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CN106410121A - Preparation method of LiNiVO4 lithium ion battery anode material - Google Patents

Preparation method of LiNiVO4 lithium ion battery anode material Download PDF

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Publication number
CN106410121A
CN106410121A CN201610988929.9A CN201610988929A CN106410121A CN 106410121 A CN106410121 A CN 106410121A CN 201610988929 A CN201610988929 A CN 201610988929A CN 106410121 A CN106410121 A CN 106410121A
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CN
China
Prior art keywords
graphene
linivo
lithium ion
ion battery
slowly added
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Pending
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CN201610988929.9A
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Chinese (zh)
Inventor
张达明
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Wuxi Mingsheng Strong Blower Co Ltd
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Wuxi Mingsheng Strong Blower Co Ltd
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Priority to CN201610988929.9A priority Critical patent/CN106410121A/en
Publication of CN106410121A publication Critical patent/CN106410121A/en
Pending legal-status Critical Current

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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a preparation method of an anode material. The preparation method comprises the following steps: adding a graphene solution into V2O5 powder, H2O2, anhydrous LiAc and Ni(Ac)2.4H2O which are used as raw materials; preparing a graphene-loaded lithium nickel vanadium oxide lithium battery anode material in combination with a hydrothermal synthesis technology by use of a sol-gel method. The specific capacities of first charge and discharge of the material reach 982 mAh/g and 872 mAh/g, respectively; the first coulombic efficiency is 95.7%; the coulombic efficiency is stabilized to be 95% or above after cycling for 100 times.

Description

A kind of LiNiVO4Lithium ion battery negative material preparation method
Technical field
The present invention relates to technical field of new energies, more particularly, to a kind of LiNiVO4Lithium ion battery negative material preparation side Method.
Background technology
In recent years, growing with portable equipment and electric automobile, lithium ion battery material is proposed higher Require.Wherein there is the material LiNiVO of inverse spinel structure4Due to its excellent with cycle performance, higher voltage platform just standby Paid close attention to by people.But it there is problems that：Specific capacity is relatively low, and in cyclic process, diffusion impedance is larger, different preparation method Larger to its performance impact etc., this bavin factor constrains the development of this material.And the electronics in Novel Carbon Nanomaterials Graphene Mobility can reach 2 × l05cm2/ V s, has excellent electric conductivity；And thermal conductivity is up to 5000W/ (m K)；Theoretical ratio Surface area is up to 2630m2/g.Research shows that the presence of Graphene can improve the electron conductivity of material, shortens lithium ion and expands Scattered path, the structure simultaneously for material plays Stabilization.After addition Graphene is as conductive additive, can greatly change The cyclical stability of kind lithium ion battery, high rate during charging-discharging and security performance.
Content of the invention
It is an object of the invention to proposing a kind of LiNiVO4The preparation method of lithium ion battery negative material, it adds suitable Amount Graphene, improves the performance of material.
For reaching this purpose, the present invention employs the following technical solutions：
A kind of LiNiVO4Lithium ion battery negative material preparation method, including：
(1) under room temperature, by V2O5It is slowly added in hydrogen peroxide, obtain the faint yellow V of homogeneous transparent2O5Colloidal sol, reacts 0.5- Form V russet after 2h2O5·nH2O wet gel；
(2) anhydrous lithium acetate is slowly added into V2O5·nH2In O wet gel, stir 20-60min, react to transparence, It is slow added into nickel acetate, reacts to transparence, its addition makes Li:Ni:V presses metal atomic molar than for 3:(0.5-2): (0.5-2)；
(3) it is slowly added to citric acid, add graphene solution, continuously stirred, obtain graphene-supported LiNiVO4Before Drive body, wherein Graphene accounts for 80-98wt% in presoma；
(4) by described graphene-supported LiNiVO4Presoma reacts 18-36h in a kettle. at 75-90 DEG C, cold But to room temperature；
(5) product is washed and be vacuum dried at 170-190 DEG C, obtain graphene-supported LiNiVO4Lithium ion battery Negative material.
The graphene-supported LiNiVO that the present invention obtains4Relatively it is suitable as lithium cell cathode material.
The present invention is with V2O5Powder, H2O2, anhydrous LiAc and Ni (Ac)2·4H2O is raw material, adds graphene solution, adopts Sol-gel process simultaneously prepares graphene-supported lithium nickel vanadium oxygen lithium cell cathode material with reference to Hydrothermal Synthesiss technology.
In the XRD figure of target product, nearby LiNiVO in 2 θ=36 °4Characteristic peak (311), show the present invention relatively low At a temperature of be obtained crystal form LiNiVO4.
The sample of the SEM photograph display synthesis of material is in coralliform, is covered with a nanometer bulbous protrusion above, is evenly distributed, ball Shape short grained size is about more than ten nanometers, the not only big specific surface area of material of this nanostructured, improve material with The contact area of electrolyte, also provides more active position for embedding in a large number of lithium ion.
The specific volume scape discharging first and charging of material divides business to reach 982mAh/g and 872mAh/g, coulombic efficiency first 95.7%.After 100 times circulate, coulombic efficiency is stablized more than 95%.Can see from cyclic voltammetry curve, pass through After 5 circulations, the corresponding cyclic voltammetry curve of material essentially coincides, and shows that the structure sill of material after cyclic voltammetric keeps Constant, this shows that this electrode material has good cycle performance.
Specific embodiment
To further illustrate technical scheme below by specific embodiment.
Embodiment 1
A kind of LiNiVO4Lithium ion battery negative material preparation method, including：
(1) under room temperature, by V2O5It is slowly added in hydrogen peroxide, obtain the faint yellow V of homogeneous transparent2O5Colloidal sol, reacts 0.5h After form V russet2O5·nH2O wet gel；
(2) anhydrous lithium acetate is slowly added into V2O5·nH2In O wet gel, stir 20min, react to transparence, then It is slowly added to nickel acetate, reacts to transparence, its addition makes Li:Ni:V presses metal atomic molar than for 3:0.5:0.5；
(3) it is slowly added to citric acid, add graphene solution, continuously stirred, obtain graphene-supported LiNiVO4Before Drive body, wherein Graphene accounts for 80wt% in presoma；
(4) by described graphene-supported LiNiVO4Presoma reacts 18h in a kettle. at 75 DEG C, is cooled to room Temperature；
(5) product is washed and be vacuum dried at 170 DEG C, obtain graphene-supported LiNiVO4Lithium ion battery negative Material.
Embodiment 2
A kind of LiNiVO4Lithium ion battery negative material preparation method, including：
(1) under room temperature, by V2O5It is slowly added in hydrogen peroxide, obtain the faint yellow V of homogeneous transparent2O5Colloidal sol, after reaction 2h Form V russet2O5·nH2O wet gel；
(2) anhydrous lithium acetate is slowly added into V2O5·nH2In O wet gel, stir 60min, react to transparence, then It is slowly added to nickel acetate, reacts to transparence, its addition makes Li:Ni:V presses metal atomic molar than for 3:2:2；
(3) it is slowly added to citric acid, add graphene solution, continuously stirred, obtain graphene-supported LiNiVO4Before Drive body, wherein Graphene accounts for 98wt% in presoma；
(4) by described graphene-supported LiNiVO4Presoma reacts 36h in a kettle. at 90 DEG C, is cooled to room Temperature；
(5) product is washed and be vacuum dried at 190 DEG C, obtain graphene-supported LiNiVO4Lithium ion battery negative Material.
Embodiment 3
A kind of LiNiVO4Lithium ion battery negative material preparation method, including：
(1) under room temperature, by V2O5It is slowly added in hydrogen peroxide, obtain the faint yellow V of homogeneous transparent2O5Colloidal sol, after reaction 1h Form V russet2O5·nH2O wet gel；
(2) anhydrous lithium acetate is slowly added into V2O5·nH2In O wet gel, stir 40min, react to transparence, then It is slowly added to nickel acetate, reacts to transparence, its addition makes Li:Ni:V presses metal atomic molar than for 3:1:1；
(3) it is slowly added to citric acid, add graphene solution, continuously stirred, obtain graphene-supported LiNiVO4Before Drive body, wherein Graphene accounts for 95wt% in presoma；
(4) by described graphene-supported LiNiVO4Presoma reacts 24h in a kettle. at 80 DEG C, is cooled to room Temperature；
(5) product is washed and be vacuum dried at 180 DEG C, obtain graphene-supported LiNiVO4Lithium ion battery negative Material.
The material that embodiment 1-3 prepares first discharge and charge specific volume scape divide business reach 982mAh/g and 872mAh/g, coulombic efficiency 95.7% first.After 100 times circulate, coulombic efficiency is stablized more than 95%.

Claims (1)

1. a kind of LiNiVO4Lithium ion battery negative material preparation method, including：
(1) under room temperature, by V2O5It is slowly added in hydrogen peroxide, obtain the faint yellow V of homogeneous transparent2O5Colloidal sol, after reaction 0.5-2h Form V russet2O5·nH2O wet gel；
(2) anhydrous lithium acetate is slowly added into V2O5·nH2In O wet gel, stir 20-60min, react to transparence, then delay Slow addition nickel acetate, reacts to transparence, its addition makes Li:Ni:V presses metal atomic molar than for 3:(0.5-2): (0.5-2)；
(3) it is slowly added to citric acid, add graphene solution, continuously stirred, obtain graphene-supported LiNiVO4Presoma, Wherein Graphene accounts for 80-98wt% in presoma；
(4) by described graphene-supported LiNiVO4Presoma reacts 18-36h in a kettle. at 75-90 DEG C, is cooled to room Temperature；
(5) product is washed and be vacuum dried at 170-190 DEG C, obtain graphene-supported LiNiVO4Lithium ion battery negative material Material.
CN201610988929.9A 2016-11-10 2016-11-10 Preparation method of LiNiVO4 lithium ion battery anode material Pending CN106410121A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111834615A (en) * 2019-04-23 2020-10-27 四川佰思格新能源有限公司 High-specific-capacity composite negative electrode material, preparation method and lithium ion battery
CN114613978A (en) * 2022-03-23 2022-06-10 合肥工业大学 Preparation of nickel-doped Li based on sol-gel system3V2O5Method for preparing anode material of lithium ion battery

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105070910A (en) * 2015-07-20 2015-11-18 安阳工学院 Preparation method and application of carbon-coated lithium nickel vanadium oxide nano material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105070910A (en) * 2015-07-20 2015-11-18 安阳工学院 Preparation method and application of carbon-coated lithium nickel vanadium oxide nano material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
孙兴川: "石墨烯负载锂镍钒氧的制备及电化学性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111834615A (en) * 2019-04-23 2020-10-27 四川佰思格新能源有限公司 High-specific-capacity composite negative electrode material, preparation method and lithium ion battery
CN111834615B (en) * 2019-04-23 2021-11-16 四川佰思格新能源有限公司 Composite negative electrode material, preparation method and lithium ion battery
CN114613978A (en) * 2022-03-23 2022-06-10 合肥工业大学 Preparation of nickel-doped Li based on sol-gel system3V2O5Method for preparing anode material of lithium ion battery
CN114613978B (en) * 2022-03-23 2023-03-14 合肥工业大学 Preparation of nickel-doped Li based on sol-gel system 3 V 2 O 5 Method for preparing anode material of lithium ion battery

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