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The success of semiconductor electronics is built on the creation of compact, low-power switching elements that offer routing, logic and memory functions. The availability of nanoscale optical switches could have a similarly transformative impact on the development of dynamic and programmable metasurfaces, optical neural networks and quantum information processing. Phase-change materials are uniquely suited to enable their creation as they offer high-speed electrical switching between amorphous and crystalline states with notably different optical properties. Their high refractive index has already been harnessed to fashion them into compact optical antennas. Here, we take the next important step, by showing electrically-switchable phase-change antennas and metasurfaces that offer strong, reversible, non-volatile, multi-phase switching and spectral tuning of light scattering in the visible and near-infrared spectral ranges. Their successful implementation relies on a careful joint thermal and optical optimization of the antenna elements that comprise a silver strip that simultaneously serves as a plasmonic resonator and a miniature heating stage. Our metasurface affords electrical modulation of the reflectance by more than fourfold at 755 nm. A metasurface comprising electrically controlled heating units and a phase-change material offer non-volatile and reversible modulation of reflectance by more than fourfold.

The highly engineerable scattering properties of resonant optical antennas underpin the operation of metasurface-based flat optics. Thus far, the choice of antenna has been limited to shaped metallic and high-index semiconductor nanostructures that support geometrical plasmonic or Mie resonances. Whereas these resonant elements offer strong light–matter interaction and excellent control over the scattering phase and amplitude, their electrical tunability has proven to be quite limited. Here, we demonstrate how excitonic resonances in atomically thin semiconductors can be harnessed as a different, third type of resonance to create mutable, flat optics. These strong materials-based resonances are unmatched in their tunability with various external stimuli. To illustrate the concept, we first demonstrate how excitons can enhance the focusing efficiency of a millimetre-scale, patterned WS2 zone plate lens. We also show how electrical gating can completely turn on and off the exciton resonance and thereby modulate the focusing efficiency by 33%.By harnessing the excitonic resonances of a monolayer of WS2 in the visible spectral range, large-area, actively tunable and atomically thin optical lenses can be realized.

Wear mechanisms including fracture and plastic deformation at the nanoscale are central to understand sliding contacts. Recently, the combination of tip-induced material erosion with the sensing capability of secondary imaging modes of AFM, has enabled a slice-and-view tomographic technique named AFM tomography or Scalpel SPM. However, the elusive laws governing nanoscale wear and the large quantity of atoms involved in the tip-sample contact, require a dedicated mesoscale description to understand and model the tip-induced material removal. Here, we study nanosized sliding contacts made of diamond in the regime whereby thousands of nm 3 are removed. We explore the fundamentals of high-pressure tip-induced material removal for various materials. Changes in the load force are systematically combined with AFM and SEM to increase the understanding and the process controllability. The nonlinear variation of the removal rate with the load force is interpreted as a combination of two contact regimes each dominating in a particular force range. By using the gradual transition between the two regimes, (1) the experimental rate of material eroded on each tip passage is modeled, (2) a controllable removal rate below 5 nm/scan for all the materials is demonstrated, thus opening to future development of 3D tomographic AFM.

Controlling nanoscale tip‐induced material removal is crucial for achieving atomic‐level precision in tomographic sensing with atomic force microscopy (AFM). While advances have enabled volumetric probing of conductive features with nanometer accuracy in solid‐state devices, materials, and photovoltaics, limitations in spatial resolution and volumetric sensitivity persist. This work identifies and addresses in‐plane and vertical tip‐sample junction leakage as sources of parasitic contrast in tomographic AFM, hindering real‐space 3D reconstructions. Novel strategies are proposed to overcome these limitations. First, the contrast mechanisms analyzing nanosized conductive features are explored when confining current collection purely to in‐plane transport, thus allowing reconstruction with a reduction in the overestimation of the lateral dimensions. Furthermore, an adaptive tip‐sample biasing scheme is demonstrated for the mitigation of a class of artefacts induced by the high electric field inside the thin oxide when volumetrically reduced. This significantly enhances vertical sensitivity by approaching the intrinsic limits set by quantum tunneling processes, allowing detailed depth analysis in thin dielectrics. The effectiveness of these methods is showcased in tomographic reconstructions of conductive filaments in valence change memory, highlighting the potential for application in nanoelectronics devices and bulk materials and unlocking new limits for tomographic AFM. This work addresses in‐plane and vertical tip‐sample junction current leakage as the fundamental sources of parasitic contrast in tomographic scanning probe microscopy (SPM), hindering real‐space 3D reconstruction. After that it proposes and demonstrates a novel strategy called adaptive scalpel SPM to mitigate this effect and significantly improve the 3D reconstructions.

Electrical atomic force microscopies (AFMs) have emerged as leading metrology techniques for evaluating the quality of 2D materials. Their advantages include high‐resolution electrical mapping, non‐destructive measurement, and the ability to probe nanoscale defects and transport properties. Conductive AFM (C‐AFM) has been particularly instrumental, enabling the direct observation of individual vacancies and vacancy clusters, voids, wrinkles, and cracks. Despite this incredible versatility, C‐AFM remains a two‐probes method, thus it is limited by the need for physical back‐contact. Creating this back contact is complex and time‐consuming. More importantly, this requirement prevents C‐AFM from being a viable in‐line metrology technique. Here, it is demonstrated that a low‐energy e‐beam impinging on the sample surface can be used to perform C‐AFM, in a new configuration that is electron‐beam (e‐beam) excited conductive atomic force microscopy (EBC‐AFM). This approach enables comparable results to classic C‐AFM sensitivity, while unlocking applications that were not previously possible. After introducing the experimental setup, the main parameters associated with the e‐beam and their impact on the C‐AFM measurement are studied. Finally, using several 2D materials as testbeds, the competitive electrical mapping capabilities of EBC‐AFM for defect assessment are demonstrated. Furthermore, this technique overcomes limitations for studying isolated flakes and enables wafer‐scale characterization of 2D materials. Electron‐beam excited conductive atomic force microscopy is demonstrated. Here, a low‐energy e‐beam impinging on the sample surface can be used to perform C‐AFM in a new configuration that enables comparable results to classic C‐AFM sensitivity, while unlocking applications previously not possible in terms of large‐area analysis and wafer‐scale metrology.

The continuous demand for improved performance in energy storage is driving the evolution of Li-ion battery technology toward emerging battery architectures such as 3D all-solid-state microbatteries (ASB). Being based on solid-state ionic processes in thin films, these new energy storage devices require adequate materials analysis techniques to study ionic and electronic phenomena. This is key to facilitate their commercial introduction. For example, in the case of cathode materials, structural, electrical and chemical information must be probed at the nanoscale and in the same area, to identify the ionic processes occurring inside each individual layer and understand the impact on the entire battery cell. In this work, we pursue this objective by using two well established nanoscale analysis techniques namely conductive atomic force microscopy (C-AFM) and secondary ion mass spectrometry (SIMS). We present a platform to study Li-ion composites with nanometer resolution that allows one to sense a multitude of key characteristics including structural, electrical and chemical information. First, we demonstrate the capability of a biased AFM tip to perform field-induced ionic migration in thin (cathode) films and its diagnosis through the observation of the local resistance change. The latter is ascribed to the internal rearrangement of Li-ions under the effect of a strong and localized electric field. Second, the combination of C-AFM and SIMS is used to correlate electrical conductivity and local chemistry in different cathodes for application in ASB. Finally, a promising starting point towards quantitative electrochemical information starting from C-AFM is indicated.

The ability to develop ferroelectric materials using binary oxides is critical to enable novel low-power, high-density non-volatile memory and fast switching logic. The discovery of ferroelectricity in hafnia-based thin films, has focused the hopes of the community on this class of materials to overcome the existing problems of perovskite-based integrated ferroelectrics. However, both the control of ferroelectricity in doped-HfO2 and the direct characterization at the nanoscale of ferroelectric phenomena, are increasingly difficult to achieve. The main limitations are imposed by the inherent intertwining of ferroelectric and dielectric properties, the role of strain, interfaces and electric field-mediated phase, and polarization changes. In this work, using Si-doped HfO2 as a material system, we performed a correlative study with four scanning probe techniques for the local sensing of intrinsic ferroelectricity on the oxide surface. Putting each technique in perspective, we demonstrated that different origins of spatially resolved contrast can be obtained, thus highlighting possible crosstalk not originated by a genuine ferroelectric response. By leveraging the strength of each method, we showed how intrinsic processes in ultrathin dielectrics, i.e., electronic leakage, existence and generation of energy states, charge trapping (de-trapping) phenomena, and electrochemical effects, can influence the sensed response. We then proceeded to initiate hysteresis loops by means of tip-induced spectroscopic cycling (i.e., “wake-up”), thus observing the onset of oxide degradation processes associated with this step. Finally, direct piezoelectric effects were studied using the high pressure resulting from the probe’s confinement, noticing the absence of a net time-invariant piezo-generated charge. Our results are critical in providing a general framework of interpretation for multiple nanoscale processes impacting ferroelectricity in doped-hafnia and strategies for sensing it.

In this study, we comprehensively investigate the constant voltage stress (CVS) time-dependent breakdown and cycle-to-breakdown while considering metal-ferroelectric-metal (MFM) memory, which has distinct domain sizes induced by different doping species, i.e., Yttrium (Y) (Sample A) and Silicon (Si) (Sample B). Firstly, Y-doped and Si-doped HfO2 MFM devices exhibit domain sizes of 5.64 nm and 12.47 nm, respectively. Secondly, Si-doped HfO2 MFM devices (Sample B) have better CVS time-dependent breakdown and cycle-to-breakdown stability than Y-doped HfO2 MFM devices (Sample A). Therefore, a larger domain size showing higher extrapolated voltage under CVS time-dependent breakdown and cycle-to-breakdown evaluations was observed, indicating that the domain size crucially impacts the stability of MFM memory.

Conductive atomic force microscopy (CAFM) is a powerful tool for studying resistive switching at the nanoscale. By applying sequences of I-V curves and biased scans the write, erase and read operations in a dielectric can be simulated in situ. CAFM can be used to monitor the inhomogeneities produced by a previous device level stress, for example conductive filaments formation and disruption. In this case the removal of the top electrode may be a problem. One attractive solution is to etch the top electrode using the CAFM tip for dielectric surface analysis, and one may also etch the dielectric to observe the shape of the filament in three dimensions. The genuine combination of electrical and mechanical stresses via CAFM tip can lead to additional setups, such as pressure modulated conductance microscopy. In the future, new experiments and CAFM related techniques may be designed to deep into the knowledge of resistive switching.