Choose the Right Instrument for Your Battery Analysis

Guide to Lithium-ion Battery Solutions C10G-E092 Guide to Lithium-ion Battery Solutions C10G-E092 2 3 Test / Evaluation Items Test / Evaluation Items (Detail) Instrument Application Example Material Testing Compression Test Micro Compression Tester MCT Compression test of positive electrode active materials P6 Compression test of solid electrolyte raw materials P7 Tensile Test Puncture Test DIC Analysis AUTOGRAPH Precision Universal Tester AG Tensile test of the separator P8 Tensile strength measurement of the separator P9 Puncture strength measurement of the separator P10 Evaluating the strain characteristics of separators after puncture damage P11 Thermal Analysis Evaluation of Meltability Differential Scanning Calorimeter DSC Evaluation of decomposition characteristics and thermal stability of each component P12 Determination of the melting temperature and calorimetry of separators P13 Moisture Measurement Thermogravimetric Analyzer TGA Measurement of moisture content in the electrode active material P14 Heat Shrinkage Measurement Thermomechanical Analyzer TMA Measurement of the shrinkage of the separator P15 Organic / Inorganic Component Analysis Component Analysis Internal Gas Component Analysis Estimated Amount of Internal Gas Generated Deterioration Evaluation Fourier Transform Infrared Spectrophotometer FTIR Comparison of spectra under argon and atmospheric atmospheres P16 Component analysis of electrolytes and solvents used in electrolyte solution P17 Ion Chromatograph IC Deterioration evaluation of electrolyte solution P18 Gas Chromatograph/ Single Quadrupole GC-MS GC/GCMS Analysis of the solvents used in electrolyte solution and component analysis of additives P19 Simultaneous analysis of internal gas P20 Confirmation of changes in gas composition due to deterioration P21 Test / Evaluation Items Test / Evaluation Items (Detail) Instrument Application Example Internal Structure Evaluation Internal Structure Observation Non-Destructive Inspection In-situ Observation (charge / discharge, stress) Microfocus X-Ray CT System SMX Non-destructive observation of the current collector and of the lower part of the battery P22 Internal observation of cells that have been charged and discharged 100 to 1500 times P23 Non-destructive observation of the internal structure of an exploded Lithium-ion Battery P24 Non-destructive observation of an internal structure before and after a charge / discharge test P25 Microanalysis Observation and Elemental Mapping Analysis and Chemical Bonding State Analysis of Minute Parts Electron Probe Microanalyzer EPMA Observation and elemental analysis of minute parts of the positive electrode cross section P26 Evaluate the chemical bonding state of the active material of the positive electrode P27 Observation of Surface Shape and Evaluation of Physical Properties of Minute Parts In-situ Observation (in Liquid / Heating) Scanning Probe Microscope/ Atomic Force Microscope SPM/AFM Observation of the surface shape and measurement of the potential distribution of minute parts of the positive electrode P28 Surface shape observation and force curve measurement of the binder in electrolyte solution P30 Particle Characterization Particle Size Measurement Laser Diffraction Particle Size Analyzer SALD Particle size measurement of electrode materials P32 Particle Size Measurement and Image Analysis Dynamic Particle Image Analysis System DIA Particle size measurement and image analysis of active materials P33 Table of Contents (Test / Evaluation Item) Click here for Table of Contents (Unit) 4 5 Material Instrument Application Example Positive Electrode Active Material / Conductive Additive / Binder Micro Compression Tester MCT Compression test of active materials P6 Differential Scanning Calorimeter DSC Evaluation of the decomposition characteristics and thermal stability of each component P12 Thermogravimetric Analyzer TGA Measurement of moisture content in the active material P14 Electron Probe Microanalyzer EPMA Observation and elemental mapping analysis and chemical bonding state analysis of minute parts P26 Scanning Probe Microscope / Atomic Force Microscope SPM/AFM Observation of the surface shape and measurement of the potential distribution of minute parts P28 Surface shape observation and force curve measurement of the binder in electrolyte solution P30 Laser Diffraction Particle Size Analyzer SALD Particle size measurement of electrode materials P32 Dynamic Particle Image Analysis System DIA Particle size measurement and image analysis of electrode materials P33 Negative Electrode Active Material / Conductive Additive / Binder Micro Compression Tester MCT Compression test of active materials P6 Differential Scanning Calorimeter DSC Evaluation of decomposition characteristics and thermal stability of each component P12 Thermogravimetric Analyzer TGA Measurement of moisture content in the active material P14 Electron Probe Microanalyzer EPMA Observation and elemental mapping analysis and chemical bonding state analysis of minute parts P26 Scanning Probe Microscope / Atomic Force Microscope SPM/AFM Observation of the surface shape and measurement of the potential distribution of minute parts P28 Surface shape observation and force curve measurement of the binder in electrolyte solution P30 Laser Diffraction Particle Size Analyzer SALD Particle size measurement of Electrode Materials P32 Dynamic Particle Image Analysis System DIA Particle size measurement and image analysis of electrode materials P33 Material Instrument Application Example Separator AUTOGRAPH Precision Universal Tester AG Tensile test of the separator P8 Tensile strength measurement of the separator P9 Puncture strength measurement of the separator P10 Evaluating the strain characteristics of separators after puncture damage P11 Differential Scanning Calorimeter DSC Determination of the melting temperature and calorimetry of separators P13 Thermomechanical Analyzer TMA Measurement of the shrinkage of the separator P15 Electrolyte Solution Solvent / Electrolyte / Additive Fourier Transform Infrared Spectrophotometer FTIR Comparison of spectra under argon and atmospheric atmospheres P16 Component analysis of electrolytes and solvents used in electrolyte solution P17 Ion Chromatograph IC Deterioration evaluation of electrolyte solution P18 Gas Chromatograph/ Single Quadrupole GC-MS GC/GCMS Analysis of the solvents used in electrolyte solution and component analysis of additives P19 Solid Electrolyte Micro Compression Tester MCT Compression test of solid electrolyte raw materials P7 Electron Probe Microanalyzer EPMA Observation and elemental mapping analysis and chemical bonding state analysis of minute parts P26 Scanning Probe Microscope / Atomic Force Microscope SPM/AFM Observation of the surface shape and measurement of the potential distribution of minute parts P28 Laser Diffraction Particle Size Analyzer SALD Particle size measurement of electrode materials P32 Battery cell Module / Internal Gas Microfocus X-Ray CT System SMX Non-destructive observation of the current collector and of the lower part of the battery P22 Internal observation of cells that have been charged and discharged 100 to 1500 times P23 Non-destructive observation of the internal structure of an exploded Lithium-ion Battery P24 Non-destructive observation of the internal structure before and after a charge / discharge test P25 Gas Chromatograph/ Single Quadrupole GC-MS GC/GCMS Simultaneous analysis of internal gas P20 Confirmation of changes in gas composition due to deterioration P21 Table of Contents (Unit) Click here for Table of Contents (Test / Evaluation Item) 6 7 index index Compression test of various materials that construct a Lithium-ion Battery Test force-displacement graph • Consideration of conditions for battery packaging and restraint pressure • Examination of manufacturing process conditions (change in strength during heating) Micro Compression Tester MCT Series Inner structural materials of a Lithium-ion Battery are subjected to external force during production processes and to pressure during use. Therefore, evaluating the strength of each structural material is important to maintain consistent quality. Below are the results of compression tests performed on Lithium-ion Battery materials using the Micro Compression Testing Machine. Compression Test Results Sample Name Fracture strength [mN] Particle size [µm] Strength [MPa] LiMn2O4 1.67 13.0 7.79 LiCoO2 16.23 13.3 72.75 The force is on the vertical axis, the displacement is on the horizontal axis, and fracture occurs at the inflection point where the displacement becomes horizontal. The fracture strength of the lithium cobalt oxide LiCoO2 particle was measured to be 72.75 MPa compared to 7.79 MPa for the lithium manganese oxide, LiMn2O4. Compression test of positive electrode active materials Two types of positive electrode active materials Before After Compression Test Results Sample Name Fracture strength [mN] Particle size [µm] Strength [MPa] A 1.25 1.765 315 B 0.63 4.265 27 By measuring the fracture strength, we can compare the correlation with the ease of molding as an electrolyte. Comparing particles A and B shows that the fracture strength of particle B is about 1/10 weaker. This indicates that the particles adhere well to each other during the molding process. Compression test of solid electrolyte raw materials Two types of solid electrolyte raw materials Purpose Samples Data Result Purpose Samples Data Result Test force-displacement graph Displacement (μm) Force (mN) Displacement (μm) Force (mN) Click here for product page Click here for product page Material Testing 8 9 index index The separator is installed so that it is in contact with the positive and negative electrodes. Since the temperature rises during charging, it is necessary to maintain mechanical strength even as the temperature changes. The following shows an example of measuring how the strength of a separator in the tensile test and the piercing test changes with respect to temperature changes, and an example of evaluating the strain characteristics after piercing damage. Tensile Test Results Specimen Lithium Battery Separator Specimen Name A B C Elastic Modulus (MPa) 902 1856 1376 Tensile Strength (MPa) 165 118 101 Break Point Strain (%) 27.6 31.7 29.1 From the measurement results, it can be seen that the separator with high tensile strength is A. Tensile test of separator Three types of separators Separator (1) is produced by near uniaxial stretching in the machine direction (MD), and separator (2) is produced by biaxial stretching at a low stretching ratio. Despite the increase in elongation properties at 60°C, excellent mechanical strength is maintained. Tensile strength measurement of a separator (Condition : 25 °C, 60 °C, and 90 °C) Two types of separators, prepared in dumbbell shapes along both the length and width direction Purpose Samples Data Result Samples Purpose Data Result Specimen Lithium Battery Separator Specimen Name A B C Thickness (µm) 20 20 10 Stress-strain graph Mechanical properties of separator (1) and (2) in the short side and long side directions Long side: Machine Direction Short side: Transverse Direction 25 °C 60 °C 90 °C Sample Tensile strength (MPa) Rupture strain (%) Tensile strength (MPa) Rupture strain (%) Tensile strength (MPa) Rupture strain (%) (1)Short side 36.9 471.4 35.4 898.8 19.3 1044.0 (1)Long side 175.6 26.8 162.5 57.0 129.9 76.7 (2)Short side 78.2 138.5 68.8 347.6 33.8 427.9 (2)Long side 129.5 34.1 118.3 105.3 58.7 367.2 Strength measurement and strain characteristic evaluation of a separator at high temperature • Various mechanical strength measurements of Lithium-ion Battery materials • Evaluation of the piercing strength of a separator packed with high density • Visualization of strain distribution by DIC analysis AUTOGRAPH Precision Universal Tester AGX-V Stress-strain graph Separator (1) Separator (2) Click here for product page Click here for product page Material Testing 10 11 index index Strain distribution under tensile load We evaluated the strain characteristics of a separator after puncture to investigate how a damaged separator may act under stress. DIC analysis is a method of comparing random patterns on the surface of an object before and after the object is deformed to determine the amount of pattern movement and measure strain. Using the DIC analysis method, we can visually see that the area around the damaged area in the center turns red where stress is concentrated and strain is the largest. Evaluating the strain characteristics of separators after puncture damage Separator after puncture test Test Force-Displacement Curve Comparing the results at 25 °C and 60 °C, we can see that the maximum test force is the same, but the maximum displacement value is higher at 60 °C. Next, comparing the characteristic values at 60 °C and 90 °C, we can see that the maximum test force decreases at 90 °C, but the maximum displacement is the same. From the above, it can be seen that the lithium-ion battery separator used in this test has an increase in elongation characteristics but no decrease in strength at 60 °C. Puncture strength measurement of a separator (Under environment of 25 °C, 60 °C, 90 °C) Separator Maximum Test Force / Displacement for Each Temperature Test Temperature (°C) Maximum Test Force (N) Maximum Displacement (mm) 25 3.85 4.45 60 4.07 6.63 90 2.13 6.68 Purpose Samples Data Result Purpose Samples Data Result Click here for product page Click here for product page Material Testing Puncture location Mark 12 13 index index DSC Measurement of Electrode Active Materials DSC Measurement of Separators In some cases, lithium-ion batteries may generate abnormal heat due to overcharging, which may lead to problems such as ignition, in the worst case. To ensure the safety of the battery, it is important to evaluate the decomposition characteristics and thermal stability of each component by DSC during heating. The upper curve shows the active material after charging. The active material becomes unstable due to charging, and a large exothermic peak due to decomposition is observed from around 200 °C. The exothermic peak around 290 °C is thought to be from the electrolyte. Evaluation of decomposition characteristics and thermal stability of each component Charged/Uncharged electrode active material and electrolyte solution The endothermic peaks were observed at around 100 °C to 140 °C, which is expected to be the melting point of polyethylene. When the separator is exposed to high temperature, it shrinks near the melting temperature, which affects the insulation. For safety reasons, it is necessary to know the temperature at which the separator contracts, and the measurement of the melting temperature by DSC is an indicator of the contraction temperature. Determining the melting temperature and calorimetry of separators Three types of separators Purpose Samples Data Result Purpose Samples Data Result Evaluate the decomposition characteristics and thermal stability of battery materials during heating • Examination of Lithium-ion Battery safety • Selection of compound for electrode material and selection of compounding conditions • Evaluation of physical properties of polymer materials by crystallinity Differential Scanning Calorimeter DSC-60 Plus Click here for product page Click here for product page Thermal Analysis 14 15 index index Moisture evaluation during heating of electrode active material Evaluation of shrinkage amount when the separator is heated TGA Measurement of Electrode Active Materials TMA Measurement of Separators It is important to control the moisture content in lithium-ion batteries because it affects their lifetime. The moisture content of a material can be measured using a thermogravimetric analyzer (TGA). In general, the higher the shrinkage temperature and the smaller the amount of shrinkage, the safer it is. Thermomechanical analysis (TMA) was used to measure mainly the shrinkage of the separator. A weight loss rate at 200 °C was determined, and the moisture content was 0.033% and 0.214%, respectively. According to the data, the start of shrinkage begins approximately between 80 °C and 100°C. In terms of the amount of shrinkage, the amount of shrinkage is larger in the MD direction than in the TD direction for both No. 1 and 2 . Measurement of moisture content in the active material Positive/Negative electrode active material Measure the shrinkage of the separator The two directions of the separator called the MD (machine direction) and TD (transverse direction) Purpose Samples Purpose Samples Data Data Result Result • A small amount of water content can be detected • Evaluation of connectivity by measuring the dehydration process temperature • Measurement is possible in the atmosphere of air or nitrogen • It is possible to measure the amount of shrinkage and shrinkage stress at each temperature • Continuous recording of a sample's dimensional changes as temperature changes or over time in the order of µm • Tensile measurement, expansion measurement, and needle insertion measurement are possible with one unit Thermogravimetric Analyzers TGA-50 series Thermomechanical Analyzer TMA-60 Click here for product page Click here for product page Thermal Analysis 16 17 index index Infrared Spectra of EC+DEC (3 : 7) Electrolyte Solution Containing 1M LiPF6 Infrared Spectra of EC+DEC (3 : 7) Electrolyte Solution Containing 1M LiPF6 (red) and EC+DEC (3 : 7) Solution (black) Difference Spectrum between EC+DEC (3 : 7) Electrolyte Solution Containing 1M LiPF6 and EC+DEC (3 : 7) Solution It is desirable to handle and characterize the cell components under an atmosphere not affected by water vapor or oxygen. The IRSpirit, a compact FTIR, can be installed in a glove box, thus enabling the evaluation of cell components in a high-purity argon atmosphere with low dew point and low oxygen concentration. Although the optical properties of argon and air are very different, the left image shows that the infrared spectra acquired under both atmospheres were almost identical, appearing to be unaffected by the difference in atmosphere. Note that in the right image, the broad absorption of symmetric and antisymmetric OH-stretching vibrations from water molecules were observed between 3400 and 3700 cm-1 in the air atmosphere. Meanwhile, the influence was negligible in the infrared spectrum in the argon atmosphere. Comparison of spectra under argon and air atmospheres EC+DEC (3 : 7) Electrolyte Solution Containing 1M LiPF6 1M LiPF6 : Lithium Hexafluorophosphate EC : Ethylene Carbonate DEC : Diethyl Carbonate Purpose Samples Data Result The red and black arrows on the left are characteristic absorptions of each component. To clarify the difference between the two spectra, the red line minus the black line is shown on the right. In the frequency range of 700 ~ 1000 cm -1, characteristic vibrational modes in which EC or DEC and lithium ions are solvated are observed. Therefore, it can be assumed that the four absorption lines shown in the right figure are characteristic absorption lines in which EC or DEC and lithium ions are solvated. The data shown above was provided by Associate Professor Takashi Ito at Frontier Research Institute for Interdisciplinary Sciences, Tohoku University. We would like to take this opportunity to express our sincere gratitude. Please also see the article in FTIR TALK LETTER Vol. 35. Spectrum comparison in the presence and absence of LiPF6 EC + DEC (3: 7) Electrolyte Solution (Containing 1M LiPF6) EC + DEC (3: 7) Electrolyte Solution (Not containing 1M LiPF6) 1M LiPF6 : Lithium Hexafluorophosphate EC : Ethylene Carbonate DEC : Diethyl Carbonate Samples Purpose Data Result *Since IRSpirit can be controlled wirelessly, a sample can be measured while the FTIR unit is installed in a glove box (custom order required). Evaluation of electrolyte solution in an inert atmosphere • Raw material confirmation, foreign matter screening analysis • Small design allows it to be used in glove boxes and draft chambers Fourier Transform Infrared Spectrophotometer IRSpirit™ Click here for product page Click here for product page Organic / Inorganic Component Analysis 18 19 index index Comparison of components between new and deteriorated electrolyte solutions Lithium hexafluorophosphate is commonly used as the electrolyte solution. It is hydrolyzed by the trace amount of water contained in the electrolyte solution. Fluoride ions generated by this decomposition affect battery performance, so analysis of decomposition is important in the quality control process. The electrolyte solution in a Lithium-ion Battery is composed of organic solvent (mainly carbonate-based), electrolyte and additives. It is important to evaluate the electrolyte solution and the deterioration state of the electrolyte solution due to charging and discharging. GCMS is useful for the analysis of those constituents. A peak was not detected in the new electrolyte solution (New), but only in the deteriorated electrolyte solution (Degraded Product). Dimethyl carbonate, ethyl methyl carbonate, and ethylene carbonate, which are used as solvents, were identified from library search results. Vinylene carbonate, which was used as an additive, was also identified. Evaluation of Lithium Hexafluorophosphate Decomposition in Electrolyte Solution Solvents used in electrolyte solution and component analysis of additives Electrolyte Solution (New, deteriorated: accelerated deterioration test) Electrolyte Solution Purpose Samples Purpose Samples Result Result Chromatogram of Electrolyte Solution (New) Chromatogram of Electrolyte Solution (Degraded Product) Data Data • Evaluation of products generated by decomposition of electrolyte • Shorten analysis time by utilizing a column switching system • Evaluation of reaction products generated by deterioration • Qualitative analysis of unknown components that cannot be identified only by retention time information Ion Chromatograph HIC-ESP Single Quadrupole GC-MS GCMS-QP™2020 NX Qualitative analysis of solvents and trace additives used in electrolyte solutions Click here for product page Click here for product page Organic / Inorganic Component Analysis 20 21 index index Component analysis of internally generated gas and deterioration evaluation due to charging and discharging It is necessary to analyze the internally generated gas when conducting a deterioration evaluation of a Lithium-ion Battery. We will introduce an example of simultaneous analysis of internal gas using a system equipped with the unique BID detector. It eliminates the need for carrier gas switching and the combined use of multiple devices, which was required in the past, and enables easier and faster measurement. The GC-BID enables simultaneous analysis of inorganic gas components (H2, O2, N2, CO, CO2) and lower hydrocarbon components (CH4, C2H4, C2H6, C3H6, C3H8) in the battery. Simultaneous analysis of internal gas Internal gas Purpose Samples Result Simultaneous analysis of internal gas Data Changes in the composition of internal gas due to deterioration As the capacity retention rate decreases, the ratio of hydrogen decreases and the ratio of hydrocarbon increases. Confirmation of changes in gas composition due to deterioration Internal gas obtained from four batteries with different capacity retention rates Purpose Samples Data Result • BID (Barrier-discharge Ionization Detector) is more sensitive than TCD, and can deal with objects that cannot be detected by FID • Detect inorganic gases and hydrocarbons simultaneously • Qualitative analysis when combined with GCMS Gas Chromatograph Nexis™ GC-2030 Component Concentration Ratio (%) Click here for product page Click here for product page Organic / Inorganic Component Analysis 22 23 index index Non-destructive observation of internal structures and deterioration evaluation after charging and discharging The X-ray CT device can observe the internal structure non-destructively. Therefore, it is used for analysis of defective products, comparison of non-defective products / defective products, comparison before and after charging / discharging, and observation of internal structures in cycle tests. In many cases, it is used for finished battery products. It is also used for observing the three-dimensional structure of minute parts such as electrodes. The green frame is the positive electrode current collector, the red frame is the negative electrode current collector, and the blue frame is the X-ray CT image of the lower part of the battery. You can see in detail how the negative electrode is bent. Non-destructive observation of the current collector and of the lower part of the battery Large Lithium-ion Battery for a vehicle. W114mm×D48mm×H184mm Purpose Samples Result The X-ray CT image of a large Lithium-ion Battery for a vehicle Data Cross-sectional image of a Lithium-ion Battery in a charge-discharge cycle test (100 ~ 1500 times) This data shows results from repeatedly charging and discharging the Lithium-ion Battery and scanning at 100 times, 500 times, 1000 times, and 1500 times. Because X-ray CT can observe the inside non-destructively, it is not necessary to prepare a lot of samples for a cycle test. Therefore, it is possible to track the state changes over time for the same sample. Internal observation of cells that have been charged and discharged 100 to 1500 times Small-capacity Lithium-ion Battery that has been charged / discharged Purpose Samples Data Result • Non-destructive internal observation is possible • Data can be confirmed immediately after shooting by high-speed calculation • Confirmation of detailed parts with a high-resolution detector Microfocus X-Ray CT System inspeXio™ SMX™-225CT series Click here for product page Click here for product page Internal Structure Evaluation 24 25 index index セル内部構造の非破壊観察および充放電後の劣化評価 The cross-sectional image of an 18650 type Lithium-ion Battery before and after a charge / discharge test is shown. As shown in the red circles, you can see a deformation near the center of the battery due to expansion and contraction of the inside caused by charging and discharging. Even if the battery has no problem in appearance, it’s possible to observe any internal deformations using X-ray CT. Non-destructive observation of an internal structure before and after a charge / discharge test An 18650 type Lithium-ion Battery You can see that the inside is greatly deformed by the explosion. With X-ray CT, it is possible to observe the condition without destroying it, so it is possible to exactly confirm what kind of deformation has occurred from a load test. Non-destructive observation of the internal structure of an exploded Lithium-ion Battery An 18650 type Lithium-ion Battery that was overcharged, heated, and exploded Purpose Samples Data Result Purpose Samples Result Cross-sectional image inspeXio™ SMX™-225CT FPD HR Plus with attached charge / discharge system Cross-sectional image of 18650 type Lithium-ion Battery before and after a charge / discharge test 3D image (movie) Data Charge / discharge instrument Click here for product page Click here for product page Internal Structure Evaluation 26 27 index index Observation of minute parts of the positive electrode, elemental analysis and chemical bond state analysis A positive electrode has a structure in which a mixture of the active material, binder, and conductive additive are coated on a collector made of aluminum foil. Evaluation of the distribution of these components is important to improve cell performance and quality control, and when conducting failure analysis. Above data is the result of a mapping analysis of the positive electrode cross section. Not only coarse particles with sizes of several μm, but also fine particles with sizes of less than 1 μm, the condition of boundaries and the element distribution can be observed. Observation and elemental analysis of minute parts of a positive electrode's cross section Positive electrode active material Purpose Samples Result Element mapping analysis of the cross section of a positive electrode Data State analysis of the positive electrode surface Spectrum of Mn on Positive Electrode Surface and Enlarged View of Peak Tops The difference shown in the spectrum is due to a peak shift between the initial state and the charged state. EPMA can detect changes in the state of chemical bonds aimed at small parts. Evaluate the chemical bonding state of the active material of a positive electrode Comparison of initial state and charged state Purpose Samples Data Result Samples were provided by the National Institute of Advanced Industrial Science and Technology Samples were provided by the National Institute of Advanced Industrial Science and Technology • Both high sensitivity and high spatial resolution are achieved due to excellent electron probe characteristics • Chemical bond state analysis of minute parts is possible • Wide area mapping by stage scan Electron Probe Microanalyzer EPMA™-8050G Initilal State Charged State Click here for product page Click here for product page Microanalysis 28 29 index index Observation of the shape of minute areas of battery material and measurement of conductive distribution Positive and negative electrodes contain active materials, conductive aids, and binders. In order to improve the conductivity between the active materials, a conductive aid is added, and each is bound and held by a binder. Evaluating how these elements are distributed in the positive electrode and how conductive paths are formed helps improve the performance of Lithium-ion Batteries. We observed the surface shape and current distribution by measuring the minute amount of current flowing through the conductive cantilever while applying a voltage to the positive electrode. We observed the surface shape and current distribution by measuring a minute amount of current flowing through the conductive cantilever while applying a voltage to the positive electrode. From the topography image, it is not possible to determine where conductive aids, active materials, and binders are. However, in the current image, you can see the three areas of red, yellow-green, and blue in order of conductivity. It can be estimated that the red areas are conductive additives, the yellow-green areas are active materials, and the blue areas are binders. This data compares EPMA and SPM data within the same area. EPMA evaluates the distribution of elements whereas SPM evaluates the distribution of shape and conductivity. By analyzing the state of materials from multiple instruments, it is possible to evaluate the uneven distribution and isolated state of a battery's material components, which can help with quality improvement and product development. Evaluation of element distribution and conductivity distribution in the same field of view Positive electrode sheet of the NCM (lithium nickel manganese cobalt oxide) Result Samples Purpose Data Result Observation of surface shape and measurement of potential distribution of minute parts of a positive electrode Positive electrode sheet of the NCM (lithium nickel manganese cobalt oxide) Purpose Samples Data Applied Voltage : -2.7V Topography Image Current Image (Low Contrast) Current Image (High Contrast) • Observation near the interface and grasp of physical properties • Confirmation of the conductivity of minute parts • Observation of minute parts and evaluation of physical properties are possible the air atmosphere Scanning Probe Microscope SPM-Nanoa™ Click here for product page Click here for product page Microanalysis 30 31 index index 各種部材の微小領域の形状観察および導電性分布測定 The deflection of the cantilever was measured when the probe was pushed into the sample by about 15 nm, and a force curve was obtained. Point B on the force curve indicates the start of the depression, and point A indicates a 15 nm depression from point B. The amount of binder deformation can be obtained from the difference between the amount of indentation and the amount of deflection from point B to point A. From the data obtained, the amount of binder deformation indicates that (2) is the least rigid and (3) is the most rigid. It was confirmed that the flat binders (2) and (3) were uniformly gelled in the electrolyte. SPM enables observation of an electrolyte in a real-world environment! Result Result Data Data Surface shape observation in electrolyte solution Force curve measurement in electrolyte solution Binder for negative electrode Binder for negative electrode Samples Samples Purpose Purpose Sample Provision:Komaba Lab of Tokyo University of Science Protuberant Flat Flat (1) (3) (2) Sample Provision:Komaba Lab of Tokyo University of Science (1) (2) (3) Click here for product page Click here for product page Microanalysis 32 33 index index Carbon black particle size and dispersion / aggregation evaluation The grain size and grain size distribution of carbon black have a great influence on an electrode's characteristics and the quality and yield of the final product. For proper evaluation, it is important to know the dispersion / aggregation state of the target sample. SALD-2300 realizes highly sensitive measurement of scattered light, and can perform highly reliable measurement even with weak scattered light from primary particles after dispersion processing. It can be seen that by the homogenizer dispersion treatment, aggregates of about 10 μm are dispersed in the fine particles in the submicron region. Particle size distribution measurement of particles with different dispersed states Carbon black particle Purpose Samples Result Measurement of dispersed solvent Data Particle size distribution measurement and shape confirmation of active material particles DIA can detect trace amounts of coarse particles. By detecting coarse particles in the positive electrode material powder, it is possible to prevent deterioration of Lithium-ion Battery performance and improve safety. Coarse particles in powder used for a positive electrode can lead to performance issues and degradation of the material. These particles can be detected and distinguished either through the image analysis window or a plot based on specific parameters. This allows the quality of the powdered raw material to be easily verified. Detection of coarse particles contained in positive electrode material Positive electrode material powder Purpose Samples Result Data • Black samples that easily absorb light can be detected • Analysis while maintaining the state of slurry • Monitoring of aggregation and dispersion status • Abnormal particles (foreign matter, agglomeration) are detected • Acquire images of individual particles and check the shape • Detect trends and abnormal values by statistical analysis Laser Diffraction Particle Size Analyzer SALD-2300 Dynamic Particle Image Analysis System iSpect™ DIA-10 Click here for product page Click here for product page Particle Characterization Guide to Lithium-ion Battery Solutions © Shimadzu Corporation, 2022 / First Edition: June 2022, 3655-01210-PDFIT, C10G-E092 www.shimadzu.com/an/ For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. Company names, products/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation, its subsidiaries or its affiliates, whether or not they are used with trademark symbol “TM” or “®”. Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “®”. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own. The contents of this publication are provided to you “as is” without warranty of any kind, and are subject to change without notice. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication.