Ligand-protected Pt6 sub-nanocluster and preparation method thereof, and catalyst and preparation method and application thereof
A sub-nano, catalyst technology, applied in the field of electrochemistry, can solve problems such as reducing catalyst activity and affecting catalyst stability
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[0030] The invention provides a ligand-protected Pt 6The preparation method of the sub-nanometer cluster comprises the following steps: a ligand solution, chloroplatinic acid, a reducing agent and an alcohol are mixed for a reduction reaction to obtain a reduction product solution, and the reduction product is a ligand-protected Pt 6 sub-nanometer clusters; the ligand is a phosphine compound, the solvent of the ligand solution is a weak polar solvent, the polarity value of the weak polar solvent is 1-5, and the reducing agent is an amine complex things.
[0031] In the present invention, the phosphine compound is preferably one or more of triphenylphosphine, tributylphosphine, diphenylphosphine and dimethylphenylphosphine, more preferably triphenylphosphine; The amine complexes are preferably one or more of borane tert-butylamine complexes, boron trifluoride-monoethylamine complexes, borane-trimethylamine complexes and triethylborane amine complexes several, more preferably ...
Embodiment 1
[0051] (1) Thoroughly mix 200 μL of 20 mmol / L triphenylphosphine in toluene, 200 μL of 20 mmol / L chloroplatinic acid aqueous solution and 5 mL of ethanol.
[0052] (2) Vigorously stir the mixed solution obtained in step (1) and add 30 μL of 50 mmol / L ethanol solution of borane tert-butylamine complex, and react for 30 minutes until dark brown ligand-protected Pt 6 Subnano cluster solution.
[0053] figure 1 Protection of Pt for the resulting ligand 6 UV absorption spectrum (a) and ESI-MS spectrum (b) of subnano clusters; in figure 1 In the UV absorption spectrum in , Pt appeared at 385 and 355nm 6 The characteristic absorption peak of the sub-nanometer cluster, the peak at m / z=2400Da in the ESI-MS spectrum, the combined UV absorption spectrum and ESI-MS spectrum, and the calculation based on the molecular weight of the intermediate product, this example successfully synthesized a stable Existing Pt 6 subnanometer clusters.
Embodiment 2
[0055] (1) Get the ligand protection Pt prepared in 5mL embodiment 1 6 The subnano-cluster solution was mixed with 10, 20, and 40 mg of carbon black, respectively, and then 45 mL of ethanol was added, and mixed and stirred for 6 hours to obtain carbon-supported Pt with a loading of 8%, 4%, and 2%, respectively. 6 Subnano cluster solution.
[0056] (2) The solution obtained in step (1) is separated by suction filtration, and then vacuum-dried overnight at room temperature to obtain carbon-supported Pt 6 Subnanometer Cluster Catalysts.
[0057] figure 2 Pt on carbon with a loading of 2% 6 Electron microscope images of sub-nano cluster catalysts, where (a) is spherical aberration electron microscope images, (b) is TEM images, (c) and (d) are HAADF-STEM images of different parts; according to figure 2 It can be seen that Pt 6 Subnanometer clusters are evenly dispersed on the surface of carbon black.
[0058] Hydrogen electrocatalytic oxidation performance test: Take 2.5 mg...
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