CN103076572A - Method for quickly judging cathode coating process influence on battery cycle performance according to electrochemical impedance spectroscopy (EIS) - Google Patents
Method for quickly judging cathode coating process influence on battery cycle performance according to electrochemical impedance spectroscopy (EIS) Download PDFInfo
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- CN103076572A CN103076572A CN2012105832518A CN201210583251A CN103076572A CN 103076572 A CN103076572 A CN 103076572A CN 2012105832518 A CN2012105832518 A CN 2012105832518A CN 201210583251 A CN201210583251 A CN 201210583251A CN 103076572 A CN103076572 A CN 103076572A
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Abstract
The invention relates to the technical field of lithium ion batteries, and discloses a method for quickly judging cathode coating process influence on battery cycle performance according to an electrochemical impedance spectroscopy (EIS). The method comprises that a series of different cathode pieces are produced through regulating the cathode coating process parameters of a cathode coating machine, cycle performance tests are carried out on the lithium ion battery which is produced by different cathode pieces, the EIS of the lithium ion battery is measured, a corresponding relation of the EIS and the cycle performance of the lithium ion battery is built, and the cathode coating process parameter influence on the lithium ion battery cycle performance is predetermined according to the corresponding relation and the measured lithium ion battery EIS. The scheme is adopted, the method can be used for quickly predetermining the cathode coating process parameter influence on the lithium ion battery cycle performance without testing the battery charge and discharge cycle performances, accordingly, the cost and time for battery cycle performance tests are saved, and the optimum cathode coating process parameters can be quickly found out.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly a kind of according to the quick method of judging that the negative pole coating process affects cycle performance of battery of EIS spectrum.
Background technology
Along with making constant progress of science and technology, various portable electric appts are widely used such as smart mobile phone, laptop computer etc., and people are more and more higher to the degree of dependence of electronic product.Simultaneously, these electronic equipments are also more and more harsher to the requirement of electrochmical power source performance.And lithium ion battery is widely used in the middle of the electronic product with advantages such as its energy density height, voltage stabilization, memory-less effect and environmental protections.Along with the continuous expansion in lithium ion battery applications field, people are also more and more higher to the requirement of its cycle life.
The factor that affects cycle life of lithium ion battery is a lot, such as positive and negative pole material, cementing agent is to the cohesive strength of active substance, forms the quality of solid electrolyte membrane (SEI film), both positive and negative polarity capacity matching in the battery design, discharges and recharges standard, electrolyte content, electrolysis additive etc.Yet in the middle of lithium ion battery manufacturing process, the adjustment of technological parameter also can exert an influence to the cycle performance of lithium ion battery.
At present, be that the full battery of lithium ion is carried out charge and discharge cycles according to certain standard to the most direct determination methods of cycle performance of lithium ion battery.This method reliability is high, and shortcoming is length consuming time, circulates 500 times the bimestrial time of basic need.Therefore, how to judge fast the cycle performance of battery, and then determine that best coating process parameter has become a problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide a kind of composing according to EIS to judge fast the negative pole coating process to the method for cycle performance of battery impact, be intended to solve at present and judge that by the measurement cycle performance of battery different negative pole coating process parameters are on the long problem high with cost of the time of the impact of battery performance.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of according to the method for the quick judgement of EIS spectrum negative pole coating process on the cycle performance of battery impact, may further comprise the steps:
The coating process parameter of regulating the negative pole coating machine prepares different negative plates;
The full battery of different lithium ion that described negative plate is made carries out the cycle performance test;
Measure the electrochemical impedance spectroscopy of the full battery of described lithium ion under full power state;
Set up the corresponding relation between described electrochemical impedance spectroscopy and cycle performance;
According to the electrochemical impedance spectroscopy of described corresponding relation and lithium battery, judge that described negative pole coating process parameter is on the impact of lithium battery cycle performance.
Described coating process parameter comprises coating speed, oven temperature and the rotation speed of fan of negative pole coating machine.
2 ~ 10 m/mins of described coating speeds, described oven temperature are 50 ~ 130 ° of C, and described fan speed is 500 ~ 1000 rev/mins.
Adopt Arbin MITS Pro battery test system that the full battery of described lithium ion is carried out the cycle performance of battery test.
Described cycle performance of battery test is adopted and is discharged and recharged standard, and wherein, the 1C constant-current charge is to 4.2V, and 4.2V constant-voltage charge, cut-off current 0.05C, 1C constant-current discharge are a cycle period to 3.0V.
Adopt electrochemical workstation that the full battery of described lithium ion is carried out the electrochemical impedance spectroscopy test.
The measuring voltage of the full battery of described lithium ion is 4.19V when electrochemical impedance spectroscopy is tested, and the survey frequency scope is 50mHZ-1000HZ, and voltage amplitude is 5mV.
The present invention is by carrying out electrochemical impedance spectrometry and cycle performance test to the full battery of lithium ion that utilizes different negative pole coating processes to make different negative plate preparations under full power state, and set up corresponding relation between the test of electrochemical impedance spectrometry and cycle performance, utilize the electrochemical impedance spectroscopy of this corresponding relation and measurement to judge that different negative pole coating process parameters are on the impact of battery performance.Because the electrochemical impedance spectroscopy measuring speed of battery is fast, realized according to EIS spectrum fast prediction cycle performance of battery, and then judge best negative pole coating process parameter, thereby greatly saved at present and judged that by measuring cycle performance of battery different negative pole coating process parameters on time and the cost of the impact of battery performance, have improved work efficiency.
Description of drawings
Fig. 1 is each baking oven distributing position synoptic diagram of open country coating machine;
Fig. 2 is the full battery of lithium ion loop test result under room temperature 1C of preparation among the embodiment 1 ~ 4;
Fig. 3 is the electrochemical impedance spectroscopy of the full battery of lithium ion of the preparation of embodiment 1 ~ 4;
Fig. 4 is that room temperature 1C cycle battery Capacitance reserve is in the cycle index more than 85% and the relation between electrode reaction resistance.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing, the present invention is further elaborated.
The present invention judges the negative pole coating process to the cycle performance of battery impact fast by the EIS spectrum, and is of the present invention according to the method for the quick judgement of EIS spectrum negative pole coating process on the cycle performance of battery impact, specifically may further comprise the steps:
The coating process parameter of regulating the negative pole coating machine prepares different negative plates;
The full battery of different lithium ion that described negative plate is made carries out the cycle performance test;
Measure the electrochemical impedance spectroscopy of the full battery of described lithium ion under full power state;
Set up the corresponding relation between described electrochemical impedance spectroscopy and cycle performance;
According to the electrochemical impedance spectroscopy of described corresponding relation and lithium battery, judge that described negative pole coating process parameter is on the impact of lithium battery cycle performance.
In the embodiment of the invention, described negative pole coating machine adopts the open country coating machine, and referring to shown in Figure 1, the open country coating machine comprises three baking ovens, is followed successively by baking oven 1, baking oven 2, baking oven 3; During coating, enter the coating machine oven dry from the import of coating machine after, from the outlet on right side out.This coating method adopts roll-type, and the type of heating of three baking ovens of coating machine is the oil temperature heating, after slurry is coated on tinsel, adopts heat oven dry and the dried dual mode of wind jointly to carry out, and the moisture in the negative plate is discharged.
Described coating process parameter comprises coating speed, each oven temperature and the rotation speed of fan of negative pole coating machine.
Described negative pole coating speed is 2-10 m/min, and described each oven temperature is 50 ° of C-130 ° of C, and described fan speed is 500-1000 rev/min.
In the embodiment of the invention, the positive plate of using at the full battery of making lithium ion adopts identical coating process to make, the positive and negative plate and the membrane winding that prepare are assembled into the full battery of lithium ion, with the full battery liquid-filling of lithium ion, change into and aging after, obtain testing the full battery of lithium ion of usefulness, carry out cycle life test and electrochemical impedance spectrometry.
Adopt Arbin MITS Pro battery test system that the full battery of described lithium ion is carried out the cycle performance of battery test.
Described cycle performance of battery test is adopted and is discharged and recharged standard, and wherein, the 1C constant-current charge is to 4.2V, and 4.2V constant-voltage charge, cut-off current 0.05C, 1C constant-current discharge are a cycle period to 3.0V.
Adopt electrochemical workstation the full battery of described lithium ion to be carried out the electrochemical impedance spectroscopy test of battery.
When electrochemical impedance spectroscopy was tested, the measuring voltage of the full battery of described lithium ion was 4.19V, and the survey frequency scope is 50mHZ-1000HZ, and voltage amplitude is 5mV.
Below, by specific embodiment implementation of the present invention and superiority are described.
The making of test battery
The making of positive plate: with cobalt acid lithium, conductive agent, Kynoar (PVDF glue), 1-METHYLPYRROLIDONE (NMP) by a certain percentage mix and blend, be coated with, roll, shear the acquisition positive plate.
Negative plate is made: with Delanium, sodium carboxymethyl cellulose (CMC), conductive agent, cementing agent and deionized water mix and blend according to a certain percentage, coating rolls, and shears to obtain negative plate.
Battery core is made; With positive and negative plate coiling, assembling, oven dry, fluid injection, change into, aging, obtain electrochemical impedance (EIS) and the full battery of the circulation needed lithium ion of measurement.
Electrochemical impedance spectroscopy (EIS) is measured: the full battery of lithium ion of making is carried out electrochemical impedance spectroscopy (EIS) measure.Wherein, the measuring voltage of the full battery of lithium ion is 4.19V, and the survey frequency scope is 50mHZ-1000HZ, and voltage amplitude is 5mV, and the testing apparatus that adopts is the German ZAHNER IM6 of company electrochemical workstation.
Cycle performance test: the full battery of described lithium ion is carried out the cycle performance test.Described circulation standard is that the 1C constant-current charge is to 4.2V; 4.2V constant-voltage charge, cut-off current 0.05C; The 1C constant-current discharge is to 3.0V, and the testing apparatus that adopts is Arbin MITS Pro battery test system.
Set up the corresponding relation of electrochemical impedance (EIS) and cycle performance: according to electrochemical impedance spectroscopy (EIS) and cycle performance data, obtain the empirical relationship of electrochemical impedance spectroscopy (EIS) and cycle performance, and then judge the quality of negative pole coating process parameter.
Embodiment 1:
Behind the even good cathode size that the above-mentioned making negative plate of acquisition is used, begin coating at the open country coating machine.Wherein coating speed is 2.5 meter per seconds, and coating method is roll-type.The Temperature Setting of 1# baking oven is 55 ° of C, and fan speed is 700 rev/mins; The Temperature Setting of 2# baking oven is 75 ° of C, and fan speed is 900 rev/mins; The Temperature Setting of 3# baking oven is 90 ° of C; Fan speed is 1000 rev/mins.
Embodiment 2:
Behind the even good cathode size that the above-mentioned making negative plate of acquisition is used, begin coating at the open country coating machine.Wherein coating speed is 2.2 meter per seconds, and coating method is roll-type.The Temperature Setting of 1# baking oven is 100 ° of C, and fan speed is 500 rev/mins; The Temperature Setting of 2# baking oven is 110 ° of C, and fan speed is 500 rev/mins; The Temperature Setting of 3# baking oven is 125 ° of C, and fan speed is 500 rev/mins.
Embodiment 3:
Behind the even good cathode size that the above-mentioned making negative plate of acquisition is used, begin coating at the open country coating machine.Wherein coating speed is 2.5 meter per seconds, and coating method is roll-type.The Temperature Setting of 1# baking oven is 85 ° of C, and fan speed is 800 rev/mins; The Temperature Setting of 2# baking oven is 90 ° of C, and fan speed is 1000 rev/mins; The Temperature Setting of 3# baking oven is 80 ° of C, and fan speed is 1200 rev/mins.
Embodiment 4:
Behind the even good cathode size that the above-mentioned making negative plate of acquisition is used, begin coating at the open country coating machine.Wherein coating speed is 2.5 meter per seconds, and coating method is roll-type.The Temperature Setting of 1# baking oven is 100 ° of C, and fan speed is 500 rev/mins; The Temperature Setting of 2# baking oven is 110 ° of C, and fan speed is 500 rev/mins; The Temperature Setting of 3# baking oven is 125 ° of C, and fan speed is 500 rev/mins.
Fig. 2 is the cycle performance of the full battery of lithium ion prepared of embodiment 1 ~ 4 different negative pole coating processes.Wherein, the cycle index that remains on more than 85% of embodiment 1 ~ 4 circulation volume is respectively 221,700,303,452 times.
Fig. 3 is the electrochemical impedance spectroscopy measurement result of full battery among the embodiment 1 ~ 4.According to Fig. 2 ~ 3, we can draw, to produce used material and production technology identical when positive pole, electrolytic solution, barrier film, and when only having the negative pole coating process there are differences, the cycle performance of the battery that the Mid Frequency impedance (electrode reaction resistance) of full battery is larger is excellent.By R (QR
Sur) the W Analog Circuits Analysis, the R among the embodiment 1 ~ 4
SurBe respectively 29.1m Ω, 34.9m Ω, 32.1m Ω and 34m Ω, wherein R is the pure physical impedance in the circuit, Q is horizontal phase element, R
SurBe the electrochemical surface reaction impedance, W is the impedance of lithium ion solid-state diffusion.
Need to prove that in order more clearly to compare, the data among the figure have been ignored the pure physical resistance impedance part in the battery system.
Fig. 4 is the full battery electrochemical surface reaction impedance of embodiment 1 ~ 4 and the relation of circulating battery number of times.The circulating battery number of times refers to that capability retention is in the cycle index more than 85%.As can be seen from the figure, along with the increase of electrochemical surface reaction impedance, cycle index increases.Only have when electrochemical impedance and just can reach 500 Capacitance reserves more than 85% greater than the cycle performance of the battery of 34.2m Ω.Therefore, we so that can determine that the negative pole coating process of embodiment 2 is better than embodiment 1, embodiment 3 and embodiment 4.
The present invention by the corresponding relation of setting up battery electrochemical impedance spectrum and cycle performance of battery after, later stage can be judged fast according to the electrochemical impedance spectroscopy of battery the difference of cycle performance of battery, needn't carry out the cycle performance test to battery again, thereby greatly saved the time of experiment, and then select fast best negative pole coating process parameter, so that the cycle performance of battery obtains the best.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. judge fast that according to EIS spectrum the negative pole coating process on the method for cycle performance of battery impact, is characterized in that for one kind, may further comprise the steps:
The coating process parameter of regulating the negative pole coating machine prepares different negative plates;
The full battery of different lithium ion that described negative plate is made carries out the cycle performance test;
Measure the electrochemical impedance spectroscopy of the full battery of described lithium ion under full power state;
Set up the corresponding relation between described electrochemical impedance spectroscopy and cycle performance;
According to the electrochemical impedance spectroscopy of described corresponding relation and lithium battery, judge that described negative pole coating process parameter is on the impact of lithium battery cycle performance.
2. described according to the method for the quick judgement of EIS spectrum negative pole coating process on the cycle performance of battery impact according to claim 1, it is characterized in that described coating process parameter comprises coating speed, oven temperature and the rotation speed of fan of negative pole coating machine.
3. described according to the quick method of judging that the negative pole coating process affects cycle performance of battery of EIS spectrum according to claim 2, it is characterized in that, 2 ~ 10 m/mins of described coating speeds, described oven temperature are 50 ~ 130 ° of C, and described fan speed is 500 ~ 1000 rev/mins.
4. described composing according to EIS judges that fast the negative pole coating process on the method for cycle performance of battery impact, is characterized in that according to claim 1, adopts Arbin MITS Pro battery test system that the full battery of described lithium ion is carried out cycle performance of battery and tests.
5. described according to the quick method of judging that the negative pole coating process affects cycle performance of battery of EIS spectrum according to claim 4, it is characterized in that, described cycle performance of battery test is adopted and is discharged and recharged standard, wherein, the 1C constant-current charge is to 4.2V, 4.2V constant-voltage charge, cut-off current 0.05C, the 1C constant-current discharge is a cycle period to 3.0V.
6. described according to the method for the quick judgement of EIS spectrum negative pole coating process on the cycle performance of battery impact according to claim 1, it is characterized in that the employing electrochemical workstation carries out the electrochemical impedance spectroscopy test to the full battery of described lithium ion.
7. described according to the quick method of judging that the negative pole coating process affects cycle performance of battery of EIS spectrum according to claim 6, it is characterized in that, the measuring voltage of the full battery of described lithium ion is 4.19V when electrochemical impedance spectroscopy is tested, the survey frequency scope is 50mHZ-1000HZ, and voltage amplitude is 5mV.
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| CN107768708A (en) * | 2017-08-28 | 2018-03-06 | 天津力神电池股份有限公司 | The fast appraisement method of lithium battery graphite cathode material cycle performance |
| CN108196123A (en) * | 2017-12-27 | 2018-06-22 | 惠州亿纬锂能股份有限公司 | A kind of evaluation method of lithium ion battery cell internal resistance exception |
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Application publication date: 20130501 |