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Particle appearance regulatory lithium iron phosphate preparation method

A particle, phosphate ion technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of rare reports on morphology control and adjustment, and achieve low cost, excellent rate performance, and low reaction temperature. Effect

Active Publication Date: 2009-04-22
QINGHAI TAIFENG XIANXING LITHIUM ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the hydrothermal method has been applied to LiFePO 4 Synthesis of (S.F.Yang, P.Y.Zavalij, M.S.Whittingham.Electrochem.Commun., 3(9)(2001):505), but reports on morphology control and regulation are rare

Method used

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  • Particle appearance regulatory lithium iron phosphate preparation method
  • Particle appearance regulatory lithium iron phosphate preparation method
  • Particle appearance regulatory lithium iron phosphate preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 0.3mol LiOH·H 2 O, 0.1mol FeSO 4 ·7H 2 O and 0.1mol H 3 PO 4 Mix, add 1000ml deionized water to dissolve, then add 30% sucrose, then transfer to 1000ml polytetrafluoroethylene reaction vessel, react at 175°C for 5 hours. After cooling, wash with deionized water and ethanol, centrifuge and dry. Finally, it was pyrolyzed at 500° C. for 1 hour in a sealed tube furnace protected by nitrogen to obtain the lithium iron phosphate granular product.

[0026] The obtained lithium iron phosphate product is olivine structure, adopts Cu target Kα radiation, λ=0.15406nm, obtains the X-ray diffraction pattern of this product, as figure 1 shown. Through the field emission scanning electron microscope, it can be seen that the lithium iron phosphate particles are rod-shaped, about 1 μm in length, and 0.2-0.4 μm in width and height, such as figure 2 shown. The charge and discharge curve of the product is as follows Figure 8 As shown, the voltage range is 2.0-4.1V, the temperatu...

Embodiment 2

[0028] 0.005mol FePO 4 and 0.01mol LiOH·H 2 O mixed, add 200mL water / ethanol (1:1 / V:V) mixed solvent, then add 50% citric acid, then transfer to a polytetrafluoroethylene reaction vessel, and react at 200°C for 5 hours. After cooling, it was washed with deionized water and ethanol, centrifuged, dried, and calcined at 600°C for 5 hours in an argon-protected sealed tube furnace to obtain a lithium iron phosphate product. The product is uniform and spindle-shaped, about 0.3-0.6 μm wide and 3-5 μm long (see image 3 ).

Embodiment 3

[0030] 0.12mol LiOH·H 2 O, 0.04mol (NH 4 ) 2 Fe(SO 4 ) 2 12H 2 O and 0.04mol(NH 4 ) 2 HPO 4 Mix, add 400ml of water / ethylene glycol (5:1 / V:V) mixed solution, add 4% PAA, then transfer to a polytetrafluoroethylene reaction vessel, and react at 220°C for 2 hours. After cooling, wash with deionized water and ethanol, centrifuge and dry to obtain lithium iron phosphate particle product. The product is a short rod, about 0.8 μm long, about 0.2 μm wide, and arranged in an array (see Figure 4 ). Example 4

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Abstract

The invention discloses a modulating method of LiFePO4 particle shape, which comprises the following steps: blending one or more composition with lithium ion, ferric ion and phosphate radical ion; adding solvent and certain quantity of crystal growing inhibitor; proceeding solvent heat reaction under certain temperature; washing; filtering; drying; sintering to improve crystallizing property; obtaining the product with regular shape and size.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to a method for preparing lithium iron phosphate particles. technical background [0002] As a new cathode material for lithium-ion batteries, LiMPO 4 Homologs especially LiFePO 4 It has received extensive attention and in-depth research (A.K.Padhi, K.S.Nanjundaswarmy, J.B.Goodenough, J.Electrochem.Soc.144(4)(1997)1184). LiFePO 4 With a theoretical capacity of 170mAh / g, the actual capacity can exceed 160mAh / g, which is higher than commercial LiCoO 2 To be higher, the discharge platform is about 3.4V, than LiCoO 2 slightly lower. However, it has a wide range of sources of raw materials, low cost, high safety, and environmental friendliness, and is especially suitable for batteries for various high-power electrical appliances and power batteries for automobiles. The disadvantage is that the conductivity is relatively small (~10 -9 S / cm), the lithium ion diffusion performanc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58
CPCY02E60/12Y02E60/10
Inventor 倪江锋周恒辉陈继涛张新祥
Owner QINGHAI TAIFENG XIANXING LITHIUM ENERGY TECH CO LTD
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