Quantification of trace-level silicon doping in Al_xGa_1–xN films using wavelength-dispersive X-ray microanalysis

Wavelength dispersive X-ray (WDX) spectroscopy was used to measure silicon atom concentrations in the range 35–100 ppm (corresponding to (3–9) ×10¹⁸ cm^-3) in doped AlxGa1–xN films using an electron probe microanalyser also equipped with a cathodoluminescence (CL) spectrometer. Doping with Si is the usual way to produce the n-type conducting layers that are critical in GaN and AlxGa1–xN-based devices such as LEDs and laser diodes. Previously we have shown excellent agreement for Mg dopant concentrations in p-GaN measured by WDX with values from the more widely used technique of secondary ion mass spectrometry (SIMS). However, a discrepancy between these methods has been reported when quantifying the n-type dopant, silicon. We identify the cause of discrepancy as inherent sample contamination and propose a way to correct this using a calibration relation. This new approach, using a method combining data derived from SIMS measurements on both GaN and Al_xGa_1–xN samples, provides the means to measure the Si content in these samples with account taken of variations in the ZAF corrections. This method presents a cost effective and time saving way to measure the Si doping and can also benefit from simultaneously measuring other signals, such as CL and electron channeling contrast imaging.