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Method for manufacturing lithium metal phosphate

一种锂金属磷酸盐、磷酸盐的技术，应用在非金属元素、碱金属化合物、化学仪器和方法等方向，能够解决粒子成长及工序费用增加等问题，达到工序便利、电池特性优异、特性提高的效果

Active Publication Date: 2015-10-28
SAMSUNG SDI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses amorphous iron phosphate in which iron and phosphate atoms are randomly mixed as a precursor, so there are problems in that a high temperature is required in the calcination process, and particle growth and process costs are caused by this high-temperature synthesis process. increase

Method used

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  • Method for manufacturing lithium metal phosphate
  • Method for manufacturing lithium metal phosphate
  • Method for manufacturing lithium metal phosphate

Examples

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preparation example Construction

[0038] The present invention relates to the preparation method of lithium metal phosphate using crystalline iron phosphate or metal-doped crystalline iron phosphate as a precursor, and provides a lithium metal phosphate (LiMFePO) shown in the following formula I 4 , LMP) preparation method, comprising: the step of mixing slurry-like or cake-like crystalline iron phosphate and lithium raw material; and the step of heat-treating the above-mentioned mixture,

[0039] Formula I

[0040] Li M 1-n Fe n PO 4

[0041] Wherein, M is selected from the group consisting of Ni, Co, Mn, Cr, Zr, Nb, Cu, V, Ti, Zn, Al, Ga and Mg, and 0

[0042] The crystalline iron phosphate (FP) is a (quasi) strengite structure in which octahedral and tetrahedral structures share corners (Corner-sharing), which is similar to the olivine structure of lithium iron phosphate (Olivine), that is, octahedral and tetrahedral structure sharing line-sharing (line-sharing) structure is similar, so compared w...

Embodiment 1

[0058] (1) Amorphous iron phosphate hydrate (amorphous FePO 4 2H 2 O) Synthesis

[0059] Weigh FeCl in such a way that the molar ratio of [Fe]:[P] is 1:1 3 ·6H 2 O and (NH 4 ) 2 HPO 4 and added to pure water for mixing to form a slurry. At this time, the ratio of the solid content to the solvent was 10%. Next, add ammonia water (NH 4 OH) to adjust the pH to 4.5. Next, the pH-adjusted slurry was stirred at 60° C. for 15 minutes. Next, the reaction slurry was washed three times with a centrifuge to obtain a cake-like non-crystalline iron phosphate hydrate.

[0060] (2) Crystalline iron phosphate hydrate (crystalline FePO 4 2H 2 O) Synthesis and Synthesis of LFP Using It

[0061] Pure water was added to the filter cake of amorphous iron phosphate hydrate obtained above to form a slurry. At this time, the volume ratio of the solid content to the solvent was 10%. Phosphoric acid (H 3 PO 4 ) to adjust the pH to 2. Next, the pH-adjusted slurry was stirred at 95°C fo...

Embodiment 2

[0063] (1) Amorphous iron phosphate hydrate (amorphous FePO 4 2H 2 O) Synthesis

[0064] In the same manner as in the above-mentioned Example 1, a filter cake-shaped amorphous iron phosphate hydrate was obtained.

[0065] (2) Crystalline iron phosphate hydrate (crystalline FePO 4 2H 2 O) Synthesis and Synthesis of LFP Using It

[0066] Pure water was added to the non-crystalline iron phosphate hydrate filter cake obtained above to form a slurry. At this time, the volume ratio of the solid content to the solvent was 10%. Phosphoric acid (H 3 PO 4 ) to adjust the pH to 2. Next, the pH-adjusted slurry was stirred at 95° C. for 3 hours. At the point when the color of the slurry became light, the reaction was terminated. Then, the reaction slurry was washed 3 times with a centrifuge, and the water content of the washed filter cake was measured. On this basis, LiOH was added as a lithium raw material so that the molar ratio of [Li]:[Fe] was 1:1. Sucrose (sucrose) was adde...

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Abstract

The present invention relates to a method for manufacturing lithium metal phosphate (LMP) having, as a precursor, crystalline iron phosphate having a (meta)strengite structure or metal-doped crystalline iron phosphate having a (meta)strengite structure, the method comprising the steps of: mixing a lithium raw material with crystalline iron phosphate in slurry phase or cake phase; and heat-treating the mixture. The method, by having a lithium (Li) raw material and a carbon (C) coating material mixed with crystalline iron phosphate in slurry phase or cake phase, allows elements Li, Fe, P and C to be homogeneously mixed, and then, by having the elements dried simultaneously, enables manufacturing of high-quality LMP. Therefore, the present invention is not only capable of providing convenience during the manufacturing process for lithium metal phosphate, but also capable of providing a lithium secondary battery positive electrode active material having excellent battery characteristics.

Description

technical field [0001] The present invention relates to the preparation method of lithium metal phosphate salt, more specifically, relate to the following method: In order to prepare the lithium metal phosphate (LiMFePO 4 , hereinafter referred to as LMP), the crystalline iron phosphate (FePO 4 , hereinafter referred to as FP) or metal-doped crystalline iron phosphate (MFePO 4 , hereinafter referred to as MFP) are mixed with slurry-like or cake-like lithium (Li) raw materials and carbon (C) coating materials, and the Li, Fe, P and C elements are dried simultaneously, so that the above-mentioned elements are uniformly mixed, and finally Capable of synthesizing high-quality LMP. Background technique [0002] The olivine structure type lithium metal phosphate (LMP) generally used as an anode active material for lithium secondary batteries is produced by the following two methods. [0003] The first approach is to prepare lithium metal phosphates using ferrous iron feedstock....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/00C01G53/00H01M10/052
CPCH01M4/5825C01B25/45H01M10/0525Y02E60/122Y02P70/54H01M4/0471H01M4/366H01M4/587H01M4/625Y02E60/10C01D15/00C01G53/00H01M10/052C01P2006/40
Inventor 宋炫妸张东圭金钟珉申载胜
Owner SAMSUNG SDI CO LTD
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