Nanoscale Characterisation

Nanoscale characterisation encompasses a suite of techniques aimed at probing the structure, composition and properties of materials at dimensions below 100 nm. By extending beyond the diffraction limit of light, methods such as electron‐based microscopies, scanned‐probe modalities and advanced spectroscopies reveal morphology, crystallography, chemical state and mechanical and electromagnetic behaviour with nanometre to atomic resolution. Such insights underpin developments in catalysis, electronics, energy conversion, biomaterials and beyond, by linking local heterogeneity to global performance. Recent advances integrate in situ or operando environments, multi‐modal detection and quantitative modelling to deliver dynamic, quantitative maps of material responses under realistic conditions. This progress transforms characterisation from a static ‘‘snapshot’’ into a time‐resolved view of structure–property relations at the smallest scales.

Research from Nature Portfolio

Operando transmission electron microscopy of palladium nanoparticles in methane‐oxidising atmospheres has uncovered oscillatory redox dynamics, with simultaneous imaging and mass‐spectrometric monitoring showing coexisting Pd and PdO phases and identifying strained PdO as the active state. In a complementary study of CO oxidation, real‐time TEM revealed periodic morphological switching between rounded high‐index facets and flat low‐index facets, each transition synchronising with bursts of catalytic turnover under constant feed conditions. Accelerating near‐field electromagnetic imaging, monolithic silicon cantilever probes combined with self‐referenced homodyne detection have achieved drift‐free, Johnson‐noise‐limited microwave impedance microscopy with 15 nm spatial resolution and 0.26 zF/√Hz sensitivity, obviating specialised cancellation circuits and opening new pathways for nanoscale permittivity mapping.

Research from all publishers

In advanced atomic force microscopy, dip‐coated gold nanoparticle arrays on microcantilevers have been shown to tune higher eigenmodes into integer harmonics of the fundamental resonance, yielding threefold improvements in multifrequency contrast and enabling seamless nanomechanical mapping of polymer blends. A combined AFM–theoretical–simulation framework has quantified hydration‐dependent elastic moduli of poly(vinyl alcohol) nanofibres under controlled humidity, revealing sub‐nanometre changes in chain interactions that govern viscoelastic response. In microwave scanning probes, dynamic ferric‐chloride etching of coaxial connectors has produced ultra‐sharp tips with ~1 µm apex radii; finite‐element simulations and imaging of metal–dielectric patterns confirm their efficacy for non‐contact sub‐100 nm near‐field microwave microscopy.

Nanoscale Characterisation publication trend

The graph below shows the total number of articles in nanoscale characterisation across all publications each year (not limited to Nature Index journals).

Technical terms

Operando microscopy: Imaging of materials under realistic reaction conditions, including temperature, pressure and gas environment.

Atomic Force Microscopy (AFM): A scanned‐probe technique employing a cantilevered tip to map surface topography and mechanical properties via force interactions.

Cantilever eigenmode: A resonant vibration mode of the AFM cantilever, exploited in multifrequency AFM for parallel mechanical observables.

Viscoelasticity: Material behaviour combining elastic and viscous responses, characterised in dynamic AFM by amplitude and phase under oscillatory loading.

Homodyne detection: A signal‐processing method mixing a received microwave signal with a reference at the same frequency to extract amplitude and phase with drift cancellation.

References

1. Redox dynamics and surface structures of an active palladium catalyst during methane oxidation. Nature Communications (2024).
2. Periodic structural changes in Pd nanoparticles during oscillatory CO oxidation reaction. Nature Communications (2022).
3. Johnson-noise-limited cancellation-free microwave impedance microscopy with monolithic silicon cantilever probes. Nature Communications (2024).
4. Incongruous Harmonics of Vibrating Solid‐Solid Interface. Small (2024).
5. Quantitative Dynamic AFM Hydration‐Adsorption Design for Hygroscopic and Bio‐Compatible Polymeric Nanofibers. Small Structures (2024).
6. Fabrication of Ultra-Sharp Tips by Dynamic Chemical Etching Process for Scanning Near-Field Microwave Microscopy. Sensors (2023).