Preparation method of electrochemical sensor based on loaded bi-metal co-doped nano composite material
A nano-composite material and co-doping technology, which is applied in the field of preparation of electrochemical sensors, can solve the problems of cumbersome process, low yield and the like, and achieve the effects of simple preparation, low cost, and increased electron transfer capability.
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Embodiment 1
[0039] Example 1 FeCo-TiO 2 / MoS 2 preparation of
[0040] (1) Add 0.6 g of molybdenum disulfide powder, 0.2 mmol of iron salt and 0.2 mmol of cobalt salt into 3 mL of n-butyllithium solution, and stir for 12 hours under nitrogen protection at 60 °C to obtain the reacted solution;
[0041] (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 cobalt;
[0042] (3) Add 500 mg of molybdenum disulfide nanomaterials co-intercalated with iron and cobalt prepared in step (2) into 5 mL of tetrabutyl titanate, stir for 1 hour, then slowly add 0.5 mL of hydrofluoric acid while stirring acid, then reacted in a reactor at 160°C for 18 hours;
[0043] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultra...
Embodiment 2
[0049] Example 2 FeCo-TiO 2 / MoS 2 preparation of
[0050] (1) Add 0.6 g of molybdenum disulfide powder, 1.0 mmol of iron salt and 1.0 mmol of cobalt salt into 5 mL of n-butyllithium solution, and stir for 24 hours under nitrogen protection at 30 °C to obtain the reacted solution;
[0051] (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 cobalt;
[0052] (3) Add 200 mg of molybdenum disulfide nanomaterials co-intercalated with iron and cobalt 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;
[0053] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultra...
Embodiment 3
[0059] Example 3 FeCo-TiO 2 / MoS 2 preparation of
[0060] (1) Add 0.6 g of molybdenum disulfide powder, 2.0 mmol of iron salt and 2.0 mmol of cobalt salt into 10 mL of n-butyllithium solution, and stir for 48 hours under nitrogen protection at 50 °C to obtain the reacted solution;
[0061] (2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 50 °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 cobalt;
[0062] (3) Add 10 mg of molybdenum disulfide nanomaterials co-intercalated with iron and cobalt prepared in step (2) into 5 mL of tetrabutyl titanate, stir for 1 hour, then slowly add 0.8 mL of hydrofluoric acid while stirring acid, then reacted in a reactor at 200°C for 24 hours;
[0063] (4) The reaction product obtained in step (3) was centrifuged and washed three times with ultra...
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