Focused Ion Beam-induced Fluorescence Spectroscopy: Mechanisms, Characterization, Instrumentation, and Application

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This dissertation provides an investigation into the physics of photon emission as a result of energetic ion bombardment on material surfaces and the development of a novel technique in the form of Focused Ion Beam-induced Fluorescence Spectroscopy (FIB-FS) capable of performing 2D and 3D elemental analysis from these signals at the nanoscale. It details the engineering and design of highly sensitive, versatile prototype instrumentation that detects these photons and provides methods and workflows developed to characterize, optimize, and extract various forms of information from the specimen using FIB-FS. Characterization of the technique’s fundamental limits are included in the first recorded measurements of lateral resolution and depth resolution on calibrated certified standards. A lateral resolution of 15.5 nm, a depth resolution of 12.8 nm, parts-per-million trace concentration detection sensitivity, and the ability to detect light elements such as Li and H are reported along with a demonstration of its application to Li-ion battery research and development. The results are benchmarked against well-established techniques of energy-dispersive X-ray spectroscopy (EDX) and secondary ion mass spectrometry (SIMS) to show FIB-FS as both complementary and competitive. Furthermore, the technique is used to investigate materials under various chemical environments and bombardment conditions, elucidating the physical nature behind the mechanisms of sputtered atom excitation and photon emission. Photon yields from excited sputtered atoms with different charge states under various oxygen environments are reported that are not explained with existing models, laying the groundwork for a new mechanistic description. FIB-FS is demonstrated as a high-resolution, sensitive, multifaceted analytical technique for multidimensional elemental analysis at the nanoscale and is poised for the advancement of fundamental insights into atomic excitation processes.
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