# Seeing inside a working battery

> Battery characterisation set-ups on one page: an operando X-ray diffraction cell, XPS of the SEI without air with sputter depth profiling, synchrotron X-ray tomography of an 18650 cell, neutron imaging of gas in a pouch cell, operando neutron diffraction of a cylindrical cell, and why neutrons see lithium. The set-ups and numbers are quoted from the cited papers; no panel is measured data.

- Page: https://www.labcanvas.com/templates/energy-storage-guides/seeing-inside-working-battery
- Open in the LabCanvas editor (LabCanvas account): https://www.labcanvas.com/editor.html?template=battery-characterisation-inside
- Updated: 2026-10-14
- Category: Battery & energy storage guides
- Method: Operando and post-mortem imaging
- Product: Operando diffraction, XPS, X-ray tomography and neutron set-ups for working cells
- Key result: Instruments and cells drawn by LabCanvas after the cited set-ups; no panel is a diffraction pattern, spectrum, radiograph or tomogram, and beams, distances and windows are drawn, not to scale
- Figure: 1920 × 1080 px, 45 editable layers (6 generated objects with settings)

## Steps

1. **Operando diffraction**: An operando cell that closely mimics a standard coin cell works in reflection mode on a conventional powder X-ray diffractometer, so both anode and cathode materials can be studied; it uses graphite as the X-ray window instead of beryllium, and was tested on Li₄Ti₅O₁₂, LiMn₂O₄ and a layered sodium-ion cathode (Shen 2014). In transmission, a single-layer pouch cell with Mo Kα radiation followed the phase evolution of an NCM811 cathode (Shao 2025); standard cells have to be customised for operando diffraction (Bianchini 2015)
2. **XPS without air**: Cells are opened in an argon-filled glovebox and the electrodes moved to the XPS chamber in a transfer box (Shao 2025) or by vacuum transfer (Xiao 2014). Intense 13-step sputter depth profiling with a polyatomic ion gun gave a detailed model of the SEI on the graphite anode of commercial NMC/graphite cells, though charging under the X-ray beam means compounds cannot be assigned from binding energies alone (Niehoff 2013); cryo-XPS with argon gas-cluster ions profiled the vitrified wet SEI of lithium metal, graded from LiF and lithium carbonate on the electrolyte side to lithium oxide and carbide next to the electrode (Wang 2025)
3. **X-ray tomography**: At ESRF beamline ID15A a 76 keV monochromatic beam imaged LG 18650 NMC cells during thermal runaway: radiographs at 1,250 frames per second and tomograms at 2.5 Hz (500 projections) or 1.25 Hz (1,000 projections) as the cell turned continuously through 360°; steel and copper attenuate most and show white, NMC bright grey. Gas pockets formed between the electrode layers once the shell passed 100 °C, delaminating them (Finegan 2015). X-ray CT shows lithium diffusion only indirectly, neutron CT directly (Ziesche 2020)
4. **Neutron imaging**: Neutrons pass through the operating cell and the change in transmission gives a radiograph: lithium and hydrogen scatter neutrons strongly while aluminium, carbon and nickel interact only weakly, so the hydrocarbon-based electrolyte makes evolving gas visible. At ICON (SINQ), cold neutrons of 3–10 Å through a 7.1 m flight tube and a 2 cm aperture gave one 10 s image every minute; the gas collected at the edges of the pouch (Michalak 2015)
5. **Neutron diffraction**: Operando neutron powder diffraction at NOMAD (SNS): a customised NMC622 || graphite cylindrical cell, its jelly roll in a thin-walled quartz tube, charged from 0.27 C to 4.4 C with a pattern every 62 s; the stage II → stage I transition of the graphite was rate-limiting in fast charging. Neutrons penetrate without heating the cell and see light elements, but hydrogen-rich electrolyte adds incoherent scattering (Wu 2021); they are sensitive to lithium site occupancy (Bianchini 2015)
6. **Why neutrons see lithium**: The X-ray absorption cross-section increases with the atomic number, while the neutron cross-section varies non-linearly across the periodic table: lithium and hydrogen scatter neutrons strongly, while aluminium, carbon and nickel interact only weakly (Michalak 2015)

## Strengths

- A coin-like operando cell runs on a conventional powder diffractometer (Shen 2014)
- Radiographs at 1,250 frames per second follow thermal runaway as it happens (Finegan 2015)
- Neutrons see lithium and hydrogen strongly (Michalak 2015)

## Limitations

- Charging under the X-ray beam means XPS compounds cannot be assigned from binding energies alone (Niehoff 2013)
- Hydrogen-rich electrolyte adds incoherent neutron scattering (Wu 2021)
- Standard cells have to be customised for operando diffraction (Bianchini 2015)

## References

1. Shen et al., “An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer”, Rev. Sci. Instrum. 2014. https://doi.org/10.1063/1.4896198 (primary)
2. Shao et al., “Multiscale interfacial stabilization via prelithiation separator engineering for Ah-level anode-free lithium batteries”, Nat. Commun. 2025. https://doi.org/10.1038/s41467-025-59521-8 (primary)
3. Bianchini et al., “Spinel materials for Li-ion batteries: new insights obtained by operando neutron and synchrotron X-ray diffraction”, Acta Crystallogr. B 2015. https://doi.org/10.1107/S2052520615017199 (primary)
4. Xiao et al., “Unraveling manganese dissolution/deposition mechanisms on the negative electrode in lithium ion batteries”, Phys. Chem. Chem. Phys. 2014. https://doi.org/10.1039/c4cp00833b (primary)
5. Niehoff, Passerini & Winter, “Interface investigations of a commercial lithium ion battery graphite anode material by sputter depth profile X-ray photoelectron spectroscopy”, Langmuir 2013. https://doi.org/10.1021/la400764r (primary)
6. Wang et al., “Depth-Resolved Probing of Native Solid Electrolyte Interphase Formation and Dynamics in Li Metal Batteries by Cryogenic X-Ray Photoelectron Spectroscopy”, J. Am. Chem. Soc. 2025. https://doi.org/10.1021/jacs.5c09519 (primary)
7. Finegan et al., “In-operando high-speed tomography of lithium-ion batteries during thermal runaway”, Nat. Commun. 2015. https://doi.org/10.1038/ncomms7924 (primary)
8. Ziesche et al., “4D imaging of lithium-batteries using correlative neutron and X-ray tomography with a virtual unrolling technique”, Nat. Commun. 2020. https://doi.org/10.1038/s41467-019-13943-3 (primary)
9. Michalak et al., “Gas Evolution in Operating Lithium-Ion Batteries Studied In Situ by Neutron Imaging”, Sci. Rep. 2015. https://doi.org/10.1038/srep15627 (primary)
10. Wu et al., “Structural Evolution and Transition Dynamics in Lithium Ion Battery under Fast Charging: An Operando Neutron Diffraction Investigation”, Adv. Sci. 2021. https://doi.org/10.1002/advs.202102318 (primary)
11. Maibach et al., “A high pressure x-ray photoelectron spectroscopy experimental method for characterization of solid-liquid interfaces demonstrated with a Li-ion battery system”, Rev. Sci. Instrum. 2015. https://doi.org/10.1063/1.4916209 (further reading)

Credit: Drawn by LabCanvas after Finegan et al., Nat. Commun. 2015 (doi:10.1038/ncomms7924), Shen et al., Rev. Sci. Instrum. 2014, Niehoff, Passerini & Winter, Langmuir 2013, Michalak et al., Sci. Rep. 2015 and Wu et al., Adv. Sci. 2021, and the papers in the details.

## Questions

**What does the “Seeing inside a working battery” template show?** Battery characterisation set-ups on one page: an operando X-ray diffraction cell, XPS of the SEI without air with sputter depth profiling, synchrotron X-ray tomography of an 18650 cell, neutron imaging of gas in a pouch cell, operando neutron diffraction of a cylindrical cell, and why neutrons see lithium. The set-ups and numbers are quoted from the cited papers; no panel is measured data.

**What are the steps shown in “Seeing inside a working battery”?** 1. Operando diffraction: An operando cell that closely mimics a standard coin cell works in reflection mode on a conventional powder X-ray diffractometer, so both anode and cathode materials can be studied; it uses graphite as the X-ray window instead of beryllium, and was tested on Li₄Ti₅O₁₂, LiMn₂O₄ and a layered sodium-ion cathode (Shen 2014). In transmission, a single-layer pouch cell with Mo Kα radiation followed the phase evolution of an NCM811 cathode (Shao 2025); standard cells have to be customised for operando diffraction (Bianchini 2015). 2. XPS without air: Cells are opened in an argon-filled glovebox and the electrodes moved to the XPS chamber in a transfer box (Shao 2025) or by vacuum transfer (Xiao 2014). Intense 13-step sputter depth profiling with a polyatomic ion gun gave a detailed model of the SEI on the graphite anode of commercial NMC/graphite cells, though charging under the X-ray beam means compounds cannot be assigned from binding energies alone (Niehoff 2013); cryo-XPS with argon gas-cluster ions profiled the vitrified wet SEI of lithium metal, graded from LiF and lithium carbonate on the electrolyte side to lithium oxide and carbide next to the electrode (Wang 2025). 3. X-ray tomography: At ESRF beamline ID15A a 76 keV monochromatic beam imaged LG 18650 NMC cells during thermal runaway: radiographs at 1,250 frames per second and tomograms at 2.5 Hz (500 projections) or 1.25 Hz (1,000 projections) as the cell turned continuously through 360°; steel and copper attenuate most and show white, NMC bright grey. Gas pockets formed between the electrode layers once the shell passed 100 °C, delaminating them (Finegan 2015). X-ray CT shows lithium diffusion only indirectly, neutron CT directly (Ziesche 2020). 4. Neutron imaging: Neutrons pass through the operating cell and the change in transmission gives a radiograph: lithium and hydrogen scatter neutrons strongly while aluminium, carbon and nickel interact only weakly, so the hydrocarbon-based electrolyte makes evolving gas visible. At ICON (SINQ), cold neutrons of 3–10 Å through a 7.1 m flight tube and a 2 cm aperture gave one 10 s image every minute; the gas collected at the edges of the pouch (Michalak 2015). 5. Neutron diffraction: Operando neutron powder diffraction at NOMAD (SNS): a customised NMC622 || graphite cylindrical cell, its jelly roll in a thin-walled quartz tube, charged from 0.27 C to 4.4 C with a pattern every 62 s; the stage II → stage I transition of the graphite was rate-limiting in fast charging. Neutrons penetrate without heating the cell and see light elements, but hydrogen-rich electrolyte adds incoherent scattering (Wu 2021); they are sensitive to lithium site occupancy (Bianchini 2015). 6. Why neutrons see lithium: The X-ray absorption cross-section increases with the atomic number, while the neutron cross-section varies non-linearly across the periodic table: lithium and hydrogen scatter neutrons strongly, while aluminium, carbon and nickel interact only weakly (Michalak 2015).

**Which papers is “Seeing inside a working battery” based on?** Shen et al., “An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer”, Rev. Sci. Instrum. 2014 (doi:10.1063/1.4896198); Shao et al., “Multiscale interfacial stabilization via prelithiation separator engineering for Ah-level anode-free lithium batteries”, Nat. Commun. 2025 (doi:10.1038/s41467-025-59521-8); Bianchini et al., “Spinel materials for Li-ion batteries: new insights obtained by operando neutron and synchrotron X-ray diffraction”, Acta Crystallogr. B 2015 (doi:10.1107/S2052520615017199); Xiao et al., “Unraveling manganese dissolution/deposition mechanisms on the negative electrode in lithium ion batteries”, Phys. Chem. Chem. Phys. 2014 (doi:10.1039/c4cp00833b); Niehoff, Passerini & Winter, “Interface investigations of a commercial lithium ion battery graphite anode material by sputter depth profile X-ray photoelectron spectroscopy”, Langmuir 2013 (doi:10.1021/la400764r); Wang et al., “Depth-Resolved Probing of Native Solid Electrolyte Interphase Formation and Dynamics in Li Metal Batteries by Cryogenic X-Ray Photoelectron Spectroscopy”, J. Am. Chem. Soc. 2025 (doi:10.1021/jacs.5c09519); Finegan et al., “In-operando high-speed tomography of lithium-ion batteries during thermal runaway”, Nat. Commun. 2015 (doi:10.1038/ncomms7924); Ziesche et al., “4D imaging of lithium-batteries using correlative neutron and X-ray tomography with a virtual unrolling technique”, Nat. Commun. 2020 (doi:10.1038/s41467-019-13943-3); Michalak et al., “Gas Evolution in Operating Lithium-Ion Batteries Studied In Situ by Neutron Imaging”, Sci. Rep. 2015 (doi:10.1038/srep15627); Wu et al., “Structural Evolution and Transition Dynamics in Lithium Ion Battery under Fast Charging: An Operando Neutron Diffraction Investigation”, Adv. Sci. 2021 (doi:10.1002/advs.202102318); Maibach et al., “A high pressure x-ray photoelectron spectroscopy experimental method for characterization of solid-liquid interfaces demonstrated with a Li-ion battery system”, Rev. Sci. Instrum. 2015 (doi:10.1063/1.4916209).

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