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202941 https://hdl.handle.net/2286/R.2.N.202941 http://rightsstatements.org/vocab/InC/1.0/ All Rights Reserved 2025 103 pages Doctoral Dissertation Academic theses en Bustamante, Michael Navrotsky, Alexandra Green, Mathew Muhich, Christopher Yang, Sui Arizona State University Partial requirement for: Ph.D., Arizona State University, 2025 Field of study: Materials Science and Engineering Gallium-based liquid metal alloys (Ga-LMAs) have applications in soft robotics, microelectronics, self-healing materials, and 2D material synthesis. But within calorimetry, they have been critical for precise high temperature energetic measurements of metals, alloys, and other multicomponent non-oxides. This thesis demonstrates that Ga-LMAs hold promise to modernize commercial thermal analysis calorimeters and methods. These advancements can collect data for equilibria that are not adequate or hard to measure in traditional high temperature calorimetry (HTC) techniques, the solutions presented are employed in specific examples. The systems tested were air-sensitive materials that require complex instruments and controlled atmosphere for reactivity prevention, and those with slow dissolution rates in standard oxide melts. These approaches expand the use of thermal analysis instruments and can test liquid states, facilitating the exploration of new compositional spaces, compounds, and solutions.The aim of this work is also to investigate and create solutions for the limitations of current calorimetry techniques, including oxidative/metallic melt solution calorimetries, advances in the use of Ga, Ga-base, and other metallic solvents paired with custom-designed add-ons can enhance data collection in calorimetry. These methodologies enable direct calculation of enthalpies of formation (ΔHf) and mixing (ΔHmix) for alloys that can be compared to thermodynamic modeling tools while potentially stabilizing new high temperature phases/intermetallics. The processes implemented, in the AlexSYS and MHTC-96 calorimeters (Setaram), yielded accurate results, showing strong agreement with measurements in conventional HTC. Engineering Chemical Engineering Chemistry Cementitious waste forms characterization using CEMGEMS Drop Solution Calorimetry in Metallic Solvents experimental calorimetry Liquid Metal Calorimetry Through the Oxidative Solution Method MHTC-96 Custom Design High Temperature Drop Solution Calorimetry: Expanding the Horizons of Non-Oxide Thermodynamics via Customized Ga-based Experimental Techniques