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Preparation method of lithium iron phosphate battery material

A lithium iron phosphate battery, phosphoric acid technology, applied in battery electrodes, secondary batteries, nanotechnology for materials and surface science, etc., can solve the difficulty of increasing raw material screening, high magnetic foreign matter in lithium iron phosphate, battery cycle Issues such as lifetime and safety performance impact

Active Publication Date: 2019-02-12
BEIJING TAIFENG XIANXING NEW ENERGY TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But also have obvious deficiency in the disclosed invention, as CN106744780A, it adopts the iron source Fe of high compaction 3 o 4 and Fe 2 o 3 , Fe 3 o 4 As a strong magnetic substance, it is easy to cause high magnetic foreign matter in lithium iron phosphate, which will affect the cycle life and safety performance of the battery
And in CN10725698A need to be big (0.6~3 μm), the FePO of small particle size (0.05~0.3 μm) 4 Raw materials are screened, which increases the difficulty of raw material screening in the process of industrialization

Method used

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  • Preparation method of lithium iron phosphate battery material
  • Preparation method of lithium iron phosphate battery material
  • Preparation method of lithium iron phosphate battery material

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Mix iron source (ferrous sulfate), phosphorus source (phosphoric acid + ammonium dihydrogen phosphate) and plasticizer (sodium hydroxide) in a molar ratio of 0.9:(0.5+0.5):0.9 and dissolve in 500ml deionized water, The concentration of Fe ions is 1mol / L; all materials are mixed evenly and transferred to a 1L three-necked flask, and placed in an electric heating mantle for heating, using an electric stirrer to stir at a speed of 200rpm, and the temperature of the solution system rises to 50 ° C, adding 0.15molH 2 o 2 (30% of the molar amount of iron source) to make Fe 2+ Fully oxidize, heat the oxidized solution system to 85°C for 4 hours, and obtain xFePO 4 (H 2 O) 2 ·(1-x)Fe 2 o 3 The pink precipitate was analyzed by X-ray diffractometer software and x was 0.928; the pink precipitate was pre-fired in a muffle furnace at 550°C for 5 hours to obtain 0.928FePO 4 0.072 Fe 2 o 3 Composite; the X-ray diffraction spectrum, field emission electron microscopy and parti...

Embodiment 2

[0051] Iron source (ferrous sulfate + ferrous chloride), phosphorus source (ammonium dihydrogen phosphate) and plasticizer (NaHCO 3+NaOH) according to the molar ratio (0.2+0.65):1:(0.3+0.3) and dissolved in 600ml of deionized water for mixing, in which the concentration of Fe ions is 1.1mol / L, and all materials are mixed evenly and then transferred to a 1L three-necked flask , and placed in an electric heating mantle for heating, using an electric stirrer to stir at a speed of 200rpm, so that the temperature of the solution system rose to 60 ° C, adding 0.198molH 2 o 2 (30% of the molar amount of iron source) to make Fe 2+ Fully oxidize, heat the oxidized system to 90°C for 2 hours to obtain xFePO 4 (H 2 O) 2 ·(1-x)Fe 2 o 3 Pink precipitate; x equal to 0.911 calculated from X-ray diffractometer software.

[0052] The white precipitate was pre-fired in a muffle furnace at 550°C for 4 hours to obtain 0.911FePO 4 0.089Fe 2 o 3 complex; the complex, Li 2 CO 3 , NH 4 h...

Embodiment 3

[0055] Mix iron source (ferrous sulfate), phosphorus source (ammonium dihydrogen phosphate) and plasticizer (sodium carbonate) in a molar ratio of 1.05:1:0.1 and dissolve in 700ml of deionized water, wherein the Fe ion concentration is 0.5mol / L, all materials were mixed evenly and transferred to a 1L three-neck flask, and placed in a water bath with magnetic stirring for heating, the speed was adjusted to 400rpm, the temperature of the solution system rose to 55°C, and 0.175molH 2 o 2 (50% of the molar amount of iron source) to make Fe 2+ Fully oxidize, heat the oxidized system to 85°C for 10 hours to obtain xFePO 4 (H 2 O) 2 ·(1-x)Fe 2 o 3 Pink precipitate; x equal to 0.935 calculated from X-ray diffractometer software.

[0056] The white precipitate was pre-fired in a muffle furnace at 600°C for 3 hours to obtain 0.935FePO 4 0.065 Fe 2 o 3 complex; the complex, LiOH and phosphorus source supplement ((NH 4 ) 2 HPO 4 +NH 4 h 2 PO 4 ) is mixed in molar ratio acc...

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Abstract

The invention provides a preparation method of a lithium iron phosphate battery material. The method comprises the steps that an iron source, a phosphate source and a molding agent are dissolved in deionized water after being mixed; a mixed solution is heated to 50-70 DEG C for stirring while heating, and H2O2 is added for complete oxidation; the oxidized solution is heated to 80-95 DEG C, and heat preservation is conducted for 1-10 h to obtain pink or white sediment; the pink or white sediment is subjected to pre-sintering, pre-sintering temperature is 450-650 DEG C, and pre-sintering time is1-8 h, so that a compound is obtained; the compound, a lithium source and a phosphate source supplement are mixed, a carbon source is added, and in a sand mill, wet grinding is conducted to obtain amaterial in required particle size; the material is subjected to sintering in an inert atmosphere or reductive atmosphere after being dried, sintering temperature is 700-850 DEG C, and sintering timeis 5-20 h, so that the high-compaction high-capacity LiFePO4 / C material is obtained.

Description

technical field [0001] The invention belongs to the technical field of batteries, and in particular relates to a preparation method of a lithium iron phosphate battery material. Background technique [0002] As an efficient energy storage device for sustainable energy, lithium-ion batteries have undergone tremendous development since their commercialization in 1991. Commonly used cathode materials for lithium-ion batteries are lithium cobalt oxide (LiCoO 2 ), lithium manganate (LiMn 2 o 4 ), lithium nickelate (LiNiO 2 ), ternary materials (LiNi x mn y co 1-x-y o 2 ) and lithium iron phosphate (LiFePO 4 )Wait. Lithium iron phosphate cathode material is widely used in electric vehicles due to its advantages of high safety, long cycle life, cheap and easy-to-obtain raw materials, and no pollution to the environment. With the adjustment of the state's subsidy policy for electric vehicles and the impact of the market, lithium iron phosphate needs to increase its own ene...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/366H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 张淑萍马家璨范永新成富圈杨新河周恒辉
Owner BEIJING TAIFENG XIANXING NEW ENERGY TECH CO LTD
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