CN106920952B - A kind of preparation method of modified nickel lithium manganate cathode material - Google Patents
A kind of preparation method of modified nickel lithium manganate cathode material Download PDFInfo
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- CN106920952B CN106920952B CN201710298934.1A CN201710298934A CN106920952B CN 106920952 B CN106920952 B CN 106920952B CN 201710298934 A CN201710298934 A CN 201710298934A CN 106920952 B CN106920952 B CN 106920952B
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- 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
The present invention discloses a kind of preparation method of modified nickel lithium manganate cathode material, after it is the following steps are included: first mix cerium iron complex oxides and lithium salts, nickel salt, manganese salt, ball milling dispersion is carried out again, after being then dried in vacuo, obtains the presoma of cerium iron complex oxides cladding nickel ion doped material；By presoma in air atmosphere with 700 ~ 1000 DEG C of 5 ~ 20h of calcining at constant temperature, natural cooling obtains modified nickel lithium manganate cathode material.Nickel ion doped surface is coated on by cerium iron complex oxides; stable protective layer is formed, electrolyte can be effectively reduced and be contacted with nickel ion doped, reduces electrolyte in the oxygenolysis of positive electrode surface; to improve chemical stability of the positive electrode in battery system, and improve cycle performance.
Description
Technical field
The invention belongs to lithium battery material fields, and in particular to a kind of preparation method of modified nickel lithium manganate cathode material.
Background technique
Lithium ion battery has many advantages, such as that specific energy is high, has extended cycle life and stablize with discharge performance, closely as secondary energy sources
With factors, lithium ion battery and its correlation such as universal and ballooning oil prices of electric car under national new energy strategy over year
Field is rapidly developed, however is urgently broken through in current lithium-ion battery system there are still many technical problems, as can
Metric density is relatively low, at high cost, security performance is not good enough etc..
Spinel-type nickel ion doped (LiNi0.5Mn1.5O4) it is to grow up on the basis of LiMn2O4, there is good follow
Ring performance, reversible capacity 146.7mAh/g, and have a up to discharge platform of 4.7V, it is considered to be it is most promising
High potential anode material for lithium-ion batteries.However anodic potentials height means the reproducibility enhancing of negative regions, this also causes
After nickel ion doped matching graphite cathode, the dynamics that surface SEI film is formed changes, and cannot be formed with the SEI of effect
Electrolyte and carbon material is isolated in film, and the cycle performance of negative electrode material is caused to substantially reduce.In addition, since nickel ion doped battery is being made
During standby, ambient moisture is difficult to control again, causes inside battery moisture content excessively high, and then cause chain electrochemical reaction,
Promote electrolyte decomposition, and releases a large amount of gas.Especially nickel ion doped battery is after high-temperature storage, inside battery meeting
Assemble a large amount of gas, the swelling of battery clearly, seriously constrains the performance of battery performance.
Summary of the invention
It is an object of the present invention to provide a kind of preparation method of modified nickel lithium manganate cathode material, this method process letters
Single, non-environmental-pollution is low in cost, and obtained product purity is high, and performance is stablized, and is suitable for large-scale industrialized production.
Technical scheme is as follows:
A kind of preparation method of modified nickel lithium manganate cathode material comprising following steps:
(1) after mixing cerium iron complex oxides and lithium salts, nickel salt, manganese salt, then ball milling dispersion is carried out, be then dried in vacuo
Afterwards, the presoma of cerium iron complex oxides cladding nickel ion doped material is obtained；
(2) by the presoma of step (1) in air atmosphere with 700~1000 DEG C of 5~20h of calcining at constant temperature, natural cooling
Obtain modified nickel lithium manganate cathode material.
Further scheme, the lithium salts, nickel salt, Li, Ni, Mn elemental mole ratios are 1.05:0.5:1.5 in manganese salt.
Further scheme, the molecular formula of the cerium iron complex oxides are Ce1-x FexO2, 0.05≤x≤0.2 in formula.
The mass ratio of further scheme, the cerium iron complex oxides and theoretical synthesis nickel ion doped is (0.01-0.1):
1。
Further scheme, the lithium salts are one or both of lithium hydroxide, lithium acetate, lithium carbonate.
Further scheme, the nickel salt are one or both of nickel nitrate, nickel acetate, nickel sulfate, nickel chloride.
Further scheme, the manganese salt are one or both of manganese nitrate, manganese acetate, manganese sulfate, manganous chloride.
Further scheme, the medium of ball milling dispersion is deionized water, dehydrated alcohol, ethylene glycol, third in the step (1)
One or both of ketone, dimethylformamide.
This patent passes through cerium iron complex oxides Ce1-xFexO2(0.05≤x≤0.2) is coated on nickel ion doped surface, is formed
Stable protective layer can effectively reduce electrolyte and contact with nickel ion doped, reduce electrolyte in the oxidation point of positive electrode surface
Solution, to improve chemical stability of the positive electrode in battery system, and improves cycle performance.
In addition, presoma is to be dispersed by ball-milling medium ball milling, then obtained by high-temperature calcination in preparation process of the present invention
Ce1-xFexO2(0.05≤x≤0.2) coats nickel ion doped material, and process is simple and easy to control；And the Ce of cladding1-xFexO2With vertical
Square fluorite structure, chemical property is excellent, and can effectively reduce electrolyte and contact with positive electrode, to reduce electrolyte
In the oxygenolysis of positive electrode surface, high rate performance and stable circulation performance of the positive electrode in battery system are improved.
Detailed description of the invention
Fig. 1 is the SEM spectrum for the Modified Nickel lithium manganate material that embodiment 1 synthesizes；
Fig. 2 is the charging and discharging curve figure for the Modified Nickel lithium manganate material 0.5C multiplying power that embodiment 1 synthesizes；
Fig. 3 is 50 weeks cyclic curves of the Modified Nickel lithium manganate material 0.5C multiplying power that embodiment 1 synthesizes.
Specific embodiment
Embodiment 1
(1) lithium carbonate, nickel acetate and manganese acetate are weighed by Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5, further according to
Ce0.95Fe0.05O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is that 0.01:1 weighs Ce0.95Fe0.05O2, by Ce0.95Fe0.05O2
After lithium carbonate, nickel acetate, manganese acetate mixing, deionized water is added and carries out ball milling dispersion, obtains Ce0.95Fe0.05O2Cladding
LiNi0.5Mn1.5O4The presoma of material.
(2) 700 DEG C of calcining at constant temperature 20h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1)
Obtain Ce0.95Fe0.05O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.
In conjunction with attached drawing, illustrate that Modified Nickel lithium manganate material object that the present invention is prepared mutually characterizes and electricity with embodiment 1
Chemical property:
Fig. 1 is the SEM spectrum for the Modified Nickel lithium manganate material that embodiment 1 synthesizes, as can be seen from Figure 1 Ce1-xFexO2?
The uniform cladding nickel ion doped surface of grain is conducive to improve nickel ion doped in charge and discharge process holding structural stability, and raising follows
Ring performance.
Lithium battery pond made by the modification nickel lithium manganate cathode material that embodiment 1 synthesizes, 0.5C charging and discharging curve figure
Such as Fig. 2, as can be seen from Figure 2 under 0.5C multiplying power, capacity is in 130.3mAh/g.50 weeks cyclic curves of 0.5C multiplying power are as schemed
3, as can be seen from Figure 3 under 0.5C multiplying power, capacity retention ratio is still maintained at 98.08% after it experienced 50 weeks circulations, says
It is bright to pass through Ce0.95Fe0.05O2Coating nickel ion doped material has good cyclical stability.
Embodiment 2
(1) lithium hydroxide, nickel sulfate and sulphur are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped
Sour manganese, further according to Ce0.9Fe0.1O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is that 0.05:1 weighs Ce0.9Fe0.1O2, will
Ce0.9Fe0.1O2After the mixing of lithium hydroxide, nickel sulfate and manganese sulfate, dehydrated alcohol is added and carries out ball milling dispersion, obtains
Ce0.9Fe0.1O2Coat LiNi0.5Mn1.5O4The presoma of material.
(2) 800 DEG C of calcining at constant temperature 15h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1)
Obtain Ce0.9Fe0.1O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.
Embodiment 2 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be
98.21%.
Embodiment 3
(1) lithium acetate, nickel nitrate and nitric acid are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped
Manganese, further according to Ce0.9Fe0.1O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is that 0.07:1 weighs Ce0.9Fe0.1O2, will
Ce0.9Fe0.1O2After the mixing of lithium acetate, nickel nitrate and manganese nitrate, ethylene glycol is added and carries out ball milling dispersion, obtains Ce0.9Fe0.1O2
Coat LiNi0.5Mn1.5O4The presoma of material.
(2) 900 DEG C of calcining at constant temperature 10h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1)
Obtain Ce0.9Fe0.1O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.
Embodiment 3 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be
98.34%.
Embodiment 4
(1) lithium hydroxide, nickel chloride and two are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped
Manganese chloride, further according to Ce0.85Fe0.15O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is 0.09:1, weighs Ce0.85Fe0.15O2,
By Ce0.85Fe0.15O2Ball milling dispersion is carried out with acetone is added after the mixing of lithium hydroxide, nickel chloride and manganous chloride, is obtained
Ce0.85Fe0.15O2Coat LiNi0.5Mn1.5O4The presoma of material.
(2) 900 DEG C of calcining at constant temperature 15h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1)
Obtain Ce0.85Fe0.15O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.
Embodiment 4 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be
98.15%.
Embodiment 5
(1) lithium carbonate, nickel sulfate and sulfuric acid are weighed by the Li:Ni:Mn elemental mole ratios 1.05:0.5:1.5 of nickel ion doped
Manganese, further according to Ce0.8Fe0.2O2And LiNi0.5Mn1.5O4Theory synthesis mass ratio is 0.1:1, weighs Ce0.8Fe0.2O2, will
Ce0.8Fe0.2O2Ball milling dispersion is carried out with dimethylformamide is added after lithium carbonate, nickel acetate, manganese acetate mixing, is obtained
Ce0.8Fe0.2O2Coat LiNi0.5Mn1.5O4The presoma of material.
(2) 1000 DEG C of calcining at constant temperature 5h, then natural cooling in air atmosphere after being dried in vacuo the presoma of step (1)
Obtain Ce0.8Fe0.2O2Coat LiNi0.5Mn1.5O4Modification nickel lithium manganate cathode material.
Embodiment 5 synthesize modification nickel lithium manganate cathode material experienced 50 weeks recycle after capacity retention ratio be
97.56%.
Above content is only to structure of the invention example and explanation, affiliated those skilled in the art couple
Described specific embodiment does various modifications or additions or is substituted in a similar manner, without departing from invention
Structure or beyond the scope defined by this claim, is within the scope of protection of the invention.
Claims (7)
1. a kind of preparation method of modified nickel lithium manganate cathode material, it is characterised in that: the following steps are included:
(1) after mixing cerium iron complex oxides and lithium salts, nickel salt, manganese salt, then ball milling dispersion is carried out, after being then dried in vacuo,
Obtain the presoma of cerium iron complex oxides cladding nickel ion doped material；The molecular formula of the cerium iron complex oxides is Ce1-x
FexO2, 0.05≤x≤0.2 in formula；
(2) by the presoma of step (1) in air atmosphere with 700 ~ 1000 DEG C of 5 ~ 20h of calcining at constant temperature, natural cooling is changed
Property nickel lithium manganate cathode material.
2. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the lithium
Salt, nickel salt, Li, Ni, Mn elemental mole ratios are 1.05:0.5:1.5 in manganese salt.
3. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the cerium
The mass ratio of iron compound oxide and theoretical synthesis nickel ion doped is (0.01-0.1): 1.
4. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the lithium
Salt is one or both of lithium hydroxide, lithium acetate, lithium carbonate.
5. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the nickel
Salt is one or both of nickel nitrate, nickel acetate, nickel sulfate, nickel chloride.
6. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the manganese
Salt is one or both of manganese nitrate, manganese acetate, manganese sulfate, manganous chloride.
7. a kind of preparation method of modified nickel lithium manganate cathode material according to claim 1, it is characterised in that: the step
Suddenly the medium that ball milling disperses in (1) is one of deionized water, dehydrated alcohol, ethylene glycol, acetone, dimethylformamide or two
Kind.
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| CN108305999A (en) * | 2017-12-30 | 2018-07-20 | 宁夏科捷锂电池股份有限公司 | It is a kind of to use β-Ga2O3To LiMn2O4The method that positive electrode carries out coating modification |
| CN111628147B (en) * | 2020-04-25 | 2022-05-03 | 湖南鑫碳新材料有限公司 | Composite lithium ion battery positive electrode material and preparation method thereof |
| CN114156481B (en) * | 2021-12-01 | 2023-04-07 | 西安交通大学 | Atomic-level doped lithium nickel manganese oxide positive electrode material and preparation method and application thereof |
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| CN102257659A (en) * | 2009-12-01 | 2011-11-23 | 松下电器产业株式会社 | Positive electrode active material for nonaqueous electrolyte secondary battery and method for producing same |
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