CN108682843A - A kind of preparation method, anode material for lithium-ion batteries and the application of rock salt anode material for lithium-ion batteries - Google Patents
A kind of preparation method, anode material for lithium-ion batteries and the application of rock salt anode material for lithium-ion batteries Download PDFInfo
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- CN108682843A CN108682843A CN201810395136.5A CN201810395136A CN108682843A CN 108682843 A CN108682843 A CN 108682843A CN 201810395136 A CN201810395136 A CN 201810395136A CN 108682843 A CN108682843 A CN 108682843A
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- ion batteries
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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
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- 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 kind of preparation methods of rock salt anode material for lithium-ion batteries, include the following steps：(1) by lithium source, high-valence state manganese source, lower valency manganese source is ground is calcined under inert atmosphere after mixing, furnace cooling grinds to obtain LiMnO2Presoma；(2) LiMnO that will be obtained in step (1)2Presoma with lithium peroxide is ground calcines and make annealing treatment under inert atmosphere after mixing, furnace cooling obtains above-mentioned rock salt anode material for lithium-ion batteries Li4Mn2O5.The present invention correspondingly provides a kind of rock salt anode material for lithium-ion batteries and its application.Rock salt anode material for lithium-ion batteries Li in the present invention4Mn2O5For the rock-salt type structure of pure phase, free from admixture phase, electrochemical performance.
Description
Technical field
The invention belongs to the electrode materials and its preparation side of battery material field more particularly to a kind of lithium ion battery
Method, application.
Background technology
As the improvement of people's living standards, and traffic, communication and electronic information technology drastically development.Novel lithium from
The development of sub- battery, which evolves as, can reach high energy, longevity, safety and cheap, while reduce pollution and recoverable
Trend, this makes lithium ion battery towards higher energy density, the volume and capacity ratio of bigger, better safety and environment friend
Good property direction is developed.Meanwhile China's energy reserves amount is relatively low, import will also be leaned on by surpassing 50% oil demand amount at present, this
The serious fast development for limiting China's economy, especially present oil price grow steadily, and automobile power cell is grown rapidly
Epoch now, exploitation Vehicular dynamic battery become very necessary.
However, the performance of existing lithium ion battery be not achieved the following electric vehicle and energy-storage system application want
It asks, is required to continue to improve to improve.Anode material for lithium-ion batteries is always the most important field of lithium electricity research.Just with regard to lithium electricity
For the Materials trend of pole, the energy density and power density of lithium electricity are improved, this can be the basic hair of lithium battery over the next several years
Open up direction.Therefore, new electrode materials are developed, the performance of lithium ion battery is further promoted, is seeking to have height ratio capacity just
Pole material further promotes the energy density of lithium ion battery, it has also become the main direction of studying of current lithium ion battery.
The anode material for lithium-ion batteries generally used at present mainly has cobalt acid lithium (LiCoO2), LiFePO4
(LiFePO4), stratiform ternary material (LiNixMnyCo1-x-yO2), nickel galaxite (LiNi0.5Mn1.5O4) etc..But these materials
The specific capacity of material is in 270mAh/g hereinafter, such as nickel galaxite (LiNi0.5Mn1.5O4) although it has the work of 4.7V electric
Pressure, but its theoretical capacity only has 147mAh/g, and it practical can only achieve 130mAh/g.In addition, these above-mentioned materials there is also
It is expensive, the problems such as capacity attenuation is very fast under hot conditions.It would therefore be highly desirable to develop, a kind of specific capacity is high, of low cost, environment
Friendly anode material for lithium-ion batteries.
Invention content
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, one kind is provided
Preparation method, anode material for lithium-ion batteries and the application of anode material for lithium-ion batteries, above-mentioned lithium ion battery have specific volume
Measure the advantages such as high, of low cost.In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of preparation method of rock salt anode material for lithium-ion batteries, includes the following steps：
(1) by lithium source, high-valence state manganese source, lower valency manganese source is ground is calcined under inert atmosphere after mixing, with stove
Cooling grinding obtains LiMnO2Presoma；
(2) LiMnO that will be obtained in step (1)2Presoma and lithium peroxide are ground after mixing in inert atmosphere
Lower calcining simultaneously makes annealing treatment, and furnace cooling obtains above-mentioned rock salt anode material for lithium-ion batteries Li4Mn2O5。
In above-mentioned preparation method, it is preferred that the lithium source is lithium hydroxide or lithium carbonate, and the addition of the lithium source is it
1.05-1.15 times of theoretical amount.Lithium source has certain volatilization in high-temperature burning process, and when dispensing will properly increase its use
Amount can replenish the loss that lithium volatilizees in high-temperature burning process；But excessive lithium can cause to generate dephasign in product, lead
It causes object mutually impure, influences material property, its dosage of general control, which is 1.05-1.15 times of theoretical amount, to be advisable.
In above-mentioned preparation method, it is preferred that the high-valence state manganese source, lower valency manganese source chemical valence be respectively positive tetravalence with
Positive divalent, the high-valence state manganese source are 1 with the molar ratio that lower valency manganese source is added：1.
In above-mentioned preparation method, it is preferred that the high-valence state manganese source is manganese dioxide, and the lower valency manganese source is manganese carbonate
Or manganese monoxide.
In above-mentioned preparation method, it is preferred that be incorporated as its theoretical amount 1.30-1.40 times of the lithium peroxide.It crosses
Lithia easily forms molten mass in temperature-rise period, and volatilization loss is larger, in order to ensure products therefrom is pure phase, it is necessary to appropriate mistake
Amount.
In above-mentioned preparation method, the LiMnO that is obtained in step (1)2Presoma should not be put long after being prepared, and be typically prepared
Subsequent step (2) is carried out after obtaining (the brand-new LiMnO in step (1) is utilized i.e. in step (2)2Presoma), to ensure
LiMnO2The high reaction activity of presoma prepares anode material for lithium-ion batteries Li convenient for subsequent reactions4Mn2O5.Phase in the present invention
It is as follows to close chemical equation：
2LiOH+MnO2+ MnO=2LiMnO2+H2O
Li2CO3+MnO2+ MnO=2LiMnO2+CO2
Li2CO3+MnCO3+MnO2=2LiMnO2+2CO2
2Li2O2+4LiMnO2=2Li4Mn2O5+O2
In above-mentioned preparation method, it is preferred that in the step (1), calcination temperature is 900-1000 DEG C, calcination time 8-
10h.900-1000 DEG C of high-temperature calcination can ensure that a solid phase reaction carries out completely, and improve the crystallinity of product.Temperature
Too low, products obtained therefrom object is mutually impure；Temperature is excessively high, and particle is broken.
In above-mentioned preparation method, it is preferred that in the step (2), calcination temperature is 800-900 DEG C, calcination time 6-
12h；The temperature of annealing is 500-600 DEG C, and the annealing time is 3-6h.800-900 DEG C of calcination temperature can ensure
Solid phase reaction is complete, and improves the crystallinity of product；Annealing under low temperature can eliminate the crystalline substance in high-temperature burning process
Lattice defect improves the crystallinity of product, eliminates dephasign.
In above-mentioned preparation method, the step (1) is nitrogen or argon gas atmosphere with the inert atmosphere in step (2).Step
(1) inert atmosphere protection is used, is that presoma generates spinelle LiMn by oxidation in a solid phase reaction in order to prevent2O4Dephasign
And influence follow-up synthesis.Step (2) is protected using inert gas atmosphere, is to prevent the titanium dioxide in air for air-isolation
Carbon, water etc. are reacted with lithium peroxide, make its failure.
The technical concept total as one, the present invention also provides a kind of rock salt anode material for lithium-ion batteries, the rocks
The chemical formula of salt form anode material for lithium-ion batteries is：Li4Mn2O5, the crystal form of the rock salt anode material for lithium-ion batteries is
The theoretical specific capacity of the rock salt crystal form of single pure phase, no dephasign, the rock salt anode material for lithium-ion batteries reaches
355mAh/g.In the present invention, if there is other impurities phase in rock salt anode material for lithium-ion batteries, chemical property is unstable
It is fixed, using the LiMnO of brand-new2Presoma, lithium peroxide and annealing process can ensure the positive material being prepared in the present invention
Without dephasign in material.
The technical concept total as one, the present invention also provides a kind of answering for above-mentioned rock salt anode material for lithium-ion batteries
With the rock salt anode material for lithium-ion batteries to be used to prepare to the anode of lithium ion battery.Above-mentioned positive electrode is carried out
Chemical property analysis shows that：Under the conditions of 50mA/g, first discharge specific capacity is in 320mAh/g-330mAh/g；It follows for 30 times
After ring, capacity retention ratio is more than 98.5%.
Compared with the prior art, the advantages of the present invention are as follows：
1, the rock salt anode material for lithium-ion batteries Li in the present invention4Mn2O5Specific capacity it is high, be conventional lithium ion electricity
2-3 times of pond positive electrode.
2, by using the LiMnO of brand-new in the present invention2The control of the conditions such as presoma, lithium peroxide and annealing process,
Rock salt anode material for lithium-ion batteries Li4Mn2O5For the rock-salt type structure of pure phase, free from admixture phase, electrochemical performance.
3, preparation method of the present invention is easy to operate, raw material is cheap and easy to get, result favorable reproducibility, product are unanimously good, has pole
Big industrial application value.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is Li made from the embodiment of the present invention 14Mn2O5XRD diagram；
Fig. 2 is Li made from the embodiment of the present invention 24Mn2O5SEM figure；
Fig. 3 is Li made from the embodiment of the present invention 34Mn2O5First charge-discharge curve graph；
Fig. 4 is Li made from the embodiment of the present invention 34Mn2O5Cycle performance curve graph.
Specific implementation mode
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of rock salt anode material for lithium-ion batteries Li4Mn2O5Preparation method, include the following steps：
(1) mono- hydronium(ion) lithias of 9.231g, 8.694g manganese dioxide, 7.094g manganese oxide are mixed and planetary ball mill is added
30min is ground in machine to be sufficiently mixed, and obtains uniform mixture；
(2) step (1) is obtained into mixture and is heated to 1000 DEG C of calcining 8h, calcining in tube furnace, in a nitrogen atmosphere
After with stove natural cooling, calcined product is ground to obtain the brand-new LiMnO of black2Presoma；
(3) presoma 8.000g and 2.535g lithium peroxides obtained by step (2) are weighed, is placed in planetary ball mill and grinds
After 30min, it is warming up to 900 DEG C of calcination processing 6h in tube furnace, under nitrogen atmosphere, is cooled to 550 DEG C of annealing 3h later,
Furnace cooling after annealing finally obtains black powder material, the rock salt lithium ion cell positive as in the present embodiment
Material Li4Mn2O5。
Fig. 1 is Li made from the present embodiment4Mn2O5XRD diagram, as seen from the figure, the positive electrode obtained in the present embodiment is
The pure phase substance of rock salt structure, free from admixture phase.
By Li obtained in the present embodiment4Mn2O5Anode material for lithium-ion batteries is assembled into the test of CR2032 type button cells
The chemical property of material.As a result it shows：Under the conditions of 50mA/g, first discharge specific capacity 320.5mAh/g；It follows for 30 times
After ring, discharge capacitance 99.0%.
Wherein, above-mentioned assembling and test condition are as follows：
(1) by rock salt anode material for lithium-ion batteries Li obtained in the present embodiment4Mn2O5With acetylene black, polyvinylidene fluoride
Alkene (PVDF) is 8 according to mass ratio:1:1 ratio uniform mixing, is then pressed into piece, then the side with punching using tablet press machine
The dish-shaped thin slice of a diameter of 6mm is made in formula, and is dried in vacuo 12h under the conditions of 80 DEG C, and electrode slice is made；
(2) with the LiPF of 1mol/L6For electrolyte, microporous polypropylene membrane (Celgard 2400) is diaphragm, metal lithium sheet
For reference electrode, CR2032 type button cells are made in material in the glove box full of argon gas；
(3) under the conditions of 25 DEG C, the Land-CT2001A battery test system button type batteries of Wuhan Lan electricity companies are utilized
Carry out constant current charge-discharge test, test voltage ranging from 2.50V-4.95V.
Embodiment 2：
A kind of rock salt anode material for lithium-ion batteries Li4Mn2O5Preparation method, include the following steps：
(1) 7.770g lithium carbonates, 8.694g manganese dioxide, 7.094g manganese oxide are mixed to be added in planetary ball mill and is ground
30min is sufficiently mixed, and obtains uniform mixture；
(2) step (1) is obtained into mixture and is heated to 900 DEG C of calcining 10h, calcining in tube furnace, in a nitrogen atmosphere
After with stove natural cooling, calcined product is ground to obtain the brand-new LiMnO of black2Presoma；
(3) presoma 8.000g and 2.730g lithium peroxides obtained by step (2) are weighed, is placed in planetary ball mill and grinds
After 30min, it is warming up to 800 DEG C of calcination processing 7h in tube furnace, under nitrogen atmosphere, is cooled to 500 DEG C of annealing 3h later,
Furnace cooling after annealing finally obtains black powder material, the rock salt lithium ion cell positive as in the present embodiment
Material Li4Mn2O5。
The positive electrode obtained in the present embodiment is the pure phase substance of rock salt structure, free from admixture phase.It is obtained in the present embodiment
Positive electrode be powdery granule (as shown in Figure 2).
By Li obtained in the present embodiment4Mn2O5Anode material for lithium-ion batteries is assembled into the test of CR2032 type button cells
The chemical property of material.As a result it shows：Under the conditions of 50mA/g, first discharge specific capacity 325.5mAh/g；It follows for 30 times
After ring, discharge capacitance 99.5%.
Wherein, above-mentioned assembling and test condition are same as Example 1.
Embodiment 3：
A kind of rock salt anode material for lithium-ion batteries Li4Mn2O5Preparation method, include the following steps：
(1) 7.770g lithium carbonates, 11.495g manganese carbonates, 7.094g manganese oxide are mixed to be added in planetary ball mill and is ground
30min is sufficiently mixed, and obtains uniform mixture；
(2) step (1) is obtained into mixture and is heated to 900 DEG C of calcining 9h, calcining knot in tube furnace, in a nitrogen atmosphere
With stove natural cooling after beam, calcined product is ground to obtain the brand-new LiMnO of black2Presoma；
(3) presoma 8.000g and 2.630g lithium peroxides obtained by step (2) are weighed, is placed in planetary ball mill and grinds
After 30min, it is warming up to 800 DEG C of calcination processing 8h in tube furnace, under nitrogen atmosphere, is cooled to 600 DEG C of annealing 4h later,
Furnace cooling after annealing finally obtains black powder material, the rock salt lithium ion cell positive as in the present embodiment
Material Li4Mn2O5。
The positive electrode obtained in the present embodiment is the pure phase substance of rock salt structure, free from admixture phase.
By Li obtained in the present embodiment4Mn2O5Anode material for lithium-ion batteries is assembled into the test of CR2032 type button cells
The chemical property of material.As a result as shown in Figure 3 and Figure 4, from Fig. 3 and Fig. 4：Under the conditions of 50mA/g, discharge for the first time
Specific capacity is 327.5mAh/g；After 30 cycles, discharge capacitance 98.7%.
Wherein, above-mentioned assembling and test condition are same as Example 1.
Claims (10)
1. a kind of preparation method of rock salt anode material for lithium-ion batteries, which is characterized in that include the following steps：
(1) by lithium source, high-valence state manganese source, lower valency manganese source is ground is calcined under inert atmosphere after mixing, cooling grinding
Obtain LiMnO2Presoma；
(2) LiMnO that will be obtained in step (1)2Presoma with lithium peroxide is ground is calcined under inert atmosphere after mixing
And it makes annealing treatment to get to above-mentioned rock salt anode material for lithium-ion batteries Li4Mn2O5。
2. preparation method according to claim 1, which is characterized in that the lithium source be lithium hydroxide or lithium carbonate, it is described
The addition of lithium source is 1.05-1.15 times of its theoretical amount.
3. preparation method according to claim 1, which is characterized in that the high-valence state manganese source, lower valency manganese source chemical combination
Valence is respectively positive tetravalence and positive divalent, and the high-valence state manganese source is 1 with the molar ratio that lower valency manganese source is added：1.
4. preparation method according to claim 3, which is characterized in that the high-valence state manganese source is manganese dioxide, described low
Valence state manganese source is manganese carbonate or manganese monoxide.
5. preparation method according to claim 1, which is characterized in that the lithium peroxide is incorporated as its theoretical amount
1.30-1.40 again.
6. preparation method according to any one of claims 1-5, which is characterized in that in the step (1), calcination temperature
It is 900-1000 DEG C, calcination time 8-10h.
7. preparation method according to any one of claims 1-5, which is characterized in that in the step (2), calcination temperature
It is 800-900 DEG C, calcination time 6-12h；The temperature of annealing is 500-600 DEG C, and the annealing time is 3-6h.
8. a kind of rock salt anode material for lithium-ion batteries, which is characterized in that the rock salt anode material for lithium-ion batteries
Chemical formula is：Li4Mn2O5, the crystal form of the rock salt anode material for lithium-ion batteries is the rock salt crystal form of single pure phase.
9. rock salt anode material for lithium-ion batteries according to claim 8, which is characterized in that the rock salt lithium ion
Cell positive material is prepared by the preparation method described in any one of claim 1-7.
That 10. a kind of preparation method as described in any one of claim 1-7 is prepared or as described in claim 8 or 9
Rock salt anode material for lithium-ion batteries application, which is characterized in that by the rock salt anode material for lithium-ion batteries use
In the anode for preparing lithium ion battery.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694167A (en) * | 2011-08-30 | 2012-09-26 | 中国科学院宁波材料技术与工程研究所 | Modified lithium manganate positive pole material and preparation method thereof |
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2018
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694167A (en) * | 2011-08-30 | 2012-09-26 | 中国科学院宁波材料技术与工程研究所 | Modified lithium manganate positive pole material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| JINHAN YAO，ET AL.: ""Enhanced cycle ability of spinel LiMn2O4 by controlling the phase purity and structural strain"", 《JOURNAL OF PHYSICS AND CHEMISTRY OF SOLIDS》 * |
| M. FREIRE，ET AL.: ""A new active Li–Mn–O compound for high energy density Li-ion batteries"", 《NATURE MATERIALS》 * |
| MARIA DIAZ-LOPEZ，ET AL.: ""Local Structure and Lithium Diffusion Pathways in Li4Mn2O5 High Capacity Cathode Probed by Total Scattering and XANES"", 《CHEM. MATER.》 * |
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