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Preparation method for lithium ion fast conductor modified lithium iron phosphate material

A lithium iron phosphate, fast conductor technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of low tap density, material capacity attenuation, low lithium ion diffusion coefficient, etc., to achieve good electrical conductivity and improve power performance. Effect

Inactive Publication Date: 2012-06-27
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when using the solid-phase method, it is difficult to mix various solid components fully, so the various components in the obtained lithium iron phosphate positive electrode active material, especially the conductive agent, are not uniformly dispersed, which directly affects the conductivity of the positive electrode active material.
[0004] So far, there have been many reports on the synthesis methods of materials. The most researched and most likely to realize industrialization is the high-temperature solid-phase method, but lithium iron phosphate has its inherent shortcomings, such as low lithium ion diffusion coefficient and poor conductivity. etc. Therefore, the materials prepared by the conventional method have disadvantages such as poor electrochemical performance, uneven particle size distribution, and low tap density.
In order to improve the performance of the material, it is generally doped or coated, such as C coating (CN101172599, CN101442117, CN101764205A, CN101777636A), transition metal doping (CN1785799), rare earth doping (CN1830764, CN101630738), etc., The above methods can improve the performance of lithium iron phosphate to a certain extent, but the performance improvement is not too significant
Especially in the selection of rare earth elements, which are usually common rare earths, but the valence changes a lot, resulting in easy disproportionation during the reaction and product charging and discharging, and the performance of its lithium iron phosphate is significantly reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 0.7 mol of LiOH to 120 ml of deionized water, and add 0.075 mol of PO(OC 4 h 9 ) 3 with 0.05 moles of Ti(OC 4 h 9 ) 4 And keep stirring, dropwise add ammonia water to adjust the pH value to 7.0. Then 1 mole of lithium iron phosphate was weighed and added to the above solution, and 0.0225 mole of MgO was added at the same time. The above mixture was stirred for 2 hours and then spray dried. Then dry at 120°C for 2 hours, calcinate the obtained powder at 600°C for 5 hours in an inert atmosphere of nitrogen, cool naturally, and grind to obtain a surface-coated lithium ion fast conductor 0.1LiTi 2 (PO 4 ) 3 - MgO lithium iron phosphate powder, the mass percentage of the surface coating is 3%, and the initial capacity of 40C of the synthetic material is 101mAh / g.

[0020] The electrochemical performance test of the material is carried out according to the following method. First, the positive electrode material is coated into an electrode sheet. The adhesive use...

Embodiment 2

[0022] Weigh 0.2003g of lithium carbonate, 2.7115g of aluminum nitrate and 1.2472g of ammonium dihydrogen phosphate, put the three in a 400ml deionized water bath and stir evenly, the temperature of the water bath is 80°C, add ammonia water dropwise to adjust the pH to 6.0. Weigh 100g of lithium iron phosphate, add it into a beaker and continue stirring, spray dry, then dry at 120°C for 2 hours, calcinate the obtained powder at 700°C for 10 hours in an inert atmosphere of nitrogen, cool naturally, and grind to obtain a lithium-ion fast conductor coated on the surface Lithium Iron Phosphate. Through physical and chemical analysis, it is concluded that the thickness of lithium ion fast conductor is about 30nm, and its molecular expression is: Li 3 al 2 P 3 o 12 , the coating mass ratio is 1.5%. The button battery was prepared according to the method of Example 1. The initial capacity at 40C was 121mAh / g, and the capacity remained above 90% after 300 cycles.

Embodiment 3

[0024]Weigh 0.7015g, 4.3765g, 0.1159g and 1.9969g of lithium hydroxide, n-butyl titanate, silicon dioxide and ammonium dihydrogen phosphate respectively, place them in 100ml of deionized water and stir evenly in a water bath, the temperature of the water bath is 80°C, Add ammonia water dropwise to adjust the pH value to 6.5. Weigh 150g of lithium iron phosphate, add it into a beaker and continue to stir for 2 hours, spray dry, then dry at 120°C for 2 hours, calcinate the obtained powder in a tube furnace in an inert atmosphere of argon at 550°C for 15 hours, cool naturally, and grind to obtain a surface coating Lithium iron phosphate as fast conductor of lithium ions. Through physical and chemical analysis, it is concluded that the thickness of lithium ion fast conductor is about 50nm, and its molecular expression is: Li 1.3 Ti 2 Si 0.3 P 2.7 o 12 , the coating mass ratio is 3%. The button battery was prepared according to the method of Example 1. The initial capacity at...

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Abstract

The invention relates to a lithium ion battery positive material, in particular to a preparation method for a lithium ion fast conductor modified lithium phosphate material. The preparation method is characterized by comprising the following steps: (1) according to the components of the lithium ion fast conductor, covering raw materials including a lithium source, an A source, a B source, an N source, a silicon source and a phosphorus source are mixed with lithium iron phosphate to be covered to form a precursor, and then the precursor is dried; (2) the obtained precursor is sintered in an inert atmosphere, the sintering temperature is 400-1,000 DEG C, and the soaking time is 2-20 hrs. In the preparation method, a layer of lithium ion fast conductor film is compound on the surface of a nano lithium iron phosphate, so as to greatly improve the power performance of the nano lithium iron phosphate; particularly, the glass state lithium ion fast conductor is a well-know favorable and stable lithium conductor, at the same time, favorable conductivity is acquired by adulterating a transition metal; and adopting the material prepared by the invention to manufacture batteries, more than 40 c high current charging / discharging can be achieved.

Description

technical field [0001] The invention relates to a lithium ion battery cathode material, in particular to a preparation method of a lithium ion fast conductor modified lithium iron phosphate material. 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] In the prior art, the positive electrode active material LiFePO is generally prepared by solid phase method or wet chemical method. 4 , such as CN 1401559A discloses a lithium iron phosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 刘涛涛
Owner IRICO
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