CN109856113A - A kind of evaluation method for cathode of lithium battery graphite - Google Patents
A kind of evaluation method for cathode of lithium battery graphite Download PDFInfo
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Abstract
The invention discloses a kind of evaluation methods for cathode of lithium battery graphite, comprising the following steps: carries out imaging analysis to graphite using Raman spectrum imaging technology, obtains the defective data of graphite；Using high-purity silicon powder as standard specimen, 002 peak of test gained graphite is calibrated, degree of graphitization is calculated by 002 interplanar distance d002 after calibration indirectly；Graphite is assembled into button electricity or soft-package battery, uses electrochemical workstation to apply situation of change of the voltage/current as disturbing signal to obtain system with disturbance, to analyze the parameter of graphite assembly system；Graphite is assembled into finished battery, its normal-temperature circulating performance, low-temperature circulating performance, over-charging, over-discharge performance and security performance are tested in electric performance test cabinet；When gained finished battery is scrapped, or after there is battery capacity diving phenomenon, disassembled to analyze failure cause.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of evaluation sides for cathode of lithium battery graphite
Method.
Background technique
The only way of new-energy automobile industry is one of the emerging industry in China and China marches toward automobile power.Newly
Energy automobile includes pure electric automobile, hybrid vehicle etc..New-energy automobile mainly includes that battery, charging pile, vehicle three are big
Aspect, wherein the most commonly used is lithium ion batteries in terms of battery.
Lithium ion battery primary structure includes anode, cathode, diaphragm, four major part of electrolyte, and negative electrode material is as lithium
The quality of the chief component of ion battery, performance directly influences the performance of lithium ion battery.There are commonly stones for cathode
The non-carbon such as carbon-based materials and alloy, metal and its oxide such as ink, indefiniteness charcoal, Carbon fibe, coke, MCMB, nano carbon tube
Based material.Wherein, electronic conductivity is high, lithium ion diffusion coefficient is big, layer structure volume before and after embedding lithium due to having for graphite
Change the high advantages such as low with intercalation potential of small, embedding lithium capacity, becomes the commercial Li-ion battery negative electrode material of current mainstream.
There are many characterizing methods of negative electrode material and lithium battery, for example the superficial phenomenon analysis of negative electrode material can be used
SEM and TEM is for being imaged；Also molecular vibration spectrum such as Raman can be used, molecular vibration information is also provided；The electricity of lithium battery
Performance standard is even more multiplicity, such as safety test (puncture, toast, overcharging), normal temperature circulation, life test etc..In design battery core
When, it is necessary to choose suitable positive and negative electrode material, and when screening cathode graphite, graphite be divided into artificial graphite, natural graphite or
The two different proportion mixes, it is therefore desirable to carry out overall merit point by performance of the multinomial test analysis to cathode graphite
Analysis, to determine its application and to judge its service life.Current all kinds of test method fish mesh mix, not architectonical, this
It proposes that a system, orderly method carry out overall merit to it in patent, mainly covers microstructured test and small battery core electricity
The electric performance test in pond.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of evaluation sides for cathode of lithium battery graphite
Method shows evidence-based to the evaluation and test of graphite more system, orderly from microstructure to macroscopical electrical property, and method accurately may be used
It leans on, evaluation method is simple and easy, easy to spread.
A kind of evaluation method for cathode of lithium battery graphite proposed by the present invention, comprising the following steps:
(1) imaging analysis is carried out to graphite using Raman spectrum imaging technology, obtains the defective data of graphite；
(2) 002 peak of test gained graphite is calibrated as standard specimen using high-purity silicon powder, it is brilliant by 002 after calibration
Degree of graphitization is calculated in interplanar distance d002 indirectly；
(3) graphite is assembled into button electricity or soft-package battery, voltage/current is applied as disturbance letter using electrochemical workstation
Number to obtain system with the situation of change of disturbance, to analyze the parameter of graphite assembly system；
The parameter of graphite assembly system specifically: impedance, CV circulation, transference number of ions etc.；
(4) graphite is assembled into finished battery, its normal-temperature circulating performance, low-temperature circulating is tested in electric performance test cabinet
Energy, over-charging, over-discharge performance and security performance (such as puncture, toast, falling)；When gained finished battery is scrapped, or go out
After existing battery capacity diving phenomenon, disassembled to analyze failure cause.
Preferably, in the Raman spectrum imaging technology of step (1), test point is at least 400, using the numerical value of ID/IG
Distribution is with evaluating graphite defect.In the Raman spectrum of graphite, the peak G belongs to the stretching vibration of sp2 carbon atom, is the feature of graphite
Peak, the peak D is lower with the intensity rate at the peak G, and the fault of construction in graphite is fewer, and degree of graphitization is higher.
Preferably, in step (2), using the angle-data at 111 peak of 002 peak of gained graphite and silicon, with reference to Bragg equation
That is 2dsin θ=λ calculates 002 surface layer spacing of graphite as follows:
D002=λ/2sin [(28.442- θ 1+ θ 2)/2]；
Wherein, d002 is 002 surface layer spacing of graphite, and unit isThe wave of 1 spectral line of K α in the X-ray that λ launches for copper target
Long, numerical value isθ 1 is the 2 θ angles at 111 peak of silicon；θ 2 is the 2 θ angles at 002 peak of graphite；28.442 being silicon 111
The internal standard angle of crystal face；
Calculate degree of graphitization as follows again:
G=(3.44-d002)/(3.44-3.354) × 100%；
Wherein, g is degree of graphitization；3.44 be the interlamellar spacing of the unordered overlapping of graphite, and unit isD002 is above-mentioned gained stone
Black 002 surface layer spacing, unit are3.354 interlamellar spacings orderly overlapped for graphite, unit are
Degree of graphitization is to measure charcoal element substance to pass through structural rearrangement, the close journey for improving graphite of crystal from amorphous carbon
Degree.When graphite is as lithium ion battery negative material, this index parameter of degree of graphitization has directiveness in battery production
Meaning.
Preferably, in the first Zhou Xunhuan of step (3), lithium ion Ying Xiancong lithium piece is embedded in graphite, therefore graphite assembly system
It should first carry out bearing and sweep, then just be swept.
Preferably, in step (4), it is end-of-life that battery capacity, which is down to 80%,.
Preferably, in step (4), further includes: the first effect of graphite, gram volume.
Preferably, in step (4), battery capacity diving phenomenon is that battery capacity capacity declines to a great extent.
Compared with prior art, a kind of evaluation method for cathode of lithium battery graphite provided by the invention, by drawing
Defect analysis, XRD internal standard analysis degree of graphitization, electrochemical workstation analysis impedance and the cyclic reversibility of graceful light spectrum image-forming, meter
Calculate lithium ion transference number；Its high rate performance, high-temperature behavior etc. are tested using electric performance test cabinet, calculates its first effect, gram volume etc.,
Above-mentioned evaluation method shows evidence-based, side from microstructure to macroscopical electrical property to the evaluation and test of graphite more system, orderly
Method is accurate and reliable, evaluation method is simple and easy, easy to spread.
Detailed description of the invention
Fig. 1 is the distributed number schematic diagram of the ID/IG of sample 3 and sample 18 in the embodiment of the present invention.
Fig. 2 is that degree of graphitization tests spectrogram in the embodiment of the present invention.
Fig. 3 is the impedance EIS curve graph of button electricity or soft-package battery in step of the embodiment of the present invention (3).
Fig. 4 is the cyclic voltammetric CV curve graph of button electricity or soft-package battery in step of the embodiment of the present invention (3).
Fig. 5 is the capacity attenuation figure of finished battery in step of the embodiment of the present invention (4).
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment
A kind of evaluation method for cathode of lithium battery graphite, comprising the following steps:
(1) graphite is tabletted, spectrum is carried out to sample by XYZ three-dimensional automatic adjustment platform on Raman spectrometer
Imaging acquisition is located at 1582cm since the Raman spectrum of graphite in graphite-structure is there are two main Raman peaks-1The peak G at place
Be located at 1330cm-1The peak D at place；
As shown in Figure 1, the distributed number schematic diagram of the ID/IG of numbered samples 3 and numbered samples 18, as can be seen from Figure
The ID/IG of sample 3 disperses than Distribution value, illustrates that sample homogeneity is poor；And the ID/IG of sample 18 is said than Distribution value Relatively centralized
Its bright homogeneity is relatively preferable；The ID/IG ratio of the discovery of the ID/IG ratio of comparative sample 3 and sample 18, sample 18 is concentrated
It is distributed in 0.1 or so, and the ID/IG ratio of sample 18 is distributed between 0.2-0.8, greater than the ID/IG ratio of sample 18, is said
The defect of bright sample 3 is more than sample 18；
(2) high-purity silicon powder for choosing 325 mesh, it is pressed graphite (C) with graphite sample: silicon powder (Si) is 7:3 with mass ratio
Mixing；Mixed sample powder addition hyaloid sample platform is sprawled uniformly as far as possible, and using sheet glass by it by flattening；It is put into X
X ray diffractometer x measures；
As shown in Fig. 2, degree of graphitization detection is carried out to the China fir China fir graphite that lot number is CP7-H15-170303, in XRD data
2 θ angle numbers at middle 002 peak for reading graphite and at 111 peaks of silicon, with reference to Bragg equation (2dsin θ=λ), by following public affairs
Formula calculates 002 surface layer spacing of graphite:
D002=λ/2sin [(28.442- θ 1+ θ 2)/2]；
Wherein, d002 is 002 surface layer spacing of graphite, and unit isThe wave of 1 spectral line of K α in the X-ray that λ launches for copper target
Long, numerical value isθ 1 is the 2 θ angles at 111 peak of silicon；θ 2 is the 2 θ angles at 002 peak of graphite；28.442 being silicon 111
The internal standard angle of crystal face；
Calculate degree of graphitization as follows again:
G=(3.44-d002)/(3.44-3.354) × 100%；
Wherein, g is degree of graphitization；3.44 be the interlamellar spacing of the unordered overlapping of graphite, and unit isD002 is above-mentioned gained stone
Black 002 surface layer spacing, unit are3.354 interlamellar spacings orderly overlapped for graphite, unit are
It brings above-mentioned formula into be calculated, obtaining degree of graphitization result is 93.02%；
(3) preparation of samples is carried out according to the conjunction slurry ratio of cathode graphite, wherein graphite: conductive black SP: carboxymethyl cellulose
Element: SBR emulsion=95.5:1.5:1.5:1.5 first takes carboxymethyl cellulose to be added into water and carries out gluing 2-3h, then plus
Enter graphite and conductive black SP continues to stir 2h, is subsequently added into SBR emulsion stirring 1h and then is coated, dries, roll-in
Etc. programs, be finally assembling to button electricity or soft-package battery；
Button electricity or soft-package battery are put into electromagnetic shielding box, and by working electrode and electrode is connected to starts to test on tab
Impedance EIS and cyclic voltammetric CV curve；
EIS low frequency range is that lithium ion spreads corresponding impedance, can be used for evaluating diffusion coefficient of the lithium ion in graphite；
CV can also be used for evaluation lithium ion diffusion coefficient, can be used for the property of electrode reaction, mechanism and Kinetics parameters of electrode processes
Research method, this method coordination electrode potential are repeatedly scanned at any time with triangular waveform is one or many with different rates, electricity
Gesture range is to make that different reduction and oxidation reaction, and record current-potential curve can alternately occur on electrode；
As shown in figure 4, lithium ion Ying Xiancong lithium piece is embedded in graphite when graphite half-cell CV is recycled for the first time, therefore should first be born
It sweeps, then is just swept；Lithium ion first can form SEI film in graphite surface before being embedded in graphite, be used to form the lithium of SEI film from
Son can not it is subsequent just sweep when return to lithium piece cathode, to cause graphite half-cell discharge capacity > initial charge capacity for the first time；
In addition, the diffusion coefficient of lithium ion in the material can also be tested by CV method, thus the high rate performance of evaluating graphite
And security performance.
(4) graphite is assembled into finished battery according to corresponding technique, and is recycled in test cabinet, finished battery capacity
Decay pattern is as shown in Figure 5.
To sum up, the present invention analyzes degree of graphitization, electrochemistry work by the defect analysis to Raman spectrum imaging, XRD internal standard
Make station analysis impedance and cyclic reversibility, also calculates lithium ion transference number；Its high rate performance, height are tested using electric performance test cabinet
Warm nature can wait, and calculate its first effect, gram volume etc., and above-mentioned evaluation method is to the evaluation and test of graphite more system, orderly, from microstructure
Evidence-based to the performance of macroscopical electrical property, method is accurate and reliable, evaluation method is simple and easy, easy to spread.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of evaluation method for cathode of lithium battery graphite, which comprises the following steps:
(1) imaging analysis is carried out to graphite using Raman spectrum imaging technology, obtains the defective data of graphite；
(2) 002 peak of test gained graphite is calibrated, 002 interplanar after calibration is passed through as standard specimen using high-purity silicon powder
Degree of graphitization is calculated indirectly away from d002；
(3) by graphite be assembled into button electricity or soft-package battery, use electrochemical workstation apply voltage/current as disturbing signal with
Acquisition system with disturbance situation of change, to analyze the parameter of graphite assembly system；
(4) graphite is assembled into finished battery, tested in electric performance test cabinet its normal-temperature circulating performance, low-temperature circulating performance,
Over-charging, over-discharge performance and security performance；When gained finished battery is scrapped, or after there is battery capacity diving phenomenon, into
Row dismantling is to analyze failure cause.
2. being used for the evaluation method of cathode of lithium battery graphite according to claim 1, which is characterized in that the Raman of step (1)
In spectral imaging technology, test point is at least 400, uses the numeric distribution of ID/IG with evaluating graphite defect.
3. being used for the evaluation method of cathode of lithium battery graphite according to claim 1, which is characterized in that in step (2), use
The angle-data at 111 peak of 002 peak of gained graphite and silicon calculates graphite with reference to Bragg equation, that is, 2dsin θ=λ as follows
002 surface layer spacing:
D002=λ/2sin [(28.442- θ 1+ θ 2)/2]；
Wherein, d002 is 002 surface layer spacing of graphite, and unit isThe wavelength of 1 spectral line of K α in the X-ray that λ launches for copper target, number
Value isθ 1 is the 2 θ angles at 111 peak of silicon；θ 2 is the 2 θ angles at 002 peak of graphite；28.442 be silicon in 111 crystal faces
Internal standard angle；
Calculate degree of graphitization as follows again:
G=(3.44-d002)/(3.44-3.354) × 100%；
Wherein, g is degree of graphitization；3.44 be the interlamellar spacing of the unordered overlapping of graphite, and unit isD002 is above-mentioned gained graphite 002
Surface layer spacing, unit are3.354 interlamellar spacings orderly overlapped for graphite, unit are
4. being used for the evaluation method of cathode of lithium battery graphite according to claim 1, which is characterized in that the head week of step (3)
In circulation, lithium ion Ying Xiancong lithium piece is embedded in graphite, therefore graphite assembly system should be carried out first bearing and be swept, then just be swept.
5. being used for the evaluation method of cathode of lithium battery graphite according to claim 1, which is characterized in that in step (4), battery
It is end-of-life that capacity, which is down to 80%,.
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| CN110726712A (en) * | 2019-11-01 | 2020-01-24 | 湖南航天天麓新材料检测有限责任公司 | Method for measuring graphitization degree of non-uniform graphite |
| CN111551572A (en) * | 2020-05-21 | 2020-08-18 | 安徽科达新材料有限公司 | Method for rapidly evaluating cycle performance of graphite material in battery |
| CN116609367A (en) * | 2023-07-19 | 2023-08-18 | 天津力神电池股份有限公司 | Selection method and application of target silicon anode material |
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