CN103078082A - High-volume V2O5 film anode material for lithium ion battery - Google Patents

High-volume V2O5 film anode material for lithium ion battery Download PDF

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CN103078082A
CN103078082A CN2012105575082A CN201210557508A CN103078082A CN 103078082 A CN103078082 A CN 103078082A CN 2012105575082 A CN2012105575082 A CN 2012105575082A CN 201210557508 A CN201210557508 A CN 201210557508A CN 103078082 A CN103078082 A CN 103078082A
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colloidal sol
lithium ion
ion battery
sol
film
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CN103078082B (en
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余丹梅
文嘉植
陈昌国
谯亚娟
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Chongqing University
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Chongqing University
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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

Abstract

The invention discloses a high-volume V2O5 film anode material for a lithium ion battery. A preparation method of the high-volume V2O5 film anode material for a lithium ion battery comprises the following steps of 1, preparing V2O5 sol by mixing V2O5 powder and H2O2 with stirring, 2, preparing sol having different concentrations by preparing the V2O5 sol into the sol respectively having concentrations of 0.002-0.016mol/L, 3, pre-treating a Pt substrate by immersing the Pt substrate in hydrogen peroxide for 10 min, flushing by deionized water and naturally drying in air, and 4, preparing a V2O5 film electrode by taking 10 microliters of the V2O5 sol having the required concentration, laying the V2O5 sol on the Pt substrate, naturally drying in air, putting the Pt substrate with the dried V2O5 sol into a muffle furnace having a temperature of 500 DEG C, carrying out calcination for 2 hours, and naturally cooling to a room temperature to obtain a V2O5 film electrode. The high-volume V2O5 film anode material for a lithium ion battery has a special microstructure and can improve a specific capacity of a lithium ion battery.

Description

A kind of high power capacity V for lithium ion battery 2O 5The film positive electrode
Technical field
The invention belongs to the electrode material field, particularly a kind of high power capacity V for lithium ion battery 2O 5The film positive electrode.
Background technology
Lithium ion battery is the novel storage battery that grows up on the lithium battery basis last century, have the advantages such as voltage is high, specific energy large, have extended cycle life, various daily miniature portable power supplys have been widely used at present, as the power supply renewal product, might be applied to the high-power electric appliance field in the future.In recent years, along with the appearance of high-performance negative pole system, electrolytical research has also obtained remarkable progress.Comparatively speaking, anode material for lithium-ion batteries research comparatively lags behind, and has limited the further raising of lithium ion battery overall performance.The positive electrode that research and comparison is many at present mainly contains the LiMO of layer structure 2(wherein: M=Ni, Co, Mn etc.) also comprises the mixing of multicomponent system, but its specific capacity is low and the problem such as cyclicity is still waiting to solve.Spinel-type LiMn 2O 4Have security performance good, easily the advantage such as synthetic also is the present more anode material for lithium-ion batteries of research, but has the John-Teller effect in charge and discharge process, and the structure distorted has reduced the symmetry of spinel structure, causes the cycle performance variation.The LiMPO of olivine crystal structure 4(wherein: M=Fe, Mn, Ni, Co etc.) has Heat stability is good, security performance advantages of higher, and the transition metal oxide that has surpassed layer structure in the stability of charged state, make it be specially adapted to power battery material, but exist the irreversible capacity problem that causes because conductivity is low, the method for improvement is on the one hand: prepare the powder body material that particle is thin, purity is high by changing synthetic method; Improve its conductivity by doping metals powder or metal ion on the other hand, increase reversible capacity.
Triclinic V 2O 5, with VO 4The tetragonal pyramid unit is combined into chain by oxo bridge, interchain is connected to form a multiple chain by another oxo bridge again, thereby consist of the layered arrangement that is parallel to [001] plane, be fit to very much the embedding of taking off of lithium ion, but have still in actual applications that ion transportation is low, conductivity is low, charge-discharge performance is poor, the problem such as specific capacity and energy density are low, limited its application in the lithium ion battery field.
Summary of the invention
Purpose of the present invention in order to overcome above-mentioned the deficiencies in the prior art, solves capacity of lithium ion battery little exactly, the problem that special capacity fade is serious, and a kind of high power capacity V for lithium ion battery is provided 2O 5The film positive electrode.
That involved in the present invention is a kind of high power capacity V for lithium ion battery 2O 5The film positive electrode is characterized in that this material prepares by the following method: (1) preparation vanadic oxide colloidal sol: the hydrogen peroxide (H that gets 3mL 30% 2O 2) solution places the beaker of 25 mL, then with 0.146 g vanadic oxide (V of accurate weighing 2O 5) powder puts into beaker, at room temperature fully slowly stir and make V 2O 5Powder dissolves fully, then adds 2 mL deionized waters and continues to be stirred to the stable rufous colloidal sol of formation; (2) colloidal sol of preparation variable concentrations: with above-mentioned V 2O 5Colloidal sol is distinguished constant volume to 50mL-400ml, obtains concentration range and is: the V of 0.002 mol/L to 0.016 mol/L 2O 5Colloidal sol; (3) preliminary treatment Pt substrate: pending Pt sheet is immersed in the hydrogen peroxide fully, soaked 10 minutes, then rinse natural air drying with deionized water well; (4) preparation V 2O 5Membrane electrode: the V that measures the desired concn of 10 μ L with pipettor 2O 5Colloidal sol spreads over through on the pretreated Pt sheet, behind natural air drying under the room temperature, places 500 ℃ Muffle furnace to calcine 2 hours, naturally cools to room temperature, namely obtains V 2O 5Membrane electrode.
V by this method preparation 2O 5The electrode material pattern is special, has two stable charge and discharge platform, shows high embedding lithium capacity and good cycle performance, has broad application prospects.And this method does not relate to the use of conductive agent, bonding agent in the manufacturing process of electrode, and electrode material directly spreads over one step of electrode basement and finishes, and manufacture craft is simple, and is easy and simple to handle, and process is easy to control, environmental protection.
The V of the present invention's preparation 2O 5Thin-film electrode material adopts three-electrode system, with the LiClO of 1 mol/L 4/ PC is electrolyte, V 2O 5Membrane electrode is work electrode, and the Pt sheet is auxiliary electrode, and Ag/AgCl is reference electrode, shows this V by cyclic voltammetric and constant current charge-discharge test 2O 5Film has two obvious charge and discharge platform, good cycle, and when charging and discharging currents density was 400mA/g, its initial discharge specific capacity can reach 714mAh/g, and had at present the lithium ion battery V of bibliographical information now 2O 5Positive electrode, specific discharge capacity only be ~ 377mAh/g, thereby, with existing lithium ion battery V 2O 5Positive electrode is compared, V provided by the invention 2O 5The film positive electrode can effectively solve the low problem of lithium ion battery specific capacity, has significantly improved V 2O 5Using value as anode material for lithium-ion batteries.
 
Description of drawings
Fig. 1 is that collosol concentration is the V of 0.008mol/L 2O 5The SEM of film positive electrode;
Fig. 2 is that collosol concentration is the V of 0.008mol/L 2O 5The cyclic voltammetry curve of film positive electrode when sweep speed is 0.01V/s;
Fig. 3 is that collosol concentration is the V of 0.008mol/L 2O 5The film positive electrode is constant current charge-discharge capacity curve under the 400mA/g condition in the quality current density;
Fig. 4 is that collosol concentration is the V of 0.008mol/L 2O 5The charging and discharging curve of film positive electrode under different current densities;
Fig. 5 is that collosol concentration is the V of 0.008mol/L 2O 5The discharge capacity attenuation curve of film positive electrode under different current densities;
Fig. 6 is the V of 0.008mol/L for several collosol concentrations 2O 5The initial charge/discharge capacity comparison of film positive electrode;
Fig. 7 is that collosol concentration is the V of 0.016mol/L 2O 5Film is constant current charge-discharge capacity curve under the 400mA/g condition in the quality current density;
Fig. 8 is that collosol concentration is the V of 0.0054mol/L 2O 5Film is constant current charge-discharge capacity curve under the 400mA/g condition in the quality current density;
Fig. 9 is that collosol concentration is the V of 0.004mol/L 2O 5Film is constant current charge-discharge capacity curve under the 400mA/g condition in the quality current density;
Figure 10 is that collosol concentration is the V of 0.0032mol/L 2O 5Film is constant current charge-discharge capacity curve under the 400mA/g condition in the quality current density;
Figure 11 is that collosol concentration is the V of 0.002mol/L 2O 5Film is constant current charge-discharge capacity curve under the 400mA/g condition in the quality current density.
Embodiment
The present invention is further described as follows below in conjunction with drawings and Examples:
Embodiment 1
A kind of high power capacity V for lithium ion battery 2O 5The preparation method of film positive electrode is as follows:
(1) preparation vanadic oxide colloidal sol: the hydrogen peroxide (H that gets 3mL 30% 2O 2) solution places the beaker of 25 mL, then with 0.146 g vanadic oxide (V of accurate weighing 2O 5) powder puts into beaker, at room temperature fully slowly stir and make V 2O 5Powder dissolves fully, then adds 2 mL deionized waters and continues to be stirred to the stable rufous colloidal sol of formation;
(2) compound concentration is the V of 0.008mol/L 2O 5Colloidal sol: with above-mentioned V 2O 5The colloidal sol constant volume obtains the V that concentration is 0.008 mol/L to 100ml 2O 5Colloidal sol;
(3) preliminary treatment Pt substrate: pending Pt sheet is immersed in the hydrogen peroxide fully, soaked 10 minutes, then rinse natural air drying with deionized water well;
(4) preparation V 2O 5Membrane electrode: the V that measures the desired concn of 10 μ L with pipettor 2O 5Colloidal sol spreads over through on the pretreated Pt sheet, behind natural air drying under the room temperature, places 500 ℃ Muffle furnace to calcine 2 hours, naturally cools to room temperature, namely obtains V 2O 5Membrane electrode.
The test of employing three-electrode system, V 2O 5Membrane electrode is work electrode, and Ag/AgCl did pretreated Pt sheet as to electrode as reference electrode, carried out the test of cyclic voltammetric and constant current charge-discharge.
The V that the present embodiment is prepared 2O 5The electronic scanning figure (SEM) of membrane electrode as shown in Figure 1, as can be seen from the figure, V 2O 5Film is to be made of the particle of structure in the form of sheets, and has all good features of even compactness.
The V that the present embodiment is prepared 2O 5The cyclic voltammetry curve of membrane electrode, as shown in Figure 2, the scanning voltage scope is-0.2V ~ 0.6V vs. Ag/AgCl to sweep speed and be 0.01V/s.As can be seen from the figure, at V 2O 5Two pairs of obvious redox peaks are arranged on the cyclic voltammetry curve of film, Li is described +Ion is at V 2O 5Embedding on the membrane electrode is taken off process and is carried out in two steps, and does not have irreversible transition, is conducive to improve the performance of lithium ion battery.V 2O 5Film is that an oxidation peak respectively appears in 0.14V and 0.34V place at voltage, corresponding Li +Ion is at V 2O 5Deviate from process on the membrane electrode; At-0.04V and 0.19V place a reduction peak appears respectively, corresponding Li +Ion is at V 2O 5Telescopiny on the membrane electrode, and the potential difference at first pair of oxidation/reduction peak differs 0.18V, and the potential difference at second pair of oxidation/reduction peak differs 0.15V, and V is described 2O 5Thin-film electrode material has good invertibity.
The V of the present embodiment preparation 2O 5The constant current charge-discharge capacity curve of membrane electrode, as shown in Figure 3, charging and discharging currents is 5.84*10 -6A(quality current density: 400mA/g), the charging/discharging voltage scope is-0.1 ~ 0.5V vs. Ag/AgCl, on scheming, can find out, on charging and discharging curve, have two stably discharge voltage plateaus, curve is full, when final discharging voltage, the curve downward trend just increases suddenly, and this illustrates that this material has good discharge performance.
The V of the present embodiment preparation 2O 5Charging and discharging curve under the different current densities of membrane electrode as shown in Figure 4, as can be seen from the figure, when current density was 400mA/g, discharge voltage plateau was the most steady, discharge capacity is maximum, and along with the increase of charging and discharging currents density, V 2O 5The discharge capacity of membrane electrode descends to some extent, but changes not quite, illustrates that this material can discharge and recharge under high current density.
The V of the present embodiment preparation 2O 5The discharge capacity attenuation curve of membrane electrode under different current densities as shown in Figure 5, as can be seen from the figure, along with the increase of discharge current density, V 2O 5The discharge capacity attenuation rate of membrane electrode changes little, and after 10 circulations, attenuation rate is respectively 14.49%, 15.07%, 22.81%, 25.47%, is more or less the same, and hence one can see that, this V 2O 5Membrane electrode still has good cycle performance along with the increase of current density.
Fig. 6 is under the same conditions, and several concentration are the V of 0.008mol/L 2O 5The initial charge/discharge capacity comparison of film sample, charging and discharging currents density is 400mA/g, and average initial discharge capacity is: 703.56mAh/g, as can be seen from the figure the stability of this material property and reappearance are all better.
Embodiment 2
A kind of high power capacity V for lithium ion battery 2O 5Preparation method's concrete steps of film positive electrode, with embodiment 1, wherein:
In (2) step, the present embodiment is that compound concentration is the V of 0.016mol/L 2O 5Colloidal sol: with above-mentioned V 2O 5The colloidal sol constant volume obtains the V that concentration is 0.016 mol/L to 50ml 2O 5Colloidal sol.
Concentration is the V of 0.016mol/L 2O 5The V of colloidal sol preparation 2O 5The film positive electrode the quality current density be under the 400mA/g condition the constant current charge-discharge capacity curve as shown in Figure 7.
Embodiment 3
A kind of high power capacity V for lithium ion battery 2O 5Preparation method's concrete steps of film positive electrode, with embodiment 1, wherein:
In (2) step, the present embodiment is that compound concentration is the V of 0.0054mol/L 2O 5Colloidal sol: with above-mentioned V 2O 5The colloidal sol constant volume obtains the V that concentration is 0.0054 mol/L to 150ml 2O 5Colloidal sol.
Concentration is the V of 0.0054mol/L 2O 5The V of colloidal sol preparation 2O 5The film positive electrode the quality current density be under the 400mA/g condition the constant current charge-discharge capacity curve as shown in Figure 8.
Embodiment 4
A kind of high power capacity V for lithium ion battery 2O 5Preparation method's concrete steps of film positive electrode, with embodiment 1, wherein:
In (2) step, the present embodiment is that compound concentration is the V of 0.004mol/L 2O 5Colloidal sol: with above-mentioned V 2O 5The colloidal sol constant volume obtains the V that concentration is 0.004 mol/L to 200ml 2O 5Colloidal sol.
Concentration is the V of 0.004mol/L 2O 5The V of colloidal sol preparation 2O 5The film positive electrode the quality current density be under the 400mA/g condition the constant current charge-discharge capacity curve as shown in Figure 9.
Embodiment 5
A kind of high power capacity V for lithium ion battery 2O 5Preparation method's concrete steps of film positive electrode, with embodiment 1, wherein:
In (2) step, the present embodiment is that compound concentration is the V of 0.0032mol/L 2O 5Colloidal sol: with above-mentioned V 2O 5The colloidal sol constant volume obtains the V that concentration is 0.0032 mol/L to 250ml 2O 5Colloidal sol.
Concentration is the V of 0.0032mol/L 2O 5The V of colloidal sol preparation 2O 5The film positive electrode the quality current density be under the 400mA/g condition the constant current charge-discharge capacity curve as shown in figure 10.
Embodiment 6
A kind of high power capacity V for lithium ion battery 2O 5Preparation method's concrete steps of film positive electrode, with embodiment 1, wherein:
In (2) step, the present embodiment is that compound concentration is the V of 0.002mol/L 2O 5Colloidal sol: with above-mentioned V 2O 5The colloidal sol constant volume obtains the V that concentration is 0.002 mol/L to 400ml 2O 5Colloidal sol.
Concentration is the V of 0.002mol/L 2O 5The V of colloidal sol preparation 2O 5The film positive electrode the quality current density be under the 400mA/g condition the constant current charge-discharge capacity curve as shown in figure 11.

Claims (1)

1. high power capacity V who is used for lithium ion battery 2O 5The film positive electrode, this material prepares by the following method:
(1) preparation V 2O 5Colloidal sol: get the hydrogen peroxide solution of 3mL 30% in the beaker of 25 mL, then with 0.146 g V 2O 5Powder is put into beaker, fully slowly stirs under the room temperature and makes V 2O 5Powder dissolves fully, then adds 2 mL deionized waters and continues to be stirred to the stable rufous colloidal sol of formation;
(2) colloidal sol of preparation variable concentrations: with above-mentioned V 2O 5Colloidal sol is distinguished constant volume to 50mL-400ml, obtains concentration range and is: the V of 0.002 mol/L to 0.016 mol/L 2O 5Colloidal sol;
(3) preliminary treatment Pt substrate: the Pt sheet is immersed in the hydrogen peroxide, soaked 10 minutes, then rinse natural air drying with deionized water well;
(4) preparation V 2O 5Membrane electrode: the V that gets 10 μ L desired concns with pipettor 2O 5Colloidal sol spreads on the pretreated Pt sheet, behind the natural air drying, places 500 ℃ Muffle furnace to calcine 2 hours, naturally cools to room temperature, namely obtains V 2O 5Membrane electrode.
CN201210557508.2A 2012-12-20 2012-12-20 High-volume V2O5 film anode material for lithium ion battery Expired - Fee Related CN103078082B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105070881A (en) * 2015-07-13 2015-11-18 重庆大学 High-capacity V2O5.nH2O thin-film electrode material for lithium ion battery
CN106830078A (en) * 2017-02-28 2017-06-13 嘉兴学院 A kind of vanadic anhydride micron order film and preparation method thereof
CN110467221A (en) * 2019-09-17 2019-11-19 安徽建筑大学 A kind of NaV6O15The preparation method of film and NaV obtained6O15Film

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012051619A2 (en) * 2010-10-15 2012-04-19 University Of Washington Through Its Center For Commercialization V2o5 electrodes with high power and energy densities

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012051619A2 (en) * 2010-10-15 2012-04-19 University Of Washington Through Its Center For Commercialization V2o5 electrodes with high power and energy densities

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DAWEI LIU ET AL: "V2O5 xerogel electrodes with much enhanced lithium-ion intercalation properties with N2 annealing", 《JOURNAL OF MATERIALS CHEMISTRY》 *
M.D.LEVI ET AL: "Li-insertion into thin monolithic V2O5 films electrodes characterized by a variety of electroanalytical techniques", 《JOURNAL OF POWER SOURCES》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105070881A (en) * 2015-07-13 2015-11-18 重庆大学 High-capacity V2O5.nH2O thin-film electrode material for lithium ion battery
CN106830078A (en) * 2017-02-28 2017-06-13 嘉兴学院 A kind of vanadic anhydride micron order film and preparation method thereof
CN110467221A (en) * 2019-09-17 2019-11-19 安徽建筑大学 A kind of NaV6O15The preparation method of film and NaV obtained6O15Film

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