CN108075132A - A kind of preparation method of the nickel cobalt manganese persursor material with special internal structure - Google Patents
A kind of preparation method of the nickel cobalt manganese persursor material with special internal structure Download PDFInfo
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- CN108075132A CN108075132A CN201711382666.8A CN201711382666A CN108075132A CN 108075132 A CN108075132 A CN 108075132A CN 201711382666 A CN201711382666 A CN 201711382666A CN 108075132 A CN108075132 A CN 108075132A
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- nickel cobalt
- cobalt manganese
- internal structure
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- preparation
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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
- 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
-
- 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
Abstract
The present invention relates to the material prepared technology field of ternary cathode material of lithium ion battery, more particularly to a kind of preparation method of the nickel cobalt manganese persursor material with special internal structure.The present invention adds in reducing agent in the liquid of bottom, the Mn that can be aoxidized part3+It is reduced into Mn2+, the oxidation during nucleus is formed is reduced, improves the crystallinity of nucleus, the internal structure of composition rule arrangement forms a kind of special internal structure outwards radially arranged by particle centre.Because internal structure aligns to a certain extent, energy needed for lithium ion diffusion, raising Li can be reduced+Diffusion coefficient contributes to lithium ion diffusion, deintercalation, reduces lithium nickel mixing, so that positive electrode has good capacity retention ratio and cycle performance after sintering.
Description
Technical field
It is more particularly to a kind of that there is spy the present invention relates to the material prepared technology field of ternary cathode material of lithium ion battery
The preparation method of the nickel cobalt manganese persursor material of different internal structure.
Background technology
Nowadays, the rapid development of mobile electronic device, electric vehicle and hybrid vehicle promotes lithium ion battery
Technology is advanced by leaps and bounds.But anode material for lithium-ion batteries at present, as cobalt acid lithium, LiFePO4 all have capacity is low to lack
Point, it is impossible to meet the requirement of future source of energy development.And nickle cobalt lithium manganate is good and cheap with specific capacity height, thermal stability
The advantages that, it is most potential one kind in anode material for lithium-ion batteries, has very in fields such as electric car, electric tools
Good application prospect.
Nickel cobalt manganese hydroxide, i.e. nickel-cobalt-manganese ternary presoma can synthesize nickel cobalt by adding in lithium source by high temperature sintering
LiMn2O4.Size, pattern, structure of ternary precursor etc. have a direct impact the technical indicator of nickle cobalt lithium manganate, therefore forerunner
Body is most important to the production of ternary material.At present, the common method for preparing nickel cobalt manganese hydroxide crystallizes hydroxide in order to control
Object coprecipitation, but the nickel cobalt manganese persursor material internal structure that existing method is prepared rule cannot arrange in certain direction
Row, lithium ion be not easy deintercalation, cation easily occur mixing, sintered positive electrode do not have good capacity retention ratio and
Cycle performance.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of internal structure, rule is arranged in certain direction
Row contribute to lithium ion deintercalation, reduce cationic mixing, and positive electrode has good capacity retention ratio and cyclicity after sintering
The preparation method of the nickel cobalt manganese persursor material of energy.
In order to achieve the above object, the preparation of a kind of nickel cobalt manganese persursor material with special internal structure of the invention
Method comprises the following specific steps that：
(1) the nickel cobalt manganese salt solution that concentration of metal ions is 1.0~3.0mol/L is configured, configuration concentration is 150~300g/
The sodium hydroxide solution of L, configuration concentration are 10%~30% ammonium hydroxide；
(2) deionized water is added in into sealing reaction kettle to lower floor's agitating paddle is just flooded, opens stirring, it is warming up to 50~
70 DEG C, lead to nitrogen or argon gas when inert gas shieldings 2 are small more than；
(3) reducing agent, sodium hydroxide solution and ammonium hydroxide, control reducing agent, sodium hydroxide solution, ammonium hydroxide are added in into bottom liquid
Each enter the flow of reaction kettle, the ammonia density of regulation system is 6.0~12.0g/L, pH value is 10.0~12.0, reducing agent
Quality is the 0.1%~10.0% of three metal ion species gross mass of nickel cobalt manganese；
(4) nickel cobalt manganese salt solution, sodium hydroxide solution and ammonium hydroxide are added in into reaction kettle simultaneously, control nickel cobalt manganese salt solution,
Sodium hydroxide solution, ammonium hydroxide each enter reaction kettle flow, make system maintain pH value 10.0~12.0, ammonia concn 6.0~
12.0g/L, until granularity reaches 3.0~15.0 μm of desired value；
(5) generated hydroxide precipitation concentration is the potassium hydroxide or hydroxide of 0.1~0.5mol/L after reacting
Sodium solution washs 120~180min, then with pure water rinsing 2~3 times；
(6) finally the nickel cobalt manganese hydroxide filter cake after washing is placed in baking oven and dried to get to special internal
The nickel cobalt manganese persursor material of structure.
Preferably, nickel used in the nickel cobalt manganese salt solution, cobalt, manganese salt are nickel, cobalt, the sulfate of manganese, chlorate,
One or more in nitrate.
Preferably, speed of agitator control is in 300~500rpm.
Preferably, the reducing agent is vulcanized sodium or sodium sulfite.
Preferably, the control of the temperature of washing potassium hydroxide or sodium hydroxide solution and pure water is at 50~80 DEG C.
Preferably, filter cake drying temperature is 80~120 DEG C, drying time is 8~20h.
During nickel cobalt manganese persursor material is prepared using existing coprecipitation method, nickel cobalt manganese salt solution, hydroxide
Sodium solution and ammonium hydroxide exposure in air, can be there are certain dissolved oxygens in solution, thus Mn2+It is oxidizable, cause a part of Mn2 +It is oxidized to Mn3+, Mn3+Presence can cause that grain crystalline is poor, uniformity is not high, and then influence the property of follow-up positive electrode
Energy.The present invention adds in reducing agent in the liquid of bottom, the Mn that can be aoxidized part3+It is reduced into Mn2+, during reducing nucleus formation
Oxidation, improves the crystallinity of nucleus, the internal structure of composition rule arrangement, form it is a kind of by particle centre outwards radially
The special internal structure of arrangement.Because internal structure aligns to a certain extent, energy needed for lithium ion diffusion can be reduced,
Improve Li+Diffusion coefficient contributes to lithium ion diffusion, deintercalation, reduces lithium nickel mixing, so that positive electrode is with good after sintering
Good capacity retention ratio and cycle performance.
Description of the drawings
Fig. 1 is the internal structure schematic diagram of nickel cobalt manganese persursor material of the present invention.
Fig. 2 is the electron-microscope scanning figure of nickel cobalt manganese persursor material internal structure of the present invention.
Specific embodiment
Present invention work is further illustrated with reference to embodiment, but the invention is not limited in specific embodiments.
Embodiment 1：
A kind of preparation method of the nickel cobalt manganese persursor material with special internal structure, comprises the following steps：
(1) the nickel cobalt manganese salt solution that concentration of metal ions is 2.0mol/L, configuration concentration of sodium hydroxide solution 250g/ are configured
L configures ammonia concn 21%；
(2) deionized water is added in into sealing reaction kettle to heat up to lower floor's agitating paddle, speed of agitator 400rpm is just flooded
To 60 DEG C, lead to nitrogen or argon gas when gas shields 2 are small more than；
(3) reducing agent, sodium hydroxide solution, ammonium hydroxide are added in into bottom liquid, adjusting ammonia density is 8.0~10.0g/L, pH value
For 10.0~12.0, the quality of reducing agent is the 5% of three metal ion species gross masses；
(4) nickel cobalt manganese salt solution, sodium hydroxide solution, ammonium hydroxide are added in into reaction kettle simultaneously, and maintain pH value 10.0~
12.0,8.0~10.0g/L of ammonia density, until granularity reaches 3.0~15.0 μm of desired value；
(5) potassium hydroxide or sodium hydroxide solution that generated hydroxide precipitation is 0.3mol/L with concentration after reacting
Wash 150min, then with pure water rinsing 3 times；
(6) by the nickel cobalt manganese hydroxide filter cake after washing be placed in baking oven 105 DEG C of dry 15h to get to Na≤
0.01%th, S≤0.1% has special internal structure nickel cobalt manganese persursor material.
Embodiment 2：
A kind of preparation method of the nickel cobalt manganese persursor material with special internal structure, comprises the following steps：
(1) the nickel cobalt manganese salt solution that concentration of metal ions is 1.0mol/L, configuration concentration of sodium hydroxide solution 150g/ are configured
L configures ammonia concn 10%；
(2) deionized water is added in into sealing reaction kettle to heat up to lower floor's agitating paddle, speed of agitator 300rpm is just flooded
To 50 DEG C, lead to nitrogen or argon gas when gas shields 2 are small more than；
(3) reducing agent, sodium hydroxide solution, ammonium hydroxide are added in into bottom liquid, adjusting ammonia density is 6.0~8.0g/, pH value is
10.0~12.0, the quality of reducing agent is the 0.1% of three metal ion species gross masses；
(4) nickel cobalt manganese salt solution, sodium hydroxide solution, ammonium hydroxide are added in into reaction kettle simultaneously, and maintain pH value 10.0~
12.0,6.0~8.0g/L of ammonia density, until granularity reaches 3.0~15.0 μm of desired value；
(5) potassium hydroxide or sodium hydroxide solution that generated hydroxide precipitation is 0.1mol/L with concentration after reacting
Wash 180min, then with pure water rinsing 3 times；
(6) by the nickel cobalt manganese hydroxide filter cake after washing be placed in baking oven 80 DEG C of dry 20h to get to Na≤
0.01%th, S≤0.1% has special internal structure nickel cobalt manganese persursor material.
Embodiment 3：
A kind of preparation method of the nickel cobalt manganese persursor material with special internal structure, comprises the following steps：
(1) the nickel cobalt manganese salt solution that concentration of metal ions is 3.0mol/L, configuration concentration of sodium hydroxide solution 300g/ are configured
L configures ammonia concn 30%；
(2) deionized water is added in into sealing reaction kettle to heat up to lower floor's agitating paddle, speed of agitator 500rpm is just flooded
To 70 DEG C, lead to nitrogen or argon gas when gas shields 2 are small more than；
(3) reducing agent, sodium hydroxide solution, ammonium hydroxide are added in into bottom liquid, adjusting ammonia density is 10.0~12.0g/L, pH
It is worth for 10.0~12.0, the quality of reducing agent is the 10% of three metal ion species gross masses；
(4) nickel cobalt manganese salt solution, sodium hydroxide solution, ammonium hydroxide are added in into reaction kettle simultaneously, and maintain pH value 10.0~
12.0,10.0~12.0g/L of ammonia density, until granularity reaches 3.0~15.0 μm of desired value；
(5) potassium hydroxide or sodium hydroxide solution that generated hydroxide precipitation is 0.5mol/L with concentration after reacting
Wash 120min, then with pure water rinsing 2 times；
(6) by the nickel cobalt manganese hydroxide filter cake after washing be placed in baking oven 120 DEG C of dry 8h to get to Na≤
0.01%th, S≤0.1% has special internal structure nickel cobalt manganese persursor material.
Claims (6)
1. a kind of preparation method of the nickel cobalt manganese persursor material with special internal structure, it is characterised in that：Including having as follows
Body step：
(1) the nickel cobalt manganese salt solution that concentration of metal ions is 1.0~3.0mol/L is configured, configuration concentration is 150~300g/L's
Sodium hydroxide solution, configuration concentration are 10%~30% ammonium hydroxide；
(2) deionized water is added in into sealing reaction kettle to lower floor's agitating paddle is just flooded, stirring is opened, is warming up to 50~70
DEG C, lead to nitrogen or argon gas when inert gas shieldings 2 are small more than；
(3) reducing agent, sodium hydroxide solution and ammonium hydroxide are added in into bottom liquid, control reducing agent, sodium hydroxide solution, ammonium hydroxide are each
Into the flow of reaction kettle, the ammonia density of regulation system is 6.0~12.0g/L, pH value is 10.0~12.0, the quality of reducing agent
For the 0.1%~10.0% of three metal ion species gross mass of nickel cobalt manganese；
(4) nickel cobalt manganese salt solution, sodium hydroxide solution and ammonium hydroxide are added in into reaction kettle, control nickel cobalt manganese salt solution, hydrogen-oxygen simultaneously
Change sodium solution, ammonium hydroxide each enter reaction kettle flow, make system maintain pH value 10.0~12.0, ammonia concn 6.0~
12.0g/L, until granularity reaches 3.0~15.0 μm of desired value；
(5) potassium hydroxide or sodium hydroxide that generated hydroxide precipitation concentration is 0.1~0.5mol/L after reacting are molten
Liquid washs 120~180min, then with pure water rinsing 2~3 times；
(6) finally the nickel cobalt manganese hydroxide filter cake after washing is placed in baking oven and dried to get to special internal structure
Nickel cobalt manganese persursor material.
2. a kind of preparation method of nickel cobalt manganese persursor material with special internal structure according to claim 1,
It is characterized in that：Nickel, cobalt, manganese salt used in the nickel cobalt manganese salt solution are nickel, in cobalt, the sulfate of manganese, chlorate, nitrate
One or more.
3. a kind of preparation method of nickel cobalt manganese persursor material with special internal structure according to claim 1,
It is characterized in that：Speed of agitator is controlled in 300~500rpm.
4. a kind of preparation method of nickel cobalt manganese persursor material with special internal structure according to claim 1,
It is characterized in that：The reducing agent is vulcanized sodium or sodium sulfite.
5. a kind of preparation method of nickel cobalt manganese persursor material with special internal structure according to claim 1,
It is characterized in that：The temperature of washing potassium hydroxide or sodium hydroxide solution and pure water is controlled at 50~80 DEG C.
6. a kind of preparation method of nickel cobalt manganese persursor material with special internal structure according to claim 1,
It is characterized in that：Filter cake drying temperature is 80~120 DEG C, and drying time is 8~20h.
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| CN201711382666.8A CN108075132A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of the nickel cobalt manganese persursor material with special internal structure |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109250764A (en) * | 2018-08-30 | 2019-01-22 | 华友新能源科技（衢州）有限公司 | Partial size nickel cobalt manganese persursor material preparation method in a kind of power type |
| CN109713297A (en) * | 2018-12-26 | 2019-05-03 | 宁波容百新能源科技股份有限公司 | A kind of nickelic positive electrode and preparation method thereof that primary particle aligns |
| CN110957482A (en) * | 2019-11-30 | 2020-04-03 | 华友新能源科技（衢州）有限公司 | Hexavalent element-added nickel-cobalt-manganese composite hydroxide and preparation method thereof |
| CN112151790A (en) * | 2020-08-26 | 2020-12-29 | 万华化学集团股份有限公司 | High-nickel ternary cathode material precursor, crystal face controllable growth method thereof, ternary cathode material and lithium ion battery |
| CN113880148A (en) * | 2021-10-22 | 2022-01-04 | 广东佳纳能源科技有限公司 | Ternary precursor and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109250764A (en) * | 2018-08-30 | 2019-01-22 | 华友新能源科技（衢州）有限公司 | Partial size nickel cobalt manganese persursor material preparation method in a kind of power type |
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| CN109713297A (en) * | 2018-12-26 | 2019-05-03 | 宁波容百新能源科技股份有限公司 | A kind of nickelic positive electrode and preparation method thereof that primary particle aligns |
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| CN110957482A (en) * | 2019-11-30 | 2020-04-03 | 华友新能源科技（衢州）有限公司 | Hexavalent element-added nickel-cobalt-manganese composite hydroxide and preparation method thereof |
| CN110957482B (en) * | 2019-11-30 | 2021-08-03 | 华友新能源科技（衢州）有限公司 | Hexavalent element-added nickel-cobalt-manganese composite hydroxide and preparation method thereof |
| CN112151790A (en) * | 2020-08-26 | 2020-12-29 | 万华化学集团股份有限公司 | High-nickel ternary cathode material precursor, crystal face controllable growth method thereof, ternary cathode material and lithium ion battery |
| CN112151790B (en) * | 2020-08-26 | 2022-03-08 | 万华化学集团股份有限公司 | High-nickel ternary cathode material precursor, crystal face controllable growth method thereof, ternary cathode material and lithium ion battery |
| CN113880148A (en) * | 2021-10-22 | 2022-01-04 | 广东佳纳能源科技有限公司 | Ternary precursor and preparation method and application thereof |
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Application publication date: 20180525 |