CN108565426A - Li3VO4/LiVO2Composite lithium ion battery cathode material and preparation method thereof - Google Patents
Li3VO4/LiVO2Composite lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN108565426A CN108565426A CN201810339008.9A CN201810339008A CN108565426A CN 108565426 A CN108565426 A CN 108565426A CN 201810339008 A CN201810339008 A CN 201810339008A CN 108565426 A CN108565426 A CN 108565426A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The present invention provides a kind of Li3VO4/LiVO2The preparation method of composite lithium ion battery cathode material, specifically by lithium carbonate, vanadic anhydride and hexamethylenetetramine mixed dissolution in the beaker equipped with 35ml absolute ethyl alcohols, and quickly stirring 1h makes each component be sufficiently mixed;Obtained mixed solution is transferred in water heating kettle liner, 10 ~ 30h is reacted in 100 DEG C ~ 180 DEG C convection ovens, cooled to room temperature obtains interphase product, is made of supernatant liquid and lower sediment;The supernatant liquor in interphase product is isolated, this supernatant liquor is placed in 60 ~ 85 DEG C of baking ovens and is dried, it is in faint yellow to be ground to powder, and calcining 5 ~ 10h at 450 ~ 650 DEG C in nitrogen or argon atmosphere obtains composite material.The material is applied on lithium ion battery negative material by the present invention, it is shown that preferable chemical property.
Description
Technical field
The present invention relates to a kind of novel cathode material for lithium ion batteries, more particularly to Li3VO4/LiVO2Composite negative pole
Material belongs to field of electrochemical power source.
Technical background
In recent years, it as the fast development of lithium-ion battery system, application field are constantly widened, is set by portable electronic
Standby field is gradually extended to the fields such as electric vehicle and extensive energy storage engineering, this undoubtedly proposes lithium ion battery higher
It is required that.The lithium ion battery negative material important role of performer in the battery.Currently, commercialized negative electrode of lithium ion battery is
Graphite-like carbon material, Li4Ti5O12, but the two has been difficult to meet mesh in energy density, security performance, cycle life etc.
The preceding market demand.Development has both the novel high property of high-energy density, high safety performance, long circulation life and environmental-friendly feature
Energy lithium-ion battery system is the following only way.Positive electrode type relative abundance, and develop more mature, negative material
System is more single, and the research and development of negative material are most important for Development of Novel high performance lithium ion battery system.
Li3VO4It is a kind of novel insertion/deintercalation type negative material, intercalation potential concentrates on 0.5 ~ 1.0 V, fills, puts
Motor is managed:xLi+ + Li3VO4 + xe-↔ Li3+xVO4(x≤3).With commercialized graphite(372mAh/g)It compares, has
Higher theoretical capacity capacity(592 mAh/g)With the discharge platform of safety, compared to Li4Ti5O12(175mAh/g)There is higher
Theoretical capacity and lower discharge platform, realize the unification of security performance and energy density, great research and practical value.
Promote Li3VO4The major way of negative material performance is to enhance its electric conductivity and lithium ion diffuser efficiency.Tradition improves Li3VO4
The method of electric conductivity is mainly compound with carbon material such as graphene, natural graphite, agraphitic carbon etc., but this compound it is difficult to simultaneously
It influences the particle size of material and then improves its lithium ion diffuser efficiency.LiVO2Itself it also can be used as a kind of negative material, and its
Electric conductivity is far above Li3VO4.By adjusting Li, V ratio in reaction raw materials and regulating and controlling reaction environment, it is expected to obtain Li3VO4/
LiVO2Composite material.High conductance LiVO2It mutually can enhance composite material monolithic conductive performance, while effectively inhibit Li3VO4It is being sintered
Grain growth in the process promotes its lithium ion diffuser efficiency, gained Li3VO4/LiVO2Composite material is expected to obtain excellent electrification
Learn performance.For this purpose, this patent has developed a kind of Li based on solvent heat3VO4/LiVO2Composite material and preparation method thereof utilizes solvent
Ingredient and the distribution for adjusting intermediate phase precursor, Li is obtained in conjunction with solid-phase sintering3VO4With LiVO2Equally distributed Li3VO4/
LiVO2Composite material.
Invention content
A kind of composite lithium ion battery cathode material involved in the present invention, the negative material are Li3VO4/LiVO2Composite wood
Material, the material are graininess.Specific preparation method, steps are as follows:Lithium carbonate, vanadic anhydride and hexamethylenetetramine are distinguished
It is dissolved in the beaker of absolute ethyl alcohol, and quickly stirring makes each component be sufficiently mixed, and obtains mixed solution;Obtained mixing is molten
Liquid is transferred in water heating kettle liner, and 5 ~ 30h is reacted in 100 DEG C ~ 180 DEG C convection ovens, and cooled to room temperature is reacted
Object;Then the supernatant liquor in the reactant obtained is isolated, this supernatant liquor is placed in 60 ~ 85 DEG C of baking ovens and is dried, grinding
It is in faint yellow to powder, calcining 5 ~ 10h at 450 ~ 650 DEG C in nitrogen or argon atmosphere obtains composite material.
The molar ratio of above-mentioned lithium, vanadium and hexamethylenetetramine is 1 ~ 5:1:2 ~ 10, solvent hot solvent is absolute ethyl alcohol.
Li3VO4Itself has extremely strong water solubility, it is difficult to be directly obtained by hydro-thermal method.It can be obtained by solvent thermal reaction
To the lower Li of yield3VO4, most Li, V are still dissolved in solvent.The principle of this patent is exactly to utilize alcohol solvent heat
The evenly dispersed interphase solution of Li, V is prepared in reaction.Using the reproducibility of ethyl alcohol to V5+It carries out appropriate in-situ reducing and combines
At soluble precursor.Meanwhile the special dispersion performance promotion each ingredient of interphase of ethyl alcohol is evenly dispersed.Then sintered
Cheng Zhong is obtained by solid phase reaction with V5+And V3+Li3VO4/LiVO2Composite material.
Li according to the present invention3VO4/LiVO2Preparation method, material and the performance of composite material have following aobvious
The characteristics of work:
1)Synthesis technology is simple, easily operated, and controllability is good;
2)Prepared Li3VO4/LiVO2Composite material granular size is smaller, about 100 nm.Wherein, Li3VO4With LiVO2It is compound
Uniformly.
3)Li obtained by the present invention3VO4/LiVO2Composite material, which is used as lithium ion battery negative material, has higher appearance
Amount, lower charge and discharge platform and good cycle performance.
Description of the drawings
The XRD spectrum of sample prepared by Fig. 1 embodiments 1.
The SEM of sample prepared by Fig. 2 embodiments 1 schemes.
The preceding charge and discharge curve graph three times of sample prepared by Fig. 3 embodiments 1(a), cycle performance figure(b).
The cycle performance figure of sample prepared by Fig. 4 embodiments 2.
The cycle performance figure of sample prepared by Fig. 5 embodiments 3.
Specific implementation mode:
Embodiment 1
Steps are as follows for materials synthesis:
(1)By lithium carbonate, vanadic anhydride and hexamethylenetetramine are according to molar ratio 4:1:5 weigh 4mmol respectively, 1mmol and
5mmol is dissolved in the beaker equipped with 35ml absolute ethyl alcohols, and quickly stirring 1h makes each component be sufficiently mixed, and it is uniform to obtain color
Solution;
(2)By step(1)In obtained mixed solution be transferred in water heating kettle liner, reacted in 120 DEG C of convection ovens for 24 hours,
Cooled to room temperature obtains reactant;
(3)By step(2)In supernatant liquor in obtained reactant isolate, this supernatant liquor is placed in 70 DEG C of baking ovens and is dried
Dry, it is in faint yellow to be ground to powder, and calcining 5h at 500 DEG C in nitrogen protection atmosphere obtains composite material.
By prepared Li3VO4/LiVO2Composite sample carries out XRD tests, as shown in Figure 1.It is located at 44.5 in figureo
With Li3VO4's(051)Crystal face corresponds to, and is located at 64.2oWith LiVO2's(440)Crystal face corresponds to, and test result shows prepared
Sample is Li3VO4And LiVO2Mixture, correspond to Li3VO4XRD card JCPDS, no.24-0666 correspond to LiVO2XRD
Card JCPDS, no.36-0041.The pattern of prepared sample is via sem analysis, as shown in Fig. 2, prepared sample is in particle
Shape.Battery is made in the material of 1 gained of embodiment as follows:By Li obtained3VO4/LiVO2Composite sample and second
Acetylene black and Kynoar are 8 by weight:1:1 ratio mixing, is made slurry by solvent of N- first class pyrrolidones, coats
On the copper foil of 10 μ m thicks, after dry at 60 DEG C, it is cut into the disk of 14mm, 12h is dried in vacuo at 120 DEG C.With gold
It is to electrode to belong to lithium foil, and Celgard 2400 is diaphragm, 1 M LiPF6/DMC: EC=1:1 solution is electrolyte, is protected in argon gas
CR2025 type batteries are assembled into the glove box of shield.Battery pack stands 8h after installing, then is carried out with CT2001A battery test systems
Constant current charge-discharge test, test voltage are 3 ~ 0.02V.Fig. 3 is prepared Li3VO4/LiVO2Composite material is as lithium-ion electric
The specific capacity of charge and discharge for the first time that pond negative material is shown is respectively 573.9,931mAh/g, charge and discharge specific volume after 40 cycles
Amount is respectively 486.9,494.7mAh/g, it is shown that good stable circulation performance.
Embodiment 2
Steps are as follows for materials synthesis:
(1)By lithium carbonate, vanadic anhydride and hexamethylenetetramine are according to molar ratio 2:1:5 weigh 2mmol respectively, 1mmol and
5mmol is dissolved in the beaker equipped with 35ml absolute ethyl alcohols, and quickly stirring 1h makes each component be sufficiently mixed, and it is uniform to obtain color
Solution;
(2)By step(1)In obtained mixed solution be transferred in water heating kettle liner, reacted in 140 DEG C of convection ovens for 24 hours,
Cooled to room temperature obtains reactant;
(3)By step(2)In supernatant liquor in obtained reactant isolate, this supernatant liquor is placed in 70 DEG C of baking ovens,
Until drying, it is in faint yellow to be ground to powder, and calcining 5h at 550 DEG C in nitrogen protection atmosphere obtains composite material.
Battery is made by method described in embodiment 1 in the material of 2 gained of embodiment.Fig. 4 is prepared Li3VO4/
LiVO2Composite material is respectively 509.5,887mAh/ as the specific capacity of charge and discharge for the first time that lithium ion battery negative material is shown
G, 40 times cycle after charge and discharge specific capacity be respectively 482.9,488.4mAh/g, it is shown that good stable circulation performance.
Embodiment 3
Steps are as follows for materials synthesis:
(1)By lithium carbonate, vanadic anhydride and hexamethylenetetramine are according to molar ratio 1:1:5 weigh 1mmol respectively, 1mmol and
5mmol is dissolved in the beaker equipped with 35ml absolute ethyl alcohols, and quickly stirring 1h makes each component be sufficiently mixed, and it is uniform to obtain color
Solution;
(2)By step(1)In obtained mixed solution be transferred in water heating kettle liner, reacted in 160 DEG C of convection ovens for 24 hours,
Cooled to room temperature obtains reactant;
(3)By step(2)In supernatant liquor in obtained reactant isolate, this supernatant liquor is placed in 70 DEG C of baking ovens,
Until drying, it is in faint yellow to be ground to powder, and calcining 5h at 600 DEG C in argon atmosphere obtains composite material.
Battery is made by method described in embodiment 1 in the material of 3 gained of embodiment.Fig. 5 is prepared Li3VO4/
LiVO2Composite material as the specific capacity of charge and discharge for the first time that lithium ion battery negative material is shown is respectively 433.8,
721.1mAh/g, charge and discharge specific capacity is respectively 397.5,397.6mAh/g after 40 cycles, it is shown that cycle is steady well
Qualitative energy.
Claims (4)
1. a kind of composite lithium ion battery cathode material, which is characterized in that the composite negative pole material ingredient is Li3VO4/LiVO2。
2. a kind of preparation method of composite cathode material for lithium ion cell, its step are as follows:
(1)By lithium carbonate, vanadic anhydride and hexamethylenetetramine mixed dissolution in absolute ethyl alcohol, and stirring makes each component fill
Divide mixing, obtains mixed solution;
(2)By step(1)In obtained mixed solution be transferred in water heating kettle liner, it is anti-in 100 DEG C ~ 180 DEG C convection ovens
5 ~ 30h, cooled to room temperature is answered to obtain reactant;
(3)By step(2)In supernatant liquor in obtained reactant isolate, supernatant liquor drying is ground to powder in light
Yellow calcines in nitrogen or argon atmosphere and obtains Li3VO4/LiVO2Composite material.
3. lithium ion battery Li according to claim 23VO4/LiVO2The preparation method of composite negative pole material, feature exist
In, lithium carbonate, the molar ratio of vanadic anhydride and hexamethylenetetramine is 1 ~ 5:1:2~10.
4. lithium ion battery Li according to claim 23VO4/LiVO2The preparation method of composite negative pole material, feature exist
In the drying temperature of the supernatant liquor is 60-85 DEG C;Calcination temperature is 450-650 DEG C, calcination time 5-10h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111834624A (en) * | 2020-07-28 | 2020-10-27 | 湖南工学院 | Two-dimensional LiV3O8Graphene composite material and preparation method and application thereof |
CN114684783A (en) * | 2022-04-11 | 2022-07-01 | 浙江大学 | Additive capable of improving hydrogen storage performance of lithium magnesium nitrogen hydride and preparation and application thereof |
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CN103474641A (en) * | 2013-09-25 | 2013-12-25 | 三峡大学 | Lithium ion battery anode material Li3VO4 and preparation method thereof |
CN104201340A (en) * | 2014-08-22 | 2014-12-10 | 东莞市迈科科技有限公司 | Preparation method of lithium ion battery material lithium vanadate |
CN107623111A (en) * | 2017-08-10 | 2018-01-23 | 三峡大学 | A kind of composite lithium ion battery cathode material Li3VO4/ Ag and preparation method thereof |
CN107845781A (en) * | 2016-09-19 | 2018-03-27 | 微宏动力系统(湖州)有限公司 | Lithium ion secondary battery cathode active material, its preparation method and lithium rechargeable battery |
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US20130168611A1 (en) * | 2010-10-27 | 2013-07-04 | Ocean's King Lighting Science & Technology Co., Ltd., | Composite electrode material, manufacturing method and application thereof |
CN103474641A (en) * | 2013-09-25 | 2013-12-25 | 三峡大学 | Lithium ion battery anode material Li3VO4 and preparation method thereof |
CN104201340A (en) * | 2014-08-22 | 2014-12-10 | 东莞市迈科科技有限公司 | Preparation method of lithium ion battery material lithium vanadate |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111834624A (en) * | 2020-07-28 | 2020-10-27 | 湖南工学院 | Two-dimensional LiV3O8Graphene composite material and preparation method and application thereof |
CN114684783A (en) * | 2022-04-11 | 2022-07-01 | 浙江大学 | Additive capable of improving hydrogen storage performance of lithium magnesium nitrogen hydride and preparation and application thereof |
CN114684783B (en) * | 2022-04-11 | 2023-04-14 | 浙江大学 | Additive capable of improving hydrogen storage performance of lithium magnesium nitrogen hydride and preparation and application thereof |
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