CN107024662A - A kind of analysis test method of charging and discharging lithium battery performance and Mechanism of electrochemical behaviors of anhydrous - Google Patents
A kind of analysis test method of charging and discharging lithium battery performance and Mechanism of electrochemical behaviors of anhydrous Download PDFInfo
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- CN107024662A CN107024662A CN201710141678.5A CN201710141678A CN107024662A CN 107024662 A CN107024662 A CN 107024662A CN 201710141678 A CN201710141678 A CN 201710141678A CN 107024662 A CN107024662 A CN 107024662A
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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]
- G01R31/378—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator
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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
Abstract
The present invention relates to a kind of charging and discharging lithium battery performance and the analysis test method of Mechanism of electrochemical behaviors of anhydrous, its technical characterstic is：Comprise the following steps：Step 1, electrode active material particles are fabricated to after electrode of lithium cell the electrode of lithium cell is assembled into lithium battery；Step 2, to lithium battery enter pretreatment；Step 3, lithium battery is subjected to charging and discharging lithium battery performance test under different temperatures and different electric current；Step 4, the cut-out point that charging and discharging lithium battery process is set；Step 5, disassemble in inert gas environment lithium battery and stripping electrode；Step 6, under different cut-out points lithium battery electrode plate carry out X-ray diffraction analysis, detection electrode of lithium cell discharge and recharge product change；Step 7, the reaction mechanism equation according to different cut-out points, so as to infer the mechanism of electrode reaction.The present invention can effectively judge the degree that change of the active material in charge and discharge process, electrochemical reaction are carried out, and then can study the discharge and recharge reaction mechanism of battery.
Description
Technical field
The invention belongs to charging and discharging lithium battery technical field of measurement and test, it is related to lithium battery measuring technology and interim phenetic analysis
The analysis test method of technology, especially a kind of charging and discharging lithium battery performance and Mechanism of electrochemical behaviors of anhydrous.
Background technology
At present, the advantages of lithium battery is by its small volume, capacity big and stable operating voltage and become very potential
Novel energy carrier.Understand operation principle, the change of battery active material in charge and discharge process of lithium battery interior in depth
And the degree of reaction progress is the important step in lithium battery design, R＆D work.During researching and developing, preparing lithium battery
It is required to carry out analysis and test to the performance and charge/discharge operation principle of lithium battery.
However, the X-ray diffractometer and in situ X-ray diffraction diffractometer on domestic market can not effective detection different temperatures
Product of the bottom electrode in the different discharge and recharge stages changes.Its reason is：On the one hand, (original position) X-ray diffractometer is independent
Instrument and equipment, it is impossible to which the battery test apparatus different from model cooperates with high-low temperature test chamber；On the other hand, X-ray without
Method is shot through battery case and electrode product is characterized.
According to the record of foreign literature, it is existing can test electrode product in situ X-ray diffraction diffractometer be designed, designed,
The personalized test equipment of transformation, it is not only expensive but also without versatility.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of reasonable in design, testing cost is low and test
Method has the charging and discharging lithium battery performance of versatility and the analysis test method of Mechanism of electrochemical behaviors of anhydrous.
The present invention solves its technical problem and takes following technical scheme to realize：
The analysis test method of a kind of charging and discharging lithium battery performance and Mechanism of electrochemical behaviors of anhydrous, comprises the following steps：
Step 1, electrode active material particles are fabricated to electrode of lithium cell, respectively to electrode active material particles and lithium electricity
The electrode of lithium cell is assembled into lithium battery by pond electrode after carrying out X-ray diffraction analysis；
Step 2, carry out charging and discharging lithium battery performance test before to lithium battery enter pretreatment；
Step 3, lithium battery is subjected to charging and discharging lithium battery performance test under different temperatures and different electric current, and calculates it
The charging and discharging currents under different temperatures and different electric currents, draw charging and discharging lithium battery curve map；
Step 4, the flex point for finding in the charging and discharging lithium battery curve map of step 3 electrode reaction, and the flex point is set
For the cut-out point of charging and discharging lithium battery process；
Step 5, stop at the different cut-out points after the charge and discharge process of lithium battery, lithium electricity is disassembled in inert gas environment
It is stored in after pond and stripping electrode in inert gas environment；
Step 6, by under different cut-out points lithium battery electrode plate carry out X-ray diffraction analysis, detect lithium battery
The discharge and recharge product change of pole；
Step 7, the reaction mechanism equation according to the derivation electrode of lithium cell discharge and recharge of the discharge and recharge product of different cut-out points,
So as to the carry out degree and the mechanism of electrode reaction of inference analysis charging and discharging lithium battery course of reaction.
Moreover, the specific method of the step 1 is：Active material particle progress X to make electrode of lithium cell is penetrated
After line diffraction analysis, electrode of lithium cell is made with electrode active material particles；Then X-ray diffraction point is carried out to electrode of lithium cell
After analysis, judging the distribution of each element in the active material particle and the phase composition of electrode of lithium cell and active material particle is
It is no uniform；Electrode of lithium cell is finally assembled into lithium battery；
Moreover, the preprocess method of the step 2 is：After lithium battery outer application vacuum grease, high/low temperature is placed on
In chamber, it is 80 DEG C to set holding temperature, is incubated 2 hours；
Moreover, lithium battery is carried out charging and discharging lithium battery performance test by the step 3 under different temperatures and electric current
Concretely comprise the following steps：
(1) to set room temperature test temperature respectively be 20 DEG C, low-temperature test temperature is -10 DEG C and high temperature test temperature is 40 DEG C
With 80 DEG C, the electric multiplying power of current charge-discharge be 0.1C, 0.5C, 1C and 2C；
(2) when room temperature is tested, battery is stood 5 minutes；In high temperature or low-temperature test, lithium battery is stood 30
Minute, to ensure the equalized temperature inside and outside battery；
(3) the electric multiplying power of any current charge-discharge in selection 0.1C, 0.5C, 1C and 2C, carries out lithium battery constant-current discharge test, if
Lithium battery final discharging voltage is put for 1.0V；
(4) after constant-current discharge test terminates, lithium battery is stood 30 minutes；
(5) the electric multiplying power of any current charge-discharge in selection 0.1C, 0.5C, 1C and 2C, carries out lithium battery constant-current charge test, makes
Charging current is identical with discharge current size, and sets lithium cell charging final voltage to be 2.5V；
(6) after constant-current charge test terminates, lithium battery is stood 5 minutes；
(7) it is 2.3V to set charging voltage, and charging termination condition is that charging current is less than 0.05C, carries out lithium battery constant pressure
Charging measurement；
(8) after constant-voltage charge test terminates, lithium battery is stood 30 minutes；
(9) return to step 3, under different temperatures and the electric multiplying power of current charge-discharge, are followed successively according to step (3) to step (8)
Ring back and forth carries out charging and discharging lithium battery performance test.
Moreover, the specific method of calculating lithium battery charging and discharging currents under different temperatures and different electric currents of the step 3
For：
Using the calculation formula of lithium battery charge and discharge electric current as follows, charging and discharging lithium battery electric current is calculated：
The electric multiplying power of the quality of active material × active material theoretical capacity × current charge-discharge in charge and discharge electric current=electrode
Wherein, active material theoretical capacity calculation formula is as follows：
In above formula, n is the mole electron number that electrode reaction is shifted, and M is the molal weight of active material.
Moreover, the specific method of the step 5 is：After stopping the charge and discharge process of lithium battery at cut-out point, by lithium electricity
Pond is transferred in the glove box full of inert gas, and the control of glove box dew point is at -70 DEG C and following；Divide in inert gas environment
Solve lithium battery, and after electrode is peeled off in EC electrolyte, the electrode stripped down is placed in glove box be pre-filled with it is lazy
Property gas the sample bottle with rubber seal in, fill vacuum grease on the outside of the sample bottle sealing-plug.
Moreover, the specific method of the step 6 is：By the electrode slice stripped down from the sample bottle full of inert gas
Take out, be immediately placed in the sample storehouse of X-ray diffractometer and vacuumize or be filled with inert gas, to electricity after test condition is met
Pole piece carries out X-ray diffraction analysis, and in analysis result, the hyle for constituting electrode is removed or demarcated, remaining material
Electrode product as in charge and discharge process.
Advantages and positive effects of the present invention are：
1st, the invention provides a kind of charging and discharging lithium battery performance and the analysis test method of Mechanism of electrochemical behaviors of anhydrous, the country is utilized
Existing general sign equipment changes to the product under different temperatures, under different current densities in electrode of lithium cell charge and discharge process
Interim sign is carried out, so as to infer the carry out degree of charging and discharging lithium battery course of reaction and the mechanism of electrode reaction.
2nd, the present invention is divided before charge-discharge test by carrying out X-ray diffraction to CuFeS2 active materials and CuFeS2 electrodes
Analysis and transmission electron microscope observation can determine each element in active material and the phase composition of electrode and active material particle
Distribution it is whether uniform.In addition, active material can effectively be judged by carrying out X-ray diffraction analysis to electrode in discharge process
The degree that change, electrochemical reaction in charge and discharge process are carried out, and then the discharge and recharge reaction mechanism of battery can be studied.
3rd, the present invention can be under inert gas shielding by the stripping electrode easily aoxidized, and carries out electrode product analysis survey
Examination, so as to derive the discharge and recharge reaction mechanism of electrode.Simple to operate, with low cost, reliable results of the invention, synthesis is used
The home equipment of independent function can solve the charging and discharging lithium battery test equipment of domestic generally existing and electrode product analysis is set
Back-up from the problem of；High expense needed for purchase external nonstandard integral test system and consumptive material and correlation have been saved simultaneously
Labour cost, has filled up the blank that charging and discharging lithium battery Analysis on Mechanism is carried out using many general equipment.
4th, the present invention can solve the problem that the problem of electrode change is difficult detection in electrode charge and discharge process.Meanwhile, the present invention is suitable
For the charge and discharge cycles under different temperatures.
Brief description of the drawings
Fig. 1 is the process chart of the present invention；
Fig. 2 is four of Li/CuFeS2 batteries of the present invention under the conditions of room temperature (20 DEG C), 0.1C (0.1C=60mA/g) multiplying power
Secondary charging and discharging curve figure；
Fig. 3 is the X-ray diffraction spectrogram of the CuFeS2 active materials of the present invention；
Fig. 4 is the X-ray diffraction spectrogram of the CuFeS2 electrodes of the present invention；
Fig. 5 is distribution map of the different elements of the present invention in CuFeS2 particles；
Fig. 6 is the Li/CuFeS2 batteries of the present invention cutting on the first time charging and discharging curve under 60mA/g current densities
Breakpoint setup figure；
Fig. 7 is discharge and recharge product figure of the CuFeS2 electrodes in different cut-out points of the present invention.
Embodiment
The embodiment of the present invention is described in further detail below in conjunction with accompanying drawing：
The analysis test method of a kind of charging and discharging lithium battery performance and Mechanism of electrochemical behaviors of anhydrous, as shown in figure 1, including following step
Suddenly：
Step 1, electrode active material particles are fabricated to electrode of lithium cell, respectively to electrode active material particles and lithium electricity
The electrode of lithium cell is assembled into lithium battery by pond electrode after carrying out X-ray diffraction analysis；
The specific method of the step 1 is：X-ray diffraction is carried out to the active material particle to make electrode of lithium cell
After analysis, electrode of lithium cell is made with electrode active material particles；Then electrode of lithium cell is carried out after X-ray diffraction analysis,
Judge whether the distribution of each element in the active material particle and the phase composition of electrode of lithium cell and active material particle is equal
It is even；Electrode of lithium cell is finally assembled into lithium battery.
In the present embodiment, electrode of lithium cell is prepared as electrode active material particles by taking chalcopyrite CuFeS2 as an example,
Using Bruker AXS D8Focus types X-ray diffractometer, (radiation source is CuK α, 10 ° -80 ° of scanning range, operating voltage and electricity
Stream is respectively 40kV and 40mA) X-ray diffraction analysis are carried out to electrode active material particles and overall electrode of lithium cell, it is raw
It is right into the X-ray diffraction spectrogram and the X-ray diffraction spectrogram of CuFeS2 electrodes of CuFeS2 active materials as shown in Figure 3 and Figure 4
The phase composition of active material particle and electrode of lithium cell is characterized；And use NEC company JEM-2100F type high-resolution
The composition and Elemental redistribution of the subsidiary EDS devices of rate transmission electron microscope and X-ray mapping devices to electrode active material particles
Tested, distribution map of the generation different elements as shown in Figure 5 in CuFeS2 particles, and then judge electrode active material
Whether the distribution of each element is uniform in grain.
Step 2, before charging and discharging lithium battery performance test to lithium battery enter pretreatment；
Lithium battery needs to carry out homogenization heat treatment before various tests, and its specific processing method is：On the outside of lithium battery
Coat after vacuum grease, be placed in high-low temperature test chamber, it is 80 DEG C to set holding temperature, is incubated 2 hours；
In the present embodiment, the thermal environment of lithium battery utilizes the GDW-220 types of Cangzhou Xin Xing test apparatuses Co., Ltd
High-low temperature test chamber is realized.In battery outer application vacuum grease to avoid the electrolyte in battery from excessively volatilizing.
Step 3, lithium battery is subjected to charging and discharging lithium battery performance test under different temperatures and different electric current, and calculates it
The charging and discharging currents under different temperatures and different electric currents, draw charging and discharging lithium battery curve map as shown in Figure 2；
Lithium battery is subjected to concretely comprising the following steps for charging and discharging lithium battery performance test under different temperatures and electric current：
(1) to set room temperature test temperature respectively be 20 DEG C, low-temperature test temperature is -10 DEG C and high temperature test temperature is 40 DEG C
With 80 DEG C, the electric multiplying power of current charge-discharge be 0.1C, 0.5C, 1C and 2C；
(2) when room temperature is tested, battery is stood 5 minutes；In high temperature or low-temperature test, lithium battery is stood 30
Minute, to ensure the equalized temperature inside and outside battery；
(3) the electric multiplying power of any current charge-discharge in selection 0.1C, 0.5C, 1C and 2C, carries out lithium battery constant-current discharge test, if
Lithium battery final discharging voltage is put for 1.0V；
(4) after constant-current discharge test terminates, lithium battery is stood 30 minutes；
(5) the electric multiplying power of any current charge-discharge in selection 0.1C, 0.5C, 1C and 2C, carries out lithium battery constant-current charge test, makes
Charging current is identical with discharge current size, and sets lithium cell charging final voltage to be 2.5V；
(6) after constant-current charge test terminates, lithium battery is stood 5 minutes；
(7) it is 2.3V to set charging voltage, and charging termination condition is that charging current is less than 0.05C, carries out lithium battery constant pressure
Charging measurement；
(8) after constant-voltage charge test terminates, lithium battery is stood 30 minutes；
(9) return to step 3, under different temperatures and the electric multiplying power of current charge-discharge, are followed successively according to step (3) to step (8)
Ring back and forth carries out charging and discharging lithium battery performance test.
It is described calculating lithium battery specific method of charging and discharging currents under different temperatures and different electric currents be：
Battery is set to carry out charge-discharge test under different temperatures and electric multiplying power 0.1C, 0.5C, 1C and the 2C of different current charge-discharges.
By taking the electric multiplying power 0.1C of current charge-discharge as an example, illustrate that the calculation formula of charge and discharge electric current is as follows：
The electric multiplying power of the quality of active material × active material theoretical capacity × current charge-discharge in charge and discharge electric current=electrode
(0.1C)
It is 1.0V to set lithium battery final discharging voltage, and end of charge voltage is 2.5V.
Wherein, active material theoretical capacity calculation formula is as follows：
In above formula, n is the mole electron number that electrode reaction is shifted, and M is the molal weight of active material.
In the present embodiment, electrode is prepared using chalcopyrite CuFeS2 as active material particle in test process.In electrode
In reaction, the electron number n=4, CuFeS2 of every mole of CuFeS2 transfer molal weight are 184g/mol.So, CuFeS2's
Active material theoretical capacity is 583mAh/g.
Therefore the current density under electric multiplying power 0.1C, 0.5C, 1C and the 2C of different current charge-discharges is respectively 58.3mA/g,
292mA/g, 583mA/g and 1.2A/g.Charging and discharging lithium battery can be calculated further according to the actual mass of active material in electrode
Charging and discharging currents in test.
In the present embodiment, the quality of active material is 1.5g in electrode, then the electric current of discharge and recharge is under 0.1C multiplying powers
58.3mA/g × 1.5g=87.45mA.
In the present embodiment, charging and discharging lithium battery curve map as shown in Figure 2 is drawn.
Fig. 2 is tested four charge and discharges of the lithium battery under the conditions of room temperature (20 DEG C), 0.1C (0.1C=60mA/g) multiplying power
Electrical testing curve map, and the progress follow-up test analysis by taking this curve as an example.Other test conditions, such as -10 DEG C of low-temperature test, high temperature
40 DEG C and 80 DEG C of test and different current charge-discharge electric multiplying power 0.1C, 0.5C, 1C and 2C, the charging and discharging curve drawn out and
Fig. 2 is compared, and can only be changed in discharge capacity and the aspect of the slope of curve two, and the global shape of curve is constant.
In the present embodiment, using Wuhan LAND (blue electricity) Electronics Co., Ltd. CT-2001A type battery test systems to electricity
Pond carries out charge-discharge test；Battery is controlled using the GDW-220 types high-low temperature test chamber of Cangzhou Xin Xing test apparatuses Co., Ltd
Environment temperature during discharge and recharge.
Step 4, the flex point for finding in the charging and discharging lithium battery curve map of step 3 electrode reaction, and the flex point is set
For the cut-out point of charging and discharging lithium battery process；
In the present embodiment, as shown in fig. 6, the cut-out point of charging and discharging lithium battery process is (a)-(g)；
Fig. 6 is tested first time charging and discharging curve figure of the lithium battery under 60mA/g current densities.Can from figure
Go out, either discharge curve (a-b-c-d) or charging curve (e-f-g) have flex point, i.e. cut-out point.Because,
The charge and discharge process of different phase can be carried out in battery charge and discharge process, and the connecting points between various process are on curve
Flex point.Therefore, we set different flex points to test the different phase knot in battery charge and discharge process on charging and discharging curve
Electrode change after beam, so as to analyze the actual content that electrode is changed in different phase.
Step 5, stop at the different cut-out points after the charge and discharge process of lithium battery, lithium electricity is disassembled in inert gas environment
It is stored in after pond and stripping electrode in inert gas environment；
The specific method of the step 5 is：After stopping the charge and discharge process of lithium battery at cut-out point, lithium battery is shifted
Into the glove box full of argon gas (or other inert gases), the control of glove box dew point is at -70 DEG C and following；In ar gas environment
Lithium battery is decomposed, and in the middle stripping of EC electrolyte (ethylene carbonate), (ethylene carbonate is generally lithium battery body by electrode
Liquid electrolyte) after, the electrode stripped down is placed on to the band that argon gas (or other inert gases) are pre-filled with glove box
Have in the sample bottle of rubber seal, fill vacuum grease to strengthen its sealing property on the outside of the sample bottle sealing-plug.
The sample bottle is stored in the glove box full of argon gas, next step operation is waited.Electricity under different test temperatures
Pond is both needed to carry out after equalized temperature in glove box, and lithium battery and stripping electrode are disassembled according to the method described above.
Step 6, by under different cut-out points lithium battery electrode plate carry out X-ray diffraction analysis, detect lithium battery
The discharge and recharge product change of pole.
The specific method of the step 6 is：The electrode slice stripped down is taken out from the sample bottle full of inert gas,
It is immediately placed in the sample storehouse of X-ray diffractometer and vacuumizes or be filled with inert gas, to electrode slice after test condition is met
X-ray diffraction analysis are carried out, and in analysis result, the hyle for constituting electrode is removed or demarcated, remaining material is
Electrode product in charge and discharge process.
In the present embodiment, CuFeS2 electrodes different cut-out points discharge and recharge product figure, as shown in Figure 7.
Fig. 7 is that different flex points (cut-out point) stop after discharge and recharge tested battery in figure 6, and carries out X-ray to electrode
X-ray diffraction spectrum ((a)-(g)) obtained by diffraction analysis, this diffraction spectra can be with phase group of the show electrode under current state
Into.Diffraction spectra (a) is that the X-ray diffraction spectrum of corresponding electrode is put with (a) in Fig. 6, and now electrode is original non-sparking electrode.From
As can be seen that now electrode is by active material CuFeS in diffraction spectra2, polytetrafluoroethylene (PTFE) and electrically conductive graphite composition.With putting
Material change on the progress of electricity, electrode is undergone (c), eventually become (d) by (b), and electrode group now turns into final electric discharge production
Thing Cu, Fe, Li2(Cu generation necessarily causes Fe and Li to S2S generation, now Fe and Li2S is noncrystalline state, it is impossible to show that X is penetrated
Line diffraction maximum, but Fe and Li are generally accepted in industry2S presence, because CuFeS2Decompose and necessarily form Cu, Fe simple substance and M2Sization
M is Li in compound, the method), the complete intermediate product Li of unreacted0.65CuFeS2And electrode prepares materials conductive graphite and poly-
Tetrafluoroethene.And in charging process (e-f-g), electrode can inversely be carried out along above-mentioned reaction, CuFeS is ultimately formed2's
Active material.
Step 7, the reaction mechanism equation according to the derivation electrode of lithium cell discharge and recharge of the discharge and recharge product of different cut-out points,
So as to the carry out degree and the mechanism of electrode reaction of inference analysis charging and discharging lithium battery course of reaction.
In the present embodiment, it may infer that the reaction mechanism equation of electrode reaction of the electrode of lithium cell in charge and discharge process
Formula is：
It is emphasized that embodiment of the present invention is illustrative, rather than it is limited, therefore present invention bag
Include and be not limited to embodiment described in embodiment, it is every by those skilled in the art's technique according to the invention scheme
The other embodiment drawn, also belongs to the scope of protection of the invention.
Claims (7)
1. the analysis test method of a kind of charging and discharging lithium battery performance and Mechanism of electrochemical behaviors of anhydrous, it is characterised in that：Comprise the following steps：
Step 1, electrode active material particles are fabricated to electrode of lithium cell, respectively to electrode active material particles and lithium battery
The electrode of lithium cell is assembled into lithium battery by pole after carrying out X-ray diffraction analysis；
Step 2, carry out charging and discharging lithium battery performance test before to lithium battery enter pretreatment；
Step 3, lithium battery is subjected to charging and discharging lithium battery performance test under different temperatures and different electric current, and calculates it not
Charging and discharging currents under synthermal and different electric currents, draw charging and discharging lithium battery curve map；
Step 4, the flex point for finding in the charging and discharging lithium battery curve map of step 3 electrode reaction, and the flex point is set to lithium
The cut-out point of battery charge and discharge process；
Step 5, stop at the different cut-out points after the charge and discharge process of lithium battery, lithium battery is disassembled in inert gas environment simultaneously
It is stored in after stripping electrode in inert gas environment；
Step 6, by carrying out X-ray diffraction analysis, detection electrode of lithium cell to the lithium battery electrode plate under different cut-out points
Discharge and recharge product changes；
Step 7, the reaction mechanism equation according to the derivation electrode of lithium cell discharge and recharge of the discharge and recharge product of different cut-out points, so that
The carry out degree of inference analysis charging and discharging lithium battery course of reaction and the mechanism of electrode reaction.
2. the analysis test method of a kind of charging and discharging lithium battery performance according to claim 1 and Mechanism of electrochemical behaviors of anhydrous, it is special
Levy and be：The specific method of the step 1 is：X-ray diffraction is carried out to the active material particle to make electrode of lithium cell
After analysis, electrode of lithium cell is made with electrode active material particles；Then electrode of lithium cell is carried out after X-ray diffraction analysis,
Judge whether the distribution of each element in the active material particle and the phase composition of electrode of lithium cell and active material particle is equal
It is even；Electrode of lithium cell is finally assembled into lithium battery.
3. the analysis test method of a kind of charging and discharging lithium battery performance according to claim 1 or 2 and Mechanism of electrochemical behaviors of anhydrous, its
It is characterised by：The preprocess method of the step 2 is：After lithium battery outer application vacuum grease, thermocycling is placed on
In case, it is 80 DEG C to set holding temperature, is incubated 2 hours.
4. the analysis test method of a kind of charging and discharging lithium battery performance according to claim 1 or 2 and Mechanism of electrochemical behaviors of anhydrous, its
It is characterised by：Lithium battery is carried out the specific of charging and discharging lithium battery performance test by the step 3 under different temperatures and electric current
Step is：
(1) to set room temperature test temperature respectively be 20 DEG C, low-temperature test temperature is -10 DEG C and high temperature test temperature is 40 DEG C and 80
DEG C, the electric multiplying power of current charge-discharge be 0.1C, 0.5C, 1C and 2C；
(2) when room temperature is tested, battery is stood 5 minutes；In high temperature or low-temperature test, lithium battery is stood 30 points
Clock, to ensure the equalized temperature inside and outside battery；
(3) the electric multiplying power of any current charge-discharge in selection 0.1C, 0.5C, 1C and 2C, carries out lithium battery constant-current discharge test, sets lithium
Battery discharge final voltage is 1.0V；
(4) after constant-current discharge test terminates, lithium battery is stood 30 minutes；
(5) the electric multiplying power of any current charge-discharge in selection 0.1C, 0.5C, 1C and 2C, carries out lithium battery constant-current charge test, makes charging
Electric current is identical with discharge current size, and sets lithium cell charging final voltage to be 2.5V；
(6) after constant-current charge test terminates, lithium battery is stood 5 minutes；
(7) it is 2.3V to set charging voltage, and charging termination condition is that charging current is less than 0.05C, carries out lithium battery constant-voltage charge
Test；
(8) after constant-voltage charge test terminates, lithium battery is stood 30 minutes；
(9) return to step 3, under different temperatures and the electric multiplying power of current charge-discharge, are circulated past successively according to step (3) to step (8)
Charging and discharging lithium battery performance test is carried out again.
5. the analysis test method of a kind of charging and discharging lithium battery performance according to claim 1 or 2 and Mechanism of electrochemical behaviors of anhydrous, its
It is characterised by：The calculating lithium battery of the step 3 specific method of charging and discharging currents under different temperatures and different electric currents is：
Using the calculation formula of lithium battery charge and discharge electric current as follows, charging and discharging lithium battery electric current is calculated：
The electric multiplying power of the quality of active material × active material theoretical capacity × current charge-discharge in charge and discharge electric current=electrode
Wherein, active material theoretical capacity calculation formula is as follows：
In above formula, n is the mole electron number that electrode reaction is shifted, and M is the molal weight of active material.
6. the analysis test method of a kind of charging and discharging lithium battery performance according to claim 1 or 2 and Mechanism of electrochemical behaviors of anhydrous, its
It is characterised by：The specific method of the step 5 is：After stopping the charge and discharge process of lithium battery at cut-out point, lithium battery is turned
Move in the glove box full of inert gas, the control of glove box dew point is at -70 DEG C and following；Lithium is decomposed in inert gas environment
Battery, and after electrode is peeled off in EC electrolyte, the electrode stripped down is placed in glove box and is pre-filled with indifferent gas
In the sample bottle with rubber seal of body, vacuum grease is filled on the outside of the sample bottle sealing-plug.
7. the analysis test method of a kind of charging and discharging lithium battery performance according to claim 1 or 2 and Mechanism of electrochemical behaviors of anhydrous, its
It is characterised by：The specific method of the step 6 is：The electrode slice stripped down is taken from the sample bottle full of inert gas
Go out, be immediately placed in the sample storehouse of X-ray diffractometer and vacuumize or be filled with inert gas, to electrode after test condition is met
Piece carries out X-ray diffraction analysis, and in analysis result, the hyle for constituting electrode is removed or demarcated, remaining material is
For the electrode product in charge and discharge process.
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| CN111505507A (en) * | 2019-01-31 | 2020-08-07 | 北京新能源汽车股份有限公司 | Battery aging treatment method |
| CN114114055A (en) * | 2022-01-25 | 2022-03-01 | 天津力神电池股份有限公司 | Method for rapidly evaluating cycle performance of lithium ion soft package battery system |
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| CN110058170A (en) * | 2019-04-04 | 2019-07-26 | 桑顿新能源科技有限公司 | A kind of lithium ion battery analysis lithium nondestructive characterisation (NDC) method |
| CN114114055A (en) * | 2022-01-25 | 2022-03-01 | 天津力神电池股份有限公司 | Method for rapidly evaluating cycle performance of lithium ion soft package battery system |
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