Alkali/Transition Metal Halo-And Hydroxy-Phosphates And Related Electrode Active Materials
a technology of transition metal and active materials, applied in the field of alkali/transition metal haloand hydroxyphosphates and related electrode active materials, can solve the problems of insufficient voltage, insufficient charge capacity, and many cathode materials known in the art without one or more of these characteristics, etc., to achieve enhanced cycling capability, enhanced reversibility, and enhanced capacity
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example 1
[0157] An electrode active material comprising Li2NiPO4F, representative of the formula Li1+xNiPO4Fx, is made as follows. First, a LiNiPO4 precursor is made according to the following reaction scheme.
0.5 Li2CO3+0.334 Ni3(PO4)2.7H2O+0.334 (NH4)2HPO4→
LiNiPO4+2.833H2O+0.667 NH3+0.5 CO2
[0158] A mixture of 36.95 g (0.5 mot) of Li2CO3, 164.01 (0.334 mol) of Ni3(PO4)2.7H2O, and 44.11 g (0.334 mol) of (NH4)2HPO4 is made, using a mortar and pestle. The mixture is pelletized, and transferred to a box oven equipped with a atmospheric air gas flow. The mixture is heated, at a ramp rate of about 2° C. minute to an ultimate temperature of about 800° C., and maintained at this temperature for 16 hours. The product is then cooled to ambient temperature (about 21° C.).
[0159] Li1+xNiPO4Fx is then made from the LiNiPO4 precursor. In the Example that follows, x is 1.0, so that the active material produced is represented by the formula Li2NiPO4F. The material is made according to the following reacti...
example 2
[0162] An electrode active material comprising Li1+xCoPO4Fx is made as follows. First, a LiCoPO4 precursor is made according to the following reaction scheme.
0.334 Li3PO4+0.334 CO3(PO4)2.8H2O→LiCoPO4+2.833H2O
A mixture of 38.6 g (0.334 mol) of Li3PO4 and 170.29 g (0.334 mol) of CO3(PO4)2.8H2O is made, using a mortar and pestle. The mixture is pelletized, and transferred to a box oven equipped with a atmosphere air gas flow. The mixture is heated at a ramp rate of about 2° / minute to an ultimate temperature of about 800° C., and maintained at this temperature for about 8 hours. The product is then cooled to about 25° C.
[0163] Li1+xCoPO4Fx is then made from the LiCoPO4 precursor according to the following reaction scheme.
LiCoPO4+xLiF→Li1+xCoPO4Fx
[0164] Illustrative for x equals 1.0, a mixture of 160.85 g (1.0 mol) of LiCoPO4 and 25.94 g (1.0 mol) of LiF is made using a mortar and pestle. The mixture is then pelletized, and transferred to a temperature-controlled tube furnace equip...
example 3
[0165] An electrode active material comprising Li1+xFePO4Fx is made as follows. First, a LiFePO4 precursor is made according to the following reaction scheme.
LiH2PO4+0.5 Fe2O3+0.5C→LiFePO4+0.5 CO+1.0H2O
[0166] A mixture of 103.93 (1.0 mol) of LiH2PO4, 79.86 g (0.5 mol) of Fe2O3, and 12.0 g (1.0 mol) of carbon (a 100% weight excess) is made, using a mortar and pestle. The mixture is pelletized, and transferred to a temperature-controlled tube furnace equipped with a argon gas flow. The mixture is heated at a ramp rate of about 2° C. / minute to an ultimate temperature of about 750° C. in the inert atmosphere, and maintained at this temperature for about 8 hours. The product is then cooled to ambient temperature (about 20° C.).
[0167] The Li1+xFePO4Fx is then from the LiFePO4 precursor according to the following reaction scheme.
LiFePO4+xLiF→Li1-xFePO4Fx
For the case where x=1.0, a mixture of 157.76 g (1.0 mol) of LiFePO4 and 25.94 g (1.0 mol) of LiF is made using a mortar and pestle....
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