Thesis presented December 20, 2018
Abstract: The aim of the thesis is to develop a methodology for the investigation of Mg which acts as p-type doping in GaN. We relate the spatial distribution of the dopants with their electrical activity which is achieved by coupling two complementary approaches, Atom Probe Tomography (APT) and Off-axis electron holography. These measurements have also been combined with high-resolution electron microscopy (HR-(S)TEM) for the structural characterization. APT is a unique characterization technique, based on the field effect evaporation of individual atoms of a needle shape sample, allowing the analysis of nano-devices both in terms of morphology and composition in three dimensions at the atomic scale. Off-axis electron holography uses an electron biprism to form an interference pattern from which the electrostatic potential arising from the active dopants can be determined.
In this work the experimental procedure has been optimized for both techniques including specimen preparation, the microscope parameters and data treatment to recover accurate information about the position and activity of the dopants. For the holography measurements, a careful analysis of the artifacts that are present in these specimen has been performed to understand the effects of specimen preparation and charging under electron irradiation. We have performed these experiments at high temperature
in situ in the TEM (400 °C) as this increases the ionized dopant concentrations and reduces the artifacts that are present in our measurements. Having developed the methodology, these two techniques are then used to study the effect of temperature and dopant concentrations on the growth of Mg-doped GaN by MOCVD. We have been able to show by APT the existence of precipitates of Mg which are present from a concentration of 3
19 cm
-3 whose size and density depends on the growth temperature and the total nominal dopant concentration.
Their presence reduces the concentration of dopants that are potentially active in the specimens. However, the measurements of active dopants by holography combined with simulations suggest that the presence of these precipitates do not dominate the electrical properties of the material and that even in very highly doped specimens up to 2
20 cm
-3 the total active dopant concentrations are still higher than expected from previously published studies. The correlation between these techniques will provide valuable information to improve the Mg activation GaN which is currently a big issue for device manufacture.
Keywords: Atom probe tomography, transmission electron microscoppy, GaN nanostructures, Electron holography, Mg doping
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