CN105428644B - A kind of preparation method of the nickel lithium manganate cathode material with laminar microscopic appearance - Google Patents
A kind of preparation method of the nickel lithium manganate cathode material with laminar microscopic appearance Download PDFInfo
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- CN105428644B CN105428644B CN201610000340.3A CN201610000340A CN105428644B CN 105428644 B CN105428644 B CN 105428644B CN 201610000340 A CN201610000340 A CN 201610000340A CN 105428644 B CN105428644 B CN 105428644B
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- microscopic appearance
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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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- 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
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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
- H01M4/52—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
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
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Abstract
The present invention is a kind of preparation method of the nickel lithium manganate cathode material with laminar microscopic appearance, and its step is：Material solution is configured：According to LiNi0.5Mn1.5O4Stoichiometric proportion, which weighs soluble lithium salt, manganese salt and nickel salt and is dissolved in deionized water, forms homogeneous solution, and metal ion total concentration is 0.3 3M；Solution immerses：Filter paper is totally immersed in step（1）Solution in, control temperature 30 90oC, the immersion time is 0.1 24 hours, is filtered after immersion；Sample solidifies：By step（2）The filter paper for absorbing material solution of gained is 100 300 oCUnder be heating and curing and obtain presoma；Sample is calcined：By presoma 400 900oStove is cold after being calcined under C or air cooling obtains microscopic appearance for laminar nickel lithium manganate cathode material.The present invention controls thing by microscopic appearance of filter paper, is removed automatically during roasting, without template, technological process is simple；Gained LiNi0.5Mn1.5O4Material has laminar microscopic appearance, and product grain is small, good dispersion, can improve the high rate performance of material, and specific discharge capacity is high.
Description
Technical field
The present invention is a kind of preparation method of the nickel lithium manganate cathode material with laminar microscopic appearance, belongs to lithium ion
Cell art.
Background technology
Currently, the energy density and power density of hybrid vehicle and lithium ion battery used for electric vehicle by positive electrode
Influence larger, LiNi0.5Mn1.5O4Specific capacity and nearly 4.7V high voltage platform with ~ 130mAh/g, it is potential to be that one kind has
The anode material for lithium-ion batteries of application prospect.But, LiNi0.5Mn1.5O4Material will be in high power lithium ion cell system
Using high rate performance is still to improve.Preparing has special appearance, loose and porous structure LiNi0.5Mn1.5O4Material can be obtained
Preferable high rate performance, loose and porous structure LiNi of the preparation with special appearance conventional at present0.5Mn1.5O4The method of material
Mainly from sacrifice template etc., but there is following defect in the method：
（1）Sol-gel process can obtain the good LiNi with nano-scale particle of good dispersion, homogeneity0.5Mn1.5O4Material
Material, but complex technical process, additive are more, preparation time is long, are difficult to prepare the LiNi with special appearance0.5Mn1.5O4Material
Material.
（2）Prepared from template is sacrificed by hydro-thermal method, thermal decomposition method etc. with nano wire, nanometer rods, hollow ball etc.
Manganese-base oxide, hydroxide or the carbonate of microscopic appearance, then thing is controlled as pattern, lithium salts and nickel salt is added to prepare
LiNi with microscopic appearances such as nano wire, nanometer rods, hollow balls0.5Mn1.5O4Material.It can prepare and provide from sacrifice template
There is the LiNi of special loose porous pattern0.5Mn1.5O4Material, can improve the high rate performance of such material.But the method step is more,
Time is long, limits its development.
The content of the invention
The purpose of the present invention proposes a kind of nickel ion doped positive pole with laminar microscopic appearance aiming above mentioned problem
The preparation method of material, this method controls thing by pattern of filter paper, can obtain the nickel ion doped with laminar microscopic appearance
Positive electrode, filter paper is without subsequent treatment, and technique is simple, operation is few, and effect is good.
The purpose of the present invention is realized by following means：
A kind of preparation method of the nickel lithium manganate cathode material with laminar microscopic appearance, comprises the following steps：
（1）Material solution is configured：According to LiNi0.5Mn1.5O4It is molten that stoichiometric proportion weighs soluble lithium salt, manganese salt and nickel salt
Homogeneous solution is formed in deionized water, metal ion total concentration is 0.3-3M；
（2）Solution immerses：Filter paper is totally immersed in step（1）Solution in, control temperature 30-90oC, immerses the time
For 0.1-24 hours, filtered after immersion；
（3）Sample solidifies：By step（2）The filter paper for absorbing material solution of gained is in 100-300 oCUnder be heating and curing
Obtain presoma；
（4）Sample is calcined：By presoma in 400-900oStove is cold after being calcined under C or air cooling to obtain microscopic appearance be flake
Nickel lithium manganate cathode material.
Step（1）Described in soluble lithium salt, manganese salt and nickel salt be nitrate, acetate or oxalates in one kind or
It is several.
Step（2）Described filter paper is pulp type cellulose quantitative filter paper.
Step（3）Heat time be 0.1-10 hours.
Step（4）Roasting time to presoma was controlled at 0.5-48 hours.
The present invention is used as pattern by filter paper and controls thing, and material solution is absorbed during filter paper is immersed by filter paper, by
To the restriction of filter paper layer laminated structure, during solidification, raw material can only react in the space structure of filter paper, " duplication " filter paper it is micro-
See appearance structure.During high-temperature roasting, filter paper, which is oxidized, to be removed, and raw material cured product is generated with " duplication " filter paper
The laminar product of structure.
Beneficial effects of the present invention are：
（1）Filter paper controls thing directly as microscopic appearance, plays a part of controlling pattern in the curing process, in roasting
Automatic to remove, without to prepare the presoma with special appearance in addition as sacrificing template certainly, therefore technological process is simple；
（2）The LiNi prepared by thing is controlled by microscopic appearance of filter paper0.5Mn1.5O4Material has laminar microcosmic shape
Looks, and product grain is small, good dispersion, can improve the high rate performance of material, as shown in Fig. 2 under 10C multiplying powers prepared by this method
LiNi0.5Mn1.5O4Material still has 98mAh/g specific discharge capacity.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram of the synthetic sample of embodiment sample 1.
Fig. 2 is specific discharge capacity figure of the synthetic sample of embodiment sample 1 under different multiplying.
Embodiment
Below the present invention is further illustrated with example.
Embodiment 1
By lithium nitrate, lithium acetate, manganese nitrate, manganese acetate, nickel nitrate, nickel acetate（Li:Mn:Ni=1:1.5:0.5（Mole
Than））By nitrate：Acetate=1：1（Mol ratio）Ratio dissolve in deionized water, control the metal ion total concentration to be
1.5M.It is totally immersed in after filter paper is cut into the square that the length of side is 2cm afterwards in material solution, is heated to 60 DEG C and is kept for 1 hour,
Filtering.Filtration product is put into baking oven, is heating and curing at 150 DEG C 2 hours, afterwards moves into cured product in Muffle furnace,
It is calcined 2 hours at 700 DEG C, stove is cold, produces sample 1.
Embodiment 2
By lithium nitrate, lithium acetate, manganese nitrate, manganese acetate, nickel nitrate, nickel acetate（Li:Mn:Ni=1:1.5:0.5（Mole
Than））By nitrate：Acetate=0.5:1（Mol ratio）Ratio dissolve in deionized water, control the metal ion total concentration to be
1M.It is totally immersed in after filter paper is cut into the square that the length of side is 2cm afterwards in material solution, is heated to 60 DEG C and is kept for 1 hour, mistake
Filter.Filtration product is directly placed into the Muffle kiln roasting 2 hours that preset temperature is 750 DEG C, air cooling produces sample 2.
The battery performance test tables of data of the embodiment sample of table 1（0.5C charges, 1C electric discharges）
Fig. 1 schemes for the SEM of the synthetic sample of embodiment sample 1.It can be seen that prepared LiNi0.5Mn1.5O4Material
Laminar microscopic appearance is showed under 5000 times of multiplication factors, the thin slice is made up of one layer or several layers of molecules, shown
The microscopic appearance characteristic feature of material prepared by this method.
Fig. 2 is specific discharge capacity figure of the synthetic sample of embodiment sample 1 under different multiplying, and 1C represents 150mA/g herein
Current density.Figure it is seen that embodiment sample 1 is under different multiplying powers, the conservation rate of capacity is preferable, or even at 10C times
This method prepares LiNi under rate0.5Mn1.5O4Material still has 98mAh/g specific discharge capacity.
Claims (5)
1. a kind of preparation method of the nickel lithium manganate cathode material with laminar microscopic appearance, it is characterised in that including following step
Suddenly：
（1）Material solution is configured：According to LiNi0.5Mn1.5O4Stoichiometric proportion weighs soluble lithium salt, manganese salt and nickel salt and is dissolved in
Homogeneous solution is formed in ionized water, metal ion total concentration is 0.3-3M；
（2）Solution immerses：Filter paper is totally immersed in step（1）Solution in, control temperature 30-90oC, the immersion time is 0.1-
24 hours, filtered after immersion；
（3）Sample solidifies：By step（2）The filter paper for absorbing material solution of gained is in 100-300oIt is heating and curing under C before obtaining
Drive body；
（4）Sample is calcined：By presoma in 700-750oStove is cold after being calcined under C or air cooling obtains microscopic appearance for laminar nickel
Manganate cathode material for lithium.
2. there is the preparation method of the nickel lithium manganate cathode material of laminar microscopic appearance, its feature according to claim 1
It is step（1）Described in soluble lithium salt, manganese salt and nickel salt be nitrate, acetate or oxalates in one kind or many
Kind.
3. there is the preparation method of the nickel lithium manganate cathode material of laminar microscopic appearance, its feature according to claim 1
It is step（2）Described filter paper is pulp type cellulose quantitative filter paper.
4. there is the preparation method of the nickel lithium manganate cathode material of laminar microscopic appearance, its feature according to claim 1
It is step（3）Heat time be 0.1-10 hours.
5. there is the preparation method of the nickel lithium manganate cathode material of laminar microscopic appearance, its feature according to claim 1
It is step（4）Roasting time to presoma was controlled at 0.5-48 hours.
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