Method for preparing nitrogen-carbon doped metal oxide and nitrogen-carbon doped metal oxide
An oxide and metal technology, applied in the field of nitrogen-carbon doped metal oxides, can solve the problems of poor conductivity, large irreversible capacity, and large volume change, and achieve excellent lithium storage performance, increase application value, and small volume change.
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[0025] An embodiment of the present invention provides a method for preparing a nitrogen-carbon-doped metal oxide, which includes: mixing polyaniline and N-methylpyrrolidone, and adding MIL-101(Fe) to prepare PAN@MIL-101(Fe ); Calcination of PAN@MIL-101(Fe).
[0026] In the preparation method provided in this example, polyaniline is introduced into MIL-101(Fe) as a nitrogen source, so that the nitrogen source can be doped in the pores of MIL-101(Fe).
[0027] In detail, the ratio of polyaniline and N-methylpyrrolidone is 1:10-15, the above-mentioned one part of polyaniline can be 1g, 1.5g, 1mg, etc., one part of N-methylpyrrolidone can be 1mL, 1.5mL Etc., for example: 1.5g polyaniline is dissolved in 20mL N-methylpyrrolidone, 10g polyaniline is dissolved in 150mL N-methylpyrrolidone, etc.
[0028] Further, by mixing the activated MIL-101(Fe) with polyaniline and N-methylpyrrolidone, the method for activating MIL-101(Fe) includes: soaking MIL-101(Fe) with ethanol, acetone, etc...
Embodiment 1
[0045] 2mmol (800mg) ferric nitrate nonahydrate [Fe(NO 3 ) 3 9H 2 O], 2mmol (328mg) terephthalic acid (H 2 BDC), 10ml of water and 0.2ml of hydrofluoric acid were added to a 23ml polytetrafluoroethylene bottle, and filtered to obtain a green powder; the green powder obtained by filtration was dispersed into 40mLN, N-dimethylformamide (DMF), in Reflux at 130°C for 7 hours, and filter while hot; disperse the green powder obtained by washing with DMF in 40 mL of methanol solution, reflux at 85°C for one night, filter and dry, and finally obtain a green powder, which is MIL-101(Fe).
[0046] Dissolve 1.5g of polyaniline in 20mL of N-methylpyrrolidone (NMP), then disperse 0.3g of activated MIL-101(Fe) in the solution, and stir overnight to allow polyaniline to fully disperse in MIL-101( Fe) obtained PAN@MIL-101(Fe).
[0047] The obtained PAN@MIL-101(Fe) precursor was placed in a tube furnace, calcined at 600 °C for 2 hours in an argon atmosphere, and cooled naturally to room te...
Embodiment 2
[0049] 2mmol ferric nitrate nonahydrate [Fe(NO 3 ) 3 9H 2 O], 1mmol terephthalic acid (H 2 BDC), 11ml of water and 0.2ml of hydrofluoric acid were mixed, filtered to obtain a green powder; the filtered green powder was dispersed in 44mL of N,N-dimethylformamide (DMF), refluxed at 140°C for 8h, while hot Filtration; the green powder obtained by washing with DMF was dispersed in 44 mL of methanol solution, refluxed at 95° C. for 8 h, filtered and dried to obtain a green powder, that is, MIL-101(Fe).
[0050] Dissolve 2.1g of polyaniline in 22.5mL of N-methylpyrrolidone (NMP), then disperse 0.3g of activated MIL-101(Fe) in the solution, and stir for 12 hours to allow the polyaniline to fully disperse in the MIL-101 (Fe) to obtain PAN@MIL-101(Fe).
[0051] The obtained PAN@MIL-101(Fe) precursor was placed in a tube furnace, calcined at 700 °C for 2 hours in an argon atmosphere, and cooled naturally to room temperature to obtain Fe nanoparticles 2 o 3 / N-C composite material,...
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