Correlated atom probe tomography, cross-sectional scanning transmission electron microscopy, and cathodoluminescence spectroscopy are used to analyze InGaN/GaN multiquantum wells (QWs) in nanowire array light-emitting diodes (LEDs). Tomographic analysis of the In distribution, interface morphology, and dopant clustering reveals material quality comparable to that of planar LED QWs. The position-dependent CL emission wavelength of the nonpolar side-facet QWs and semipolar top QWs is correlated with In composition.

GaN nanowires oriented along the nonpolar a-axis were analyzed using pulsed laser atom probe tomography (APT). Stoichiometric mass spectra were achieved by optimizing the temperature, applied dc voltage, and laser pulse energy. Local variations in the measured stoichiometry were observed and correlated with facet polarity using scanning electron microscopy. Fewer N atoms were detected from nonpolar and Ga-polar surfaces due to uncorrelated evaporation of N(2) ions following N adatom diffusion. The observed differences in Ga and N ion evaporation behaviors are considered in detail to understand the influence of intrinsic materials characteristics on the reliability of atom probe tomography analysis. We find that while reliable analysis of III-N alloys is possible, the standard APT procedure of empirically adjusting analysis conditions to obtain stoichiometric detection of Ga and N is not necessarily the best approach for this materials system.

Surface crystallography and polarity are shown to influence the detection probability of In, Ga, and N ions during atom probe tomography analysis of InxGa1−xN m-plane, c-plane, and (202¯1¯) quantum wells. A N deficit is observed in regions of the reconstruction generated from Ga-polar surfaces, and the probability of detecting group-III atoms is lower in InxGa1−xN quantum wells than in GaN barrier layers. Despite these artifacts, the detected In mole fraction is consistent throughout a given quantum well regardless of the crystal orientation of the quantum well or the evaporation surface from which the reconstruction was generated.

Focused ion beam (FIB) milling and lift‐out was used to prepare atom probe tomography (APT) specimens from GaN‐InGaN multi‐quantum well (MQW) nanowire arrays. Modifications to the conventional FIB lift‐out technique enable the site‐specific analysis of different regions of a single nanowire heterostructure. Three dimensional (3‐D) reconstructions of quantum wells generated by analysis along different directions with respect to the heterointerface demonstrate both the capabilities and limitations of atom probe tomographic analysis. The methods described herein can be applied to the site‐specific analysis of other complex 3‐D heterostructures. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)

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