A kind of transition metal chalcogenide material and preparation method thereof
A technology of transition metal chalcogenides and compounds, applied in cobalt compounds, chemical instruments and methods, nanotechnology for materials and surface science, etc., can solve problems such as difficulties in monitoring and mass production, and difficult dimensions
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[0049] The present invention provides a method for preparing a transition metal chalcogenide material, which comprises the following steps:
[0050] (1) Mixing the cobalt-iron inorganic salt solution, the inorganic alkali solution and the sodium nitrate solution to react to obtain the cobalt-iron hydrotalcite nanosheets;
[0051] The solute in the cobalt-iron inorganic salt solution is an inorganic cobalt salt and an inorganic iron salt;
[0052] The solvent of the sodium nitrate solution is formamide and water;
[0053] (2) Under an inert atmosphere, reduce sodium borohydride and selenium powder in water to obtain a reduction reaction solution;
[0054] Under an inert atmosphere, mixing the reduction reaction liquid and absolute ethanol to obtain a reduction treatment liquid;
[0055] (3) Under an inert atmosphere, mixing the hydrosol of the cobalt-iron hydrotalcite nanosheets and the reduction treatment solution to perform a primary selenization reaction to obtain a selenization reacti...
Embodiment 1
[0076] Solution A: Co(NO 3 ) 2 ·6H 2 O, Fe(NO 3 ) 3 ·9H 2 O is dissolved in 60 mL of deionized water, mixed well, and used as an inorganic salt solution for later use. Co(NO 3 ) 2 ·6H 2 O and Fe(NO 3 ) 3 ·9H 2 The ratio of the amount of O substance is 2:1, of which Fe(NO 3 ) 3 ·9H 2 O is 0.6mmol;
[0077] Solution B: Dissolve NaOH in 54mL deionized water as an alkaline solution for later use, NaOH is 13.5mmol;
[0078] Solution C: NaNO 3 Dissolved in deionized water containing 25% (volume ratio) of formamide for later use, in which NaNO 3 0.6mmol; Among them, 15mL formamide, 45mL deionized water;
[0079] Solution A and solution B were added dropwise to solution C at the same time at a uniform rate, and the overall pH condition was controlled to 9-10. The dropwise addition was carried out while stirring under 80°C oil bath conditions. The titration was completed within 30 minutes. After the reaction, the obtained hydrotalcite colloid was taken out by centrifugal separation, and the ...
Embodiment 2
[0085] Solution A: Co(NO 3 ) 2 ·6H 2 O, Fe(NO 3 ) 3 ·9H 2 O is dissolved in 60 mL of deionized water, mixed well, and used as an inorganic salt solution for later use. Co(NO 3 ) 2 ·6H 2 O and Fe(NO 3 ) 3 ·9H 2 The ratio of the amount of O substance is 3:1, where Fe(NO 3 ) 3 ·9H 2 O is 0.6mmol;
[0086] Solution B: Dissolve NaOH in 54mL deionized water as an alkaline solution for later use, NaOH is 13.5mmol;
[0087] Solution C: NaNO 3 Dissolved in deionized water containing 25% (volume ratio) of formamide for later use, in which NaNO 3 0.6mmol; Among them, 15mL formamide, 45mL deionized water;
[0088] Solution A and solution B were added dropwise to solution C at the same time at a uniform rate, and the overall pH condition was controlled to 9-10. The dropwise addition was carried out while stirring under 80°C oil bath conditions. The titration was completed within 30 minutes. After the reaction, the obtained hydrotalcite colloid was taken out by centrifugal separation, and the col...
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