Method for preparing alpha-nickel sulfide and carbon nanometer rodlike composite material in in-situ mode

A nano-rod-like, composite material technology, applied in nanotechnology, hybrid/electric double-layer capacitor manufacturing and other directions, can solve the problems of large volume change, rapid capacitor capacity decay, etc., to achieve simple preparation process, controllable morphology, product Shape controllable effect

Inactive Publication Date: 2014-12-24
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the volume of NiS changes greatly during charging and discharging, which easily leads to rapid decay of capacitor capacity.

Method used

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  • Method for preparing alpha-nickel sulfide and carbon nanometer rodlike composite material in in-situ mode
  • Method for preparing alpha-nickel sulfide and carbon nanometer rodlike composite material in in-situ mode
  • Method for preparing alpha-nickel sulfide and carbon nanometer rodlike composite material in in-situ mode

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Disperse 0.3 g of dimethylglyoxime in 30 ml of absolute ethanol, and adjust the pH value of the dimethylglyoxime solution to 13.0 with 0.5 mol / L sodium hydroxide ethanol solution. Dissolve 0.3g of nickel chloride in 800mL of water, and add the dimethylglyoxime solution dropwise into the solution of nickel chloride under ultrasonic conditions to obtain a red flocculent substance. The above-mentioned red flocculent product was suction filtered, washed, and dried, and its scanning electron microscope photo was as follows: figure 1 As shown in (a); the above powder was calcined at 500 ° C for 1 h under Ar atmosphere to obtain a black powder, that is, nanorod-shaped carbon-coated nickel, and its scanning electron micrograph is as follows figure 1 (b) shown.

Embodiment 2

[0033] 5 milligrams of nano-rod-shaped carbon-coated nickel (prepared according to the method of Example 1) was added to 50 grams of glycerol solution for ultrasonic dispersion, then 75 milligrams of thiourea was added, stirred evenly and refluxed for 1 hour, naturally cooled to room temperature, and centrifuged , After washing, the α-nickel sulfide and carbon nanorod composite is obtained, and its scanning electron microscope and XRD pictures are as follows figure 2 (a) and (b) shown.

Embodiment 3

[0035] In the absence of nano-rod-shaped carbon-coated nickel, 2.5 mg of rod-shaped carbon and 2.5 mg of nano-nickel particles were added to 50 g of glycerol solution for ultrasonic dispersion, stirred evenly, refluxed in a two-necked flask for 0.8 hours, and cooled naturally to room temperature , after centrifugation and washing, agglomerated carbon nanorods and β-nickel sulfide particles were obtained. The scanning electron microscope and XRD pictures are as follows: image 3 Shown in (a) and (b), this result proves that nano-rod-shaped carbon-coated nickel of the present invention has a good nano-confinement effect on the crystal phase of the product in the reflow vulcanization process, thereby obtaining α-nickel sulfide with a single crystal phase and Carbon nanorod composites.

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Abstract

The invention discloses a method for preparing an alpha-nickel sulfide and carbon nanometer rodlike composite material in an in-situ mode. The method is mainly characterized in that the method that nanometer rodlike carbon wraps nickel in an in-situ backflow vulcanizing mode is adopted to prepare the alpha-nickel sulfide and carbon nanometer rodlike composite material, and controllable adjusting on the nickel sulfide crystalline phase is achieved through the nanometer limited range action of a carbon nanometer rod . Compared with the existing synthetic technology, according to the alpha-nickel sulfide and carbon nanometer rodlike composite material synthesized through the method, the crystalline phase of the alpha-nickel sulfide is single, the alpha-nickel sulfide is distributed evenly in the carbon nanometer rod, the synthesis process is simple, repeatability is good, and a supercapacitor electrode made of the nanometer composite material has a large specific capacitance value and good circulation stability.

Description

technical field [0001] The invention relates to a method for in-situ preparation of alpha-nickel sulfide and carbon nano-rod composite material by using a solvothermal method. Background technique [0002] Metal sulfides such as FeS 2 ,CoS x ,MoS 2 And NiS are potential supercapacitor electrode materials due to their high theoretical capacity. NiS is rich in resources, low toxicity, and good conductivity, and has attracted extensive attention from researchers in recent years. However, the volume of NiS changes greatly during charging and discharging, which easily leads to rapid decay of capacitor capacity. At present, many studies have tried to improve its electrochemical performance through various methods, such as ball milling to reduce particle size, liquid phase synthesis or shape modification to control its particle shape. Another effective way to improve the electrical properties of metal sulfides is to form complexes with matrix materials, such as Co 9 The compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/86B82Y40/00
CPCY02E60/13
Inventor 董晓臣孙陈诚黄维
Owner NANJING UNIV OF TECH
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