Lithium ion phosphate positive electrode material of nanometer core shell structure and preparation method thereof

A positive electrode material, lithium iron phosphate technology, applied in the direction of structural parts, battery electrodes, electrical components, etc., can solve the problems of uneven materials, reduced compaction density, and reduced powder processing and use effects

Inactive Publication Date: 2012-04-18
SHANGHAI PYLON TECH CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, lithium iron phosphate also has obvious deficiencies. The low theoretical density leads to a reduction in the tap density of the powder and the compaction density during powder processing, especially carbon coating and nanonization will lead to powder agglomeration and material Inhomogeneity and other problems reduce the processing and use effect of powder again; at the same time, the large-scale production of powder is also more difficult due to the problem of primary particle shape and particle size control, and faces the substantive problem of unstable product batches
[0004] For the stable control of the morphology and particle size of lithium iron phosphate particles, researchers usually use methods such as controlling the morphology and particle size of the precursor mixture, strengthening the mixing and grinding conditions of the precursor (such as multi-stage pulverization of powder), and optimizing the sintering system; using these method, the secondary morphology of the powder can be better controlled, but because it is difficult to ensure the stability of the primary particle and its polymerization state, it has little effect on the stability of the batch of products produced on a large scale [WO03 / 088383A1; CN1547273A; CN101150191A ], and will significantly increase the energy consumption cost of the preparation process; while using methods such as hydrothermal synthesis and liquid phase precipitation [CN101159328A; CN101327922A], the primary morphology is stable and controllable, but it is difficult to scale production, and the cost of equipment and process control are higher

Method used

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  • Lithium ion phosphate positive electrode material of nanometer core shell structure and preparation method thereof
  • Lithium ion phosphate positive electrode material of nanometer core shell structure and preparation method thereof
  • Lithium ion phosphate positive electrode material of nanometer core shell structure and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] With Fe(NO 3 ) 3 9H 2 O. Li 3 PO 4 , NH 4 h 2 PO 4 It is the raw material of positive electrode material, and citric acid C6H8O7 is used as the precursor of porous carbon structure and nano-carbon layer. The ratio of lithium source, iron source, phosphorus source and citric acid is according to Li:Fe:P:citric acid=1:1:1 : 5 (molar ratio) for weighing, Fe(NO 3 ) 3 9H 2 O 1.212kg (about 3mol), Li 3 PO 4 0.12kg (about 1mol), NH 4 h 2 PO 4 0.230kg (about 2mol), citric acid 1kg (about 5mol), mix well and control the order of addition (dissolve the ammonium salt NH first 4 h 2 PO 4 , citric acid C6H8O7), then add 10L-20L deionized water, stir vigorously for 10-90min, then add Fe(NO 3 ) 3 9H 2 O. Li 3 PO 4 The mixed solution was fully stirred and dissolved to obtain a reddish-brown transparent solution. Use an appropriate amount of ammonia water to adjust the pH to 1, then place the solution in an electric blast oven, and dry it at 150°C for 3 hours to ...

Embodiment 2

[0043] With Fe(NO 3 ) 3 9H 2 O, LiOH·H 2 O, NH 4 h 2 PO 4 As the raw material of the positive electrode material, Al(NO 3 ) 3 9H 2 O is the precursor of the porous structure. Experiments were carried out with citric acid C6H8O7 and ethylene glycol as the precursor of the nano-carbon layer. The ratio of lithium source, iron source, phosphorus source, aluminum source and citric acid is weighed according to Li: Fe: P: Al: citric acid = 1: 0.95: 0.05: 5 (molar ratio), Fe(NO 3 ) 3 9H 2 O 1.212kg (about 3mol), LiOH·H 2 O0.36kg (about 3mol), NH 4 h 2 PO 4 0.345kg (about 3mol), Al(NO 3 ) 3 9H 2 O 0.056kg (about 0.015mol), citric acid 0.9kg (about 4.4mol), mix well and control the order of addition (dissolve the ammonium salt NH first 4 h 2 PO 4 , citric acid C6H8O7), then add 10L-20L deionized water, stir vigorously for 10-90min, then add Fe(NO 3 ) 3 9H 2 O, LiOH·H 2 O, Al(NO 3 )3 9H 2 The mixed solution of O was fully stirred and dissolved to obtain a reddi...

Embodiment 3

[0047] FePO 4 2H 2 O. Li 2 CO 3 As raw material, control Li:Fe:P molar ratio to 1:1:1, weigh FePO 4 2H 2 O0.370kg (about 2mol), weigh Li 2 CO 3 0.220kg (about 1mol), typically 35%, with 1.2kg of ethanol as a solvent, add 180g of commercial carbon airgel that is fully pulverized, add surfactants, 50g of oleic acid, 10g of PVA (polyvinyl alcohol), ethylene glycol Alcohol 50g, after high-speed dispersion, let it stand for 30 minutes to fully impregnate the slurry and airgel, and the impregnation time is controlled at 30 minutes. After the impregnation process is completed, the pH value of the slurry is adjusted to 6, and the suspension system is destroyed and separated into layers. After pouring and separating the solvent, it is dried by electric heating at 50 degrees for 8 hours, and the mixture is calcined. Place it in an atmosphere furnace for high-temperature calcination, the protective atmosphere is 3L / min of high-purity nitrogen, the heating rate is 10°C / min, and it...

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Abstract

The invention discloses a lithium ion phosphate positive electrode material of a nanometer core shell structure. The positive electrode material is provided with an inner core active material and a conductive outer shell structure; a conductive agent is an outer shell material; the active material is of an inner core structure; and the structure formula of the inner core active material is LiFe[1-x]MxP[1-y]AyO4, wherein x is greater than or equal to 0, y is less than or equal to 0.1, M is a transition metal element, and A is silicon. Additionally, the invention also discloses a preparation method of the lithium ion phosphate positive electrode material. According to the preparation method in the invention, a porous material is adopted as a synthesis microreactor, and a lithium ion phosphate precursor is loaded and filled in holes, namely, the inner core active precursor reversely wraps a porous precursor so as to form a special nanometer core shell structure, thus the topography granularity of primary granule is controlled; and the lithium ion phosphate positive electrode material of the nanometer core shell structure is prepared by adopting a liquid phase mixed material and solid phase sintering technology. According to the invention, on the premise that the electrical performance of the positive electrode material is not influenced, a nanometer core shell structured active substance with uniform and controllable topography and granularity is synthesized; and the preparation method disclosed by the invention has lower technology, devices and control costs, which is beneficial to large-scale production.

Description

technical field [0001] The invention relates to a lithium ion secondary battery positive electrode material, which is used in the field of energy materials; in particular, it relates to a lithium iron phosphate positive electrode material with a nano-core-shell structure with controllable morphology and particle size; in addition, the invention also relates to the preparation of a porous material The invention relates to a lithium iron phosphate cathode material with a nano core-shell structure. Background technique [0002] The lithium iron phosphate material has outstanding characteristics such as environmental protection, excellent cycle performance and safety performance; the electrical conductivity of the lithium iron phosphate material after carbon coating, nanometerization, and ion doping modification is greatly improved [WO2007 / 0649934A2; CN101636861A; CN100517817C] , so that the stability and life of high-rate discharge are much higher than traditional mature lithiu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 王科伟田强陈小刚安静张军
Owner SHANGHAI PYLON TECH CO LTD
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