CN101635376A - Performing method of flexible-packaging lithium-iron-phosphate aqueous positive-pole lithium battery - Google Patents
Performing method of flexible-packaging lithium-iron-phosphate aqueous positive-pole lithium battery Download PDFInfo
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- CN101635376A CN101635376A CN200910203350A CN200910203350A CN101635376A CN 101635376 A CN101635376 A CN 101635376A CN 200910203350 A CN200910203350 A CN 200910203350A CN 200910203350 A CN200910203350 A CN 200910203350A CN 101635376 A CN101635376 A CN 101635376A
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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
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- 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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a performing method of a flexible-packaging lithium-iron-phosphate aqueous positive-pole lithium battery, belonging to the technical field of lithium battery production. The performing method comprises the following charge-discharge stages: a low-content and constant-current charge stage with a current range from 0.005C to 0.5C; a high-voltage and constant-voltage charge stage with a voltage range from 3.9V to 4.5V and the content voltage from 0.005C to 0.5C; a low-current and constant-current discharge stage with the current range from 0.1C to 1C; and the low-current and constant-current self-charge stage with the current range from 0.1C to1C. Aiming at the characteristics that the aqueous binder is adopted at the lithium-iron-phosphate aqueous positive pole, the invention enables lithium iron phosphate and an aqueous binder to match with each other and is suitable for lithium-iron-phosphate aqueous positive poles and carbon negative poles as well as flexible-packaging lithium-iron-phosphate aqueous positive-pole lithium batteries comprising electrolytes containing organic solvents and lithium salts; appropriate overcharge is adopted in the forming process so as to fully generate side reaction, and side reaction products can be pumped in the secondary vacuum seal; and the lithium-iron-phosphate battery with low cost, high security and long service life can be manufactured.
Description
Technical field
The pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery of the present invention belongs to the lithium battery production technical field, particularly relates to a kind of pre-chemical synthesizing method of flexible package ferric phosphate lithium cell.
Background technology
Current lithium battery mainly adopts cobalt acid lithium (LiCoO
2) be positive electrode.Novel LiFePO 4 of anode material (LiFePO
4) and its contrast, have advantages such as fail safe is good, cost is low, have extended cycle life.In the lithium battery production process, positive electrode needs to be bonded on the collector by the binding agent that is dissolved in the solvent, and solvent then flashes to gas and discharges in the bonding process.At present the oiliness binding agent that generally uses in the industry need be arranged in pairs or groups and use oil-based solvent---N-methyl pyrrolidone (NMP), and this solvent cost height, need high temperature evaporation, and waste gas has peculiar smell and toxicity necessarily.Aqueous binders is a solvent with water, and cost declines to a great extent, and evaporation also only needs low temperature, and waste gas is steam, and safety non-toxic is the important breakthrough on the lithium battery industry technology.
Changing in advance is the important step of its performance performance quality of decision in the flexible package lithium cell production process.The effect that changes in advance mainly contains two aspects: 1. the lithium ion of positive electrode embeds negative material and forms solid electrolyte interface (SEI film) on its surface, makes negative material keep stable performance at inside battery; 2. trace water and other objectionable impurities that will remain in inside battery are reacted into gas, after the secondary of bleeding seals, get rid of outside cell body.Battery is after changing in advance and the secondary of bleeding seals, and internal structure is basicly stable, and the key property of battery is also just definite substantially.Dissimilar lithium batteries adopts different both positive and negative polarities to form and design, inevitable corresponding different pre-chemical synthesizing method.The mode that changes in advance of the anodal lithium battery of existing flexible package LiFePO4 oiliness is to fill half-fullly to battery with the little electric current of 0.05 constant～0.5C, and voltage is at 3.4～3.6V, treats that the SEI film generates and produced behind the gas horse back secondary of bleeding and seals.If with this kind in advance the mode of changing into be applied on the flexible package LiFePO4 aqueous positive-pole lithium battery, the battery of then producing as long as slightly overcharge or general high temperature under deposit all can inflatable, cycle life is also poor than the anodal lithium battery of flexible package LiFePO4 oiliness.At the characteristics of LiFePO4 aqueous positive-pole use aqueous binders, use this anodal flexible package lithium cell must adopt the suitable mode that changes in advance, could really bring into play the advantage that its fail safe is good, cost is low, have extended cycle life.
Summary of the invention
The object of the present invention is to provide a kind of pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery, make the type battery can give full play to the advantage that fail safe is good, cost is low, have extended cycle life.
The pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery of the present invention is to adopt to have the multistage charge and discharge system in high voltage constant voltage charge stage to carry out.
To the battery constant voltage charge, high voltage constant voltage charge voltage range is 3.9V～4.5V with the voltage that is higher than the battery normal operating range in the present invention, and constant voltage charge to electric current drops to 0.005C～0.5C to be ended.
Multistage charge and discharge system of the present invention comprises little electric current constant current charge stage, high voltage constant voltage charge stage, little electric current constant-current discharge stage, little half charging stage of electric current constant current.
The little electric current constant current charge stage, current range was 0.005C～0.5C to constant-current charging of battery, and constant current charge to the voltage setting value of next stage ends.
The high voltage constant voltage charge stage, voltage range was 3.9V～4.5V to the battery constant voltage charge, and constant voltage charge to electric current drops to 0.005C～0.5C to be ended.
The little electric current constant-current discharge stage is carried out the discharge fully of little electric current to battery, and current range is 0.1C～1C, and constant-current discharge to the normal lower voltage limit that uses ends.
Little half charging stage of electric current constant current is carried out half charging of little electric current to battery, and current range is 0.1C～1C, ends behind constant current charge time 0.3～8h.
The pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery of the present invention, form by the following stage of discharging and recharging:
1, the little electric current constant current charge stage, current range: 0.005C～0.5C, constant current charge to the magnitude of voltage of the setting of next stage ends;
2, the high voltage constant voltage charge stage, voltage range: 3.9V～4.5V, constant voltage charge to electric current drop to 0.005C～0.5C to be ended;
3, the little electric current constant-current discharge stage, current range: 0.1C～1C, constant-current discharge to the normal lower voltage limit that uses ends;
4, little half charging stage of electric current constant current, current range: 0.1C～1C ends behind constant current charge time 0.3～8h.
The little electric current constant current charge stage: current range: 0.005C～0.5C.This stage is the formation and development stage of SEI film on the water-based ferric phosphate lithium ion battery negative.Suitable charging current can guarantee the rise time of SEI film and the uniformity of rete simultaneously.
High voltage constant voltage charge stage: voltage range 3.9V～4.5V is the critical stage in changing in advance.Test as can be known according to cyclic voltammetry scan the water-based iron phosphate lithium positive pole, when the water-based iron phosphate lithium positive pole is in when being higher than the battery working voltage, irreversible chemical reaction and process gas can take place in microcomponent in the aqueous binders and electrolyte, after the microcomponent reaction exhausted, gas yield just no longer increased.If microcomponent fails to remove, in the residual cell body, then when battery slightly overcharges or is heated will inflatable, the inside battery structure changes, performance descends rapidly.In the high voltage constant voltage charge stage, battery remains on the voltage continuation charging down that charges normal the upper limit a little more than LiFePO4, above-mentioned microcomponent and electrolyte are fully reacted, the while process gas, and in the two envelope operations of bleeding thereafter, be removed, thereby avoided owing to slightly overcharging or slightly being heated inflatable taking place in the battery use afterwards.
The little electric current constant-current discharge stage: current range: 0.1C～1C.When battery is full power state, lithium ion is transferring on the carbon negative pole material by lithium iron phosphate positive material nearly all, it is unsteady state that the both is in, if battery wears out under this state and then can destroy the SEI rete that has generated, therefore also will discharge to battery.Once after the discharge completely, whether electrical properties such as capacity, platform that can the Preliminary detection battery by discharge curve are normal, and judge whether battery is carried out ensuing processing step with this.
Little half charging stage of electric current constant current: current range: 0.1C～1C.Make an appointment with the lithium ion of half to move on the carbon negative pole material again in the lithium iron phosphate positive material, then positive and negative pole material is all got back to stable state, thereby make battery get back to half the most stable electricity condition, so that the SEI rete on the positive pole of battery and the negative pole, particularly negative pole can keep stable, safety in ageing process.
The pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery of the present invention, use the characteristics of aqueous binders at the LiFePO4 aqueous positive-pole, LiFePO4 and aqueous binders are cooperatively interacted, be applicable to by LiFePO4 aqueous positive-pole and carbon negative pole, and the lithium battery that contains the electrolyte composition of organic solvent and lithium salts, can produce high safety, low-cost, long-life flexible package ferric phosphate lithium cell.
Description of drawings
Accompanying drawing 1 is a rated capacity 700mAh's, the voltage-time curve that changes in advance of flexible package LiFePO4 aqueous positive-pole lithium battery.
Accompanying drawing 2 is a rated capacity 700mAh's, the electric current-time graph that changes in advance of flexible package LiFePO4 aqueous positive-pole lithium battery.
Accompanying drawing 3 is a rated capacity 10Ah's, the voltage-time curve that changes in advance of flexible package LiFePO4 aqueous positive-pole lithium battery.
Accompanying drawing 4 is a rated capacity 10Ah's, the electric current-time graph that changes in advance of flexible package LiFePO4 aqueous positive-pole lithium battery.
Embodiment
Embodiment 1: the changing in advance of low capacity flexible package LiFePO4 aqueous positive-pole lithium battery.
As rated capacity 700mAh of accompanying drawing 1, accompanying drawing 2 expressions, flexible package LiFePO4 aqueous positive-pole lithium battery change into curve in advance, wherein accompanying drawing 1 is a voltage-time curve, accompanying drawing 2 is electric current-time graph.Battery is made up of positive pole, negative pole, electrolyte, packaging film etc., wherein just very be bonded in LiFePO 4 material on the aluminium collector with aqueous binders, negative pole is the material with carbon element that is bonded on the copper collector, electrolyte is made up of organic solvent and lithium salts, and the battery wrapping film is aluminum plastic film and is provided with air bag.Battery injects and just enters pre-formation process after electrolyte also once seals, and changes into the system of discharging and recharging in advance and is provided with as follows:
1. shelved 120 minutes;
The 2. little electric current constant current charge stage: the 0.2C constant current charge ends to 4.0V;
3. high voltage constant voltage charge stage: the 4.0V constant voltage charge ends to 0.02C;
4. shelved 5 minutes;
The 5. little electric current constant-current discharge stage: the 0.5C constant-current discharge ends to 2.0V;
6. shelved 5 minutes;
7. little half charging stage of electric current constant current: 0.5C constant current charge 72 minutes.
The effect of shelving 120 minutes is battery to be changed in advance shelve a period of time before, makes electrolyte fully soak into positive and negative pole material and barrier film; Shelving after the high voltage constant voltage charge stage 5 minutes and shelving 5 minutes after the little electric current constant-current discharge stage, is the short time that discharges and recharges the gap to shelve process.
Embodiment 2: capacity flexible package LiFePO4 aqueous positive-pole lithium battery changes in advance greatly.
As rated capacity 10Ah of accompanying drawing 3,4 expression, flexible package LiFePO4 aqueous positive-pole lithium battery change into curve in advance, wherein accompanying drawing 3 is a voltage-time curve, accompanying drawing 4 is electric current-time graph.The component of battery is with embodiment 1, but constituent content increases greatly.Similarly, battery injects and enters pre-formation process after electrolyte also once seals, and changes into the system of discharging and recharging in advance and is provided with as follows:
1. shelved 300 minutes;
The 2. little electric current constant current charge stage: the 0.1C constant current charge ends to 4.0V;
3. high voltage constant voltage charge stage: the 4.0V constant voltage charge ends to 0.01C;
4. shelved 5 minutes;
The 5. little electric current constant-current discharge stage: the 0.1C constant-current discharge ends to 2.0V;
6. shelved 5 minutes;
7. little half charging stage of electric current constant current: 0.15C constant current charge 240 minutes.
Battery capacity is big, and both positive and negative polarity content is big, so shelved 300 minutes, electrolyte could fully soak into positive and negative pole material and barrier film; Several current ratios that discharge and recharge the stage are little than embodiment 1 all, and the electrochemical reaction that can guarantee to occur on the positive and negative pole material is more abundant, more even; Shelving after the high voltage constant voltage charge stage 5 minutes, and shelved 5 minutes after the little electric current constant-current discharge stage, is the short time that discharges and recharges the gap to shelve process equally.
The battery that changes in advance through above-mentioned system is bled and after secondary seals, is just become the LiFePO4 aqueous positive-pole lithium battery of excellent performance.
Experimental results show that, change in advance through above-mentioned work step, and the battery made after sealing of the secondary that wears out and bleed, performance such as capacity, platform is normal, battery charge is to 4.0V inflatable not, deposits 180 days not inflatables under 70 ℃, and can normal charge and discharge cycles, overcharge, cross put, safety tests such as acupuncture, thermal shock are qualified, capacity maintenance＞80% after 2000 times circulate.Experiment as a comparison, get above-mentioned same be positive pole with the water-based LiFePO4, inject 700mAh and 10Ah battery after electrolyte also once seals, adopt the current conventional system that changes in advance, promptly, seal two steps through the aging and secondary of bleeding same as described above then and make battery with the 0.1C 8h that charges.Prepared battery charge like this to 4.0V and circulation several times, perhaps 50 ℃ deposit 24 hours all can inflatable, the capacity maintenance that circulate after 2000 times only has an appointment 70%, obviously there is defective in performance.
Claims (5)
1, a kind of pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery is characterized in that adopting the multistage charge and discharge system in high voltage constant voltage charge stage to carry out.
2, the pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery according to claim 1, it is characterized in that with the voltage that is higher than the battery normal operating range the battery constant voltage charge, high voltage constant voltage charge voltage range is 3.9V～4.5V, and constant voltage charge to electric current drops to 0.005C～0.5C to be ended.
3, the pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery according to claim 1 is characterized in that the multistage charge and discharge system comprises little electric current constant current charge stage, high voltage constant voltage charge stage, little electric current constant-current discharge stage, little half charging stage of electric current constant current.
4, the pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery according to claim 3, it is characterized in that the little electric current constant current charge stage is to constant-current charging of battery, current range is 0.005C～0.5C, constant current charge to the voltage setting value of next stage ends, the high voltage constant voltage charge stage is to the battery constant voltage charge, voltage range is 3.9V～4.5V, constant voltage charge to electric current drops to 0.005C～0.5C to be ended, the little electric current constant-current discharge stage is carried out the discharge fully of little electric current to battery, current range is 0.1C～1C, constant-current discharge to the normal lower voltage limit that uses ends, little half charging stage of electric current constant current is carried out half charging of little electric current to battery, current range is 0.1C～1C, ends behind constant current charge time 0.3～8h.
5, a kind of pre-chemical synthesizing method of flexible package LiFePO4 aqueous positive-pole lithium battery is characterized in that being made up of the following stage of discharging and recharging:
The little electric current constant current charge stage, current range: 0.005C～0.5C, constant current charge to the magnitude of voltage of the setting of next stage ends;
In the high voltage constant voltage charge stage, voltage range: 3.9V～4.5V, constant voltage charge to electric current drop to 0.005C～0.5C to be ended;
The little electric current constant-current discharge stage, current range: 0.1C～1C, constant-current discharge to the normal lower voltage limit that uses ends;
Little half charging stage of electric current constant current, current range: 0.1C～1C ends behind constant current charge time 0.3～8h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102299385A (en) * | 2011-07-29 | 2011-12-28 | 南京双登科技发展研究院有限公司 | Soft package lithium iron phosphate power battery initial charge formation method |
| CN102856590A (en) * | 2012-09-21 | 2013-01-02 | 深圳市美拜电子有限公司 | Forming and capacity grading method of lithium ion secondary battery |
| CN103066329A (en) * | 2011-10-24 | 2013-04-24 | 深圳市比克电池有限公司 | Lithium ion battery activation method |
| CN103515653A (en) * | 2012-06-28 | 2014-01-15 | 深圳市海盈科技有限公司 | Formation method of soft-packed lithium ion battery |
| CN107681214A (en) * | 2017-08-02 | 2018-02-09 | 东莞市迈科科技有限公司 | A kind of lithium-ion electric core mends lithium method |
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| CN102299385A (en) * | 2011-07-29 | 2011-12-28 | 南京双登科技发展研究院有限公司 | Soft package lithium iron phosphate power battery initial charge formation method |
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| CN103066329A (en) * | 2011-10-24 | 2013-04-24 | 深圳市比克电池有限公司 | Lithium ion battery activation method |
| CN103515653B (en) * | 2012-06-28 | 2015-12-09 | 深圳市海盈科技股份有限公司 | The chemical synthesizing method of soft bag lithium ionic cell |
| CN103515653A (en) * | 2012-06-28 | 2014-01-15 | 深圳市海盈科技有限公司 | Formation method of soft-packed lithium ion battery |
| CN102856590B (en) * | 2012-09-21 | 2014-11-26 | 深圳市美拜电子有限公司 | Forming and capacity grading method of lithium ion secondary battery |
| CN102856590A (en) * | 2012-09-21 | 2013-01-02 | 深圳市美拜电子有限公司 | Forming and capacity grading method of lithium ion secondary battery |
| CN107681214A (en) * | 2017-08-02 | 2018-02-09 | 东莞市迈科科技有限公司 | A kind of lithium-ion electric core mends lithium method |
| WO2019109283A1 (en) * | 2017-12-07 | 2019-06-13 | 广州丰江电池新技术股份有限公司 | Lithium ion battery charging method for correcting compensation voltage |
| CN109786875A (en) * | 2019-01-23 | 2019-05-21 | 曹怡珺 | A kind of chemical synthesizing method improving lithium ion battery standing time |
| 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 |
| CN110459817A (en) * | 2019-07-24 | 2019-11-15 | 中国科学院山西煤炭化学研究所 | A kind of nickelic quick chemical synthesis technology of ternary power battery of Soft Roll |
| CN110459817B (en) * | 2019-07-24 | 2022-09-30 | 中国科学院山西煤炭化学研究所 | Soft package high-nickel ternary power battery formation process |
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Open date: 20100127 |