Method for preparing ferrous phosphate radical lithium salt of lithium ion battery

A lithium-ion battery, ferrous phosphate-based technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as limited application and poor conductivity, and achieve improved conductivity, good carbon-encapsulation effect, and improved electronic The effect of mobility

Inactive Publication Date: 2011-01-19
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Goodenoug hours [A.K.Pad hours i, K.S.Nanjundaswarmy, J.B.Goodenoug hours, J.Electroc hours em.Soc., 144 (1997) 1188] etc. synthesized a kind of iron-containing lithium salt LiFePO 4 , using this material as a positive electrode material for lithium-ion batteries has a higher theoretical specific capacity (170mAh / g), which is greater than that of commercial LiCoO 2 The actual capacity performance of 140mAh / g has attracted great attention of researchers, but due to the poor conductivity of this material, it can only be charged and discharged at a very small rate, which greatly limits its application in practical batteries. application in

Method used

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  • Method for preparing ferrous phosphate radical lithium salt of lithium ion battery
  • Method for preparing ferrous phosphate radical lithium salt of lithium ion battery
  • Method for preparing ferrous phosphate radical lithium salt of lithium ion battery

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Lithium iron phosphate is prepared by grinding and mixing, and the preparation process is as follows:

[0028] 1) will Li 3 PO 4 and Fe 3 (PO 4 ) 2 Mixed into a mixture with a molar ratio of 1:1;

[0029] 2) Grind the mixture obtained in step 1) with a ball mill for 1-2 hours, and add an appropriate amount of alcohol during grinding for better grinding;

[0030] 3) Put the milled mixture into a high-temperature furnace, and heat it for pretreatment under a protective atmosphere of nitrogen and hydrogen, wherein the volume ratio of nitrogen and hydrogen is 9.5:0.5, and the furnace chamber pressure is 1.5×10 5 Pa, the temperature is 600 ℃ ~ 700 ℃, pretreatment 10 ~ 20 hours;

[0031] 4) Cool down to room temperature after the pretreatment, take out the material, add alcohol and carbon black and re-grind evenly, where carbon black accounts for carbon black and LiFePO 4 5-15% of the total weight, the carbon black can also be replaced by organic carbon, acetylene blac...

Embodiment 2

[0035] Prepare doped lithium iron phosphate by grinding and mixing, the preparation process is as follows:

[0036] 1) will Li 3 PO 4 , Fe 3 (PO 4 ) 2 , Mg 3 (PO 4 ) 2 mixed to form a mixture, in which, Li 3 PO 4 and Fe 3 (PO 4 ) 2 The molar ratio of Li is 1:0.5, Li 3 PO 4 and Mg 3 (PO 4 ) 2 The molar ratio of 1:0.5;

[0037] 2) Grind the mixture formed in step 1) with a ball mill for 1-2 hours, and add an appropriate amount of alcohol during the grinding for better grinding;

[0038] 3) Put the material obtained after grinding into a high-temperature furnace, and heat it under a protective atmosphere of nitrogen and hydrogen for pretreatment. The volume ratio of nitrogen and hydrogen is 9.5:0.5, and the pressure of the furnace chamber is 1.5×10 5 Pa, the temperature is 600℃~700℃, and the pretreatment is 10~20 hours;

[0039] 4) After the pretreatment is completed, it is lowered to room temperature, the material is taken out, and alcohol and carbon black are...

Embodiment 3

[0043] Lithium iron phosphate is prepared by spray-drying the mixture, and this method can obtain nano-sized LiFePO 4 Powder, its preparation process is as follows:

[0044] 1) will Li 3 PO 4 and Fe 3 (PO 4 ) 2 Mix at a molar ratio of 1:1 to form a mixture;

[0045] 2) Add deionized water to the above mixture to form a solution A of 1.5-2 mol / L, and then add a polymer compound as a thickener to form a solution B, wherein the thickener accounts for 30% by mass of the solution B ~40%, the thickener is one of polyethylene glycol, polyacrylic acid or polyvinyl alcohol;

[0046] 3) Spray drying: Dry the solution B formed in step 2) into a mixed powder in an air-flow spray dryer, wherein the feed solution is injected with a peristaltic pump at a sampling speed of 20-25ml / min, and the gas flow rate of the nozzle is Controlled by the pressure of compressed air, atomization is generated at about 0.15MPa, the air inlet temperature is 400-500°C, the air outlet temperature is 200-300...

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Abstract

The invention provides a method for preparing ferrous phosphate radical lithium salt of a lithium ion battery, which comprises the following steps of: mixing Li3PO4 and Fe3(PO4)2 into a mixture; mixing uniformly by adopting a grinding or atomizing mode; transferring the uniformly mixed mixture into a high temperature furnace, pretreating under the protection of mixed nitrogen and hydrogen, wherein the volume ratio of the nitrogen to the hydrogen is 9.5:0.5; the pressure of the furnace chamber is 1.5*105Pa, the temperature is 600 to 700 and the time is 10 to 20 hours; after the temperature is reduced to room temperature, taking the material out, and adding carbon black and alcohol for uniform mixing; transferring the uniformly mixed material into the high temperature furnace, and performing high temperature treatment under the protection of nitrogen, wherein the pressure of the furnace chamber is 1.2*105Pa, the temperature is 700 to 900 DEG C and the time is 10 to 20 hours; and finally, reducing the temperature to room temperature. The lithium iron phosphate prepared by the method has good conductivity and electron mobility; and the process is simple.

Description

technical field [0001] The invention relates to the preparation of a lithium ion battery cathode active material, in particular to a preparation method of a lithium ion battery ferrous phosphate lithium salt. Background technique [0002] Since the advent of lithium-ion batteries in 1991, their cathode materials have been a hot spot in material research. The current research mainly focuses on transition metal oxides containing lithium, and the transition metals are mainly nickel, cobalt, and manganese. In recent years, due to the abundance of iron in the earth's crust, its cheap price, and environmental friendliness, based on Fe 2+ / Fe 3+ Redox-coupled substances have aroused great interest, so people are racing to study iron-containing lithium salts to replace current cathode materials. [0003] Goodenoug hours [A.K.Pad hours i, K.S.Nanjundaswarmy, J.B.Goodenoug hours, J.Electroc hours em.Soc., 144 (1997) 1188] etc. synthesized a kind of iron-containing lithium salt LiFe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45
Inventor 李俊
Owner IRICO
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