CN104681808B - Method for preparing strontium salt doped lithium nickel manganese oxide cathode material of lithium ion battery - Google Patents
Method for preparing strontium salt doped lithium nickel manganese oxide cathode material of lithium ion battery Download PDFInfo
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- CN104681808B CN104681808B CN201510071733.9A CN201510071733A CN104681808B CN 104681808 B CN104681808 B CN 104681808B CN 201510071733 A CN201510071733 A CN 201510071733A CN 104681808 B CN104681808 B CN 104681808B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a method for preparing a strontium salt doped lithium nickel manganese oxide cathode material of a lithium ion battery. The method comprises the following steps: raw material preparation, reaction synthesis and high temperature sintering. The product of the method provided by the invention is a novel ternary metal oxide cathode material, and the material forms a lithium ion battery with Li or C to ensure high specific capacity, high rate capability and good cycle performance; moreover, the material is good in electrical property uniformity, simple in process, and low in cost and does not need complex and expensive preparation equipment.
Description
Technical field
The present invention relates to battery material technical field, more particularly to a kind of lithium ion battery of strontium salt doping nickel ion doped is just
Pole material preparation method.
Background technology
Spinel-type nickel ion doped grows up on the basis of lithium manganate having spinel structure, is have as LiMn2O4
The positive electrode of three-dimensional lithium ion tunnel, reversible capacity is 146.7mAh/g, is with being more or less the same for LiMn2O4, but voltage platform
4.7-5.1V or so, cyclical stability under more than 20%, and high temperature will be higher by also than original than the 4V voltage platforms of LiMn2O4
LiMn2O4 be improved.During lithium ion battery charge and discharge cycles, Mn3+ ions are readily soluble in nickel ion doped material
In the organic electrolyte of ionic is molten, the electric conductivity that causes material is poor, utilization rate is low, hinder the diffusion of lithium ion for solution
Slowly, the reversibility that thus causes battery is poor, following under capability retention low and high temperature or under big multiplying power in cyclic process
The problems such as ring poor performance.One of common solution, in nickel ion doped material doping and Li+, Ni2+, Mn4+, O2- etc. from
Other higher ions of sub- active force occupy relevant position, combine to form the chemical bond more more stable than Mn-O bond energy to stablize with O
Nickel ion doped lattice structure, effectively suppresses because Mn3+ is dissolved in the problem that electrolyte makes nickel ion doped lattice subside, so as to can
With capability retention in the reversibility of raising battery and cyclic process；The two of its solution, in the table of nickel ion doped material
Bread covers the protection materials of a layer and electrolyte directly contact, can there is the oxidation work for suppressing the metal ion of high-valence state to electrolyte
With so that electrolyte is more stable, moreover it is possible to the dissolution of Mn3+ is prevented in certain degree, protection materials stability action is played
While, additionally it is possible to improve the stability and capacity in the cyclic process under electric conductivity, the high temperature of material or under big multiplying power
Conservation rate.
In sum, there is following weak point in prior art：
1st, the dissolving of effectively solving manganese ion is unable to, so as to cause cycle performance of battery poor；
2nd, other element ions of doping, such as Cr, Co, Fe, because ionic valence condition is in the redox electrochemistry of battery
Change greatly in course of reaction, and the ionic radius of different valence state differs greatly, the distortion of lattice being easily caused in cyclic process, from
And make battery performance integrally be deteriorated；
3rd, Surface coating is carried out to the nickel ion doped of spinel structure, area size and clad that clad is coated
Thickness evenness differ.
The content of the invention
The method for preparing anode material of lithium-ion battery of nickel ion doped it is an object of the invention to provide a kind of strontium salt is adulterated,
Complex process in prior art is solved, operation is difficult, high energy consumption, high cost, the poor problem of products obtained therefrom electrology characteristic.
The present invention is achieved in that a kind of method for preparing anode material of lithium-ion battery of strontium salt doping nickel ion doped,
Methods described comprises the steps：
The preparation of A, raw material:By lithium salt material, manganese salt material, nickel salt material and strontium salt material, by lithium salts：Manganese salt：Nickel salt：
Strontium salt=10-30%：20-60%：20-40%：The mass percent precise of 2-10%, is dissolved in respectively 300-500ml and goes
Corresponding lithium salt solution, manganese salt solution, nickel salt solution and strontium salt solution are obtained in ionized water or acid；
B, it is synthesized:By lithium salts, manganese salt, nickel salt, strontium salt solution, it is put into by the order of manganese salt, nickel salt, lithium salts, strontium salt
In container, there is fluffy solid up to solution in high-speed stirred 3-6 hour, then with vibration of ultrasonic wave until fluffy solid viscosity
Equally, make fluffy solid form homogeneous state, cotton-shaped mixed solution is moved in reactor, be 180-300 DEG C, pressure in temperature
Power is isothermal reaction 12-18 hours in the environment of 0.5-2MPa, then naturally cools to room temperature, and the product in reactor is first used
Absolute ethanol washing, repeated washing 3-5 time is used to obtain product A after deionized water；
C, high temperature sintering:By product A in vacuum drying chamber 80-150 DEG C of freeze-day with constant temperature 6-12 hour, obtain desciccate
B, then product B is put in atmosphere furnace, in 750 DEG C of constant temperature, oxidizing roasting 4-8 is little in the environment of oxygen flow 0.1-0.5L/min
When, finally give the nickel ion doped of the spinel structure doped with strontium.
The present invention further technical scheme be：Lithium salt material described in step A is lithium carbonate, lithium acetate, lithium chloride, sulphur
One or more in sour lithium, lithium nitrate, the manganese salt material is in manganese carbonate, manganese acetate, manganese chloride, manganese sulfate, manganese nitrate
One or more, the nickel salt material be nickelous carbonate, nickel acetate, nickel chloride, nickel sulfate, nickel nitrate in one or more,
The strontium salt material is one or more in strontium acetate, strontium chloride, strontium sulfate, strontium nitrate.
The invention has the beneficial effects as follows：Product of the present invention is the new positive electrode of ternary metal oxide, the material and Li or C
Composition lithium ion battery, with higher specific capacity, high-rate characteristics and good cycle performance；And the electrology characteristic of the material
Preferably, process is simple, cost is relatively low, without the need for the Preparation equipment of complex and expensive for uniformity.
Description of the drawings
Fig. 1 is that a kind of anode material for lithium-ion batteries one of strontium salt doping nickel ion doped of the present invention is preferably implemented
XRD；
Fig. 2 is that a kind of anode material for lithium-ion batteries one of strontium salt doping nickel ion doped of the present invention is preferably implemented
SEM schemes；
Fig. 3 is a kind of filling for the preferably enforcement of anode material for lithium-ion batteries one of strontium salt doping nickel ion doped of the present invention
Discharge test figure.
Specific embodiment
With reference to the accompanying drawings and detailed description the present invention is described further.
A kind of method for preparing anode material of lithium-ion battery of strontium salt doping nickel ion doped, methods described includes following step
Suddenly：
The preparation of A, raw material:By lithium salt material, manganese salt material, nickel salt material and strontium salt material, by lithium salts：Manganese salt：Nickel salt：
Strontium salt=10-30%：20-60%：20-40%：The mass percent precise of 2-10%, is dissolved in respectively 300-500ml and goes
Corresponding lithium salt solution, manganese salt solution, nickel salt solution and strontium salt solution are obtained in ionized water or acid；
B, it is synthesized:By lithium salts, manganese salt, nickel salt, strontium salt solution, it is put into by the order of manganese salt, nickel salt, lithium salts, strontium salt
In container, there is fluffy solid up to solution in high-speed stirred 3-6 hour, then with vibration of ultrasonic wave until fluffy solid viscosity
Equally, make fluffy solid form homogeneous state, cotton-shaped mixed solution is moved in reactor, be 180-300 DEG C, pressure in temperature
Power is isothermal reaction 12-18 hours in the environment of 0.5-2MPa, then naturally cools to room temperature, and the product in reactor is first used
Absolute ethanol washing, repeated washing 3-5 time is used to obtain product A after deionized water；
C, high temperature sintering:By product A in vacuum drying chamber 80-150 DEG C of freeze-day with constant temperature 6-12 hour, obtain desciccate
B, then product B is put in atmosphere furnace, in 750 DEG C of constant temperature, oxidizing roasting 4-8 is little in the environment of oxygen flow 0.1-0.5L/min
When, finally give the nickel ion doped of the spinel structure doped with strontium.
Lithium salt material described in step A is lithium metal, lithia, lithium carbonate, lithium acetate, lithium hydroxide, lithium chloride, sulfuric acid
One or more in lithium, lithium nitrate, the manganese salt material is manganese metal, manganese oxide, manganese carbonate, manganese acetate, manganous hydroxide, chlorine
Change one or more in manganese, manganese sulfate, manganese nitrate, the nickel salt material is metallic nickel, nickel oxide, nickelous carbonate, nickel acetate, hydrogen
One or more in nickel oxide, nickel chloride, nickel sulfate, nickel nitrate, the strontium salt material be Preparation of Metallic Strontium, strontium oxide strontia, strontium acetate,
One or more in strontium chloride, strontium sulfate, strontium nitrate.
In currently preferred one embodiment：Lithia, manganese acetate, nickel oxide, strontium oxide strontia are pressed into lithia：Acetic acid
Manganese：Nickel oxide：Strontium oxide strontia=20%：50%：20%：10% mass percent precise, is dissolved in respectively 300ml deionizations
Corresponding lithium salt solution, manganese salt solution, nickel salt solution and strontium salt solution are obtained in water or acid；By lithium salts, manganese salt, nickel salt, strontium salt
Solution, is put in container by the order of manganese salt, nickel salt, lithium salts, strontium salt, and high-speed stirred fluffy solid occurs in 4 hours up to solution,
With ultrasonic echography until forming homogeneous state；Cotton-shaped mixed solution is moved in reactor, is 200 DEG C, pressure in temperature
For isothermal reaction in the environment of 0.9MPa 14 hours or so；When naturally cooling to room temperature, by the product in reactor point
Other deionized water, absolute ethyl alcohol centrifuge washing 5 times, obtain synthetic product A；By product A in vacuum drying chamber 100 DEG C of constant temperature
Lower drying 8 hours, obtains desciccate B, then B is put in atmosphere furnace, aoxidizes under oxygen flow 0.2L/min, 750 DEG C of constant temperature
Calcining 5 hours, finally gives the nickel ion doped of the spinel structure doped with strontium.
In presently preferred embodiment：Lithium acetate, manganese oxide, metallic nickel, strontium acetate are pressed into lithium acetate：Oxygen
Change manganese：Metallic nickel：Strontium acetate=30%：40%：20%：10% mass percent precise, the molten 400ml deionizations of difference
Corresponding lithium salt solution, manganese salt solution, nickel salt solution and strontium salt solution are obtained in water or acid；By lithium salts, manganese salt, nickel salt, strontium salt
Solution, is put in container by the order of manganese salt, nickel salt, lithium salts, strontium salt, and high-speed stirred fluffy solid occurs in 5 hours up to solution,
With ultrasonic echography until forming homogeneous state；Cotton-shaped mixed solution is moved in reactor, is 250 DEG C, pressure in temperature
For isothermal reaction in the environment of 1.5MPa 15 hours or so；When naturally cooling to room temperature, by the product in reactor point
Other deionized water, absolute ethyl alcohol centrifuge washing 5 times, obtain synthetic product A；By product A in vacuum drying chamber 120 DEG C of constant temperature
Lower drying 10 hours, obtains desciccate B, then B is put in atmosphere furnace, aoxidizes under oxygen flow 0.3L/min, 750 DEG C of constant temperature
Calcining 6 hours, finally gives the nickel ion doped of the spinel structure doped with strontium.
In presently preferred embodiment：Lithium sulfate, manganese chloride, nickel chloride, strontium chloride are pressed into lithium sulfate：Chlorine
Change manganese：Nickel chloride：Strontium chloride=15%：40%：40%：5% mass percent precise, the molten 300ml deionizations of difference
Corresponding lithium salt solution, manganese salt solution, nickel salt solution and strontium salt solution are obtained in water or acid；By lithium salts, manganese salt, nickel salt, strontium salt
Solution, is put in container by the order of manganese salt, nickel salt, lithium salts, strontium salt, and high-speed stirred fluffy solid occurs in 6 hours up to solution,
With ultrasonic echography until forming homogeneous state；Cotton-shaped mixed solution is moved in reactor, is 300 DEG C, pressure in temperature
For isothermal reaction in the environment of 1.8MPa 17 hours or so；When naturally cooling to room temperature, by the product in reactor point
Other deionized water, absolute ethyl alcohol centrifuge washing 5 times, obtain synthetic product A；By product A in vacuum drying chamber 140 DEG C of constant temperature
Lower drying 11 hours, obtains desciccate B, then B is put in atmosphere furnace, aoxidizes under oxygen flow 0.5L/min, 750 DEG C of constant temperature
Calcining 8 hours, finally gives the nickel ion doped of the spinel structure doped with strontium.
Strontium is the more stable conductor material of a kind of valence state and ionic radius.Strontium is due to its very strong absorption X-ray radiation work(
Can be with unique physical and chemical performance, and it is each to be widely used in electronics, chemical industry, metallurgy, military project, light industry, medicine and optics etc.
Individual field.Barium, strontium, calcium and magnesium are both alkaline-earth metal, are also the more element of content in the earth's crust.Strontium is a kind of active positive gold
Category, it is easy to be oxidized to stable, colourless Sr2+, redox electrochemical reaction process of its ionic valence condition in battery
In it is unchanged, thus be not result in the distortion of lattice in cyclic process, make cycle performance have improvement.
In addition, from Fig. 1, Fig. 2 and Fig. 3, its XRD peak type is sharp, back end is smooth, show that synthesized material is crystalline substance
The intact spinel structure of shape, bright its body phase material of its SEM chart is closely connected with skin-material, middle gapless, its body phase
Material defines melting structure with skin-material, and constant with the compacted density for ensureing material, charging and discharging curve figure shows with this
The bright obtained anode material of lithium battery nickel ion doped doped with strontium, its excellent electrical property.
Product of the present invention is the new positive electrode of ternary metal oxide, the material and Li or C composition lithium ion batteries, is had
Higher specific capacity, high-rate characteristics and good cycle performance；And the electrology characteristic uniformity of the material is preferably, technique letter
Single, cost is relatively low, without the need for the Preparation equipment of complex and expensive.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The present invention be embodied as be confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of without departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (2)
1. a kind of strontium salt is adulterated the method for preparing anode material of lithium-ion battery of nickel ion doped, it is characterised in that：Methods described bag
Include following steps：
The preparation of A, raw material:By lithium salt material, manganese salt material, nickel salt material and strontium salt material, by lithium salts：Manganese salt：Nickel salt：Strontium salt
=10-30%：20-60%：20-40%：The mass percent precise of 2-10%, is dissolved in respectively 300-500ml deionizations
Corresponding lithium salt solution, manganese salt solution, nickel salt solution and strontium salt solution are obtained in water or acid；
B, it is synthesized:By lithium salts, manganese salt, nickel salt, strontium salt solution, by the order of manganese salt, nickel salt, lithium salts, strontium salt container is put into
In, there is fluffy solid up to solution in high-speed stirred 3-6 hour, then with vibration of ultrasonic wave until fluffy solid viscosity one
Sample, makes fluffy solid form homogeneous state, and cotton-shaped mixed solution is moved in reactor, is 180-300 DEG C, pressure in temperature
For isothermal reaction 12-18 hours in the environment of 0.5-2MPa, room temperature is then naturally cooled to, the product in reactor is first spent
Absolute ethanol washing, repeated washing 3-5 time is used to obtain product A after ionized water；
C, high temperature sintering:By product A in vacuum drying chamber 80-150 DEG C of freeze-day with constant temperature 6-12 hour, obtain desciccate B, then
Product B is put in atmosphere furnace, in 750 DEG C of constant temperature, oxidizing roasting 4-8 hours in the environment of oxygen flow 0.1-0.5L/min,
Finally give the nickel ion doped of the spinel structure doped with strontium.
2. according to claim 1 a kind of strontium salt is adulterated the method for preparing anode material of lithium-ion battery of nickel ion doped, and it is special
Levy and be：Lithium salt material described in step A is one or more in lithium carbonate, lithium acetate, lithium chloride, lithium sulfate, lithium nitrate,
The manganese salt material is one or more in manganese carbonate, manganese acetate, manganese chloride, manganese sulfate, manganese nitrate, and the nickel salt material is
One or more in nickelous carbonate, nickel acetate, nickel chloride, nickel sulfate, nickel nitrate, the strontium salt material be strontium acetate, strontium chloride,
One or more in strontium sulfate, strontium nitrate.
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| CN106099082A (en) * | 2016-08-31 | 2016-11-09 | 四川剑兴锂电池有限公司 | The surface cladding type nickel ion doped material of a kind of hydro-thermal method modification, lithium battery and preparation method thereof |
| CN111504928B (en) * | 2020-06-05 | 2023-06-16 | 深圳麦德凯诺医药科技有限公司 | Method for detecting dissolution rate of calcium acetate tablets |
| CN112751026A (en) * | 2021-01-19 | 2021-05-04 | 贵州大学 | Modification method for doping synthesis of binary lithium nickel manganese oxide positive electrode material |
| CN113506869A (en) * | 2021-05-07 | 2021-10-15 | 鹏盛国能(深圳)新能源集团有限公司 | Lithium battery and anode thereof |
| CN114551838A (en) * | 2022-02-25 | 2022-05-27 | 中南大学 | Modified single crystal type cobalt-free high-nickel ternary positive electrode material and preparation method thereof |
| WO2024062866A1 (en) * | 2022-09-22 | 2024-03-28 | パナソニックＩｐマネジメント株式会社 | Positive electrode active material for secondary batteries, and secondary battery |
| WO2024062848A1 (en) * | 2022-09-22 | 2024-03-28 | パナソニックＩｐマネジメント株式会社 | Secondary battery positive electrode active material and secondary battery |
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| KR20060111393A (en) * | 2005-04-22 | 2006-10-27 | 주식회사 엘지화학 | New system of lithium ion battery containing material with high irreversible capacity |
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| EP2221903A2 (en) * | 2009-02-19 | 2010-08-25 | Samsung SDI Co., Ltd. | Positive electrode for rechargeable lithium battery and rechargeable lithium battery including same |
| CN102386394A (en) * | 2011-11-04 | 2012-03-21 | 上海空间电源研究所 | Preparation method for lithium manganese nickel oxide served as high voltage lithium ion anode material |
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