In the surge of recent successes of 2D materials following the rise of graphene, molybdenum disulfide (2D-MoS₂) has been attracting growing attention from both fundamental and applications viewpoints, owing to the combination of its unique nanoscale properties. For instance, the bandgap of 2D-MoS₂, which changes from direct (in the bulk form) to indirect for ultrathin films (few layers), offers new prospects for various applications in optoelectronics. In this review, we present the latest scientific advances in the field of synthesis and characterization of 2D-MoS₂ films while highlighting some of their applications in energy harvesting, gas sensing, and plasmonic devices. A survey of the physical and chemical processing routes of 2D-MoS₂ is presented first, followed by a detailed description and listing of the most relevant characterization techniques used to study the MoS₂ nanomaterial as well as theoretical simulations of its interesting optical properties. Finally, the challenges related to the synthesis of high quality and fairly controllable MoS₂ thin films are discussed along with their integration into novel functional devices.

Tungsten disulfide nanosheets were successfully prepared by one-step chemical vapor deposition using tungsten oxide and thiourea in an inert gas environment. The size of the obtained nanosheets was subsequently reduced down to below 20 nm in width and 150 nm in length using high-energy ball milling, followed by 0.5 and 1 wt% graphene loading. The corresponding vibrational and structural characterizations are consistent with the fabrication of a pure WS₂ structure for neat sampling and the presence of the graphene characteristic vibration modes in graphene@WS₂ compounds. Additional morphological and crystal structures were examined and confirmed by high-resolution electron microscopy. Subsequently, the investigations of the optical properties evidenced the high optical absorption (98%) and lower band gap (1.75 eV) for the graphene@WS₂ compared to the other samples, with good band-edge alignment to water-splitting reaction. In addition, the photoelectrochemical measurements revealed that the graphene@WS₂ (1 wt%) exhibits an excellent photocurrent density (95 μA/cm² at 1.23 V bias) compared with RHE and higher applied bias potential efficiency under standard simulated solar illumination AM1.5G. Precisely, graphene@WS₂ (1 wt%) exhibits 3.3 times higher performance compared to pristine WS₂ and higher charge transfer ability, as measured by electrical impedance spectroscopy, suggesting its potential use as an efficient photoanode for hydrogen evolution reaction.

Reference samples are commonly used for the calibration and quantification of nanoscale electrical measurements of capacitances and dielectric constants in scanning microwave microscopy (SMM) and similar techniques. However, the traceability of these calibration samples is not established. In this work, we present a detailed investigation of most possible error sources that affect the uncertainty of capacitance measurements on the reference calibration samples. We establish a comprehensive uncertainty budget leading to a combined uncertainty of 3% in relative value (uncertainty given at one standard deviation) for capacitances ranging from 0.2 fF to 10 fF. This uncertainty level can be achieved even with the use of unshielded probes. We show that the weights of uncertainty sources vary with the values and dimensions of measured capacitances. Our work offers improvements on the classical calibration methods known in SMM and suggests possible new designs of reference standards for capacitance and dielectric traceable measurements. Experimental measurements are supported by numerical calculations of capacitances to reveal further paths for even higher improvements.

The importance of high dielectric constant materials in the development of high frequency nano-electronic devices is undeniable. Their polarization properties are directly dependent on the value of their relative permittivity. We report here on the nanoscale metrological quantification of the dielectric constants of two high-κ materials, lead zirconate titanate (PZT) and lead magnesium niobate-lead titanate (PMN-PT), in the GHz range using scanning microwave microscopy (SMM). We demonstrate the importance of the capacitance calibration procedure and dimensional measurements on the weight of the combined relative uncertainties. A novel approach is proposed to correct lateral dimension measurements of micro-capacitive structures using the microwave electrical signatures, especially for rough surfaces of high-κ materials. A new analytical expression is also given for the capacitance calculations, taking into account the contribution of fringing electric fields. We determine the dielectric constant values ε_PZT = 445 and ε_PMN-PT = 641 at the frequency around 3.6 GHz, with combined relative uncertainties of 3.5% and 6.9% for PZT and PMN-PT, respectively. This work provides a general description of the metrological path for a quantified measurement of high dielectric constants with well-controlled low uncertainty levels.

Measuring resistances at the nanoscale has attracted recent attention for developing microelectronic components, memory devices, molecular electronics, and two-dimensional materials. Despite the decisive contribution of scanning probe microscopy in imaging resistance and current variations, measurements have remained restricted to qualitative comparisons. Reference resistance calibration samples are key to advancing the research-to-manufacturing process of nanoscale devices and materials through calibrated, reliable, and comparable measurements. No such calibration reference samples have been proposed so far. In this work, we demonstrate the development of a multi-resistance reference sample for calibrating resistance measurements in conductive probe atomic force microscopy (C-AFM) covering the range from 100 Ω to 100 GΩ. We present a comprehensive protocol for in situ calibration of the whole measurement circuit encompassing the tip, the current sensing device, and the system controller. Furthermore, we show that our developed resistance reference enables the calibration of C-AFM with a combined relative uncertainty (given at one standard deviation) lower than 2.5% over an extended range from 10 kΩ to 100 GΩ and lower than 1% for a reduced range from 1 MΩ to 50 GΩ. Our findings break through the long-standing bottleneck in C-AFM measurements, providing a universal means for adopting calibrated resistance measurements at the nanoscale in the industrial and academic research and development sectors.

Noninvasive and depth‐sensitive measurements of dielectric properties are becoming of great interest in advanced and complex nanostructured architectures. Here, a straightforward parallel approach applicable in peak force Kelvin probe force microscopy for a 3D measurement of dielectric constants at the nanoscale is demonstrated. The proposed approach features a simultaneous measurement of the mechanical, electrical, and depth‐dependent dielectric properties applied to embedded nanostructures. The findings provide initial elements for further development of experimental dielectric nano‐tomography methods for characterizing buried and embedded systems and dielectric interfaces.