A kind of in-situ preparation method of nano-rod composite material of α-nickel sulfide and carbon
A technology of nano-rods and composite materials, which is applied in the direction of nanotechnology, hybrid/electric double-layer capacitor manufacturing, etc., can solve the problems of large volume change and rapid capacitor capacity decay, and achieve simple preparation process, controllable shape, and easy The effect of the operation
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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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