Positive electrode active material, positive electrode containing the positive electrode active material, and lithium secondary battery
A lithium secondary battery, content technology, applied in battery electrodes, circuits, electrical components, etc., can solve problems such as residual impurities and incomplete reaction products
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Embodiment 1
[0239] Weigh FePO 4 2H 2 O (200g, from Changsha Hekang Chemical Company, battery grade, D 90 2.92μm), Li 2 CO 3 (molar ratio 2:1, from Chengdu Chemical Chemical Company, battery grade, D 90 2.84μm), Brij 35 (accounting for FePO 4 2H 2 3.5 wt% of O from Croda), and deoxygenated isopropanol (accounting for FePO 4 2H 2 50wt% of O) was added to a zirconia cylindrical container equipped with 5mm zirconia balls, wherein the weight ratio of balls / powder materials was 2:1. In a Retsch model PM100 planetary ball mill, the ball milled for 30 minutes at a speed of 400 rpm under an argon atmosphere. After grinding, the slurry was evaporated to dryness at 80 °C. Then, according to the method disclosed in US2002 / 0195591 A1, the mixture was heated to 600° C. at a heating rate of 10° C. / min in a tube furnace (Zhengzhou CY Scientific Instrument Co., Ltd.) with a dry deoxygenated nitrogen gas stream, and at this temperature Keep warm for 60min.
[0240] A carbon deposition material w...
Embodiment 2
[0254] As in Example 1, repeat the synthetic process of material-a1, different batches of FePO 4 2H 2 O (500g FePO for each synthesis 4 2H 2 O), then nano-grinding with 200 μm yttrium-stabilized zirconia balls in an alcohol base for 90 min, followed by spray-drying of the suspension.
[0255] For each batch, 300g of nanomaterials were placed in the furnace tube of a rotary kiln (Zhengzhou CY Scientific Instrument Company, model CY-R200X-100IC), and dry nitrogen was introduced into the furnace tube, and the temperature was raised to 200 °C at a heating rate of 10 °C / min. ℃, keep warm for 60min, and then continuously feed the mixed gas of vaporized benzene and argon (containing 3% benzene by volume). After heating up to 640°C at a rate of 20°C / min, the temperature was kept for 1 hour to obtain carbon-deposited LiFePO 4 . The sulfur content and carbon content in each batch were determined by the combustion analysis method with a carbon / sulfur analyzer (LECO Company), and the...
Embodiment 3
[0279] As in Example 1, with high-purity FePO 4 2H 2 O (100kg), battery-grade Li 2 CO 3 (molar ratio 1:2), Pluronic P-123 (relative to FePO 4 2H 2 O 2wt.%; Polyethylene glycol-polypropylene glycol-polyethylene glycol triblock copolymer, produced by BASF) Repeat the synthesis process of material-a1. The precursors were ground in 200 L of degassed methanol using a MasterMill model 18 basket mill (from Netzsch). After the solvent evaporated, the material (referred to as material-a3) was placed in a ceramic crucible, placed in a roller kiln blown in dry oxygen-free nitrogen, and treated at 600 °C for 60 minutes, then cooled and stored in nitrogen.
[0280] A carbon deposition material with a carbon content of 0.35wt% (measured by LECO) was obtained, and its composition was determined to contain 73.7wt% LiFePO by XRD analysis. 4 , Li3PO4 and Fe with a molar ratio of 1:1 remain 3 (PO 4 ) 2 phase, with Spectral analysis showed no Fe(III).
[0281] A 2 Kg batch of material...
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