CN105576228A - Method for preparing lithium manganate to serve as lithium-ion battery by sol-gel method - Google Patents

Method for preparing lithium manganate to serve as lithium-ion battery by sol-gel method Download PDF

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Publication number
CN105576228A
CN105576228A CN201510860972.2A CN201510860972A CN105576228A CN 105576228 A CN105576228 A CN 105576228A CN 201510860972 A CN201510860972 A CN 201510860972A CN 105576228 A CN105576228 A CN 105576228A
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CN
China
Prior art keywords
preparation
sol
lithium
ion battery
limn2o4
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Pending
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CN201510860972.2A
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Chinese (zh)
Inventor
张淑芬
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Shaanxi Qiyuan Technology Development Co Ltd
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Shaanxi Qiyuan Technology Development Co Ltd
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Priority to CN201510860972.2A priority Critical patent/CN105576228A/en
Publication of CN105576228A publication Critical patent/CN105576228A/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
    • H01M4/36—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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00—Compounds of manganese
    • C01G45/12—Manganates manganites or permanganates
    • C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
    • C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
    • C01G45/1257—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing lithium, e.g. Li2MnO3, Li2[MxMn1-xO3
    • 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
    • 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
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to the technical field of solar battery preparation, in particular to a method for preparing lithium manganate to serve as a lithium-ion battery by a sol-gel method. The method includes the steps of firstly, preparing LiMn2O4; secondly, preparing electrodes; thirdly, preparing the battery. The method has the advantages that the components of raw materials can be evenly mixed in an atomic-scale manner, so that good product chemical uniformity and high purity are achieved, stoichiometric ratio can be controlled precisely, heat treatment temperature can be lowered evidently, and heat treatment time can be shortened evidently; since the spinel LiMn2O4 is synthesized by the sol-gel method, the composition and the structure are optimized, electrochemical performance is improved and preparation cost is prepared.

Description

Sol-gal process prepares the method for LiMn2O4 as lithium ion battery
Technical field
The present invention relates to solar cell preparing technical field, be specifically related to a kind of sol-gal process and prepare the method for LiMn2O4 as lithium ion battery.
Background technology
Over nearly 10 years, the research and development of lithium-ions battery is subject to global extensive concern always, and wherein the research of positive electrode is a very important link in lithium-ions battery research and development.Spinel-type LiMn 20 4material, as one of the positive electrode of lithium rechargeable battery having most competition potential, has the advantages such as aboundresources, cheap, safety, pollution be little.And along with the development of nanometer technology, researchers recognize the superiority of Application of micron in lithium rechargeable battery.
Nanometer LiMn 20 4material is in Lithium-ion embeding/deintercalation process, and the aspects such as its chemical property, crystal structure, granule-morphology, physical property all show special behavior: on the one hand, nanometer LiMn 20 4high voidage be that lithium ion provides a large amount of embedded space positions, improve embedding lithium capacity and energy density; On the other hand, because lithium ion the evolving path is short, be conducive to lithium ion quick embedding and embedding go out, kinetically having a clear superiority in.Meanwhile, nanometer LiMn 20 4under high current charge-discharge, degree of polarization is little, and reversible capacity is high, and cycle performance is better.Current LiMn 20 4synthetic method numerous, sol-gal process is the material synthesis method of a kind of advanced person.
Summary of the invention
The present invention is intended to propose a kind of sol-gal process and prepares the method for LiMn2O4 as lithium ion battery.
Technical program of the present invention lies in:
Sol-gal process prepares the method for LiMn2O4 as lithium ion battery, comprises the following steps:
(1) LiMn 20 4preparation;
(2) preparation of electrode;
(3) preparation of battery.
Described LiMn 20 4preparation method be:
(1) by Li +: Mn 2+=1:2 ratio takes lithium nitrate, manganese acetate respectively, dissolves successively in deionized water under magnetic stirring, stirs 10mm and forms the homogeneous aqueous solution that concentration of metal ions is 0.5mol/L;
(2) add acrylic acid, volume is the half adding deionized water volume, drips the pH=2 of nitre acid-conditioning solution; Continue to stir 30min, put by this solution and regulate 150 DEG C in an oven, insulation 15h, obtains tan xerogel;
(3) by xerogel grind after, put into Muffle furnace again air atmosphere sinter.
The preparation method of described electrode is: by active material LiMn 20 4, 12%PVDF solution, conductive black in mass ratio 84:8:8 and dispersant NMP add in mortar and mix, be stirred to slurry and there is good plasticity, then be coated in equably on aluminium foil with scraper, thickness is 200um, dry two hours in 120 DEG C of baking ovens, then roll electrode slice with roller press; Electrode slice is struck out the circular positive plate of required 14mm, positive plate, in vacuum drying chamber, at 110 DEG C after dry 8h, weighs, puts into dry glove box.
The preparation method of described battery is: with lithium sheet for reference electrode, lmol/LLiPF 6/ EC+DEC is electrolyte, and polypropylene screen Celgard2400 is barrier film, assembled formation button cell in glove box.
Technique effect of the present invention is:
Method feed components provided by the invention can reach the Homogeneous phase mixing of atom level, and product chemical uniformity is good, and purity is high, and stoichiometric proportion can accurately control: heat treatment temperature can significantly reduce, and heat treatment time can significantly shorten.Therefore, sol-gal process synthetic spinel type LiMn is adopted 20 4, to composition, the structure of optimizing material, improve material electrochemical performance, reduce preparation cost and there is very large attraction.
Embodiment
Sol-gal process prepares the method for LiMn2O4 as lithium ion battery, comprises the following steps:
(1) LiMn 20 4preparation;
(2) preparation of electrode;
(3) preparation of battery.
Wherein, LiMn 20 4preparation method be:
(1) by Li +: Mn 2+=1:2 ratio takes lithium nitrate, manganese acetate respectively, dissolves successively in deionized water under magnetic stirring, stirs 10mm and forms the homogeneous aqueous solution that concentration of metal ions is 0.5mol/L;
(2) add acrylic acid, volume is the half adding deionized water volume, drips the pH=2 of nitre acid-conditioning solution; Continue to stir 30min, put by this solution and regulate 150 DEG C in an oven, insulation 15h, obtains tan xerogel;
(3) by xerogel grind after, put into Muffle furnace again air atmosphere sinter.
Wherein, the preparation method of electrode is: by active material LiMn 20 4, 12%PVDF solution, conductive black in mass ratio 84:8:8 and dispersant NMP add in mortar and mix, be stirred to slurry and there is good plasticity, then be coated in equably on aluminium foil with scraper, thickness is 200um, dry two hours in 120 DEG C of baking ovens, then roll electrode slice with roller press; Electrode slice is struck out the circular positive plate of required 14mm, positive plate, in vacuum drying chamber, at 110 DEG C after dry 8h, weighs, puts into dry glove box.
Wherein, the preparation method of battery is: with lithium sheet for reference electrode, lmol/LLiPF 6/ EC+DEC is electrolyte, and polypropylene screen Celgard2400 is barrier film, assembled formation button cell in glove box.

Claims (4)

1. sol-gal process prepares the method for LiMn2O4 as lithium ion battery, it is characterized in that: comprise the following steps:
(1) LiMn 20 4preparation;
(2) preparation of electrode;
(3) preparation of battery.
2. sol-gal process according to claim 1 prepares the method for LiMn2O4 as lithium ion battery, it is characterized in that: described LiMn 20 4preparation method be:
(1) by Li +: Mn 2+=1:2 ratio takes lithium nitrate, manganese acetate respectively, dissolves successively in deionized water under magnetic stirring, stirs 10mm and forms the homogeneous aqueous solution that concentration of metal ions is 0.5mol/L;
(2) add acrylic acid, volume is the half adding deionized water volume, drips the pH=2 of nitre acid-conditioning solution; Continue to stir 30min, put by this solution and regulate 150 DEG C in an oven, insulation 15h, obtains tan xerogel;
(3) by xerogel grind after, put into Muffle furnace again air atmosphere sinter.
3. sol-gal process according to claim 1 prepares the method for LiMn2O4 as lithium ion battery, it is characterized in that: the preparation method of described electrode is: by active material LiMn 20 4, 12%PVDF solution, conductive black in mass ratio 84:8:8 and dispersant NMP add in mortar and mix, be stirred to slurry and there is good plasticity, then be coated in equably on aluminium foil with scraper, thickness is 200um, dry two hours in 120 DEG C of baking ovens, then roll electrode slice with roller press; Electrode slice is struck out the circular positive plate of required 14mm, positive plate, in vacuum drying chamber, at 110 DEG C after dry 8h, weighs, puts into dry glove box.
4. sol-gal process according to claim 1 prepares the method for LiMn2O4 as lithium ion battery, it is characterized in that: the preparation method of described battery is: with lithium sheet for reference electrode, lmol/LLiPF 6/ EC+DEC is electrolyte, and polypropylene screen Celgard2400 is barrier film, assembled formation button cell in glove box.
CN201510860972.2A 2015-12-01 2015-12-01 Method for preparing lithium manganate to serve as lithium-ion battery by sol-gel method Pending CN105576228A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106602057A (en) * 2017-01-05 2017-04-26 广州盘太能源科技有限公司 Preparation method for positive electrode material of lithium ion battery
CN108933243A (en) * 2018-07-11 2018-12-04 合肥师范学院 A kind of height ratio capacity sodium-ion battery positive material and preparation method thereof and sodium-ion battery
CN110642303A (en) * 2019-08-30 2020-01-03 广东新凌嘉新能源股份有限公司 Improved power ternary cylindrical lithium battery positive electrode material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106602057A (en) * 2017-01-05 2017-04-26 广州盘太能源科技有限公司 Preparation method for positive electrode material of lithium ion battery
CN108933243A (en) * 2018-07-11 2018-12-04 合肥师范学院 A kind of height ratio capacity sodium-ion battery positive material and preparation method thereof and sodium-ion battery
CN108933243B (en) * 2018-07-11 2021-07-13 合肥师范学院 High-specific-capacity sodium ion battery positive electrode material, preparation method thereof and sodium ion battery
CN110642303A (en) * 2019-08-30 2020-01-03 广东新凌嘉新能源股份有限公司 Improved power ternary cylindrical lithium battery positive electrode material and preparation method thereof

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Application publication date: 20160511