CN109696111A - Test the method and its application of the expansion rate of electrode active material - Google Patents
Test the method and its application of the expansion rate of electrode active material Download PDFInfo
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- CN109696111A CN109696111A CN201811608794.4A CN201811608794A CN109696111A CN 109696111 A CN109696111 A CN 109696111A CN 201811608794 A CN201811608794 A CN 201811608794A CN 109696111 A CN109696111 A CN 109696111A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B5/00—Measuring arrangements characterised by the use of mechanical techniques
- G01B5/30—Measuring arrangements characterised by the use of mechanical techniques for measuring the deformation in a solid, e.g. mechanical strain gauge
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/16—Investigating or analyzing materials by the use of thermal means by investigating thermal coefficient of expansion
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Abstract
The present invention provides the methods of test electrode active material expansion rate, the method for evaluating and testing electrode and battery quality.The method of the test electrode active material expansion rate includes: to provide original electrodes piece, and original electrodes piece includes matrix and the electrode material layer that is arranged on the surface of matrix, and electrode active material and non-active material are contained in electrode material layer；Pressurized treatments are carried out to original electrodes piece, and measure effective original thickness of the electrode material layer in original electrodes piece under pressurised conditions；Original electrodes piece is assembled into battery and battery is made to work the predetermined time, obtains expansion electrode piece；Pressurized treatments are carried out to expansion electrode piece, and measure effective expanded thickness of the electrode material layer in expansion electrode piece under pressurised conditions；Based on effective original thickness and effective expanded thickness, the expansion rate of electrode active material is determined.This method is simple and convenient, and test result eliminates the factor bring error in electrode slice in addition to electrode active material expansion, and accuracy is high, feasibility is good.
Description
Technical field
The present invention relates to field of material technology, and in particular, to tests method, the evaluation and test of the expansion rate of electrode active material
The method of the method and evaluation and test battery quality of electrode quality.
Background technique
In the related art, (such as silica-base material, silicon-carbon are multiple for the electrode active material in the power batteries such as lithium ion battery
Condensation material etc.) expansion rate with higher in use, so as to cause power battery cycle life reduce, security performance
It is poor.Therefore, the expansion rate for accurately testing electrode active material has important meaning for the design and research of power battery
Justice.However, it is still not high for the accuracy of electrode active material expansion rate test at present, and step is many and diverse, poor feasibility.
Thus, the relevant technologies of the expansion rate of existing test electrode active material still have much room for improvement.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention
One purpose be to propose a kind of simple and convenient, test result can exclude in electrode slice in addition to electrode active material expansion because
The method of plain bring error, the expansion rate for the test electrode active material that accuracy is high or feasibility is good.
In one aspect of the invention, the present invention provides a kind of methods of expansion rate for testing electrode active material.Root
According to the embodiment of the present invention, this method comprises: providing original electrodes piece, the original electrodes piece includes matrix and is arranged described
Electrode material layer on the surface of matrix contains electrode active material and non-active material in the electrode material layer；To described
Original electrodes piece carries out pressurized treatments, and measures having for the electrode material layer in the original electrodes piece under pressurised conditions
Imitate original thickness L；The original electrodes piece is assembled into battery and makes the battery work predetermined time, obtains expansion electrode
Piece；Pressurized treatments are carried out to the expansion electrode piece, and measure the electrode in the expansion electrode piece under pressurised conditions
Effective expanded thickness D of material layer；Based on effective original thickness L and effective expanded thickness D, the electrode active is determined
The expansion rate of property material.Inventors have found that this method is simple and convenient, test result is eliminated in electrode slice except electrode active material
Factor bring error other than expansion, accuracy is high, feasibility is good.
According to an embodiment of the invention, effective original thickness L through the following steps that measurement: under pressurised conditions
Measure the thickness X of the original electrodes piece；Measure the thickness L of matrix described in the original electrodes piece1, the effectively original thickness
Spend L=X-L1。
According to an embodiment of the invention, effective original thickness L through the following steps that measurement: utilize vernier caliper
Measure the first height L of compression mold0；Original electrodes piece sample is put into the inner cavity of the compression mold, and described in utilization
Second height L of compression mold described in vernier caliper measurement2；By the compression mold in a thickness direction to the original electricity
Pole piece sample carries out pressurized treatments, obtains the load-deformation curve of the original electrodes piece sample, and answer according to the stress-
Varied curve determines the inelastic deformation amount L of the electrode material layer3；The original electrodes piece sample is measured using spiral micrometer
Described in matrix thickness L1, effective original thickness L=L2-L1-L0-L3。
According to an embodiment of the invention, effective expanded thickness D through the following steps that measurement: under pressurised conditions
Measure the thickness H of the expansion electrode piece；Measure the thickness D of matrix described in the expansion electrode piece1, effective expansion thickness
Spend D=H-D1。
According to an embodiment of the invention, effective expanded thickness D through the following steps that measurement: utilize vernier caliper
Measure the first height D of compression mold0；Expansion electrode piece sample is put into the inner cavity of the compression mold, and described in utilization
Second height D of compression mold described in vernier caliper measurement2；By the compression mold in a thickness direction to the expansion electricity
Pole piece sample carries out pressurized treatments, obtains the load-deformation curve of the expansion electrode piece sample, and answer according to the stress-
Varied curve determines the inelastic deformation amount D of the electrode material layer3；The expansion electrode piece sample is measured using spiral micrometer
Described in matrix thickness D1, effective expanded thickness D=D2-D1-D0-D3。
According to an embodiment of the invention, the interior chamber size one of the size of the original electrodes piece sample and the compression mold
It causes；The size of the expansion electrode piece sample and the interior chamber size of the compression mold are consistent.
According to an embodiment of the invention, being put into multiple original electricity being stacked in the inner cavity of the compression mold
Pole piece sample or expansion electrode piece sample.
According to an embodiment of the invention, before the expansion electrode piece sample is put into the inner cavity of the compression mold,
Further comprise: pretreated step is carried out to the expansion electrode piece sample.
According to an embodiment of the invention, the original electrodes piece sample or the expansion electrode piece sample are by described
What original electrodes piece or the expansion electrode piece obtained after being punched out, in the original electrodes piece or the expansion electrode piece
Between partially constitute the original electrodes piece sample or the expansion electrode piece sample.
In another aspect of the invention, the present invention provides a kind of methods for evaluating and testing electrode quality.It is according to the present invention
The step of embodiment, this method is tested including the use of expansion rate of the mentioned-above method to the electrode active material.
Inventors have found that this method is simple and convenient, the test result of the expansion rate of electrode active material is eliminated in electrode slice except electricity
Factor bring error other than the expansion of pole active material, accuracy is high, feasibility is good, and has mentioned-above test electrode
All feature and advantage of the method for the expansion rate of active material, no longer excessively repeat herein.
In an additional aspect of the present invention, the present invention provides a kind of methods for evaluating and testing battery quality.It is according to the present invention
The step of embodiment, this method is evaluated and tested including the use of quality of the mentioned-above method to the electrode.Inventors have found that
This method is simple and convenient, and accuracy is high, feasibility is good, and all features of the method with mentioned-above evaluation and test electrode quality
And advantage, it no longer excessively repeats herein.
Detailed description of the invention
Fig. 1 shows the process signal of the method for the expansion rate of the test electrode active material of one embodiment of the invention
Figure.
Fig. 2 shows the original electrodes piece of one embodiment of the invention or the schematic diagram of the section structure of expansion electrode piece.
Fig. 3 shows the flow diagram of the effective original thickness L of measurement of one embodiment of the invention.
Fig. 4 shows the flow diagram of the effective original thickness L of measurement of another embodiment of the present invention.
Fig. 5 a and Fig. 5 b show the effective original thickness L's of measurement or the effective expanded thickness D of measurement of the embodiment of the present invention
Flow diagram.
Fig. 6 shows that the stress-of original electrodes piece sample and expansion electrode piece sample in one embodiment of the invention is answered
Varied curve.
Fig. 7 shows original electrodes piece or expansion electrode piece and original electrodes piece sample or the expansion of the embodiment of the present invention
The planar structure schematic diagram of electrode slice sample.
Fig. 8 shows the flow diagram of the effective expanded thickness D of measurement of one embodiment of the invention.
Fig. 9 shows the flow diagram of the effective expanded thickness D of measurement of another embodiment of the present invention.
Figure 10 shows the flow diagram of the effective expanded thickness D of measurement of another embodiment of the invention.
Appended drawing reference:
10: original electrodes piece, expansion electrode piece 11: matrix 12: electrode material layer 20: original electrodes piece sample, expansion
Electrode slice sample 100: compression mold 110: ontology 120: pressure unit 130: inner cavity
Specific embodiment
The embodiment of the present invention is described below in detail.The embodiments described below is exemplary, and is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Particular technique or condition are not specified in embodiment, according to text in the art
It offers described technology or conditions or is carried out according to product description.Reagents or instruments used without specified manufacturer,
For can be with conventional products that are commercially available.
The present invention is the following discovery based on inventor and completes:
In the related art, electrode slice be assembled into battery and in use, electrode active material therein in use
Expansion rate with higher, cycle life reduction, the security performance that will lead to battery are poor.Therefore, electrode active is accurately tested
Property material expansion rate for power battery design and research it is meaningful.However, those skilled in the art are known, before removing
Other than electrode active material described in face, inevitably can also have conductive agent (such as conductive black) in electrode material layer
With the non-active materials such as binder (such as polytetrafluoroethylene (PTFE)).And it is current in the related technology, test electrode active material
Expansion rate when, there is no in view of the influence of conductive agent and binder for test result in electrode material layer.However, invention
People has found that conductive agent and binder test expansion rate in electrode material layer after a large amount of careful investigations and experimental verification
As a result error is that can not ignore.
In order to keep test result of the invention more accurate, further, inventor is also observantly noticed in electrode
When piece is disassembled from battery, since electrode slice without charge and discharge cycles (namely original electrodes piece herein) and passes through
After charge and discharge cycles (namely expansion electrode piece herein), the type of electrode active material is different in electrode material layer, fills
Electrode active material before discharge cycles in electrode material layer by charge and discharge cycles, electrode reaction occurs after, meeting
It chemically reacts.Therefore, the electrode active material in charge and discharge cycles (i.e. generation electrode reaction) front and back, electrode material layer
Material category is different.After electrode slice on battery is disassembled, electrode material layer can due to stress disappearance and produce
It is born from the expansion of body, since the elasticity modulus of different types of material is different, before and after charge and discharge cycles, the electrode material
Layer loses itself expansion for squeezing and generating due to disassembling from battery, also can be to the expansion rate of electrode active material
Test result brings error.Inventor has found that the error is in test electrode active after largely deep investigation and experimental verification
It is also that cannot ignore when the expansion rate of property material.
Further, inventor is also found before and after electrode slice carries out charge and discharge cycles, on the one hand, due to electrode material
Electrode active material in the bed of material expands, thus can not be formed between the particle and particle of electrode active material more intensive
Accumulation mode, cause the gap between the particle of electrode active material and particle to increase, also can be to the swollen of electrode active material
The test result of swollen rate generates error；On the other hand, after electrode reaction occurs, it also will form one in electrode material layer surface
Layer passivating film (such as SEI film etc.), since the passivating film also has certain thickness, thus also can be to electrode active material
The test result of expansion rate generates certain influence, so as to cause error.
In conclusion the expansion rate test method of electrode active material in the related art do not consider conductive agent and
Binder expansion bring error, electrode material layer generate itself expansion bring error, electrode activity material due to losing to squeeze
Material, which expands, causes the gap in electrode active material between particle and particle to increase bring error and electrode reaction
Product bring error.Inventor conducts in-depth research the method for test electrode active material, is passing through test of many times
It surprisingly finds afterwards, in above-mentioned error source, electrode material layer squeezes itself expansion generated and electrode activity due to losing
Gap in material between particle and particle increases, due to being all from electrode material layer itself, above-mentioned expansion or gap
Increase is very easy to be gone back by compression；In addition, since the elasticity modulus of the product of conductive agent, binder and electrode reaction is remote
Less than electrode active material, thus it is also to be easily compressed that conductive agent, binder and electrode reaction product, which expand,.?
That is inventor has found after largely studying, by when testing the expansion rate of electrode active material, to electrode slice into
Row pressurized treatments can exclude above-mentioned error in the test result of expansion rate so that the accuracy of test result it is high, can
Row is good, and simple, convenient.
Based on this, in one aspect of the invention, the present invention provides a kind of expansion rates for testing electrode active material
Method.According to an embodiment of the invention, referring to Fig.1, this method comprises:
S100: providing original electrodes piece 10, (for structural schematic diagram referring to Fig. 2), the original electrodes piece 10 includes 11 He of matrix
Electrode material layer 12 on the surface of described matrix is set, electrode active material and non-live is contained in the electrode material layer 12
Property material.
According to an embodiment of the invention, the original electrodes piece 10 refers to without impregnating in the electrolytic solution and without charge and discharge
The electrode slice of circulation, source are not particularly restricted, such as can be the electrode slice that direct self-electrode piece manufacturer buys, as long as
It did not impregnated in the electrolytic solution and without charge and discharge cycles, and can be used as original electrodes piece 10 of the present invention.It tests as a result,
Material source is extensive, is easy to get, it is easy to accomplish industrialization.
According to an embodiment of the invention, the electrode material layer 12 in the original electrodes piece 10 both can be set in matrix 11
A surface on (structural schematic diagram referring to Fig. 2), also can be set on two surfaces of matrix 11.Test material as a result,
It is from a wealth of sources, be easy to get, it is easy to accomplish industrialization.
According to an embodiment of the invention, the material of matrix 11 can be the material of matrix in conventional electrodes piece, such as can be with
It is sheet metal etc..In some embodiments of the invention, the material of matrix 11 can be aluminium foil or copper foil.It tests as a result,
Material source is extensive, is easy to get, it is easy to accomplish industrialization.
S200: pressurized treatments (structural schematic diagram reference Fig. 2) is carried out to the original electrodes piece 10, and under pressurised conditions
Measure effective original thickness L of the electrode material layer 12 in the original electrodes piece 10.
According to an embodiment of the invention, the technological parameter of the pressurized treatments is not particularly limited, as long as previously mentioned, plus
Pressure processing enables to expansion or increase from above-mentioned error to be compressed, and not for pressure of pressurized treatments etc.
It is particularly limited.
According to an embodiment of the invention, it should be noted that effective original thickness L refer to be discharged it is described herein
Error after, be infinitely close to the thickness of electrode active material actual thickness in electrode material layer 12.It is preceding to have addressed, to swollen
When swollen rate is tested, the only expansion of electrode active material is meaningful for the research and development and design of electrode.Therefore, in step
In rapid S200, which refers to the thickness of electrode active material in electrode material layer 12, is measuring original electrodes
In piece 10 after the thickness of the electrode active material of electrode material layer 12, it may be implemented directly to calculate the swollen of the electrode active material
Swollen rate, and accuracy is high, feasibility is good.
In some embodiments of the invention, referring to Fig. 2 and Fig. 3, effective original thickness L is through the following steps that survey
Amount:
S210: the thickness X of the original electrodes piece 10 is measured under pressurised conditions.
According to an embodiment of the invention, the thickness X of original electrodes piece 10 refers to electrode in original electrodes piece 10 referring to Fig. 2
The sum of material layer 12 and the thickness of matrix 11, the concrete mode for measuring the thickness X is not particularly limited, as long as meeting the requirements, this
Field technical staff can according to need carry out flexible choice.In some embodiments of the invention, the method for measuring thickness X can
To be to be measured using ruler or be measured using vernier caliper or spiral micrometer etc..It is simple, convenient as a result,
It is easy to industrialization.
S220: the thickness L of matrix described in the original electrodes piece 10 is measured1, effective original thickness L=X-L1。
According to an embodiment of the invention, passing through the thickness L of matrix in measurement original electrodes piece 101, available front institute
The effective original thickness L stated, to eliminate matrix 11 in original electrodes piece 10 for the expansion rate of electrode active material
The influence of test result, by such calculation, when testing the expansion rate, used original electricity when not requiring to test
Pole piece and expansion electrode piece use same matrix, because being brought matrix to expansion rate in last test result
Error deduct.Test material is from a wealth of sources as a result, selection is flexible, it is easy to accomplish industrialization.
In other embodiments of the invention, further, referring to Fig. 4, Fig. 5 a to Fig. 5 b, effective original thickness
L through the following steps that measurement:
S210 ': the first height L of vernier caliper measurement compression mold 100 is utilized0(structural schematic diagram is referring to Fig. 5 a).
According to an embodiment of the invention, the first height L of measurement compression mold 1000Mode can be using vernier calliper
Ruler measures.It is simple, convenient as a result, and accuracy of measurement is higher.
According to an embodiment of the invention, as long as the compression mold 100 can be realized to original electrodes piece pressure i.e.
Can, ontology 110, pressure unit 120 and inner cavity 130 are included at least (structural schematic diagram referring to Fig. 5 a), to realize to original
Electrode slice 10 carries out pressurized treatments.
According to an embodiment of the invention, the specific type of the compression mold 100 is not particularly limited, as long as can be real
The process of existing pressurized treatments, specific type those skilled in the art can carry out flexible choice according to actual needs.At this
In some embodiments of invention, the compression mold 100 can be compression mold used in infrared spectrum analysis.Come as a result,
Source is extensive and the compression mold in infrared spectrum analysis is directly brought use, without the expansion to test electrode active material
The separately fabricated compression mold 100 of rate.
S220 ': the original electrodes piece sample (including electrode material layer 12 and matrix 11) is put into the compression mold
In 100 inner cavity 130, and utilize the second height L of compression mold 100 described in the vernier caliper measurement2(structural schematic diagram
Referring to Fig. 5 b).
According to an embodiment of the invention, measuring the second height L of the compression mold 1002Mode can be using trip
Mark slide calliper rule measure.It is simple, convenient as a result, and accuracy of measurement is higher.
According to an embodiment of the invention, having obtained the first height L of compression mold 100 due in abovementioned steps0And it will
Original electrodes piece sample is put into the second height L of the compression mold 100 after the inner cavity 130 of compression mold 1002, thus may be used
To obtain the thickness of original electrodes piece sample, and it is easy to operate, accuracy is high, it is easy to accomplish industrialization, and convenient for subsequent for original
Beginning electrode slice sample carries out pressurized treatments.
In some embodiments of the invention, the size of the original electrodes piece sample and the compression mold 100 is interior
130 size of chamber is consistent.As a result, due in progress pressurized treatments subsequent to the original electrodes piece sample, the original electrodes piece
Sample can't expand on the direction perpendicular to thickness direction, thus in the thickness progress using original electrodes piece sample
When expansion rate calculates, the accuracy of calculating ensure that, so that this method is further for the accuracy of the test of expansion rate
It improves.
According to an embodiment of the invention, multiple stackings can also be directly placed into the inner cavity 130 of the compression mold 100
The original electrodes piece sample being arranged.As a result, due to being put into multiple original electrodes piece samples being stacked, list is eliminated
A sample for uncertainty brought by measurement result, be put into the inner cavity 130 it is multiple be stacked it is described original
After electrode slice sample, then the measurement of subsequent step is carried out, this method can be made to test the expansion rate of electrode active material
As a result it further increases.
According to an embodiment of the invention, the original electrodes piece sample 20 can be by the original electricity referring to Fig. 7
Pole piece 10 is (it should be noted that since Fig. 7 is that planar structure schematic diagram only shows electricity in the original electrodes piece 10
Pole material layer 12, is not shown matrix) be punched out after obtain, the middle section of the original electrodes piece 10 constitutes described original
Electrode slice sample 20.The thickness of the middle section of original electrodes piece 10 is more uniform as a result, and the thickness expanded after use
Degree is also more uniform, therefore constitutes the original electrodes piece sample 20 using intermediate portion, this method can be made for electricity
The test result of the expansion rate of pole active material further increases.
S230 ': the original electrodes piece sample 20 is carried out at pressurization in a thickness direction by the compression mold 100
Reason obtains the load-deformation curve (referring to Fig. 6) of the original electrodes piece sample 20, and true according to the load-deformation curve
The inelastic deformation amount L of the fixed electrode material layer3。
According to an embodiment of the invention, preceding addressed, in electrode material layer 12, due to the expansion rate of electrode active material
Conductive agent and binder expansion, electrode material layer 12 are due to losing itself expansion, electrode activity that squeeze and generate in test method
Material expansion leads to the thickness of the product of the increase of the gap in electrode active material between particle and particle and electrode reaction
Degree, for electrode active material, is easily compressed.That is, aforementioned swollen, gap increase and thickness
The elasticity modulus of degree is much smaller than the elasticity modulus of electrode active material (it should be noted that, although expansion and gap are theoretically
It is not entity, it will be appreciated by a person skilled in the art that can be considered as expansion and the elasticity modulus in gap zero) here.Cause
And it can be by carrying out pressurized treatments to original electrodes piece to exclude brought by test result of the above-mentioned factor for expansion rate
Error.
According to an embodiment of the invention, expansion, gap increase and the thickness of the product of electrode reaction based on noted earlier
Elasticity modulus be much smaller than the elasticity modulus of electrode active material, thus carried out at pressurization to the original electrodes piece sample 20
When reason, aforementioned swollen, gap increase and the thickness of the product of electrode reaction is inelastic deformation, and electrode active material category
In elastic deformation.So electrode active material is at by pressurization when carrying out pressurized treatments to the original electrodes piece sample
Generation elastic deformation when reason records the load-deformation curve of original electrodes piece sample, has elastically-deformable electrode activity material
The stress and strain of material is in a linear relationship.In addition, according to the stress-strain of Hooke's law and material theory, to stress-strain song
Line carries out linear fit (referring to Fig. 6), obtains the intersection point (i.e. point a and b in Fig. 6) of itself and strain reference axis, line segment oa and line
Section ob is inelastic deformation amount.Thus, when testing original electrodes piece sample, those skilled in the art can be managed
Solution can obtain the inelastic deformation amount L of original electrodes piece sample according to the corresponding relationship between strain and inelastic deformation amount3,
(hereinafter when testing expansion electrode piece sample, expansion electrode piece can be obtained in the length of line segment oa i.e. in corresponding diagram 6
The inelastic deformation amount D of sample3, i.e., the length of the line segment ob in corresponding diagram 6).It obtains as a result, aforementioned in expansion rate test process
In, conductive agent and binder expansion, electrode material layer due to lose squeeze generate itself expansion, electrode active material occur it is swollen
The swollen gap caused in electrode active material between particle and particle increases and the thickness of the product of electrode reaction is for test
As a result brought error.
S240 ': the thickness L of matrix described in the original electrodes piece sample is measured using spiral micrometer1, described effective
Original thickness L=L2-L1-L0-L3。
According to an embodiment of the invention, passing through the thickness L of matrix in measurement original electrodes piece sample1, available front
Effective original thickness L, to eliminate the matrix in original electrodes piece sample for the expansion rate of electrode active material
Test result influence, by such calculation, when testing the expansion rate, do not require test when it is used original
Electrode slice sample and expansion electrode piece sample use same matrix, because in last test result, by matrix to swollen
Error brought by swollen rate deducts.Test material is from a wealth of sources as a result, selection is flexible, it is easy to accomplish industrialization.
According to an embodiment of the invention, obtaining the first height L of compression mold 100 in aforementioned measurement0, in the tabletting mould
The second height L of compression mold 100 after original electrodes piece is put into the inner cavity 130 of tool 1002, electrode material layer non-resilient shape
Variables L3And the thickness L of matrix described in original electrodes piece sample1On the basis of, effective original thickness L=L2-L1-
L0-L3.The thickness for obtaining electrode active material in electrode material layer as a result, the electrode material layer in measuring original electrodes piece
After the thickness of electrode active material, the expansion rate for directly calculating the electrode active material may be implemented, and above-mentioned due to deducting
Factor bring error, therefore accuracy is high, feasibility is good.
According to an embodiment of the invention, after measuring effective original thickness L, this method further include:
S300: the original electrodes piece is assembled into battery and the battery is made to work the predetermined time, obtains expansion electrode
Piece.
According to an embodiment of the invention, making its work predetermined time after the original electrodes piece is assembled into battery
Purpose be expansion electrode piece in order to obtain, thus according to effective expanded thickness L of electrode material layer in the original electrodes piece
The expansion rate of the electrode active material is obtained with effective expanded thickness D of electrode material layer in the expansion electrode piece.
According to an embodiment of the invention, the predetermined time can for conventional batteries work time, if guarantee so that
The expansion electrode piece is that the original electrodes piece occurs to obtain after expansion completely, the specific predetermined time not by
Especially limitation, those skilled in the art no longer can excessively repeat herein according to actual needs into property flexible choice.
S400: pressurized treatments are carried out to the expansion electrode piece, and are measured in the expansion electrode piece under pressurised conditions
The electrode material layer effective expanded thickness D.
According to an embodiment of the invention, carrying out all steps and technique of pressurized treatments to expansion electrode piece, can refer to
The step of carrying out pressurized treatments to original electrodes piece and technique carry out, and no longer excessively repeat herein.
In some embodiments of the invention, referring to Fig. 2 and Fig. 8, the electrode material layer in expansion electrode piece has
Imitate expanded thickness D through the following steps that measurement:
S410: the thickness H of the expansion electrode piece 10 is measured under pressurised conditions.
S420: the thickness D of matrix described in the expansion electrode piece 10 is measured1, effective expanded thickness D=H-D1。
According to an embodiment of the invention, above-mentioned all steps and technique, can refer to (S210 the step of to original electrodes piece
And S220) and technique progress, it no longer excessively repeats herein.
In other embodiments of the invention, further, referring to Fig. 5 a to Fig. 5 b and Fig. 9, effective expanded thickness D
Through the following steps that measurement:
S410 ': the first height D of vernier caliper measurement compression mold 100 is utilized0(structural schematic diagram is referring to Fig. 5 a).
S420 ': the expansion electrode piece sample (including electrode material layer 12 and matrix 11) is put into the compression mold
In 100 inner cavity 130, and utilize the second height D of compression mold 100 described in the vernier caliper measurement2(structural schematic diagram
Referring to Fig. 5 b).
S430 ': the expansion electrode piece sample 20 is carried out at pressurization in a thickness direction by the compression mold 100
Reason obtains the load-deformation curve (referring to Fig. 6) of the expansion electrode piece sample 20, and true according to the load-deformation curve
The inelastic deformation amount D of the fixed electrode material layer3。
S440 ': the thickness D of matrix described in the expansion electrode piece sample is measured using spiral micrometer1, described effective
Original thickness D=D2-D1-L0-D3。
According to an embodiment of the invention, above-mentioned all material, step and technique and rationale, can refer to original
Material, step (S210 ', S220 ', S230 ' and S240 '), technique and the rationale of beginning electrode slice, it is no longer excessive herein
It repeats.
In other embodiments of the invention, referring to Fig.1 0, vernier caliper measurement compression mold is utilized in abovementioned steps
100 the first height D0After (S410 '), the expansion electrode piece sample is put into the inner cavity 130 of the compression mold 100
In, and utilize the second height D of compression mold 100 described in the vernier caliper measurement2Before (S420 '), the step further include:
S450 ': the expansion electrode piece sample is pre-processed.
According to an embodiment of the invention, pre-processing to the expansion electrode piece sample can be specially by the expansion
Electrode slice carries out immersion treatment, so that when being assembled into battery work in front electrode reaction institute occurs for expansion electrode piece sample of going out
The electrolyte drawn, in order to avoid corrosion of the electrolyte for compression mold is caused, to protect compression mold anti-for a long time
It is multiple to use, and make after compression mold long-time Reusability, the accuracy for measuring the electrode active material is still higher.
According to an embodiment of the invention, expansion electrode piece can be immersed in DMC (dimethyl carbonate) by aforementioned immersion treatment
Middle progress, the time of the immersion treatment can be 1min~2min, when carrying out immersion treatment, dew point < -35 DEG C, environment
Temperature can be (25 ± 2) DEG C.In some embodiments of the invention, the time of the immersion treatment can be 1min,
1.2min, 1.4min, 1.6min, 1.8min or 2min etc..Thus, it is possible to more fully remove aforementioned swollen electrode slice institute
The electrolyte drawn, and pretreatment time is shorter, so that the efficiency of the test method is higher.
S500: it is based on effective original thickness L and effective expanded thickness D, determines the electrode active material
Expansion rate.
According to an embodiment of the invention, the expansion rate of the electrode active material is calculated according to the following formula:
Expansion rate η=[(D-L)/L] × 100%, wherein D be mentioned-above expansion electrode piece effective expanded thickness,
L is effective original thickness of mentioned-above original electrodes piece；
Inventor has found after largely studying as a result, by test electrode active material expansion rate when, to electricity
Pole piece carries out pressurized treatments, and conductive agent and binder expansion band in electrode material layer can be excluded in the test result of expansion rate
The error come, electrode material layer generate itself expansion bring error, electrode active material and expand and lead due to losing to squeeze
The gap in electrode active material between particle and particle is caused to increase the product bring mistake of bring error and electrode reaction
Difference, so that the accuracy of test result is high, feasibility is good and simple, convenient.
In another aspect of the invention, the present invention provides a kind of methods for evaluating and testing electrode quality.It is according to the present invention
The step of embodiment, this method is tested including the use of expansion rate of the mentioned-above method to the electrode active material.
Inventors have found that this method is simple and convenient, the test result of the expansion rate of electrode active material is eliminated in electrode slice except electricity
Factor bring error other than the expansion of pole active material, accuracy is high, feasibility is good, and has mentioned-above test electrode
All feature and advantage of the method for the expansion rate of active material, no longer excessively repeat herein.
According to an embodiment of the invention, the electrode both can may be cathode, shape, thickness or table for anode
Surface state etc. is not particularly limited, can be using method of the present invention to electrode active material as long as meeting the requirements
Expansion rate tested, thus realize the quality of the electrode is evaluated and tested.
According to an embodiment of the invention, it will be understood by those skilled in the art that the method for the evaluation and test electrode quality is except packet
It includes other than the step of being tested using the mentioned-above expansion rate to the electrode active material, can also include other steps
Suddenly, it no longer excessively repeats herein.
In an additional aspect of the present invention, the present invention provides a kind of methods for evaluating and testing battery quality.It is according to the present invention
The step of embodiment, this method is evaluated and tested including the use of quality of the mentioned-above method to the electrode.Inventors have found that
This method is simple and convenient, and accuracy is high, feasibility is good, and all features of the method with mentioned-above evaluation and test electrode quality
And advantage, it no longer excessively repeats herein.
According to an embodiment of the invention, it will be understood by those skilled in the art that the battery includes that conventional batteries are had
Other structures, such as electrode, battery diaphragm and electrolyte etc., do not repeating excessively herein.
According to an embodiment of the invention, the type of the battery is unrestricted, and as long as meeting the requirements, those skilled in the art
Can according to need carry out flexible choice, such as can include but is not limited to lithium ion battery etc..
According to an embodiment of the invention, the purposes of the battery is not particularly limited, and as long as meeting the requirements, art technology
Personnel can according to need carry out flexible choice, such as may include for electric car.
According to an embodiment of the invention, it will be understood by those skilled in the art that the method for the evaluation and test battery quality is except packet
It includes other than mentioned-above the step of being evaluated and tested using quality of the mentioned-above method to the electrode, can also include it
His step, no longer excessively repeats herein.
In the description of the present invention, it is to be understood that, term " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom" "inner", "outside", " up time
The orientation or positional relationship of the instructions such as needle ", " counterclockwise ", " axial direction ", " radial direction ", " circumferential direction " be orientation based on the figure or
Positional relationship is merely for convenience of description of the present invention and simplification of the description, rather than the device or element of indication or suggestion meaning must
There must be specific orientation, be constructed and operated in a specific orientation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance
Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or
Implicitly include one or more of the features.In the description of the present invention, the meaning of " plurality " is two or more,
Unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, fisrt feature in the second feature " on " or " down " can be with
It is that the first and second features directly contact or the first and second features pass through intermediary mediate contact.Moreover, fisrt feature exists
Second feature " on ", " top " and " above " but fisrt feature be directly above or diagonally above the second feature, or be merely representative of
First feature horizontal height is higher than second feature.Fisrt feature can be under the second feature " below ", " below " and " below "
One feature is directly under or diagonally below the second feature, or is merely representative of first feature horizontal height less than second feature.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of method for the expansion rate for testing electrode active material characterized by comprising
Original electrodes piece is provided, the original electrodes piece includes matrix and the electrode material that is arranged on the surface of described matrix
Layer, electrode active material and non-active material are contained in the electrode material layer；
Pressurized treatments are carried out to the original electrodes piece, and measure the electrode in the original electrodes piece under pressurised conditions
Effective original thickness L of material layer；
The original electrodes piece is assembled into battery and makes the battery work predetermined time, obtains expansion electrode piece；
Pressurized treatments are carried out to the expansion electrode piece, and measure the electrode in the expansion electrode piece under pressurised conditions
Effective expanded thickness D of material layer；
Based on effective original thickness L and effective expanded thickness D, the expansion rate of the electrode active material is determined.
2. the method according to claim 1, wherein effective original thickness L is through the following steps that measurement
:
The thickness X of the original electrodes piece is measured under pressurised conditions；
Measure the thickness L of matrix described in the original electrodes piece1, effective original thickness L=X-L1。
3. according to the method described in claim 2, it is characterized in that, effective original thickness L is through the following steps that measurement
:
Utilize the first height L of vernier caliper measurement compression mold0；
Original electrodes piece sample is put into the inner cavity of the compression mold, and utilizes tabletting mould described in the vernier caliper measurement
Second height L of tool2；
Pressurized treatments are carried out to the original electrodes piece sample in a thickness direction by the compression mold, are obtained described original
The load-deformation curve of electrode slice sample, and determine according to the load-deformation curve the non-resilient shape of the electrode material layer
Variables L3；
The thickness L of matrix described in the original electrodes piece sample is measured using spiral micrometer1, effective original thickness L=
L2-L1-L0-L3。
4. method described in any one of claim 1 to 3, which is characterized in that effective expanded thickness D be by with
Lower step measurement:
The thickness H of the expansion electrode piece is measured under pressurised conditions；
Measure the thickness D of matrix described in the expansion electrode piece1, effective expanded thickness D=H-D1。
5. according to the method described in claim 4, it is characterized in that, effective expanded thickness D is through the following steps that measurement
:
Utilize the first height D of vernier caliper measurement compression mold0；
Expansion electrode piece sample is put into the inner cavity of the compression mold, and utilizes tabletting mould described in the vernier caliper measurement
Second height D of tool2；
Pressurized treatments are carried out to the expansion electrode piece sample in a thickness direction by the compression mold, obtain the expansion
The load-deformation curve of electrode slice sample, and determine according to the load-deformation curve the non-resilient shape of the electrode material layer
Variables D3；
The thickness D of matrix described in the expansion electrode piece sample is measured using spiral micrometer1, effective expanded thickness D=
D2-D1-L0-D3。
6. according to the method described in claim 5, it is characterized in that, the size of the original electrodes piece sample and the tabletting mould
The interior chamber size of tool is consistent；The size of the expansion electrode piece sample and the interior chamber size of the compression mold are consistent.
7. according to the method described in claim 5, being set it is characterized in that, being put into multiple stackings in the inner cavity of the compression mold
The original electrodes piece sample or expansion electrode piece sample set.
8. according to the method described in claim 5, it is characterized in that, the expansion electrode piece sample is put into the tabletting mould
Before the inner cavity of tool, further comprise:
Pretreated step is carried out to the expansion electrode piece sample,
Optionally, the original electrodes piece sample or the expansion electrode piece sample are by the original electrodes piece or described
What expansion electrode piece obtained after being punched out, the middle section of the original electrodes piece or the expansion electrode piece constitutes the original
Beginning electrode slice sample or the expansion electrode piece sample.
9. a kind of method for evaluating and testing electrode quality, which is characterized in that including the use of side according to any one of claims 1 to 8
The step of method tests the expansion rate of the electrode active material.
10. a kind of method for evaluating and testing battery quality, which is characterized in that including the use of method as claimed in claim 9 to the electricity
The step of quality of pole is evaluated and tested.
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