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Synthesis of NiCo2S4 nanotube arrays on Ni foam

First of all, the Ni foam (1 cm × 1 cm × 1.6 mm) was pretreated with 5%


HCl, ethanol and deionized (DI) water to remove impurities and oxides
from the surface and dried in the oven. NiCo2S4 nanotube arrays were
obtained through a two-step hydrothermal reaction. First, 2 mmol
NiCl2·6H2O, 4 mmol CoCl2·6H2O and 12 mmol urea were dissolved in 35 ml
DI water with stirring continuously. Then the solution was transferred into
a 50 ml Teflon-lined stainless autoclave with 8 pieces of bare Ni foams in it.
The autoclave was kept at 120 °C for 6 h in the oven and cooled down to
room temperature. The products were collected by washing with DI water
and ethanol, then dried in the oven at 60 °C for 12 h as precursors. Second,
the precursors were placed in a 50 ml Teflon-lined stainless autoclave with
35 ml sodium sulfide solution (0.2 M) and kept at 120 °C for 14 h. Finally,
the products were collected by washing with DI water and ethanol, and
then dried at 60 °C for 12 h to obtain NiCo2S4 nanotubes. The mass loading
of NiCo2S4 was 7.5 mg, corresponding with the gain weight of Ni foam.
Source: NiCo2S4@Co(OH)2 core-shell nanotube arrays in situ grown on Ni
foam for high performances asymmetric supercapacitors
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panelRuiLi1SenlinWang1ZongchuanHuangFengxiaLuTaobinHe

2.1.1. Synthesis of Mn-Co precursor


At first, an 80 ml solution of water and ethanol (in 1:1 volume ratio) was prepared and
then 1.0 mmol of manganese nitrate hexahydrate and 2.0 mmol of cobalt nitrate
hexahydrate were dissolved in it with continuous stirring on a hot plate for 30 minutes.
Then, 10.0 mmol of urea was added into the above solution with continued stirring for
another 30 minutes whereby a clear solution was obtained. Separately, Ni foam
substrates (1.5 cm × 1.5 cm) were cleaned in 5% HCl solution to remove any surface
oxide layer and washed with deionized water. Then the cleaned nickel substrates were
dipped in the reaction solution and transferred to a Teflon-lined autoclave and kept at
140 °C for 6 h. After that the nickel foam was taken out from the autoclave, cleaned
several times with deionized water and isopropyl alcohol and dried in a vacuum oven at
110 °C for 6 h.
Carbon Doped MnCo2S4 Microcubes Grown on Ni foam as High Energy Density Faradaic
Electrode
Author links open overlay
panelAtinPramanikabSandipanMaitiaMonjoySreemanycSourindraMahan
Preparation of FG-Ni foam

Graphite oxide was prepared by a modified Hummers method. In a typical


preparation procedure, 92 mL of concentrated H2SO4 solution was added into
a 1000 mL three-neck flask which was placed in a low temperature thermostat
bath of 3 °C. Then a mixture of graphite power (4 g) and NaNO3 (2 g) was
added into the solution under continuous stirring. Potassium permanganate
(12 g) was then slowly added into the above solution and kept in cooling
condition for 2 h. Afterwards, the temperature of the thermostat bath was
raised from 3 °C to 35 °C, and the dark green mixed solution was stirred for
another 2 h. Distilled water (184 mL) was gradually added into the dark brown
solution, and the mixture was heated to 75 °C. After stirring for 10 min, a
suitable amount of 5% H2O2 was slowly added into the mixture to remove the
unreacted potassium permanganate. The color of the mixed solution turned
from dark brown into brilliant yellow. The reaction equation can be expressed
as follows:
(1)5KMnO4 + 5H2O2 + 3H2SO4 = 2MnSO4 + K2SO4 + 5O2↑ + 8H2O
The mixture was filtered and washed using 10% HCl until the sulfate ions
could not be detected by BaCl2. The graphite oxide in the state of colloid was
kept at room temperature.
After pickling and alkaline cleaning, the Ni foam was soaked into the GO
colloid for 0.5 h, and excess GO was scraped off the Ni foam with a copper
slice. The GO-coated Ni foam was then put into a drying oven and dried at
30 °C for 2 h. By microwave irradiation of the dried GO-coated Ni foam in a
microwave oven at 1000 W for 2 min in ambient condition, a silver black FG-
Ni foam sample was obtained.

The schematic procedure for the preparation of FG-Ni foam is shown in Fig. 1.
For comparison, the functional graphene (FG) was also prepared by reducing
GO under the same condition.
Source Microwave-assisted synthesis of functionalized graphene on Ni
foam as electrodes for supercapacitor application
Author links open overlay
panelZidongHuangHaiyanZhangYimingChenWenguangWangYutingChenYaobinZhong

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