Preparation method for lithium ferrous phosphate anode material coated by directly reduced nanocarbon
A technology of lithium iron phosphate and positive electrode materials, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of difficult control of nanotube growth efficiency, uneven distribution of carbon nanotubes, unstable electrochemical performance, etc. , to achieve the effects of increased discharge voltage platform, simple preparation process, and good cycle performance
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Embodiment 1
[0026] 1) Preparation of carbon nanotubes by direct reduction
[0027] According to Na 2 SO 3 Weigh Na with a weight ratio of 1:1 to carbon nanotubes 2 SO 3 ; 2 SO 3 Mix with distilled water 200 times its volume to make Na 2 SO 3 solution, adding carbon nanotubes to Na 2 SO 3 In the solution, heat treatment at 30° C. for 1 h in an ultrasonic oscillator; after suction filtration and washing, dry at room temperature for 3 h under a pressure of 10 Pa to prepare direct reduced carbon nanotubes.
[0028] 2) Weigh lithium dihydrogen phosphate and ferrous oxalate according to the molar ratio of lithium ion: ferrous ion: phosphate ion: 0.95: 0.90: 0.95; weigh 3.62% of the theoretical output of lithium ferrous phosphate based on the weight of the reaction compound direct reduction of carbon nanotubes. Measure distilled water according to 0.8 times the volume of the total volume of lithium dihydrogen phosphate and ferrous oxalate.
[0029] Mix the weighed lithium dihydrogen p...
Embodiment 2
[0031] 1) Preparation of direct reduction graphene
[0032] Weigh sodium borohydride at 1: 1000 according to the weight ratio of sodium borohydride and graphene; Sodium borohydride is mixed with deionized water of 200 times its volume to prepare sodium borohydride solution, and graphene is added to sodium borohydride solution heat treatment at 90°C for 1 h in an ultrasonic oscillator; after suction filtration and washing, dry at room temperature for 3 h at a pressure of 10132 Pa to obtain directly reduced graphene.
[0033] 2) Weigh the reaction compounds lithium dihydrogen phosphate and ferrous oxalate according to the molar ratio of lithium ion: ferrous ion: phosphate ion 1.10: 1.05: 1.10. 14.5% by weight of the theoretical yield of lithium iron phosphate calculated on the basis of the weight of the reaction compound weighs directly reduced graphene. Measure ethanol according to 20 times the total volume of lithium dihydrogen phosphate and ferrous oxalate.
[0034] Mix wei...
Embodiment 3
[0036] 1) Preparation of graphene oxide by direct reduction
[0037] Weigh hydrazine hydrate at 1:100 according to the weight ratio of hydrazine hydrate and graphene oxide; hydrazine hydrate is mixed with distilled water 200 times its volume to obtain a hydrazine hydrate solution, and graphene oxide is added to the hydrazine hydrate solution. Heat treatment at 50°C for 1 h in a shaker; filter and wash with suction and dry at room temperature at 100 Pa for 3 h to prepare directly reduced graphene oxide.
[0038] 2) according to lithium ion: ferrous ion: the molar ratio of phosphate ion is 1.00: 1.00: 1.00 weighing reaction compound lithium acetate, ferrous oxalate, phosphoric acid; 8.1% of the theoretical yield of ferrous phosphate based on the weight of reaction compound calculation % wt. direct reduced graphene oxide. Measure formaldehyde based on 10 times the total volume of lithium acetate, ferrous oxalate, and phosphoric acid.
[0039] Mix the weighed lithium acetate, fe...
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