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Preparation of multi-position doped lithium iron phosphate positive electrode material and application thereof

A technology of lithium iron phosphate and cathode materials, which is applied in the field of preparation of electrochemical power supply materials, can solve the problems of limited doping effect, and achieve the effects of uniform composition, wide application prospects, and wide selection of materials

Active Publication Date: 2009-01-07
甘肃大象能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the existing results, the method of adding conductive materials can greatly improve the cycle capacity of lithium iron phosphate cathode materials, especially the rate capacity performance, while the effect of doping lithium and iron sites alone is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 0.0495 moles of high-purity lithium carbonate Li 2 CO 3 , 0.0005 mole lanthanum oxalate nonahydrate La 2 (C 2 o 4 ) 3 9H 2 O, 0.099 moles of ferrous oxalate Fe(C 2 o 4 )·2H 2 O, 0.001 mole cobalt oxalate tetrahydrate Co(C 2 o 4 )·4H 2 O, 0.098 mole ammonium dihydrogen phosphate NH 4 h 2 PO 4 and 0.002 mole boric acid H 3 BO 3 Mix, add to a nylon tank, add 25ml of absolute alcohol, seal and mix for 6 hours on a planetary ball mill with zirconia as the ball milling medium, then dry at 60°C, sieve, and under a nitrogen atmosphere of 0.3 liters per minute, use The heating rate is 5°C / min to 400°C, keep at this temperature for 8 hours, cool down to room temperature with the furnace, take out the pre-fired material and add 0.4 mole thiourea to the nylon tank, add an appropriate amount of absolute alcohol, seal and ball mill for 10 hours , dried at 70°C, sieved, and then raised to 700°C at a rate of 4°C / min under a nitrogen atmosphere of 0.3 liters / min, kept fo...

Embodiment 2

[0051] 0.1 molar battery-grade lithium acetate CH 3 COOLi, 0.098 mole ferrous chloride FeCl 2 , 0.001 mole cerium oxalate Ce nonahydrate 2 (C 2 o 4 ) 3 9H 2 O, 0.09 moles of diammonium hydrogen phosphate and 0.01 moles of tungstic acid H 2 WO 4 Mix, add to a nylon tank, add 75ml of absolute alcohol, seal and mix for 5 hours on a planetary ball mill with alumina balls as the grinding medium, and dry the material at 50°C under an argon atmosphere of 0.3 liters / min to Raise the heating rate to 450°C at a rate of 5°C / min, keep it warm for 9 hours, and cool to room temperature with the furnace to obtain pre-fired material, use industrial alcohol as the medium for ball milling for 9 hours, and dry the material at 65°C after drying in 0.3 liters / min of argon Under the gas atmosphere, the temperature was raised to 720 °C at a rate of 4 °C / min, kept for 7 hours, and cooled to room temperature with the furnace, and the nominal composition formula was LiFe 0.98 Ce 0.02 P 0.9 W ...

Embodiment 3

[0054] 0.096 mole industrial grade lithium hydroxide LiOH·H 2 O, 0.002 mole europium oxalate Eu 2 (C 2 o 4 ) 3 10H 2 O, 0.0976 moles of ferrous acetate, 0.0024 moles of manganese oxalate Mn(C 2 o 4 )·2H 2 O, 0.1 mole ammonium phosphate (NH 4 ) 3 PO 4 Mix it into a nylon tank, add 70ml of industrial alcohol, seal it, and mix it for 7 hours on a planetary ball mill with stainless steel balls as the grinding medium. After drying at 50°C, dry it at 0.3 liters / min in a nitrogen atmosphere at 5°C / min. Raise the heating rate to 480°C in 1 minute, keep it warm for 5 hours, and cool it to room temperature with the furnace to get the pre-fired material, use industrial alcohol as the medium for ball milling for 11 hours, and dry the material at 60°C. Raise the temperature to 650°C at a rate of 4°C / min, keep the temperature for 4 hours, and cool down to room temperature with the furnace, and the nominal composition formula is Li 0.96 Eu 0.04 Fe 0.976 mn 0.024 PO 4 positive ...

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Abstract

The invention discloses a preparation method of a multi-place doped lithium iron phosphate anode material and an application thereof, which belong to the technical field of the preparation of electrochemical power materials. The multi-place doped lithium iron phosphate anode material is expressed by the following formula: Li1-xAxFe1-yByP1-zCzO4Ddelta, wherein, at least two of x, y, x and delta can not be expressed zero at the same time. Multi-place doped anode material lithium iron phosphate powder which is used in a secondary lithium-ion battery and has good crystallization performance and even composition is prepared by adopting a solid phase method and a simple mixing and drying process; compared with the method doping in a certain crystal lattice place, the multi-place doped anode material lithium iron phosphate powder has wide doping material source, which can greatly improve the basic capacity and cycling electrical performance of matrix and is applied to a stable industrialized production and non-high-purity materials. The multi-place lithium iron phosphate of the invention is taken as the anode material and is usually used in the secondary lithium-ion battery and the secondary lithium-ion battery is taken as a power source.

Description

Technical field [0001] The invention belongs to the technical field of electrochemical power supply material preparation. In particular, it relates to a preparation method and application of a multi-site doped lithium iron phosphate cathode material as a commonly used secondary lithium ion battery and secondary lithium ion battery for power energy. Background technique [0002] In 1997, J.B. Goodenough et al. first proposed LiFePO in U.S. Patent USA 5,910,382. 4 As a cathode material for secondary lithium-ion batteries. In the same year, M.Armand et al. disclosed LiFePO in U.S. Patent USA6,514,640 4 Materials that undergo iron site doping and phosphorus site substitution. LiFePO 4 It has many advantages such as cheap, non-toxic, non-hygroscopic, good environmental compatibility, rich mineral resources, high capacity, and good stability. However, the electronic conductivity of this material is poor, which greatly limits the application of the material at higher current d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/48H01M4/04C01B25/45H01M4/62
CPCY02E60/10
Inventor 罗绍华诸葛福长
Owner 甘肃大象能源科技有限公司
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