CN110133527A - A method of capacity attenuation is analyzed based on three electrode lithium ion batteries - Google Patents
A method of capacity attenuation is analyzed based on three electrode lithium ion batteries Download PDFInfo
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 145
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000004458 analytical method Methods 0.000 claims abstract description 21
- 230000032683 aging Effects 0.000 claims abstract description 18
- 238000012360 testing method Methods 0.000 claims description 53
- 230000008569 process Effects 0.000 claims description 27
- 230000005611 electricity Effects 0.000 claims description 10
- 239000007773 negative electrode material Substances 0.000 claims description 10
- 239000007774 positive electrode material Substances 0.000 claims description 10
- 230000003247 decreasing effect Effects 0.000 claims description 5
- 238000002474 experimental method Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000003672 processing method Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000009659 non-destructive testing Methods 0.000 abstract description 2
- 208000032953 Device battery issue Diseases 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 229910052493 LiFePO4 Inorganic materials 0.000 description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910017246 Ni0.8Co0.1Mn0.1 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000006183 anode active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006182 cathode active material Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000003447 ipsilateral effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000005502 phase rule Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/385—Arrangements for measuring battery or accumulator variables
- G01R31/387—Determining ampere-hour charge capacity or SoC
- G01R31/388—Determining ampere-hour charge capacity or SoC involving voltage measurements
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/392—Determining battery ageing or deterioration, e.g. state of health
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of methods based on three electrode lithium ion batteries analysis capacity attenuation, it can carry out non-destructive testing lithium ion battery, in the case where not disassembling battery, pass through the discharge voltage profile V-Q figure and voltage derivative curve dV/dQ-Q figure under different cycle-indexes in analysis circulation aging, the reason of judging capacity of lithium ion battery decaying, and then it can propose the basic reason of battery failure, and the performance improvement for battery from now on provides foundation and direction.
Description
Technical field
The present invention relates to technical field of lithium ion, are analyzed more particularly to a kind of based on three electrode lithium ion batteries
The method of capacity attenuation.
Background technique
Environmental pollution and lack of energy are the two large problems of facing mankind.For the dual-pressure of response environment and the energy,
In recent years, in the world majority state all using Development of EV as the important channel of energy-saving and emission-reduction.Power battery is electronic vapour
The performance indicator of one of core component of vehicle, power battery directly affects the overall performance of electric car.In order to guarantee electronic vapour
The traveling and security performance of vehicle just will replace retired lithium battery after electric automobile during traveling is to certain mileage number.Usually
In battery industry, the index whether retired as evaluation battery using battery capacity.However, lithium ion battery is in service stage meeting
There is capacity continuous decrement problem.So the mechanism for researching and analysing capacity of lithium ion battery decaying is extremely important.
The capacity attenuation of lithium ion battery may due to the loss of battery anode active material, battery cathode active material
Loss or battery can be caused by the reasons such as the loss of lithium ion.The battery of different positive and negative pole materials, different circulation industrials
Condition and different environmental conditions cause the mechanism of the decaying of the capacity of battery also not identical.
Research for battery capacity decaying mechanism, generally requires to disassemble on battery, utilizes XRD(X-
RayDiffraction, X-ray diffraction), SEM(ScanningElectronMicroscope, scanning electron microscope) etc. side
Method analyzes the situation of change of the positive and negative anodes of battery, so that judgement obtains the decaying mechanism of battery.But on practical electric vehicle
Battery for, in this way damage battery method be completely it is infeasible.
Summary of the invention
In order to make up the defect of prior art, the present invention provides a kind of based on three electrode lithium ion batteries analysis capacity attenuation
Method.
The technical problems to be solved by the invention are achieved by the following technical programs:
A method of capacity attenuation being analyzed based on three electrode lithium ion batteries, is included the following steps:
S1., three electrode lithium ion batteries are provided；
S2. circulation burn-in test is carried out to the three electrodes lithium ion battery, during the circulation burn-in test, interval one
Determine cycle-index, the test of the battery capacity under different cycle-indexes is carried out to the three electrodes lithium ion battery；Wherein, the electricity
Tankage test includes: a. constant-current charge to setting charge cutoff voltage；B. constant-voltage charge is to setting electric current；C. it is carried out after standing
Constant-current discharge；E. in battery capacity test process, with the electricity of three electrode lithium ion batteries in predeterminated frequency acquisition discharge process
Tankage Q data and voltage V data, wherein the voltage V data include full battery voltage VFData, cathode voltage VPData and
Cathode voltage VNData；
S3. aging is recycled to after arriving defined battery life cut-off condition in three electrode lithium ion batteries, stop circulation aging and survey
Examination；
S4. the discharge voltage profile V-Q figure under different cycle-indexes, the discharge voltage profile V- are drawn in the same coordinate system
Q figure includes full battery voltage curve VF- Q, cathode voltage curve VP- Q and cathode voltage curve VN-Q；
S5. the reason of being schemed according to the discharge voltage profile V-Q, analyzing capacity of lithium ion battery decaying.
Further, the reason of being schemed according to the discharge voltage profile V-Q, analyzing capacity of lithium ion battery decaying specifically wraps
It includes:
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the lithium-ion electric pool capacity
The main reason for amount decaying, loses for inside lithium ion cell positive electrode active materials；
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the lithium-ion electric pool capacity
The main reason for amount decaying, can be lost for the loss of inside lithium ion cell negative electrode active material or battery with lithium ion；
Wherein, cathode voltage curve VPIf-Q is decreased obviously in electric discharge latter stage, full battery voltage curve V is judgedF- Q figure
In, ended in electric discharge latter stage with cathode voltage, otherwise, then judges to end in electric discharge latter stage with cathode voltage.
Further, if full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, then also wrapped
It includes:
Collected battery capacity Q data and voltage V data are subjected to differential process, obtain dQ and dV；
Using collected battery capacity Q data as X-axis data, the ratio of dV/dQ uses gaussian filtering number as Y-axis data
After being filtered according to ratio of the processing method to dV/dQ, voltage derivative curve dV/dQ-Q figure is obtained；Wherein, the voltage
Differential curve dV/dQ-Q figure includes full battery voltage derivative curve dVF/ dQ-Q, cathode voltage differential curve dVP/ dQ-Q and cathode
Voltage derivative curve dVN/dQ-Q；
By cathode voltage differential curve dV obtained in the battery capacity test under different cycle-indexesN/ dQ-Q is in same coordinate
The reason of Right Aligns in system, analysis capacity of lithium ion battery decaying；
If the right half part of each cathode voltage differential song essentially coincides, the main of the capacity of lithium ion battery decaying is judged
Reason be lithium ion battery can be lost with lithium ion, otherwise judge the capacity of lithium ion battery decaying the main reason for for lithium from
Sub- inside battery negative electrode active material loss.
Further, the battery capacity test comprises the steps of:
A. under 25 DEG C ± 2 DEG C of isoperibol, with unitary current I constant-current charge to charge cutoff voltage V1；
B. constant-voltage charge is carried out to three electrode lithium ion batteries with constant pressure V1, until electric current is down to 0.05I cut-off, after charging
Stand 60min；
C. with unitary current I constant-current discharge to discharge cut-off voltage V2,60min is stood after electric discharge；
D. discharge capacity is calculated；
E. step a ~ d is repeated, when continuous very poor 3% less than rated value of test result three times, test is terminated in advance, takes finally
Result average value three times；
F. in battery capacity test process, with the battery capacity of three electrode lithium ion batteries in predeterminated frequency acquisition discharge process
Q data and voltage V data, wherein the voltage V data include full battery voltage VFData, cathode voltage VPData and negative electricity
Press VNData.
Further, the unitary current I is 0.2C, and charge cutoff voltage V1 is 4.2V；The predeterminated frequency is 10s-
30s。
Further, circulation burn-in test is that high temperature accelerates circulation experiment, specifically:
(1) under 45 DEG C ± 2 DEG C of isoperibol, to three electrode lithium ion batteries, constant-current charge is arrived at constant current 0.5C
4.2V, then using constant-voltage charge is carried out, until the electric current of three electrode lithium ion batteries drops to 0.01Cn；(2) 1 hour is stood
Afterwards, constant-current discharge is carried out at constant current 1C, until voltage is reduced to 2.75V, standing 1 hour；(3) discharge capacity is calculated；(4) weight
Multiple step (1)-step (3) is recycled.
Further, the circulation burn-in test is high power charging-discharging circulation.
Further, three electrode lithium ion batteries recycle aging to discharge capacity with respect to initial discharge capacity in step S3
Conservation rate drops to 80%, stops circulation burn-in test.
The invention has the following beneficial effects:
The present invention provide it is a kind of based on three electrode lithium ion batteries analysis capacity attenuation method, can to lithium ion battery into
Row non-destructive testing, it is bent by the discharge voltage under different cycle-indexes in analysis circulation aging in the case where not disassembling battery
Line V-Q figure and voltage derivative curve dV/dQ-Q figure, judge the reason of capacity of lithium ion battery is decayed, and then can propose battery
The basic reason of failure, and the performance improvement for battery from now on provides foundation and direction.
Detailed description of the invention
Fig. 1 is the discharge voltage profile V-Q figure under the different cycle-indexes of one embodiment of the invention；
Fig. 2 is the voltage derivative curve dV/dQ-Q figure under some cycle-index of one embodiment of the invention；
Fig. 3 is the voltage derivative curve dV under the different cycle-indexes of one embodiment of the inventionN/ dQ-Q figure.
Specific embodiment
A method of capacity attenuation being analyzed based on three electrode lithium ion batteries, is included the following steps:
S1., three electrode lithium ion batteries are provided；
In the present invention, the structure of three electrode lithium ion batteries is not especially limited, can pass through technology for this technology personnel
Handbook is learnt or is known by routine experiment method.As an example, the three electrodes lithium ion battery can be
CN204130649U discloses a kind of three-electrode battery, including upper cover, with upper cover fasten lower cover, and setting upper cover, under
Positive plate, negative electrode tab, isolation film, electrolyte in lid, reference electrode, wherein reference electrode is the micron metal of prefabricated plating lithium layer
Platinum filament or copper wire；The three electrodes lithium ion battery may be a kind of three electricity of lithium ion battery disclosed in CN202949008U
Pole device, anode, the length of cathode, width are 1~3cm；Reference electrode is metal lithium sheet, and diameter is 10~20mm, thick
Degree is 0.2cm；The tab of anode, cathode and reference electrode is drawn from the not ipsilateral of shell respectively.It is appreciated that of the invention
Three electrode lithium ion batteries include but is not limited to several structures enumerated supra, and it is unlisted in the present embodiment to be also possible to other
In but by other structures well-known to those skilled in the art.
S2. circulation burn-in test is carried out to the three electrodes lithium ion battery, during the circulation burn-in test,
Every certain cycle-index, the test of the battery capacity under different cycle-indexes is carried out to the three electrodes lithium ion battery.
Wherein, battery capacity test includes: a. constant-current charge to setting charge cutoff voltage；B. constant-voltage charge is to setting
Constant current；C. constant-current discharge is carried out after standing；E. in battery capacity test process, in predeterminated frequency acquisition discharge process
The battery capacity Q data and voltage V data of three electrode lithium ion batteries, wherein the voltage V data include full battery voltage VF
Data, cathode voltage VPData and cathode voltage VNData；
More specifically, the battery capacity test comprises the steps of:
A. under 25 DEG C ± 2 DEG C of isoperibol, with unitary current I constant-current charge to charge cutoff voltage V1；
B. constant-voltage charge is carried out to three electrode lithium ion batteries with constant pressure V1, until electric current is down to 0.05I cut-off, after charging
Stand 60min；
C. with unitary current I constant-current discharge to discharge cut-off voltage V2,60min is stood after electric discharge；
D. discharge capacity is calculated；
E. step a ~ d is repeated, when continuous very poor 3% less than rated value of test result three times, test is terminated in advance, takes finally
Result average value three times；
F. in battery capacity test process, with the battery capacity of three electrode lithium ion batteries in predeterminated frequency acquisition discharge process
Q data and voltage V data, wherein the voltage V data include full battery voltage VFData, cathode voltage VPData and negative electricity
Press VNData.Preferably, the unitary current I is 0.2C, and charge cutoff voltage V1 is 4.2V.
Preferably, the predeterminated frequency is 10s-30s.Predeterminated frequency is too short, and data volume is too big；Predeterminated frequency is too long, nothing
Method, which is flutterred, grasps phase transition process, loses the meaning of analysis.
In the present invention, the circulation burn-in test can accelerate circulation experiment for high temperature, or high power charging-discharging
Circulation, it will be understood that circulation burn-in test of the invention includes but is not limited to several test methods enumerated supra, can also be with
Be other it is unlisted in the present embodiment but by it is well-known to those skilled in the art other circulation ageing testing methods.
In the present invention, to the battery capacity Q data and voltage V data of three electrode lithium ion batteries in acquisition discharge process
Device is not especially limited, and can be acquired using the device that routinely uses in the prior art, preferably, three electrode lithiums from
Sub- battery is separately connected the anode of three electrode lithium ion batteries using Arbin and cathode carries out battery capacity test, utilizes simultaneously
Agilent acquires the voltage on a termination electrode relative to reference electrode.Full battery voltage V in this wayFData, cathode voltage VPData
With cathode voltage VNData can obtain simultaneously.
It is appreciated that the electrode of three electrode lithium ion batteries is respectively anode, cathode and reference electrode.Full electricity in the present invention
Cell voltage VFRefer to the voltage data between anode and cathode；Cathode voltage VPCriticize the voltage data between pole and reference electrode；
Cathode voltage VNRefer to the voltage data between cathode and reference electrode.
Lithium ion battery is a kind of chemical cell, and electrochemical reaction occurs for the internal moment in charge and discharge process, this is just needed
A kind of method for wanting in situ detection inside battery chemical reaction, the present invention is based on three electrode lithium ion batteries to carry out capacity attenuation
Analysis, reference electrode is introduced, and can be carried out in-situ monitoring to inside battery, be can be convenient researcher and more fully understand that battery exists
The electrochemical reaction that positive and negative anodes occur in charge and discharge process.
S3. aging is recycled to after arriving defined battery life cut-off condition in three electrode lithium ion batteries, it is old to stop circulation
Change test；
Preferably, three electrode lithium ion batteries recycle conservation rate of the aging to discharge capacity with respect to initial discharge capacity and drop to
80%, stop circulation burn-in test.
S4. the discharge voltage profile V-Q figure under different cycle-indexes is drawn in the same coordinate system, the discharge voltage is bent
Line V-Q figure includes full battery voltage curve VF- Q, cathode voltage curve VP- Q and cathode voltage curve VN-Q；
Using voltage V data as ordinate data, battery capacity Q data as abscissa in the discharge voltage profile V-Q figure
Data.
S5. the reason of being schemed according to the discharge voltage profile V-Q, analyzing capacity of lithium ion battery decaying.
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the lithium-ion electric
The main reason for tankage is decayed loses for inside lithium ion cell positive electrode active materials；
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the lithium-ion electric pool capacity
The main reason for amount decaying, can be lost for the loss of inside lithium ion cell negative electrode active material or battery with lithium ion.At this point,
It needs further to analyze, specific analytical method are as follows:
Collected battery capacity Q data and voltage V data are subjected to differential process, obtain dQ and dV；
Using collected battery capacity Q data as X-axis data, the ratio of dV/dQ uses gaussian filtering number as Y-axis data
After being filtered according to ratio of the processing method to dV/dQ, voltage derivative curve dV/dQ-Q figure is obtained；Wherein, the voltage
Differential curve dV/dQ-Q figure includes full battery voltage derivative curve dVF/ dQ-Q, cathode voltage differential curve dVP/ dQ-Q and cathode
Voltage derivative curve dVN/dQ-Q；
By cathode voltage differential curve dV obtained in the battery capacity test under different cycle-indexesN/ dQ-Q is in same coordinate
The reason of Right Aligns in system, analysis capacity of lithium ion battery decaying；
If the right half part of each cathode voltage differential song essentially coincides, the main of the capacity of lithium ion battery decaying is judged
Reason be lithium ion battery can be lost with lithium ion, otherwise judge the capacity of lithium ion battery decaying the main reason for for lithium from
Sub- inside battery negative electrode active material loss.
Lithium ion battery can simplify in use for charging, standing, electric discharge continuous repetition.In charging process,
Lithium ion is deviate from from anode, obtains electronics in negative terminal surface across diaphragm；In discharge process, lithium ion is deviate from from cathode, passes through
Diaphragm is embedded into anode.The present invention is using lithium ion battery discharge process as research object.Lithium ion is deviate from from cathode, insertion
When to anode, anode as lithium ion host structure without extra vacancy point embedding lithium ion when, according to Gibbs phase rule, anode is electric
Position decrease speed will be accelerated, and reach discharge cut-off voltage so as to cause full battery voltage.In the present invention, cathode voltage curve
VPIf-Q is decreased obviously in electric discharge latter stage, i.e. cathode voltage curve VP- Q in electric discharge latter stage there is one to be put down relative to voltage
The small tail that platform is decreased obviously, the appearance of this small tail of voltage show that positive electrode active materials can embedding lithium ion
Host structure, the decline of small tail is more, more showing that full battery voltage is influenced by cathode voltage bigger at this time, so judging full battery
Voltage curve VFIn-Q figure, ended in electric discharge latter stage with cathode voltage, otherwise, then judges to cut in electric discharge latter stage with cathode voltage
Only.When active lithium-ion is deviate from from cathode, cathode voltage platform will be gradually lifted, in electric discharge end, cathode voltage curve
The rate of climb will be accelerated.It is heretofore described that cathode voltage curve and for the first time battery capacity are needed to refer to cathode voltage cut-off
Cathode potential specific value when calibration.
" active material " mentioned in description of the invention refers to participating in charge and discharge in lithium ion battery plus-negative plate
The material of lithium ion intercalation/deintercalation reaction in journey, common positive electrode active materials include LiFePO4 (LFP), cobalt acid lithium
(LCO), LiMn2O4 (LMO) and nickel-cobalt-manganese ternary material (NCM) or nickel cobalt aluminium ternary material (NCA) etc., common negative electrode active
Material includes graphite and lithium titanate etc..
The present invention will now be described in detail with reference to examples, and the examples are only preferred embodiments of the present invention,
It is not limitation of the invention.
A method of capacity attenuation being analyzed based on three electrode lithium ion batteries, is included the following steps:
S1. three electrode lithium ion batteries are provided, the three electrodes lithium ion battery uses nominal capacity for the ternary of 2.75Ah circle
Column lithium ion battery Li [Ni0.8Co0.1Mn0.1] O2；
S2. circulation burn-in test is carried out to the three electrodes lithium ion battery, during the circulation burn-in test, interval
100 weeks, the test of the battery capacity under different cycle-indexes is carried out to the three electrodes lithium ion battery；
Wherein, the battery capacity test comprises the steps of:
A. under 25 DEG C ± 2 DEG C of isoperibol, with 0.2C constant-current charge to charge cutoff voltage 4.2V；
B. constant-voltage charge is carried out to three electrode lithium ion batteries with constant pressure 4.2V, until electric current is down to 0.01C cut-off, charging terminates
After stand 60min；
C. with 0.2C constant-current discharge to discharge cut-off voltage, 60min is stood after electric discharge；
D. discharge capacity is calculated；
E. step a ~ d is repeated, when continuous very poor 3% less than rated value of test result three times, test is terminated in advance, takes finally
Result average value three times；
F. in battery capacity test process, with three electrode lithium ion batteries during predeterminated frequency 10s acquisition constant-current discharge
Battery capacity Q data and voltage V data, wherein the voltage V data include full battery voltage VFData, cathode voltage VPData
With cathode voltage VNData；
S3. the conservation rate that three electrode lithium ion batteries recycle aging to the opposite initial discharge capacity of discharge capacity drops to 80%,
Stop circulation burn-in test；
S4. the discharge voltage profile V-Q figure under different cycle-indexes, the discharge voltage profile V- are drawn in the same coordinate system
Q figure includes full battery voltage curve VF- Q, cathode voltage curve VP- Q and cathode voltage curve VN-Q；As shown in Figure 1；
S5. the reason of being schemed according to the discharge voltage profile V-Q, analyzing capacity of lithium ion battery decaying:
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the lithium-ion electric pool capacity
The reason of amount decaying, loses for inside lithium ion cell positive electrode active materials；
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the lithium-ion electric pool capacity
The reason of amount decaying, can be lost for the loss of inside lithium ion cell negative electrode active material or battery with lithium ion；
Wherein, cathode voltage curve VPIf-Q is decreased obviously in electric discharge latter stage, full battery voltage curve V is judgedF- Q figure
In, ended in electric discharge latter stage with cathode voltage, otherwise, then judges to end in electric discharge latter stage with cathode voltage.
If full battery voltage curve VFIn-Q figure, ended in electric discharge latter stage with cathode voltage, then further include: will collect
Battery capacity Q data and voltage V data carry out differential process, obtain dQ and dV；Collected battery capacity Q data is made
For X-axis data, the ratio of dV/dQ is filtered as Y-axis data using ratio of the gaussian filtering data processing method to dV/dQ
After wave processing, voltage derivative curve dV/dQ-Q figure is obtained, as shown in Figure 2；Wherein, the voltage derivative curve dV/dQ-Q figure packet
Include full battery voltage derivative curve dVF/ dQ-Q, cathode voltage differential curve dVP/ dQ-Q and cathode voltage differential curve dVN/dQ-
Q；Referring to Fig. 3, by cathode voltage differential curve dV obtained in the battery capacity test under different cycle-indexesN/ dQ-Q is same
The reason of Right Aligns in one coordinate system, analysis capacity of lithium ion battery decaying；If the right half part of each cathode voltage differential song
The reason of essentially coinciding, then judging capacity of lithium ion battery decaying can be lost for lithium ion battery with lithium ion, otherwise be sentenced
The reason of capacity of lithium ion battery that breaks is decayed loses for inside lithium ion cell negative electrode active material.
The circulation burn-in test specifically: (1) under 45 DEG C ± 2 DEG C of isoperibol, to three electrode lithium ion batteries
Constant-current charge is to 4.2V at constant current 0.5C, then using constant-voltage charge is carried out, until the electric current of three electrode lithium ion batteries
Drop to 0.01C；(2) after standing 1 hour, constant-current discharge is carried out at constant current 1C, until voltage is reduced to 2.75V, standing 1 is small
When；(3) discharge capacity is calculated；(4) step (1)-step (3) are repeated and carries out loop test.
It can be seen in FIG. 1 that initial period of the lithium ion battery in circulation aging, full battery voltage curve VF- Q figure is
Ended with cathode voltage, is gradually converted into circulation ageing process and is ended with cathode voltage.Show that lithium ion battery is starting
Recycle aging when, the capacity of lithium ion battery decay the reason of for inside lithium ion cell negative electrode active material loss or electricity
The loss of Chi Keyong lithium ion.However positive electrode active materials circulation is very fast in circulation ageing process, so that positive electrode active materials damage
Mistake is increasingly becoming the reason of capacity of lithium ion battery decaying.
In fig. 3 it can be seen that the right half part of each cathode voltage differential song essentially coincides, then the lithium-ion electric is judged
The reason of tankage is decayed can be lost for lithium ion battery with lithium ion.
Therefore it may be concluded that the lithium ion battery is in circulation ageing process, the decaying of battery capacity early period is main former
Because being that lithium ion battery can be lost with lithium ion.In the circulation aging later period, the capacity attenuation main cause of battery is positive-active
Material loss, reason may be that positive electrode active materials structural phase transition causes.
Embodiments of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as, as long as skill obtained in the form of equivalent substitutions or equivalent transformations
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (8)
1. a kind of method based on three electrode lithium ion batteries analysis capacity attenuation, which comprises the steps of:
S1., three electrode lithium ion batteries are provided；
S2. circulation burn-in test is carried out to the three electrodes lithium ion battery, during the circulation burn-in test, interval one
Determine cycle-index, the test of the battery capacity under different cycle-indexes is carried out to the three electrodes lithium ion battery；Wherein, the electricity
Tankage test includes: a. constant-current charge to setting charge cutoff voltage；B. constant-voltage charge is to setting electric current；C. it is carried out after standing
Constant-current discharge；E. in battery capacity test process, with the electricity of three electrode lithium ion batteries in predeterminated frequency acquisition discharge process
Tankage Q data and voltage V data, wherein the voltage V data include full battery voltage VFData, cathode voltage VPData and
Cathode voltage VNData；
S3. aging is recycled to after arriving defined battery life cut-off condition in three electrode lithium ion batteries, stop circulation aging and survey
Examination；
S4. the discharge voltage profile V-Q figure under different cycle-indexes, the discharge voltage profile V- are drawn in the same coordinate system
Q figure includes full battery voltage curve VF- Q, cathode voltage curve VP- Q and cathode voltage curve VN-Q；
S5. the reason of being schemed according to the discharge voltage profile V-Q, analyzing capacity of lithium ion battery decaying.
2. the method as described in claim 1 based on three electrode lithium ion batteries analysis capacity attenuation, which is characterized in that according to
The reason of discharge voltage profile V-Q figure, analysis capacity of lithium ion battery decaying, specifically includes:
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the capacity of lithium ion battery
The main reason for decaying is the loss of inside lithium ion cell positive electrode active materials；
If full battery voltage curve VFIn-Q figure, is ended in electric discharge latter stage with cathode voltage, judge the capacity of lithium ion battery
The main reason for decaying is that inside lithium ion cell negative electrode active material loses or battery can be lost with lithium ion；
Wherein, cathode voltage curve VPIf-Q is decreased obviously in electric discharge latter stage, full battery voltage curve V is judgedF- Q figure
In, ended in electric discharge latter stage with cathode voltage, otherwise, then judges to end in electric discharge latter stage with cathode voltage.
3. the method as claimed in claim 2 based on three electrode lithium ion batteries analysis capacity attenuation, which is characterized in that if
Full battery voltage curve VFIn-Q figure, ended in electric discharge latter stage with cathode voltage, then further include:
Collected battery capacity Q data and voltage V data are subjected to differential process, obtain dQ and dV；
Using collected battery capacity Q data as X-axis data, the ratio of dV/dQ uses gaussian filtering number as Y-axis data
After being filtered according to ratio of the processing method to dV/dQ, voltage derivative curve dV/dQ-Q figure is obtained；Wherein, the voltage
Differential curve dV/dQ-Q figure includes full battery voltage derivative curve dVF/ dQ-Q, cathode voltage differential curve dVP/ dQ-Q and cathode
Voltage derivative curve dVN/dQ-Q；
By cathode voltage differential curve dV obtained in the battery capacity test under different cycle-indexesN/ dQ-Q is in the same coordinate system
The reason of middle Right Aligns, analysis capacity of lithium ion battery decaying: if the right half part of each cathode voltage differential song essentially coincides,
The main reason for then judging capacity of lithium ion battery decaying can be lost for lithium ion battery with lithium ion, otherwise described in judgement
The main reason for capacity of lithium ion battery is decayed loses for inside lithium ion cell negative electrode active material.
4. the method as described in claim 1 based on three electrode lithium ion batteries analysis capacity attenuation, which is characterized in that described
Battery capacity test comprises the steps of:
A. under 25 DEG C ± 2 DEG C of isoperibol, with unitary current I constant-current charge to charge cutoff voltage V1；
B. constant-voltage charge is carried out to three electrode lithium ion batteries with constant pressure V1, until electric current is down to 0.05I cut-off, after charging
Stand 60min；
C. with unitary current I constant-current discharge to discharge cut-off voltage V2,60min is stood after electric discharge；
D. discharge capacity is calculated；
E. step a ~ d is repeated, when continuous very poor 3% less than rated value of test result three times, test is terminated in advance, takes finally
Result average value three times；
F. in battery capacity test process, with the battery capacity of three electrode lithium ion batteries in predeterminated frequency acquisition discharge process
Q data and voltage V data, wherein the voltage V data include full battery voltage VFData, cathode voltage VPData and negative electricity
Press VNData.
5. the method as claimed in claim 4 based on three electrode lithium ion batteries analysis capacity attenuation, which is characterized in that described
Unitary current I is 0.2C, and charge cutoff voltage V1 is 4.2V；The predeterminated frequency is 10s-30s.
6. the method as described in claim 1 based on three electrode lithium ion batteries analysis capacity attenuation, which is characterized in that circulation
Burn-in test is that high temperature accelerates circulation experiment, specifically:
(1) under 45 DEG C ± 2 DEG C of isoperibol, to three electrode lithium ion batteries, constant-current charge is arrived at constant current 0.5C
4.2V, then using constant-voltage charge is carried out, until the electric current of three electrode lithium ion batteries drops to 0.01Cn；(2) 1 hour is stood
Afterwards, constant-current discharge is carried out at constant current 1C, until voltage is reduced to 2.75V, standing 1 hour；(3) discharge capacity is calculated；(4) weight
Multiple step (1)-step (3) is recycled.
7. the method as described in claim 1 based on three electrode lithium ion batteries analysis capacity attenuation, which is characterized in that described
Burn-in test is recycled as high power charging-discharging circulation.
8. the method as described in claim 1 based on three electrode lithium ion batteries analysis capacity attenuation, which is characterized in that step
The conservation rate that three electrode lithium ion batteries recycle aging to the opposite initial discharge capacity of discharge capacity in S3 drops to 80%, stops
Recycle burn-in test.
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