The low evaporation temperature and carcinogen classification of commonly used molybdenum trioxide (MoO3) precursor render it unsuitable for the safe and practical synthesis of molybdenum disulfide (MoS2). Furthermore, as evidenced by several experimental findings, the associated reaction constitutes a multistep process prone to the formation of uncontrolled amounts of intermediate MoS2−yOy phase mixed with the MoS2 crystals. Here, molybdenum dioxide (MoO2), a chemically more stable and safer oxide than MoO3, was utilized to successfully grow cm-scale continuous films of monolayer MoS2. A high-resolution optical image stitching approach and Raman line mapping were used to confirm the composition and homogeneity of the material grown across the substrate. A detailed examination of the surface morphology of the continuous film revealed that, as the gas flow rate increased by an order of magnitude, the grain-boundary separation dramatically reduced, implying a transition from a kinetically to thermodynamically controlled growth. Importantly, the single-step vapor-phase sulfurization (VPS) reaction of MoO2 was shown to suppress intermediate state formations for a wide range of experimental parameters investigated and is completely absent, provided that the global S:Mo loading ratio is set higher than the stoichiometric ratio of 3:1 required by the VPS reaction.

We report on a corroborative study of the structural, morphological and electrical property alterations of free-standing graphene oxide (GO) papers subject to thermal reduction. Structural analysis performed using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and Raman techniques prove that the onset of major structural changes, characterized by removal of oxygen functionalities, occur in the 200–300 °C temperature range. The results are corroborated with related morphological changes observed using Scanning electron microscopy (SEM) and Atomic force microscopy (AFM) imaging. Elemental analysis shows the GO paper reduced at 600 °C to contain an 85 wt. % carbon content and a remnant oxygen level of 13.31 wt. %. At the highest reduction temperatures, we see evidence of vacancy-type defects impeding the overall effectiveness of the reduction process. Detailed electrical resistance measurements and current–voltage (I-V) profiling conducted using four-point probe method reveals a several orders of magnitude drop in the sample resistance once the reduction temperature exceeds 200 °C, in good agreement with the structural and morphological changes. The fundamental insights revealed through these studies will be important for future applications where the electrical and mechanical properties of free-standing GO and reduced graphene oxide (rGO) are exploited in practical devices. Graphical abstract

Research in van der Waals heterostructures has been rapidly progressing in the past decade, thanks to the art of sequential and deterministic placement of one two-dimensional (2D) material over another. The successful creation of heterostructures however has relied largely on expensive transfer systems that are not easily accessible to researchers. Although a few reports on low-cost systems have recently surfaced, the full functionality, portability features, and overall effectiveness of such systems are still being explored. In this work, we present an "all-inone" low-cost transfer setup that is compact, lightweight, and portable and which can be quickly installed with a facile and do it yourself (DIY)-style anaerobic glovebox option that performs at par with commercial anaerobic systems. The "installable" glovebox option means the user has the convenience of quickly converting the working environment into an inert one when air-sensitive 2D materials are used. The lowest RH values obtained in our glovebox is <3%, and the O 2 levels rapidly drop from 21% to less than 0.1% in just a few minutes of purging the chamber with inert gas. The transfer system is also equipped with a light-weight PID-controlled substrate heating option that can be easily assembled within just a few hours. We test the versatility of our low-cost system by the successful creation of hexagonal boron nitride (hBN)-encapsulated graphene and hBN-encapsulated molybdenum disulphide (MoS 2 ) heterostructures using the hot pickup technique and graphene-hBN, MoS 2 -hBN, twisted MoS 2 , and twisted MoS 2 on hBN stacks using the wetting technique, and a MoS 2 -hBN-graphene vertical tunneling heterostructure was formed using a combination approach. The effectiveness of the DIY glovebox is proven with the demonstration of extended stability of freshly exfoliated black phosphorous (BP) flakes, their encapsulation between thin hBN layers, and the formation of electrically contacted BP devices with a protective hBN top layer. At an overall price point of approximately 1000 $, the versatile setup presented here is expected to further contribute to the growth of research in 2D materials, in particular, for researchers initially faced with overcoming a huge entry-level threshold to work in the field of 2D materials and van der Waals heterostructures.

Free-standing reduced graphene oxide (rGO) has been gaining popularity for its use in supercapacitors and battery applications due its facile synthesis, multilayered structure, and high-current carrying capacity. Pertinent to successful implementation of such applications, however, is the need to develop a thorough understanding of the electrical properties of such materials when subject to high applied electric fields. In this work, we undertake a detailed study of high-field electrical properties of mm-scale, lightly-reduced, rGO papers. Our results reveal that the I-V curves exhibit substantial nonlinearity with associated hysteresis that depends strongly on the applied electric field. The nonlinear behaviour which was interpreted using conventional transport models of Fowler-Nordheim (FN) tunneling and space charge limited conduction (SCLC) revealed that while these models provided good qualitative fits to our data, they were quantitatively lacking, thus leaving the issue of high-field transport mechanisms in rGO open for debate. Careful I-V cycling experiments with measurement time-delay introduced between cycles revealed that the observed hysteresis contained recoverable and non-recoverable parts that we identified as arising from charge trapping and Joule heating effects, respectively. Time-dependent measurements showed that these effects were characterized by two distinct time scales. Importantly, the Joule heating was found to cause a permanent conductivity improvement in the rGO via the "current annealing" effect by effectively eliminating oxygenated groups from the rGO. The analysis of the electrical breakdown in our samples resembled a thermal runaway-like event that resulted in premature damage to the rGO. Finally, we investigated the low-field resistivity in the 80 – 300 K temperature range. The reduced activation energy analysis revealed a robust power law behaviour below 230 K, while deviating from this trend at higher temperatures. For samples that received current annealing treatment, a reduced value for the power law exponent was obtained, confirming the effective lowering of disordered regions.