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Visualizing Electrode Particle Degradation in Lithium-Ion Batteries with Tescan AMBER X 2

Multimodal characterization using FIB-SEM with integrated ToF-SIMS and Raman spectroscopy reveals the microstructural and chemical mechanisms behind capacity loss and internal resistance growth.

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How Degraded Electrode Particles Undermine Battery Performance

Driven by cycling, heat, and side reactions, electrode particle degradation is one of the leading causes of capacity loss and internal resistance growth in lithium-ion batteries. Graphite anodes exfoliate, cathode particles fracture, and lithium inventory is lost.

In this application note, Tescan demonstrates how AMBER X 2 Plasma FIB-SEM, equipped with STEM, ToF-SIMS, and Raman spectroscopy, enables precise characterization of structural and chemical changes in both anode and cathode materials. These insights support strategies for longer battery life and safer energy storage.

Why Study Electrode Degradation

with Tescan

01
Root of the Problem

Why Electrode Degradation Limits Battery Lifespan

Every charge and discharge cycle subtly alters the microstructure of electrode particles. Graphite anodes exfoliate as lithium intercalates between layers. Over time, this creates internal gaps and increases resistance. On the cathode side, NMC particles crack under mechanical and chemical stress, fragmenting and losing contact.

These failures not only reduce energy capacity but also promote side reactions and loss of lithium inventory. Because these processes occur at the micro- and nanoscale, precise tools are needed to study them in detail — both structurally and chemically.

02
Materials and Methods

Multimodal FIB-SEM and Correlative Chemical Analysis

Electrode degradation was studied in commercial graphite anodes and NMC cathodes using the Tescan AMBER X 2 Plasma FIB-SEM system. Samples were transferred from the glovebox via inert gas transfer. Imaging techniques included SEM, STEM, 3D FIB-SEM tomography, and 3D ToF-SIMS tomography.

Raman spectroscopy was also applied, all within the same platform. Lamellae for cross-sectional and TEM-level analysis were prepared in situ. This multimodal workflow enabled full correlation between surface features, internal microstructures, and chemical composition — information critical for degradation analysis.

03
Results and Discussion

Exfoliation, Fracturing, and Lithium Trapping Visualized in 3D

Graphite anodes showed clear exfoliation on both the surface and in TEM lamellae. 3D FIB-SEM and ToF-SIMS tomography revealed that lithium-based compounds accumulate in these regions, confirming loss of lithium inventory and active materials due to graphite particle degradation. NMC cathodes, analyzed via cross section and Raman mapping, showed fractured particles and clear signs of inhomogeneous cycling behavior.

Raman spectra revealed peak broadening and shifts indicating internal stress and non-uniform lithium distribution. Some particles were inactive — not participating in cycling — further reducing capacity. These results confirm the value of multimodal analysis for guiding material improvements and battery lifespan extension strategies.

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Tescan Instruments & Technology

Used in This Workflow

Tescan AMBER X 2

Tescan AMBER X 2 combines plasma FIB milling with ultra-high-resolution SEM and integrated chemical analysis tools — ideal for studying electrode materials at every scale.

  •  Field-free UHR SEM with low-kV imaging for surface-sensitive features 

  • Plasma FIB for fast volume sectioning and lamella preparation

  • Integrated STEM for nanometer-scale subsurface analysis

  • Compatible with inert atmosphere transfer for air-sensitive samples 
AMBER-X2

Tescan ToF-SIMS and Raman Spectroscopy – Integrated Chemical Mapping Tools

Integrated into the AMBER X 2 platform, these tools reveal material composition, lithium distribution, and cycling-induced changes.

  • Identification of lithium compounds inside degraded regions using 3D ToF-SIMS tomography

  • Structural disorder and inactive particle mapping with Raman spectroscopy

  • Correlation of morphology, defect sites, and chemical evolution 

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Tescan
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130405923 us US 37.09024 -95.712891 25.3575 29.349345 20.67957527 42.082797 39.91384763 -33.693421 13.93320106 3.039986586 31.997988 38.050985 47.579533 48.1485965 58.375799 54.663142 19.195447 56.975106 50.493053 45.868592 10.79556993 44.35660598 43.2371604 55.536415 14.557577179752773 32.100937 -6.116829 -6.212299277967318 23.7104 -33.471062 31.998740087 -23.69149395 43.462349 51.529848 49.1893523 49.197486 25.072375 31.075811 1.299027 40.676979 52.30150662 51.013813 35.684121 37.479653 52.246622 40.581349 39.911632 -26.1811371 41.818215 33.429928 -12.08688

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