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Hydrogen lithography has been used to template phosphine-based surface chemistry to fabricate atomic-scale devices, a process we abbreviate as atomic precision advanced manufacturing (APAM). Here, we use mid-infrared variable angle spectroscopic ellipsometry (IR-VASE) to characterize single-nanometer thickness phosphorus dopant layers (δ-layers) in silicon made using APAM compatible processes. A large Drude response is directly attributable to the δ-layer and can be used for nondestructive monitoring of the condition of the APAM layer when integrating additional processing steps. The carrier density and mobility extracted from our room temperature IR-VASE measurements are consistent with cryogenic magneto-transport measurements, showing that APAM δ-layers function at room temperature. Finally, the permittivity extracted from these measurements shows that the doping in the APAM δ-layers is so large that their low-frequency in-plane response is reminiscent of a silicide. However, there is no indication of a plasma resonance, likely due to reduced dimensionality and/or low scattering lifetime.
In this article, we review focused ion beam serial sectioning microscopy paired with analytical techniques, such as electron backscatter diffraction or x-ray energy-dispersive spectrometry, to study materials chemistry and structure in three dimensions. These three-dimensional microanalytical approaches have been greatly extended due to advances in software for both microscope control and data interpretation. Samples imaged with these techniques reveal structural features of materials that can be quantitatively characterized with rich chemical and crystallographic detail. We review these technological advances and the application areas that are benefitting. We also consider the challenges that remain for data collection, data processing, and visualization, which collectively limit the scale of these investigations. Further, we discuss recent innovations in quantitative analyses and numerical modeling that are being applied to microstructures illuminated by these techniques.