CN108455676A - A kind of preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4 - Google Patents

A kind of preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4 Download PDF

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CN108455676A
CN108455676A CN201810263476.2A CN201810263476A CN108455676A CN 108455676 A CN108455676 A CN 108455676A CN 201810263476 A CN201810263476 A CN 201810263476A CN 108455676 A CN108455676 A CN 108455676A
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lithium
manganese
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anode material
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CN108455676B (en
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杨改
王波
秦显忠
蔡飞鹏
蒋波
高金华
陈花
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Energy Research Institute of Shandong Academy of Sciences
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    • 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
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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
    • 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
    • H01M4/50—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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Abstract

A kind of preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4, includes the following steps：Compound concentration be the manganese salt solution of 0.5 3M, a concentration of 1 5M citric acid solution and a concentration of 0.5 3M alkaline aqueous solution, first manganese salt solution is mixed with citric acid solution, alkaline solution is poured into mixed solution again after a small amount of water dilution is added, manganese precipitation is obtained after 20 30h of mixed solution aging, it will in proportion be mixed with lithium source after manganese precipitation repeatedly washing, dry, pre-burning, manganate cathode material for lithium obtained after 700 750 DEG C of high-temperature roastings.Lithium manganate material prepared by this method has that simple for process, product particle is thin, and specific capacity is high, the excellent feature of high rate performance.

Description

A kind of preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4
Technical field
The invention belongs to technical field of energy material, more particularly to a kind of anode material for lithium-ion batteries nano spinel manganese The preparation method of sour lithium.
Background technology
Currently in use and exploitation anode material for lithium-ion batteries mainly has：Layer structure cobalt acid lithium (LCO) and its Derivative Ni cobalt acid lithium (NCA) and nickel manganese cobalt acid lithium (NCM), lithium manganate having spinel structure (LMO) and its derivative Ni LiMn2O4 (LNMO), olivine-type LiFePO4 (LFP) etc..Lithium manganate material have it is resourceful, at low cost, pollution-free, safety is good, Wind is listened in the advantages that good rate capability, the daily output for accounting for global video automobile sales volume nearly 20%, and use is exactly lithium manganate battery.The material Material presently, there are the problem of be the factors such as dissolving, jahn teller effect and electrolyte decomposition during charge and discharge cycles due to manganese Caused by its capacity attenuation it is very fast, to constrain its commercialized development, numerous studies show lithium manganate material nanosizing Afterwards, the embedding dislocation point of lithium ion is increased, reduces material polarization, so that its structure is more stablized, chemical property also gets a promotion.
CN101237044 A disclose a kind of rock salt LiMn2O4 and preparation method thereof.Nano-scale lithium ion battery anode Material rock salt LiMn2O4 is Li2-XHXMnO3(0 X≤0.5 ＜).Using oxidizing manganese salt, obtained precipitation is transferred to Containing in lithium hydroxide (LiOH) solution water heating kettle；Or be directly mixed and stirred for oxidant, manganese salt and LiOH solution, it shifts Into water heating kettle；Above-mentioned water heating kettle is handled at 140~250 DEG C, after obtained sediment is filtered and is washed dry to get to Positive material rock salt Mn lithium of nano lithium ion battery.
Invention content
The object of the present invention is to provide it is a kind of it is simple for process, be suitable for industrialized production anode material for lithium-ion batteries nanometer The preparation method of spinel lithium manganate.
It is that nano material can be effective by preparing the reason of nano material improves manganate cathode material for lithium chemical property The generation for inhibiting Jiang Taile side reactions, inhibits the dissolving of manganese, shortens lithium ion deintercalation path, its specific surface area of increase appropriate, Also the electrode reaction rate of material surface can be improved.
A kind of preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4, includes the following steps：
(1) compound concentration is the manganese salt solution of 0.5-3M, the citric acid solution of a concentration of 1-5M and a concentration of 0.5-3M Alkaline aqueous solution；
(2) manganese salt solution is mixed in proportion with citric acid solution, a small amount of water dilution is added；
(3) alkaline solution is poured into the mixed solution of step (2), is stood after shaking up；
(4) step (3) resulting material is separated by solid-liquid separation, 80-100 DEG C of drying in an oven after washing precipitate repeatedly 2-6h obtains the manganese precipitation containing the crystallization water；
(5) step (4) products therefrom anhydrous manganese is obtained to precipitate after 500-600 DEG C of pre-burning；
(6) using a small amount of deionized water or absolute ethyl alcohol as medium, anhydrous manganese precipitation obtained by step (5) is distinguished with lithium source In terms of manganese and lithium, according to Li:The molar ratio of Mn=1-1.05 is mixed, is dried；
(7) step (6) products therefrom is being obtained into nanometer lithium manganate just in Muffle furnace after 700-750 DEG C of heat treatment 10-20h Pole material.
In the above preparation method, the manganese salt solution in step (1) is replaced with nickel manganese mixed solution, obtains nano nickel mangaic acid Lithium anode material；Nickel manganese molar ratio in the wherein described nickel manganese mixed solution is Ni:Mn=x:2-x, wherein x are that wherein x is 0.1-1.5, preferably 0.5-1.0.
In the above preparation method, the manganese salt described in step (1) be manganese sulfate, manganese acetate and manganese nitrate in one kind or It is a variety of；Alkaline aqueous solution is one or more in sodium hydroxide, ammonium hydroxide, sodium carbonate.
In the above preparation method, with citric acid respectively with manganese and citrometer, molar ratio is the Mn salt described in step (2) Mn:CA=2~0.5.
In the above preparation method, step (6) described lithium source is one or more in lithium hydroxide, lithium carbonate.
The beneficial effects of the invention are as follows prepare nano spinel manganate cathode material for lithium, LiMn2O4 using citric acid auxiliary law After material nano, the embedding dislocation point of lithium ion is increased, reduces material polarization, so that its structure is more stablized, chemical property Also it gets a promotion.
Description of the drawings：
Fig. 1 is the scanning electron microscope (SEM) photograph of present invention gained manganese carbonate product, and grain size is in 100-200nm；
Fig. 2 is the electron microscope of nanometer lithium manganate prepared by the present invention, and grain size is about 100nm.
Specific implementation mode
Embodiment 1
Manganese nitrate solution, the citric acid solution of 2M and the sodium carbonate liquor of 1M of 1M are configured, measures 20ml manganese nitrates respectively And 10ml citric acid solutions, after being mixed in beaker plus 100ml deionized waters dilute, and 50ml sodium carbonate is added in mixed solution Solution, mixing stand 10h after shaking up, and are washed with deionized water after precipitation is filtered, are taken out after 80 DEG C of dry 2h of baking oven repeatedly Manganese sesquioxide managnic oxide is obtained after 500 DEG C of heat treatment 6h in Muffle furnace, 15.8g manganese sesquioxide managnic oxides and 4g lithium carbonates are weighed, with anhydrous Ethyl alcohol is to be taken out in 80 DEG C of drying of baking oven after medium is fully ground mixing, is placed in take out after 750 DEG C of heat treatment 20h in Muffle furnace and obtain Obtain nanometer lithium manganate positive electrode.It is anode with the nanometer lithium manganate material, lithium piece is cathode assembled battery, measures it in room temperature Lower 3-4.5V voltage ranges, the first discharge specific capacity under 0.1C and 10C multiplying powers is respectively 128mAh/g and 100mAh/g.
Embodiment 2
The present embodiment place same as Example 1 repeats no more, the difference is that：Configure the nickel manganese mixed solution of 1M (Ni:Mn=1:3, molar ratio) instead of the manganese nitrate solution of 1M, nickel manganese mixed oxides are obtained after precipitation, pre-burning, are weighed 16g mixed oxides and 2.2g lithium hydroxides remove after being fully ground mixing as medium using deionized water in 60 DEG C of drying of baking oven, It is placed in take out after 720 DEG C of heat treatment 10h in Muffle furnace and obtains nano nickel lithium manganate positive electrode.With the nano nickel lithium manganate material For anode, lithium piece is cathode assembled battery, measures its 3-4.5V voltage range at room temperature, under 0.1C and 10C multiplying powers for the first time Specific discharge capacity is respectively 130mAh/g and 110mAh/g.
Embodiment 3
It directly weighs 15.8g and analyzes pure manganese sesquioxide managnic oxide and 4g lithium carbonates, mixing is fully ground by medium of absolute ethyl alcohol It is taken out afterwards in 80 DEG C of drying of baking oven, is placed in Muffle furnace and takes out acquisition manganate cathode material for lithium after 750 DEG C of heat treatment 20h.With this Lithium manganate material is anode, and lithium piece is cathode assembled battery, measures its ratio of electric discharge for the first time under 0.1C and 10C multiplying powers at room temperature Capacity is respectively 112mAh/g and 80mAh/g.
Comparative example 1
It configures the liquor potassic permanganate of 1M, 4g lithium carbonates is added, dried after being fully ground mixing as medium using absolute ethyl alcohol Obtained washing of precipitate and drying are placed in Muffle furnace and take out acquisition nanostructured manganese after 750 DEG C of heat treatment 20h by 160 DEG C of processing of case Sour lithium anode material.It is anode with the nanometer lithium manganate material, lithium piece is cathode assembled battery, measures its 3-4.5V at room temperature Voltage range, the first discharge specific capacity under 0.1C and 10C multiplying powers is respectively 114mAh/g and 85mAh/g.

Claims (6)

1. a kind of preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4, includes the following steps：
(1) compound concentration be the manganese salt solution of 0.5-3M, a concentration of 1-5M citric acid solution and a concentration of 0.5-3M alkalinity Aqueous solution；
(2) manganese salt solution is mixed in proportion with citric acid solution, a small amount of water dilution is added；
(3) alkaline solution is poured into the mixed solution of step (2), is stood after shaking up；
(4) step (3) resulting material is separated by solid-liquid separation, repeatedly 80-100 DEG C of dry 2- in an oven after washing precipitate 6h obtains the manganese precipitation containing the crystallization water；
(5) step (4) products therefrom anhydrous manganese is obtained to precipitate after 500-600 DEG C of pre-burning；
(6) using a small amount of deionized water or absolute ethyl alcohol as medium, by anhydrous manganese precipitation obtained by step (5) with lithium source respectively with manganese With lithium meter, according to Li:The molar ratio of Mn=1-1.05 is mixed, is dried；
(7) step (6) products therefrom is obtained into nanometer lithium manganate anode material in Muffle furnace after 700-750 DEG C of heat treatment 10-20h Material.
2. according to the method described in claim 1, it is characterized in that：Replace the manganese salt in step (1) molten with nickel manganese mixed solution Liquid obtains nano nickel lithium manganate positive electrode；Nickel manganese molar ratio in the wherein described nickel manganese mixed solution is Ni:Mn=x:2-x, Wherein x is 0.1-1.5, preferably 0.5-1.0.
3. according to the method described in claim 1, it is characterized in that：Manganese salt described in step (1) be manganese sulfate, manganese acetate and It is one or more in manganese nitrate.
4. according to the method described in claim 1, it is characterized in that：Alkaline aqueous solution in step (1) is sodium hydroxide, ammonia It is one or more in water, sodium carbonate.
5. the preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4, feature exist according to claim 1 In：Mn salt described in step (2) is with citric acid respectively with manganese and citrometer, molar ratio Mn:CA=2~0.5.
6. the preparation method of anode material for lithium-ion batteries nano spinel LiMn2O4, feature exist according to claim 1 In：Step (6) described lithium source is one or more in lithium hydroxide, lithium carbonate.
CN201810263476.2A 2018-03-28 2018-03-28 Preparation method of nano spinel lithium manganate serving as lithium ion battery cathode material Expired - Fee Related CN108455676B (en)

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