CN117074398A - Pre-lithiated material effectiveness detection method and pole piece pre-lithiated material detection method - Google Patents
Pre-lithiated material effectiveness detection method and pole piece pre-lithiated material detection method Download PDFInfo
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- CN117074398A CN117074398A CN202311317535.7A CN202311317535A CN117074398A CN 117074398 A CN117074398 A CN 117074398A CN 202311317535 A CN202311317535 A CN 202311317535A CN 117074398 A CN117074398 A CN 117074398A
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- 239000000463 material Substances 0.000 title claims abstract description 272
- 238000001514 detection method Methods 0.000 title claims description 19
- 238000006138 lithiation reaction Methods 0.000 claims abstract description 84
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000009826 distribution Methods 0.000 claims abstract description 39
- 230000008859 change Effects 0.000 claims abstract description 35
- 238000003825 pressing Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical group C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 32
- 238000002845 discoloration Methods 0.000 claims description 25
- 238000005507 spraying Methods 0.000 claims description 9
- 230000002596 correlated effect Effects 0.000 claims description 8
- 229930002877 anthocyanin Natural products 0.000 claims description 3
- 235000010208 anthocyanin Nutrition 0.000 claims description 3
- 239000004410 anthocyanin Substances 0.000 claims description 3
- 150000004636 anthocyanins Chemical class 0.000 claims description 3
- 230000000875 corresponding effect Effects 0.000 claims description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 48
- 229910052744 lithium Inorganic materials 0.000 description 36
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 34
- 238000006243 chemical reaction Methods 0.000 description 14
- JXGGISJJMPYXGJ-UHFFFAOYSA-N lithium;oxido(oxo)iron Chemical compound [Li+].[O-][Fe]=O JXGGISJJMPYXGJ-UHFFFAOYSA-N 0.000 description 14
- 238000005520 cutting process Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000005056 compaction Methods 0.000 description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 description 6
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical group [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical class [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 4
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical class [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 3
- 229910001947 lithium oxide Inorganic materials 0.000 description 3
- GLNWILHOFOBOFD-UHFFFAOYSA-N lithium sulfide Chemical class [Li+].[Li+].[S-2] GLNWILHOFOBOFD-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- PNUGDRJNKILROY-UHFFFAOYSA-N [C].[Si].[Li] Chemical compound [C].[Si].[Li] PNUGDRJNKILROY-UHFFFAOYSA-N 0.000 description 1
- RXBBZJPEEIUBJG-UHFFFAOYSA-N [O].[Si].[Li] Chemical compound [O].[Si].[Li] RXBBZJPEEIUBJG-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HPGPEWYJWRWDTP-UHFFFAOYSA-N lithium peroxide Chemical compound [Li+].[Li+].[O-][O-] HPGPEWYJWRWDTP-UHFFFAOYSA-N 0.000 description 1
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/7756—Sensor type
- G01N2021/7759—Dipstick; Test strip
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The application provides a method for detecting the effectiveness of a pre-lithiated material and a method for detecting the pre-lithiated material in a pole piece, wherein the method for detecting the effectiveness of the pre-lithiated material comprises the following steps: obtaining a pre-lithiated material; covering test paper on the surface of the pre-lithiation material, dripping an alkaline color change indicator on one side of the test paper far away from the pre-lithiation material, and standing for a first preset time; after applying pressure to the test paper and the pre-lithiation material for a second preset time, stopping applying pressure; observing whether the test paper changes color; when the test paper changes color, the pre-lithiated material fails; when the test paper is not discolored, the prelithiation material is effective. The method for detecting the effectiveness of the pre-lithiated material and the method for detecting the pre-lithiated material in the pole piece are simple and convenient, have low cost, can rapidly detect the effectiveness of the pre-lithiated material, and determine whether the pole piece contains the pre-lithiated material and the distribution state.
Description
Technical Field
The application relates to the technical field of detection of pre-lithiated materials, in particular to a method for detecting the effectiveness of a pre-lithiated material and a method for detecting the pre-lithiated material in a pole piece.
Background
The new energy industry develops rapidly, and people put higher demands on the energy density and the circulation level of the battery, and the currently effective method is to add a pre-lithiation material in the pole piece, wherein the pre-lithiation material can provide additional lithium ions, complement the short plate effect caused by the first effect difference of the anode and the cathode, and can improve the energy density of the battery. And redundant lithium ions can be stored in the negative electrode, so that capacity attenuation caused by active lithium loss in the cycling process is slowed down, and the cycle life of the battery is prolonged.
The pre-lithiated material is unstable in air and can cause material failure and capacity reduction after long-time exposure, so that the detection of the effectiveness of the pre-lithiated material is extremely important, the detection of the effectiveness of the pre-lithiated material in the prior art is mainly carried out by manufacturing a button cell, and the capacity of the pre-lithiated material is directly tested to represent the failure degree of the material, but the method is time-consuming and labor-consuming, the consistency of the button test is difficult to ensure, and the failure degree of the material cannot be well described; in some technologies, the surface morphology of the prelithiation material is observed through a visual means such as a Scanning Electron Microscope (SEM) to illustrate the change of the performance, but the change of the surface morphology has delay to the failure of the material, the material is often failed, but the surface morphology of the material is not obviously changed, the accuracy is poor, and the cost is high, so that a method for rapidly and effectively detecting the effectiveness of the prelithiation material is needed.
In addition, after the pre-lithiated material is added into a battery system to prepare a battery, because the appearance and the appearance of the pre-lithiated material are consistent with those of other common main materials, the pre-lithiated material is difficult to distinguish from other main materials when a scanning electron microscope is adopted for detection, whether the pole piece contains the pre-lithiated material or not cannot be determined, and the distribution state of the pre-lithiated material in the pole piece cannot be known, so that a method capable of rapidly detecting the pre-lithiated material in the pole piece is needed.
Disclosure of Invention
Therefore, the application aims to provide a method for detecting the effectiveness of a pre-lithiated material and a method for detecting the pre-lithiated material in a pole piece, which are used for solving the technical problems.
In a first aspect of the present application, there is provided a method for detecting the effectiveness of a prelithiated material, comprising: obtaining a pre-lithiated material; covering test paper on the surface of the pre-lithiation material, dripping an alkaline color change indicator on one side of the test paper far away from the pre-lithiation material, and standing for a first preset time; after applying pressure to the test paper and the pre-lithiation material for a second preset time, stopping applying pressure; observing whether the test paper changes color; when the test paper changes color, the pre-lithiated material fails; when the test paper is not discolored, the prelithiation material is effective.
Further, the degree of failure of the prelithiated material is positively correlated to the degree of discoloration of the test paper.
Further, the obtaining a prelithiated material, followed by: the pre-lithiated material is placed in a container and compacted such that the pre-lithiated material is tightly packed.
Further, the pre-lithiation material is an anode pre-lithiation material or a cathode pre-lithiation material, the first preset time is 2s to 6s, the second preset time is 10s to 30s, and the alkaline color-changing indicator is free of water.
In a second aspect of the present application, a method for detecting a prelithiated material in a pole piece is provided, comprising: acquiring a first pole piece; contacting the first pole piece with water to obtain a second pole piece; covering test paper on the surface of the wet second pole piece, and dripping an alkaline color change indicator on one side of the test paper far away from the pre-lithiation material; observing whether the test paper changes color; when the test paper changes color, the second pole piece contains a pre-lithiation material; when the test paper does not change color, the second pole piece does not contain a pre-lithiation material.
Further, the addition amount of the pre-lithiated material is positively correlated with the degree of discoloration of the test paper.
Further, the detection method of the pre-lithiated material in the pole piece further comprises the following steps: and determining the distribution state of the pre-lithiation material in the second pole piece according to the color distribution in the color-changing area of the test paper.
Further, the determining the distribution state of the prelithiation material in the second pole piece according to the color distribution in the color-changing area of the test paper includes: randomly acquiring a plurality of color-changing subareas from the color-changing area; determining the brightness level of the color of each color-changing subarea; calculating to obtain the maximum level difference of the brightness levels corresponding to the color-changing subareas; when the maximum level difference is larger than a preset level difference, the distribution state is in an uneven state; and when the maximum grade difference is smaller than or equal to the preset grade difference, the distribution state is a uniform state.
Further, the contacting the first pole piece with water to obtain a second pole piece includes: and spraying water on the surface of the first pole piece to react for a third preset time to obtain a second pole piece, or placing the first pole piece in humid air to react for a fourth preset time to obtain the second pole piece.
Further, the third preset time is 5s to 20s, the fourth preset time is more than 24h, the relative humidity of the humid air is more than or equal to 50%, the pre-lithiated material is an anode pre-lithiated material or a cathode pre-lithiated material, and the alkaline color-changing indicator is a phenolphthalein indicator, a litmus indicator or an anthocyanin indicator.
From the foregoing, it can be seen that the present application provides a method for detecting the effectiveness of a prelithiated material, comprising obtaining a prelithiated material; covering test paper on the surface of the pre-lithiated material, dropwise adding an alkaline color change indicator on one side of the test paper far away from the pre-lithiated material, and standing for a first preset time to moisten the test paper and the pre-lithiated material under the test paper; after the test paper and the pre-lithiation material are subjected to pressure for a second preset time, stopping the pressure application, so that the alkaline color-changing indicator is fully contacted with the pre-lithiation material; if the pre-lithiated material fails, lithium hydroxide and/or lithium carbonate are generated on the surface of the pre-lithiated material, whether the test paper changes color or not is observed, and when the test paper changes color, the pre-lithiated material fails; when the test paper does not change color, the pre-lithiation material is effective, the test paper is contacted with lithium hydroxide and/or lithium carbonate after absorbing the alkaline color change indicator, and color change reaction occurs on the test paper, so that pollution to the pre-lithiation material is avoided, and the color change condition is convenient to observe.
The application also provides a detection method of the pre-lithiated material in the pole piece, which comprises the steps of obtaining a first pole piece; the first pole piece is contacted with water to obtain a second pole piece, and if the pole piece contains a pre-lithiation material, residual lithium on the surface of the pre-lithiation material can be converted into lithium hydroxide; covering test paper on the surface of the wet second pole piece, absorbing the reacted water, and dripping an alkaline color-changing indicator on one side of the test paper far away from the pre-lithiation material; observing whether the test paper changes color; the alkaline color-changing indicator undergoes a color-changing reaction when encountering lithium hydroxide, and when the test paper changes color, the second pole piece contains a pre-lithiation material; when the test paper does not change color, the second pole piece does not contain the pre-lithiation material, the test paper is arranged to facilitate observation of the color change condition, and the distribution position of lithium hydroxide can be reflected on the color change area of the test paper, so that the distribution state of the pre-lithiation material in the pole piece is determined.
The method for detecting the effectiveness of the pre-lithiated material and the method for detecting the pre-lithiated material in the pole piece are simple and convenient, have low cost, can rapidly detect the effectiveness of the pre-lithiated material, and determine whether the pole piece contains the pre-lithiated material and the distribution state.
Drawings
In order to more clearly illustrate the technical solutions of the present application or related art, the drawings that are required to be used in the description of the embodiments or related art will be briefly described below, and it is apparent that the drawings in the following description are only embodiments of the present application, and other drawings may be obtained according to the drawings without inventive effort to those of ordinary skill in the art.
FIG. 1 is a schematic flow chart of a method for detecting the effectiveness of a prelithiated material in an embodiment of the application;
FIG. 2 is a schematic flow chart of a method for detecting a prelithiated material in a pole piece in an embodiment of the application;
FIG. 3 is a white paper test chart of comparative example 1 of the present application;
FIG. 4 is a chart of the white paper test of example 7 of the present application;
fig. 5 is a white paper test chart of embodiment 10 of the present application.
Detailed Description
The present application will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present application more apparent.
It should be noted that unless otherwise defined, technical or scientific terms used in the embodiments of the present application should be given the ordinary meaning as understood by one of ordinary skill in the art to which the present application belongs. The terms "first," "second," and the like, as used in embodiments of the present application, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
Along with the increasing demand of energy, secondary batteries are the focus of attention, and lithium ion secondary batteries are widely used in daily life of people due to the advantages of long cycle life, high and stable battery voltage, better cycle performance than other secondary batteries, capability of quick charge and discharge, higher specific capacity of batteries, lower self-discharge rate of batteries, low pollution to the environment and the like.
The new energy industry develops rapidly, and people put higher demands on the energy density and the circulation level of the battery, and the currently effective method is to add a pre-lithiation material in the pole piece, wherein the pre-lithiation material can provide additional lithium ions, complement the short plate effect caused by the first effect difference of the anode and the cathode, and can improve the energy density of the battery. And redundant lithium ions can be stored in the negative electrode, so that capacity attenuation caused by active lithium loss in the cycling process is slowed down, and the cycle life of the battery is prolonged.
The pre-lithiated material is unstable in air and can cause material failure and capacity reduction after long-time exposure, so that the detection of the effectiveness of the pre-lithiated material is extremely important, the detection of the effectiveness of the pre-lithiated material in the prior art is mainly carried out by manufacturing a button cell, and the capacity of the pre-lithiated material is directly tested to represent the failure degree of the material, but the method is time-consuming and labor-consuming, the consistency of the button test is difficult to ensure, and the failure degree of the material cannot be well described; in some technologies, the surface morphology of the prelithiated material is observed through visual means such as a Scanning Electron Microscope (SEM) to show the change of the performance, but the change of the surface morphology has delay to the failure of the material, the material is often failed, but the surface morphology of the material is not obviously changed, the accuracy is poor, and the cost is high. Therefore, a method for rapidly and effectively detecting the effectiveness of a prelithiated material is needed.
In addition, after the pre-lithiated material is added into a battery system to prepare a battery, because the appearance and the appearance of the pre-lithiated material are consistent with those of other common main materials, the pre-lithiated material is difficult to distinguish from other main materials when a scanning electron microscope is adopted for detection, whether the pole piece contains the pre-lithiated material or not cannot be determined, and the distribution state of the pre-lithiated material in the pole piece cannot be known quickly, so that a method capable of detecting the pre-lithiated material in the pole piece quickly is needed.
In the process of realizing the application, the surface of the pre-lithiated material is found to have a plurality of residual lithium and compounds thereof, and the residual lithium reacts with air or water to generate lithium hydroxide and lithium carbonate, so that the surface of the material is alkalized and the material is invalid, and the color-changing reaction of the alkaline color-changing indicator can be considered to judge whether the pre-lithiated material is invalid or not; for detection of the pre-lithiated material in the pole piece, the pole piece can be contacted with water first, then the color change reaction of the alkaline color change indicator is utilized to judge whether the pole piece contains the pre-lithiated material, and the color distribution of the color change area can be observed by means of test paper to determine the distribution state of the pre-lithiated material in the pole piece.
The following describes the technical solution of the present application in detail by specific embodiments and with reference to fig. 1 to 5.
In some embodiments of the present application, a method for detecting effectiveness of a prelithiated material is provided, as shown in fig. 1, including the following steps:
s11, obtaining the pre-lithiated material.
The pre-lithiation material is a positive electrode pre-lithiation material or a negative electrode pre-lithiation material, the positive electrode pre-lithiation material comprises one or more of lithium oxide, lithium nitride, lithium sulfide or lithium metal salt, the lithium oxide is for example lithium oxide, lithium peroxide and the like, the lithium nitride is for example lithium nitride, inert lithium nitride and the like, the lithium sulfide is for example lithium sulfide and the like, the lithium metal salt is for example one or more of lithium-rich nickel acid lithium, lithium-rich ferrite lithium, lithium-rich cobalt acid lithium, lithium-rich manganate lithium and lithium-rich ternary material, and the method is not particularly limited; the negative electrode pre-lithiation material includes pre-lithium graphite, pre-lithium silicon carbon, pre-lithium silicon oxygen, etc., and is not particularly limited.
S12, covering test paper on the surface of the pre-lithiation material, dropwise adding an alkaline color-changing indicator on one side of the test paper far away from the pre-lithiation material, and standing for a first preset time.
Covering the surface of the pre-lithiation material with test paper, dripping an alkaline color change indicator on one side of the test paper far away from the pre-lithiation material to cover the pre-lithiation material, and standing for a first preset time to moisten the test paper and the pre-lithiation material under the test paper.
The first preset time is 2s to 6s, for example, 2s, 3s, 4s, 5s or 6s, etc., and is not particularly limited, the alkaline color-changing indicator does not contain water, for example, a phenolphthalein indicator, etc., so that the reaction of water and residual lithium of the pre-lithiated material is avoided, the effectiveness judgment is influenced, the test paper is white fiber paper, for example, the alkaline color-changing indicator is conveniently absorbed, and the color change condition is observed.
And S13, stopping pressing after the test paper and the pre-lithiation material are subjected to pressure for a second preset time.
After a second preset time, such as 10s to 30s, for example, 10s, 15s, 20s, 25s or 30s, the pressure is applied, such as 5N to 10N, for example, 6N, 7N, 8N or 9N, etc., without limitation.
S14, observing whether the test paper changes color or not.
S15, when the test paper changes color, the pre-lithiated material fails; when the test paper is not discolored, the prelithiation material is effective.
If residual lithium on the failure surface of the pre-lithiated material generates lithium hydroxide and/or lithium carbonate, observing whether the test paper changes color, and when the test paper changes color, representing that the pre-lithiated material fails; when the test paper does not change color, the pre-lithiation material is effective; the test paper is contacted with lithium hydroxide and/or lithium carbonate after absorbing the alkaline color-changing indicator, and color-changing reaction occurs on the test paper, so that on one hand, the pre-lithiation material is prevented from being polluted, and on the other hand, the color-changing condition can be conveniently observed.
The method for detecting the effectiveness of the pre-lithiated material is simple and convenient, low in cost, capable of rapidly detecting the effectiveness of the pre-lithiated material, and high in accuracy.
In some embodiments, the degree of failure of the prelithiated material is positively correlated to the degree of discoloration of the test paper.
The failure degree of the pre-lithiation material is positively correlated with the color-changing degree of the test paper, the more the pre-lithiation material fails, the more lithium hydroxide and/or lithium carbonate are generated on the surface, the more obvious the color-changing reaction is, and the greater the color-changing degree of the test paper is, so that the failure degree of the pre-lithiation material can be judged according to the color-changing degree of the test paper.
In some embodiments, step S11 is followed by:
and S111, placing the pre-lithiated material in a container for compaction so as to enable the pre-lithiated material to be closely packed.
The container is, for example, a surface dish, etc., and is not particularly limited, and the pre-lithiated material is placed in the container and compacted so as to enable the pre-lithiated material to be closely packed, thereby facilitating the subsequent full contact with the test paper.
In some embodiments of the present application, a method for detecting a prelithiated material in a pole piece is provided, as shown in fig. 2, including the following steps:
s21, obtaining a first pole piece.
The first pole piece can be cut into strips, so that subsequent contact reaction with water is facilitated, the cutting size is for example 5cm x 1cm, the first pole piece is not limited in detail, and the first pole piece is for example a positive pole piece or a negative pole piece.
S22, contacting the first pole piece with water to obtain a second pole piece.
The first pole piece is contacted with water to obtain a second pole piece, if the pole piece contains a pre-lithiation material, residual lithium on the surface of the pre-lithiation material can be converted into lithium hydroxide, and the main material in the pole piece has higher stability and hardly reacts with water; the pre-lithiation material is, for example, a positive electrode pre-lithiation material or a negative electrode pre-lithiation material, and the main material is, for example, a common positive electrode main material or a negative electrode main material.
S23, covering the surface of the wet second pole piece with test paper, and dripping an alkaline color change indicator on one side of the test paper far away from the pre-lithiation material.
And covering the surface of the wet second pole piece with test paper, absorbing the reacted water, and dripping an alkaline color-changing indicator which is a phenolphthalein indicator, a litmus indicator or an anthocyanin indicator and the like on one side of the test paper far away from the pre-lithiation material, wherein the test paper is white fiber paper and the like, and is not particularly limited.
S24, observing whether the test paper changes color or not.
S25, when the test paper changes color, the second pole piece contains a pre-lithiation material; when the test paper does not change color, the second pole piece does not contain a pre-lithiation material.
When the alkaline color-changing indicator encounters lithium hydroxide and the test paper changes color, as shown in fig. 4, the second pole piece contains a pre-lithiated material; when the test paper does not change color, as shown in fig. 3, the second pole piece does not contain the pre-lithiation material, the test paper is arranged to facilitate observation of the color change condition, and the distribution position of lithium hydroxide can be reflected on the color change area of the test paper, so that the distribution state of the pre-lithiation material in the pole piece is determined.
The detection method of the pre-lithiated material in the pole piece is simple and convenient, has low cost and short test waiting period compared with the detection method of a scanning electron microscope and the like, and can rapidly determine whether the pole piece contains the pre-lithiated material and the distribution state.
In some embodiments, the amount of pre-lithiated material added is positively correlated to the degree of discoloration of the test paper.
The adding amount of the pre-lithiation material in the pole piece is positively correlated with the color-changing degree of the test paper, the more the adding amount of the pre-lithiation material is, the more lithium hydroxide is generated on the surface, the more obvious the color-changing reaction is, and the larger the color-changing degree of the test paper is, so that the adding amount of the pre-lithiation material can be judged according to the color-changing degree of the test paper.
In some embodiments, the method for detecting a prelithiated material in a pole piece further comprises:
s26, determining the distribution state of the pre-lithiation material in the second pole piece according to the color distribution in the color-changing area of the test paper.
As shown in fig. 5, the color distribution in the color-changing area can be clearly seen on the test paper, the area with larger color change represents that the content of lithium hydroxide in the position is more, and lithium hydroxide is obtained by the reaction of the pre-lithiation material, so that the content of the pre-lithiation material in the position is more, and similarly, the area with smaller color change on the test paper represents that the content of the pre-lithiation material in the position is less, the distribution uniformity of the pre-lithiation material can be determined according to the color distribution uniformity of the color-changing area, if the color distribution is uniform, the color distribution uniformity of the pre-lithiation material in the pole piece is represented, as shown in fig. 5, the color depth of the color-changing area of the test paper is different, so that the distribution of the pre-lithiation material is not uniform.
In some embodiments, step S26 includes:
s261, randomly acquiring a plurality of color-changing subareas from the color-changing area.
A plurality of color-changing subareas are randomly obtained from the color-changing area, the shape of the color-changing subareas is rectangular or circular, and the like, the number of the color-changing subareas is 4 to 8, for example 4, 5, 6, 7 or 8, the number of the color-changing subareas is not limited, the judgment accuracy of the uniform state is reduced, the number of the color-changing subareas is also prevented from being excessive, and the processing capacity is increased; the plurality of color-changing subareas are not overlapped in the color-changing areas, so that the accidental of subsequent calculation is reduced; as shown in fig. 5, rectangles in the figure are color-changing areas of the test paper, and 4 color-changing subareas are randomly acquired in the color-changing areas, namely square areas in the figure.
S262, determining the brightness level of the color of each color-changing subarea.
The brightness level of the color of each color-changing subregion can be determined using a brightness tester or a color scale comparison method, for example, the brightness level comprises 1 level to 9 levels, and the lower the number of levels, the darker the color.
And S263, calculating and obtaining the maximum level difference of the brightness levels corresponding to the color-changing subareas.
S264, when the maximum level difference is larger than a preset level difference, the distribution state is in an uneven state; and when the maximum grade difference is smaller than or equal to the preset grade difference, the distribution state is a uniform state.
The preset level difference is two-stage, and when the maximum level difference is greater than two-stage, the distribution state is represented as uneven state; and when the maximum grade difference is smaller than or equal to two stages, the representative distribution state is a uniform state, so that the distribution uniformity of the pre-lithiated material in the pole piece is judged.
In some embodiments, step S22 includes:
s221, spraying water on the surface of the first pole piece to react for a third preset time to obtain a second pole piece, or placing the first pole piece in humid air to react for a fourth preset time to obtain the second pole piece.
The water is sprayed on the surface of the first pole piece to react for a third preset time to obtain the second pole piece, the third preset time is 5s to 20s, for example, 5s, 10s, 15s or 20s, and the like, the method is not particularly limited, the water covers the surface of the first pole piece, the alkalization reaction of the pre-lithiation material can be rapidly realized, and the detection period is shortened.
The first pole piece is placed in humid air for reacting for a fourth preset time to obtain a second pole piece, the fourth preset time is more than 24 hours, such as 36 hours, 48 hours, 60 hours or 72 hours, and the like, the relative humidity of the humid air is more than or equal to 50%, such as 50%, 60%, 70% or 80%, and the like, the relative humidity of the humid air is not limited, the pole piece reacts with water in the humid air, the fluidity of generated lithium hydroxide can be reduced relative to direct water spraying, the correspondence between the color change position of test paper and the position of an actual pre-lithiated material is ensured, and the accuracy of the subsequent uniform state judgment is improved.
Example 1
Obtaining fresh pre-lithiated material lithium-rich lithium ferrite, namely newly prepared lithium-rich lithium ferrite which is not exposed to air; placing lithium-rich lithium ferrite into a surface dish for compaction so as to tightly pack the pre-lithiated material; covering the surface of the pre-lithiated material in a surface dish with white paper, dropwise adding a phenolphthalein indicator on one side of the white paper far away from the pre-lithiated material to cover the surface dish, and standing for 2s; after applying 5N pressure to the white paper and the pre-lithiated material for 10s, stopping applying pressure; the white paper was observed for discoloration.
Example 2
Fresh pre-lithiated material lithium-rich lithium ferrite is obtained and exposed in the air for 5 days; then placing the lithium-rich lithium ferrite into a surface dish for compaction so as to tightly pack the pre-lithiated material; covering the surface of the pre-lithiated material in a surface dish with white paper, dropwise adding a phenolphthalein indicator on one side of the white paper far away from the pre-lithiated material to cover the surface dish, and standing for 2s; after applying 5N pressure to the white paper and the pre-lithiated material for 10s, stopping applying pressure; the white paper was observed for discoloration.
Example 3
Fresh pre-lithiated material lithium-rich lithium ferrite is obtained and exposed in the air for 10 days; then placing the lithium-rich lithium ferrite into a surface dish for compaction so as to tightly pack the pre-lithiated material; covering the surface of the pre-lithiated material in a surface dish with white paper, dropwise adding a phenolphthalein indicator on one side of the white paper far away from the pre-lithiated material to cover the surface dish, and standing for 2s; after applying 5N pressure to the white paper and the pre-lithiated material for 10s, stopping applying pressure; the white paper was observed for discoloration.
Example 4
Fresh pre-lithiated material pre-lithiated silica is obtained and exposed and stored in the air for 10 days; then placing the pre-lithiated silica in a surface dish for compaction so as to tightly pack the pre-lithiated material; covering the surface of the pre-lithiated material in a surface dish with white paper, dropwise adding a phenolphthalein indicator on one side of the white paper far away from the pre-lithiated material to cover the surface dish, and standing for 2s; after applying 5N pressure to the white paper and the pre-lithiated material for 10s, stopping applying pressure; the white paper was observed for discoloration.
Example 5
Fresh pre-lithiation material lithium-rich lithium ferrite is obtained, and water is sprayed on the surface of the lithium-rich lithium ferrite; then placing the lithium-rich lithium ferrite into a surface dish for compaction so as to tightly pack the pre-lithiated material; covering the surface of the pre-lithiated material in a surface dish with white paper, dropwise adding a phenolphthalein indicator on one side of the white paper far away from the pre-lithiated material to cover the surface dish, and standing for 2s; after applying 5N pressure to the white paper and the pre-lithiated material for 10s, stopping applying pressure; the white paper was observed for discoloration.
Table 1 examples 1-5 table of detection results of prelithiated materials
The test results of examples 1 to 5 are shown in table 1, and the non-failed pre-lithiated material was tested to have no discoloration, the failed pre-lithiated material was all subject to discoloration, and the more severe the failure, the greater the degree of discoloration.
Comparative example 1
And obtaining a first pole piece, wherein the main material of the first pole piece is lithium iron phosphate, and the first pole piece contains 5% of pre-lithiated material lithium-rich lithium ferrite by mass percent.
Cutting a first pole piece into a right triangle with the diameter of 3mm or less, covering white paper on the surface of the first pole piece, and dripping a phenolphthalein indicator on one side of the white paper far away from the pre-lithiation material to cover the first pole piece; the white paper was observed for discoloration.
Example 6
And obtaining a first pole piece, wherein the main material of the first pole piece is lithium iron phosphate, and the first pole piece does not contain a pre-lithiation material.
Cutting the first pole piece into right triangle with the diameter of 3mm and the diameter of 3mm, spraying water on the surface of the first pole piece to react for 5s to obtain a second pole piece; covering the surface of the second pole piece with white paper, and dripping a phenolphthalein indicator on one side of the white paper far away from the pre-lithiation material to cover the second pole piece; the white paper was observed for discoloration.
Example 7
And obtaining a first pole piece, wherein the main material of the first pole piece is lithium iron phosphate, and the first pole piece contains 5% of pre-lithiated material lithium-rich lithium ferrite by mass percent.
Cutting the first pole piece into right triangle with the diameter of 3mm and the diameter of 3mm, spraying water on the surface of the first pole piece to react for 5s to obtain a second pole piece; covering the surface of the second pole piece with white paper, and dripping a phenolphthalein indicator on one side of the white paper far away from the pre-lithiation material to cover the second pole piece; the white paper was observed for discoloration.
Example 8
And obtaining a first pole piece, wherein the main material of the first pole piece is lithium iron phosphate and contains 5% of pre-lithiated material lithium-rich lithium nickelate by mass.
Cutting the first pole piece into right triangle with the diameter of 3mm and the diameter of 3mm, spraying water on the surface of the first pole piece to react for 5s to obtain a second pole piece; covering the surface of the second pole piece with white paper, and dripping a phenolphthalein indicator on one side of the white paper far away from the pre-lithiation material to cover the second pole piece; the white paper was observed for discoloration.
Example 9
And obtaining a first pole piece, wherein the main material of the first pole piece is lithium iron phosphate, and the first pole piece contains 50% of pre-lithiated material lithium-rich lithium ferrite.
Cutting the first pole piece into right triangle with the diameter of 3mm and the diameter of 3mm, spraying water on the surface of the first pole piece to react for 5s to obtain a second pole piece; covering the surface of the second pole piece with white paper, and dripping a phenolphthalein indicator on one side of the white paper far away from the pre-lithiation material to cover the second pole piece; the white paper was observed for discoloration.
Example 10
And obtaining a first pole piece, wherein the main material of the first pole piece is lithium iron phosphate, and the first pole piece contains 5% of pre-lithiated material lithium-rich lithium ferrite by mass percent.
Cutting the first pole piece into pole piece strips with the length of 5cm and the length of 1cm, placing the pole piece strips in moist air to react for 3 days to obtain a second pole piece, wherein the relative humidity of the air is 50%; covering the surface of the second pole piece with white paper, and dripping a phenolphthalein indicator on one side of the white paper far away from the pre-lithiation material to cover the second pole piece; the white paper was observed for discoloration.
Example 11
And obtaining a first pole piece, wherein the main material of the first pole piece is graphite and contains pre-lithiation material pre-lithiation silica with the mass fraction of 10%.
Cutting the first pole piece into right triangle with the diameter of 3mm and the diameter of 3mm, spraying water on the surface of the first pole piece to react for 5s to obtain a second pole piece; covering the surface of the second pole piece with white paper, and dripping a phenolphthalein indicator on one side of the white paper far away from the pre-lithiation material to cover the second pole piece; the white paper was observed for discoloration.
Table 2 comparative example 1 and tables of pole piece test results of examples 6-11
The test results of comparative example 1 and examples 6 to 11 are shown in table 2, and the pole pieces which are not contacted with water and contain the pre-lithiated material are not subjected to a discoloration reaction, the pole pieces which are contacted with water and do not contain the pre-lithiated material are not subjected to a discoloration reaction, the pole pieces which are contacted with water and contain the pre-lithiated material are all subjected to a discoloration reaction, and the higher the content of the pre-lithiated material is, the greater the degree of discoloration is.
Example 7 was sprayed to contact water, and the experimental result is shown in fig. 4, and it can be seen that the color distribution is in a sheet shape, and the color at the corners is darker than the color in the middle area, which is caused by the more water diffusion; whereas example 10 was in contact with water by means of humid air, the experimental results are shown in fig. 5, and it can be seen that the color distribution is in scattered spots, which can more accurately represent the position of the prelithiated material.
And randomly selecting 4 square color-changing subareas in the rectangular color-changing area in fig. 5, comparing and determining the brightness level of the color of each color-changing subarea by adopting a color scale table, wherein the brightness level is sequentially 5 levels, 8 levels, 2 levels and 5 levels from left to right, calculating to obtain the maximum level difference of the color-changing subarea as six levels, the preset level difference as two levels, and the maximum level difference as greater than the preset level difference, wherein the distribution state is represented as an uneven state.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the application is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the application, the steps may be implemented in any order, and there are many other variations of the different aspects of the embodiments of the application as described above, which are not provided in detail for the sake of brevity.
In addition, where details are set forth to describe example embodiments of the application, it will be apparent to one skilled in the art that embodiments of the application may be practiced without, or with variation of, these details. Accordingly, the description is to be regarded as illustrative in nature and not as restrictive.
Well-known power/ground connections to other components may or may not be shown in the drawings provided to simplify the illustration and discussion, and so as not to obscure embodiments of the present application. Furthermore, the devices may be shown in block diagram form in order to avoid obscuring the embodiments of the present application, and also in view of the fact that specifics with respect to implementation of such block diagram devices are highly dependent upon the platform within which the embodiments of the present application are to be implemented (i.e., such specifics should be well within purview of one skilled in the art). Where specific details are set forth in order to describe example embodiments of the application, it should be apparent to one skilled in the art that embodiments of the application can be practiced without, or with variation of, these specific details. Accordingly, the description is to be regarded as illustrative in nature and not as restrictive.
While the application has been described in conjunction with specific embodiments thereof, many alternatives, modifications, and variations of those embodiments will be apparent to those skilled in the art in light of the foregoing description. The present embodiments are intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, and the like, which are within the spirit and principles of the embodiments of the application, are intended to be included within the scope of the application.
Claims (10)
1. The method for detecting the effectiveness of the prelithiation material is characterized by comprising the following steps of:
obtaining a pre-lithiated material;
covering test paper on the surface of the pre-lithiation material, dripping an alkaline color change indicator on one side of the test paper far away from the pre-lithiation material, and standing for a first preset time;
after applying pressure to the test paper and the pre-lithiation material for a second preset time, stopping applying pressure;
observing whether the test paper changes color;
when the test paper changes color, the pre-lithiated material fails; when the test paper is not discolored, the prelithiation material is effective.
2. The method of claim 1, wherein the degree of failure of the pre-lithiated material is positively correlated with the degree of discoloration of the test paper.
3. The method of claim 1, wherein the obtaining the pre-lithiated material, after which comprises:
the pre-lithiated material is placed in a container and compacted such that the pre-lithiated material is tightly packed.
4. The method for detecting the effectiveness of a prelithiation material according to claim 1, wherein the prelithiation material is a positive electrode prelithiation material or a negative electrode prelithiation material, the first predetermined time is 2s to 6s, the second predetermined time is 10s to 30s, and the basic color change indicator is free of water.
5. The detection method of the pre-lithiated material in the pole piece is characterized by comprising the following steps:
acquiring a first pole piece;
contacting the first pole piece with water to obtain a second pole piece;
covering test paper on the surface of the wet second pole piece, and dripping an alkaline color change indicator on one side of the test paper far away from the pre-lithiation material;
observing whether the test paper changes color;
when the test paper changes color, the second pole piece contains a pre-lithiation material; when the test paper does not change color, the second pole piece does not contain a pre-lithiation material.
6. The method for detecting a pre-lithiated material in a pole piece of claim 5, wherein the amount of pre-lithiated material added is positively correlated to the degree of discoloration of the test paper.
7. The method for detecting a prelithiated material in a pole piece of claim 5, further comprising: and determining the distribution state of the pre-lithiation material in the second pole piece according to the color distribution in the color-changing area of the test paper.
8. The method for detecting a pre-lithiated material in a pole piece of claim 7, wherein said determining a distribution state of said pre-lithiated material in said second pole piece from a color distribution in a color change region of said test paper comprises:
randomly acquiring a plurality of color-changing subareas from the color-changing area;
determining the brightness level of the color of each color-changing subarea;
calculating to obtain the maximum level difference of the brightness levels corresponding to the color-changing subareas;
when the maximum level difference is larger than a preset level difference, the distribution state is in an uneven state; and when the maximum grade difference is smaller than or equal to the preset grade difference, the distribution state is a uniform state.
9. The method for detecting a prelithiation material in a pole piece according to claim 5, wherein the contacting the first pole piece with water to obtain a second pole piece comprises:
and spraying water on the surface of the first pole piece to react for a third preset time to obtain a second pole piece, or placing the first pole piece in humid air to react for a fourth preset time to obtain the second pole piece.
10. The method according to claim 9, wherein the third preset time is 5s to 20s, the fourth preset time is greater than 24h, the relative humidity of the humid air is greater than or equal to 50%, the pre-lithiated material is a positive pre-lithiated material or a negative pre-lithiated material, and the alkaline color-changing indicator is a phenolphthalein indicator, a litmus indicator or an anthocyanin indicator.
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