CN103915616A - Preparation method of lithium battery LiNi0.5Mn1.5O4 positive electrode material with hollow structure - Google Patents
Preparation method of lithium battery LiNi0.5Mn1.5O4 positive electrode material with hollow structure Download PDFInfo
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- CN103915616A CN103915616A CN201410152043.1A CN201410152043A CN103915616A CN 103915616 A CN103915616 A CN 103915616A CN 201410152043 A CN201410152043 A CN 201410152043A CN 103915616 A CN103915616 A CN 103915616A
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- lithium
- mnco
- nickel
- ethyl alcohol
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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
- 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
- H01M4/36—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 discloses a preparation method of a lithium battery LiNi0.5Mn1.5O4 positive electrode material with a hollow structure. The method comprises the following steps: preparing MnCO3 precursor micro-spheres with high monodispersity and uniform sizes from soluble manganese salt and sodium bicarbonate serving as raw materials at the room temperature by taking water and a small amount of ethanol as reaction solvents; reacting a precursor surface layer with Li2CO3 and nickel nitrate according to a Coriolis-Tyndall effect by taking the MnCO3 precursor obtained in the precious step as a spherical template as well as an Mn source to generate the lithium battery LiNi0.5Mn1.5O4 positive electrode material with a remarkable simple structure. The method has the characteristics of simple process, cheap raw materials, room-temperature preparation of a template material, low cost, controllability of the microstructure and size of the positive electrode material, and the like.
Description
Technical field
The present invention relates to lithium battery material technical field, relate in particular to a kind of lithium battery LiNi of hollow structure
0.5mn
1.5o
4the preparation method of positive electrode.
Background technology
Lithium ion battery is as a kind of novel green high-energy battery, because its operating voltage is high, specific capacity is large, have extended cycle life, self-discharge rate is low, memory-less effect and the advantage such as environmentally friendly, is widely used in the portable sets such as mobile phone, video camera, notebook computer.And along with in electric automobile, cordless power tool and military application, the energy density of lithium ion battery is had higher requirement, this just needs the positive electrode of development of new.LiCoO with stratiform
2and LiNiO
2compare, the lithium manganese oxide of spinel-type becomes one of focus of current anode material for lithium-ion batteries research because of advantages such as inexpensive, practical, environmentally safe, high-energy-densities.But, in lithium ion battery, the lithium manganese oxide of spinel-type is in deep discharge process, its thing changes Tetragonal into by Emission in Cubic, the volume of structure cell unit has increased by 6.5%, cause spinel structure generation deformation, produce destruction, make capacity attenuation, so it can only discharge and recharge in 4V region, but there is obvious energy loss.In order to improve the cycle performance of such material, people have adopted the LiM with spinel structure of Transition metal substituted
xmn
2-xo
4(M:Cr, Co, Fe, Ni, Cu) caused people's extensive concern, and they exist a high voltage platform more than 4.5V, have higher energy density.In this class material, study maximum be LiNi
0.5mn
1.5o
4, because it only exists high voltage platform near 4.7V, and there is higher capacity and good cycle performance.At present, LiNi
0.5mn
1.5o
4synthetic method a lot, have sol-gel processing, coprecipitation, compound carbonate method, ultrasonic atomization high-temperature decomposition, high temperature solid-state method etc.But about with MnCO
3micron ball is that presoma and spherical template are prepared the high-performance lithium battery LiNi with hollow sphere architectural feature
0.5mn
1.5o
4positive electrode there is not yet report.Solid phase method synthesis technique is simple, and cost is low, and is easy to practical application very much, is the industrial method that battery material extensively adopts of preparing.
The present invention's manganese sulfate, sodium acid carbonate is that raw material is prepared a kind of MnCO in the aqueous solution that contains a small amount of ethanol
3micron ball precursor.The MnCO that utilizes homogeneous to disperse
3micron ball, as manganese source and template, reacts and ion diffusion effect by solid-phase sintering, and lithium ion and nickel ion generate in micron ball surface reaction
LiNi
0.5mn
1.5o
4nano particle because ion diffusion rate difference is assembled into hollow micron ball.The present invention has the features such as technique is simple, raw material is cheap, cost is low, appearance and size is controlled.
Summary of the invention
The object of the invention is for high pressure anode material for lithium-ion batteries LiNi
0.5mn
1.5o
4the problems such as ion diffusion rate is low, and cyclical stability is undesirable, provide a kind of LiNi with special hollow structure and size homogeneous
0.5mn
1.5o
4positive electrode.
The MnCO that the present invention utilizes
3micron ball, as template and manganese source, is to prepare in the mixed solvent generation precipitation reaction of second alcohol and water by soluble manganese salt and sodium acid carbonate.Without adopting surfactant, additive, preparation method is simple.
The present invention adopts following technical scheme:
The lithium battery LiNi of a kind of hollow structure of the present invention
0.5mn
1.5o
4the preparation method's of positive electrode concrete steps are as follows:
(1) take soluble manganese salt and sodium acid carbonate as reaction raw materials, the mol ratio of manganese salt and sodium acid carbonate is 3:1～1:5, manganese salt and sodium acid carbonate are dissolved in and in absolute ethyl alcohol, make the mixture mixing, the mol ratio of absolute ethyl alcohol and solid salt is 10:1～100:1, at room temperature above-mentioned dispersed mixture is added to the water and prepares precursor MnCO
3micron ball, the volume ratio of institute's water and absolute ethyl alcohol is 10:1～50:1;
(2) precursor MnCO step (1) being obtained
3micron ball is collected by centrifugal or filtration, is then dried processing, and baking temperature is at 20～100 ℃;
(3) MnCO step (2) being obtained
3micron ball mixes with lithium, nickel raw material, MnCO
3, lithium, nickel mol ratio be 1.5:1～1.5:0.5, described by MnCO
3micron ball, lithium, nickel method for mixing raw materials are planetary type ball-milling or mortar mill;
(4) solid mixture step (3) being obtained in air atmosphere at 700～1000 ℃ sintered heat insulating 8～36h, obtain hollow structure LiNi after naturally cooling to room temperature
0.5mn
1.5o
4positive electrode.
In step (1), soluble manganese salt is manganese sulfate.
In step (1), the mol ratio of manganese salt and sodium acid carbonate is preferably 1:1; The mol ratio of absolute ethyl alcohol and solid salt is preferably 50:1; The volume ratio of water and absolute ethyl alcohol is preferably 20:1.
In step (2), baking temperature is preferably 60 ℃.
In step (3), described lithium raw material is lithium carbonate or lithium hydroxide, and nickel raw material is nickel oxide or nickel nitrate.
In step (3), and the MnCO that obtains of step (2)
3micron ball and lithium, nickel raw material are dispersed in absolute ethyl alcohol, and the mol ratio of absolute ethyl alcohol and above-mentioned raw materials summation is 10:1～20:1, are fully mixed and are placed on blowing-type oven for drying by planetary type ball-milling or mortar mill.
In step (3), MnCO
3, lithium, nickel mol ratio be preferably 1.5:1.2:0.5.
In step (4), preferably sintered heat insulating 24h at 800 ℃.
The overall diameter of the hollow microsphere structure that the present invention makes is 2～3 μ m, wall thickness 0.5～1.5 μ m of hollow microsphere structure.
Good effect of the present invention is as follows:
(1) method provided by the invention has the features such as technique is simple, raw material sources are extensive, cost is low, appearance and size is controlled, is easy to realize suitability for industrialized production.
(2) as the MnCO of predecessor template
3micron ball has template sizing concurrently and manganese source double action is provided.
(3) prepared hollow structure LiNi
0.5mn
1.5o
4positive electrode is formed by nanocrystalline self assembly.
(4) prepared hollow structure LiNi
0.5mn
1.5o
4positive electrode ionic conductivity excellence, is assembled in charge-discharge performance in battery and stablizes.
Accompanying drawing explanation
Fig. 1 is the lithium battery LiNi of hollow structure in embodiment 2
0.5mn
1.5o
4the process chart of the preparation process of positive electrode.
Fig. 2 is the precursor MnCO of preparation in embodiment 1
3the XRD collection of illustrative plates of micron ball.
Fig. 3 is the precursor MnCO of preparation in embodiment 1
3the stereoscan photograph of micron ball.
Fig. 4 is the precursor MnCO of preparation in embodiment 1
3the transmission electron microscope photo of micron ball.
Fig. 5 is the spinel-type LiNi of the hollow structure of preparation in embodiment 1
0.5mn
1.5o
4xRD collection of illustrative plates.
Fig. 6 is the spinel-type LiNi of the hollow structure of preparation in embodiment 1
0.5mn
1.5o
4transmission electron microscope photo.
Fig. 7 is the lithium battery LiNi of the hollow structure of preparation in embodiment 1
0.5mn
1.5o
4the typical charging and discharging curve figure of positive electrode.
Fig. 8 is the lithium battery LiNi of the hollow structure of preparation in embodiment 1
0.5mn
1.5o
4the cycle performance schematic diagram of positive electrode.
Embodiment
The following examples are to describe in further detail of the present invention.
Embodiment 1.
Under room temperature magnetic agitation, 1.7075g manganese sulfate and 4.1163g sodium acid carbonate are scattered in 35mL absolute ethyl alcohol, this solution is joined in 700mL absolute ethyl alcohol, generate immediately white opacity solution, continue to stir 3h it is reacted completely, with this MnCO of centrifugal process separated and collected
3after presoma product, with absolute ethanol washing, 60 ℃ of vacuumizes.X-ray diffractogram and electromicroscopic photograph explanation product are MnCO
3micron ball (Fig. 2, Fig. 3 and Fig. 4).By the synthetic 1.724g said method MnCO obtaining
3micron ball and 1.454g nickel nitrate, 0.384g lithium carbonate ground and mixed.The good pressed powder of abundant ground and mixed is placed in to Muffle furnace 800 ℃ of sintering 24h under air atmosphere.X-ray diffractogram and transmission electron microscope photo illustrate the spinel-type LiNi that this black product is hollow structure
0.5mn
1.5o
4.(Fig. 5, Fig. 6).
Embodiment 2.
At room temperature, prepare precursor MnCO according to embodiment 1
3micron ball, and it is dispersed in 15mL absolute ethyl alcohol together with 1.454g nickel nitrate, 0.384g lithium carbonate.Fully mix and be placed on blowing-type oven for drying by planetary ball mill ball milling 1h, be placed in Muffle furnace 800 ℃ of sintering 24h under air atmosphere, obtain hollow structure spinel-type LiNi
0.5mn
1.5o
4.
Embodiment 3.
At room temperature, prepare precursor MnCO according to embodiment 1
3micron ball, by the synthetic 1.724g said method MnCO obtaining
3micron ball and 1.454g nickel nitrate, 0.461g lithium carbonate ground and mixed.The good pressed powder of abundant ground and mixed is placed in to Muffle furnace 800 ℃ of sintering 24h under air atmosphere.Obtain the spinel-type LiNi of hollow structure
0.5mn
1.5o
4.
Embodiment 4.
At room temperature, prepare precursor MnCO according to embodiment 1
3micron ball, and it is dispersed in 15mL absolute ethyl alcohol together with 1.454g nickel nitrate, 0.461g lithium carbonate.Fully mix and be placed on blowing-type oven for drying by planetary ball mill ball milling 1h, be placed in Muffle furnace 800 ℃ of sintering 24h under air atmosphere, obtain hollow structure spinel-type LiNi
0.5mn
1.5o
4.
The lithium battery LiNi of embodiment 5. hollow structures of the present invention
0.5mn
1.5o
4the performance of positive electrode
By the lithium battery LiNi of hollow structure of the present invention
0.5mn
1.5o
4the experimental data that positive electrode is assembled in the aspect such as charge-discharge cycle in battery is as follows.
Assembling button cell, the preparation of anode electrode is the hollow structure LiNi prepared by embodiment 1
0.5mn
1.5o
4positive electrode: binding agent: the mass percent of conductive agent is 90: 6: 4, metal lithium sheet is negative electrode.The charge-discharge performance of test battery under 2C multiplying power, discharge capacity is 120mAh/g first.After 200 charge and discharge cycles, capacity is that 118mAh/g(capability retention is 98%), a coulomb efficiency for charge-discharge remains on 90～100%.(Fig. 7, Fig. 8)
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (10)
1. the lithium battery LiNi of a hollow structure
0.5mn
1.5o
4the preparation method of positive electrode, is characterized in that: the concrete steps of described method are as follows:
(1) take soluble manganese salt and sodium acid carbonate as reaction raw materials, the mol ratio of manganese salt and sodium acid carbonate is 3:1～1:5, manganese salt and sodium acid carbonate are dissolved in and in absolute ethyl alcohol, make the mixture mixing, the mol ratio of absolute ethyl alcohol and solid salt is 10:1～100:1, at room temperature above-mentioned dispersed mixture is added to the water and prepares precursor MnCO
3micron ball, the volume ratio of institute's water and absolute ethyl alcohol is 10:1～50:1;
(2) precursor MnCO step (1) being obtained
3micron ball is collected by centrifugal or filtration, is then dried processing, and baking temperature is at 20～100 ℃;
(3) MnCO step (2) being obtained
3micron ball mixes with lithium, nickel raw material, MnCO
3, lithium, nickel mol ratio be 1.5:1～1.5:0.5, described by MnCO
3micron ball, lithium, nickel method for mixing raw materials are planetary type ball-milling or mortar mill;
(4) solid mixture step (3) being obtained in air atmosphere at 700～1000 ℃ sintered heat insulating 8～36h, obtain hollow structure LiNi after naturally cooling to room temperature
0.5mn
1.5o
4positive electrode.
2. preparation method as claimed in claim 1, is characterized in that: in step (1), soluble manganese salt is manganese sulfate.
3. preparation method as claimed in claim 1, is characterized in that: in step (1), the mol ratio of manganese salt and sodium acid carbonate is 1:1.
4. preparation method as claimed in claim 1, is characterized in that: in step (1), the mol ratio of absolute ethyl alcohol and solid salt is 50:1.
5. preparation method as claimed in claim 1, is characterized in that: in step (1), the volume ratio of institute's water and absolute ethyl alcohol is 20:1.
6. preparation method as claimed in claim 1, is characterized in that: in step (2), baking temperature is 60 ℃.
7. preparation method as claimed in claim 1, is characterized in that: in step (3), described lithium raw material is lithium carbonate or lithium hydroxide, and nickel raw material is nickel oxide or nickel nitrate.
8. preparation method as claimed in claim 1, is characterized in that: in step (3), and the MnCO that obtains of step (2)
3micron ball and lithium, nickel raw material are dispersed in absolute ethyl alcohol, and the mol ratio of absolute ethyl alcohol and above-mentioned raw materials summation is 10:1～20:1, are fully mixed and are placed on blowing-type oven for drying by planetary type ball-milling or mortar mill.
9. preparation method as claimed in claim 1, is characterized in that: in step (3), and MnCO
3, lithium, nickel mol ratio be 1.5:1.2:0.5.
10. preparation method as claimed in claim 1, is characterized in that: in step (4), and sintered heat insulating 24h at 800 ℃.
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Cited By (5)
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|---|---|---|---|---|
| CN106082361A (en) * | 2016-06-03 | 2016-11-09 | 北京理工大学 | A kind of preparation method of anode material for lithium-ion batteries hollow porous nano/submicron multilevel hierarchy nickel ion doped |
| CN109599553A (en) * | 2018-11-20 | 2019-04-09 | 湘潭大学 | A kind of hollow sphere nickel sodium manganate and preparation method thereof, sodium-ion battery positive plate and sodium-ion battery |
| CN110970612A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | Preparation of transition metal oxide positive electrode material and application of transition metal oxide positive electrode material in sodium ion battery |
| WO2020127526A1 (en) * | 2018-12-19 | 2020-06-25 | Haldor Topsøe A/S | Lithium positive electrode active material |
| CN114105221A (en) * | 2021-11-23 | 2022-03-01 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Diamond high-voltage LiNi prepared by template method for lithium ion battery0.5Mn1.5O4Method for preparing anode material |
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| CN110970612A (en) * | 2018-09-29 | 2020-04-07 | 中国科学院大连化学物理研究所 | Preparation of transition metal oxide positive electrode material and application of transition metal oxide positive electrode material in sodium ion battery |
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| CN114105221A (en) * | 2021-11-23 | 2022-03-01 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | Diamond high-voltage LiNi prepared by template method for lithium ion battery0.5Mn1.5O4Method for preparing anode material |
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