CN105514411B - A kind of synthetic method of anode material for lithium-ion batteries - Google Patents
A kind of synthetic method of anode material for lithium-ion batteries Download PDFInfo
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- CN105514411B CN105514411B CN201510951028.8A CN201510951028A CN105514411B CN 105514411 B CN105514411 B CN 105514411B CN 201510951028 A CN201510951028 A CN 201510951028A CN 105514411 B CN105514411 B CN 105514411B
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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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- 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 invention discloses a kind of synthetic methods of anode material for lithium-ion batteries, belong to anode material for lithium-ion batteries technical field, and the granularity and pattern for regulating and controlling presoma by controlling the linear pH value in coprecipitation reaction change.A kind of synthetic method of anode material for lithium-ion batteries of the present invention, the anode material for lithium-ion batteries is lithium-rich manganese base material, the at least one of ternary material, this synthetic method is in any one in coprecipitation process and several periods △ t, pH value is at any time in control kettle or addition salting liquid volume changes linearly, reach control primary particle and offspring speed of growth linear change, make primary particle that the speed of growth of graded be presented from particle interior, achieve the purpose that control chemical property, be conducive to mass production, bright prospects with large-scale application.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, more particularly to a kind of anode material for lithium-ion batteries
Synthetic method.
Background technology
Chemical coprecipitation is most widely used in chemical synthesis in liquid phase powder body material, is usually added into material liquid
Precipitating reagent appropriate, making each component in solution by evenly mixing, stoichiometrically co-precipitation comes out, or molten
First reaction is settled out a kind of intermediate product in liquid, then its calcining and decomposing is prepared target product.It can be according to reality using the technique
Condition to be tested to regulate and control the granularity of product, pattern, active principle can reach the other uniform mixing of atom, molecular level in product,
Equipment is simple, and operation is easy.
Traditional chemical coprecipitation is in precursor synthesis, and in the case where other conditions are constant, control pH is one
Definite value achievees the purpose that make particle to increase by the increase in reaction time, and the whole process consuming time is longer, and with grain
The fixed pH value of growth of son cannot meet the requirement of particle growth, and production may also be not achieved in the granularity obtained in this way and pattern
Requirement.
In hydroxide as the coprecipitation reaction process of precipitating reagent, pH controls degree of supersaturation, affects nucleus generation
Rate and rate of crystalline growth.When the other conditions such as complexing agent and concentration are constant, pH is increased, and solution degree of supersaturation improves, at
Nuclear reaction is promoted, and particulate nucleation quantity is more, and the primary particle in secondary spherical particle is tiny.Conversely, when reducing pH, crystal
Nucleation rate is inhibited, and nucleation rate is slow, and primary particle growth becomes large-sized.It is anti-by controlling co-precipitation in the present invention
It answers middle pH value to change linearly, can promote primary particle that the graded of grain size is gradually presented with reaction process, to control
Second particle is by the internal primary particle pattern to outer surface.Because the particle specific surface area of small size is big, head effects height, multiplying power
It is high, safety is low, large-sized particle specific surface area is small, cycle and safe, thus in order to obtain different grain size and
The presoma of pattern, it is necessary to control linear pH variations.In addition, in the ternary material of Co deposited synthesis gradient composition, into
Material mouth conveying is gradient solution, and loading solution component needs at any time or charging volume changes in gradient.And different element groups
The loading solution divided, needs to grow at various ph values, therefore be also required to pH and accordingly in gradient change.The present invention discloses one
Kind pH value is with reaction time or the coprecipitation of the linear rate variation of charging volume.
Invention content
The problems in deficiency and actual production building-up process in view of the above method, it is coprecipitated it is an object of the invention to control
The linear pH value formed sediment in reacting changes come the granularity and pattern for regulating and controlling presoma, and provides a kind of anode material for lithium-ion batteries
Synthetic method.
The technical scheme is that：A kind of synthetic method of anode material for lithium-ion batteries, it is characterised in that：The lithium from
Sub- cell positive material is lithium-rich manganese base material, at least one of ternary material, and positive electrode material precursor synthesis uses
Be improved coprecipitation, i.e., in any one and several periods △ t of coprecipitation reaction, control in kettle pH value with
Reaction time or addition salting liquid volume change linearly.
It is described in period △ t, pH linear changes contain linear increase and linear reduction, linear change rate are big
Small value is ranging from, i.e., in △ t1In reaction time section, rate of change V1, in △ t2When, variation
Rate is V2。
The molecular formula of the ternary material is Li1+nNixCoyM1-x-yO2, wherein M be Mn, Al, Mg, Zr, Ce, Ti, Ca,
At least one element of Fe, and 0≤n ＜ 0.1,0.3≤x<1,0.1≤y<1,0<x+y<1.
The molecular formula of the lithium-rich manganese base material is, wherein 0<n<
1,0<x<1,0<y<1,0<z<1 and x+y+z=1.
Ranging from 1min ~ 72h of described any one and several periods △ t.
The variation range of the pH value be 10 ~ 13 between certain two values between variation.
The ternary material or lithium-rich manganese base material is obtained through two-step sintering by the presoma synthesized, pre-burning temperature
300 ~ 500 DEG C of degree, burn-in time are 1 ~ 10h, and the temperature of secondary clacining is 600 ~ 1000 DEG C, time of secondary clacining is 10 ~
20h。
Beneficial effects of the present invention are：Control in coprecipitation process pH in pH value linear change and nucleating growth various process
It is worth the change of rate of change, reaches control primary particle and offspring speed of growth linear change, in control presoma pattern
Under the premise of, the particle growth time is reduced, production efficiency is improved, is conducive to mass production, with the wide of large-scale application
Wealthy foreground.
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 only this
Some embodiments of invention without having to pay creative labor, may be used also for those of ordinary skill in the art
With obtain other attached drawings according to these attached drawings.
Fig. 1 is the variation that the pH value that embodiment 1 controls linearly reduces.
Fig. 2 is the linearly increasing variation of the pH value of the control of embodiment 2.
Fig. 3 is the pH value multistage linear variation that embodiment 3 controls.
Fig. 4 is the multistage linear variation for the pH value another kind situation that embodiment 4 controls.
Specific implementation mode
The embodiment of the present invention provides a kind of preparation method of anode active material of lithium ion battery, wherein maximum technical characteristic
In any one and several periods △ t in coprecipitation reaction, to control in kettle pH value with the reaction time or that salt is added is molten
Liquid product changes linearly, and salting liquid volume, which is added, to be obtained by charging rate and feed time；In period △ t, pH lines
Property variation contain it is linear increase and linear reduction, linear change rate sizes values are ranging from,
The value of pH can with one section variation can also multistage change；The control of pH value is adjusted for automation charging equipment that program controls
The problems such as saving, realize automated production, avoiding manual control trueness error and cost increase.
It enumerates embodiment below the present invention is concretely demonstrated, however, the present invention is not limited to these examples.
Embodiment 1
In 10L reaction kettles, control nitrogen Ventilation Rate is in 200mL/min removal solution and top oxygen, stirring
It is 50 DEG C that 1000rpm controls temperature in the kettle simultaneously.
Configure the aqueous metallic ions of 3M, wherein nickel sulfate：Cobaltous sulfate：Manganese sulfate molar ratio is 5：2：3, then with
10mL/min speed enters reaction kettle, while the automation that sodium hydrate aqueous solution is controlled according to the pH value that Fig. 1 is set by program
Equipment is automatically added in kettle, and pH when reaction starts is set as 10, and control ph linearly increases, and pH value rate of change V is, reaction time 26h, at the same time ammonia spirit it is dense to be continuously pumped into ammonium hydroxide in the kettle needed for maintaining in reaction kettle
It spends constant.
It synthesizes obtained presoma and prepares required positive electrode, 400 DEG C of calcined temperature, burn-in time through two-step sintering
Temperature for 6h, secondary clacining is 900 DEG C, and the time of secondary clacining is 12h.
Embodiment 2
In 10L reaction kettles, control nitrogen Ventilation Rate is in 200mL/min removal solution and top oxygen, stirring
It is 50 DEG C that 1000rpm controls temperature in the kettle simultaneously.
Configure the aqueous metallic ions of 3M, wherein nickel sulfate：Cobaltous sulfate：Manganese sulfate molar ratio is 5：2：3, then with
10mL/min speed enters reaction kettle, while the automation that the pH value that sets according to fig. 2 of sodium hydrate aqueous solution is controlled by program
Equipment is automatically added in kettle, and pH when reaction starts is set as 12.5, control ph linear reduction, and pH value rate of change V is, reaction time 26h, at the same time ammonia spirit it is dense to be continuously pumped into ammonium hydroxide in the kettle needed for maintaining in reaction kettle
It spends constant.
It synthesizes obtained presoma and prepares required positive electrode, 400 DEG C of calcined temperature, burn-in time through two-step sintering
Temperature for 6h, secondary clacining is 900 DEG C, and the time of secondary clacining is 12h.
Embodiment 3
In 10L reaction kettles, control nitrogen Ventilation Rate is in 200mL/min removal solution and top oxygen, stirring
It is 50 DEG C that 1000rpm controls temperature in the kettle simultaneously.
Configure the aqueous metallic ions of 3M, wherein nickel sulfate：Cobaltous sulfate：Manganese sulfate molar ratio is 6：2：2, then with
10mL/min speed enters reaction kettle, while the automation that the pH value that sets according to fig. 3 of sodium hydrate aqueous solution is controlled by program
Equipment is automatically added in kettle, and pH when reaction starts is set as 10, and control ph multistage linear increases, first segment pH rate of changes
V1For, reaction time 10h；Second stage linearly increases, pH rate of changes V2For, the reaction time is
2h；Phase III pH value linearly increases, pH rate of changes V3For, reaction time 4h., at the same time ammonia spirit connect
It is constant to continue ammonia concn in the kettle for being pumped into and remaining required in reaction kettle.
It synthesizes obtained presoma and prepares required positive electrode, 400 DEG C of calcined temperature, burn-in time through two-step sintering
Temperature for 6h, secondary clacining is 800 DEG C, and the time of secondary clacining is 15h.
Embodiment 4
In 10L reaction kettles, control nitrogen Ventilation Rate is in 200mL/min removal solution and top oxygen, stirring
It is 50 DEG C that 1000rpm controls temperature in the kettle simultaneously.
Configure the aqueous metallic ions of 3M, wherein nickel sulfate：Cobaltous sulfate：Manganese sulfate molar ratio is 6：2：2, then with
10mL/min speed enters reaction kettle, while the automation that the pH value that sets according to fig. 3 of sodium hydrate aqueous solution is controlled by program
Equipment is automatically added in kettle, and pH when reaction starts is set as 10, and control ph multistage linear increases, first segment pH rate of changes
V1For, reaction time 10h；Second stage linearly increases, pH rate of changes V2For, the reaction time is
4h；Phase III pH value linear reduction, pH rate of changes V3For, reaction time 6h., at the same time ammonia spirit
It is constant to be continuously pumped into ammonia concn in the kettle needed for being maintained in reaction kettle.
It synthesizes obtained presoma and prepares required positive electrode, 400 DEG C of calcined temperature, burn-in time through two-step sintering
Temperature for 6h, secondary clacining is 800 DEG C, and the time of secondary clacining is 15h.
Claims (3)
1. a kind of synthetic method of anode material for lithium-ion batteries, it is characterised in that：The anode material for lithium-ion batteries is rich lithium
At least one of Mn-based material, ternary material, positive electrode material precursor synthesis use improved coprecipitation, i.e.,
In any one and several periods △ t of coprecipitation reaction, pH value is controlled in kettle with the reaction time or salting liquid is added
Volume changes linearly；
It is described in period △ t, pH linear changes contain it is linear increase and linear reduction, linear change rate sizes values
Ranging from, i.e., in △ t1In reaction time section, rate of change V1, in △ t2When, rate of change
For V2；
The molecular formula of the ternary material is Li1+nNixCoyM1-x-yO2, wherein M is Mn, Al, Mg, Zr, Ce, Ti, Ca, Fe
At least one element, and 0≤n ＜ 0.1,0.3≤x<1,0.1≤y<1,0<x+y<1；
The molecular formula of the lithium-rich manganese base material is, wherein 0<n<1,0<x
<1,0<y<1,0<z<1 and x+y+z=1；
Ranging from 1min ~ 72h of described any one and several periods △ t.
2. a kind of synthetic method of anode material for lithium-ion batteries as described in claim 1, it is characterised in that：The pH value
Variation range be 10 ~ 13 between certain two values between variation.
3. a kind of synthetic method of anode material for lithium-ion batteries as described in claim 1, it is characterised in that：The ternary
Material or lithium-rich manganese base material are obtained through two-step sintering by the presoma synthesized, 300 ~ 500 DEG C of calcined temperature, when pre-burning
Between be 1 ~ 10h, the temperature of secondary clacining is 600 ~ 1000 DEG C, and the time of secondary clacining is 10 ~ 20h.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510951028.8A CN105514411B (en) | 2015-12-19 | 2015-12-19 | A kind of synthetic method of anode material for lithium-ion batteries |
| PCT/CN2016/084412 WO2017101262A1 (en) | 2015-12-19 | 2016-06-01 | Synthesis method for positive electrode material of lithium ion battery |
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| CN201510951028.8A CN105514411B (en) | 2015-12-19 | 2015-12-19 | A kind of synthetic method of anode material for lithium-ion batteries |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105514411B (en) * | 2015-12-19 | 2018-08-10 | 山东玉皇新能源科技有限公司 | A kind of synthetic method of anode material for lithium-ion batteries |
| CN107204423B (en) * | 2017-05-18 | 2020-06-09 | 山东玉皇新能源科技有限公司 | Preparation method and application of high-rate ternary cathode material |
| CN107346824B (en) * | 2017-05-27 | 2020-06-09 | 山东玉皇新能源科技有限公司 | Preparation method and application of gradient ternary cathode material |
| CN108281639A (en) * | 2018-01-31 | 2018-07-13 | 山东德朗能新能源科技有限公司 | A kind of long-life nickle cobalt lithium manganate cylindrical lithium ion battery production method |
| CN111370679A (en) * | 2018-12-25 | 2020-07-03 | 宁德时代新能源科技股份有限公司 | Positive active material precursor, preparation method thereof and positive active material |
| CN113415830B (en) * | 2021-08-24 | 2021-11-05 | 金驰能源材料有限公司 | Preparation method of lithium ion battery anode material precursor |
| CN113571695B (en) * | 2021-09-23 | 2022-01-04 | 长沙理工大学 | Preparation method of gradient ternary cathode material with coating layer |
| CN113800577B (en) * | 2021-09-28 | 2023-08-15 | 南通金通储能动力新材料有限公司 | Method for preparing ternary precursor with small particle size |
| CN114204008A (en) * | 2021-11-23 | 2022-03-18 | 格林美（江苏）钴业股份有限公司 | Preparation method of high-voltage lithium cobalt oxide positive electrode material |
| CN114408984A (en) * | 2021-12-31 | 2022-04-29 | 宜宾光原锂电材料有限公司 | Method for recycling mother liquor in precursor preparation process |
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| CN101202343A (en) * | 2006-12-15 | 2008-06-18 | 中国电子科技集团公司第十八研究所 | Lithium ion battery positive pole material cobalt nickel oxide manganses lithium and method for making same |
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| CN103545504A (en) * | 2013-10-17 | 2014-01-29 | 江西赣锋锂业股份有限公司 | Preparation method of ternary anode material precursor |
| CN103956479A (en) * | 2014-05-20 | 2014-07-30 | 天津理工大学 | Preparation method of spherical high-capacity lithium-rich positive electrode material |
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| CN103413931B (en) * | 2013-08-08 | 2016-01-20 | 北京大学 | Boron doped lithium-enriched cathodic material of lithium ion battery and preparation method thereof |
| CN105514411B (en) * | 2015-12-19 | 2018-08-10 | 山东玉皇新能源科技有限公司 | A kind of synthetic method of anode material for lithium-ion batteries |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101202343A (en) * | 2006-12-15 | 2008-06-18 | 中国电子科技集团公司第十八研究所 | Lithium ion battery positive pole material cobalt nickel oxide manganses lithium and method for making same |
| CN101229928A (en) * | 2007-01-25 | 2008-07-30 | 长沙力元新材料股份有限公司 | Method for preparing spherical nickel-cobalt lithium manganate material |
| CN102092798A (en) * | 2010-12-01 | 2011-06-15 | 兰州金川新材料科技股份有限公司 | Method for continuously synthesizing precursor of lithium ion battery positive material |
| CN103545504A (en) * | 2013-10-17 | 2014-01-29 | 江西赣锋锂业股份有限公司 | Preparation method of ternary anode material precursor |
| CN103956479A (en) * | 2014-05-20 | 2014-07-30 | 天津理工大学 | Preparation method of spherical high-capacity lithium-rich positive electrode material |
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| CN105514411A (en) | 2016-04-20 |
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