Method for preparing porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material
A porous spherical, physical method technology, applied in the direction of electrical components, battery electrodes, nanotechnology, etc., can solve the problems of uneven particle size distribution, slow lithium ion diffusion rate, low electronic conductivity, etc., to achieve good electrical conductivity and material Excellent processing performance and uniform particle size distribution
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Embodiment 1
[0040] Physical method: Weigh 10kg iron phosphate (molecular formula: FePO 4 2H 2 O), in nitrogen (molecular formula: N 2 ) atmosphere, bake at 400°C for 3h to form a dry powder. Get this powder 5Kg, lithium carbonate (molecular formula: Li 2 CO 3 ) 0.9886Kg, dopant magnesium hydroxide (molecular formula: Mg(OH) 2 ) 16g, dopant aluminum oxide 13.5g, add dispersant isopropanol (molecular formula: C 3 h 8 O) 13.9734Kg, forming a slurry. Pore-forming agent citric acid (molecular formula: C 6 h 8 O) 0.0844Kg, stabilizer sodium polystyrene sulfonate (molecular formula: [C 8 h 7 SO 3 Na] n ) 0.0844Kg, coating agent single-wall carbon nanotube 0.0844Kg, add 1Kg isopropanol (molecular formula: C 3 h 8 O), ultrasonically dispersed for 10min, and then poured into the slurry. The above slurry is milled with a stirring ball mill at 400 rad / min for 4 hours, and then sand-milled with a horizontal sand mill at 3800 rad / min for 3.5 hours to form a slurry with primary particles ...
Embodiment 2
[0042] Hydrothermal synthesis method: according to lithium: iron: phosphorus molar ratio is 2: 0.98: 1, weighs 3.97Kg ferrous chloride (molecular formula: FeCl 2 4H 2 0), 0.838Kg lithium hydroxide (molecular formula: LiOH·H 2 O), 1.957Kg phosphoric acid (molecular formula: H 3 PO 4 ), 36g dopant vanadium pentoxide (molecular formula: V 2 o 5 ), add 10.367Kg deoxygenated deionized water (molecular formula: H 2 (0), pH value is 8.67, forms slurry, moves in the autoclave. Coating agent carbon black 0.135Kg, stabilizer cetyltrimethylammonium bromide (molecular formula: C 16 h 33 (CH 3 ) 3 NBr) 0.135Kg, pore forming agent polyvinyl butyral (molecular formula: C 16 h 28 o 5 ) 0.135Kg, put into 8Kg deoxygenated deionized water, ultrasonically disperse for 10min, and put into the slurry. The above high-pressure reaction kettle is a sealed kettle body, nitrogen (molecular formula: N 2 ) protection, the feeding temperature is 80°C, and the stirring speed is 160rad / min. Th...
Embodiment 3
[0045] Co-precipitation method: according to the Li:Fe:P ratio of 2:1:1, ferrous sulfate with a concentration of 110mol / L (molecular formula: FeSO 4 ·7H 2 O), the concentration is 110mol / L ammonium dihydrogen phosphate (molecular formula: NH 4 h 2 PO 4 ) solution and a concentration of 220mol lithium hydroxide (molecular formula: LiOH·H 2 O), the configuration concentration is the NH of 210mol / L 3 ·H 2 O. The mixed solution is added to a certain volume of deoxygenated deionized water (molecular formula: H 2 O) in the reactor, use NH 3 ·H 2 The value of the O adjustment system is 7.0, the temperature of the reaction system is 45° C., and the stirring speed is 120 r / min. A precipitation reaction occurs until the end of the reaction. Nitrogen (N 2 )Protect. Precipitated powder, deoxidized deionized water (molecular formula: H 2 O) Washing to form a slurry. Dopant TiO 2 0.1wt%, pore forming agent polyvinylpyrrolidone (molecular formula: [C 6 h 9 NO] n ) 3wt%, stabi...
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