild in reaction condition, easy to control, low in cost, and simple and convenient in process and procedure.

Description

technical field [0001] The invention relates to the field of graphene materials, in particular to a three-dimensional mesoporous NiCo 2 o 4 / The preparation method of nitrogen-doped graphene composite electrode material. Background technique [0002] With its unique two-dimensional hexagonal network structure, graphene exhibits excellent properties such as large specific surface area, good electron mobility, and high stability. Therefore, it has excellent application potential as a matrix material in the field of supercapacitors. However, the literature shows that the actual capacity of graphene is smaller than the theoretical capacity and decays faster, which requires nitrogen doping to adjust the electronic structure of graphene. The introduction of N, B and other heteroatoms between graphene sheets can effectively transform graphene from a zero-band gap semi-metal into a semiconductor, forming n-type or p-type doped graphene. (Zhang C H, Fu L, etc., Adv.Mater.2011, 23...

Claims

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Application Information

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IPC IPC(8): H01G11/86H01G11/24H01G11/30H01G11/36H01G11/46B82Y30/00
CPCY02E60/13H01G11/86B82Y30/00H01G11/24H01G11/30H01G11/36H01G11/46
Inventor 章明美李远谢吉民闫早学潘登辉荆俊杰
Owner JIANGSU UNIV
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