We demonstrate a combination of micro four-point probe (M4PP) and non-contact terahertz time-domain spectroscopy (THz-TDS) measurements for centimeter scale quantitative mapping of the sheet conductance of large area chemical vapor deposited graphene films. Dual configuration M4PP measurements, demonstrated on graphene for the first time, provide valuable statistical insight into the influence of microscale defects on the conductance, while THz-TDS has potential as a fast, non-contact metrology method for mapping of the spatially averaged nanoscopic conductance on wafer-scale graphene with scan times of less than a minute for a 4-in. wafer. The combination of M4PP and THz-TDS conductance measurements, supported by micro Raman spectroscopy and optical imaging, reveals that the film is electrically continuous on the nanoscopic scale with microscopic defects likely originating from the transfer process, dominating the microscale conductance of the investigated graphene film.
The significant progress in terms of fabricating large-area graphene films for transparent electrodes, barriers, electronics, telecommunication and other applications has not yet been accompanied by efficient methods for characterizing the electrical properties of large-area graphene. While in the early prototyping as well as research and development phases, electrical test devices created by conventional lithography have provided adequate insights, this approach is becoming increasingly problematic due to complications such as irreversible damage to the original graphene film, contamination, and a high measurement effort per device. In this topical review, we provide a comprehensive overview of the issues that need to be addressed by any large-area characterisation method for electrical key performance indicators, with emphasis on electrical uniformity and on how this can be used to provide a more accurate analysis of the graphene film. We review and compare three different, but complementary approaches that rely either on fixed contacts (dry laser lithography), movable contacts (micro four point probes) and non-contact (terahertz timedomain spectroscopy) between the probe and the graphene film, all of which have been optimized for maximal throughput and accuracy, and minimal damage to the graphene film. Of these three, the main emphasis is on THz time-domain spectroscopy, which is non-destructive, highly accurate and allows both conductivity, carrier density and carrier mobility to be mapped across arbitrarily large areas at rates that by far exceed any other known method. We also detail how the THz conductivity spectra give insights on the scattering mechanisms, and through that, the microstructure of graphene films subject to different growth and transfer processes. The perspectives for upscaling to realistic production environments are discussed. TOPICAL REVIEWOriginal content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence.
The origin of threshold voltage instability with gate voltage in MoS 2 transistors is poorly understood but critical for device reliability and performance. Reversibility of the temperature dependence of hysteresis and its inversion with temperature in MoS 2 transistors has not been demonstrated. In this work, we delineate two independent mechanisms responsible for thermally assisted hysteresis inversion in gate transfer characteristics of contact resistance-independent multilayer MoS 2 transistors. Variable temperature hysteresis measurements were performed on gated four-terminal van der Pauw and two-terminal devices of MoS 2 on SiO 2 . Additional hysteresis measurements on suspended (~100 nm air gap between MoS 2 and SiO 2 ) transistors and under different ambient conditions (vacuum/nitrogen) were used to further isolate the mechanisms. Clockwise hysteresis at room temperature (300 K) that decreases with increasing temperature is shown to result from intrinsic defects/traps in MoS 2 . At higher temperatures a second, independent mechanism of charge trapping and de-trapping between the oxide and p + Si gate leads to hysteresis collapse at~350 K and anti-clockwise hysteresis (inversion) for temperatures >350 K. The intrinsic-oxide trap model has been corroborated through device simulations. Further, pulsed current-voltage (I-V) measurements were carried out to extract the trap time constants at different temperatures. Non-volatile memory and temperature sensor applications exploiting temperature dependent hysteresis inversion and its reversibility in MoS 2 transistors have also been demonstrated. npj 2D Materials and Applications (2017) 1:34 ; doi:10.1038/s41699-017-0038-y INTRODUCTION Among two-dimensional materials, graphene 1,2 was the first to be isolated and studied with respect to electronic applications. Due to lack of an energy bandgap in graphene, other 2D materials such as layered transition metal dichalcogenides (TMDs) comprising a wide selection of materials with different bandstructures, and therefore different electrical and optical properties, have garnered significant attention.3-5 Molybdenum disulfide (MoS 2 ) has emerged as a prospective candidate for transistor applications. The presence of a direct bandgap (~1.8 eV) in monolayer form and an indirect bandgap (~1.2 eV) in multilayer MoS 2 makes it a promising channel material for field effect transistors (FETs).
The electrical performance of graphene synthesized by chemical vapor deposition and transferred to insulating surfaces may be compromised by extended defects, including for instance grain boundaries, cracks, wrinkles, and tears. In this study, we experimentally investigate and compare the nano- and microscale electrical continuity of single layer graphene grown on centimeter-sized single crystal copper with that of previously studied graphene films, grown on commercially available copper foil, after transfer to SiO2 surfaces. The electrical continuity of the graphene films is analyzed using two noninvasive conductance characterization methods: ultrabroadband terahertz time-domain spectroscopy and micro four-point probe, which probe the electrical properties of the graphene film on different length scales, 100 nm and 10 μm, respectively. Ultrabroadband terahertz time-domain spectroscopy allows for measurement of the complex conductance response in the frequency range 1-15 terahertz, covering the entire intraband conductance spectrum, and reveals that the conductance response for the graphene grown on single crystalline copper intimately follows the Drude model for a barrier-free conductor. In contrast, the graphene grown on commercial copper foil shows a distinctly non-Drude conductance spectrum that is better described by the Drude-Smith model, which incorporates the effect of preferential carrier backscattering associated with extended, electronic barriers with a typical separation on the order of 100 nm. Micro four-point probe resistance values measured on graphene grown on single crystalline copper in two different voltage-current configurations show close agreement with the expected distributions for a continuous 2D conductor, in contrast with previous observations on graphene grown on commercial copper foil. The terahertz and micro four-point probe conductance values of the graphene grown on single crystalline copper shows a close to unity correlation, in contrast with those of the graphene grown on commercial copper foil, which we explain by the absence of extended defects on the microscale in CVD graphene grown on single crystalline copper. The presented results demonstrate that the graphene grown on single crystal copper is electrically continuous on the nanoscopic, microscopic, as well as intermediate length scales.
The evolution of grapheneʼs electrical transport properties due to processing with the polymer polymethyl methacrylate (PMMA) and heat are examined in this study. The use of stencil (shadow mask) lithography enables fabrication of graphene devices without the usage of polymers, chemicals or heat, allowing us to measure the evolution of the electrical transport properties during individual processing steps from the initial as-exfoliated to the PMMA-processed graphene. Heating generally promotes the conformation of graphene to SiO2 and is found to play a major role for the electrical properties of graphene while PMMA residues are found to be surprisingly benign. In accordance with this picture, graphene devices with initially high carrier mobility tend to suffer a decrease in carrier mobility, while in contrast an improvement is observed for low carrier mobility devices. We explain this by noting that flakes conforming poorly to the substrate will have a higher carrier mobility which will however be reduced as heat treatment enhance the conformation. We finally show the electrical properties of graphene to be reversible upon heat treatments in air up to 200 °C.
Carrier mobility and chemical doping level are essential figures of merit for graphene, and large-scale characterization of these properties and their uniformity is a prerequisite for commercialization of graphene for electronics and electrodes. However, existing mapping techniques cannot directly assess these vital parameters in a non-destructive way. By deconvoluting carrier mobility and density from non-contact terahertz spectroscopic measurements of conductance in graphene samples with terahertz-transparent backgates, we are able to present maps of the spatial variation of both quantities over large areas. The demonstrated non-contact approach provides a drastically more efficient alternative to measurements in contacted devices, with potential for aggressive scaling towards wafers/minute. The observed linear relation between conductance and carrier density in chemical vapour deposition graphene indicates dominance by charged scatterers. Unexpectedly, significant variations in mobility rather than doping are the cause of large conductance inhomogeneities, highlighting the importance of statistical approaches when assessing large-area graphene transport properties.
We report a new microscale Hall effect measurement method for characterization of semiconductor thin films without need for conventional Hall effect geometries and metal contact pads. We derive the electrostatic potential resulting from current flow in a conductive filamentary sheet with insulating barriers and with a magnetic field applied normal to the plane of the sheet. Based on this potential, analytical expressions for the measured four-point resistance in presence of a magnetic field are derived for several simple sample geometries. We show how the sheet resistance and Hall effect contributions may be separated using dual configuration measurements. The method differs from conventional van der Pauw measurements since the probe pins are placed in the interior of the sample region, not just on the perimeter. We experimentally verify the method by micro-four-point probe measurements on ultrashallow junctions in silicon and germanium. On a cleaved silicon ultrashallow junction sample we determine carrier mobility, sheet carrier density, and sheet resistance from micro-four-point probe measurements under various experimental conditions, and show with these conditions reproducibility within less than 1.5%.
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