Characterization and analytical techniques articles within Nature Communications

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  • Article
    | Open Access

    Intrinsic mechanical properties of sub-100 nm thin films are markedly difficult to obtain, yet an ever-growing necessity for emerging fields such as soft organic electronics. Here, the authors present a shear motion assisted transfer technique for fabricating free-standing sub-100 nm thin films and measuring their inherent structural–mechanical properties.

    • Luke A. Galuska
    • , Eric S. Muckley
    •  & Xiaodan Gu

  • Article
    | Open Access

    Van der Waals (vdW) magnets have allowed researchers to explore the two dimensional limit of magnetisation; however experimental challenges have hindered analysis of magnetic domains. Here, using an NV centre based probe, the authors analyse the nature of magnetic domains in the vdW magnet, CrBr3.

    • Qi-Chao Sun
    • , Tiancheng Song
    •  & Jörg Wrachtrup

  • Article
    | Open Access

    Polarimetry provides information about physical characteristics of cometary dust. Here, the authors show that the polarization of interstellar comet 2I/Borisov exceeds the typical values for comets, and this together with its polarimetrically homogenous coma suggests a more pristine nature of the object.

    • S. Bagnulo
    • , A. Cellino
    •  & M. Devogèle

  • Article
    | Open Access

    Low secretion rates and evaporation pose challenges for collecting resting thermoregulatory sweat for non-invasive analysis of body physiology. Here the authors present wearable microfluidics-based patches for continuous sweat monitoring at rest that enable detection of pH, Cl−, and levodopa for dynamic sweat analysis related to routine activities, stress events, hypoglycemia-induced sweating, and Parkinson’s disease.

    • Hnin Yin Yin Nyein
    • , Mallika Bariya
    •  & Ali Javey

  • Article
    | Open Access

    Electrical nano-sensors hold promise for biofluid interrogation, but their performance is still below the state of the art. Here, self-powered monolayer graphene microelectrodes are shown to enable real-time interrogation of whole-blood flows with 6-month stability and sub-micron/second resolution.

    • Xiaoyu Zhang
    • , Eric Chia
    •  & Jinglei Ping

  • Article
    | Open Access

    The electrical conductivity is critical to understand warm dense matter, but the accurate measurement is extremely challenging. Here the authors use multi-cycle THz pulses to measure the conductivity of gold foils strongly heated by free-electron laser, determining the individual contributions of electron-electron and electron-ion scattering.

    • Z. Chen
    • , C. B. Curry
    •  & S. H. Glenzer

  • Article
    | Open Access

    The obtention and study of actinide elements is challenging due to various factors including their radioactivity and scarcity. Herein, the authors characterize the atomic and electronic structure of Am, Cm, Bk, and Cf compounds using a transmission electron microscopy-based workflow that only requires nanogram amounts of the actinide element.

    • Alexander Müller
    • , Gauthier J.-P. Deblonde
    •  & Andrew M. Minor

  • Article
    | Open Access

    Measuring real time magnetization dynamics resulting from Hall effects is hard due to the small signal size. Here Sala et al demonstrate a method of performing Hall resistance measurements with sub-ns resolution, and use it to investigate the switching of GdFeCo dots induced by spin-orbit torques.

    • G. Sala
    • , V. Krizakova
    •  & P. Gambardella

  • Article
    | Open Access

    The charging of Fe and Mn oxide anodes in lithium-ion batteries are believed to form rocksalt phases via reconstructive conversion reactions. Here, the authors show that MxOy (M = Fe, Mn) transform into non-native body-centred cubic FeO and zincblende MnO via topotactic displacement-like pathways.

    • Xiao Hua
    • , Phoebe K. Allan
    •  & Andrew L. Goodwin

  • Article
    | Open Access

    Magnetic reconnection and plasma turbulence occur in atmospheric and magnetized laboratory plasmas. Here the authors report evolution of magnetic islands and plasma turbulence in tokamak plasmas using high resolution 2D electron cyclotron emission diagnostics.

    • Minjun J. Choi
    • , Lāszlo Bardōczi
    •  & George McKee

  • Article
    | Open Access

    Ferroelectric domain wall profiles can be modeled by phenomenological Ginzburg-Landau theory, with different candidate models and parameters. Here, the authors solve the problem of model selection by developing a Bayesian inference framework allowing for uncertainty quantification and apply it to atomically resolved images of walls. This analysis can also predict the level of microscope performance needed to detect specific physical phenomena.

    • Christopher T. Nelson
    • , Rama K. Vasudevan
    •  & Sergei V. Kalinin

  • Article
    | Open Access

    Single-cell immunoblotting previously separated proteins on a polyacrylamide slab in the xy direction and was limited by throughput and sample consumption. Here the authors adapt the system to separate proteins in the z direction, allowing for closer spacing of sample wells and improved sample consumption.

    • Samantha M. Grist
    • , Andoni P. Mourdoukoutas
    •  & Amy E. Herr

  • Article
    | Open Access

    Controlled particle acceleration in plasmas requires precise measurements of the excited wakefield. Here the authors report and demonstrate a high-resolution method to measure the effective longitudinal electric field of a beam-driven plasma-wakefield accelerator.

    • S. Schröder
    • , C. A. Lindstrøm
    •  & J. Osterhoff

  • Article
    | Open Access

    Optical atomic clocks are useful tools for frequency metrology. Here the authors explore the stability of the atomic clocks and the role of the spin squeezed states for the noise reduction in these clocks.

    • Marius Schulte
    • , Christian Lisdat
    •  & Klemens Hammerer

  • Article
    | Open Access

    Machine learning driven research holds big promise towards accelerating materials’ discovery. Here the authors demonstrate CAMEO, which integrates active learning Bayesian optimization with practical experiments execution, for the discovery of new phase- change materials using X-ray diffraction experiments.

    • A. Gilad Kusne
    • , Heshan Yu
    •  & Ichiro Takeuchi

  • Article
    | Open Access

    Shark teeth have short lifespans yet can be subject to significant mechanical damage. Here, the authors report on a site-specific damage mechanism in shark teeth enameloid, which maintains tooth functional shape, providing experimental evidence that tooth architecture may have influenced the diversification of shark ecologies over evolution.

    • Shahrouz Amini
    • , Hajar Razi
    •  & Peter Fratzl

  • Article
    | Open Access

    Study of structural inhomogeneities in zeolites is important but limited by conventional techniques. Here the authors employ in situ free-electron-laser-based time-resolved coherent X-ray diffraction imaging to visualize the effect of these inhomogeneities during catalytic deoxygenation of NOx.

    • Jinback Kang
    • , Jerome Carnis
    •  & Hyunjung Kim

  • Perspective
    | Open Access

    Discovering a sustainable route to ammonia as a fertiliser and as an energy carrier is critically important, but many recent reports on the electrochemical nitrogen reduction are false positives. Here the authors uncover the emerging experimental traps and detail protocols to reliably avoid them.

    • Jaecheol Choi
    • , Bryan H. R. Suryanto
    •  & Alexandr N. Simonov

  • Article
    | Open Access

    Additive manufacturing promises a major transformation of the production of high economic value metallic materials. Here, the authors describe a new class of 3D printable superalloys that are amenable to crack-free 3D printing via electron beam melting as well as selective laser melting.

    • Sean P. Murray
    • , Kira M. Pusch
    •  & Tresa M. Pollock

  • Article
    | Open Access

    Understanding active-site geometry and structural evolution during electrocatalysis is important for further development. Here the authors use operando X-ray absorption spectroscopy combined with electrochemical impedance spectroscopy to investigate single atom catalysts derived from Vitamin B12.

    • Hsiang-Ting Lien
    • , Sun-Tang Chang
    •  & Li-Chyong Chen

  • Article
    | Open Access

    Achieving higher efficiencies for thin-film solar cells always requires identification of the limiting factors. Here Krause et al. show that inhomogeneously distributed net doping or lifetime have little impact while recombination at grain boundaries is one of the main loss mechanisms for high performance Cu(In,Ga)Se2 solar cells.

    • Maximilian Krause
    • , Aleksandra Nikolaeva
    •  & Daniel Abou-Ras

  • Article
    | Open Access

    Air-stability is a critical challenge faced by layered sodium transition metal oxide cathodes. Here, the authors depict a general and in-depth model of the structural/chemical evolution of P2-type layered oxides in air and propose an evaluation rule for the air-stability of layered sodium cathodes.

    • Wenhua Zuo
    • , Jimin Qiu
    •  & Yong Yang

  • Article
    | Open Access

    Atomic force microscopy-infrared (AFM-IR) spectroscopic imaging techniques offer a non-perturbative, molecular contrast for characterization of nanomaterials; however, data are often complicated by the measurement apparatus, sample preparation conditions and low signal-to-noise ratio. Here, the authors demonstrate a closed-loop controlled AFM-IR instrument design to address measurement artifacts and reduce noise up to 5x compared to previous methods.

    • Seth Kenkel
    • , Shachi Mittal
    •  & Rohit Bhargava

  • Article
    | Open Access

    Structural alloys have distinct microstructural features known as twins that are preferential sites for fatigue crack initiation and need to be better understood to mitigate catastrophic failures. Here, the authors show unusually large stress gradients near a twin boundary, using X-ray techniques and modelling.

    • Sven Gustafson
    • , Wolfgang Ludwig
    •  & Michael D. Sangid

  • Article
    | Open Access

    Strong metal–support interactions (SMSI) are effective in tuning the structures and catalytic performances of catalysts but limited by the poor exposure of active sites. Here, the authors develop a strategy to engineer SMSI via a reverse route, which is in favor of metal site exposure while embracing the SMSI.

    • Peiwen Wu
    • , Shuai Tan
    •  & Huiyuan Zhu

  • Article
    | Open Access

    Great advances have been made in CO2 electroreduction, however, the role of wettability-controlled interfacial structures remains poorly understood. Here, the authors apply confocal laser scanning microscopy to gain deeper understanding of these phenomena in gas diffusion electrodes.

    • Run Shi
    • , Jiahao Guo
    •  & Tierui Zhang

  • Article
    | Open Access

    Calorimetrically measuring the heat of single cells is currently not possible due to the sensitivity of existing calorimeters. Here the authors present on-chip single cell calorimetry, with a sensitivity over ten-fold greater than the current gold-standard.

    • Sahngki Hong
    • , Edward Dechaumphai
    •  & Renkun Chen

  • Article
    | Open Access

    Calorimetry is widely used for metabolic studies, but measurements of single cells and small organisms are limited by the sensitivity of current techniques. Here the authors develop a sensitive platform for performing time-resolved metabolic measurements of single C. elegans worms from larval to adult stages.

    • Sunghoon Hur
    • , Rohith Mittapally
    •  & Edgar Meyhofer

  • Article
    | Open Access

    Electronics and magnetic phase transitions typically do not involve mechanical degrees of freedom directly, but their impact on thermodynamic properties affects the mechanical response of a material. Here the authors show that resonators made from 2D materials exhibit anomalies at phase transitions.

    • Makars Šiškins
    • , Martin Lee
    •  & Peter G. Steeneken

  • Perspective
    | Open Access

    As the field of metal-organic frameworks is maturing, understanding the dynamics of open frameworks is progressing and rational approaches are under development. Here, the authors outline challenges and potential routes to engineering the spatio-temporal evolution of dynamic metal-organic frameworks.

    • Jack D. Evans
    • , Volodymyr Bon
    •  & Stefan Kaskel

  • Article
    | Open Access

    Single-entity electrochemistry has been proposed for studying properties of single nanoparticles (NPs). Here, the authors make use of adsorption-mediated motion of Ag NPs to take individual NP size measurements using electrochemical impacts with excellent agreement to standard imaging techniques.

    • Hui Ma
    • , Jian-Fu Chen
    •  & Yi-Tao Long

  • Article
    | Open Access

    How nanoparticle (NP) catalysts re-structure under reaction conditions and how these changes associate with catalytic activity remains poorly understood. Here, the authors present operando TEM studies of Pd NPs during CO oxidation, which show reversible changes in both structure and activity with temperature.

    • See Wee Chee
    • , Juan Manuel Arce-Ramos
    •  & Utkur Mirsaidov

  • Article
    | Open Access

    Visualising single-molecule reactions, to understand their mechanisms, is a challenging task. Here, the authors investigate disulfide exchange reactions with thiolates immobilised on a gold nanoparticle through a label-free optoplasmonic sensor, and detect individual disulfide interactions in solution

    • Serge Vincent
    • , Sivaraman Subramanian
    •  & Frank Vollmer

  • Article
    | Open Access

    Knowing compositional motifs of nanoparticle catalysts in operando conditions is crucial towards understanding their catalytic behavior. Here, the authors develop a physics-driven machine learning approach to predict adsorption sites for a CO molecule over platinum nanoparticles in a multitude of coordination environments.

    • Joshua L. Lansford
    •  & Dionisios G. Vlachos

  • Article
    | Open Access

    Eliminating the need for cleanroom fabrication for thermomechanical characterization of organic samples in a biomedical setting remains a challenge. Here, the authors propose the use of a single drug and collagen particles as resonators, enabling direct measurements on a material during thermal cycling.

    • Peter Ouma Okeyo
    • , Peter Emil Larsen
    •  & Anja Boisen

  • Article
    | Open Access

    Physical unclonable functions with inherent randomness are promising candidates for secure labeling systems. Here the authors demonstrate such a function using gap-enhanced Raman tags to create high-capacity and high-security labels for anticounterfeiting.

    • Yuqing Gu
    • , Chang He
    •  & Jian Ye

  • Article
    | Open Access

    Understanding enzyme active sites can elucidate fundamental enzymatic reaction pathways and inform designs for synthetic catalysts. Here, authors employ operando X-ray absorption spectroelectrochemistry to assess copper ions in bilirubin oxidase during oxygen reduction electrocatalysis.

    • Lucyano J. A. Macedo
    • , Ayaz Hassan
    •  & Frank N. Crespilho

  • Article
    | Open Access

    Identifying reacting species locally with nanometer precision is a major challenge in electrochemical surface science. Using operando Raman nanoscopy, authors image the reversible, concurrent formation of nanometer-spatially separated Au2O3 and Au2O species during Au nanodefect oxidation.

    • Jonas H. K. Pfisterer
    • , Masoud Baghernejad
    •  & Katrin F. Domke

  • Article
    | Open Access

    Probing inevitable defects in two- dimensional materials is challenging. Here, the authors tackle this issue by using tip-enhanced Raman spectroscopy (TERS) to obtain distinctly different Raman features of edge defects in atomically thin MoS2, and further probe their unique electronic properties as well as identify the armchair and zigzag edges.

    • Teng-Xiang Huang
    • , Xin Cong
    •  & Bin Ren

  • Article
    | Open Access

    Polar-faceted nanocrystals often have complex atomic surface configurations that are very difficult to characterize. Here, the authors are able to determine detailed structural information about the polar facets of ceria nanocubes by using 17O and 1H solid-state NMR spectroscopy, in combination with density functional theory calculations.

    • Junchao Chen
    • , Xin-Ping Wu
    •  & Luming Peng

  • Article
    | Open Access

    The shape and energy of frontier orbitals determine the reactivity of molecular systems. Combining orbital tomography based on photoelectron spectroscopy with electron diffraction and DFT, the authors investigate a complex multi-configurational adsorbate system revealing adsorptions geometries and hierarchy and geometry of molecular orbitals.

    • Pavel Kliuiev
    • , Giovanni Zamborlini
    •  & Luca Castiglioni

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