A kind of preparation method of bimetallic co-doped two-dimensional nano-electrode material
A two-dimensional nanometer and electrode material technology, applied in circuits, photovoltaic power generation, electrical components, etc., can solve the problems of cumbersome process and low yield, and achieve the effects of no precious metal doping, low cost and time saving
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Embodiment 1
[0023] Example 1 FeMn-TiO 2 / MoS 2 preparation of
[0024] (1) Add 0.6 g of molybdenum disulfide powder, 0.2 mmol of iron salt and 0.2 mmol of manganese salt into 3 mL of n-butyllithium solution, and stir for 12 hours under nitrogen protection at 60 °C to obtain the reacted solution;
[0025] (2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 60 °C. After the treatment, wash the treated solution with a non-polar solvent, and dry it in vacuum to obtain iron , Molybdenum disulfide nanomaterials co-intercalated with manganese;
[0026] (3) Add 500 mg of molybdenum disulfide nanomaterials co-intercalated with iron and manganese prepared in step (2) into 5 mL of tetrabutyl titanate, and after stirring for 1 hour, slowly add 0.5 mL of hydrofluoric acid while stirring acid, then reacted in a reactor at 160°C for 18 hours;
[0027] (4) The reaction product obtained in step (3) was centrifuged and washed thre...
Embodiment 2
[0033] Example 2 FeMn-TiO 2 / MoS 2 preparation of
[0034] (1) Add 0.6 g of molybdenum disulfide powder, 1.0 mmol of iron salt and 1.0 mmol of manganese salt into 5 mL of n-butyllithium solution, and stir for 24 hours under nitrogen protection at 30 °C to obtain the reacted solution;
[0035](2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 30 °C. After the treatment, wash the treated solution with a non-polar solvent, and dry it in vacuum to obtain iron , Molybdenum disulfide nanomaterials co-intercalated with manganese;
[0036] (3) Add 200 mg of molybdenum disulfide nanomaterials co-intercalated with iron and manganese prepared in step (2) into 5 mL of tetrabutyl titanate, stir for 1 hour, then slowly add 0.6 mL of hydrofluoric acid while stirring acid, then reacted in a reactor at 180°C for 20 hours;
[0037] (4) The reaction product obtained in step (3) was centrifuged and washed three times wi...
Embodiment 3
[0043] Example 3 FeMn-TiO 2 / MoS 2 Photoelectrochemical test of
[0044] The FeMn-TiO prepared in Example 1 2 / MoS 2 dissolved in water to obtain FeMn-TiO at a concentration of 5 mg / mL 2 / MoS 2 Sol, take 0.02 mL FeMn-TiO 2 / MoS 2 The sol is modified on the ITO electrode, the saturated calomel electrode is used as the reference electrode, and the platinum wire electrode is used as the auxiliary electrode to form a three-electrode system, which is connected to the photoelectrochemical detection equipment; 15mL Tris with pH=5.4 is added to the electrolytic cell successively. -HCl buffer solution and 5 mL of 10 mmol / L L-ascorbic acid-2-phosphate trisodium salt AAP solution; using i-t test means, test the resulting photocurrent intensity, which can reach 0.2 mA, indicating that the prepared FeMn-TiO 2 / MoS 2 It has practical application value.
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