One sentence summary:We describe a general liquid-phase method to exfoliate layered compounds to give monoand few-layer flakes in large quantities. TMDs consist of hexagonal layers of metal atoms, M, sandwiched between two layers of chalcogen atoms, X, with stoichiometry MX 2 . While the bonding within these tri-layer sheets is covalent, adjacent sheets stack via van der Waals interactions to form a 3D crystal. TMDs occur in more than 40 different types (2, 3) depending on the combination of chalcogen (S, Se or Te) and transition metal(3). Depending on the co-ordination and oxidation state of the metal atoms, TMDs can be metallic, semi-metallic or semiconducting(2, 3), e.g. WS 2 is a semiconductor while NbSe 2 is a metal(3). In addition, superconductivity(4) and charge density wave effects(5) have been observed in some TMDs. This versatility makes them potentially useful in many areas of electronics.However, like graphene(6), layered materials must be exfoliated to fulfil their full potential. For example, films of exfoliated Bi 2 Te 3 should display enhanced thermoelectric efficiency by suppression of thermal conductivity(7). Exfoliation of 2D topological insulators such as Bi 2 Te 3 and Bi 2 Se 3 would reduce residual bulk conductance, 4 highlighting surface effects. In addition, we can expect changes in electronic properties as the number of layers is reduced e.g. the indirect bandgap of bulk MoS 2 becomes direct in few-layer flakes(8). Although exfoliation can be achieved mechanically on a small scale(9, 10), liquid phase exfoliation methods are required for many applications(11).Critically, a simple liquid exfoliation method would allow the formation of novel hybrid and composite materials. While TMDs can be chemically exfoliated in liquids(12-14), this method is time consuming, extremely sensitive to the environment and incompatible with most solvents.We demonstrate exfoliation of bulk TMD crystals in common solvents to give mono-and few layer nano-sheets. This method is insensitive to air and water and can potentially be scaled up to give large quantities of exfoliated material. In addition, we show that this procedure allows the formation of hybrid films with enhanced properties.We initially sonicated commercial MoS 2 , WS 2 and BN (15, 16) powders in a number of solvents with varying surface tensions. The resultant dispersions were centrifuged and the supernatant decanted (Section S3). Optical absorption spectroscopy showed that the amount of material retained (characterised by / A l C α = , where A/l is the absorbance per length, α is the extinction coefficient and C is the concentration) was maximised for solvents with surface tension close to 40 mJ/m 2 (17, 18) ( Fig. 1A-C). Detailed analysis, within the framework of Hansen solubility parameter theory(19), shows successful solvents to be those with dispersive, polar and H-bonding components of the cohesive energy density within certain well-defined ranges (Section S4, Figs. S2-S3). This can be interpreted to mean that successful solvents are those w...

Few-layer black phosphorus (BP) is a new two-dimensional material which is of great interest for applications, mainly in electronics. However, its lack of environmental stability severely limits its synthesis and processing. Here we demonstrate that high-quality, few-layer BP nanosheets, with controllable size and observable photoluminescence, can be produced in large quantities by liquid phase exfoliation under ambient conditions in solvents such as N-cyclohexyl-2-pyrrolidone (CHP). Nanosheets are surprisingly stable in CHP, probably due to the solvation shell protecting the nanosheets from reacting with water or oxygen. Experiments, supported by simulations, show reactions to occur only at the nanosheet edge, with the rate and extent of the reaction dependent on the water/oxygen content. We demonstrate that liquid-exfoliated BP nanosheets are potentially useful in a range of applications from ultrafast saturable absorbers to gas sensors to fillers for composite reinforcement.

Layered two-dimensional (2D) materials display great potential for a range of applications, particularly in electronics. We report the large-scale synthesis of thin films of platinum diselenide (PtSe), a thus far scarcely investigated transition metal dichalcogenide. Importantly, the synthesis by thermally assisted conversion is performed at 400 °C, representing a breakthrough for the direct integration of this material with silicon (Si) technology. Besides the thorough characterization of this 2D material, we demonstrate its promise for applications in high-performance gas sensing with extremely short response and recovery times observed due to the 2D nature of the films. Furthermore, we realized vertically stacked heterostructures of PtSe on Si which act as both photodiodes and photovoltaic cells. Thus, this study establishes PtSe as a potential candidate for next-generation sensors and (opto-)electronic devices, using fabrication protocols compatible with established Si technologies.

High‐performance sensors based on molybdenum disulfide (MoS2) grown by sulfurization of sputtered molybdenum layers are presented. Using a simple integration scheme, it is found that the electrical conductivity of MoS2 films is highly sensitive to NH3 adsorption, consistent with n‐type semiconducting behavior. A sensitivity of 300 ppb at room temperature is achieved, showing the high potential of 2D transition metal‐dichalcogenides for sensing.

Semiconducting 2D MoS2 flakes produced by liquid phase exfoliation are contacted with metal electrodes, which are defined by electron beam lithography. Electrical analysis of the metal–semiconductor–metal structures reveals high mobilities for individual MoS2 flakes. Thus, scalable liquid‐phase exfoliation of layered semiconductor compounds can yield novel materials with potential uses in future electronic devices.

Please cite this article in press as: R. Gatensby, et al., Controlled synthesis of transition metal dichalcogenide thin films for electronic applications, Appl. Surf. Sci. (2014) Two dimensional transition metal dichalcogenides (TMDs) are exciting materials for future applications in nanoelectronics, nanophotonics and sensing. In particular, sulfides and selenides of molybdenum (Mo) and tungsten (W) have attracted interest as they possess a band gap, which is important for integration into electronic device structures. However, the low throughput synthesis of high quality TMD thin films has thus far hindered the development of devices, and so a scalable method is required to fully exploit their exceptional properties. Within this work a facile route to the manufacture of devices from MoS 2 and WS 2 , grown by vapour phase sulfurisation of pre-deposited metal layers, is presented. Highly homogenous TMD films are produced over large areas. Fine control over TMD film thickness, down to a few layers, is achieved by modifying the thickness of the pre-deposited metal layer. The films are characterised by Raman spectroscopy, electron microscopy and X-ray photoelectron spectroscopy. The thinnest films exhibit photoluminescence, as predicted for monolayer MoS 2 films, due to confinement in two dimensions. By using shadow mask lithography, films with well-defined geometries were produced and subsequently integrated with standard microprocessing process flows and electrically characterised. In this way, MoS 2 based sensors were produced, displaying sensitivity to NH 3 down to 400 ppb. Our device manufacture is versatile, and is adaptable for future nanoscale (opto-) electronic devices as it is reproducible, cost effective and scalable up to wafer scale.

We report the manufacture of novel graphene diode sensors (GDS), which are composed of monolayer graphene on silicon substrates, allowing exposure to liquids and gases. Parameter changes in the diode can be correlated with charge transfer from various adsorbates. The GDS allows for investigation and tuning of extrinsic doping of graphene with great reliability. The demonstrated recovery and long-term stability qualifies the GDS as a new platform for gas, environmental, and biocompatible sensors.

The unique properties and atomic thickness of two-dimensional (2D) materials enable smaller and better nanoelectromechanical sensors with novel functionalities. During the last decade, many studies have successfully shown the feasibility of using suspended membranes of 2D materials in pressure sensors, microphones, accelerometers, and mass and gas sensors. In this review, we explain the different sensing concepts and give an overview of the relevant material properties, fabrication routes, and device operation principles. Finally, we discuss sensor readout and integration methods and provide comparisons against the state of the art to show both the challenges and promises of 2D material-based nanoelectromechanical sensing.