CN107768708A - The fast appraisement method of lithium battery graphite cathode material cycle performance - Google Patents
The fast appraisement method of lithium battery graphite cathode material cycle performance Download PDFInfo
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Abstract
The present invention relates to a kind of fast appraisement method of lithium battery graphite cathode material cycle performance, it is characterized in that：Using electrochemical impedance spectroscopy, the electrode test of full battery three and dQ/dV V curves based on capacity increment, with reference to local SOC round-robin methods, the cycle performance of Fast Evaluation graphite cathode material is realized.Beneficial effect：The present invention has non-demolition feature in situ, it is not necessary to destroys the cycle performance of the i.e. detectable battery of battery；Test period is short, efficiency high, can save for 40% 70% testing time；Cost is low, can substantially reduce energy consumption, greatly save man power and material；Process is simple to operation；Normal temperature environment can be carried out, without complex conditions；It is highly reliable, it is more obvious than conventional method to shorten the testing time.Suitable for the limitation of circular batteries, square battery and soft-package battery, not limited by dimensions, it can be widely applied for producing greatly, electricity can be saved significantly on, cost can be significantly reduced, save man power and material.
Description
Technical field
The invention belongs to electrochemical field, more particularly to a kind of Fast Evaluation of lithium battery graphite cathode material cycle performance
Method.
Background technology
The method of Evaluation: Current lithium battery graphite cathode material cycle performance mainly still makes full battery, then according to one
Fixed circulation standard carries out cycle life test.It is full full of putting mostly, until the 80% of initial lifetime terminates test.With one
As exemplified by the relatively low consumer battery of 3C classes of life requirements, the cycle life of 500 times to 1000 times is typically required, using 1C
Full be full of puts standard, has tested the cycle life of 500 times to 1000 times and has taken around 50 days to 100 days；Again with the storage of long-life
Exemplified by energy battery, the cycle life of 3000 to 6000 times is typically required, using 1C charge and discharge standards, has been tested 3000 times to 6000 times
Cycle life take around 300 days to 600 days.It will be apparent that so long test period not only wastes the substantial amounts of time, and
It can increase including the great amount of cost such as human and material resources and power consumption.Even novel anode material prepares its evaluation method still
So use the above method.A kind of lithium ion battery negative material manufacture method as disclosed in patent document 1691373, including it is as follows
Step：(1) graphite is mixed with covering material with solvent, vacuumized, desolvation, native graphite is coated on cladding material raw material
In, (2) and then material is subjected to thermal polymerization, native graphite surface obtains the clad of microencapsulation；(3) step (2) is obtained
The product obtained is carbonized or carried out graphitization, obtains the carbon cathode material of Surface coating artificial stone layer of ink, is this hair
Bright lithium ion battery negative material.The cell negative electrode material testing result obtained is:Tap density compares table more than 1.08
Area is below 2.20, and discharge capacity is in more than 350mAh/g (irreversible capacity is less than 25mAh/g), first charge-discharge effect first
Rate circulates 450 times more than 93% and still retains more than the 90% of capacity first.Patent document 104882608A discloses a kind of N
The preparation method of 3D graphenes/graphite lithium ion battery negative material is adulterated, weighs graphite oxide, ascorbic acid and urea dissolving
Ultrasonic disperse is heated to forming sticky semigel state after water, adds graphite to form thicker material after continuing stirring.Will
Mixing concentrated thing, which is moved in autoclave, to be continued to react, and is taken out sample and is filtered, washs, dries, after being calcined in tube furnace
To N doping 3D graphenes/graphite combination electrode material.Electrode active material is mixed with acetylene black and Kynoar binding agent
Uniformly, it is applied to copper foil surface and battery electrode piece is made, half-cell is assembled into glove box and charge-discharge performance survey is carried out to it
Examination.Found by detection, N doped graphenes/graphite combination electrode material capacity under 0.2C multiplying powers still has 500mAh/g, circulates
Charging and discharging capacity remains to keep more than 90% after 100 times, has good high rate performance and cyclical stability.
Given this method of traditional evaluation negative pole cycle performance takes that oversize, energy consumption is larger, cost is too high, it is necessary to occupy
Test equipment long period, invisible and increase equipment cost.A kind of Fast Evaluation silicon/carbon/graphite in lithium ion batteries is urgently studied in the industry to bear
The method of pole material circulation performance.
The content of the invention
It is an object of the invention to overcome the shortcomings of above-mentioned technology, and provide a kind of lithium battery graphite cathode material cyclicity
The fast appraisement method of energy, can will not both be caused to damage to battery again with the cycle performance of rapid evaluation negative material.
The present invention to achieve the above object, using following technical scheme：A kind of lithium battery graphite cathode material cycle performance
Fast appraisement method, it is characterized in that：Utilize electrochemical impedance spectroscopy, the electrode test of full battery three and dQ/ based on capacity increment
DV-V curves, with reference to local SOC round-robin methods, the cycle performance of Fast Evaluation graphite cathode material is realized, is comprised the following steps that：
1) Soft Roll laminated batteries are prepared with common process, positive pole uses LiFePO 4 (LFP), and negative pole uses A and two kinds of B
Graphite cathode, the gram volume of two kinds of graphite cathodes is in 340mAh/g, and efficiency is 90% to full battery first, cycle performance it is excellent
It is bad have it is to be assessed；
2) the full electrode of battery three is made：It is implanted into using metal lithium sheet as reference electrode among aluminum plastic film, with the one of nickel lug
End and lithium piece are combined together by physical impact, pass through aluminium with PE or the coated metal lithium sheet of ceramic diaphragm, the other end of nickel lug
The airbag of plastic film draws reference electrode as lead；
3) battery is carried out to the activation of 3-5 circulation on battery test system：
Charge standard：1C constant currents are to 3.65V；3.65V constant pressures, 0.05C cut-offs, rest 10min；
Electric discharge standard：1C is put to 2V, rest 10min, using the discharge capacity of last circulation as normal capacity, with most
The charging curve or discharge curve data of the latter circulation carry out differential process with data processing software, make dQ/dV-V curves；
(1) normal capacity before circulating or after circulation is determined；
(2) the dQ/dV-V curves before circulating or after circulation are determined, dV voltage samples are 0.03V；
(3) before test loop or after circulation full battery EIS；
(4) using three electrode potentials that battery is tested on battery test system：Need to use three channel monitoring electrode electricity
Position, A channel monitoring anodic potentials, channel B monitor full cell potential, C-channel monitoring negative pole current potential；
4) cyclic process：
(1) SOC locally accelerates circulation standard：1C current charge-discharges, the electricity between electricity difference DELTA SOC selections 30% -80%
Amount；Circulated with time control SOC, battery is first vented electricity to 2V, is then charged to cut-off electricity (charge cutoff electricity with the charging interval
Measure scope 30%-100%), put to cut-off electricity (electric discharge cut-off electricity scope 0-70%) with discharge time, then cut in charging
Only loop test is carried out between electricity and electric discharge cut-off electricity；
(2) during Δ SOC=30%, SOC electricity interval selections 0-30%, 30%-60%, 40%-70%, 70%-
100%；
During Δ SOC=40%, SOC electricity interval selections 0-40%, 30%-70%, 40%-80%, 50%-90%；
During Δ SOC=50%, SOC electricity interval selections 0-50%, 25-75%, 30-80%, 40-90%, 50-100%；
During Δ SOC=60%, SOC electricity interval selections 0-60%, 10-70%, 20-80%, 30%-90%, 40-
100%；
During Δ SOC=70%, SOC electricity interval selections 0-70%, 10-80%, 20-90%, 30-100%；
During Δ SOC=80%, SOC electricity interval selections 0-80%, 10-90%, 20-100%；
5) by taking Δ SOC=40% as an example, with time control SOC, circulated, charged in 40-80%SOC electricity section
End electricity SOC=80%, electric discharge cut-off electricity SOC=40%, repeat the above steps 3 after 500 circulations,
6) result of step 3 and step 5 is contrasted, is analyzed, draws test result, you can Fast Evaluation graphite is born
The cycle performance of pole material.
Beneficial effect：Compared with prior art, the present invention has non-demolition feature in situ, it is not necessary to it is i.e. detectable to destroy battery
The cycle performance of battery；Test period is short, efficiency high, can save 40%-70% testing time；Cost is low, can be significantly
Energy consumption is reduced, greatlys save man power and material；Method is simple to operate, and process is simple to operation；Normal temperature environment can be carried out, without
Complex conditions；It is highly reliable, it is more obvious than conventional method to shorten the testing time.Suitable for circular batteries, square battery and Soft Roll
The limitation of battery, not limited by dimensions, it can be widely applied for producing greatly, electricity can be saved significantly on, cost can be significantly reduced,
Save man power and material.
Brief description of the drawings
Fig. 1 is the front and rear EIS figures of two kinds of graphite circulations of AB；
Fig. 2 is the schematic diagram of negative pole current potential before and after two kinds of graphite circulations of AB；
Fig. 3 is the front and rear dQ/dV-V curves of two kinds of graphite circulations of AB；
Fig. 4 a are the capacity sustainment rate accelerated method test results after two kinds of graphite circulations of AB of the present invention；
Fig. 4 b are the results of the capacity sustainment rate after two kinds of graphite circulations of conventional recycle method of testing test AB；
Fig. 5 is the inventive method compared with the time of conventional recycle method.
Embodiment
Describe the embodiment of the present invention in detail with reference to preferred embodiment.
A kind of fast appraisement method of lithium battery graphite cathode material cycle performance is present embodiments provided, utilizes electrochemistry
Impedance spectrum (EIS), the electrode test of full battery three and the dQ/dV-V curves based on capacity increment, with reference to local SOC round-robin methods,
The cycle performance of Fast Evaluation graphite cathode material is realized, is comprised the following steps that：
1st, the laminated batteries of Soft Roll 4360143 are prepared, for positive pole by taking LiFePO 4 (LFP) as an example, negative pole uses graphite cathode,
It is two kinds of graphite of A and B respectively, capacity and efficiency is suitable first, the gram volume of two kinds of graphite cathodes is in 340mAh/g, full battery
Efficiency is 90% first；Make the full electrode of battery three：It is implanted into using metal lithium sheet as reference electrode among aluminum plastic film, with nickel pole
One end of ear and lithium piece are combined together by physical impact, with PE or the coated metal lithium sheet of ceramic diaphragm, the other end of nickel lug
Lead is used as by the airbag of aluminum plastic film and draws reference electrode；
The 2nd, battery is carried out to 3-5 activation, standard is put using full be full of：1C constant currents are to 3.65V, 3.65V constant pressures, 0.05C
Cut-off, rest 10min, standard of discharging：1C is put to 2V, rest 10min.Purpose is：
(1) determine 1C initial capacities as normal capacity；
(2) initial dQ/dV-V curves, dV voltage samples section 0.03V are determined；
(3) EIS of initial fresh cells is tested；
(4) three electrode potentials of battery are tested, it is main to monitor negative pole current potential.
3rd, cyclic process：
SOC locally accelerates circulation：1C current charge-discharges, Δ SOC are that 80%SOC is arrived in 40%, SOC electricity scope selection 40%,
Battery is first vented electricity to 2V, second step and charges to 80%SOC, charging interval 48min with time control by the first step, and the 3rd step is used
Time control is discharged to 40% electricity, discharge time 24min, rest 10min, and the 4th step is recharged to 80%SOC, the charging interval
24min, the 3rd step and the 4th step are a circulation；Circulated 500 times between 80%SOC 40%；
4th, by taking Δ SOC=40% as an example, with time control SOC, circulated, charged in 40-80%SOC electricity section
End electricity SOC=80%, electric discharge cut-off electricity SOC=40%, repeat the above steps 2 after 500 circulations,
(1) capacity after circulating is determined 500 times；
(2) dQ/dV-V curves after circulating are determined 500 times, dV voltage samples are 0.03V；
(3) EIS of battery after circulating is tested 500 times；
(4) three electrode potentials of battery after circulating are tested 500 times, monitor negative pole current potential；
5th, the result of step 2 and step 4 is contrasted, is analyzed, draws test result, you can Fast Evaluation graphite is born
The cycle performance of pole material.
Local electricity difference DELTA SOC refers to the difference between battery high SOC and low SOC, and minimum SOC is 0, highest
SOC is 100%.
Operation principle
It is bent that the present invention combines electrochemical impedance spectroscopy (EIS), the electrode test of full battery three, the dQ/dV-V based on capacity increment
Line and the method for local SOC circulations come the cycle performance of Fast Evaluation graphite cathode material, electrochemical impedance spectroscopy (EIS), full electricity
The electrode test of pond three and dQ/dV-V curves based on capacity increment are all nondestructive methods in situ, and battery will not be caused to damage
Wound can be used to assess the performance of negative material, and the method for combining local SOC circulations being capable of Fast Evaluation graphite cathode material
Cycle performance.It is that full be full of is put to accelerate circulation and 3-5 circulation by the part of 50-50000 times, you can it is determined that after circulation
Capacity, two contrasts just draw capacity dimension holdup；Pass through the full dQ/ front and rear with regard to circulation can be drawn full of the discharge and recharge data put
DV-V curves.Wherein 50-50000 times is local acceleration circulation；3-5 circulation is full full of putting, it is determined that the capacity after circulation.
Two contrasts just draw capacity dimension holdup；By full bent with regard to the front and rear dQ/dV-V of circulation can be drawn full of the discharge and recharge data put
Line.
Device therefor：Electrochemical workstation, battery testing arbin equipment
Wherein SOC, full name are State of Charge, state-of-charge, are also dump energy, representative is that battery uses
Residual capacity and the ratio of the capacity of its fully charged state after lying idle for a period of time or for a long time, commonly use percentage table
Show.Its span is 0~100%, represents that battery discharge is complete as SOC=0, represents that battery is complete as SOC=100%
It is full of.The method of local SOC circulations refers to select suitable local electricity scope to carry out loop test between 0-100% electricity
Method, such as select local electricity difference DELTA SOC=40%, then local SOC electricity scope can be from 0-40%, 30-
70% or 40-80% is selected.By taking 40% to 80% local electricity section as an example, charge cutoff electricity is 80%SOC, electric discharge cut-off
For 40% electricity, then the method for local SOC circulation is exactly the method for carrying out loop test between local electricity section herein.
Experimental procedure：
1) laminated batteries of Soft Roll 4360143 of preparation are carried out to the activation of 5 circulations, the circulation standard of activation：Charging：1C
Constant current 3.65V constant pressures, 0.05C cut-offs, rest 10min, is discharged to 3.65V：1C is put to 2V, rest 10min, is repeated 5 times, is taken
The capacity of last circulation is standard initial capacity C1；
2) the full electrode of battery three is prepared using metal lithium sheet as reference electrode, LFP is positive pole, and graphite is negative pole；
3) before circulating：(1) full battery EIS tests, (2) full electrode test of battery three, (3) are with the hits of arbin equipment
According to making dQ/dV-V curves；
4) loop test：1C current cycle charge and discharges, Δ SOC=40%, SOC section 40-80%, cycle-index are 500 times
Or 1000 times；
5) after loop test：Repeat step 1, obtains the capacity C 2 after 500 circulations, and C2/C1 obtains 500 circulations
Capacity sustainment rate afterwards；Repeat step 3；
6) EIS, the test of three electrode potentials, dQ/dV-V curves and C2/C1 results, the cyclicity of more different negative poles are passed through
Energy.
With traditional evaluation method comparative effectiveness
Fig. 1 is EIS test results, illustrates the EIS test results before and after two kinds of graphite of AB circulate 500 times, can from figure
To find out the front and rear series resistance (R of two kinds of graphite testsS) it is suitable, but the interface charge transmission after 500 circulations
Resistance (Rct) there is significantly different, B graphite RctIncrease the amplification for substantially, having 40%, A graphite only has 7% amplification, less Rct
Mean more preferable dynamic process, also just the polarization of explanation A graphite is smaller, can speculate that the circulation of A graphite may be more indirectly
It is good, but evidence is not abundant enough.
The front and rear negative pole current potential (Vs.Li of two kinds of graphite cathode circulations of Fig. 2 tests AB+/ Li) change, hence it is evident that it can be seen that
Negative pole potential change is little before and after the circulation of A graphite, but B graphite has obvious reduction in the front and rear negative pole current potential of circulation, follows for 500 times
Current potential about reduces 0.01V after ring；The current potential that graphite cathode A can also be will become apparent from from figure two is higher by about than graphite cathode B
0.06V, this also shows that negative pole current potential height is advantageous to improve cycle performance indirectly, and negative pole current potential height additionally aids improvement battery
Safety.
Fig. 3 illustrates the front and rear dQ/dV-V curves of two kinds of graphite circulations of AB, and dQ/dV-V curves are a kind of based on capacity increasing
The analytic approach of amount, three embedding lithium peak positions of negative pole can be told, embedding lithium peak position is to low potential after 500 circulations of A graphite
Mobile 0.01V, showing the polarization of battery inside battery after cycling does not increase；B graphite embedding lithium peak position after 500 circulations
0.02V is significantly moved to high potential, showing the polarization of battery inside battery after cycling substantially increases, and this also shows indirectly
The cycle performance of A graphite is better than B graphite.Figure four directly illustrates the capacity sustainment rate ratio after the circulation of two kinds of AB graphite 500 times
Compared with,
Fig. 4 (a) results show that after 500 times accelerate circulation the capacity sustainment rate of A graphite is higher by than B graphite
0.5%, in order to compare the correctness of data,
Fig. 4 (b) illustrates the circulation volume sustainment rate of two kinds of graphite conventional test methodologies of AB, and similarly, A graphite cathodes follow
Ring is more preferable, and capacity dimension holdup is higher by 0.4% after 500 times, and the test result of the two is quite coincide.
Complex chart 1, Fig. 2, Fig. 3 and Fig. 4 test result, it can be deduced that clear and definite conclusion：The cycle performance of A graphite is substantially better than
B graphite.Therefore, this experimental method has reliability, hence it is evident that can shorten the testing time than conventional method.
The time that Fig. 5 illustrates the inventive method and conventional inspection method contrasts, and this method only needs 20 days can be quick
The cycle performance of evaluating graphite negative pole, and conventional method (full are full of of 1C is put) needs 50 days.Obviously, this method have rapidity and
Validity, and using with reference to EIS, three electrode tests, dQ/dV-V curves, mutually evidence, there is sensitivity, the orientation of evaluation
More comprehensively, the degree of accuracy is higher, is advantageous to the cycle performance and screening negative material of Fast Evaluation negative material, it is a large amount of save into
This.In addition, the battery advantage that (more than 3000 times) are lasted a long time for test loop is more obvious.
Above-mentioned reference embodiment is carried out to a kind of fast appraisement method of lithium battery graphite cathode material cycle performance
It is described in detail, is illustrative rather than limited, several embodiments can be included according to limited scope, therefore not
Depart from changing and modifications under present general inventive concept, should belong within protection scope of the present invention.
Claims (3)
1. a kind of fast appraisement method of lithium battery graphite cathode material cycle performance, it is characterized in that：Using electrochemical impedance spectroscopy,
The full electrode test of battery three and the dQ/dV-V curves based on capacity increment, with reference to local SOC round-robin methods, realize Fast Evaluation
The cycle performance of graphite cathode material, is comprised the following steps that：
1) Soft Roll laminated batteries being prepared with common process, positive pole uses LiFePO 4, and negative pole uses two kinds of graphite cathodes of A and B,
The gram volume of two kinds of graphite cathodes is in 340mAh/g, and efficiency is 90% to full battery first；
2) the full electrode of battery three is made：Be implanted into using metal lithium sheet as reference electrode among aluminum plastic film, with one end of nickel lug and
Lithium piece is combined together by physical impact, passes through aluminum plastic film with PE or the coated metal lithium sheet of ceramic diaphragm, the other end of nickel lug
Airbag as lead draw reference electrode；
3) battery is carried out to the activation of 3-5 circulation on battery test system：
Charge standard：1C constant currents are to 3.65V；3.65V constant pressures, 0.05C cut-offs, rest 10min；
Electric discharge standard：1C is put to 2V, rest 10min, using the discharge capacity of last circulation as normal capacity, with last
The charging curve or discharge curve data of individual circulation carry out differential process with data processing software, make dQ/dV-V curves；
(1) normal capacity before circulating or after circulation is determined；
(2) the dQ/dV-V curves before circulating or after circulation are determined, dV voltage samples are 0.03V；
(3) before test loop or after circulation full battery electrochemical impedance spectroscopy；
(4) using three electrode potentials that battery is tested on battery test system：Using three channel monitoring electrode potentials, i.e. A leads to
Road monitors anodic potentials, and channel B monitors full cell potential, C-channel monitoring negative pole current potential；
4) cyclic process：
Locally accelerate circulation standard using SOC：1C current charge-discharges, between local electricity difference DELTA SOC selections 30% -80%
Electricity；Circulated with time control SOC, battery is first vented electricity to 2V, cut-off electricity, charge cutoff are charged to using the charging interval
Electricity scope is 30%-100%, is put using discharge time to electric discharge and ends electricity, electric discharge cut-off electricity scope is 0-70%, so
Loop test is carried out between charge cutoff electricity and electric discharge cut-off electricity, after cycle-index scope 50-50000 times, then weigh afterwards
Multiple above-mentioned steps 3；
5) result of step 3) and step 4) is contrasted, draws test result, you can the cyclicity of Fast Evaluation graphite cathode material
Energy.
2. the fast appraisement method of lithium battery graphite cathode material cycle performance according to claim 1, it is characterized in that：Step
It is rapid that 4) local electricity difference DELTA SOC refers to the difference between battery high SOC and low SOC, minimum SOC described in cyclic process
It is 0, highest SOC is 100%, and wherein optimal selection is respectively：
During Δ SOC=30%, SOC electricity interval selections 0-30%, 30%-60%, 40%-70%, 70%-100%；
During Δ SOC=40%, SOC electricity interval selections 0-40%, 30%-70%, 40%-80%, 50%-90%, 60-
100%；
During Δ SOC=50%, SOC electricity interval selections 0-50%, 25-75%, 30-80%, 40-90%, 50-100%；
During Δ SOC=60%, SOC electricity interval selections 0-60%, 10-70%, 20-80%, 30%-90%, 40-100%；
During Δ SOC=70%, SOC electricity interval selections 0-70%, 10-80%, 20-90%, 30-100%；
During Δ SOC=80%, SOC electricity interval selections 0-80%, 10-90%, 20-100%.
3. the fast appraisement method of lithium battery graphite cathode material cycle performance according to claim 1, it is characterized in that：Step
When rapid 4) described charge cutoff electricity SOC=80%, electric discharge cut-off electricity SOC=40%, 500 circulations are carried out.
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