Correlative Scanning Transmission Electron Microscopy Research Articles

Atomic-scale investigation of implanted Mg in GaN through ultra-high-pressure annealing

An area selective doping via ion implantation is a key technology to realize gallium nitride (GaN) based energy-efficient power devices; however, conventional annealing leads to the formation of numerous Mg-enriched defects, which result in inefficient p-type activation. The recent invention of ultra-high-pressure annealing (UHPA) has enabled a significant improvement in p-type activation efficiency. In this study, we investigated the formation of Mg-enriched defects in Mg implanted GaN followed by annealing under either conventional atmospheric pressure or ultra-high-pressure. Unlike the conventional annealing, UHPA leads to a much lower number density of Mg-enriched defects. Correlative scanning transmission electron microscopy, atom probe tomography, cathodoluminescence, and secondary ion mass spectrometry analyses have shown that the number density of Mg-enriched defects is substantially suppressed by the UHPA. The dissolved Mg concentrations in the GaN matrix for both the conventional and the UHPA samples are almost of the same value, approximately 2 × 1018 cm−3; however, the UHPA sample shows over one order of magnitude stronger intensity of donor–acceptor-pair emission than the conventional one. Thus, the implanted Mg is effectively activated as acceptors through the UHPA technique.

Influence of implanted Mg concentration on defects and Mg distribution in GaN

Efficient acceptor activation in gallium nitride (GaN) achieved through Mg ion-implantation depends mainly on the concentration of implanted Mg ions and the post-implantation annealing process. In this study, we conducted correlative scanning transmission electron microscopy, atom probe tomography, and cathodoluminescence (CL) measurements on Mg-implanted GaN layers with the implanted concentration ranging from 1 × 1017 cm−3 to 1 × 1019 cm−3. It was found that at the implanted concentration of ∼1 × 1018 cm−3, Mg atoms were randomly distributed with defects likely to be vacancy clusters whereas at the implanted concentration of ∼1 × 1019 cm−3, Mg-enriched clusters and dislocation loops were formed. From the CL measurements, the donor–acceptor pair (DAP) emissions from the implanted and un-implanted regions are obtained and then compared to analyze Mg activation in these regions. In the sample with Mg ∼1 × 1019 cm−3, the existence of Mg-enriched clusters and dislocations in the implanted region leads to a weaker DAP emission, whereas the absence of Mg-enriched clusters and dislocations in the sample with Mg ∼1 × 1018 cm−3 resulted in a relatively stronger DAP emission.

Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy.

Alnico alloys have long been used as strong permanent magnets because of their ferromagnetism and high coercivity. Understanding their structural details allows for better prediction of the resulting magnetic properties. However, quantitative three-dimensional characterization of the phase separation in these alloys is still challenged by the spatial quantification of nanoscale phases. Herein, we apply a dual tomography approach, where correlative scanning transmission electron microscopy (STEM) energy-dispersive X-ray spectroscopic (EDS) tomography and atom probe tomography (APT) are used to investigate the initial phase separation process of an alnico 8 alloy upon non-magnetic annealing. STEM-EDS tomography provides information on the morphology and volume fractions of Fe-Co-rich and Νi-Al-rich phases after spinodal decomposition in addition to quantitative information of the composition of a nanoscale volume. Subsequent analysis of a portion of the same specimen by APT offers quantitative chemical information of each phase at the sub-nanometer scale. Furthermore, APT reveals small, 2-4 nm Fe-rich α 1 phases that are nucleated in the Ni-rich α 2 matrix. From this information, we show that phase separation of the alnico 8 alloy consists of both spinodal decomposition and nucleation and growth processes. The complementary benefits and challenges associated with correlative STEM-EDS and APT are discussed.

Multi-microscopy study of the influence of stacking faults and three-dimensional In distribution on the optical properties of m-plane InGaN quantum wells grown on microwire sidewalls

The optical properties of m-plane InGaN/GaN quantum wells grown on microwire sidewalls were investigated carrying out a correlative scanning transmission electron microscopy (STEM), atom probe tomography (APT), and micro-photoluminescence study applied on single nanoscale field-emission tips obtained by a focused ion beam annular milling. Instead of assuming simple rectangular composition profiles, yielding misleading predictions for the optical transition energies, we can thus take into account actual compositional distributions and the presence of stacking faults (SFs). SFs were shown to be responsible for a lowering of the recombination energies of the order of 0.1 eV with respect to those expected for defect-free quantum wells (QWs). Such energy reduction allows establishing a good correspondence between the transition energies observed by optical spectroscopy and those calculated on the basis of the QWs In measured composition and distribution assessed by STEM structural analysis and APT chemical mapping.

Site controlled red-yellow-green light emitting InGaN quantum discs on nano-tipped GaN rods.

We report a method of growing site controlled InGaN multiple quantum discs (QDs) at uniform wafer scale on coalescence free ultra-high density (>80%) nanorod templates by metal organic chemical vapour deposition (MOCVD). The dislocation and coalescence free nature of the GaN space filling nanorod arrays eliminates the well-known emission problems seen in InGaN based visible light sources that these types of crystallographic defects cause. Correlative scanning transmission electron microscopy (STEM), energy-dispersive X-ray (EDX) mapping and cathodoluminescence (CL) hyperspectral imaging illustrates the controlled site selection of the red, yellow and green (RYG) emission at these nano tips. This article reveals that the nanorod tips' broad emission in the RYG visible range is in fact achieved by manipulating the InGaN QD's confinement dimensions, rather than significantly increasing the In%. This article details the easily controlled method of manipulating the QDs dimensions producing high crystal quality InGaN without complicated growth conditions needed for strain relaxation and alloy compositional changes seen for bulk planar GaN templates.