Lithium-insertion selenium compound and preparation method and application thereof
A compound and plug-in technology, applied in the direction of selenium/tellurium compounds, elemental compounds containing selenium/tellurium, chemical instruments and methods, etc., to achieve the effect of large specific surface area, high porosity, and simple preparation method
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[0033] The invention provides a preparation method of a lithium-inserted selenium compound, comprising: mixing a selenium compound and an organolithium compound in an organic solvent, heating and reacting in a protective atmosphere to obtain a lithium-inserted selenium compound; the selenium The compounds are selenium compounds of the platinum group elements.
[0034] Wherein, the present invention has no special limitation on the sources of all raw materials, which can be commercially available or self-made.
[0035] The selenium compound is a selenium compound of a platinum group element, more preferably iridium diselenide; the particle size of the selenium compound is preferably 400-600nm; the selenium compound is preferably prepared according to the following steps: the selenium powder It is mixed with platinum group metal powder and calcined in vacuum to obtain selenium compounds. The molar ratio of the selenium powder to the platinum group metal powder is preferably 2:1...
Embodiment 1
[0046] Li-IrSe of the present invention 2 The synthesis is divided into two parts, the first step is to synthesize bulk IrSe by solid phase reaction 2 ; The second step lithium ion insertion method to synthesize Li-IrSe 2 .
[0047] 1.1 Synthesis of bulk IrSe by solid state reaction 2 , and its particle size is 400nm ~ 600nm.
[0048] Mix 192.2mg of iridium powder and 157.9mg of selenium powder evenly, add them into the mortar, and grind for 50min. Transfer the ground gray sample to a quartz tube with a length of 20 cm and an inner diameter of 2 cm, and then evacuate the quartz tube to a vacuum degree of 10 -5 torr. Under vacuum, put the quartz tube containing the sample into the muffle furnace, the reaction temperature is 1000°C, the heating rate is 5°C / min, the reaction time is 15h, and then the temperature is naturally cooled to room temperature; take out the quartz tube, shake it manually a few times, and then The reaction temperature is 1000°C, the heating rate is 5...
Embodiment 2
[0059] Example 2 Bulk IrSe 2 and Li-IrSe 2 Catalytic performance test of nanocatalyst
[0060] Adopt the block body IrSe that the embodiment of the present invention 1 makes 2 and Li-IrSe 2 Nanocatalysts were tested for catalytic performance of electrocatalytic hydrogen production, oxygen production and total hydrolysis.
[0061] The block IrSe that 5mg embodiment 1 makes 2 and Li-IrSe 2 Add the nanocatalyst to the mixed solution of 0.5mL of ethanol, 0.47mL of water and 0.03mL of perfluorosulfonic acid, sonicate for 45min, then take 4μL of the sample and drop it on the glassy carbon electrode with a diameter of 3mm. After drying, the glassy carbon electrode on as the working electrode and at 0.5M H 2 SO 4 , 1.0M PBS and 1.0M KOH solution to determine its activity as a catalyst for electrochemical splitting of water to produce hydrogen and oxygen.
[0062] Regarding the electrochemical decomposition of water to produce hydrogen, the scanning speed of linear sweep voltam...
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