A three-dimensional multi-level structure highly dispersed nickel-based electrocatalytic material and its preparation method
An electrocatalytic material and highly dispersed technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of poor conductivity, few active sites, and easy aggregation of active components, etc., to achieve Effects of preventing particle agglomeration, reducing overpotential, and excellent catalytic activity
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Embodiment 1
[0031] Pretreatment of foamed nickel: Cut commercially available nickel foam into 1cm×2cm size, immerse in 20mL of acetone, ultrasonically treat for 15min, remove surface oil, wash 3 times with water, 5min each time, wash off acetone; use 2mol / L Soak in HCl for 5 minutes to remove the oxide film on the surface of nickel foam, and then wash it with water for 3 times, each time for 2 minutes, to remove the Cl - , dried under vacuum conditions for later use.
[0032] A. Use 80mL deionized water to prepare an aluminum nitrate solution with a concentration of 0.03mol / L, transfer it to a 100mL polytetrafluoroethylene liner, immerse the pretreated foam nickel sheet vertically into the above solution, and ultrasonically treat it for 30min; then Add 0.05mol urea and 0.02mol ammonium fluoride in sequence, ultrasonically treat for 2 minutes, seal the polytetrafluoroethylene liner and put it into the autoclave, react at 180°C for 12 hours, after cooling to room temperature, wash with deio...
Embodiment 2
[0036] Commercially available nickel foam is pretreated according to Example 1.
[0037] A. Use 80mL deionized water to prepare an aluminum nitrate solution with a concentration of 0.03mol / L, transfer it to a 100mL polytetrafluoroethylene liner, and handle well Immerse the foamed nickel sheet vertically into the above solution, ultrasonic treatment for 30min; then add 0.08mol urea, 0.02mol ammonium fluoride in turn, ultrasonic treatment for 2min, seal the polytetrafluoroethylene liner and put it into the autoclave, and react at 150℃ for 12h , after cooling to room temperature, washed with deionized water and ethanol three times, and dried to obtain in-situ grown nickel-based hydrotalcite NiAl-LDH / NF.
[0038] B. Place the obtained NiAl-LDH / NF in a three-necked flask of 150mL deionized water; prepare H with a concentration of 0.5mol / L 3 BO 3 solution, and added dropwise into a three-necked flask until the pH of the solution reached 4.5, and then reacted at 90° C. for 12 hour...
Embodiment 3
[0041] Commercially available nickel foam is pretreated according to Example 1.
[0042] A. Use 80mL deionized water to prepare an aluminum nitrate solution with a concentration of 0.03mol / L, transfer it to a 100mL polytetrafluoroethylene liner, immerse the pretreated foam nickel sheet vertically into the above solution, and ultrasonically treat it for 30min; then Add 0.08mol urea and 0.025mol ammonium fluoride in sequence, ultrasonically treat for 2min, seal the polytetrafluoroethylene liner and put it into the autoclave, react at 120°C for 12h, after cooling to room temperature, wash with deionized water and ethanol respectively 3 times, drying to obtain in-situ growth of nickel-based hydrotalcite NiAl-LDH / NF.
[0043] B. Place the obtained NiAl-LDH / NF in a three-necked flask of 150mL deionized water; prepare NaH with a concentration of 0.8mol / L 2 PO 4 solution, and added dropwise into a three-necked flask until the pH of the solution reached 3.5, and then reacted at 90° C...
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