CN103887508B - The coated LiNi of polyelectrolyte 0.5mn 1.5o 4the preparation method of positive electrode - Google Patents

The coated LiNi of polyelectrolyte 0.5mn 1.5o 4the preparation method of positive electrode Download PDF

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CN103887508B
CN103887508B CN201410109284.8A CN201410109284A CN103887508B CN 103887508 B CN103887508 B CN 103887508B CN 201410109284 A CN201410109284 A CN 201410109284A CN 103887508 B CN103887508 B CN 103887508B
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polyelectrolyte
lini
lithium
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CN103887508A (en
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范未峰
王国冬
代洋杰
姜忱
吴宗峻
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Jiange County Ruixin Asset Management Co.,Ltd.
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SICHUAN XING NENG NEW MATERIALS Co Ltd
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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
    • 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
    • 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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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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Abstract

The invention discloses the coated LiNi of a kind of polyelectrolyte 0.5mn 1.5o 4the preparation method of positive electrode, the coated LiNi of application polyelectrolyte solution 0.5mn 1.5o 4, then drying obtains the coated LiNi of polyelectrolyte 0.5mn 1.5o 4, described polyelectrolyte is the mixture of a kind of or above several material in Lithium polyacrylate, polymethylacrylic acid lithium, poly lithium, poly-(methyl vinyl ether copolymerization maleic acid) lithium or poly-fumaric acid lithium.This method for coating is at LiNi 0.5mn 1.5o 4surface defines one deck polyelectrolyte film, enhances the compatibility with electrolyte, therefore has the feature of height ratio capacity, high magnification, long circulation life.

Description

The coated LiNi of polyelectrolyte 0.5mn 1.5o 4the preparation method of positive electrode
Technical field
The present invention relates to a kind of preparation method of high-voltage anode material of lithium ion batteries, particularly relate to the preparation method of Surface coating spinel-type high-voltage lithium nickel manganate anode material, belong to anode material for lithium-ion batteries technical field.
Background technology
Charging/discharging voltage platform is greater than the positive electrode of 4.5V, is commonly referred to as high-voltage anode material.Such as, LiNi 0.5mn 1.5o 4, working voltage platform is 4.7V, is typical 5V high-voltage anode material.LiNi 0.5mn 1.5o 4there is three-dimensional lithium ion tunnel, the Ni of 0.5mol 2+replace and make 1molLiMn 2o 4middle Mn 3+all become Mn 4+(LiNi 0.5mn 1.5o 4) and do not affect the theoretical specific capacity of material.Meanwhile, due to LiNi 0.5mn 1.5o 4in there is not Mn 3+, do not have Jahn-Teller effect to produce structural aberration, make cycle performance, high-temperature behavior all significantly improves.
It is generally acknowledged that high potential electrolyte problem of resistance is nickel ion doped large-scale production and the key issue in application.Surface coating can improve LiNi 0.5mn 1.5o 4with the compatibility of electrolyte, improve its chemical property, many researchers have carried out the work of this respect.Such as: the AlF of CN102324512A 3surface coating, CN102983324A aluminium zinc oxide AZO Surface coating, the solid electrolyte Li of the coated and CN102683709A of the CuO surface of CN103337621A 5la 3m 2o 12(M=Ta, Nb) Surface coating.Above-mentioned surface coating method all will pass through, the mixing of electrode material and coated presoma, drying, and then high temperature 500 DEG C calcining obtains inorganic compound coating layer.Method technique is loaded down with trivial details needs high-temperature calcination again.
Summary of the invention
Deficiency for above-mentioned conventional surface method for coating of the present invention, proposes a kind of simple, quick polyelectrolyte Surface coating LiNi 0.5mn 1.5o 4the method of positive electrode, PAALi Surface coating LiNi prepared by the method 0.5mn 1.5o 4positive electrode has high working voltage platform, height ratio capacity, high magnification, long-life feature.
Technical scheme of the present invention is: the coated LiNi of a kind of polyelectrolyte 0.5mn 1.5o 4the preparation method of positive electrode, the coated LiNi of application polyelectrolyte solution 0.5mn 1.5o 4, then drying obtains the coated LiNi of polyelectrolyte 0.5mn 1.5o 4, described polyelectrolyte is the mixture of a kind of or above several material in Lithium polyacrylate, polymethylacrylic acid lithium, poly lithium, poly-(methyl vinyl ether copolymerization maleic acid) lithium or poly-fumaric acid lithium.
Further, described polyelectrolyte solution is the polyelectrolyte aqueous solution or organic solution.
Further, described polyelectrolyte solution is the aqueous solution of Lithium polyacrylate.
Further, described Lithium polyacrylate is obtained by reacting by polymer chemistry or adopts Lithium acrylate polymerization to obtain.
Further, specifically comprise the following steps:
(1) polyacrylic acid that mean molecule quantity is 1000 ~ 4000000 is taken, configuration LiOHH 2the O aqueous solution, joins LiOH dropwise in polyacrylic acid, until the pH value of solution is 8, above-mentioned gained solution is obtained solid matter Lithium polyacrylate after pervaporation, drying;
(2) Lithium polyacrylate and LiNi is taken 0.5mn 1.5o 4powder, be dissolved in water mixing, vacuumize, obtains Lithium polyacrylate Surface coating LiNi 0.5mn 1.5o 4positive electrode.
Further, specifically comprise the following steps:
(1) take mean molecule quantity be the polyacrylic acid of 3000 in container, take LiOHH 2o is dissolved in distilled water and obtains LiOH solution, LiOH dropwise is joined in polyacrylic acid, until the pH value of solution is 8, gained solution 80 DEG C heating is steamed to thick, then move to vacuum drying chamber in 100 DEG C of vacuumize 24h, obtain white solid matter Lithium polyacrylate;
(2) Lithium polyacrylate and the LiNi of certain mass is taken according to a certain percentage 0.5mn 1.5o 4powder, adds distilled water and fully dissolves mixing, moves to vacuumize vacuumize 24h at 100 DEG C, obtain Lithium polyacrylate Surface coating LiNi on electric jacket after tentatively evaporating 0.5mn 1.5o 4positive electrode.
Further, the coated part by weight of Lithium polyacrylate is 0.25 ~ 10%.Preferably, the coated part by weight of Lithium polyacrylate is 0.25 ~ 5%.
Polyelectrolyte comprises Lithium polyacrylate, polymethylacrylic acid lithium, poly lithium, poly-(methyl vinyl ether copolymerization maleic acid) lithium, poly-fumaric acid lithium, or the mixture of above several material.The side chain of above polymer all contains-COOLi group, polymer and LiOH, Li of-COOH group can be contained by side chain 2cO 3or both mixtures are obtained by polymer chemistry reaction; Also can contain-COOLi group vinyl monomer by side chain and be polymerized acquisition.Such polyelectrolyte typical is Lithium polyacrylate (PAALi), and because PAALi self-conductance rate is low, its application study for lithium ion polymer electrolyte is also less.But PAALi, is coated on electrode material, can be swelling under electrolyte effect, formation one deck is coated on the polymer film on electrode material.This film has very high lithium ion conduction ability, and meanwhile, PAALi decomposition electric potential is far above general electrolyte (LiPF 6, LiBOB etc.), the combination of two aspects can significantly improve LiNi 0.5mn 1.5o 4the chemical property of positive electrode.
The present invention compared with prior art tool has the following advantages:
1, the present invention by method for coating at LiNi 0.5mn 1.5o 4surface defines one deck polyelectrolyte film, enhances the compatibility with electrolyte, therefore has the feature of height ratio capacity, high magnification, long circulation life.
2, patent of the present invention is for the drawback of method for coating above, proposes polyelectrolyte Surface coating and improves LiNi 0.5mn 1.5o 4chemical property.This method for coating only needs low temperature drying, does not need high-temperature calcination, has simply, feature fast.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 and the charging and discharging curve of comparative example 1 under 0.5C compare.
Fig. 2 is embodiment 1 and the cycle performance curve of comparative example 1 under different multiplying.
Fig. 3 is embodiment 1 and the cycle performance curve of comparative example 1 under 1C multiplying power.
Embodiment
Embodiment 1
Taking mean molecule quantity is in polyacrylic acid 10.2g to the 200ml evaporating dish of 3000, takes LiOHH 2o2.32g, be dissolved in 36g distilled water and obtain LiOH solution, LiOH dropwise is joined in evaporating dish, until the pH value of solution is 8, above-mentioned gained solution is tentatively steamed to thick in electric jacket 80 DEG C, then mixture is moved to vacuum drying chamber in 100 DEG C of vacuumize 24h, obtain white solid matter PAALi.Take LiNi 0.5mn 1.5o 4finished product 4.975g, PAALi0.025g, in this mixture, PAALi mass fraction is 0.5%.By the LiNi taken 0.5mn 1.5o 4, PAALi0.025g fully dissolves and is mixed in 5mL water, electric jacket carries out preliminary stir evaporation after move to vacuum drying chamber in 100 DEG C of vacuumize 24h, obtain 5gLNM0.5%PAALi powder sample.
Take SuperP0.1g, LNM0.5%PAALi0.8g, solid content 3wt.% aqueous adhesive LA132(Chengdu Yindile Power Source Science and Technology Co., Ltd) 3.3ml, intermittently again add 3ml absolute ethyl alcohol and 2ml distilled water, in agate mortar, manual mixing grinding 2.5h, is deployed into the slurry of certain viscosity.Deployed slurry is coated on 20 μm of thick aluminium foils, makes with card punch the electrode slice that diameter is 1.2cm.Under vacuo after 100 DEG C of oven dry, take Cellgard2400 as barrier film, LiPF 6solution is that electrolyte is assembled into 2032 button cells, charging/discharging voltage scope 3.3 ~ 5V, measures it and is respectively 119.6mAh/g, 120.5mAh/g, 112.9mAh/g, 104.8mAh/g, 95.1mAh/g, 75.5mAh/g and 123mAh/g at the specific discharge capacity of 0.2C, 0.5C, 1C, 2C, 6C, 12C and 0.2C; Then measure its charge and discharge cycles 200 times under 1C, capability retention is 91.7%.Compare with the charging and discharging curve of comparative example 1 under 0.5C and show, the charging voltage platform of embodiment 1 is low, and discharge voltage plateau is high, and efficiency for charge-discharge significantly improves; Show with the cyclic curve of comparative example 1 under different multiplying, the high rate performance of embodiment 1 especially high rate capability significantly improves; Compare with 200 cyclic curves of comparative example 1 under 1C and show, embodiment 1 has higher specific capacity, better capability retention.
Embodiment 2
According to the method described in embodiment 1, preparation PAALi.Take LiNi 0.5mn 1.5o 4finished product 4.8500g, PAALi0.150g, in this mixture, PAALi mass fraction is 3%.By the LiNi taken 0.5mn 1.5o 4, PAALi0.150g fully dissolves and is mixed in 5mL water, electric jacket carries out preliminary stir evaporation after move to vacuum drying chamber in 100 DEG C of vacuumize 24h, obtain 5gLNM3%PAALi powder sample.According to the method preparation also assembled battery described in embodiment 1, measure it and be respectively 118.5mAh/g, 116.7mAh/g, 113.7mAh/g, 110.6mAh/g, 99.1mAh/g, 84.6mAh/g and 119.5mAh/g at the specific discharge capacity of 0.2C, 0.5C, 1C, 2C, 6C, 12C and 0.2C; Then measure its charge and discharge cycles 200 times under 1C, capability retention is 88.9%.
Embodiment 3
According to the method described in embodiment 1, preparation PAALi.Take LiNi 0.5mn 1.5o 4finished product 4.9500g, PAALi0.050g, in this mixture, PAALi mass fraction is 1%.By the LiNi taken 0.5mn 1.5o 4, PAALi0.050g fully dissolves and is mixed in 5mL water, electric jacket carries out preliminary stir evaporation after move to vacuum drying chamber in 100 DEG C of vacuumize 24h, obtain 5gLNM1%PAALi powder sample.According to the method preparation also assembled battery described in embodiment 1, measure it and be respectively 125.5mAh/g, 121.5mAh/g, 117.3mAh/g, 110.6mAh/g, 96.3mAh/g, 74.1mAh/g and 122.7mAh/g at the specific discharge capacity of 0.2C, 0.5C, 1C, 2C, 6C, 12C and 0.2C; Then measure its charge and discharge cycles 200 times under 1C, capability retention is 84.3%.
Embodiment 4
According to the method described in embodiment 1, preparation PAALi.Take LiNi 0.5mn 1.5o 4finished product 4.9875g, PAALi0.0125g, in this mixture, PAALi mass fraction is 0.25%.By the LiNi taken 0.5mn 1.5o 4, PAALi0.025g fully dissolves and is mixed in 5mL water, electric jacket carries out preliminary stir evaporation after move to vacuum drying chamber in 100 DEG C of vacuumize 24h, obtain 5gLNM0.25%PAALi powder sample.According to the method preparation also assembled battery described in embodiment 1, measure it and be respectively 119.5mAh/g, 118.6mAh/g, 109.6mAh/g, 104.1mAh/g, 92mAh/g, 78.4mAh/g and 118.7mAh/g at the specific discharge capacity of 0.2C, 0.5C, 1C, 2C, 6C, 12C and 0.2C; Then measure its charge and discharge cycles 200 times under 1C, capability retention is 88.9%.
Comparison example 1
According to the method described in embodiment 1 only to LiNi 0.5mn 1.5o 4(without PAALi) is prepared and tests chemical property.Measure it and be respectively 122.1mAh/g, 115.4mAh/g, 110.4mAh/g, 77.3mAh/g, 49.6mAh/g and 117.2mAh/g at the specific discharge capacity of 0.2C, 0.5C, 1C, 2C, 6C, 12C and 02C; Then measure its charge and discharge cycles 200 times under 1C, capability retention is 56.4%.

Claims (8)

1. the coated LiNi of polyelectrolyte 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that, the coated LiNi of application polyelectrolyte solution 0.5mn 1.5o 4, then drying obtains the coated LiNi of polyelectrolyte 0.5mn 1.5o 4, described polyelectrolyte is the mixture of a kind of or above several material in Lithium polyacrylate, polymethylacrylic acid lithium, poly lithium, poly-(methyl vinyl ether copolymerization maleic acid) lithium or poly-fumaric acid lithium.
2. the coated LiNi of a kind of polyelectrolyte according to claim 1 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that, described polyelectrolyte solution is the polyelectrolyte aqueous solution or organic solution.
3. the coated LiNi of a kind of polyelectrolyte according to claim 2 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that: described polyelectrolyte solution is the aqueous solution of Lithium polyacrylate.
4. the coated LiNi of a kind of polyelectrolyte according to claim 3 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that: described Lithium polyacrylate is obtained by reacting by polymer chemistry or adopts Lithium acrylate to be polymerized and obtains.
5. the coated LiNi of a kind of polyelectrolyte according to claim 4 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that, specifically comprises the following steps:
(1) polyacrylic acid that mean molecule quantity is 1000 ~ 4000000 is taken, configuration LiOHH 2the O aqueous solution, joins LiOH dropwise in polyacrylic acid, until the pH value of solution is 8, gained solution is obtained solid matter Lithium polyacrylate after pervaporation, drying;
(2) Lithium polyacrylate and LiNi is taken 0.5mn 1.5o 4powder, be dissolved in water mixing, vacuumize, obtains Lithium polyacrylate Surface coating LiNi 0.5mn 1.5o 4positive electrode.
6. the coated LiNi of a kind of polyelectrolyte according to claim 5 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that, specifically comprises the following steps:
(1) take mean molecule quantity be the polyacrylic acid of 3000 in container, take LiOHH 2o is dissolved in distilled water and obtains LiOH solution, LiOH dropwise is joined in polyacrylic acid, until the pH value of solution is 8, gained solution 80 DEG C heating is steamed to thick, then move to vacuum drying chamber in 100 DEG C of vacuumize 24h, obtain white solid matter Lithium polyacrylate;
(2) Lithium polyacrylate and the LiNi of certain mass is taken according to a certain percentage 0.5mn 1.5o 4powder, adds distilled water and fully dissolves mixing, moves to vacuumize vacuumize 24h at 100 DEG C, obtain Lithium polyacrylate Surface coating LiNi on electric jacket after tentatively evaporating 0.5mn 1.5o 4positive electrode.
7. the coated LiNi of a kind of polyelectrolyte according to claim 4 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that, the coated part by weight of Lithium polyacrylate is 0.25 ~ 10%.
8. the coated LiNi of a kind of polyelectrolyte according to claim 7 0.5mn 1.5o 4the preparation method of positive electrode, is characterized in that, the coated part by weight of Lithium polyacrylate is 0.25 ~ 5%.
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CN108807863A (en) * 2017-05-05 2018-11-13 宁德时代新能源科技股份有限公司 Modified positive electrode active material, preparation method thereof and electrochemical energy storage device
CN106981639B (en) * 2017-05-11 2020-07-14 江苏道赢科技有限公司 Preparation method of organic salt coated lithium iron phosphate cathode material
CN108232138A (en) * 2017-12-20 2018-06-29 中国科学院青岛生物能源与过程研究所 A kind of solid state lithium battery low internal resistance positive electrode and preparation method thereof
CN109273674A (en) * 2018-07-31 2019-01-25 广东工业大学 A kind of tertiary cathode material and its preparation method and application of Lithium polyacrylate cladding
CN113823794B (en) * 2021-08-04 2023-04-14 北京泰和九思科技有限公司 Method for modifying positive electrode material coated by organic metal framework based polymer electrolyte
CN115806290A (en) * 2022-12-06 2023-03-17 广东凯金新能源科技股份有限公司 Artificial graphite lithium ion battery cathode material and preparation method thereof

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CN102881861A (en) * 2012-09-26 2013-01-16 中南大学 High-temperature lithium ion battery anode slice
CN103534843A (en) * 2012-05-07 2014-01-22 西奥公司 Coated particles for lithium battery cathodes

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CN101807714A (en) * 2009-02-16 2010-08-18 三洋电机株式会社 Rechargeable nonaqueous electrolytic battery and manufacture method thereof
CN103534843A (en) * 2012-05-07 2014-01-22 西奥公司 Coated particles for lithium battery cathodes
CN102881861A (en) * 2012-09-26 2013-01-16 中南大学 High-temperature lithium ion battery anode slice

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Denomination of invention: Preparation of LiNi0.5Mn1.5O4anode material coated with polyelectrolyte

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