CN116754542A - Method for evaluating stability of battery slurry - Google Patents
Method for evaluating stability of battery slurry Download PDFInfo
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- CN116754542A CN116754542A CN202310776256.0A CN202310776256A CN116754542A CN 116754542 A CN116754542 A CN 116754542A CN 202310776256 A CN202310776256 A CN 202310776256A CN 116754542 A CN116754542 A CN 116754542A
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- 239000002002 slurry Substances 0.000 title claims abstract description 109
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 48
- 230000008859 change Effects 0.000 claims abstract description 30
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 10
- MWEXRLZUDANQDZ-RPENNLSWSA-N (2s)-3-hydroxy-n-[11-[4-[4-[4-[11-[[2-[4-[(2r)-2-hydroxypropyl]triazol-1-yl]acetyl]amino]undecanoyl]piperazin-1-yl]-6-[2-[2-(2-prop-2-ynoxyethoxy)ethoxy]ethylamino]-1,3,5-triazin-2-yl]piperazin-1-yl]-11-oxoundecyl]-2-[4-(3-methylsulfanylpropyl)triazol-1-y Chemical compound N1=NC(CCCSC)=CN1[C@@H](CO)C(=O)NCCCCCCCCCCC(=O)N1CCN(C=2N=C(N=C(NCCOCCOCCOCC#C)N=2)N2CCN(CC2)C(=O)CCCCCCCCCCNC(=O)CN2N=NC(C[C@@H](C)O)=C2)CC1 MWEXRLZUDANQDZ-RPENNLSWSA-N 0.000 claims abstract description 7
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 7
- 238000001107 thermogravimetry coupled to mass spectrometry Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000011156 evaluation Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000006258 conductive agent Substances 0.000 claims description 3
- 230000029087 digestion Effects 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims description 3
- 239000002562 thickening agent Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 5
- 239000011267 electrode slurry Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a method for testing the stability of battery slurry, which adopts ICP-OES and TG-MS quantitative analysis to detect the material composition of the battery slurry, and utilizes the material mass percent change rate of the slurry with the cross section at a set height to evaluate the stability of the slurry after the slurry is stood, so that the detection accuracy is high, the material which plays a great role in the stability of the slurry can be clearly obtained, and the stability of a slurry system can be improved by adjusting the physicochemical property of the material.
Description
Technical Field
The invention belongs to the technical field of battery slurry, and particularly relates to an evaluation method of battery slurry stability.
Background
Battery slurry is a suspension system mixed from different substances, which have different sedimentation rates. The interactions between different particles are complex and thus monitoring stability is very difficult. Even if uniformly mixed, the slurry is layered due to sedimentation after a certain time. In addition, aggregation can occur among particles, so that particles of different substances are unevenly distributed in the whole system, and the dispersing effect is poor.
If the slurry stability is poor, delamination occurs during the subsequent coating process, and the dispersion effect is deteriorated due to particle aggregation, the battery performance (e.g., specific capacity and cycle performance) finally produced is significantly deteriorated. The stability of the battery paste is very important for battery performance. Conventional methods include testing slurry flow, viscosity, solids content, particle size, and the like.
Examples disclosed in patent document CN 106124363B: the stability of the slurry is characterized by comparing the coincidence of two viscosity curves with the shear rate curve by testing the viscosity change of the positive and negative electrode slurry from small to large and the viscosity change of the positive and negative electrode slurry from large to small.
Examples disclosed in patent document CN109884161 a: the method comprises the steps of collecting ceramic slurry with a certain height cross section after standing for a certain time, and detecting element change of a collected slurry barrel through a mass spectrometer to represent slurry stability.
The testing modes are rough, the stability of the battery slurry cannot be accurately represented, the influence of various materials on the stability of the slurry cannot be clarified, and effective technical assistance cannot be provided for the subsequent stability improvement of the battery slurry.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention tries to provide the method for testing the stability of the battery slurry, realizes relatively accurate characterization of the stability of the battery slurry, determines the influence of various materials on the stability of the slurry, and provides technical assistance for the subsequent stability improvement of the battery slurry.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention provides a method for testing the stability of battery slurry, which comprises the following steps:
step 1, preparation of battery slurry: the battery slurry which is just prepared or uniformly dispersed and has the known actual proportion is placed in a charging barrel, sealed and kept stand.
Step 2, detecting the components of the slurry: and after standing for a set time, taking out the slurry with fixed mass at the cross section of the slurry with set height, processing, performing ICP-OES quantitative analysis and TG-MS quantitative analysis, respectively calculating the mass percentages of the materials containing metal elements, and calculating the mass percentages of the binder, the conductive agent and the thickener to obtain the slurry proportion of the slurry in the area with set height, and then calculating the percentage of the material proportion.
Step 3, stability evaluation: comparing the measured proportion of the slurry in the height area with a corresponding theoretical value, and considering that the slurry has good stability when the mass percent change rate of each material of the slurry proportion is not more than a specified value; if the mass percent change rate of the material is larger than the specified value, the slurry stability is considered to be poor, and the influence of the material on the slurry stability is larger.
Further preferably, the treating of the slurry in step 2 includes: firstly, drying treatment is carried out, and then digestion, filtration, dilution and constant volume treatment are carried out.
Further preferably, in the step 2, any area on the slurry set height cross section is sampled, each area is measured, and then a plurality of measured values are averaged and compared with a theoretical value.
Further preferably, in the step 2, the total height of the slurry in the cartridge is set to H, and the stability of the slurry is evaluated by using the material composition change rate of the slurry from 1/2 from the bottom height of the cartridge after measurement.
More preferably, in step 2, the setting time for the standing is 48 hours.
Further preferably, in step 3, the specified value of the material mass percentage change rate is selected according to the requirements of the cell production process
Further preferably, in step 3, the mass percentage change rate is obtained by the following formula:
P 1A ＝(M 1A -M 0A )/M 0A
wherein: p (P) 1A Is the mass percent change rate, M, of material A in the slurry taken at cross section 1 1A Is the mass percent of material a in the slurry taken at cross section 1; m is M 0A Is the actual mass percent of the a material when the slurry is formulated.
The invention adopts ICP-OES quantitative analysis and TG-MS quantitative analysis technology. ICP-OES refers to an inductively coupled plasma emission spectrometer, and can be used for qualitative and quantitative analysis of seventy metal elements and part of nonmetallic elements in samples in the aspects of geology, environmental protection, chemical industry, biology, medicine, food, metallurgy, agriculture and the like. TG-MS is an analytical method combining thermogravimetric loss (TGA) information with Mass Spectrogram (MS). TG is used to detect volatile components that escape from the system during heating by reheating the sample, which can decompose into gases due to the presence of volatiles or combustion.
The invention has the following advantages:
according to the method, the material composition of the battery slurry is detected by adopting ICP-OES and TG-MS quantitative analysis, the stability of the slurry is evaluated by utilizing the material proportion change rate of the slurry after standing, the detection accuracy is high, the material which plays a great role in the stability of the slurry can be clearly obtained, and the stability of a slurry system can be improved by adjusting the physicochemical property of the material.
Drawings
Fig. 1 is a flow diagram of one embodiment of a method of testing battery slurry stability.
Detailed Description
The following description of the embodiments of the present invention will be made more complete and clear by reference to the figures of the embodiments of the present invention, wherein the embodiments described are only some, but not all, of the embodiments of the present invention. It is to be understood that the present invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein, which are provided for a more thorough and complete understanding of the present invention. The drawings and examples of the present invention are for illustrative purposes only and are not intended to limit the scope of the present invention. Based on the embodiments of the present invention, those skilled in the art may obtain technical solutions without making any inventive effort, which fall within the scope of the present invention.
As shown in fig. 1, one embodiment of the method for evaluating the stability of a battery paste of the present invention specifically includes the steps of:
step 1, preparation of battery slurry: the electrode slurry with the known actual proportion which is just prepared or uniformly dispersed is placed in a charging barrel, sealed and kept stand, and the known actual proportion is taken as a theoretical value for subsequent comparison.
Step 2, detecting the components of the slurry: after standing for a certain time, taking out the slurry with fixed quality at the position of the cross section of the slurry with set height, and drying. Through digestion, filtration, dilution and constant volume, and then through ICP-OES quantitative analysis, the mass percentage of the material containing the metal elements can be obtained through calculation; and quantitatively analyzing the dried slurry through TG-MS, and calculating to obtain the mass percent of the binder, the conductive agent and the thickening agent. Thus obtaining the slurry proportion of the slurry with high height.
In this step, the standing time is set according to the production process of the battery cell, and the standing time is set to 48 hours in this embodiment.
In the step, the set height of the slurry is the position of the middle section under the combined influence of gravity and buoyancy, which can represent the stability of the whole slurry, and the total height of the slurry is preferably 1/2 of the cross section.
Preferably, a plurality of areas are taken for the same level, each area is measured, the plurality of measured values are averaged, and then the measured values are compared with a theoretical value, so that the evaluation accuracy can be improved.
Step 3, stability evaluation:
in the step, the actual measured proportion of the taken slurry is compared with a theoretical value, and when the mass percentage change rate of all materials is not more than a specified value, the stability of the slurry is considered to be good; if the percentage change rate of a certain material in a certain height is larger than a prescribed value, the slurry stability is considered to be poor. Here, the specified value of the material mass percentage change rate is selected according to the cell production process.
The mass percent change rate can be obtained by the following formula:
P 1A ＝(M 1A -M 0A )/M 0A
wherein: p (P) 1A Is the mass percent change rate, M, of material A in the slurry taken at cross section 1 1A Is a pulp taken at cross section 1The mass percentage of the material A in the material; m is M 0A Is the actual mass percent of the a material when the slurry is formulated.
In this embodiment, in order to make the measurement result more accurate, the slurry of the same cross-sectional area is sampled a plurality of times, and the component detection is performed on the withdrawn slurry, and the average value of the plurality of measured values is taken as the evaluation basis. For a plurality of samples to be compared, the mass percent of material of the slurry at the same height of the plurality of samples should be measured and the mass percent change rate of material in the slurry calculated.
Preferably, the total height of the slurry at the cartridge is set to H, and the stability of the slurry is evaluated by the material mass percent change rate of the slurry at 1/2H of the cross section from the bottom of the cartridge. The stability of the battery paste can be more accurately evaluated by using the percentage change rate of the mass of the material in the electrode paste within the cross-sectional area. The worse the slurry stability, the greater the rate of change of the mass percentages of the materials in the slurry of the cross section taken at 1/2H; if the slurry stability is good, the smaller the rate of change of the mass percent of each material in the slurry at 1/2H cross section.
Claims (10)
1. A method of testing the stability of a battery slurry, the method comprising:
step 1, preparation of battery slurry: placing the battery slurry which is just prepared or uniformly dispersed and has a known actual proportion into a charging barrel, and sealing and standing;
step 2, detecting the components of the slurry: taking out the slurry with fixed mass at the cross section of the slurry with set height after standing for set time, carrying out ICP-OES quantitative analysis and TG-MS quantitative analysis after processing, respectively calculating to obtain the mass percent of the material containing the metal elements, and calculating the mass percent of the binder, the conductive agent and the thickener to obtain the slurry proportion of the slurry in the region with set height, and then calculating the percentage of the material proportion;
step 3, stability evaluation: comparing the measured proportion of the slurry in the height area with a corresponding theoretical value, and considering that the slurry has good stability when the mass percent change rate of each material of the slurry proportion is not more than a specified value; if the mass percent change rate of the material is larger than the specified value, the slurry stability is considered to be poor, and the influence of the material on the slurry stability is larger.
2. The method for testing the stability of a battery slurry according to claim 1, wherein the treating of the slurry in step 2 comprises: drying, digestion, filtration, dilution and constant volume treatment are carried out.
3. The method for testing the stability of a battery slurry according to claim 1, wherein in the step 2, any area of the slurry having a predetermined height cross section is sampled, the sample of each area is measured, and the measured values are averaged and compared with a theoretical value.
4. A method for testing the stability of a battery paste according to claim 3, wherein in said step 2, the total height of the paste in the cartridge is set to H, and the stability of the paste is evaluated by using the material composition change rate of the paste measured from a certain height cross section from the bottom of the cartridge.
5. The method for testing the stability of battery slurry according to claim 4, wherein in the step 2, the stability of the slurry is evaluated by using a material mass percentage change rate of the slurry of a cross section at a height of 1/2H from the bottom of the cartridge.
6. The method for testing the stability of a battery paste according to claim 1, wherein in the step 2, the setting time for the standing is 48 hours.
7. The method according to claim 1, wherein in the step 3, the specified value of the material mass percentage change rate is determined according to the requirements of the cell production process.
8. The method for testing the stability of a battery slurry according to claim 1, wherein,
in the step 3, the mass percent change rate is obtained by the following formula:
P 1A ＝(M 1A -M 0A )/M 0A
wherein: p (P) 1A Is the mass percent change rate, M, of material A in the slurry taken at cross section 1 1A Is the mass percent of material a in the slurry taken at cross section 1; m is M 0A Is the actual mass percent of the a material when the slurry is formulated.
9. The method for testing the stability of a battery slurry according to claim 1, wherein,
in the step 3, when the mass percent change rate of each material taken in the cross section area of the set height is larger, the slurry stability is poorer; otherwise, the slurry has good stability.
10. The method of testing the stability of a battery slurry according to claim 1, wherein for a plurality of samples to be compared, the mass percent of each material of the samples of the slurry for a plurality of 1/2H height cross-sectional areas should be measured and the mass percent change rate of the material in the slurry calculated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310776256.0A CN116754542A (en) | 2023-06-28 | 2023-06-28 | Method for evaluating stability of battery slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310776256.0A CN116754542A (en) | 2023-06-28 | 2023-06-28 | Method for evaluating stability of battery slurry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116754542A true CN116754542A (en) | 2023-09-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310776256.0A Pending CN116754542A (en) | 2023-06-28 | 2023-06-28 | Method for evaluating stability of battery slurry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116754542A (en) |
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2023
- 2023-06-28 CN CN202310776256.0A patent/CN116754542A/en active Pending
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