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Young, Justin RSynthesis and Characterization of Novel Two-Dimensional Materials
Doctor of Philosophy, The Ohio State University, 2016, Physics
As van der Waals layered materials are reduced from bulk crystals to monolayer sheets, a host of electronic, optoelectronic, and mechanical properties emerge which differ from those of the parent materials. This variety of materials properties—coupled to the atomically thin form factor—has attracted interest from all research sectors in the past decade due to potential applications in flexible, transparent, and low-power electronics. The two-dimensional nature of these materials makes them extremely sensitive to any surface interactions presenting both a unique opportunity to tune materials properties through surface modification and also a challenge whereby any surface contaminants can dramatically degrade the material quality. In this dissertation, we investigate and utilize this surface sensitivity in three different material systems. First, we investigate electronic transport in germanane, a germanium analog of graphane, through a combination of electronic measurements on multi-layer crystals and finite-element modeling. In addition to doping this 2D material, we uncover a sensitivity of this transport to the presence of water-vapor, as well as an anisotropy between inter- and intra-layer resistivity of up to eleven orders of magnitude. The strong water sensitivity and weak inter-layer coupling mean that the transport in these samples is dominated by the topmost layer and suggests that it may be possible to measure the effects of 2D materials in bulk materials by making electrical contact to only the topmost layer. Second, we report on a templated MoS2 growth technique wherein Mo is deposited onto atomically-stepped sapphire substrates through a SiN stencil with feature sizes down to 100 nm and subsequently sulfurized at high temperature. These films have a quality comparable to the best MoS2 prepared by other methodologies, and the thickness of the resulting MoS2 patterns can be tuned layer by layer by controlling the initial Mo deposition. This approach critically enables the creation of patterned single-layer MoS2 films with pristine surfaces suitable for subsequent modification via functionalization and mechanical stacking. Further, we anticipate that this growth technique should be broadly applicable within the family of transition metal dichalcogenides. Third and finally, we present progress toward understanding how local changes to graphene’s crystal structure, such as defects, adatoms, and electromagnetic fields, affect the observable electronic and spin transport. We developed experimental methods to perform scanning probe and scanning tunneling microscopy with the simultaneous measurement of electrical transport in graphene Hall bar devices synthesized from graphene grown by chemical vapor deposition. Through the combination of these powerful experimental techniques, we plan to investigate the connection between localized surface modifications of graphene and the electronic and spin transport in these devices with eventual expansion of this technique to other 2D materials.

Committee:

Ezekiel Johnston-Halperin, Prof. (Advisor); Jay Gupta, Prof. (Committee Member); Nandini Trivedi, Prof. (Committee Member); Andrew Heckler, Prof. (Committee Member)

Subjects:

Physics

Keywords:

2D Materials; graphene; MoS2; germanane; GeH; TMDs; STM; CVD; growth

Hagerty, PhillipPhysical Vapor Deposition of Materials for Flexible Two Dimensional Electronic Devices
Master of Science (M.S.), University of Dayton, 2016, Chemical Engineering
Molybdenum Disulfide (MoS2) and Tungsten Disulfide (WS2) are two materials in a larger class of materials known as Transition Metal Dichalcogenides (TMDs) that have begun emerge as semiconducting materials. When their horizontal length scale is reduced from bulk to monolayer they demonstrate surprising combinations of properties including a direct electronic band gap and mechanical flexibility. Two dimensional (2D) materials have the potential to revolutionize performance and tailorability of electro-optical devices fabricated entirely from molecularly thin materials. In a departure from traditional exfoliation or high temperature chemical vapor deposition approaches for 2D materials synthesis, novel plasma-based physical vapor (PVD) techniques were used to fabricate uniform films over large areas. This experimental approach allowed unique studies. For example, vapor phase growth allowed systematically variation of the sulfur vacancy concentration in MoS2 and WS2 and subsequent correlation to electronic properties. This effort leads to controlled bottom-up assembly of 2D devices on flexible and standard substrates to experimentally couple the remarkable intrinsic mechanical and electronic properties of ultrathin materials, which are particularly appealing for molecular sensing. The pursuit of an all physical vapor deposited field effect transistor (FET) is the main priority for the 2D materials community as definitive demonstration of the feasibility of physical vapor deposition as a scalable technique for consumer electronics. PVD sputtered Titanium Nitride (TiN) and Tungsten (W) were experimentally characterized as potential back gated materials, Plasma Vapor Deposited (PLD) a-BN was electrically characterized as a uniform ultra-thin low temperature dielectric, and sputtered MoS2 and WS2 were electrically characterized as a semiconductor material. Tungsten deposition methods were previously researched and mimicked for smooth and conductive back gate material depositions. TiN was parameterized and the best room temperature deposition conditions were 70V applied to the sputtering gun with 25 sccm gas flow of 90% N2 and 10% Ar for 60 minutes. The best high temperature depositions were done at 500oC, 70V applied to the sputtering gun with 25 sccm gas flow of 90% N2 and 10% Ar for 30 minutes. Dielectric a-BN electrical characterization began to occur after 6nm which equated to 100 pulses, while 200 pulses equated to 16.5nm thickness. A dielectric constant of 5.90 ± .65 is reported for a-BN for under 20nm thickness. Soft probing techniques by conductively pasted gold wires on the probe tips were required to obtain true electrical measurements of 2D materials in a stacked structure, otherwise scratching would occur and uniformity would cease to exist in the film. Chemical Vapor Deposition (CVD) and mechanical exfoliation have provided the only working TMD semiconductor 2D materials in MOSFET structure to date with lithographic electrical connections. PVD sputtering as a new synthesis method for crystalline TMD with a stoichiometric ratio is achievable over large areas. Though, reduced area depositions are required for doped Silicon and Silicon Oxide (SiO2) based FET structures to limit the chance of encountering a pinhole. With reduced area and stoichiometric enhancement control, sputtered TMD films exhibit high sensitivity to oxygen and are electrically conductive even when exposed to a field effect. Increasing the grain size of the sputtered materials is the next driving force towards a fully recognizable TMD thin film transistor.

Committee:

Christopher Muratore, PhD (Committee Chair); Terrence Murray, PhD (Committee Member); Kevin Myers, DSc (Committee Member)

Subjects:

Aerospace Engineering; Aerospace Materials; Electrical Engineering; Engineering; Materials Science

Keywords:

PVD; materials; 2D materials; Nanoelectronics; TMDs; 2D Transistors; Molybdenum Disulfide; MoS2; WS2; Tungsten Disulfide