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Oxygen vacancy-contained and Fe site-doped lithium ferric phosphate and rapid solid-phase sintering method thereof

A technology of lithium iron phosphate and solid phase sintering, applied in chemical instruments and methods, phosphorus compounds, structural parts, etc., can solve problems such as unstable product performance, high energy consumption, and long sintering time, and achieve excellent processing performance of pole pieces , reduce the reaction temperature, the effect of fast reaction speed

Active Publication Date: 2010-06-30
HENGDIAN GRP DMEGC MAGNETICS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the Chinese patent CN100377392C and the Chinese patent CN1328808C, high-temperature solid-state sintering is used as the preparation method of the material, and there are problems such as high energy consumption, long sintering time, and unstable product performance.

Method used

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  • Oxygen vacancy-contained and Fe site-doped lithium ferric phosphate and rapid solid-phase sintering method thereof
  • Oxygen vacancy-contained and Fe site-doped lithium ferric phosphate and rapid solid-phase sintering method thereof
  • Oxygen vacancy-contained and Fe site-doped lithium ferric phosphate and rapid solid-phase sintering method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1: Preparation of lithium iron phosphate cathode material LiFe of the present invention 0.8 Mg 0.1 Na 0.1 PO 3.95

[0040] First, weigh lithium hydroxide monohydrate, iron oxide, magnesium hydroxide, sodium fluoride and ammonium dihydrogen phosphate according to the molar ratio of 1:0.8:0.1:0.1:1, and add glucose with a mass ratio of 12% of the mixture, and put Put it into a sand mill, the ratio of ball material to water is 2:1:1, and mix for 3.5 hours. The mixed slurry is oven-dried, then made into a block using a continuous extruder, and put into a microwave reaction furnace, under 10 liters / minute of high-purity Ar gas and hydrogen gas mixture (wherein the hydrogen volume ratio is 8 %) protection, the temperature was raised to 650° C. at a rate of 50° C. / min, kept for 45 minutes, and then cooled to room temperature. After the sintered material is crushed with a crusher, it is classified on a jet mill to obtain lithium iron phosphate with uniform parti...

Embodiment 2

[0047] Preparation of lithium iron phosphate material LiFe containing oxygen vacancies of the present invention 0.98 mn 0.02 PO 3.97 N 0.02

[0048] First, take lithium hydroxide monohydrate, iron oxide, trimanganese tetraoxide, ammonium dihydrogen phosphate and lithium nitride according to the molar ratio of 0.94: 0.49: 0.0067: 1: 0.02, and add glucose with a mass ratio of 10% of the mixture, Put it into a sand mill, the ratio of balls to water is 2:1:1, and mix for 3 hours. Spray-dry the mixed slurry with a spray-drying tower, put it into a microwave reaction furnace, under the protection of 10 liters / min of high-purity Ar gas and hydrogen gas mixture, wherein the volume ratio of hydrogen is 6%, at 50°C / min The temperature was raised to 630°C at a certain rate, kept for 45 minutes, and then cooled to room temperature. After the sintered material is crushed with a crusher, it is classified on a jet mill to obtain lithium iron phosphate with uniform particles.

[0049] T...

Embodiment 3-6 and comparative example 1-3

[0053] According to the method of Example 2, the positive electrode material for the secondary lithium ion battery of the present invention composed of Table 1 is prepared, the difference is that, for the samples replaced by Fe sites and oxygen vacancies, the required dose is added to the precursor Ratio of precursors for corresponding doping elements. The rest of the preparation steps are the same as in Example 2.

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Abstract

The invention relates to an oxygen vacancy-contained and Fe site-doped lithium ferric phosphate as a lithium ion anode material and a rapid microwave sintering preparation method thereof. The formula of the invention product is LiFe1-x-aMeaMxPO4-yNz, wherein Me is one or more of Mg, Mn or Nd, and M is one or more of Li, Na, K, Ag, Cu; 0<=x<=0.1, 0<a<=0.1, 0<y<=0.5, 0<=z<=0.5 (4.9), wherein x and z can not be 0 at the same time. The rapid microwave sintering preparation method of the invention has high production efficiency, low energy consumption, good stability of prepared product batches, as well as excellent rate capability and cycle performance.

Description

technical field [0001] The invention relates to a lithium ion battery material and a preparation method thereof, in particular to an oxygen vacancy and Fe site doped lithium ion positive electrode material lithium iron phosphate and a preparation method thereof by rapid microwave sintering. Background technique [0002] In recent years, lithium-ion batteries have developed very rapidly. The demand for lithium-ion batteries in various portable electronic products and communication tools has continued to increase, and large-scale power lithium-ion power supplies are also in the upsurge of development. Cathode materials are an important part of lithium-ion batteries, and the development of new cathode materials has become the key to the development of lithium-ion batteries. LiCoO is currently commercialized on a large scale 2 , high toxicity, high price, and certain safety problems. LiNiO 2 The cost is low, the capacity is high, but the preparation is difficult, the thermal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/1397C01B25/45H01M10/058H01M10/0525H01M4/136
CPCY02E60/12Y02E60/122Y02E60/10Y02P70/50
Inventor 金江剑王国光徐君包大新
Owner HENGDIAN GRP DMEGC MAGNETICS CO LTD
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