CN104993116B - A kind of self assembly anode material for lithium-ion batteries V2O5Preparation method - Google Patents

A kind of self assembly anode material for lithium-ion batteries V2O5Preparation method Download PDF

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CN104993116B
CN104993116B CN201510254129.XA CN201510254129A CN104993116B CN 104993116 B CN104993116 B CN 104993116B CN 201510254129 A CN201510254129 A CN 201510254129A CN 104993116 B CN104993116 B CN 104993116B
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lithium
ion batteries
anode material
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CN104993116A (en
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黄剑锋
乔晓宁
许占位
欧阳海波
李嘉胤
孔新刚
卢静
王瑞谊
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Shenzhen Zhongyuda Machinery Co ltd
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Shaanxi University of Science and Technology
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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • 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
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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

Abstract

A kind of self assembly anode material for lithium-ion batteries V2O5Preparation method, by by ammonium metavanadate and dissolving oxalic acid in deionized water, then a certain amount of diethylenetriamine or ethylenediamine are added, suspension is made under ultrasound condition, suspension is centrifuged again, presoma is dried to obtain, presoma is heat-treated again, anode material for lithium-ion batteries V is obtained2O5Compared with 600 DEG C of the prior art calcinings and solvent-thermal method, it is heat-treated in the present invention at 250 DEG C~450 DEG C, it is seen that reaction condition of the invention is gentle; energy consumption is smaller; it is easily achieved, beneficial to large-scale production, and because the present invention is without using template; so preparation process is simple; cost is relatively low, and process is easily-controllable, environmentally friendly.V produced by the present invention2O5First discharge specific capacity is 231mAh g‑1, 219mAh g are circulated by 50 circles‑1, capability retention is up to 95%, and capability retention is high.

Description

A kind of self assembly anode material for lithium-ion batteries V2O5Preparation method
Technical field
The invention belongs to technical field of lithium ion battery positive pole material preparation, and in particular to a kind of self assembly lithium ion battery Positive electrode V2O5Preparation method.
Background technology
With the development of science and technology, people are increasing to the demand of energy storage material.Lithium ion battery is because of its high-energy The advantages of density, stable cycle performance, memory-less effect and environmental protection, all kinds of pocket electronics have been widely used in it Device, the field such as hybrid vehicle and power network energy storage.For battery, its energy density depends primarily on positive pole material Material, and the actual specific capacity of the positive electrode of main flow is all in 170mAh g at present-1Left and right.Therefore, R and D have higher The anode material for lithium-ion batteries of specific capacity has important theory significance and application value.
V2O5It is used as a kind of intercalation materials of li ions of layer structure.In theory, as embedded two Li+When, theoretical specific capacity is reachable 294mAh g-1.But, V2O5Cyclical stability it is poor, this restrict V2O5It is used as the further development of battery material.At present, it is main The solution wanted is that material is carried out into nanosizing, prepares the V with self-assembled structures2O5, improve its chemical property.
At present, the anode material for lithium-ion batteries V with self-assembled structures is prepared2O5The method of powder mainly has hydro-thermal method. Liqiang Mai[Liqiang Mai,Qinyou An,Qiulong Wei,et al.Nanoflakes-Assembles Three-Dimensional Hollow-Porous V2O5as Lithium storage cathodes with High-rate Capacity[J].Small.2014,10:3232-3237.] etc. using carbosphere as template, with NH4VO3Together add ethylene glycol molten In agent, by 80 DEG C of water-bath, reaction 2.5h's arrives homogeneous solution；12h is reacted under 180 DEG C of hydrothermal conditions, product is obtained；Finally The hollow porous micro sphere that 2h prepares nanometer sheet composition is calcined at 450 DEG C.In 2.0-4.0V, 100mA g-1Under the conditions of, put first Electric specific capacity is 283mAh g-1, it is 77% that capability retention is enclosed in circulation 60.Qi Yue[Qi Yue,Hao Jiang,et al.Mesoporous single-crystalline V2O5nanorods assembled into hollow microspheres as cathode materials for high-rate and long-life lithium-ion batteries[J].ChemComn.2014,50:13362-13365.] etc. with NH4VO3For raw material, ethylene glycol is solvent, with poly- Vinylpyrrolidone (PVP) adds KBr and stirred as surfactant, and 12h is reacted under 200 DEG C of hydrothermal conditions, passes through 400 DEG C of heat treatment 2h obtain nanometer rods and are self-assembly of the V with hollow microsphere structure2O5.In 2.0-4.0V, 147mA g-1 Under the conditions of, first discharge specific capacity reaches 145.8mAh g-1, capacity is maintained at 128mAh g after 200 circle circulations-1.Above method Solvent-thermal method is used, the V with self-assembled structures is prepared2O5.But template is employed, and during water-heat process generation HTHP is higher to equipment requirement, and the yield of product is smaller and repeated not high, is unfavorable for large-scale industrial production.
The content of the invention
It is an object of the invention to provide a kind of technical process is simple, energy consumption is low, can be mass-produced with self assembly lithium Ion battery positive electrode V2O5Preparation method, the reaction temperature of this method is low, and yield is high, and reproducible, and is made Anode material for lithium-ion batteries V2O5Powder chemical composition is homogeneous, good cycling stability.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of self assembly anode material for lithium-ion batteries V2O5Preparation method, comprise the following steps：
1) ammonium metavanadate is dissolved in deionized water, is uniformly mixing to obtain 0.10~0.30molL-1NH4VO3Solution, It is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, obtains blackish green after stirring Solution, then adds diethylenetriamine or ethylenediamine into blackish green solution, well mixed to obtain solution, is designated as B solution；Its In, NH4VO3Ratio with diethylenetriamine is 0.01mol：4mL or NH4VO3Ratio with ethylenediamine is 0.01mol：4mL；
3) pH value of regulation B solution is after 0.5~4.0, ultrasonic under 800~1500W, obtains suspension；
4) suspension is centrifuged and obtains powder product, then powder product deionized water and absolute ethyl alcohol is anti- After backwashing is dried after washing, and obtains presoma；
5) presoma is heated into 1~3h at 250 DEG C~450 DEG C, obtains self assembly anode material for lithium-ion batteries V2O5。
The step 1) in ammonium metavanadate for analyze it is pure.
The step 2) in stirring time be 1~2h.
The step 3) in pH value be use 1~3molL-1What hydrochloric acid was adjusted.
The step 3) in ultrasonic time be 1~4h.
The step 4) in drying carried out in vacuum drying chamber.
The step 4) in dry temperature be 60~80 DEG C, drying time be 6~12h.
The step 5) in heating carried out in Muffle furnace.
Compared with prior art, the beneficial effect that the present invention has：
The present invention is by the way that ammonium metavanadate and dissolving oxalic acid to be added to a certain amount of diethylenetriamine in deionized water, then Or ethylenediamine, suspension is made under 800-1500W ultrasound conditions, then suspension is centrifuged, presoma is dried to obtain, then by before Drive body to be heat-treated, obtain anode material for lithium-ion batteries V2O5, with 600 DEG C of the prior art calcinings and solvent-thermal method Compare, be heat-treated in the present invention at 250 DEG C~450 DEG C, it is seen that reaction condition of the invention is gentle, and energy consumption is smaller, it is easy to Realize, beneficial to large-scale production, and because the present invention is without using template, so preparation process is simple, cost is relatively low, process It is easily-controllable, it is environmentally friendly.
V obtained by the present invention2O5It is about 50~80nm by diameter, length is about that 1 μm of nanometer rods are self-assembly of, and For coralloid loose porous road structure, chemical composition is homogeneous, and purity is higher, with larger specific surface area, can not only have Effect increase and the contact area of electrolyte, so as to promote the transmission of lithium ion, improve the chemical property of material.
In addition, V produced by the present invention2O5Open structure also for lithium ion insertion more avtive spots are provided, raising The specific capacity of electrode material；Meanwhile, the V of self-assembled nano structures2O5In lithium ion charge and discharge process, it can effectively alleviate lithium Ion is embedded in and the caused volumetric expansion of abjection, is conducive to improving the structural stability of material, and then improve the use longevity of battery Life.
V produced by the present invention2O5First discharge specific capacity is 231mAh g-1, 219mAh g are circulated by 50 circles-1, capacity Conservation rate is up to 95%, and capability retention is high.In addition, V produced by the present invention2O5It can be additionally used in catalyst, ultracapacitor and light The fields such as catalysis, are with a wide range of applications and research potential.
Brief description of the drawings
Fig. 1 is anode material for lithium-ion batteries V prepared by the embodiment of the present invention 12O5X-ray diffraction (XRD) figure of crystallite Spectrum.
Anode material for lithium-ion batteries V prepared by Fig. 2 embodiment of the present invention 22O5ESEM (SEM) photo of crystallite (is put Big multiple：20000 times).
Fig. 3 is anode material for lithium-ion batteries V prepared by the embodiment of the present invention 22O5ESEM (SEM) photo of crystallite (multiplication factor：100000 times)
Fig. 4 is anode material for lithium-ion batteries V prepared by the embodiment of the present invention 42O5Crystallite between 1.8V~4.0V voltages, 100mA g-1Under current density condition, the charge-discharge performance figure that circulation is 50 times.
Embodiment
Below in conjunction with the accompanying drawings and embodiment is described in further detail to the present invention.
V prepared by the present invention2O5Nano material is with acetylene black, polyvinylidene fluoride (PVDF) binding agent according to 8:1:1 matter After amount is than being well mixed, the homogeneous mixture that pasty state is obtained in 1-METHYLPYRROLIDONE (NMP) solution is dispersed in；It is coated in aluminium On paper tinsel, and the positive pole after 80 DEG C of vacuum drying 12h as battery.Using metal lithium sheet as negative pole, using polypropylene screen as barrier film, with Lithium-ion battery electrolytes (manufacturer：Shenzhen Xinzhoubang Technology Co., Ltd) as electrolyte, it is full high-purity in filling Button cell is assembled into the glove box of argon gas.Model CT- is produced in Shenzhen at room temperature for the charging and discharging test of battery In 3008W-5V10mA-S4 high precision test system.The voltage range of test is that (reference is in Li/Li by 4.0~1.8V+)。
Illustrated below by specific embodiment.
Embodiment 1
1) by the analytically pure ammonium metavanadate (NH of 0.01mol4VO3) be dissolved in 100mL deionized water, stir To 0.10molL-1NH4VO3Solution, is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, stirring 1h obtains blackish green molten Liquid, then adds 4mL diethylenetriamine, is well mixed under the conditions of magnetic agitation, obtains solution, be designated as B solution；
3) 2molL is used-1Hydrochloric acid regulation B solution pH value be 4.0 after, ultrasound 1h, obtains suspension under 800W；
4) suspension is centrifuged and obtains powder product, then powder product is used into deionized water and anhydrous second respectively Alcohol cyclic washing, then obtains presoma in vacuum drying chamber in drying 6h at 60 DEG C；
5) presoma is placed in Muffle furnace, 3h is heated under the conditions of 250 DEG C, obtain self assembly coralliform lithium ion battery Positive electrode V2O5。
It will be seen from figure 1 that product manufactured in the present embodiment is the V of pure phase2O5。
Embodiment 2
1) by the analytically pure ammonium metavanadate (NH of 0.015mol4VO3) be dissolved in 100mL deionized water, it is uniformly mixing to obtain 0.15mol·L-1NH4VO3Solution, is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, stirring 1.5h obtains blackish green molten Liquid, then adds diethylenetriamine, is well mixed under the conditions of magnetic agitation, obtains solution, be designated as B solution；Wherein, NH4VO3 Ratio with diethylenetriamine is 0.015mol：6mL.
3) 2molL is used-1Hydrochloric acid regulation B solution pH value be 3.5 after, ultrasound 1.5h, obtains suspension under 900W；
4) suspension is centrifuged and obtains powder product, then powder product is used into deionized water and anhydrous second respectively Alcohol cyclic washing, then obtains presoma in vacuum drying chamber in drying 8h at 70 DEG C；
5) presoma is placed in Muffle furnace, 2.5h is heated at 300 DEG C, obtaining self assembly coralliform lithium ion battery just Pole material V2O5。
From figures 2 and 3, it will be seen that V manufactured in the present embodiment2O5Constituted with the nanometer rods by a diameter of 50~80nm Coralliform multi-pore channel structure.
Embodiment 3
1) by the analytically pure ammonium metavanadate (NH of 0.02mol4VO3) be dissolved in 100mL deionized water, it is uniformly mixing to obtain 0.20mol·L-1NH4VO3Solution, is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, stirring 2h obtains blackish green molten Liquid, then adds diethylenetriamine, is well mixed under the conditions of magnetic agitation, obtains solution, be designated as B solution；Wherein, NH4VO3 Ratio with diethylenetriamine is 0.02mol：8mL.
3) 2molL is used-1Hydrochloric acid regulation B solution pH value be 3.0 after, ultrasound 2h, obtains suspension under 1000W；
4) suspension is centrifuged and obtains powder product, then powder product is used into deionized water and anhydrous second respectively Alcohol cyclic washing, then obtains presoma in vacuum drying chamber in drying 10h at 70 DEG C；
5) presoma is placed in Muffle furnace, 1.5h is heated at 350 DEG C, obtaining self assembly coralliform lithium ion battery just Pole material V2O5。
Embodiment 4
1) by the analytically pure ammonium metavanadate (NH of 0.025mol4VO3) be dissolved in 100mL deionized water, stir To 0.25molL-1NH4VO3Solution, is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, stirring 2h obtains blackish green molten Liquid, then adds diethylenetriamine, is well mixed under the conditions of magnetic agitation, obtains solution, be designated as B solution；Wherein, NH4VO3 Ratio with diethylenetriamine is 0.025mol：10mL.
3) 2molL is used-1Hydrochloric acid regulation B solution pH value be 2.0 after, ultrasound 3h, obtains suspension under 1200W；
4) suspension is centrifuged and obtains powder product, then powder product is used into deionized water and anhydrous second respectively Alcohol cyclic washing, then obtains presoma in vacuum drying chamber in drying 12h at 80 DEG C；
5) presoma is placed in Muffle furnace, 1.5h is heated at 400 DEG C, obtaining self assembly coralliform lithium ion battery just Pole material V2O5。
Figure 4, it is seen that self assembly coralliform anode material for lithium-ion batteries V made from the present embodiment2O5Put first Electric specific capacity is 231mAh g-1, 219mAh g are circulated by 50 circles-1, capability retention is up to 95%.
Embodiment 5
1) by the analytically pure ammonium metavanadate (NH of 0.03mol4VO3) be dissolved in 100mL deionized water, it is uniformly mixing to obtain 0.30mol·L-1NH4VO3Solution, is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, stirring 2h obtains blackish green molten Liquid, then adds diethylenetriamine, is well mixed under the conditions of magnetic agitation, obtains solution, be designated as B solution；Wherein, NH4VO3 Ratio with diethylenetriamine is 0.03mol：12mL.
3) 2molL is used-1Hydrochloric acid regulation B solution pH value be 0.5 after, ultrasound 4h, obtains suspension under 1500W；
4) suspension is centrifuged and obtains powder product, then powder product is used into deionized water and anhydrous second respectively Alcohol cyclic washing, then obtains presoma in vacuum drying chamber in drying 12h at 80 DEG C；
5) presoma is placed in Muffle furnace, 1h is heated at 450 DEG C, obtain self assembly coralliform lithium ion cell positive Material V2O5。
Embodiment 6
1) by the analytically pure ammonium metavanadate (NH of 0.03mol4VO3) be dissolved in 100mL deionized water, it is uniformly mixing to obtain 0.3mol·L-1NH4VO3Solution, is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, stirring 2h obtains blackish green molten Liquid, then adds ethylenediamine, is well mixed under the conditions of magnetic agitation, obtains solution, be designated as B solution；Wherein, NH4VO3With second The ratio of diamines is 0.03mol：12mL.
3) 2molL is used-1Hydrochloric acid regulation B solution pH value be 0.5 after, ultrasound 4h, obtains suspension under 1500W；
4) suspension is centrifuged and obtains powder product, then powder product is used into deionized water and anhydrous second respectively Alcohol cyclic washing, then obtains presoma in vacuum drying chamber in drying 12h at 80 DEG C；
5) presoma is placed in Muffle furnace, 1h is heated at 450 DEG C, obtain self assembly coralliform lithium ion cell positive Material V2O5。
Embodiment 7
1) by the analytically pure ammonium metavanadate (NH of 0.01mol4VO3) be dissolved in 100mL deionized water, it is uniformly mixing to obtain 0.10mol·L-1NH4VO3Solution, is designated as solution A；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, stirring 2h obtains blackish green molten Liquid, then adds ethylenediamine, is well mixed under the conditions of magnetic agitation, obtains solution, be designated as B solution；Wherein, NH4VO3With second The ratio of diamines is 0.01mol：4mL.
3) 2molL is used-1Hydrochloric acid regulation B solution pH value be 0.5 after, ultrasound 4h, obtains suspension under 1500W；
4) suspension is centrifuged and obtains powder product, then powder product is used into deionized water and anhydrous respectively Ethanol cyclic washing, then obtains presoma in vacuum drying chamber in drying 12h at 80 DEG C；
5) presoma is placed in Muffle furnace, 1h is heated at 450 DEG C, obtain self assembly coralliform lithium ion cell positive Material V2O5。

Claims (4)

1. a kind of self assembly anode material for lithium-ion batteries V2O5Preparation method, it is characterised in that comprise the following steps：
1) ammonium metavanadate is dissolved in deionized water, is uniformly mixing to obtain 0.10~0.30molL-1NH4VO3Solution, is designated as A Solution；
2) according to mol ratio ammonium metavanadate：Oxalic acid=1:1, oxalic acid is added into solution A, obtains blackish green molten after stirring Liquid, then adds diethylenetriamine or ethylenediamine into blackish green solution, well mixed to obtain solution, is designated as B solution；Its In, NH4VO3Ratio with diethylenetriamine is 0.01mol：4mL or NH4VO3Ratio with ethylenediamine is 0.01mol：4mL；
3) pH value of regulation B solution is after 0.5~4.0, ultrasonic under 800~1500W, obtains suspension；
4) suspension is centrifuged and obtains powder product, then powder product is washed repeatedly with deionized water and absolute ethyl alcohol Dried after washing, obtain presoma；
5) presoma is heated into 1~3h at 250 DEG C~450 DEG C, obtains self assembly anode material for lithium-ion batteries V2O5；
The step 1) in ammonium metavanadate for analyze it is pure；
The step 2) in stirring time be 1~2h；
The step 3) in pH value be use 1~3molL-1What hydrochloric acid was adjusted；
The step 3) in ultrasonic time be 1~4h.
2. self assembly anode material for lithium-ion batteries V according to claim 12O5Preparation method, it is characterised in that institute State step 4) in drying carried out in vacuum drying chamber.
3. self assembly anode material for lithium-ion batteries V according to claim 1 or 22O5Preparation method, it is characterised in that The step 4) in dry temperature be 60~80 DEG C, drying time be 6~12h.
4. self assembly anode material for lithium-ion batteries V according to claim 12O5Preparation method, it is characterised in that institute State step 5) in heating carried out in Muffle furnace.
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CN107365256A (en) * 2017-08-09 2017-11-21 龙岩学院 The three core vanadium clusters and its synthetic method of a kind of propeller configurations
CN107827155B (en) * 2017-10-31 2020-02-04 攀钢集团攀枝花钢铁研究院有限公司 Nano V2O5Preparation method of (1)
CN111509225B (en) * 2020-04-22 2022-06-07 中南大学 Preparation method of vanadium-based positive electrode material of zinc ion battery, product and application thereof
CN113371758B (en) * 2021-07-01 2023-02-17 陕西理工大学 Short rod self-assembly coralliform Cu 11 O 2 (VO 4 ) 6 Preparation method of flower ball
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