CN102903916A - Preparation method of nickel-doped sodium ferrous fluorophosphate cathode material - Google Patents

Preparation method of nickel-doped sodium ferrous fluorophosphate cathode material Download PDF

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Publication number
CN102903916A
CN102903916A CN2012103798137A CN201210379813A CN102903916A CN 102903916 A CN102903916 A CN 102903916A CN 2012103798137 A CN2012103798137 A CN 2012103798137A CN 201210379813 A CN201210379813 A CN 201210379813A CN 102903916 A CN102903916 A CN 102903916A
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China
Prior art keywords
nickel
cathode material
preparation
sodium
positive electrode
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Pending
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CN2012103798137A
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Chinese (zh)
Inventor
崔立峰
王聪
王辉
杨克涛
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JIANGSU KING LITHIUM CELL CO Ltd
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JIANGSU KING LITHIUM CELL CO Ltd
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Priority to CN2012103798137A priority Critical patent/CN102903916A/en
Publication of CN102903916A publication Critical patent/CN102903916A/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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Abstract

The invention relates to a manufacturing technology of lithium ion batteries cathode materials, especially relates to a preparation method of a nickel-doped sodium ferrous fluorophosphate cathode material, comprising the following steps: a, weighing iron nitrate nonahydrate, sodium dihydrogen phosphate, sodium fluoride, glucose and nickel hydroxide according to a molar ratio of Fe:PO4<3->:F:C:Ni being 0.95:2:1:1:1:0.05, dissolving the weighed ingredients in anhydrous ethanol, and conducting ball milling in an agate jar for 3-4h; b, dissolving the milled product in anhydrous ethanol, and conducting vacuum drying at 70-85 DEG C; c, under the protection of inert gas, heating up to 580-600 DEG C, preserving the heat for 9-10h, then taking out the product and milling to obtain the nickel-doped sodium ferrous fluorophosphate cathode material. According to the invention, doping modification is carried out on the sodium ferrous fluorophosphate cathode material by solid phase method, thus the capacity and cycle performance of the cathode material is effectively raised.

Description

The preparation method of nickel doped with fluorine ferrous phosphate sodium positive electrode
Technical field
The present invention relates to the manufacturing technology of anode material for lithium-ion batteries, relate to a kind of preparation method of nickel doped with fluorine ferrous phosphate sodium positive electrode.
Background technology
The fluorophosphoric acid Naferon is known anode material for lithium-ion batteries, as anode material for lithium-ion batteries, there is the relatively poor defective of cyclicity, with it as anode material for lithium-ion batteries, usually the off-capacity 40% that circulates at normal temperatures 100 times can not satisfy the needs of high-performance lithium battery.
Summary of the invention
Technical problem to be solved by this invention is that providing a kind of can carry out modification to traditional fluorophosphoric acid Naferon positive electrode, improves the preparation method of the nickel doped with fluorine ferrous phosphate sodium positive electrode of circulating battery.
The preparation method of nickel doped with fluorine ferrous phosphate sodium positive electrode of the present invention may further comprise the steps:
A. press Fe:Na:PO 4 3-: the mol ratio of F:C:Ni=0.95:2:1:1:1:0.05 takes by weighing nine water ferric nitrates, sodium dihydrogen phosphate, sodium fluoride, glucose and nickel hydroxide and is dissolved in absolute ethyl alcohol, in the agate tank ball milling 3-4 hour;
B. the product behind the ball milling is dissolved in the absolute ethyl alcohol, 70-85 ℃ of lower vacuumize;
C. under inert gas shielding, be warming up to 580-600 ℃, take out after 9-10 hour in insulation and grind, make nickel doped with fluorine ferrous phosphate sodium positive electrode.
Among the above-mentioned steps c, heating rate is 5 ℃/min in the heating process.
The present invention carries out doping vario-property by solid phase method to fluorophosphoric acid Naferon positive electrode, Effective Raise capacity and the cycle performance of positive electrode.
Embodiment
The step of the embodiment of the inventive method is as follows:
Press Fe:Na:PO 4 3-: the mol ratio of F:C:Ni=0.95:2:1:1:1:0.05 takes by weighing nine water ferric nitrates, sodium dihydrogen phosphate, sodium fluoride, glucose and nickel hydroxide and is dissolved in absolute ethyl alcohol, and ball milling is 4 hours in the agate tank; Product is dissolved in the absolute ethyl alcohol, grinds after 80 ℃ of lower vacuumizes, then under inert gas shielding, be raised to 600 ℃ with the heating rate of 5 ℃/min, after 600 ℃ of lower insulations were taken out after 10 hours, grind, make nickel doped with fluorine ferrous phosphate sodium positive electrode.The material property that obtains is as follows:
Discharge capacity discharge capacity 〉=120mAh/g first first;
Efficient 〉=85% first;
Circulation is 100 times under the normal temperature, capability retention>80%;
50 ℃ of lower circulations of high temperature 100 times, capability retention>60%.

Claims (2)

1. the preparation method of a nickel doped with fluorine ferrous phosphate sodium positive electrode is characterized in that: may further comprise the steps,
A. press Fe:Na:PO 4 3-: the mol ratio of F:C:Ni=0.95:2:1:1:1:0.05 takes by weighing nine water ferric nitrates, sodium dihydrogen phosphate, sodium fluoride, glucose and nickel hydroxide and is dissolved in absolute ethyl alcohol, in the agate tank ball milling 3-4 hour;
B. the product behind the ball milling is dissolved in the absolute ethyl alcohol, 70-85 ℃ of lower vacuumize;
C. under inert gas shielding, be warming up to 580-600 ℃, take out after 9-10 hour in insulation and grind, make nickel doped with fluorine ferrous phosphate sodium positive electrode.
2. the preparation method of nickel doped with fluorine ferrous phosphate sodium positive electrode according to claim 1, it is characterized in that: among the step c, heating rate is 5 ℃/min in the heating process.
CN2012103798137A 2012-10-09 2012-10-09 Preparation method of nickel-doped sodium ferrous fluorophosphate cathode material Pending CN102903916A (en)

Priority Applications (1)

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CN2012103798137A CN102903916A (en) 2012-10-09 2012-10-09 Preparation method of nickel-doped sodium ferrous fluorophosphate cathode material

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Application Number Priority Date Filing Date Title
CN2012103798137A CN102903916A (en) 2012-10-09 2012-10-09 Preparation method of nickel-doped sodium ferrous fluorophosphate cathode material

Publications (1)

Publication Number Publication Date
CN102903916A true CN102903916A (en) 2013-01-30

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108832112A (en) * 2018-06-26 2018-11-16 东北大学秦皇岛分校 A kind of preparation method of cobalt doped fluorophosphoric acid Naferon positive electrode
CN110931781A (en) * 2019-10-14 2020-03-27 桂林理工大学 Preparation method and application of biomass carbon/sodium iron fluorophosphate composite material
WO2021036791A1 (en) * 2019-08-28 2021-03-04 宁德时代新能源科技股份有限公司 Positive electrode material for sodium ion battery, preparation method therefor and related sodium ion battery, battery module, battery pack and device thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102126714A (en) * 2011-01-12 2011-07-20 山西泰众新能源有限公司 Preparation method of lithium iron phosphate with high tap density
CN102509789A (en) * 2011-10-17 2012-06-20 中南大学 Method for preparing positive material fluorine-doped sodium vanadium phosphate of sodium-containing lithium ion battery

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102126714A (en) * 2011-01-12 2011-07-20 山西泰众新能源有限公司 Preparation method of lithium iron phosphate with high tap density
CN102509789A (en) * 2011-10-17 2012-06-20 中南大学 Method for preparing positive material fluorine-doped sodium vanadium phosphate of sodium-containing lithium ion battery

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
BRIAN L. ELLIS ET AL: "Crystal Structure and Electrochemical Properties of A2MPO4F Fluorophosphates (A=Na,Li;M=Fe,Mn,Co,Ni)", 《CHEMISTRY OF MATERIALS》, vol. 22, no. 3, 13 November 2009 (2009-11-13) *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108832112A (en) * 2018-06-26 2018-11-16 东北大学秦皇岛分校 A kind of preparation method of cobalt doped fluorophosphoric acid Naferon positive electrode
CN108832112B (en) * 2018-06-26 2020-07-03 东北大学秦皇岛分校 Preparation method of cobalt-doped sodium ferrous fluorophosphate cathode material
WO2021036791A1 (en) * 2019-08-28 2021-03-04 宁德时代新能源科技股份有限公司 Positive electrode material for sodium ion battery, preparation method therefor and related sodium ion battery, battery module, battery pack and device thereof
EP3968410A4 (en) * 2019-08-28 2022-08-17 Contemporary Amperex Technology Co., Limited Positive electrode material for sodium ion battery, preparation method therefor and related sodium ion battery, battery module, battery pack and device thereof
CN110931781A (en) * 2019-10-14 2020-03-27 桂林理工大学 Preparation method and application of biomass carbon/sodium iron fluorophosphate composite material

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Application publication date: 20130130