Simple MOF (Metal Organic Framework) derived Fe single-site oxygen reduction electrocatalyst as well as preparation method and application thereof
An electrocatalyst, single-site technology, applied in the direction of fuel cell-type half-cell and primary-cell-type half-cell, circuit, electrical components, etc. The effect of mass production
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Embodiment 1
[0036] Fe 10 -N-C-NH 3 The preparation comprises the following steps:
[0037] (1) ZnFe 10 - Preparation of MOF: Add 320mL of nitrobenzene and 40mL of methanol into a 500mL three-necked flask, mix well and add 500mg of 2,4,6-tris(4-pyridine)-1,3,5-triazine (tpt ), heated to dissolve completely (clear solution). 540mg ZnBr 2 and 114mg FeCl 2 Dissolve in 80mL methanol solution, add dropwise to the nitrobenzene / methanol mixed solution of 2,4,6-tris(4-pyridine)-1,3,5-triazine (tpt) while stirring until the solution turned light yellow and turbid, the obtained light yellow solid precipitate was filtered under reduced pressure and dried in vacuum at 60°C for 8 hours, and the obtained material was named ZnFe 10 -MOF;
[0038] (2) Fe 10 -N-C preparation: weigh 500mg of ZnFe 10 - MOF, add 40 mg melamine as a nitrogen source, grind the two fully and place them in a porcelain boat for argon calcination. The setting program of the tube furnace is to heat up to 150°C at 10°C / min ...
Embodiment 2
[0042] Fe 5 -N-C-NH 3 The preparation comprises the following steps:
[0043] (1) ZnFe 5 - Preparation of MOF: Add 320mL of nitrobenzene and 40mL of methanol into a 500mL three-necked flask, mix well and add 500mg of 2,4,6-tris(4-pyridine)-1,3,5-triazine (tpt ), heated to dissolve completely (clear solution). 540mg ZnBr 2 and 57mg FeCl 2 Dissolve in 80mL methanol solution, add dropwise to the nitrobenzene / methanol mixed solution of 2,4,6-tris(4-pyridine)-1,3,5-triazine (tpt) while stirring until the solution turned light yellow and turbid, the obtained light yellow solid precipitate was filtered under reduced pressure and dried in vacuum at 60°C for 8 hours, and the obtained material was named ZnFe 5 -MOF;
[0044] (2) Fe 5 -N-C preparation: weigh 500mg of ZnFe 5 - MOF, add 40 mg melamine as a nitrogen source, grind the two fully and place them in a porcelain boat for argon calcination. The setting program of the tube furnace is to heat up to 150°C at 10°C / min and ho...
Embodiment 3
[0053] The Fe prepared by embodiment 1 10 -N-C, Fe 10 -N-C-NH 3 and the application of N-C prepared in Comparative Example 1 as an oxygen reduction electrocatalyst in a zinc-air battery. The steps of electrode preparation and battery performance testing are as follows:
[0054] (1) Accurately weigh 10mg of catalyst Fe 10 -N-C Inject 1.0mL of ethanol solution containing 0.84wt.% Nafion into a 2.0mL glass vial, ultrasonically 1h to prepare a uniformly dispersed slurry, then drop 10.0μL of the slurry onto the surface of a φ5mm glassy carbon electrode, and wait for Dry naturally to modify the electrode. Fe 10 -N-C-NH 3 and N-C were prepared in the same manner as Fe10-N-C to obtain modified electrodes.
[0055] (2) The modified electrode was tested for oxygen reduction reaction under alkaline conditions on CHI 730 electrochemical workstation. The counter electrode is a Pt electrode, the reference electrode is a saturated calomel electrode, and the electrolyte is 0.1M KOH so...
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