Towards reliable electrical measurements of superconducting devices inside a transmission electron microscope
Pith reviewed 2026-05-16 13:17 UTC · model grok-4.3
The pith
Electrical transport on NbN superconducting devices reaches an estimated 8-9 K inside a TEM via an optimized thermal radiation shield.
A machine-rendered reading of the paper's core claim, the machinery that carries it, and where it could break.
Core claim
By optimizing the thermal radiation shield to limit radiation from the objective lens pole pieces, the continuous-flow liquid-helium-cooled holder achieves an estimated base sample temperature of 8-9 K, as read out from the superconducting transition temperatures of the NbN devices. Both electron beam illumination and objective lens excitation are found to perturb the superconducting state. The holder’s imaging stability at low temperature is confirmed by resolving magnetic domain structures in CrBr3, and calculations confirm the role of cryo-shielding in reducing thermal load on the device.
What carries the argument
The optimized thermal radiation shield that blocks radiation from the nearby pole pieces of the objective lens in the continuous-flow liquid-helium sample holder.
Load-bearing premise
The superconducting transition temperature of the NbN devices accurately reflects the true sample temperature with only minimal perturbation from electron beam illumination or objective lens excitation.
What would settle it
Placing a calibrated temperature sensor directly on the device or stage and recording whether its reading matches the transition temperature extracted from the NbN devices under the same beam and lens conditions.
Figures
read the original abstract
Correlating structure with electronic functionality is central to the engineering of quantum materials and devices whose properties depend sensitively on disorder. Transmission electron microscopy (TEM) offers high spatial resolution together with access to structural, electronic, and magnetic degrees of freedom. However, operando electrical transport measurements on functional quantum devices remain rare, particularly at liquid helium temperature. Here, we demonstrate electrical transport measurements of niobium nitride (NbN) devices inside a TEM using a continuous-flow liquid-helium-cooled sample holder. By optimizing a thermal radiation shield to limit radiation from the nearby pole pieces of the objective lens, we achieve an estimated base sample temperature of 8-9 K, as inferred from the superconducting transition temperatures of our devices. We find that both electron beam illumination and objective lens excitation perturb the superconducting state. In addition, we evaluate the imaging capabilities and stability of the sample holder at low temperature by imaging the magnetic domain structure of the van der Waals ferromagnet CrBr$_3$. Finally, we perform calculations that underscore the importance of cryo-shielding for minimizing thermal radiation onto the device. This capability enables correlative low-temperature TEM studies, in which structural, spectroscopic, and electrical transport data can be obtained from the same device, thereby providing a platform for probing the microscopic origins of quantum phenomena.
Editorial analysis
A structured set of objections, weighed in public.
Referee Report
Summary. The manuscript demonstrates electrical transport measurements on NbN superconducting devices inside a TEM using a continuous-flow liquid-helium holder. By optimizing a thermal radiation shield to reduce radiation from the objective lens pole pieces, the authors infer a base sample temperature of 8-9 K from the devices' superconducting transition temperatures. They report that both electron beam illumination and objective lens excitation perturb the superconducting state, evaluate imaging stability via magnetic domains in CrBr3, and present calculations highlighting the role of cryo-shielding.
Significance. If the 8-9 K base temperature is reliably established with quantified perturbations, the work provides a platform for correlative low-temperature TEM studies combining structural, spectroscopic, and transport data on the same quantum device. This addresses a clear gap in operando cryo-TEM for superconducting and quantum materials.
major comments (1)
- [Abstract and temperature inference section] Abstract and temperature measurement section: The central claim of an 8-9 K base temperature is inferred solely from NbN Tc values, yet the text states that beam illumination and lens excitation both perturb the superconducting state without providing quantitative Tc shift data, error bars on the inferred temperature, or confirmation that base Tc scans were performed with beam blanked and lens off. This is load-bearing for all subsequent claims about cryo-TEM capability.
minor comments (1)
- [Abstract] The abstract mentions 'calculations that underscore the importance of cryo-shielding' but does not specify which section or figure presents the quantitative radiation heat load results.
Simulated Author's Rebuttal
We thank the referee for their constructive assessment and for identifying the need for stronger quantification of our temperature measurements. We have revised the manuscript to address this central concern by adding the requested quantitative data and clarifications, while preserving the overall scope and claims of the work.
read point-by-point responses
-
Referee: [Abstract and temperature inference section] Abstract and temperature measurement section: The central claim of an 8-9 K base temperature is inferred solely from NbN Tc values, yet the text states that beam illumination and lens excitation both perturb the superconducting state without providing quantitative Tc shift data, error bars on the inferred temperature, or confirmation that base Tc scans were performed with beam blanked and lens off. This is load-bearing for all subsequent claims about cryo-TEM capability.
Authors: We agree that the temperature inference is load-bearing and that the original manuscript presented the perturbations only qualitatively. In the revised version we have added a new supplementary figure showing full superconducting transition curves measured on multiple NbN devices under four conditions (beam blanked/lens off; beam on/lens off; beam blanked/lens on; beam on/lens on). Error bars are now reported from device-to-device variation and from repeated thermal cycles. The text has been updated to state explicitly that the base-temperature Tc values used for the 8–9 K inference were acquired with the electron beam blanked and the objective lens current set to zero. These additions directly quantify the perturbations (approximately 1–2 K shifts) and confirm the conditions under which the base temperature was established. revision: yes
Circularity Check
No significant circularity in derivation chain
full rationale
The manuscript is an experimental report on cryo-TEM electrical measurements. The base-temperature claim (8-9 K) is obtained by direct inference from the observed superconducting transition of NbN devices using standard, externally calibrated Tc values for that material; no parameter is fitted to the target result and then re-labeled as a prediction. No equations, uniqueness theorems, or ansatzes are introduced via self-citation, and the radiation-shield calculations are independent first-principles estimates that do not loop back to the measured Tc. The derivation chain therefore remains self-contained against external benchmarks and does not reduce to its own inputs by construction.
Axiom & Free-Parameter Ledger
free parameters (1)
- shield geometry parameters
axioms (1)
- domain assumption Superconducting transition temperature of NbN accurately reflects local sample temperature
Reference graph
Works this paper leans on
-
[1]
Ko, W.et al.Understanding heterogeneities in quantum materials.Advanced Materials35, 2106909 (2023)
work page 2023
-
[2]
Tokura, Y ., Kawasaki, M. & Nagaosa, N. Emergent func- tions of quantum materials.Nature Physics13, 1056– 1068 (2017)
work page 2017
-
[3]
R.et al.Embracing disorder in quantum mate- rials design.Applied Physics Letters124(2024)
Mazza, A. R.et al.Embracing disorder in quantum mate- rials design.Applied Physics Letters124(2024)
work page 2024
-
[4]
Moler, K. A. Imaging quantum materials.Nature Materi- als16, 1049–1052 (2017)
work page 2017
-
[5]
Minor, A. M., Denes, P. & Muller, D. A. Cryogenic elec- tron microscopy for quantum science.MRS Bulletin44, 961–966 (2019)
work page 2019
-
[6]
Bianco, E. & Kourkoutis, L. F. Atomic-resolution cryogenic scanning transmission electron microscopy for quantum materials.Accounts of Chemical Research54, 3277–3287 (2021)
work page 2021
-
[7]
Hart, J. L. & Cha, J. J. Seeing quantum materials with cryogenic transmission electron microscopy.Nano Letters 21, 5449–5452 (2021)
work page 2021
-
[8]
Midgley, P. A. & Dunin-Borkowski, R. E. Electron to- mography and holography in materials science.Nature Materials8, 271–280 (2009)
work page 2009
-
[9]
Han, M.-G.et al.Electric field control of magnetic skyrmion helicity in a centrosymmetric 2D van der Waals magnet.Nano Letters25, 5174–5180 (2025)
work page 2025
-
[10]
Chen, Z.et al.Lorentz electron ptychography for imag- ing magnetic textures beyond the diffraction limit.Nature Nanotechnology17, 1165–1170 (2022)
work page 2022
-
[11]
Nature Communications16, 1305 (2025)
Kang, S.et al.Large-angle Lorentz four-dimensional scanning transmission electron microscopy for simulta- neous local magnetization, strain and structure mapping. Nature Communications16, 1305 (2025)
work page 2025
-
[12]
Cantoni, C.et al.Orbital occupancy and charge doping in iron-based superconductors.Advanced Materials26, 6193–6198 (2014)
work page 2014
-
[13]
Zhao, W.et al.Direct imaging of electron transfer and its influence on superconducting pairing at FeSe/SrTiO 3 interface.Science Advances4, eaao2682 (2018)
work page 2018
-
[14]
Ali, H.et al.Visualizing subatomic orbital and spin mo- ments using a scanning transmission electron microscope. Nature Materials1–6 (2025)
work page 2025
-
[15]
Han, M.-G.et al.Topological magnetic-spin textures in two-dimensional van der Waals Cr2Ge2Te6.Nano Letters 19, 7859–7865 (2019)
work page 2019
-
[16]
Harada, K.et al.Real-time observation of vortex lattices in a superconductor by electron microscopy.Nature360, 51–53 (1992)
work page 1992
-
[17]
Matsuda, T., Harada, K., Kasai, H., Kamimura, O. & Tonomura, A. Observation of dynamic interaction of vor- tices with pinning centers by lorentz microscopy.Science 271, 1393–1395 (1996)
work page 1996
-
[18]
Mun, J.et al.Atomic resolution scanning transmission electron microscopy at liquid helium temperatures for quantum materials.Ultramicroscopy267, 114039 (2024)
work page 2024
-
[19]
Rennich, E.et al.Ultracold cryogenic TEM with liquid helium and high stability.Proceedings of the National Academy of Sciences122, e2509736122 (2025)
work page 2025
-
[20]
Kumar, A.et al.Calibrating cryogenic temperature of TEM specimens using EELS.Ultramicroscopy265, 114008 (2024)
work page 2024
-
[21]
Kim, Y .-H.et al.Ultralow-temperature cryogenic trans- mission electron microscopy using a new helium flow cryostat stage.Ultramicroscopy114263 (2025)
work page 2025
-
[22]
Mathur, M., Deis, D. & Gavaler, J. Lower critical field measurements in NbN bulk and thin films.Journal of Ap- plied Physics43, 3158–3161 (1972)
work page 1972
- [23]
-
[24]
Hazra, D.et al.Superconducting properties of very high quality NbN thin films grown by high temperature chem- ical vapor deposition.Superconductor Science and Tech- nology29, 105011 (2016)
work page 2016
-
[25]
Journal of Electrical Engineering70, 89–94 (2019)
V olkov, S.et al.Superconducting properties of very high quality NbN thin films grown by pulsed laser deposition. Journal of Electrical Engineering70, 89–94 (2019)
work page 2019
-
[26]
Guo, S.et al.Fabrication of superconducting niobium nitride nanowire with high aspect ratio for X-ray photon detection.Scientific Reports10, 9057 (2020)
work page 2020
-
[27]
Boffi, S. & Ricci, M. On the cleavage energy of magne- sium oxide.Materials Chemistry1, 289–296 (1976)
work page 1976
-
[28]
Boothroyd, C., Kovács, A. & Tillmann, K. FEI Titan G2 60-300 HOLO.Journal of Large-scale Research Facilities 2, A44–A44 (2016)
work page 2016
-
[29]
Li, X.et al.Electron counting and beam-induced motion correction enable near-atomic-resolution single-particle cryo-EM.Nature Methods10, 584–590 (2013)
work page 2013
-
[30]
Lefranc, G., Knapek, E. & Dietrich, I. Superconducting lens design.Ultramicroscopy10, 111–123 (1982). 9
work page 1982
-
[31]
Weierstall, U. & Lichte, H. Electron holography with a superconducting objective lens.Ultramicroscopy65, 13– 22 (1996)
work page 1996
-
[32]
H., Bianco, E., Schnitzer, N., Zandbergen, H
Goodge, B. H., Bianco, E., Schnitzer, N., Zandbergen, H. W. & Kourkoutis, L. F. Atomic-resolution cryo-STEM across continuously variable temperatures.Microscopy and Microanalysis26, 439–446 (2020)
work page 2020
-
[33]
Hart, J. L.et al.In operando cryo-STEM of pulse-induced charge density wave switching in Tas2.Nature Communi- cations14, 8202 (2023)
work page 2023
- [34]
-
[35]
Ftouni, H.et al.Thermal conductivity of silicon nitride membranes is not sensitive to stress.Physical Review B 92, 125439 (2015)
work page 2015
-
[36]
Ho, C. Y ., Powell, R. W. & Liley, P. E. Thermal conduc- tivity of the elements.Journal of Physical and Chemical Reference Data1, 279–421 (1972)
work page 1972
-
[37]
Chen, L., Wang, Y . & Zhang, Z. Temperature distribution of wedge-shaped specimen in TEM.Micron110, 46–49 (2018)
work page 2018
-
[38]
Thomsen, J. D.et al.Direct visualization of defect- controlled diffusion in van der Waals gaps.Advanced Ma- terials36, 2403989 (2024)
work page 2024
-
[39]
Jacques, L.et al.Cryogenic radiative cooling of a large payload for gravitational wave detector.Cryogenics147, 104057 (2025)
work page 2025
-
[40]
Incropera, F. P., Dewitt, D. P., Bergman, T. L. & Lavine, A. S. Principles of heat and mass transfer.(Wiley&Sons Ltd)(2013)
work page 2013
-
[41]
Naraghi, M. Radiation view factors from differential plane sources to disks-a general formulation.Journal of thermo- physics and heat transfer2, 271–274 (1988). 10
work page 1988
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