CN109596597A - A kind of method of evaluating graphite surface coating modification - Google Patents
A kind of method of evaluating graphite surface coating modification Download PDFInfo
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- CN109596597A CN109596597A CN201811617797.4A CN201811617797A CN109596597A CN 109596597 A CN109596597 A CN 109596597A CN 201811617797 A CN201811617797 A CN 201811617797A CN 109596597 A CN109596597 A CN 109596597A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
Abstract
This application discloses a kind of methods of evaluating graphite surface coating modification.It specifically discloses a kind of to the clad progress evaluation method through surface coated graphite material, which comprises suppress graphite material sample to be evaluated, acquisition compacted density is 1.5~2.0g/cm3Green compact, the green compact is detected with laser Raman spectrometer；With acquisition Raman image figure.This method is enough with selection graphite surface area, characterization result is intuitive, accuracy is high, representative.In addition, operation of the present invention is simple, detection is quick, there is significant advantage in assessment Graphite Coating aspect of performance.
Description
Technical field
The present invention relates to the modified fields of graphite surface, and in particular to the evaluation method modified to Graphite Coating.
Background technique
Graphite is the negative electrode material applied to lithium ion battery, with oxidation-reduction potential is low, conductivity is high, structure is steady
The significant advantages such as fixed, cheap and resourceful are the most common selections of current lithium ion battery negative material.As lithium from
The graphite material of sub- cell negative electrode material usually carries out surface coating modification.On the one hand, after surface coating modification, be conducive in stone
Black surface forms fine and close SEI film, is beneficial to prevent the last decomposition of electrolyte, prevents the total insertion of solvent molecule in electrolyte broken
Bad graphite platelet structure；On the other hand insertion, the abjection rate that lithium ion can be promoted, improve conductivity, the multiplying power of graphite material
The performances such as performance and low temperature charge and discharge., uniformly comprehensively whether the clad of graphite surface have the performance superiority and inferiority of graphite material aobvious
The influence of work.In addition, when carrying out roll-in during preparing negative electrode tab, the degree of adhesion and machine of clad and graphite surface
Tool intensity, affects whether Graphite Coating layer can rupture, or even falls off.Therefore the clad on graphite material surface
Performance superiority and inferiority is also most important to final cathode performance.
It is observed currently, the characterization method that Graphite Coating is modified mainly has by scanning electron microscope (SEM),
Carry out the methods of powder conductivity rate analysis.The shape of graphite surface can be can be visually seen by carrying out observation by scanning electron microscope
Looks, but because this method is excessively microcosmic, only it is observed that minimal amount of sample, thus be not representative, and evaluation criterion takes
Certainly in the subjective judgement of Observation personnel.Powder conductivity rate analytic approach is merely by this one aspect of the electric conductivity of graphite material
Performance carry out Indirect evaluation coating modification effect, there is the non-intuitive problem of characterization.
Therefore, to Graphite Coating situation, there are the need for carrying out intuitive, objective and representational Fast Evaluation means
It asks.
Summary of the invention
In view of this, that the purpose of the present invention is to provide a kind of characterization results is intuitive, accuracy is high and representative
Evaluate the modified method of negative electrode of lithium ion battery Graphite Coating.
According to the present invention, it provides a kind of clad to through surface coated graphite material and carries out evaluation method, it is described
Method includes:
Graphite material sample to be evaluated is suppressed, acquisition compacted density is 1.5~2.0g/cm3Green compact,
The green compact is detected with laser Raman spectrometer；With
Obtain Raman image figure.
In evaluation method of the invention, the compacting of graphite material sample is carried out using tablet press machine.
In traditional Raman spectrum detection, sample to be tested is simply compacted by being placed on glass slide, so that it may be measured.And
Method of the invention is different from traditional Raman spectrum detection, and sample to be tested of the invention uses tablet press machine under pressure
Compacting obtains the green compact with certain compacted density.After compaction treatment, the difference of adhesive force of clad surface etc. will
Further show and is finally reflected in Raman image figure.
In method of the invention, according to the relative intensity otherness and global pattern of different zones pattern in Raman image figure
The otherness of contrast carries out quick interpretation.On the whole, the relative intensity otherness of different zones pattern is smaller, and pattern is whole
The otherness of contrast is smaller, then surface cladding is better；It is on the contrary then poorer.
The Raman image figure obtained from method of the invention can intuitively reflect that graphite material to be measured is surface coated
Situation.In simple terms, pattern (light and shade distribution) uniformity of Raman image figure is (that is, the intensity distribution difference of different zones pattern
Property and global pattern poor contrast it is anisotropic) the surface coated superiority and inferiority of graphite material can be objectively responded, wherein pattern uniformity
More good then surface covering property is better (reference can be made to embodiment 1 described below and Fig. 1).This pattern uniformity with use other
Method, such as SEM, the surface cladding situation observed are consistent.
Method of the invention can carry out quick interpretation according to Raman image figure.Those skilled in the art pass through to intellectual
The material of energy, which carries out a small amount of test, can grasp the pattern of the corresponding Raman image figure of graphite material surface cladding situation, to slap
Hold method of the invention.
According to further embodiment, method of the invention further comprises that at least 300 are chosen in areas imaging
Point, it is preferable that at least 400 points are chosen, it is highly preferred that at least 500 points are chosen, to obtain Raman degree of disorder distribution map or nothing
Sequence degree average value.
Generally speaking, the variation of the Raman degree of disorder is smaller after graphite material compacting, graphite particle different zones or different graphite
Degree of disorder difference is smaller between particle, and the surface coated performance of graphite material is better.For example, graphite material sample compacting front and back
Average unordered angle value variable quantity is preferably smaller than equal to 0.15, and more preferably less than or equal to 0.10, particularly preferably less than it is equal to 0.05.
According to another embodiment, the standard deviation of degree of disorder distribution also can be used as one of evaluation criterion.For example, the degree of disorder
The standard deviation of distribution is preferably smaller than equal to 0.10, and more preferably less than or equal to 0.08.
More accurate and comparable measured value can be obtained by the measurement of the degree of disorder, to more connect to cladding quality
Close sample is further distinguished.
Evaluation method according to the present invention, wherein choosing and swashing when being detected with laser Raman spectrometer to the green compact
The testing conditions of light Raman spectrometer are to ensure in 1350cm-1、1580cm-1Nearby there is peak.Wherein 1350cm-1Corresponding to carbon D
Peak, and 1580cm-1Corresponding to the peak carbon G.
Evaluation method according to the present invention, the method can further comprise to repressed graphite material sample to be evaluated
Product are observed with scanning electron microscope.The observation of scanning electron microscope is for further intuitive evaluation.
Since the sample size of scanning electron microscope observation is few, do not have representativeness, therefore Raman can used above
More intuitive SEM photograph is further looked on the basis of image evaluation, as auxiliary evaluation.
The negative electrode material being used as in lithium ion battery through surface coated graphite material that the present invention is evaluated.
The present invention is enough with selection graphite surface area, characterization result is intuitive, accuracy is high, representative.In addition,
Operation of the present invention is simple, detection is quick, and the cladding of graphite surface can be known by the simple interpretation to Raman image figure
Situation has significant advantage in assessment Graphite Coating aspect of performance.
Detailed description of the invention
Fig. 1 is the Raman image figure (b) of the Raman image figure (a) of graphite material A and graphite material B in embodiment 1；
The Raman degree of disorder profiles versus figure that Fig. 2 is graphite material A and graphite material B in embodiment 1；
Fig. 3 is the SEM photograph of graphite material A (a) and graphite material B (b) in embodiment 1；
Fig. 4 is the battery multiplying power discharging property comparison diagram of graphite material A and graphite material B in embodiment 4；
Fig. 5 is the battery multiplying power charging performance comparison diagram of graphite material A and graphite material B in embodiment 4；
Fig. 6 is the battery temperature characteristic test comparative result figure of graphite material A and graphite material B in embodiment 4；
Under the conditions of Fig. 7 is not compacted for graphite material in embodiment 5, the Raman image figure (a) and graphite material of graphite material C
Expect the Raman image figure (b) of D；
Fig. 8 is that graphite material in compacted density is 1.70g/cm in embodiment 53Under the conditions of, the Raman image of graphite material C
Scheme the Raman image figure (b) of (a) and graphite material D；
Fig. 9 is that graphite material in compacted density is 1.85g/cm in embodiment 53Under the conditions of, the Raman image of graphite material C
Scheme the Raman image figure (b) of (a) and graphite material D；With
Figure 10 is that graphite material in compacted density is 2.1g/cm in embodiment 53Under the conditions of, the Raman image of graphite material C
Scheme the Raman image figure (b) of (a) and graphite material D.
Specific embodiment
Below in conjunction with embodiment of the present invention and attached drawing, to the technical solution in embodiment of the present invention carry out it is clear,
It is fully described by, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole implementation
Mode.Based on the embodiment in the present invention, those of ordinary skill in the art are obtained without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
The detection of 1 Raman spectrum of embodiment
Taking graphite material A, (surface coating modification artificial graphite, it is 1.5% that surface, which coats carbon left, and gram volume is about
355mAh/g, coulombic efficiency is about that 93%) (surface coating modification artificial graphite, surface coat carbon left with graphite material B for the first time
It is 1.5%, gram volume is about 355mAh/g, and coulombic efficiency is about 93%) each 1.5 ± 0.005g for the first time, in tablet press machine Carver,
Green compact is pressed into 4350 models.Calculate separately to obtain the close of the green compact of two kinds of materials according to mould sleeve area and green compact height
Degree, respectively 1.75g/cm3And 1.75g/cm3。
Green compact is respectively placed on glass slide, in Raman spectrometer (HORRIBA, Lab RAM HR Evolution) into
Row detection.Testing conditions are set, it can be in 1350cm to meet acquisition normal Raman single spectrum-1、1580cm-1There is peak in left and right.
Imaging spectral is obtained in 60 × 60 μ ms after choosing testing conditions, is obtained imaging results and is seen Fig. 1.Wherein Fig. 1 (a) is shown
It is derived from the Raman image figure of the sample of graphite material A, and Fig. 1 (b) shows the Raman image for being derived from the sample of graphite material B
Figure.From two figures it will be clear that Raman image figure shows pattern distribution and the relative mistake of contrast of different zones
Anisotropic (light and shade distributing homogeneities different in other words), pattern contrast's distribution of the different zones of Fig. 1 (b) and contrast difference
Property it is smaller, uniformity is considerably better than Fig. 1 (a), this illustrates in the present embodiment that graphite A material changes with respect to graphite B material surface cladding
Property is poor.
The measurement of the 2 Raman spectrum degree of disorder of embodiment
400 points are further uniformly chosen in each areas imaging in embodiment 1, obtain Raman degree of disorder profiles versus
Figure, Fig. 2 shows the degree of disorder distribution histograms of graphite material A, B.From Figure 2 it can be seen that compared to graphite material B, graphite material A
The degree of disorder distribution it is narrower, unordered angle value is smaller.
In addition, being computed, the degree of disorder average value of graphite material A, B are respectively 0.6742,0.4097, standard deviation difference
It is 0.1160,0.0521.
The unordered angle value of graphite material A is bigger with respect to graphite material B and distribution is more discrete, result that Fig. 2 is presented and Fig. 1 at
As result is corresponding.
Judge that the surface cladding situation of graphite material B should be significantly better than graphite material A from the detection of the above Raman spectrum.
The detection of 3 scanning electron microscope of embodiment
SEM (Japan Electronics, JSM-7610F Plus) table is carried out to A, B graphite material after compaction moulding in embodiment 1
Sign, SEM photograph result are as shown in Figure 3.By particle surface after Fig. 3 (a) visible graphite material A compacting it is visible it is obvious it is damaged, fall off
Carbon-coating, and by the visible graphite material B particle surface smooth pieces of Fig. 3 (b).The provable evaluating graphite of the present invention of SEM testing result
The method conclusion obtained and the result that SEM is observed of surface cladding situation are consistent.
4 material electric performance test of embodiment
Cathode main material is done with A, B graphite material in embodiment 1 and assembles lithium ion battery respectively, and wherein cathode proportion is stone
Ink: (SP is conductive black to SP:SBR:CMC=96.4:0.6:1.8:1.2, and SBR is butadiene-styrene rubber, and CMC is carboxymethyl cellulose
Element), positive main material is nickel-cobalt-manganternary ternary anode material.Lithium ion battery in addition to A, B graphite is respectively adopted and does cathode main material, other
Component and all fabrication process conditions are consistent.Lithium ion battery manufacture after the completion of test battery hair multiplying power discharging property, times
Rate charging performance and battery temperature characteristic.
Multiplying power discharging tests main work step are as follows: and 1C constant-current charge to 4.2V ends, and constant pressure 4.2V charges to 0.05C cut-off,
0.33C constant-current discharge is to 2.8V；1C constant-current charge ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 0.5C constant-current discharge
To 2.8V；1C constant-current charge ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 1.0C constant-current discharge to 2.8V；1C constant current
4.2V cut-off is charged to, constant pressure 4.2V charges to 0.05C cut-off, 2.0 constant-current discharges to 2.8V；1C constant-current charge is to 4.2V sections
Only, constant pressure 4.2V charges to 0.05C cut-off, 3.0C constant-current discharge to 2.8V；1C constant-current charge ends to 4.2V, and constant pressure 4.2V fills
Electricity to 0.05C end, 5.0C constant-current discharge to 2.8V.
The main work step of multiplying power charging measurement are as follows: 0.33C constant-current charge to 4.2V ends, and constant pressure 4.2V charges to 0.05C and cuts
Only, 1.0C constant-current discharge is to 2.8V；0.5C constant-current charge ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 1.0C constant current
It is discharged to 2.8V；1.0C constant-current charge ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 1.0C constant-current discharge to 2.8V；
2.0C constant-current charge ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 1.0C constant-current discharge to 2.8V；3.0C constant current is filled
Electricity ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 1.0C constant-current discharge to 2.8V.
Temperature characterisitic mainly tests work step are as follows: 25 DEG C, 1C constant-current charge to 4.2V ends, and constant pressure 4.2V charges to 0.05C
Cut-off, 1C constant-current discharge to 2.8V；45 DEG C, 1C constant-current charge to 4.2V ends, and constant pressure 4.2V charges to 0.05C cut-off, and 1C is permanent
Stream is discharged to 2.8V；10 DEG C, 1C constant-current charge to 4.2V ends, and constant pressure 4.2V charges to 0.05C cut-off, and 1C constant-current discharge is extremely
2.8V；0 DEG C, 1C constant-current charge to 4.2V ends, and constant pressure 4.2V charges to 0.05C cut-off, 1C constant-current discharge to 2.8V；- 10 DEG C,
1C constant-current charge ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 1C constant-current discharge to 2.8V；- 20 DEG C, 1C constant current is filled
Electricity ends to 4.2V, and constant pressure 4.2V charges to 0.05C cut-off, 1C constant-current discharge to 2.8V.
Battery multiplying power discharging property, multiplying power charging performance and battery temperature characteristic test result are respectively such as Fig. 4, Fig. 5, Fig. 6
It is shown.As shown in figure 4, the capacity retention ratio of graphite material B is better than graphite material A, while graphite material under different discharge-rates
Expect that the surface temperature rise of B battery is relatively lower.As shown in figure 5, the constant current of graphite material B is filled with than excellent under different rate of charge
In graphite material A, while the surface temperature rise of graphite material B battery is relatively lower.As shown in fig. 6, being transferred in different temperatures environment
The capacity retention ratio of electricity, graphite material B is better than graphite material A, while the surface temperature rise of graphite material B battery is relatively lower.By
This visible multiplying power discharging property, multiplying power charging performance and temperature property test, the capacity retention ratio of graphite material B, constant current are filled with
Than being better than graphite material A, and temperature rise is relatively lower.Especially under big multiplying power, the more harsh test condition of low temperature, stone
The temperature rise advantage relative material A of ink material B becomes apparent.
Implement influence of the 5 different compacted densities to detection
Taking graphite material C, (surface coating modification artificial graphite, it is 1.5% that surface, which coats carbon left, and gram volume is about
355mAh/g, coulombic efficiency is about that 93%) (surface coating modification artificial graphite, surface coat carbon left with graphite material D for the first time
It is 1.5%, gram volume is about 355mAh/g, and coulombic efficiency is about 93%) each four groups for the first time, and every group of quality is 1.5 ± 0.005g,
Each group is respectively labeled as tetra- groups of a, b, c and d according to different compaction treatments, wherein a group powder is not compacted, b, c and d component
Green compact is not pressed into tablet press machine (Carver, 4350 models), presses real-time control green compact height, b, c, d group powder are pressed respectively
In fact to compacted density 1.70g/cm3、1.85g/cm3And 2.1g/cm3.Graphite C, the powder a of D material, green compact b, c, d are set respectively
In on glass slide, detected in Raman spectrometer (HORRIBA, Lab RAM HR Evolution).Set testing conditions,
It can be in 1350cm to meet acquisition normal Raman single spectrum-1、1580cm-1There is peak in left and right.Choose after testing conditions 60 ×
Imaging spectral is obtained in 60 μ ms, is obtained imaging results and is seen Fig. 7, Fig. 8, Fig. 9 and Figure 10.
Fig. 7 (a), (b), which are respectively illustrated, to be derived from graphite material C, D and does not do the Raman image figure being compacted, and two kinds as the result is shown
Material light and shade distributing homogeneity is all preferable, the pattern distribution of different zones and contrast no significant difference, thus (a), (b) Raman
Image illustrates that two samples in the case where not being compacted, cannot obtain the cladding qualitative difference of two kinds of materials.
Fig. 8 (a), (b), which are respectively illustrated, is derived from graphite material C, D in compacted density 1.70g/cm3Under Raman image figure,
As a result the relative mistake of the pattern distribution evident from material C out, D Raman image figure different zones and contrast is anisotropic (in other words
Different light and shade distributing homogeneities), pattern contrast's distribution of the different zones of Fig. 8 (a) and the poor contrast opposite sex are smaller, uniformly
Property is considerably better than Fig. 8 (b), this illustrates that graphite C material is preferable with respect to graphite D material surface coating modification in the present embodiment.
Fig. 9 (a), (b), which are respectively illustrated, is derived from graphite material C, D in compacted density 1.85g/cm3Under Raman image figure.
Fig. 9 (a), (b) are respectively with respect to (a), pattern contrast's distribution of (b), the poor contrast opposite sex and uniformity hair in Fig. 8 as the result is shown
Raw certain deterioration.It is illustrated according to Fig. 9 (a), (b), also this it appears that the pattern point of material C, D Raman image figure different zones
Cloth and the relative mistake of contrast are anisotropic, and wherein pattern contrast's distribution of the different zones of Fig. 9 (a) and the poor contrast opposite sex be more
Small, uniformity is considerably better than Fig. 9 (b), illustrates that graphite C material is preferable with respect to graphite D material surface coating modification in the present embodiment,
This is consistent with the conclusion that Fig. 8 (a), (b) are obtained.
Figure 10 (a), (b), which are respectively illustrated, is derived from graphite material C, D in compacted density 2.1g/cm3Under Raman image figure.
Figure 10 is obviously dimmed with respect to the pattern in Fig. 7, Fig. 8 and Fig. 9 respectively as the result is shown, and contrast distribution, poor contrast are anisotropic and equal
Obvious deterioration occurs for even property.It is illustrated according to Figure 10 (a), (b), as the result is shown the test structure light and shade distributing homogeneity of two kinds of materials
It is all very poor, the pattern distribution of different zones and contrast no significant difference.Illustrate under excessive compacting, graphite particle has occurred
Breakage, a large amount of defects generate, and thus illustrate sample in 2.1g/cm3In the case where compacting, the cladding of two kinds of materials can not be obtained
Qualitative difference.
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the scope of the invention, it is all
Under inventive concept of the invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/transport indirectly
It is included in used in other related technical areas in scope of patent protection of the invention.
Claims (7)
1. a kind of carry out evaluation method to the clad through surface coated graphite material, which comprises
Graphite material sample to be evaluated is suppressed, acquisition compacted density is 1.5~2.0g/cm3Green compact,
The green compact is detected with laser Raman spectrometer；With
Obtain Raman image figure.
2. evaluation method according to claim 1, wherein the compacting is carried out with tablet press machine.
3. evaluation method according to claim 1, wherein according to the relatively strong of the Raman image figure different zones pattern
The poor contrast opposite sex for spending otherness and the Raman image figure global pattern carries out quick interpretation.
4. evaluation method according to claim 1, wherein the method further includes: it chooses at least in areas imaging
300 points, it is preferable that at least 400 points are chosen, it is highly preferred that at least 500 points are chosen, to obtain the distribution of the Raman degree of disorder
Figure or degree of disorder average value.
5. evaluation method according to claim 1, wherein choosing the testing conditions of laser Raman spectrometer to ensure
1350cm-1、1580cm-1Nearby there is peak.
6. evaluation method according to claim 1, wherein the method further includes: to repressed stone to be evaluated
Ink material sample is observed with scanning electron microscope.
7. evaluation method according to claim 1, wherein described be used as lithium ion battery through surface coated graphite material
In negative electrode material.
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| CN113655392A (en) * | 2021-08-02 | 2021-11-16 | 合肥国轩高科动力能源有限公司 | Method for judging surface coating uniformity of electrode material |
| CN116564405A (en) * | 2023-04-19 | 2023-08-08 | 江苏先声医学诊断有限公司 | Average-disorder-based genome sequencing mutation site filtering method |
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| CN113655392A (en) * | 2021-08-02 | 2021-11-16 | 合肥国轩高科动力能源有限公司 | Method for judging surface coating uniformity of electrode material |
| CN116564405A (en) * | 2023-04-19 | 2023-08-08 | 江苏先声医学诊断有限公司 | Average-disorder-based genome sequencing mutation site filtering method |
| CN116564405B (en) * | 2023-04-19 | 2023-12-15 | 江苏先声医学诊断有限公司 | Average-disorder-based genome sequencing mutation site filtering method |
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