Preparation method of lithium ferrous silicate anode composite material
A lithium ferrous silicate and composite material technology, which is applied in battery electrodes, electrical components, circuits, etc., can solve the problems of uneven particle size and easy mixing of impurities in lithium ferrous silicate positive electrode composite materials, and achieve controllable morphology , performance improvement, the effect of fine and uniform particle size
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[0025] The preparation method of the lithium ferrous silicate cathode composite material of the present invention is specifically implemented according to the following steps:
[0026] Step 1, add surfactant and tetraethyl orthosilicate to solvent 2 in sequence and stir thoroughly to prepare a mixed solution. The mass ratio of surfactant and tetraethyl orthosilicate is 0-3:1, and ethyl orthosilicate and solvent The molar ratio of 2 is 1:10-50, and then the pH of the mixed solution is adjusted to 9-13 with 20%-50% ammonia solution to obtain alkaline SiO 2 Lotion;
[0027] Step 2, the basic SiO obtained in step 1 2 The emulsion is adjusted to a pH of 2 to 7 with an organic acid, then oxalic acid is added to dissolve and mix evenly, and then a mixture of ferrous sulfate and solvent 1 with a molar ratio of 1:30 to 100 is added. The mixture of ferrous sulfate, oxalic acid and ethyl orthosilicate The molar ratio is 1:1:1, after washing, filtering and drying, ferrous oxalate-coated...
Embodiment 1
[0035] Step 1, add 4g of polyethylene glycol and 0.02mol orthosilicate to 30ml of ethanol in turn and stir for 10min to prepare a mixed solution, then adjust the pH of the mixed solution to 11 with 20% ammonia solution to obtain alkaline SiO 2 Lotion;
[0036] Step 2, the basic SiO obtained in step 1 2 Adjust the pH of the emulsion to 5 with ascorbic acid, then add 0.02mol oxalic acid and mix well, then add a mixture of 0.02mol ferrous sulfate and 25ml deionized water, centrifugally disperse, filter, wash and dry to obtain ferrous oxalate coated SiO 2 shell core material;
[0037] Step 3, coating SiO to the ferrous oxalate obtained in step 2 2 Add 0.02mol of Li to the core-shell material 2 CO 3 and 0.3g of conductive graphite, and then through vacuum ball milling to obtain the carbon-coated lithium ferrous silicate precursor, then put the carbon-coated lithium ferrous silicate precursor into a tube furnace and heat it up to 410°C under the protection of argon atmosphere A...
Embodiment 2
[0042] Step 1, add 0.02mol octadecyltrimethylammonium bromide and 0.025mol ethyl orthosilicate to the mixed solution of 20ml ethanol and 10ml deionized water successively and fully stir to prepare a mixed solution, then use 50% ammonia Adjust the pH to 13 in aqueous solution to obtain basic SiO 2 Lotion;
[0043] Step 2, the basic SiO obtained in step 1 2 Use a mixture of citric acid and oxalic acid to adjust the pH of the emulsion to 3, then add 0.025mol oxalic acid to dissolve and mix evenly, then add a mixture of 0.025mol ferrous sulfate and 35ml deionized water, centrifugally disperse, filter, wash and dry to obtain ferrous oxalate coated SiO 2 shell core material;
[0044] Step 3, add 0.04 mol of lithium acetate dihydrate, 11 g of sucrose and 3 g of glucose to the ferrous oxalate-coated SiO obtained in step 2 2 After uniform mixing in the solution of the core-shell material, the carbon-coated lithium ferrous silicate precursor is obtained by washing, filtering and dry...
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