CN109037815A - A kind of chemical synthesizing method of ferric phosphate lithium cell - Google Patents

A kind of chemical synthesizing method of ferric phosphate lithium cell Download PDF

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Publication number
CN109037815A
CN109037815A CN201811109967.8A CN201811109967A CN109037815A CN 109037815 A CN109037815 A CN 109037815A CN 201811109967 A CN201811109967 A CN 201811109967A CN 109037815 A CN109037815 A CN 109037815A
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China
Prior art keywords
temperature
battery
maintains
lithium cell
formation device
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Pending
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CN201811109967.8A
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Chinese (zh)
Inventor
王兆栋
张宝
江家嘉
余刚
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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Priority to CN201811109967.8A priority Critical patent/CN109037815A/en
Publication of CN109037815A publication Critical patent/CN109037815A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/42Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/44Methods for charging or discharging
    • H01M10/446Initial charging measures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/058Construction or manufacture
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a kind of chemical synthesizing methods of ferric phosphate lithium cell, and the battery for completing high temperature infiltration after fluid injection circulates to formation device first, is stood first, and then battery circulates again after primary chemical conversion and carries out a high temperature ageing to high-temperature aging room;Then the battery after a high temperature ageing is circulated to formation device, is stood first, then carries out secondary chemical conversion, finally battery circulates and carries out secondary high-temperature aging to high-temperature aging room.The present invention first stands battery when entering formation device, guarantees the stability of temperature during SEI early period film is formed;The present invention carries out a high temperature ageing after the additives such as VC tentatively restore and form SEI film, then completes subsequent chemical conversion and secondary high-temperature aging, and double aging guarantees the stability and completeness that SEI film is formed.

Description

A kind of chemical synthesizing method of ferric phosphate lithium cell
Technical field
The present invention relates to technical field of lithium batteries, the chemical synthesizing method of specifically a kind of ferric phosphate lithium cell.
Background technique
With the extensive use of lithium ion battery, properties are excellent and the lithium ion battery that has extended cycle life increasingly by To the welcome of people.In the production process of lithium ion battery, need to carry out first preactivate and stabilization to the battery of complete fluid injection Change, that is, last chemical conversion-aging process, properties and cycle life to lithium ion battery have vital shadow It rings.
Chemical conversion is exactly that the charging of a low current is carried out to the lithium ion battery manufactured, is carried out to electrode active material Activation, and the passivation thin layer for being covered on carbon electrodes, i.e. solid electrolytic are formed on the phase interface of Carbon anode and electrolyte Matter phase interface or SEI film.Aging is exactly that the battery after first time charging chemical conversion is placed on room temperature or high temperature and drying In the environment of carry out aging, mainly there are three aspects for the purpose of aging: 1, the structural rearrangement that SEI film is close and hole is small is transformed into Loose porous structure;2, the more acurrate stabilization of the voltage of battery after aging;3, electrolyte can further infiltrate pole piece, Be conducive to the stabilization of battery performance.
Correlative study is thought that SEI is reacted with Li+ by the additives such as VC, EC and PC equal solvent, trace water and HF etc. and is formed A series of organic lithium salts and inorganic lithium salt are covered on cathode graphite surface, and correlative study shows during formation charging, first The film for additive such as VC form prior to PC, EC equal solvent in 2.4V~2.8V (full battery) generation reduction reaction certain thickness SEI film is to prevent PC and Li+It is embedded in graphite altogether, vital influence is generated on electrical properties such as battery capacity, service life;Voltage into One step increases, and EC equal solvent occurs reduction reaction and forms complete SEI film, then carries out aging and obtains stable SEI film.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of chemical synthesizing methods of ferric phosphate lithium cell, so that LiFePO4 is electric Pond by chemical conversion after formed stablize effective SEI film.
The technical solution of the present invention is as follows:
A kind of chemical synthesizing method of ferric phosphate lithium cell, has specifically included following steps:
(1), the battery for completing high temperature infiltration after fluid injection is circulated to formation device, is stood, is then used first The multiplying power electric current of 0.01-0.02C charges, and charging is set as 2.8V by voltage;
(2), battery is circulated and carries out a high temperature ageing to high-temperature aging room;
(3), the battery after a high temperature ageing is circulated to formation device, is stood first, then use 0.01- The multiplying power electric current of 0.02C charges, and charging by voltage is set as 3.2V, finally using the multiplying power electric current of 0.05-0.2C into Row charging, charging are set as 3.3V by voltage;
(4), battery is circulated and carries out secondary high-temperature aging to high-temperature aging room;
(5), battery is subjected to vacuumizing and exhausting, fluid infusion and sealing and completes battery production, finally carry out downstream capacity screening And electrical property sampling observation test.
In the step (1), the battery standing time is 1-2h, and the environment temperature of formation device maintains 25-30 DEG C, environment Dew-point temperature maintains < -20 DEG C.
In the step (2), the environment temperature of high-temperature aging room maintains 40-45 DEG C, and ambient dew point temperature maintains <- 40 DEG C, a high temperature ageing time is 4-8h.
In the step (3), the battery standing time is 1-2h, and the environment temperature of formation device maintains 25-30 DEG C, environment Dew-point temperature maintains < -20 DEG C.
In the step (4), the environment temperature of high-temperature aging room maintains 40-45 DEG C, and ambient dew point temperature maintains <- 40 DEG C, secondary high-temperature ageing time is 6-12h.
In the step (5), the time of vacuumizing and exhausting is 300s, vacuum degree < -95KPa.
Advantages of the present invention:
(1), the battery core temperature that the present invention completes the infiltration of electrolyte high temperature is higher than environment temperature, first when entering formation device By battery standing to environment temperature, guarantee the stability of temperature during SEI early period film is formed;
(2), by grasping and analysing in depth the formation mechenism of SEI film, the present invention tentatively restores to be formed in additives such as VC A high temperature ageing is carried out after SEI film, then completes subsequent chemical conversion and secondary high-temperature aging, and double aging guarantees that SEI film is formed Stability and completeness;
(3), the battery of high temperature ageing of present invention completion is when entering formation device first by battery standing to environment temperature Degree guarantees the stability of temperature during SEI early period film is formed;
The SEI film that the present invention forms lithium battery is more stable and complete, and battery cycle life and storage can be improved Energy.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
Embodiment 1
A kind of chemical synthesizing method of ferric phosphate lithium cell, has specifically included following steps:
(1), then the battery circulation that high temperature infiltration is completed after fluid injection is used to formation device, first standing 1-2h The multiplying power electric current of 0.01-0.02C charges, and charging is set as 2.8V by voltage;Wherein, the environment temperature dimension of formation device It holds at 25-30 DEG C, ambient dew point temperature maintains < -20 DEG C
(2), battery is circulated and carries out a high temperature ageing 4-8h to high-temperature aging room;Wherein, the environment of high-temperature aging room Temperature maintains 40-45 DEG C, and ambient dew point temperature maintains < -40 DEG C;
(3), by the battery circulation after a high temperature ageing to formation device, first standing 1-2h, 0.01- is then used The multiplying power electric current of 0.02C charges, and charging by voltage is set as 3.2V, finally using the multiplying power electric current of 0.05-0.2C into Row charging, charging are set as 3.3V by voltage;Wherein, the environment temperature of formation device maintains 25-30 DEG C, ambient dew point temperature Degree maintains < -20 DEG C;
(4), battery is circulated and carries out secondary high-temperature aging 6-12h to high-temperature aging room;Wherein, the environment of high-temperature aging room Temperature maintains 40-45 DEG C, and ambient dew point temperature maintains < -40 DEG C;
(5), battery is carried out to vacuumizing and exhausting 300s, fluid infusion and sealing in the environment of vacuum degree < -95KPa and completes electricity Pond production finally carries out downstream capacity screening and electrical property sampling observation test.
Embodiment 2
A kind of chemical synthesizing method of ferric phosphate lithium cell, has specifically included following steps:
(1), the battery that high temperature infiltration is completed after fluid injection is circulated to formation device, using the multiplying power electric current of 0.01-0.02C It charges, charging is set as 2.8V by voltage;Wherein, the environment temperature of formation device maintains 25-30 DEG C, ambient dew point Temperature maintains < -20 DEG C
(2), battery is circulated and carries out a high temperature ageing 4-8h to high-temperature aging room;Wherein, the environment of high-temperature aging room Temperature maintains 40-45 DEG C, and ambient dew point temperature maintains < -40 DEG C;
(3), it by the battery circulation after a high temperature ageing to formation device, is carried out using the multiplying power electric current of 0.01-0.02C Charging, charging are set as 3.2V by voltage, are finally charged using the multiplying power electric current of 0.05-0.2C, charge by voltage It is set as 3.3V;Wherein, the environment temperature of formation device maintains 25-30 DEG C, and ambient dew point temperature maintains < -20 DEG C;
(4), battery is circulated and carries out secondary high-temperature aging 6-12h to high-temperature aging room;Wherein, the environment of high-temperature aging room Temperature maintains 40-45 DEG C, and ambient dew point temperature maintains < -40 DEG C;
(5), battery is carried out to vacuumizing and exhausting 300s, fluid infusion and sealing in the environment of vacuum degree < -95KPa and completes electricity Pond production finally carries out downstream capacity screening and electrical property sampling observation test.
Embodiment 3
(1), then the battery circulation that high temperature infiltration is completed after fluid injection is used to formation device, first standing 1-2h The multiplying power electric current of 0.01-0.02C charges, and charging is set as 3.2V by voltage, finally using the multiplying power electricity of 0.05-0.2C Stream charges, and charging is set as 3.3V by voltage;Wherein, the environment temperature of formation device maintains 25-30 DEG C, environment dew Point temperature maintains < -20 DEG C;
(2), battery is circulated and carries out high temperature ageing 6-12h to high-temperature aging room;Wherein, the environment temperature of high-temperature aging room 40-45 DEG C is maintained, ambient dew point temperature maintains < -40 DEG C;
(3), battery is carried out to vacuumizing and exhausting 300s, fluid infusion and sealing in the environment of vacuum degree < -95KPa and completes electricity Pond production finally carries out downstream capacity screening and electrical property sampling observation test.
Embodiment 4
(1), the battery that high temperature infiltration is completed after fluid injection is circulated to formation device, using the multiplying power electric current of 0.01-0.02C Charge, charging by voltage is set as 3.2V, finally charged using the multiplying power electric current of 0.05-0.2C, charging by Voltage is set as 3.3V;Wherein, the environment temperature of formation device maintains 25-30 DEG C, and ambient dew point temperature maintains < -20 ℃;
(2), battery is circulated and carries out high temperature ageing 6-12h to high-temperature aging room;Wherein, the environment temperature of high-temperature aging room 40-45 DEG C is maintained, ambient dew point temperature maintains < -40 DEG C;
(3), battery is carried out to vacuumizing and exhausting 300s, fluid infusion and sealing in the environment of vacuum degree < -95KPa and completes electricity Pond production finally carries out downstream capacity screening and electrical property sampling observation test.
The battery of embodiment 1-4 is subjected to 1C normal temperature circulation electric performance test and 55 DEG C of full electric high temperature storage tests, test As a result statistics is as follows:
From the experimental result of upper table it is found that being to stand cooling and twice-aged technique before taking chemical conversion using embodiment 1 Battery cycle life and storage performance are obviously improved.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (6)

1. a kind of chemical synthesizing method of ferric phosphate lithium cell, it is characterised in that: specifically included following steps:
(1), the battery for completing high temperature infiltration after fluid injection is circulated to formation device, is stood first, then use 0.01- The multiplying power electric current of 0.02C charges, and charging is set as 2.8V by voltage;
(2), battery is circulated and carries out a high temperature ageing to high-temperature aging room;
(3), the battery after a high temperature ageing is circulated to formation device, is stood first, then use 0.01-0.02C Multiplying power electric current charge, charging by voltage is set as 3.2V, is finally filled using the multiplying power electric current of 0.05-0.2C Electricity, charging are set as 3.3V by voltage;
(4), battery is circulated and carries out secondary high-temperature aging to high-temperature aging room;
(5), battery is subjected to vacuumizing and exhausting, fluid infusion and sealing and completes battery production, finally carry out downstream capacity screening and electricity Performance sampling observation test.
2. a kind of chemical synthesizing method of ferric phosphate lithium cell according to claim 1, it is characterised in that: in the step (1), The battery standing time is 1-2h, and the environment temperature of formation device maintains 25-30 DEG C, and ambient dew point temperature maintains < -20 DEG C.
3. a kind of chemical synthesizing method of ferric phosphate lithium cell according to claim 1, it is characterised in that: in the step (2), The environment temperature of high-temperature aging room maintains 40-45 DEG C, and ambient dew point temperature maintains < -40 DEG C, a high temperature ageing time For 4-8h.
4. a kind of chemical synthesizing method of ferric phosphate lithium cell according to claim 1, it is characterised in that: in the step (3), The battery standing time is 1-2h, and the environment temperature of formation device maintains 25-30 DEG C, and ambient dew point temperature maintains < -20 DEG C.
5. a kind of chemical synthesizing method of ferric phosphate lithium cell according to claim 1, it is characterised in that: in the step (4), The environment temperature of high-temperature aging room maintains 40-45 DEG C, and ambient dew point temperature maintains < -40 DEG C, secondary high-temperature ageing time For 6-12h.
6. a kind of chemical synthesizing method of ferric phosphate lithium cell according to claim 1, it is characterised in that: in the step (5), The time of vacuumizing and exhausting is 300s, vacuum degree < -95KPa.
CN201811109967.8A 2018-09-21 2018-09-21 A kind of chemical synthesizing method of ferric phosphate lithium cell Pending CN109037815A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN109888401A (en) * 2019-04-16 2019-06-14 上海卡耐新能源有限公司 A kind of chemical synthesizing method solving soft lithium ion packet power battery exception
CN110380034A (en) * 2019-07-23 2019-10-25 合肥国轩高科动力能源有限公司 A kind of positive electrode of lithium ion battery and full battery and preparation method containing it
CN111106405A (en) * 2019-12-17 2020-05-05 上海电气国轩新能源科技有限公司 Formation method of square aluminum shell lithium iron phosphate battery for energy storage
CN111987376A (en) * 2020-07-23 2020-11-24 法珞斯(苏州)能源科技有限公司 Lithium iron battery and formation aging and capacity grading process thereof
CN112255558A (en) * 2019-12-31 2021-01-22 蜂巢能源科技有限公司 Method and device for calculating battery calendar life attenuation
CN112751098A (en) * 2021-01-25 2021-05-04 唐山航天万源科技有限公司 Formation method of lithium iron phosphate battery

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CN107230799A (en) * 2017-07-10 2017-10-03 合肥国轩高科动力能源有限公司 A kind of chemical synthesizing method of lithium titanate battery
CN108110348A (en) * 2017-11-14 2018-06-01 合肥国轩高科动力能源有限公司 A kind of compound method for lithium ion battery
CN108155424A (en) * 2017-12-12 2018-06-12 江苏双登富朗特新能源有限公司 A kind of control method of novel improvement lithium ion Soft Roll laminated batteries diaphragm fold

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CN103259048A (en) * 2013-05-22 2013-08-21 南京双登科技发展研究院有限公司 Formation method for prolonging cycle life of lithium titanate battery
CN104882633A (en) * 2015-04-29 2015-09-02 山西恒昌元科技有限公司 Formation process capable of reducing self discharge of lithium ion battery
CN107230799A (en) * 2017-07-10 2017-10-03 合肥国轩高科动力能源有限公司 A kind of chemical synthesizing method of lithium titanate battery
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CN108155424A (en) * 2017-12-12 2018-06-12 江苏双登富朗特新能源有限公司 A kind of control method of novel improvement lithium ion Soft Roll laminated batteries diaphragm fold

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109888401A (en) * 2019-04-16 2019-06-14 上海卡耐新能源有限公司 A kind of chemical synthesizing method solving soft lithium ion packet power battery exception
CN109888401B (en) * 2019-04-16 2022-06-28 上海卡耐新能源有限公司 Formation method for solving abnormity of soft package lithium ion power battery
CN110380034A (en) * 2019-07-23 2019-10-25 合肥国轩高科动力能源有限公司 A kind of positive electrode of lithium ion battery and full battery and preparation method containing it
CN111106405A (en) * 2019-12-17 2020-05-05 上海电气国轩新能源科技有限公司 Formation method of square aluminum shell lithium iron phosphate battery for energy storage
CN111106405B (en) * 2019-12-17 2021-06-22 上海电气国轩新能源科技有限公司 Formation method of square aluminum shell lithium iron phosphate battery for energy storage
CN112255558A (en) * 2019-12-31 2021-01-22 蜂巢能源科技有限公司 Method and device for calculating battery calendar life attenuation
CN112255558B (en) * 2019-12-31 2023-05-12 蜂巢能源科技有限公司 Method and device for calculating battery calendar life attenuation
CN111987376A (en) * 2020-07-23 2020-11-24 法珞斯(苏州)能源科技有限公司 Lithium iron battery and formation aging and capacity grading process thereof
CN112751098A (en) * 2021-01-25 2021-05-04 唐山航天万源科技有限公司 Formation method of lithium iron phosphate battery

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