Preparation method of polypyrrole-coated nickel cobaltate nanowire array graphene electrode and its application in the detection of heavy metal lead ions
A technology of nanowire arrays and graphene electrodes, which can be used in measuring devices, electrochemical variables of materials, and material analysis through electromagnetic means, and can solve problems such as easy stacking of graphene, difficulty in having excellent properties of graphene, and complicated preparation process , to achieve the effect of reducing experimental cost, excellent electrochemical detection performance, and simple operation method
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[0030] (1) Preparation of 3D graphene electrodes
[0031] Take the purchased graphene oxide powder, add it to distilled water, mix well to obtain a concentration of 1-8mg mL -1 The above-prepared graphene oxide solution was ultrasonically transferred to a hydrothermal kettle for 2-4 hours. Put it into a muffle furnace and heat at 120-180° C. for 5-12 hours to obtain reduced graphene oxide (3D graphene) with a network 3D structure, and then perform freeze-drying treatment.
[0032] (2)NiCo 2 o 4 Nanowire Arrays - Fabrication of 3D Graphene
[0033] Using the 3D graphene prepared above as a substrate, NiCo was grown on this substrate 2 o 4 Precursor nanowire array structure. Prepare nickel chloride 1-2.5mmol, cobalt nitrate 2-5mmol, ammonium fluoride 6-15mmol, urea 10-30mmol, add in distilled water and mix and stir for 5-15min to obtain a bright and uniform pink liquid. Pour the pink liquid into a hydrothermal kettle, and the 3D graphene is suspended in the pink liquid. ...
Embodiment 1
[0042] Take the purchased graphene oxide powder, add 20mL distilled water, mix well to get 20mL (8mg mL -1 ) The graphene oxide solution prepared above was transferred to a 50mL hydrothermal kettle after ultrasonication for two hours. Put it into a muffle furnace and heat it at 180° C. for 12 hours to obtain reduced graphene oxide (3D graphene) with a network 3D structure, and then perform freeze-drying treatment.
[0043] Using the 3D graphene prepared above as a substrate, NiCo was grown on this substrate 2 o 4 Precursor nanowire array structure. Weigh 0.12 g of nickel chloride, 0.24 g of cobalt nitrate, 0.2 g of ammonium fluoride, and 1.0 g of urea, add them into 40 mL of distilled water, stir for 15 min, and obtain a bright and uniform pink liquid. Pour the pink liquid into a 50mL hydrothermal kettle, and the 3D graphene is suspended in the pink liquid. At 100°C, hydrothermally reacted for 5 hours. After the reaction, the reactor was taken out to cool to room temperatu...
Embodiment 2
[0046] Take the purchased graphene oxide powder, add it to 40mL distilled water, mix well to get 40mL (1mg mL -1 ) The graphene oxide solution prepared above was transferred to a 50mL hydrothermal kettle after ultrasonication for two hours. Put it into a muffle furnace and heat it at 180° C. for 12 hours to obtain reduced graphene oxide (3D graphene) with a network 3D structure, and then perform freeze-drying treatment.
[0047] Using the 3D graphene prepared above as a substrate, NiCo was grown on this substrate 2 o 4 Precursor nanowire array structure. Weigh 0.4 g of nickel chloride, 0.8 g of cobalt nitrate, 0.4 g of ammonium fluoride, and 0.5 g of urea, add them into 40 mL of distilled water, stir for 15 min, and obtain a bright and uniform pink liquid. Pour the pink liquid into a 50mL hydrothermal kettle, and the 3D graphene is suspended in the pink liquid. At 140°C, hydrothermally reacted for 8 hours. After the reaction, the reactor was taken out to cool to room tempe...
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