CN107230799B - 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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- CN107230799B CN107230799B CN201710555546.7A CN201710555546A CN107230799B CN 107230799 B CN107230799 B CN 107230799B CN 201710555546 A CN201710555546 A CN 201710555546A CN 107230799 B CN107230799 B CN 107230799B
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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
The invention discloses a kind of chemical synthesizing method of lithium titanate battery, main includes that pre- chemical conversion aging and low current high temperature are melted into two step of aging.The first step is melted into aging in advance, and the lithium titanate battery that fluid injection is honored as a queen in advance first, which is placed in high-temperature cabinet, to be shelved, and sufficiently after infiltration, upper fixture is melted into advance, with certain electric current constant-current charge, carries out high temperature after pre- chemical conversion and shelves.Second step, low current high temperature are melted into aging.Lithium titanate battery after pre- chemical conversion is placed in high-temperature cabinet and is heated, low current charge to high potential carries out interval floating charge with more low current, then carries out high temperature ageing, clamping plate is gone to be evacuated secondary sealing.The process employs two step den processes, so that the moisture of lithium titanate battery is sufficiently reacted, and realize cathode film formation simultaneously, have obstructed lithium titanate surface Ti3+ to the catalytic decomposition of electrolyte solvent.The gas production during lithium titanate battery high temperature circulation is greatly reduced, to improve room temperature and high temperature cyclic performance.
Description
Technical field
The present invention relates to battery technology field more particularly to a kind of chemical synthesizing methods of lithium titanate battery.
Background technique
Lithium titanate battery because its safety is good, multiplying power power-performance is good, long the advantages that in normal temperature circulation service life due to cause
The extensive attention of art circle and industry especially has batch application in the case in the fields such as electric vehicle, energy storage in recent years.However
During lithium titanate battery practical study and application, there are flatulence problems for discovery lithium titanate battery, especially at high temperature
Flatulence is more serious, has severely impacted the cycle performance of battery.
Explained currently, having the specific mechanism of comparison to the reason of lithium titanate battery flatulence, the residual moisture in battery with
And the Ti3+ on lithium titanate surface is the main reason for it produces gas to the catalytic decomposition (especially at high temperature) of electrolyte solvent.Titanium
The researchers of sour lithium material and battery are mainly changed by two aspects of lithium titanate material modification and electrolyte film for additive
The high temperature flatulence problem of kind lithium titanate battery.However the high temperature flatulence that the above method can not be fully solved lithium titanate battery is asked
Topic, it is necessary to be solved in conjunction with the preparation of lithium titanate battery, chemical synthesis technology.
In the chemical synthesis technology research of lithium titanate battery, existing research person has studied the chemical conversion work of low current and high temperature ageing
Skill (such as: Liu Jinliang, peak, Zhang Rubin, etc., the chemical synthesizing method of lithium titanate battery, Chinese patent, application number:
201410765009.1) it, has obtained preferable inhibition and has produced gas effect, but still failed to completely eliminate lithium titanate battery high temperature production gas pair
The influence of the electrical properties such as circulation.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of chemical synthesizing methods of lithium titanate battery.
A kind of chemical synthesizing method of lithium titanate battery proposed by the present invention carries out lithium titanate battery first after being melted into aging in advance
Low current chemical conversion aging is carried out again；
Pre- chemical conversion aging the following steps are included:
S1, the lithium titanate battery placement that fluid injection is honored as a queen in advance is infiltrated into first time threshold in the high temperature environment；
S2, preset is reached to lithium titanate battery constant-current charge to the cell voltage after high temperature infiltration by definite value electric current I1
The first voltage value V1；
S3, the lithium titanate battery high temperature of charging complete is shelved into second time threshold；
Low current be melted into aging the following steps are included:
S4, it cell voltage is charged to the lithium titanate battery after pre- chemical conversion aging with definite value electric current I2 in the high temperature environment reaches
To preset second voltage value V2, I2 < I1；
S5, interval floating charge is carried out to lithium titanate battery with definite value electric current I3, floating charge blanking voltage is second voltage value V2, I3
< I2；
S6, high temperature ageing is carried out to the lithium titanate battery that floating charge terminates and continues third time threshold；
S7, aging terminate, and are evacuated to lithium titanate battery, then secondary sealing.
Preferably, in step S1, the temperature of hot environment is 0-65 DEG C, first time threshold 8-24h.
Preferably, in step S2, I1 0.2C-1C, the first voltage value V1 are 2.3-2.6V.
Preferably, in step S3, the temperature that high temperature is shelved is 40-65 DEG C, second time threshold 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 third time threshold is 1-7 days.
Preferably, in step S2, then first choice carries out constant current again and fills to the lithium titanate battery upper fixture after high temperature infiltration
Electricity；In step S7, then the lithium titanate battery de-chucking terminated first to aging carries out pumping and secondary sealing again.
Lithium titanate battery chemical conversion is carried out in two steps by the chemical synthesizing method of lithium titanate battery provided by the invention, and the first step is pre-
The main purpose for being melted into aging is battery core water removal, preliminary production gas and completes the irreversible electrochemical reaction under the conditions of low potential；The
The main purpose of two step low current high temperature chemical conversion is to complete cathode lithium titanate material surface filming, and the purpose of aging is to stablize cathode
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 stablized.
Detailed description of the invention
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.
Specific embodiment
A kind of chemical synthesizing method of lithium titanate battery provided by the invention carries out lithium titanate battery first after being melted into aging in advance
Low current chemical conversion aging is carried out again.
Pre- chemical conversion aging includes the following steps S1-S3.
S1, the lithium titanate battery placement that fluid injection is honored as a queen in advance is infiltrated into first time threshold in the high temperature environment.In this step,
The temperature of hot environment is 0-65 DEG C, first time threshold 8-24h.
S2, preset is reached to lithium titanate battery constant-current charge to the cell voltage after high temperature infiltration by definite value electric current I1
The first voltage value V1.I1 is 0.2C-1C, and the first voltage value V1 is 2.3-2.6V.
S3, the lithium titanate battery high temperature of charging complete is shelved into second time threshold.In this step, temperature that high temperature is shelved
It is 40-65 DEG C, second time threshold 12-48h.
Low current chemical conversion aging includes the following steps S4-S7.
S4, it cell voltage is charged to the lithium titanate battery after pre- chemical conversion aging with definite value electric current I2 in the high temperature environment reaches
To preset 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, interval floating charge is carried out 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, high temperature ageing is carried out to the lithium titanate battery that floating charge terminates and continues third time threshold.In this step, high temperature
Aging temperature is 40-65 DEG C, and third time threshold is 1-7 days.
S7, aging terminate, and are evacuated to lithium titanate battery, then secondary sealing.
In present embodiment, in order to guarantee stabilization of the lithium titanate battery in formation process, in 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, aging is terminated first lithium titanate electricity
Then pond de-chucking carries out pumping and secondary sealing again.
Embodiment 1
Referring to Fig.1, the present embodiment carries out specifically technical solution of the present invention by taking 8Ah lithium titanate soft-package battery as an example
It is bright.Specifically, the 8Ah lithium titanate soft-package battery, just extremely auspicious Xiang ternary NCM111, cathode are self-produced lithium titanate LTO, diaphragm is
Cangzhou jewel 12+4 single side ceramic diaphragm, electrolyte are 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 battery that fluid injection, sealing are completed is placed in 55 DEG C of high-temperature cabinets, lies low and shelves 12h,
So that electrolyte sufficiently infiltrates positive and negative anodes pole piece and diaphragm, to complete high temperature infiltration.In step S2, titanium after high temperature infiltration will be completed
After acid lithium battery is placed in 4h at room temperature, upper fixture charges on the formation cabinet of 5V, 10A, and new prestige formation cabinet specifically can be selected,
Charging current I1 is 0.5C (i.e. 4A), and charge cutoff voltage, that is, the first voltage value V1 is 2.6V.In step S3, by charging complete
Lithium titanate soft-package battery is placed in aging in 55 DEG C of high-temperature cabinets and for 24 hours, is melted into so that completion is pre-.
In the present embodiment, it is specific as follows that low current is melted into aging.
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 current I2
Current charge to cell voltage reaches second voltage value V2=2.8V；Then execute step S5, with 0.05C (0.4A) electric current I3 every
Floating charge in 10 minutes is primary, and blanking voltage is second voltage value V2, that is, 2.8V.In the present embodiment, floating charge 80 times altogether in step s 5.
Then, step S6 is executed, the lithium titanate battery that floating charge is terminated is shelved in 60 DEG C of high-temperature cabinets aging 3 days；Then step is executed
S7 goes clamping plate to be evacuated, and seals again, completes the chemical conversion aging of lithium titanate battery.
Referring to Fig. 2, in the present embodiment, it will complete to be melted into the battery after aging, be placed on new prestige forming and capacity dividing cabinet and divided
Rong Hou is placed under 45 DEG C of environment, carries out 100%DOD (depth of discharge, depth of discharge) with 3C/3C (24A) electric current
Charge and discharge cycles (charging/discharging voltage section 1.5-2.7V), observation recycle 3000 weeks production gas situations, and discovery has no obvious production gas,
Lithium titanate soft-package battery recycle 3000 weeks after capacity retention ratio up to 91.4%.
Embodiment 2
The present embodiment is described in detail technical solution of the present invention by taking 8Ah lithium titanate soft-package battery as an example.Specifically
, the 8Ah lithium titanate soft-package battery, just extremely auspicious Xiang ternary NCM523, cathode is self-produced lithium titanate LTO, and diaphragm is that Cangzhou is bright
Pearl 12+4 single side ceramic diaphragm, electrolyte are 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 battery that fluid injection, sealing are completed is placed in 40 DEG C of high-temperature cabinets, lies low and shelves 8h, make
It obtains electrolyte and sufficiently infiltrates positive and negative anodes pole piece and diaphragm, to complete high temperature infiltration.In step S2, metatitanic acid after high temperature infiltration will be completed
After lithium battery is placed in 4h at room temperature, upper fixture charges on the formation cabinet of 5V, 10A, and new prestige formation cabinet specifically can be selected, fill
Electric current I1 is 0.2C (1.6A), and charge cutoff voltage, that is, the 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, it is specific as follows that low current is melted into aging.
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 current I2
Current charge to cell voltage reaches second voltage value V2=2.7V；Then step S5 is executed, it is every with 0.01C (0.08A) electric current I3
Primary every floating charge in 10 minutes, blanking voltage is second voltage value V2, that is, 2.7V.In the present embodiment, floating charge 50 altogether in step s 5
It is secondary.Then, step S6 is executed, the lithium titanate battery that floating charge is terminated is shelved in 40 DEG C of high-temperature cabinets aging 3 days；Then step is executed
Rapid S7, goes clamping plate to be evacuated, and seals again, completes the chemical conversion aging of lithium titanate battery.
Embodiment 3
The present embodiment is described in detail technical solution of the present invention by taking 8Ah lithium titanate soft-package battery as an example.Specifically
, the 8Ah lithium titanate soft-package battery, just extremely auspicious Xiang ternary NCM622, cathode is self-produced lithium titanate LTO, and diaphragm is that Cangzhou is bright
Pearl 12+4 single side ceramic diaphragm, electrolyte are 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 battery that fluid injection, sealing are completed is placed in 65 DEG C of high-temperature cabinets, lies low and shelves for 24 hours,
So that electrolyte sufficiently infiltrates positive and negative anodes pole piece and diaphragm, to complete high temperature infiltration.In step S2, titanium after high temperature infiltration will be completed
After acid lithium battery is placed in 6h at room temperature, upper fixture charges on the formation cabinet of 5V, 10A, and new prestige formation cabinet specifically can be selected,
Charging current I1 is 1C (8A), and charge cutoff voltage, that is, the 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, it is specific as follows that low current is melted into aging.
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 current I2
Constant-current charge to cell voltage reaches second voltage value V2=3.0V；Then step S5 is executed, with 0.01C (0.08A) electric current I3
Primary every floating charge in 5 minutes, blanking voltage is second voltage value V2, that is, 3.0V.In the present embodiment, floating charge 100 altogether in step s 5
It is secondary.Then, step S6 is executed, the lithium titanate battery that floating charge is terminated is shelved in 45 DEG C of high-temperature cabinets aging 5 days；Then step is executed
Rapid S7, goes clamping plate to be evacuated, and seals again, completes the chemical conversion aging of lithium titanate battery.
Lithium titanate battery after being melted into embodiment 2 and embodiment 3, by multiple charge and discharge cycles, without obvious
Produce gas.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (2)
1. a kind of chemical synthesizing method of lithium titanate battery, which is characterized in that carry out being melted into after aging again in advance first to lithium titanate battery
It carries out low current and is melted into aging；
Pre- chemical conversion aging the following steps are included:
S1, the lithium titanate battery placement that fluid injection is honored as a queen in advance is infiltrated into first time threshold in the high temperature environment；
S2, preset first is reached to lithium titanate battery constant-current charge to the cell voltage after high temperature infiltration by definite value electric current I1
Voltage value V1；
S3, the lithium titanate battery high temperature of charging complete is shelved into second time threshold；
Low current be melted into aging the following steps are included:
S4, cell voltage is charged to the lithium titanate battery after pre- chemical conversion aging with definite value electric current I2 in the high temperature environment reach pre-
If second voltage value V2, I2 < I1；
S5, interval floating charge is carried out to lithium titanate battery with definite value electric current I3, floating charge blanking voltage is second voltage value V2, I3 <
I2；
S6, high temperature ageing is carried out to the lithium titanate battery that floating charge terminates and continues third time threshold；
S7, aging terminate, and are evacuated to lithium titanate battery, then secondary sealing；
In step S1, the temperature of hot environment is 0-65 DEG C, at the first time
Threshold value is 8-24h；
In step S2, I1 0.2C-1C, the first voltage value V1 are 2.3-2.6V；
In step S3, the temperature that high temperature is shelved is 40-65 DEG C, second time threshold 12-48h；
In step S4, high ambient temperatures are 40-65 DEG C；
In step S4, definite value electric current I2 is 0.02-0.2C, and second voltage value V2 is 2.7-3.0V；
In step S5, definite value electric current I3 is 0.01-0.05C, and total time in floating charge stage is 8-48h；
In step S6, high temperature ageing temperature is 40-65 DEG C, and third time threshold is 1-7 days.
2. the chemical synthesizing method of lithium titanate battery described in claim 1, which is characterized in that preferred to be infiltrated to high temperature in step S2
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
Then fixture carries out pumping and secondary sealing again.
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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 |
| CN107732311B (en) * | 2017-10-10 | 2019-07-12 | 合肥国轩高科动力能源有限公司 | A kind of silent chemical synthesizing method of cylinder lithium titanate battery |
| CN108321436B (en) * | 2017-12-26 | 2021-02-26 | 合肥国轩高科动力能源有限公司 | Lithium ion battery formation and capacity-sharing method adopting silicon carbon as negative electrode |
| 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 |
| 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 |
| CN110854458B (en) * | 2019-11-07 | 2021-10-22 | 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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| JPH10312826A (en) * | 1997-03-10 | 1998-11-24 | Sanyo Electric Co Ltd | Nonaqueous electrolyte battery and charging method therefor |
| WO2006050117A2 (en) * | 2004-10-29 | 2006-05-11 | Medtronic, Inc. | Method of charging lithium-ion battery |
| CN105845986A (en) * | 2016-05-10 | 2016-08-10 | 厦门日臻动力电源科技有限公司 | Formation method for improving cycle performance of lithium titanate battery |
| CN106252760B (en) * | 2016-08-05 | 2018-12-18 | 四川剑兴锂电池有限公司 | A kind of chemical conversion floating charge method of lithium titanate anode lithium battery |
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