Iron manganese vanadium phosphate precursor, iron manganese vanadium lithium phosphate/carbon anode material and preparation method

An iron manganese vanadium vanadium precursor and bulk material technology, applied in chemical instruments and methods, phosphorus compounds, battery electrodes, etc., can solve the problems of many side reactions, low purity of iron manganese vanadium lithium phosphate, unstable raw materials, etc. Specific energy, simplified test content, effect of high specific power

Active Publication Date: 2017-03-08
ENERGY RES INST OF SHANDONG ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although there is also a preparation method for lithium iron manganese vanadium phosphate in the prior art, generally ferrous iron compounds are used as the iron source to directly react to generate lithium iron manganese vanadium phosphate. This preparation method basically directly reacts to generate iron manganese vanadium phosphate Lithium, because the raw material cannot exist stably, so there are many side reactions in the preparation process, and the purity of the obtained lithium iron manganese vanadium phosphate is low, so that the performance of the obtained positive electrode material cannot fully meet certain needs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 129.28g of ferric nitrate, 8.053g of manganese sulfate, 3.1195g of ammonium metavanadate, and 39.2g of phosphoric acid, add deionized water to mix and dissolve, then set the volume to 1L (the molar concentration of the acid solution is about 0.4M), and measure 200ml of concentrated ammonia water , add deionized water to set the volume to 1L (the molar concentration of lye is about 1M), pump the acid solution and lye solution into the stirred reactor filled with deionized water at a feed rate of 1L / h respectively, and control the reaction temperature 40°C, stirring rate 200rpm, reaction pH value is about 2, take out the precipitated product after reaction for 1h, separate the solid and liquid after washing several times, dry in an oven at 80°C for 5h, pre-fire in a tube furnace at 300°C under the protection of an inert atmosphere 6h to obtain iron vanadium manganese phosphate (Fe 0.8 mn 0。133 V 0.066 PO 4 ) precursor material, weigh 6g iron vanadium manganese ph...

Embodiment 2

[0036] Embodiment 2: take by weighing 282.8g ferric nitrate, 50.2g manganese nitrate, 11.698g ammonium metavanadate, 115g ammonium dihydrogen phosphate, add deionized water and mix and dissolve and settle to 1L (acid liquid molar concentration is about 1M), Measure 600ml of concentrated ammonia water, add deionized water to make up to 1L (the molar concentration of lye is about 3M), pump the acid solution and lye solution into the stirring reaction kettle filled with deionized water at a feed rate of 500mL / h In the process, the reaction temperature is controlled at 30°C, the stirring rate is 600rpm, and the reaction pH value is about 3. After 2 hours of reaction, the precipitated product is taken out, washed several times, separated from solid and liquid, dried in an oven at 80°C for 5 hours, and protected in an inert atmosphere in a tube furnace. Pre-fired at 500°C for 6 hours to obtain iron vanadium manganese phosphate (Fe 0.7 mn 0。2 V 0.1 PO 4 ) precursor material, weigh...

Embodiment 3

[0037] Example 3: 0.4M, x=0.6 ferric chloride, manganese acetate, vanadium pentoxide, lithium carbonate, sucrose

[0038] Weigh 25.952g of ferric chloride, 27.68g of manganese acetate, 14.55g of vanadium pentoxide, and 39.2g of phosphoric acid, add deionized water to mix and dissolve, then set the volume to 1L (the molar concentration of the acid solution is about 0.4M), and measure 200ml Concentrated ammonia water, add deionized water to set the volume to 1L (the molar concentration of lye is about 1M), pump the acid solution and lye solution into the stirring reaction kettle filled with deionized water at a feed rate of 1L / h respectively, and control The reaction temperature is 30°C, the stirring rate is 600rpm, and the reaction pH value is about 3. After 1 hour of reaction, the precipitated product is taken out, washed several times, separated from solid and liquid, dried in an oven at 80°C for 5 hours, and placed in a tube furnace at 500°C under the protection of an inert a...

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PUM

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Abstract

The invention discloses an iron manganese vanadium phosphate precursor, an iron manganese vanadium lithium phosphate / carbon anode material and a preparation method. The preparation method includes following steps: 1), preparing a mixed solution of ferric iron source, manganous source, pentavalent vanadium source and phosphor source, and preparing an ammonia water solution; 2), mixing the mixed solution with the ammonia water solution according to a set proportion for co-precipitation reaction to obtain a precipitation product; 3), subjecting the precipitation product to washing, drying and pre-sintering to obtain an iron manganese vanadium phosphate precursor material, well mixing the iron manganese vanadium phosphate precursor material with a lithium source and a carbon source, drying, and calcining in an inert atmosphere to obtain the iron manganese vanadium lithium phosphate / carbon anode material. The iron manganese vanadium phosphate precursor is prepared firstly, a ferric iron compound is used as an iron source in the process of preparation, control on valence state changing of iron is unique, ferric iron can be ensured to be reduced into ferrous in the subsequent carbothermic reaction step, and then the LiFe1-xMn2x / 3Vx / 3PO4 material high in both purity and electrochemical performance is obtained.

Description

technical field [0001] The invention belongs to the technical field of energy materials, in particular to an iron manganese vanadium phosphate (Fe 1-x mn 2x / 3 V x / 3 PO 4 ) precursor and lithium iron manganese vanadium phosphate / carbon (LiFe 1-x mn 2x / 3 V x / 3 PO 4 / C) preparation method. Background technique [0002] Lithium-ion battery cathode materials directly determine the performance indicators of the final battery product. At present, the commercialized lithium-ion battery cathode materials include lithium cobaltate, lithium manganese oxide, ternary materials, lithium iron phosphate, etc. Compared with other The positive electrode material has the advantages of high stability, safety, reliability, environmental protection and low price, and has become one of the ideal positive electrode materials for power and energy storage lithium-ion batteries recognized in the industry. However, the low energy density of this material hinders its large-scale application in p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525C01B25/45
CPCC01B25/45H01M4/5825H01M10/0525Y02E60/10
Inventor 杨改应皆荣高剑蔡飞鹏王波张君楠张风太
Owner ENERGY RES INST OF SHANDONG ACAD OF SCI
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