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Preparation method for lithium battery anode material LiFePO4 nano-powder body

A cathode material and nano-powder technology, applied in the field of lithium battery cathode material preparation, can solve problems such as unfavorable large-scale application, high equipment performance requirements, unfavorable large-scale production, etc., and achieve low cost, no environmental pollution, and reduced consumption. and the effect of emissions

Active Publication Date: 2009-02-18
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are some synthetic LiFePO 4 methods, but they all have some shortcomings, and the research and improvement of their synthetic methods has always been a research hotspot in this field.
At present, the existing synthetic LiFePO 4 The main methods and existing problems and shortcomings are: 1) high-temperature solid-phase synthesis method, Padhi et al. 2 o 4 ·H 2 O, (NH 4 ) 2 HPO 4 and Li 2 CO 3 As a raw material, grind and mix uniformly according to the chemical ratio and then in an inert atmosphere (such as Ar, N 2 ) under the protection of high temperature roasting reaction to prepare LiFePO 4
3) Microwave synthesis method. Microwave heating can heat the sample evenly and rapidly in a short time. This method is a simple and fast preparation method, but there are unfavorable factors that require high equipment performance and are not conducive to large-scale production.
This method is cumbersome and complicated to operate, which is not conducive to large-scale application

Method used

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  • Preparation method for lithium battery anode material LiFePO4 nano-powder body
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  • Preparation method for lithium battery anode material LiFePO4 nano-powder body

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Embodiment 1

[0033] LiFePO, a cathode material for lithium batteries 4 The preparation method of nanopowder is made up of following steps:

[0034] (1) Preparation of organic phase

[0035] Add naphthenic acid and isooctyl alcohol with an average molecular weight of 330 to the Erlenmeyer flask in a volume ratio of 2:1:1 and mix well, then add 0.1mol.L -1 Aqueous solution of ferrous sulfate, under magnetic stirring, add ammonia water to adjust the pH value to 6, continue to stir for 0.5 hours, pour the mixed solution into the separatory funnel, after standing still for 5 minutes, the solution is divided into upper and lower 2 phases at this time, separate the organic phase, Wash the organic phase 3 times with distilled water and then separate the liquid, then collect the organic phase;

[0036] (2) Preparation of water phase

[0037] Weigh 0.839g LiOH, add 6.66ml of 3mol / L H 3 PO 4 In the aqueous solution, add water to 20ml, and then add 0.167g LiOH after it is completely dissolved, ad...

Embodiment 2

[0045] A lithium battery positive electrode material LiFePO 4 The preparation method of nanopowder is made up of following steps:

[0046] (1) Preparation of organic phase

[0047] Add naphthenic acid and isooctyl alcohol with an average molecular weight of 350 in sequence in the conical flask at a volume ratio of 2:1:1, and then add 0.05mol L -1 ferric sulfate aqueous solution, adjust the pH value to 2 with ammonia water or hydrochloric acid aqueous solution, magnetically stir for about 0.5 hours, pour the mixed solution into a separating funnel, and separate the liquid after standing still for 10 minutes. At this time, the solution is divided into upper and lower phases, and the organic phase is separated. Phase, wash the organic phase twice with distilled water and then separate the liquid, then collect the organic phase;

[0048] (2) Preparation of water phase

[0049] Weigh 0.839g LiOH, add 6.66ml of 3mol / L H 3 PO 4 In the aqueous solution, add water to 20ml, and the...

Embodiment 3

[0057] A lithium battery positive electrode material LiFePO 4 The preparation method of nanopowder is made up of following steps:

[0058] (1) Preparation of organic phase:

[0059] Under stirring, mix naphthenic acid with an average molecular weight of 200 and isooctyl alcohol at a ratio of 1:3:5 by volume, and then add 0.01mol·L -1 ferrous sulfate aqueous solution, continue to stir, adjust the pH value to 6 with ammonia water or hydrochloric acid aqueous solution, continue to stir for 0.6 hours, pour it into the liquid separator, and let it stand for 5 minutes. At this time, the solution is divided into upper and lower phases, and the organic phase is separated. Phase, wash the organic phase twice with distilled water and then separate the liquid, then collect the organic phase;

[0060] (2) Preparation of water phase:

[0061] 0.5g of LiH 2 PO 4 Dissolve in 10ml of water and stir evenly to obtain the water phase;

[0062] (3) Substitution reaction and crystal formatio...

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Abstract

The invention discloses a preparation method of an anode material of lithium battery of LiFePO4 nanopowder, comprising: (1) stirring to uniformly mix naphthenic acid and isooctanol, adding ferrous sulfate solution, adjusting pH value, continuing to stir and pour it into separation apparatus, stabilizing, washing organic phase with distilled water, and collecting the organic phase; (2) taking the LiOH, adding H3PO4 solution, stirring to dissolve, adjusting pH value, adding ascorbic acid, uniformly stirring to obtain aqueous phase; (3) drawing the aqueous phase and organic phase into a high pressure autoclave, sealing, stirring and heating to react for 10 to 120 minutes, stopping heating and stirring; (4) cooling to room temperature, carrying out solid-liquid separation, washing the solid material with absolute alcohol, drying to obtain anode material of LiFePO4 nanopowder of lithium battery. The invention has low costs and contamination, wide raw material source, simple technology and process, low energy requirement, being easy for industrialization.

Description

technical field [0001] The invention relates to the field of preparation of lithium battery cathode materials, in particular to LiFePO, a lithium battery cathode material 4 Preparation method of nanopowder. Background technique [0002] LiFePO 4 It is a new type of cathode material for lithium batteries. It has excellent electrochemical properties and is superior in price and environmental protection. It is currently the most likely to completely replace LiCoO 2 positive active material. Although there are some synthetic LiFePO 4 However, they all have some shortcomings. The research and improvement of their synthetic methods have always been a research hotspot in this field. At present, the existing synthetic LiFePO 4 The main methods and existing problems and shortcomings are: 1) high-temperature solid-phase synthesis method, Padhi et al. 2 o 4 ·H 2 O, (NH 4 ) 2 HPO 4 and Li 2 CO 3 As a raw material, grind and mix uniformly according to the chemical ratio and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58C01B25/45
CPCY02E60/10
Inventor 王兴尧苗翠秦学李海港
Owner TIANJIN UNIV
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