CN109546088A - A kind of nickelic tertiary cathode material method for washing - Google Patents
A kind of nickelic tertiary cathode material method for washing Download PDFInfo
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- CN109546088A CN109546088A CN201811373563.XA CN201811373563A CN109546088A CN 109546088 A CN109546088 A CN 109546088A CN 201811373563 A CN201811373563 A CN 201811373563A CN 109546088 A CN109546088 A CN 109546088A
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- Prior art keywords
- washing
- cathode material
- tertiary cathode
- nickelic tertiary
- deionized water
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Classifications
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- 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 provides a kind of method for washing of nickelic tertiary cathode material, a certain amount of anode material of lithium battery (NCM622) is weighed first, with ultrasound a period of time after a certain amount of solid-to-liquid ratio addition deionized water stirring a period of time, then counter in 700 DEG C of oxygen atmosphere after the solution of acquisition being filtered to burn 5h, 5g is taken to be added in the deionized water of 100g in the powder obtained after drying again, it is filtered after stirring, lithium carbonate and lithium hydroxide content in filter liquor is finally tested with potentiometric titration.The present invention propose it is a kind of nickelic tertiary cathode material is handled using ultrasonic wave, reduce material surface residual alkali content method for washing；This method has simple process, easy to operate, the high advantage of Product Safety.
Description
Technical field
The invention belongs to technical field of lithium batteries, in particular to a kind of nickelic tertiary cathode material method for washing.
Background technique
Current lithium ion battery mainly has lithium manganate battery, cobalt acid lithium battery and a ternary battery, and ternary battery with
The advantages that its energy density is high, cycle life is good, environmental-friendly and its cheap and the favor by market rapidly, and apply
In fields such as digital battery, electric cars, but nickelic ternary lithium battery produces gas problem than more serious, and the safety of battery core is always
One very big technological challenge causes ternary power battery to be difficult to the test conditions such as pierce and overcharge by needle.
Carrying out washing to material is a kind of new technology for improving nickelic tertiary cathode material performance, can be reduced by washing
The residual alkali amount of material surface, but the structure of material itself will not be destroyed again.However simple handy deionized water elution cannot fill
Wash off the residual alkali for being adhering closely to powder surface with dividing.
Summary of the invention
The present invention propose it is a kind of nickelic tertiary cathode material is handled using ultrasonic wave, reduce material surface residual alkali
The method for washing of content；This method has simple process, easy to operate, the high advantage of Product Safety.
A kind of method for washing of nickelic tertiary cathode material provided by the invention, comprising the following steps:
Step 1: weighing a certain amount of anode material of lithium battery (NCM622), deionized water is added with a certain amount of solid-to-liquid ratio
Ultrasound a period of time after stirring a period of time；
Step 2: counter in 700 DEG C of oxygen atmosphere after the solution that step 1 obtains is filtered to burn 5h；
Step 3: the powder that step 2 obtains after dry being taken in a certain amount of a certain amount of deionized water of addition, is taken out after stirring
Filter；
Step 4: the filter liquor in step 3 is tested into lithium carbonate and lithium hydroxide content in solution with potentiometric titration.
In a preferred embodiment, in step 1, the quality for weighing NCM622 is 25g.
It in a preferred embodiment, is that 1:4 is stirred ultrasound with solid-liquid mass ratio in step 1.
In a preferred embodiment, in step 1, NCM622 stirs ultrasound after 5min after deionized water is added.
In a preferred embodiment, in step 1, with the frequency of 28khz, 100w after NCM622 aqueous solution stirring 5min
Power ultrasound 2min.
In a preferred embodiment, it in step 3, takes 5g powder to be added in 95g deionized water and stirs.
In a preferred embodiment, in step 4, the molar concentration of HCL titration solution used in potentiometric titration is
0.2mol/L。
Using ultrasonic wave come to positive electrode in the method for washing of nickelic tertiary cathode material provided by the invention
Reason, can reduce material surface residual alkali content, the basicity of material is effectively reduced, will not make again while improving material safety
Reduced at cycle performance, at the same battery producing gas problem also reduce to a certain extent.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is XRD diagram of the embodiment of the present invention 1 through the tertiary cathode material before and after ultrasonic wave water washing.
Fig. 2 is the SEM figure of tertiary cathode material of the embodiment of the present invention 1 after ultrasonic wave water washing.
Specific embodiment
A kind of method for washing of nickelic tertiary cathode material provided by the invention, comprising the following steps:
Step 1: weighing a certain amount of anode material of lithium battery (NCM622), deionized water is added with a certain amount of solid-to-liquid ratio
Ultrasound a period of time after stirring a period of time；
Step 2: counter in 700 DEG C of oxygen atmosphere after the solution that step 1 obtains is filtered to burn 5h；
Step 3: the powder that step 2 obtains after dry being taken in a certain amount of a certain amount of deionized water of addition, is taken out after stirring
Filter；
Step 4: the filter liquor in step 3 is tested into lithium carbonate and lithium hydroxide content in solution with potentiometric titration.
In other embodiments, sonication times can be modified.
Embodiment 1:
1. weighing 25gNCM622,100g deionized water is added, stirs 5min, with the frequency of 28khz, the power of 100w is super
Sound 5min；
2. filtering and counter in 700 DEG C of oxygen atmosphere burning 5h；
3. taking the powder after 5g drying and 95g deionized water being added, is filtered after stirring 5min, measure lithium carbonate in filter liquor
With lithium hydroxide content.
Embodiment 2:
1. weighing 25gNCM622,100g deionized water is added, stirs 5min, with the frequency of 28khz, the power of 100w is super
Sound 2min；
2. filtering and counter in 700 DEG C of oxygen atmosphere burning 5h；
3. taking the powder after 5g drying and 95g deionized water being added, is filtered after stirring 5min, measure lithium carbonate in filter liquor
With lithium hydroxide content.
Embodiment 3:
1. weighing 25gNCM622,100g deionized water is added, stirs 5min, with the frequency of 28khz, the power of 100w is super
Sound 10min；
2. filtering and counter in 700 DEG C of oxygen atmosphere burning 5h；
3. taking the powder after 5g drying and 95g deionized water being added, is filtered after stirring 5min, measure lithium carbonate in filter liquor
With lithium hydroxide content.
Referring to FIG. 1, as the result is shown by XRD of the embodiment 1 through the tertiary cathode material before and after ultrasonic wave water washing: before ultrasound
Normal distribution is presented in particle size distribution law afterwards.Wash material it is sonicated after, size distribution curve integrally moves to right, and to two
End extends.D10 reduces, and D90 increases, and illustrates that ultrasonic treatment will lead to material and generate a small amount of fine powder, but size distribution is full on the whole
Foot " YS/T 798-2012 nickle cobalt lithium manganate " professional standard: Granularity Distribution requires to be in normal distribution, and D10 is not less than 2 μm,
D50 should be 5 μm~15 μm, and D90 is not more than 30 μm.
Referring to FIG. 2, the SEM of the tertiary cathode material by embodiment 1 after ultrasonic wave water washing is as the result is shown: ultrasonic treatment
The particle of 5min, though there is a small amount of fine powder to generate, granule-morphology still keeps spherical particle and dispersion is more equal without significant change
It is even.
Using ultrasonic wave come to positive electrode in the method for washing of nickelic tertiary cathode material provided by the invention
Reason, can reduce material surface residual alkali content, the basicity of material is effectively reduced, will not make again while improving material safety
Reduced at cycle performance, at the same battery producing gas problem also reduce to a certain extent.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is to combine specific preferred embodiment to institute of the present invention
The further description of work is, and it cannot be said that specific implementation of the invention is confined to these explanations.It is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., should be included within the scope of the present invention within principle.
Claims (7)
1. a kind of nickelic tertiary cathode material method for washing, it is characterised in that: the following steps are included:
Step 1: weighing a certain amount of anode material of lithium battery (NCM622), deionized water stirring is added with a certain amount of solid-to-liquid ratio
Ultrasound a period of time after a period of time；
Step 2: counter in 700 DEG C of oxygen atmosphere after the solution that step 1 obtains is filtered to burn 5h；
Step 3: the powder that step 2 obtains after dry being taken in a certain amount of a certain amount of deionized water of addition, is filtered after stirring；
Step 4: the filter liquor in step 3 is tested into lithium carbonate and lithium hydroxide content in solution with potentiometric titration.
2. a kind of nickelic tertiary cathode material method for washing as described in claim 1, it is characterised in that: in step 1, weigh
The quality of NCM622 is 25g.
3. a kind of nickelic tertiary cathode material method for washing as described in claim 1, it is characterised in that: in step 1, with solid-liquid
Mass ratio is that 1:4 is stirred ultrasound.
4. a kind of nickelic tertiary cathode material method for washing as described in claim 1, it is characterised in that: in step 1, NCM622
Ultrasound after 5min is stirred after deionized water is added.
5. a kind of nickelic tertiary cathode material method for washing as described in claim 1, it is characterised in that: in step 1, NCM622
With the frequency of 28khz, the power ultrasound 5min of 100w after aqueous solution stirring 5min.
6. a kind of nickelic tertiary cathode material method for washing as described in claim 1, it is characterised in that: in step 3, take 5g powder
End is added in 95g deionized water and stirs.
7. a kind of nickelic tertiary cathode material method for washing as described in claim 1, it is characterised in that: in step 4, current potential drop
The molar concentration for determining HCL titration solution used in method is 0.2mol/L.
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| CN201811373563.XA CN109546088A (en) | 2018-11-19 | 2018-11-19 | A kind of nickelic tertiary cathode material method for washing |
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| CN201811373563.XA CN109546088A (en) | 2018-11-19 | 2018-11-19 | A kind of nickelic tertiary cathode material method for washing |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110336020A (en) * | 2019-07-22 | 2019-10-15 | 广东邦普循环科技有限公司 | A kind of high voltage compound lithium cobaltate cathode material and its preparation method and application |
| CN112952067A (en) * | 2021-04-01 | 2021-06-11 | 合肥国轩高科动力能源有限公司 | Preparation method of yttrium oxide graphene modified nickel cobalt lithium manganate composite material for lithium ion battery and prepared composite material |
| CN113666431A (en) * | 2021-07-30 | 2021-11-19 | 蜂巢能源科技有限公司 | Method for removing residual alkali in high-nickel ternary cathode material, high-nickel ternary cathode material and lithium ion battery |
| CN114369862A (en) * | 2021-12-23 | 2022-04-19 | 北京当升材料科技股份有限公司 | Preparation method of low-cost lithium battery ternary cathode material |
| CN115041459A (en) * | 2022-06-15 | 2022-09-13 | 江西理工大学 | Method for cleaning residual alkali on surface of anode material of lithium ion battery |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102239586A (en) * | 2009-02-05 | 2011-11-09 | Agc清美化学股份有限公司 | Surface-modified lithium-containing complex oxide for positive electrode active material for lithium ion secondary battery, and method for producing same |
| CN103400978A (en) * | 2013-08-01 | 2013-11-20 | 奇瑞汽车股份有限公司 | Method for modifying lithium nickel manganese oxide material, lithium nickel manganese oxide material and lithium ion battery |
| CN104752713A (en) * | 2013-12-30 | 2015-07-01 | 北京当升材料科技股份有限公司 | Lithium ion battery composite anode material and preparation method thereof |
| CN105810929A (en) * | 2014-12-31 | 2016-07-27 | 北京当升材料科技股份有限公司 | Treatment method for reducing residual alkalis on surface of high nickel material |
| CN108063223A (en) * | 2017-11-17 | 2018-05-22 | 合肥国轩高科动力能源有限公司 | A kind of preparation method for being modified nickelic tertiary cathode material |
| KR20180111552A (en) * | 2017-03-31 | 2018-10-11 | 주식회사 포스코이에스엠 | Manufacturing method of metal coated cathode active material And cathode active material made by the same |
| CN108777295A (en) * | 2018-05-29 | 2018-11-09 | 中航锂电（洛阳）有限公司 | A kind of nickel cobalt lithium manganate and preparation method thereof, lithium ion battery |
-
2018
- 2018-11-19 CN CN201811373563.XA patent/CN109546088A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102239586A (en) * | 2009-02-05 | 2011-11-09 | Agc清美化学股份有限公司 | Surface-modified lithium-containing complex oxide for positive electrode active material for lithium ion secondary battery, and method for producing same |
| CN103400978A (en) * | 2013-08-01 | 2013-11-20 | 奇瑞汽车股份有限公司 | Method for modifying lithium nickel manganese oxide material, lithium nickel manganese oxide material and lithium ion battery |
| CN104752713A (en) * | 2013-12-30 | 2015-07-01 | 北京当升材料科技股份有限公司 | Lithium ion battery composite anode material and preparation method thereof |
| CN105810929A (en) * | 2014-12-31 | 2016-07-27 | 北京当升材料科技股份有限公司 | Treatment method for reducing residual alkalis on surface of high nickel material |
| KR20180111552A (en) * | 2017-03-31 | 2018-10-11 | 주식회사 포스코이에스엠 | Manufacturing method of metal coated cathode active material And cathode active material made by the same |
| CN108063223A (en) * | 2017-11-17 | 2018-05-22 | 合肥国轩高科动力能源有限公司 | A kind of preparation method for being modified nickelic tertiary cathode material |
| CN108777295A (en) * | 2018-05-29 | 2018-11-09 | 中航锂电（洛阳）有限公司 | A kind of nickel cobalt lithium manganate and preparation method thereof, lithium ion battery |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110336020A (en) * | 2019-07-22 | 2019-10-15 | 广东邦普循环科技有限公司 | A kind of high voltage compound lithium cobaltate cathode material and its preparation method and application |
| CN112952067A (en) * | 2021-04-01 | 2021-06-11 | 合肥国轩高科动力能源有限公司 | Preparation method of yttrium oxide graphene modified nickel cobalt lithium manganate composite material for lithium ion battery and prepared composite material |
| CN113666431A (en) * | 2021-07-30 | 2021-11-19 | 蜂巢能源科技有限公司 | Method for removing residual alkali in high-nickel ternary cathode material, high-nickel ternary cathode material and lithium ion battery |
| CN114369862A (en) * | 2021-12-23 | 2022-04-19 | 北京当升材料科技股份有限公司 | Preparation method of low-cost lithium battery ternary cathode material |
| CN115041459A (en) * | 2022-06-15 | 2022-09-13 | 江西理工大学 | Method for cleaning residual alkali on surface of anode material of lithium ion battery |
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Application publication date: 20190329 |