CN103496741B - A kind of solid phase reaction method prepares Li 3vO 4negative material - Google Patents
A kind of solid phase reaction method prepares Li 3vO 4negative material Download PDFInfo
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- CN103496741B CN103496741B CN201310440371.7A CN201310440371A CN103496741B CN 103496741 B CN103496741 B CN 103496741B CN 201310440371 A CN201310440371 A CN 201310440371A CN 103496741 B CN103496741 B CN 103496741B
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- Y—GENERAL 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides with vanadic oxide and lithium carbonate as precursor prepares Novel cathode material for lithium ion battery Li
3vO
4.Its principle make use of high-temperature heating and provides reaction energy for reaction raw materials, makes reaction raw materials gradually solid phase reaction occur, and finally obtains the Li that crystal property is good
3vO
4.This Li
3vO
4material first charge and discharge capacity be respectively 1002,739mAh/g, after 50 circulations charge and discharge capacity be respectively 639,643mAh/g, its mean particle size is 5um, and particle is made up of the granule being about 300nm of taking measurements greatly.
Description
Technical field
The present invention relates to a class Novel cathode material for lithium ion battery, particularly a kind of Li
3vO
4preparation method and storage lithium characteristic, belong to field of electrochemical power source.
Background technology
Lithium ion battery is the third generation small battery after nickel-cadmium cell, Ni-MH battery, there is the advantages such as operating voltage is high, specific energy large, discharge potential curve is steady, self discharge is little, have extended cycle life, cryogenic property is good, memoryless, pollution-free, portable type electronic product miniaturization, lightweight, free of contamination requirement can be met.Current lithium ion battery has been widely used in the electronic product such as mobile communication, notebook computer, but as the power supply of the such as mobile device such as electric vehicle, artificial satellite, field operations communication, also needs the specific energy and the power that improve battery further.The key of research and development high-energy-density, high power lithium ion cell is to design and prepares the electrode material of high power capacity, high rate capability.At present, positive electrode is generally containing lithium transition group metallic oxide (LiCoO
2, LiFePO
4, LiN
1-y-zmn
yco
zo
zdeng), the possibility that existing cathode material structure basis increases substantially positive electrode specific capacity is little, improves the significantly raising that capacity of lithium ion battery can only rely on negative material capacity further.Traditional graphite cathode material density is lower, and volume capacity is lower, and therefore, research and development Novel cathode material for lithium ion battery becomes the key factor affecting lithium ion battery development.Ternary lithium, vfanadium compound system show good chemical property as lithium ion battery electrode material, thus receive and study comparatively widely and pay close attention to.Wherein, Li
3vO
4be ternary lithium, the barium oxide that a kind of relative molecular weight is less, be expected to show higher theoretical capacity as lithium ion battery electrode material, at present, about the research of its chemical property, there is not been reported.Based on above research background, this patent relates to a kind of straightforward procedure of invention and prepares novel tertiary compound L i
3vO
4material, shows excellent stable circulation performance using it as lithium ion battery negative.
Summary of the invention
Object of the present invention with vanadic oxide and lithium carbonate for precursor prepares Novel cathode material for lithium ion battery Li
3vO
4.Its principle make use of high-temperature heating and provides reaction energy for reaction raw materials, makes reaction raw materials gradually solid phase reaction occur, and finally obtains the Li that crystal property is good
3vO
4.
Li involved in the present invention
3vO
4synthesis material is vanadic oxide and lithium carbonate, and the reaction occurred in solid phase reaction process is:
V
2O
5+3Li
2CO
3→2Li
3VO
4+3CO
2↑(1)
In material preparation process, first by vanadic oxide and lithium carbonate in molar ratio 1:2-5 take mixing, ball milling was placed in heating container after 1 hour, was heated to 400 ~ 700 DEG C of reactions 1 ~ 10 hour under air conditions, naturally cooled and can obtain Li
3vO
4sample.
Li involved in the present invention
3vO
4negative material and preparation method have following outstanding feature:
(1) Li
3vO
4first charge and discharge capacity be respectively 1002,739mAh/g, after 50 circulations charge and discharge capacity be respectively 639,643mAh/g;
(2) synthesis technique is simple, and be easy to operation, material preparation cost is low;
(3) gained sample purity is high, and crystal property is good;
(4) prepared material capacity is high, and cycle performance is excellent;
(5) Li
3vO
4mean particle size is 5um, and particle is made up of the granule being about 300nm of taking measurements greatly.
accompanying drawing illustrates:
Li prepared by Fig. 1 embodiment 1
3vO
4xRD collection of illustrative plates;
The SEM figure of Fig. 2 embodiment 1;
The discharge curve (a) first of Fig. 3 embodiment 1 and cycle performance figure (b), wherein current density 0.1mAcm
-2.
embodiment:
Embodiment 1
Be that 1:3 takes and mixes by vanadic oxide and lithium carbonate with mol ratio, ball milling 1 hour, is transferred in crucible or quartz boat, moves in high temperature process furnances, calcine crucible or quartz boat 5 hours under 500 DEG C of conditions, in air, naturally cools and can obtain Li
3vO
4sample.Result shows, prepared sample is Li through XRD atlas analysis
3vO
4, as shown in Figure 1, diffraction maximums all in figure and the Li of rhombic system
3vO
4correspondence, lattice constant is
a=0.6319nm, b=0.5448nm,
c=0.4940nm, corresponding to XRD card JCPDS, No.38-1247; Strong and sharp-pointed diffraction maximum shows, prepared Li
3vO
4crystal property is good.Diffraction maximum without other materials is detected, and shows that prepared sample purity is very high.Prepared Li
3vO
4through SEM scanning, as seen from Figure 2, prepared Li
3vO
4mean particle size is 5um.Particle is made up of the granule being about 300nm of taking measurements greatly.With prepared Li
3vO
4particle shows as lithium ion battery negative material that charge and discharge capacity is first 739,1002mAh/g, after 50 circulations charge and discharge capacity be respectively 639,643mAh/g, show fabulous stable circulation performance (as shown in Figure 3).
Embodiment 2
Be that 1:2 takes and mixes by vanadic oxide and lithium carbonate with mol ratio, ball milling 1 hour, is transferred in crucible or quartz boat, moves in high temperature process furnances, calcine crucible or quartz boat 7 hours under 400 DEG C of conditions, in air, naturally cools and can obtain Li
3vO
4sample.
Embodiment 3
Be that 1:5 takes and mixes by vanadic oxide and lithium carbonate with mol ratio, ball milling 1 hour, is transferred in crucible or quartz boat, moves in high temperature process furnances, calcine crucible or quartz boat 6 hours under 700 DEG C of conditions, in air, naturally cools and can obtain Li
3vO
4sample.
Embodiment 4
Be that 1:3 takes and mixes by vanadic oxide and lithium carbonate with mol ratio, ball milling 1 hour, is transferred in crucible or quartz boat, moves in high temperature process furnances, calcine crucible or quartz boat 9 hours under 600 DEG C of conditions, in air, naturally cools and can obtain Li
3vO
4sample.
Claims (1)
1. the Li that a solid reaction process is obtained
3vO
4as Li
3vO
4the application of negative material on lithium ion battery, is characterized in that: prepared Li
3vO
4lattice constant be
a=0.6319nm,
b=0.5448nm,
c=0.4940nm, Li
3vO
4mean particle size is 5 μm, and particle is made up of the granule being of a size of 300nm in a large number; Specifically comprise the steps:
Be that 1:3 takes and mixes by vanadic oxide and lithium carbonate with mol ratio, ball milling 1 hour, is transferred in crucible or quartz boat, moves in high temperature process furnances, calcine crucible or quartz boat 5 hours under 500 DEG C of conditions, in air, naturally cools and can obtain Li
3vO
4sample, prepared Li
3vO
4show as lithium ion battery negative material that charge and discharge capacity is first 739,1002mAh/g, after 50 circulations charge and discharge capacity be respectively 639,643mAh/g.
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|---|---|---|---|
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| CN201310440371.7A CN103496741B (en) | 2013-09-25 | 2013-09-25 | A kind of solid phase reaction method prepares Li 3vO 4negative material |
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| CN103496741B true CN103496741B (en) | 2015-12-23 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104124446A (en) * | 2014-07-01 | 2014-10-29 | 三峡大学 | Graphite/Li3VO4 lithium ion battery composite negative electrode material and preparation method thereof |
| CN104393241B (en) * | 2014-11-14 | 2016-06-01 | 三峡大学 | The preparation method of a kind of lithium ion battery negative material |
| CN104409713B (en) * | 2014-11-14 | 2017-02-22 | 三峡大学 | Novel lithium ion battery anode material and preparation method thereof |
| CN105810928B (en) * | 2014-12-30 | 2019-02-22 | 微宏动力系统（湖州）有限公司 | A kind of lithium ion secondary battery two-phase negative electrode material and preparation method thereof |
| CN105133016B (en) * | 2015-10-09 | 2018-10-16 | 新疆大学 | The preparation method and purposes of lithium vanadate nonlinear optical crystal |
| CN106299356B (en) * | 2016-09-27 | 2019-06-21 | 苏州科技大学 | A kind of lithium ion battery lithium vanadate Li3VO4The efficient microwave radiation synthesis process of nano flower |
| CN106299301B (en) * | 2016-09-27 | 2019-06-18 | 苏州科技大学 | A kind of Li with excellent storage lithium performance3VO4The pattern of nano wire mutually regulates and controls method with object |
| CN110294494B (en) * | 2019-07-25 | 2022-04-01 | 哈尔滨工业大学 | Lithium vanadate anode lithium supplement additive and application thereof |
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| CN103145419A (en) * | 2013-04-01 | 2013-06-12 | 桂林理工大学 | Microwave dielectric ceramic Li3VO4 capable of being sintered at low temperature and preparation method thereof |
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| CN101853939A (en) * | 2009-03-31 | 2010-10-06 | 比亚迪股份有限公司 | Cathodic active material as well as preparation method and battery thereof |
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Effective date of registration: 20221118 Address after: 405400 Chongqing Kai Zhou Industrial Park, Zhao Jia light industrial food industry park No. 5 standard workshop. Patentee after: CHONGQING JIABAOCHENG ENERGY TECHNOLOGY Co.,Ltd. Address before: 443002 No. 8, University Road, Yichang, Hubei Patentee before: CHINA THREE GORGES University |