Method for preparing graphene / carbon nanotube composite material
A technology of composite materials and carbon nanotubes, applied in the direction of carbon nanotubes, multi-walled carbon nanotubes, nanocarbons, etc., can solve the problems of complex preparation process, harsh experimental conditions, high experimental cost, etc., achieve simple process, improve composite uniformity Sexuality and parameter controllable effect
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[0031] Example 1:
[0032] Add 3g graphite powder and 2g sodium nitrate into the beaker, slowly add 70mL of concentrated sulfuric acid along the cup and keep stirring; under ice bath conditions, add 30g potassium permanganate solid powder into the beaker evenly in five times and continue stirring 1h. Continue to stir for 2h in a 35°C water bath to obtain a mixed solution. Slowly add 140mL of deionized water to the solution and keep stirring for 15min, then the temperature of the system rises to about 95℃, continue to stir for 3h; add 30% H 2 O 2 Until the solution turns bright yellow. The reaction solution is filtered while hot, and washed with dilute hydrochloric acid to remove excess metal ions. The graphene oxide was prepared by centrifugation and washing to pH 7, freeze-drying for 48 hours, vacuum degree 8-pa, temperature: -10℃, and its crystal plane structure was confirmed by X-ray diffractometer. figure 1 . XRD results show that raw graphite has a peak at 2θ=26.6°, while...
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[0036] Example 2:
[0037] The preparation method of graphene / carbon nanotube composite material, the operation steps are as follows: (1) Natural graphite powder is oxidized to prepare graphene oxide; (2) Graphene oxide, nickel nitrate hexahydrate, and hexamethylenetetramine are subjected to ultrasound Hydrothermal reaction to prepare graphene / carbon nanotube composite materials.
[0038] Step (1) The operation steps are the same as in Example 1.
[0039] Step (2) The operation steps are as follows: take graphene oxide and deionized water into a beaker to ultrasonically disperse for 1 hour, then add Ni(NO3)2·6H2O and hexamethylenetetramine (HMTA) and stir well; the solution is transferred to A constant temperature reaction in a 100mL reactor; after the reaction, an excess of 1 mol / L hydrochloric acid was added to dissolve nickel hydroxide, and the black solid was collected after suction filtration, washed and vacuum dried to obtain a graphene / carbon nanotube composite material.
[00...
Example Embodiment
[0047] Example 3:
[0048] The preparation method of graphene / carbon nanotube composite material is characterized in that the operation steps are as follows: (1) Natural graphite powder is subjected to oxidation reaction to prepare graphene oxide; (2) Graphene oxide is combined with nickel nitrate hexahydrate, hexamethylene tetramine The amine undergoes ultrasonic hydrothermal reaction to prepare graphene / carbon nanotube composite material.
[0049] Step (1) The operation steps are the same as in Example 1. The different process parameters are: the freeze-drying time is 50h, the temperature is -40°C, and the vacuum degree is 10 Pa.
[0050] The operation steps of the step (2) are as follows: take graphene oxide and deionized water into a beaker for ultrasonic dispersion for 1.5 hours, then add Ni(NO3)2·6H2O and hexamethylenetetramine (HMTA) and stir well; The solution was transferred to a 100mL reactor for constant temperature reaction; after the reaction was completed, an excess c...
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