CN107230799A - A kind of chemical synthesizing method of lithium titanate battery - Google Patents
A kind of chemical synthesizing method of lithium titanate battery Download PDFInfo
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- CN107230799A CN107230799A CN201710555546.7A CN201710555546A CN107230799A CN 107230799 A CN107230799 A CN 107230799A CN 201710555546 A CN201710555546 A CN 201710555546A CN 107230799 A CN107230799 A CN 107230799A
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- lithium titanate
- titanate battery
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
- H01M10/446—Initial charging measures
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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
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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
It is main to include pre- chemical conversion aging and the low current high temperature chemical conversion step of aging two the invention discloses a kind of chemical synthesizing method of lithium titanate battery.The first step, is melted into aging in advance, the lithium titanate battery that fluid injection is honored as a queen in advance is placed in high-temperature cabinet shelved first, and fully after infiltration, upper fixture is melted into advance, with certain electric current constant-current charge, and carrying out high temperature after pre- chemical conversion shelves.Second step, the chemical conversion aging of low current high temperature.Lithium titanate battery after pre- chemical conversion is placed in high-temperature cabinet and heated, low current charge to high potential enters between-line spacing floating charge, then carry out high temperature ageing, go clamping plate to be evacuated secondary sealing with more low current.The process employs two step den processes, the moisture of lithium titanate battery is fully reacted, and realize cathode film formation simultaneously, obstruct catalytic decompositions of the lithium titanate surface Ti3+ to electrolyte solvent.The gas production during lithium titanate battery high temperature circulation is greatly reduced, so as to improve normal temperature and high temperature cyclic performance.
Description
Technical field
The present invention relates to cell art, more particularly to a kind of chemical synthesizing method of lithium titanate battery.
Background technology
Lithium titanate battery is because its security is good, multiplying power power-performance is good, normal temperature circulation long lifespan the advantages of cause
The extensive attention of art circle and industrial quarters, particularly has batch application in the case in the fields such as electric car, energy storage in recent years.But
During lithium titanate battery practical study and application, it is found that lithium titanate battery has flatulence, particularly at high temperature
Flatulence is more serious, has severely impacted the cycle performance of battery.
At present, to lithium titanate battery flatulence the reason for, has compared clear and definite mechanism and has explained, the residual moisture in battery with
And the Ti3+ on lithium titanate surface is to main cause that the catalytic decomposition of electrolyte solvent (particularly at high temperature) is its aerogenesis.Titanium
The researchers of sour lithium material and battery mainly are modified with two aspects of electrolyte film for additive to change by lithium titanate material
The high temperature flatulence problem of kind lithium titanate battery.But the high temperature flatulence that the above method can not be fully solved lithium titanate battery is asked
Topic, it is necessary to which preparation, chemical synthesis technology with reference to lithium titanate battery are solved.
In the chemical synthesis technology research of lithium titanate battery, existing researcher have studied the chemical conversion work of low current and high temperature ageing
Skill is (such as：Liu Jinliang, peak, Zhang Rubin, etc. the chemical synthesizing method of lithium titanate battery, Chinese patent, application number：
201410765009.1) preferable suppression aerogenesis effect, has been obtained, but still has failed that lithium titanate battery high temperature aerogenesis pair is completely eliminated
The influence of the electrical properties such as circulation.
The content of the invention
The technical problem existed based on background technology, the present invention proposes a kind of chemical synthesizing method of lithium titanate battery.
A kind of chemical synthesizing method of lithium titanate battery proposed by the present invention, is carried out after pre- chemical conversion aging first to lithium titanate battery
Low current chemical conversion aging is carried out again；
Pre- chemical conversion aging comprises the following steps：
S1, the lithium titanate battery that fluid injection is honored as a queen in advance is placed in hot environment to infiltration very first time threshold value；
S2, by definite value electric current I1 to high temperature infiltrate after lithium titanate battery constant-current charge to cell voltage reach it is default
First voltage value V1；
S3, the lithium titanate battery high temperature of charging complete shelved into the second time threshold；
Low current chemical conversion aging comprises the following steps：
S4, cell voltage is charged to the lithium titanate battery after pre- chemical conversion aging with definite value electric current I2 in hot environment reached
To default second voltage value V2, I2 ＜ I1；
S5, enter between-line spacing floating charge to lithium titanate battery with definite value electric current I3, floating charge blanking voltage is second voltage value V2, I3
＜ I2；
S6, the lithium titanate battery terminated to floating charge carry out high temperature ageing and continue the 3rd time threshold；
S7, aging terminate, and lithium titanate battery is evacuated, then secondary sealing.
Preferably, in step S1, the temperature of hot environment is 0-65 DEG C, and very first time threshold value is 8-24h.
Preferably, in step S2, I1 is 0.2C-1C, and first voltage value V1 is 2.3-2.6V.
Preferably, in step S3, the temperature that high temperature is shelved is 40-65 DEG C, and the second time threshold is 12-48h.
Preferably, in step S4, high ambient temperatures are 40-65 DEG C.
Preferably, in step S4, definite value electric current I2 is 0.02-0.2C, and second voltage value V2 is 2.7-3.0V.
Preferably, in step S5, definite value electric current I3 is 0.01-0.05C, and total time in floating charge stage is 8-48h.
Preferably, in step S6, high temperature ageing temperature is 40-65 DEG C, and the 3rd time threshold is 1-7 days.
Preferably, in step S2, then the lithium titanate battery upper fixture after the preferred infiltration to high temperature carries out constant current and fills again
Electricity；In step S7, then the lithium titanate battery de-chucking terminated first to aging is evacuated and secondary sealing again.
The chemical synthesizing method for the lithium titanate battery that the present invention is provided, lithium titanate battery chemical conversion is carried out in two steps, the first step is pre-
It is the irreversible electrochemical reaction under the conditions of battery core water removal, preliminary aerogenesis and completion low potential to be melted into the main purpose of aging；The
The main purpose of two step low current high temperature chemical conversion is completes negative pole lithium titanate material surface filming, and the purpose of aging is to stablize negative pole
Film forming and completion electrolyte decomposition gas generation process.The chemical synthesizing method be conducive in battery high-temperature cyclic process the reduction of gas production and
Performance is stable.
Brief description of the drawings
Fig. 1 is a kind of chemical synthesizing method flow chart of lithium titanate battery proposed by the present invention；
Fig. 2 is high-temperature cycle life figure of the lithium titanate soft-package battery of the preparation of embodiment 1 after being melted into aging.
Embodiment
A kind of chemical synthesizing method for lithium titanate battery that the present invention is provided, is carried out after pre- chemical conversion aging first to lithium titanate battery
Low current chemical conversion aging is carried out again.
Pre- chemical conversion aging comprises the following steps S1-S3.
S1, the lithium titanate battery that fluid injection is honored as a queen in advance is placed in hot environment to infiltration very first time threshold value.In this step,
The temperature of hot environment is 0-65 DEG C, and very first time threshold value is 8-24h.
S2, by definite value electric current I1 to high temperature infiltrate after lithium titanate battery constant-current charge to cell voltage reach it is default
First voltage value V1.I1 is 0.2C-1C, and first voltage value V1 is 2.3-2.6V.
S3, the lithium titanate battery high temperature of charging complete shelved into the second time threshold.In this step, the temperature that high temperature is shelved
For 40-65 DEG C, the second time threshold is 12-48h.
Low current chemical conversion aging comprises the following steps S4-S7.
S4, cell voltage is charged to the lithium titanate battery after pre- chemical conversion aging with definite value electric current I2 in hot environment reached
To default second voltage value V2, I2 ＜ I1.In this step, high ambient temperatures are 40-65 DEG C, and definite value electric current I2 is 0.02-
0.2C, second voltage value V2 are 2.7-3.0V.
S5, enter between-line spacing floating charge to lithium titanate battery with definite value electric current I3, floating charge blanking voltage is second voltage value V2, I3
＜ I2.In this step, definite value electric current I3 is 0.01-0.05C, and total time in floating charge stage is 8-48h.
S6, the lithium titanate battery terminated to floating charge carry out high temperature ageing and continue the 3rd time threshold.In this step, high temperature
Aging temperature is 40-65 DEG C, and the 3rd time threshold is 1-7 days.
S7, aging terminate, and lithium titanate battery is evacuated, then secondary sealing.
In present embodiment, in order to ensure in stabilization of the lithium titanate battery in formation process, step S2, first choice is to high temperature
Lithium titanate battery upper fixture after infiltration, then carries out constant-current charge again.In step S7, the lithium titanate electricity terminated first to aging
Pond de-chucking, is then evacuated and secondary sealing again.
Embodiment 1
Reference picture 1, the present embodiment is carried out specifically by taking 8Ah lithium titanate soft-package batteries as an example to technical scheme
It is bright.Specifically, the 8Ah lithium titanate soft-package batteries, just extremely auspicious Xiang ternary NCM111, negative pole is self-produced lithium titanate LTO, and barrier film is
Cangzhou jewel 12+4 one side ceramic diaphragms, electrolyte is that Guangzhou is bestowed by heaven lithium titanate special electrolysis liquid.
In the present embodiment, pre- chemical conversion aging is specific as follows.
In step S1, the 8Ah lithium titanate batteries that fluid injection, sealing are completed are placed in 55 DEG C of high-temperature cabinets, are lain low and are shelved 12h,
So that electrolyte fully infiltrates both positive and negative polarity pole piece and barrier film, to complete high temperature infiltration.In step S2, titanium after high temperature infiltration will be completed
Acid lithium battery is placed in after 4h at room temperature, and upper fixture is charged on 5V, 10A formation cabinet, specifically can select new prestige formation cabinet,
Charging current I1 is 0.5C (i.e. 4A), and charge cutoff voltage is that first voltage value V1 is 2.6V.In step S3, by charging complete
Lithium titanate soft-package battery is placed in aging 24h in 55 DEG C of high-temperature cabinets, to complete pre- chemical conversion.
In the present embodiment, low current chemical conversion aging is specific as follows.
In step S4, the lithium titanate battery after pre- chemical conversion is placed in 55 DEG C of high-temperature cabinets, permanent with 0.1C (0.8A) low currents I2
Current charge to cell voltage reaches second voltage value V2=2.8V；Then perform step S5, with 0.05C (0.4A) electric current I3 every
Once, blanking voltage is that second voltage value V2 is 2.8V for floating charge in 10 minutes.In the present embodiment, floating charge 80 times altogether in step s 5.
Then, step S6 is performed, the lithium titanate battery that floating charge terminates is shelved on aging 3 days in 60 DEG C of high-temperature cabinets；Then step is performed
S7, goes clamping plate to be evacuated, and seals again, completes the chemical conversion aging of lithium titanate battery.
In reference picture 2, the present embodiment, the battery after chemical conversion aging will be completed, be placed on new prestige forming and capacity dividing cabinet and divided
Rong Hou, is placed under 45 DEG C of environment, and 100%DOD (depth of discharge, depth of discharge) is carried out with 3C/3C (24A) electric current
Charge and discharge cycles (charging/discharging voltage interval 1.5-2.7V), the aerogenesis situation of observation circulation 3000 weeks, discovery has no obvious aerogenesis,
Lithium titanate soft-package battery circulate 3000 weeks after capability retention up to 91.4%.
Embodiment 2
Technical scheme is described in detail by taking 8Ah lithium titanate soft-package batteries as an example for the present embodiment.Specifically
, the 8Ah lithium titanate soft-package batteries, just extremely auspicious Xiang ternary NCM523, negative pole is self-produced lithium titanate LTO, and barrier film is that Cangzhou is bright
Pearl 12+4 one side ceramic diaphragms, electrolyte is that Guangzhou is bestowed by heaven lithium titanate special electrolysis liquid.
In the present embodiment, pre- chemical conversion aging is specific as follows.
In step S1, the 8Ah lithium titanate batteries that fluid injection, sealing are completed are placed in 40 DEG C of high-temperature cabinets, are lain low and are shelved 8h, make
Obtain electrolyte and fully infiltrate both positive and negative polarity pole piece and barrier film, to complete high temperature infiltration.In step S2, metatitanic acid after high temperature infiltration will be completed
Lithium battery is placed in after 4h at room temperature, and upper fixture is charged on 5V, 10A formation cabinet, specifically be can select new prestige formation cabinet, is filled
Electric current I1 is 0.2C (1.6A), and charge cutoff voltage is that first voltage value V1 is 2.5V.In step S3, by the titanium of charging complete
Sour lithium soft-package battery is placed in aging 12h in 40 DEG C of high-temperature cabinets, to complete pre- chemical conversion.
In the present embodiment, low current chemical conversion aging is specific as follows.
In step S4, the lithium titanate battery after pre- chemical conversion is placed in 60 DEG C of high-temperature cabinets, permanent with 0.05C (0.4A) low currents I2
Current charge to cell voltage reaches second voltage value V2=2.7V；Then step S5 is performed, it is every with 0.01C (0.08A) electric currents I3
Every floating charge in 10 minutes once, blanking voltage is that second voltage value V2 is 2.7V.In the present embodiment, floating charge 50 altogether in step s 5
It is secondary.Then, step S6 is performed, the lithium titanate battery that floating charge terminates is shelved on aging 3 days in 40 DEG C of high-temperature cabinets；Then step is performed
Rapid S7, goes clamping plate to be evacuated, seals again, completes the chemical conversion aging of lithium titanate battery.
Embodiment 3
Technical scheme is described in detail by taking 8Ah lithium titanate soft-package batteries as an example for the present embodiment.Specifically
, the 8Ah lithium titanate soft-package batteries, just extremely auspicious Xiang ternary NCM622, negative pole is self-produced lithium titanate LTO, and barrier film is that Cangzhou is bright
Pearl 12+4 one side ceramic diaphragms, electrolyte is that Guangzhou is bestowed by heaven lithium titanate special electrolysis liquid.
In the present embodiment, pre- chemical conversion aging is specific as follows.
In step S1, the 8Ah lithium titanate batteries that fluid injection, sealing are completed are placed in 65 DEG C of high-temperature cabinets, are lain low and are shelved 24h,
So that electrolyte fully infiltrates both positive and negative polarity pole piece and barrier film, to complete high temperature infiltration.In step S2, titanium after high temperature infiltration will be completed
Acid lithium battery is placed in after 6h at room temperature, and upper fixture is charged on 5V, 10A formation cabinet, specifically can select new prestige formation cabinet,
Charging current I1 is 1C (8A), and charge cutoff voltage is that first voltage value V1 is 2.6V.In step S3, by the metatitanic acid of charging complete
Lithium soft-package battery is placed in aging 48h in 65 DEG C of high-temperature cabinets, to complete pre- chemical conversion.
In the present embodiment, low current chemical conversion aging is specific as follows.
In step S4, the lithium titanate battery after pre- chemical conversion is placed in 45 DEG C of high-temperature cabinets, with 0.02C (0.16A) low currents I2
Constant-current charge to cell voltage reaches second voltage value V2=3.0V；Then step S5 is performed, with 0.01C (0.08A) electric currents I3
Every floating charge in 5 minutes once, blanking voltage is that second voltage value V2 is 3.0V.In the present embodiment, floating charge 100 altogether in step s 5
It is secondary.Then, step S6 is performed, the lithium titanate battery that floating charge terminates is shelved on aging 5 days in 45 DEG C of high-temperature cabinets；Then step is performed
Rapid S7, goes clamping plate to be evacuated, seals again, completes the chemical conversion aging of lithium titanate battery.
Lithium titanate battery after chemical conversion terminates in embodiment 2 and embodiment 3, by multiple charge and discharge cycles, without substantially
Aerogenesis.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (9)
1. a kind of chemical synthesizing method of lithium titanate battery, it is characterised in that carried out first to lithium titanate battery after pre- chemical conversion aging again
Carry out low current chemical conversion aging；
Pre- chemical conversion aging comprises the following steps：
S1, the lithium titanate battery that fluid injection is honored as a queen in advance is placed in hot environment to infiltration very first time threshold value；
S2, by definite value electric current I1 to high temperature infiltrate after lithium titanate battery constant-current charge to cell voltage reach default first
Magnitude of voltage V1；
S3, the lithium titanate battery high temperature of charging complete shelved into the second time threshold；
Low current chemical conversion aging comprises the following steps：
S4, in hot environment with definite value electric current I2 the lithium titanate battery after pre- chemical conversion aging is charged to cell voltage reach it is pre-
If second voltage value V2, I2 ＜ I1；
S5, enter between-line spacing floating charge to lithium titanate battery with definite value electric current I3, floating charge blanking voltage is second voltage value V2, I3 ＜
I2；
S6, the lithium titanate battery terminated to floating charge carry out high temperature ageing and continue the 3rd time threshold；
S7, aging terminate, and lithium titanate battery is evacuated, then secondary sealing.
2. the chemical synthesizing method of the lithium titanate battery described in claim 1, it is characterised in that in step S1, the temperature of hot environment
For 0-65 DEG C, very first time threshold value is 8-24h.
3. the chemical synthesizing method of the lithium titanate battery described in claim 1, it is characterised in that in step S2, I1 is 0.2C-1C, the
One magnitude of voltage V1 is 2.3-2.6V.
4. the chemical synthesizing method of the lithium titanate battery described in claim 1, it is characterised in that in step S3, the temperature that high temperature is shelved
For 40-65 DEG C, the second time threshold is 12-48h.
5. the chemical synthesizing method of the lithium titanate battery described in claim 1, it is characterised in that in step S4, high ambient temperatures are
40-65℃。
6. the chemical synthesizing method of the lithium titanate battery described in claim 1 or 3 or 5, it is characterised in that in step S4, definite value electric current
I2 is 0.02-0.2C, and second voltage value V2 is 2.7-3.0V.
7. the chemical synthesizing method for the lithium titanate battery that claim 6 is stated, it is characterised in that in step S5, definite value electric current I3 is 0.01-
0.05C, total time in floating charge stage is 8-48h.
8. the chemical synthesizing method of the lithium titanate battery described in claim 1, it is characterised in that in step S6, high temperature ageing temperature is
40-65 DEG C, the 3rd time threshold is 1-7 days.
9. the chemical synthesizing method of the lithium titanate battery described in claim 1, it is characterised in that in step S2, preferred that high temperature is infiltrated
Lithium titanate battery upper fixture afterwards, then carries out constant-current charge again；In step S7, the lithium titanate battery that aging terminates is gone first
Fixture, is then evacuated and secondary sealing again.
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Cited By (6)
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| CN107546418A (en) * | 2017-07-03 | 2018-01-05 | 郑州比克电池有限公司 | A kind of lithium ion battery and the method for avoiding lithium ion battery box hat bottom from blacking |
| CN107732311A (en) * | 2017-10-10 | 2018-02-23 | 合肥国轩高科动力能源有限公司 | A kind of chemical synthesizing method of remaining silent of cylinder lithium titanate battery |
| CN108321436A (en) * | 2017-12-26 | 2018-07-24 | 合肥国轩高科动力能源有限公司 | A kind of cathode uses the lithium ion battery forming and capacity dividing method of silicon-carbon |
| CN109037815A (en) * | 2018-09-21 | 2018-12-18 | 合肥国轩高科动力能源有限公司 | A kind of chemical synthesizing method of ferric phosphate lithium cell |
| CN109065826A (en) * | 2018-07-06 | 2018-12-21 | 合肥国轩高科动力能源有限公司 | A kind of wetting method of high capacity high-pressure solid negative electrode lithium ion battery |
| CN110854458A (en) * | 2019-11-07 | 2020-02-28 | 河南电池研究院有限公司 | Formation method of high-voltage soft package lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107546418A (en) * | 2017-07-03 | 2018-01-05 | 郑州比克电池有限公司 | A kind of lithium ion battery and the method for avoiding lithium ion battery box hat bottom from blacking |
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| CN108321436A (en) * | 2017-12-26 | 2018-07-24 | 合肥国轩高科动力能源有限公司 | A kind of cathode uses the lithium ion battery forming and capacity dividing method of silicon-carbon |
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| CN109065826A (en) * | 2018-07-06 | 2018-12-21 | 合肥国轩高科动力能源有限公司 | A kind of wetting method of high capacity high-pressure solid negative electrode lithium ion battery |
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| CN110854458A (en) * | 2019-11-07 | 2020-02-28 | 河南电池研究院有限公司 | Formation method of high-voltage soft package lithium ion battery |
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| CN107230799B (en) | 2019-06-11 |
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