CN104466163A - Preparation method of carbon-coating lithium ion battery positive material - Google Patents

Preparation method of carbon-coating lithium ion battery positive material Download PDF

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Publication number
CN104466163A
CN104466163A CN201410712826.0A CN201410712826A CN104466163A CN 104466163 A CN104466163 A CN 104466163A CN 201410712826 A CN201410712826 A CN 201410712826A CN 104466163 A CN104466163 A CN 104466163A
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carbon
coated
preparation
lithium
ion battery
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CN201410712826.0A
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Inventor
余志勇
刘韩星
王壮
李文姬
卢梦云
郑振宁
吴莎
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M4/36—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
    • 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

The invention belongs to the field of a lithium ion battery, and particularly relates to a preparation method of a carbon-coating lithium ion battery positive material. The method comprises the following steps: (1) ball milling positive material Li1.8Mn0.8Co0.2O2.8 with a carbon source in a mixture of ethanol and water; and (2) drying and grinding the ball milled mixture, preserving heat at a given heat treatment temperature, and cooling to obtain the carbon-coating lithium ion battery positive material. The preparation method has beneficial effects that the process is simple, the synthesis temperature is low, the cost is low, and a remarkable effect for improving the rate capacity of the Li1.8Mn0.8Co0.2O2.8 material can be realized.

Description

The preparation method of the anode material for lithium-ion batteries that carbon is coated
Technical field
The invention belongs to field of lithium ion battery, be specifically related to the anode material for lithium-ion batteries Li that a kind of carbon is coated 1.8mn 0.8co 0.2o 2.8preparation method.
Background technology
The application of lithium ion battery is just expanded to electric automobile field by portable type electronic product.This development trend is had higher requirement to the energy density of battery and power density.In recent years, rich lithium Layered Structural Positive Electrode Materials, due to its high actual specific capacity (200-250mAh/g), is considered to the very potential positive electrode system of one and develops rapidly.
Rich lithium stratified material can be considered Li 2mnO 3with LiMO 2the solid solution of (M=Mn, Ni, Co).But the conductance of this material system is usually lower, and the high rate performance which results in material is poor.Typically, the high rate performance of material reduces the particle diameter of material by technology controlling and process, the means such as the carbon of additional high price doped chemical and high conductivity and positive electrode compound are improved.These methods are at LiFePO 4etc. being proved to be the high rate performance that effectively can improve positive electrode in system.Wherein, the technical method of carbon clad anode material due to technique comparatively simple, cost is low, effective and be considered to one of good important means of feasibility.
But due to Li 2mnO 3-LiMO 2the particularity of system, existing carbon cladding process is poor effect on the rich lithium layer shape material system high rate performance of improvement.This is mainly because manganese mainly exists with+4 valency forms in lithium-rich anode material system, and traditional carbon cladding process needs to carry out high-temperature heat treatment under reducing atmosphere, and this can cause the reduction of manganese in rich lithium stratified material usually, thus the performance of deteriorated material.
Summary of the invention
The object of the present invention is to provide that a kind of cost is low, simple to operate, synthesis temperature is low and can the preparation method of the li-ion electrode positive electrode that heat treated carbon is coated under air, overcome the problem that the high rate performance of rich lithium Layered Structural Positive Electrode Materials system is not good.
The present invention solves the problems of the technologies described above adopted technical scheme: the preparation method of the anode material for lithium-ion batteries that carbon is coated, is characterized in that comprising the following steps:
1) by positive electrode Li 1.8mn 0.8co 0.2o 2.8the mixture being placed in second alcohol and water with carbon source carries out ball milling;
2), after the mixture drying after ball milling, grinding, be incubated under certain heat treatment temperature, after cooling, obtain the anode material for lithium-ion batteries that carbon is coated.
By such scheme, step 1) described in carbon source be glucose, sucrose or polyvinyl alcohol.
By such scheme, step 1) described in positive electrode Li 1.8mn 0.8co 0.2o 2.8be 1:0.05 ~ 0.10 with carbon source mass ratio.
By such scheme, step 2) described in heat treatment temperature be 400 ~ 450 DEG C.
By such scheme, step 2) described in heat treatment temperature retention time be 0.5 ~ 2h.
Positive electrode chemical formula of the present invention is Li 1.8mn 0.8co 0.2o 2.8, can 0.8Li be regarded as 2mnO 3-0.2LiCoO 2solid solution.
Beneficial effect of the present invention is: by heat-treating methods under air atmosphere, and the carbon that cracking produces is coated on positive electrode surface.What carbon source was formed under heat treatment has network-like carbon coating layer, can serve as the intergranular conductive media of positive electrode or passage, add the electron conduction of material, thus effectively improve the high rate performance of this material.This preparation method technique is simple, and synthesis temperature is low, and cost is low, at raising Li 1.8mn 0.8co 0.2o 2.8the high rate performance aspect of material has remarkable result.
Accompanying drawing explanation
Fig. 1 is not coated Li 1.8mn 0.8co 0.2o 2.8li after the coated process of different carbon source is prepared with the present invention 1.8mn 0.8co 0.2o 2.8the XRD of (positive electrode and carbon source quality are 1:0.10) contrasts collection of illustrative plates;
The carbon coated Li of Fig. 2 prepared by the embodiment of the present invention 2 1.8mn 0.8co 0.2o 2.8tEM figure;
Li after the coated process of the different carbon source of Fig. 3 prepared by the present invention 1.8mn 0.8co 0.2o 2.8(positive electrode and carbon source quality are 1:0.10) discharge curve first under 20mA/g and 50mA/g current density.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing and specific embodiment, the present invention is described in detail.
The invention process provides a kind of positive electrode active material for lithium ion battery with good high rate performance.
Comparative example
By positive active material Li 1.8mn 0.8co 0.2o 2.8mix by the mass ratio of 80:10:10 with acetylene black and Kynoar, be dissolved in 1-METHYLPYRROLIDONE, stir into pasted positive coating, be evenly coated on stainless steel substrate.The positive plate coated is placed in vacuum drying chamber, and at 80 DEG C, vacuumize was assembled for battery after 12 hours.
CR2025 type button cell is assembled in the MBRAUN glove box being full of high-purity argon gas.Wherein negative pole adopts that metal lithium sheet, electrolyte are EC:DMC (volume ratio 3:7), barrier film is Celgard.Adopt the charge-discharge performance (voltage range 2.0-4.8V) of Land CT2001A battery test system characterizing battery.
Test result shows, under the current density of 20mA/g, and Li 1.8mn 0.8co 0.2o 2.8first discharge specific capacity be 194.2mAh/g; During 50mAh/g, first discharge specific capacity is 125.4mAh/g, reduces 35.4% compared with being 20mA/g with current density.Embodiment 1
Take 2g Li 1.8mn 0.8co 0.2o 2.8be scattered in ethanol, take 0.1g glucose (C 12h 22o 11) be dissolved in 5ml deionized water, both mixing and ball milling 6h post-dryings.After sample grinding, be heated to 400 DEG C, insulation 1h, obtains the coated Li of carbon 1.8mn 0.8co 0.2o 2.8.
Adopt the method identical with comparative example 1 to prepare CR2025 type button cell, its charge-discharge performance is tested (voltage 2.0-4.8V).Test result shows, under the current density of 20mA/g, and the coated Li of carbon 1.8mn 0.8co 0.2o 2.8discharge capacity be first 220.7mAh/g; When current density is raised to 50mA/g, first discharge specific capacity is 206.7mAh/g, reduces 6.3% compared with being 20mA/g with current density.
Embodiment 2
Take 2g Li 1.8mn 0.8co 0.2o 2.8be scattered in ethanol, take 0.2g glucose (C 12h 22o 11) be dissolved in 5ml deionized water, both mixing and ball milling 6h post-dryings.After sample grinding, be heated to 400 DEG C, insulation 1h, obtains the coated Li of carbon 1.8mn 0.8co 0.2o 2.8.
Adopt the method identical with comparative example 1 to prepare CR2025 type button cell, its charge-discharge performance is tested (voltage 2.0-4.8V).Test result shows, under the current density of 20mA/g, and the coated Li of carbon 1.8mn 0.8co 0.2o 2.8discharge capacity be first 248.3mAh/g; When current density is raised to 50mA/g, first discharge specific capacity still remains on 232.5mAh/g, reduces 6.4% compared with being 20mA/g with current density.
Embodiment 3
Take 2g Li 1.8mn 0.8co 0.2o 2.8be scattered in ethanol, take 0.2g glucose (C 12h 22o 11) be dissolved in 5ml deionized water, both mixing and ball milling 6h post-dryings.After sample grinding, be heated to 450 DEG C, insulation 1h, obtains the coated Li of carbon 1.8mn 0.8co 0.2o 2.8.
Adopt the method identical with comparative example 1 to prepare CR2025 type button cell, its charge-discharge performance is tested (voltage 2.0-4.8V).Test result shows, under the current density of 20mA/g, and the coated Li of carbon 1.8mn 0.8co 0.2o 2.8discharge capacity be first 252mAh/g; When current density is raised to 50mA/g, first discharge specific capacity is 164.7mAh/g, reduces 34.6% compared with being 20mA/g with current density.
Embodiment 4
Take 2g Li 1.8mn 0.8co 0.2o 2.8be scattered in ethanol, take 0.2g glucose (C 12h 22o 11) be dissolved in 5ml deionized water, both mixing and ball milling 6h post-dryings.After sample grinding, be heated to 400 DEG C, insulation 0.5h, obtains the coated Li of carbon 1.8mn 0.8co 0.2o 2.8.
Adopt the method identical with comparative example 1 to prepare CR2025 type button cell, its charge-discharge performance is tested (voltage 2.0-4.8V).Test result shows, under the current density of 20mA/g, and the coated Li of carbon 1.8mn 0.8co 0.2o 2.8discharge capacity be first 239.9mAh/g; When current density is raised to 50mA/g, first discharge specific capacity is 176.7mAh/g, reduces 26.3% compared with being 20mA/g with current density.
Embodiment 5
Take 2g Li 1.8mn 0.8co 0.2o 2.8be scattered in ethanol, take 0.2g glucose (C 12h 22o 11) be dissolved in 5ml deionized water, both mixing and ball milling 6h post-dryings.After sample grinding, be heated to 400 DEG C, insulation 2h, obtains the coated Li of carbon 1.8mn 0.8co 0.2o 2.8.
Adopt the method identical with comparative example 1 to prepare CR2025 type button cell, its charge-discharge performance is tested (voltage 2.0-4.8V).Test result shows, under the current density of 20mA/g, and the coated Li of carbon 1.8mn 0.8co 0.2o 2.8discharge capacity be first 299.1mAh/g; When current density is raised to 50mA/g, first discharge specific capacity is 205mAh/g, reduces 31.5% compared with being 20mA/g with current density.
Embodiment 6
Take 2g Li 1.8mn 0.8co 0.2o 2.8be scattered in ethanol, take 0.2g sucrose (C 6h 12o 6h 2o) be dissolved in 5ml deionized water, both mixing and ball milling 6h post-dryings.After sample grinding, at being heated to 400 DEG C, insulation 1h, obtains the coated Li of carbon 1.8mn 0.8co 0.2o 2.8.
Adopt the method identical with comparative example 1 to prepare CR2025 type button cell, its charge-discharge performance is tested (voltage 2.0-4.8V).Test result shows, under the current density of 20mA/g, and the coated Li of carbon 1.8mn 0.8co 0.2o 2.8discharge capacity be first 229.8mAh/g; When current density is raised to 50mA/g, first discharge specific capacity is 205.5mAh/g, reduces 10.4% compared with being 20mA/g with current density.
Embodiment 7
Take 2g Li 1.8mn 0.8co 0.2o 2.8be scattered in ethanol, take 0.2g polyvinyl alcohol (PVA) and be dissolved in 5ml deionized water, both mixing and ball milling 6h post-dryings.After sample grinding, be heated at 400 DEG C, insulation 1h, obtains the coated Li of carbon 1.8mn 0.8co 0.2o 2.8.
Adopt the method identical with comparative example 1 to prepare CR2025 type button cell, its charge-discharge performance is tested (voltage 2.0-4.8V).Test result shows, under the current density of 20mA/g, and the coated Li of carbon 1.8mn 0.8co 0.2o 2.8discharge capacity be first 219.4mAh/g; When current density is raised to 50mA/g, first discharge specific capacity is 175.5mAh/g, reduces 20% compared with being 20mA/g with current density.
By the above detailed description to the embodiment of the present invention, can understand and the invention solves conventional rich lithium Layered Structural Positive Electrode Materials electricity rate and lead low, that high rate performance is poor problem.The cost of material adopted is low, and synthesis temperature is low, the coated Li of prepared carbon 1.8mn 0.8co 0.2o 2.8high rate performance is excellent.
As shown in Figure 1, be the XRD collection of illustrative plates of different carbon source powder coated in the embodiment of the present invention.As seen from the figure, coated front and back all obtain Li 1.8mn 0.8co 0.2o 2.8, the coated formation not affecting material thing phase of carbon.Figure 2 shows that the TEM figure of the coated basis material of glucose in the embodiment of the present invention 2, as can be seen from the figure the thickness of carbon-coating is about 5-10nm, evenly coated.Li after the coated process of the different carbon source of Fig. 3 prepared by the present invention 1.8mn 0.8co 0.2o 2.8(positive electrode and carbon source quality are 1:0.10) discharge curve first under 20mA/g and 50mA/g current density, can find out that the cycle performance of coated rear material improves obviously.
Be understandable that, the illustrative embodiments that above execution mode is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.

Claims (5)

1. the preparation method of the anode material for lithium-ion batteries that carbon is coated, is characterized in that comprising the following steps:
1) by positive electrode Li 1.8mn 0.8co 0.2o 2.8the mixture being placed in second alcohol and water with carbon source carries out ball milling;
2), after the mixture drying after ball milling, grinding, be incubated under certain heat treatment temperature, after cooling, obtain the anode material for lithium-ion batteries that carbon is coated.
2. the preparation method of the anode material for lithium-ion batteries that carbon according to claim 1 is coated, is characterized in that, step 1) described in carbon source be glucose, sucrose or polyvinyl alcohol.
3. the preparation method of the anode material for lithium-ion batteries that carbon according to claim 1 and 2 is coated, is characterized in that, step 1) described in positive electrode Li 1.8mn 0.8co 0.2o 2.8be 1:0.05 ~ 0.10 with carbon source mass ratio.
4. the preparation method of the anode material for lithium-ion batteries that carbon according to claim 3 is coated, is characterized in that, step 2) described in heat treatment temperature be 400 ~ 450 DEG C.
5. the preparation method of the anode material for lithium-ion batteries that the carbon according to claim 1 or 4 is coated, is characterized in that, step 2) described in heat treatment temperature retention time be 0.5 ~ 2h.
CN201410712826.0A 2014-11-28 2014-11-28 Preparation method of carbon-coating lithium ion battery positive material Pending CN104466163A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105789596A (en) * 2016-04-28 2016-07-20 北京大学深圳研究生院 Hypervolume lithium ion battery positive electrode material, and preparation method and application thereof
CN108183216A (en) * 2017-12-28 2018-06-19 国联汽车动力电池研究院有限责任公司 A kind of carbon coating lithium-rich manganese-based anode material and preparation method thereof and lithium ion battery
CN108695511A (en) * 2017-04-07 2018-10-23 王宏栋 Lithium ion battery material surface coated with conductive layer and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105789596A (en) * 2016-04-28 2016-07-20 北京大学深圳研究生院 Hypervolume lithium ion battery positive electrode material, and preparation method and application thereof
US11316160B2 (en) 2016-04-28 2022-04-26 Peking University Shenzhen Graduate School Supercapacity lithium ion battery cathode material, preparation method therefor and application thereof
CN108695511A (en) * 2017-04-07 2018-10-23 王宏栋 Lithium ion battery material surface coated with conductive layer and preparation method thereof
CN108695511B (en) * 2017-04-07 2021-04-02 王宏栋 Lithium ion battery material surface coating conductive layer and preparation method thereof
CN108183216A (en) * 2017-12-28 2018-06-19 国联汽车动力电池研究院有限责任公司 A kind of carbon coating lithium-rich manganese-based anode material and preparation method thereof and lithium ion battery
CN108183216B (en) * 2017-12-28 2020-10-09 国联汽车动力电池研究院有限责任公司 Carbon-coated lithium-rich manganese-based positive electrode material, preparation method thereof and lithium ion battery

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