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Semiconductor nanowires (NWs) are believed to play a crucial role for future applications in electronics, spintronics and quantum technologies. A potential candidate is HgTe but its sensitivity to nanofabrication processes restrain its development. A way to circumvent this obstacle is the selective area growth technique. Here, in-plane HgTe nanostructures are grown thanks to selective area molecular beam epitaxy on a semi-insulating CdTe substrate covered with a patterned SiO 2 mask. The shape of these nanostructures is defined by the in-plane orientation of the mask aperture along the <110>, <11¯0>, or <100> direction, the deposited thickness, and the growth temperature (GT). Several micron long in-plane NWs can be achieved as well as more complex nanostructures such as networks, diamond structures or rings. A good selectivity is achieved with very little parasitic growth on the mask even for a GT as low as 140 °C and growth rate up to 0.5 monolayer per second. For <110> oriented NWs, the center of the nanostructure exhibits a trapezoidal shape with {111}B facets and two grains on the sides, while <11¯0> oriented NWs show {111}A facets with adatoms accumulation on the sides of the top surface. Transmission electron microscopy observations reveal a continuous epitaxial relation between the CdTe substrate and the HgTe NW. Measurements of the resistance with four-point scanning tunneling microscopy indicates a good electrical homogeneity along the main NW axis and a thermally activated transport. This growth method paves the way toward the fabrication of complex HgTe-based nanostructures for electronic transport measurements., (© 2024 IOP Publishing Ltd. All rights, including for text and data mining, AI training, and similar technologies, are reserved.)

The methodology of statistical analysis of cathodoluminescence (CL) intensity mappings on ensembles of several hundreds of InGaN/GaN nanowires (NWs) used to quantify non-radiative recombination centres (NRCs) was validated on InGaN/GaN NWs exhibiting spatially homogeneous cathodoluminescence at the scale of single NWs. Cathodoluminescence intensity variations obeying Poisson's statistics were assigned to the presence of randomly incorporated point defects acting as NRCs. Additionally, another type of NRCs, namely extended defects leading to spatially inhomogeneous cathodoluminescence intensity at the scale of single InGaN/GaN NWs are revealed by high resolution scanning transmission electron microscopy, geometrical phase analysis and two-beam diffraction conditions techniques. Such defects are responsible for deviations from Poisson's statistics, allowing one to achieve a rapid evaluation of the crystallographic and optical properties of several hundreds of NWs in a single cathodoluminescence intensity mapping experiment., (© 2024 IOP Publishing Ltd. All rights, including for text and data mining, AI training, and similar technologies, are reserved.)

In order to elucidate the mechanisms responsible for cathodoluminescence intensity variations at the scale of single InGaN/GaN nanowire heterostructures, a methodology is proposed based on a statistical analysis on ensembles of several hundreds of nanowires exhibiting a diameter of 180, 240 and 280 nm. For 180 nm diameter, we find that intensitiy variations are consistent with incorporation of point defects obeying Poisson's statistics. For wider diameters, intensity variations at the scale of single NWs are observed and assigned to local growth conditions fluctuations. Finally, for the less luminescent nanowires, a departure from Poisson's statistics is observed suggesting the possible clustering of non independent point defects., (© 2023 IOP Publishing Ltd.)

Molecular beam epitaxy growth and optical properties of GaN quantum disks in AlN nanowires were investigated, with the purpose of controlling the emission wavelength of AlN nanowire-based light emitting diodes. Besides GaN quantum disks with a thickness ranging from 1 to 4 monolayers, a special attention was paid to incomplete GaN disks exhibiting lateral confinement. Their emission consists of sharp lines which extend down to 215 nm, in the vicinity of AlN band edge. The room temperature cathodoluminescence intensity of an ensemble of GaN quantum disks embedded in AlN nanowires is about 20% of the low temperature value, emphasizing the potential of ultrathin/incomplete GaN quantum disks for deep UV emission., (© 2023 IOP Publishing Ltd.)

The spontaneous growth of GaN nanowires (NWs) in absence of catalyst is controlled by the Ga flux impinging both directly on the top and on the side walls and diffusing to the top. The presence of diffusion barriers on the top surface and at the frontier between the top and the sidewalls, however, causes an inhomogeneous distribution of Ga adatoms at the NW top surface resulting in a GaN accumulation in its periphery. The increased nucleation rate in the periphery promotes the spontaneous formation of superlattices in InGaN and AlGaN NWs. In the case of AlN NWs, the presence of Mg can enhance the otherwise short Al diffusion length along the sidewalls inducing the formation of AlN nanotubes.

The mechanisms of plasma-assisted molecular beam epitaxial growth of GaN on muscovite mica were investigated. Using a battery of techniques, including scanning and transmission electron microscopy, atomic force microscopy, cathodoluminescence, Raman spectroscopy and x-ray diffraction, it was possible to establish that, in spite of the lattice symmetry mismatch, GaN grows in epitaxial relationship with mica, with the [11-20] GaN direction parallel to [010] direction of mica. GaN layers could be easily detached from the substrate via the delamination of the upper layers of the mica itself, discarding the hypothesis of a van der Waals growth mode. Mixture of wurtzite (hexagonal) and zinc blende (ZB) (cubic) crystallographic phases was found in the GaN layers with ratios highly dependent on the growth conditions. Interestingly, almost pure ZB GaN epitaxial layers could be obtained at high growth temperature, suggesting the existence of a specific GaN nucleation mechanism on mica and opening a new way to the growth of the thermodynamically less stable ZB GaN phase.

A promising approach of making high quality contacts on semiconductors is a silicidation (for silicon) or germanidation (for germanium) annealing process, where the metal enters the semiconductor and creates a low resistance intermetallic phase. In a nanowire, this process allows one to fabricate axial heterostructures with dimensions depending only on the control and understanding of the thermally induced solid-state reaction. In this work, we present the first observation of both germanium and copper diffusion in opposite directions during the solid-state reaction of Cu contacts on Ge nanowires using in situ Joule heating in a transmission electron microscope. The in situ observations allow us to follow the reaction in real time with nanometer spatial resolution. We follow the advancement of the reaction interface over time, which gives precious information on the kinetics of this reaction. We combine the kinetic study with ex situ characterization using model-based energy dispersive X-ray spectroscopy (EDX) indicating that both Ge and Cu diffuse at the surface of the created Cu 3 Ge segment and the reaction rate is limited by Ge surface diffusion at temperatures between 360 and 600 °C. During the reaction, germanide crystals typically protrude from the reacted NW part. However, their formation can be avoided using a shell around the initial Ge NW. H a direct Joule heating experiments show slower reaction speeds indicating that the reaction can be initiated at lower temperatures. Moreover, they allow combining electrical measurements and heating in a single contacting scheme, rendering the Cu-Ge NW system promising for applications where very abrupt contacts and a perfectly controlled size of the semiconducting region is required. Clearly, in situ TEM is a powerful technique to better understand the reaction kinetics and mechanism of metal-semiconductor phase formation.

To fully exploit the potential of semiconducting nanowires for devices, high quality electrical contacts are of paramount importance. This work presents a detailed in situ transmission electron microscopy (TEM) study of a very promising type of NW contact where aluminum metal enters the germanium semiconducting nanowire to form an extremely abrupt and clean axial metal-semiconductor interface. We study this solid-state reaction between the aluminum contact and germanium nanowire in situ in the TEM using two different local heating methods. Following the reaction interface of the intrusion of Al in the Ge nanowire shows that at temperatures between 250 and 330 °C the position of the interface as a function of time is well fitted by a square root function, indicating that the reaction rate is limited by a diffusion process. Combining both chemical analysis and electron diffraction we find that the Ge of the nanowire core is completely exchanged by the entering Al atoms that form a monocrystalline nanowire with the usual face-centered cubic structure of Al, where the nanowire dimensions are inherited from the initial Ge nanowire. Model-based chemical mapping by energy dispersive X-ray spectroscopy (EDX) characterization reveals the three-dimensional chemical cross-section of the transformed nanowire with an Al core, surrounded by a thin pure Ge (∼2 nm), Al 2 O 3 (∼3 nm), and Ge containing Al 2 O 3 (∼1 nm) layer, respectively. The presence of Ge containing shells around the Al core indicates that Ge diffuses back into the metal reservoir by surface diffusion, which was confirmed by the detection of Ge atoms in the Al metal line by EDX analysis. Fitting a diffusion equation to the kinetic data allows the extraction of the diffusion coefficient at two different temperatures, which shows a good agreement with diffusion coefficients from literature for self-diffusion of Al.

To provide a direct comparison, off-axis holography and differential phase contrast have been performed using the same microscope on the same specimens for the measurement of active dopants and piezoelectric fields. The sensitivity and spatial resolution of the two techniques have been assessed through the study of a simple silicon p-n junction observed at different bias voltages applied in-situ. For an evaluation of limitations and artefacts of the methods in more complicated systems a silicon pMOS device and an InGaN/GaN superlattice with 2.2-nm In 0.15 Ga 0.85 N quantum wells is investigated. We demonstrate the effects of dynamical scattering on the electric field measurements in the presence of local strain-induced sample tilts and its dependence on parameters like the convergence angle., (Copyright © 2019 Elsevier B.V. All rights reserved.)

In crystal growth, surfactants are additive molecules used in dilute amount or as dense, permeable layers to control surface morphologies. We investigate the properties of a strikingly different surfactant: a 2D and covalent layer with close atomic packing, graphene. Using in situ, real-time electron microscopy, scanning tunneling microscopy, kinetic Monte Carlo simulations, and continuum mechanics calculations, we reveal why metallic atomic layers can grow in a 2D manner below an impermeable graphene membrane. Upon metal growth, graphene dynamically opens nanochannels called wrinkles, facilitating mass transport while at the same time storing and releasing elastic energy via lattice distortions. Graphene thus behaves as a mechanically active, deformable surfactant. The wrinkle-driven mass transport of the metallic layer intercalated between graphene and the substrate is observed for two graphene-based systems, characterized by different physicochemical interactions, between graphene and the substrate and between the intercalated material and graphene. The deformable surfactant character of graphene that we unveil should then apply to a broad variety of species, opening new avenues for using graphene as a 2D surfactant forcing the growth of flat films, nanostructures, and unconventional crystalline phases.

Precession electron diffraction has been used to systematically measure the deformation in Si/SiGe blanket films and patterned finFET test structures grown on silicon-on-insulator type wafers. Deformation maps have been obtained with a spatial resolution of 2.0 nm and a precision of ±0.025%. The measured deformation by precession diffraction for the blanket films has been validated by comparison to energy dispersive x-ray spectrometry, X-Ray diffraction, and finite element simulations. We show that although the blanket films remain biaxially strained, the patterned fin structures are fully relaxed in the crystallographic planes that have been investigated. We demonstrate that precession diffraction is a viable deformation mapping technique that can be used to provide useful studies of state-of-the-art electronic devices.

It is demonstrated that growing InGaN nanowires in metal-rich conditions on top of GaN nanowires results in a widening of the InGaN section. It is shown that the widening is eased by stacking faults (SFs) formation, revealing facets favorable to In incorporation. It is furthermore put in evidence that partial dislocations terminating SFs efficiently contribute to elastic strain relaxation. Indium accumulation on top of the InGaN section is found to result in an axial growth rate decrease, which has been assigned to increased N-N recombination and subsequent effective nitrogen flux decrease, eventually leading to the formation of InGaN nano-umbrellas/nanoplatelets.

The structural and optical properties of axial GaN/InGaN/GaN nanowire heterostructures with high InN molar fractions grown by molecular beam epitaxy have been studied at the nanoscale by a combination of electron microscopy, extended x-ray absorption fine structure and nano-cathodoluminescence techniques. InN molar fractions up to 50% have been successfully incorporated without extended defects, as evidence of nanowire potentialities for practical device realisation in such a composition range. Taking advantage of the N-polarity of the self-nucleated GaN NWs grown by molecular beam epitaxy on Si(111), the N-polar InGaN stability temperature diagram has been experimentally determined and found to extend to a higher temperature than its metal-polar counterpart. Furthermore, annealing of GaN-capped InGaN NWs up to 800 °C has been found to result in a 20 times increase of photoluminescence intensity, which is assigned to point defect curing.

The atomic scale analysis of a ZnTe/CdSe superlattice grown by molecular beam epitaxy is reported using atom probe tomography and strain measurements from high-resolution scanning transmission electron microscopy images. CdTe interfaces were grown by atomic layer epitaxy to prevent the spontaneous formation of ZnSe bonds. Both interfaces between ZnTe and CdSe are composed of alloyed layers of ZnSe. Pure CdTe interfaces are not observed and Zn atoms are also visible in the CdSe layers. This information is critical to design superlattices with the expected optoelectronic properties., (© 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.)

The last few years have seen a great deal of progress in the development of transmission electron microscopy based techniques for strain mapping. New techniques have appeared such as dark field electron holography and nanobeam diffraction and better known ones such as geometrical phase analysis have been improved by using aberration corrected ultra-stable modern electron microscopes. In this paper we apply dark field electron holography, the geometrical phase analysis of high angle annular dark field scanning transmission electron microscopy images, nanobeam diffraction and precession diffraction, all performed at the state-of-the-art to five different types of semiconductor samples. These include a simple calibration structure comprising 10-nm-thick SiGe layers to benchmark the techniques. A SiGe recessed source and drain device has been examined in order to test their capabilities on 2D structures. Devices that have been strained using a nitride stressor have been examined to test the sensitivity of the different techniques when applied to systems containing low values of deformation. To test the techniques on modern semiconductors, an electrically tested device grown on a SOI wafer has been examined. Finally a GaN/AlN superlattice was tested in order to assess the different methods of measuring deformation on specimens that do not have a perfect crystalline structure. The different deformation mapping techniques have been compared to one another and the strengths and weaknesses of each are discussed., (Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Precession electron diffraction has been used to provide accurate deformation maps of a device structure showing that this technique can provide a spatial resolution of better than 2 nm and a precision of better than 0.02%. The deformation maps have been fitted to simulations that account for thin specimen relaxation. By combining the experimental deformation maps and simulations, we have been able to separate the effects of the stressor and recessed sources and drains and show that the Si3N4 stressor increases the in-plane deformation in the silicon channel from 0.92 to 1.52 ± 0.02%. In addition, the stress in the deposited Si3N4 film has been calculated from the simulations, which is an important parameter for device design.

Convergent beam electron diffraction (CBED), nano-beam electron diffraction (NBED or NBD), high resolution imaging (HRTEM and HRSTEM) and dark field electron holography (DFEH or HoloDark) are five TEM based techniques able to quantitatively measure strain at the nanometer scale. In order to demonstrate the advantages and disadvantages of each technique, two samples composed of epitaxial silicon-germanium layers embedded in a silicon matrix have been investigated. The five techniques are then compared in terms of strain precision and accuracy, spatial resolution, field of view, mapping abilities and ease of performance and analysis., (Copyright © 2013 Elsevier B.V. All rights reserved.)

In order to improve the performance of today's nanoscaled semiconductor devices, characterization techniques that can provide information about the position and activity of dopant atoms and the strain fields are essential. Here we demonstrate that by using a modern transmission electron microscope it is possible to apply multiple techniques to advanced materials systems in order to provide information about the structure, fields, and composition with nanometer-scale resolution. Off-axis electron holography has been used to map the active dopant potentials in state-of-the-art semiconductor devices with 1 nm resolution. These dopant maps have been compared to electron energy loss spectroscopy maps that show the positions of the dopant atoms. The strain fields in the devices have been measured by both dark field electron holography and nanobeam electron diffraction.

Dark field electron holography is a new TEM-based technique for measuring strain with nanometer scale resolution. Here we present the procedure to align a transmission electron microscope and obtain dark field holograms as well as the theoretical background necessary to reconstruct strain maps from holograms. A series of experimental parameters such as biprism voltage, sample thickness, exposure time, tilt angle and choice of diffracted beam are then investigated on a silicon-germanium layer epitaxially embedded in a silicon matrix in order to obtain optimal dark field holograms over a large field of view with good spatial resolution and strain sensitivity., (Copyright © 2010 Elsevier B.V. All rights reserved.)

Photoluminescence (PL) and time-resolved PL experiments as a function of the elaboration process are performed on Er-doped silicon-rich silicon oxide (SRO:Er) thin films grown under NH(3) atmosphere. These PL measurements of the Er(3+) emission at 1.54 microm under non-resonant pumping with the Er f-f transitions are obtained for different Er(3+) concentrations, ranging from 0.05 to 1.4 at.%, and various post-growth annealing temperatures of the layers. High resolution transmission electron microscopy (HRTEM) and energy-filtered TEM (EFTEM) analysis show a high density of Si nanostructures composed of amorphous and crystalline nanoclusters varying from 2.7 x 10(18) to 10(18) cm(-3) as a function of the post-growth annealing temperature. Measurements of PL lifetime and effective Er excitation cross section for all the samples under non-resonant optical excitation with the Er(3+) atomic energy levels show that the number of Er(3+) ions sensitized by the silicon-rich matrix decreases as the annealing temperature is increased from 500 to 1050 degrees C. The origin of this effect is attributed to the reduction of the density of sensitizers for Er ions in the SRO matrix when the annealing temperature increases. Finally, extended x-ray absorption fine-structure spectroscopy (EXAFS) shows a strong correlation between the number of emitters and the mean local order around the erbium ions.

A SiGe layer epitaxially grown on a silicon substrate is experimentally studied by convergent beam electron diffraction (CBED) experiments and used as a test sample to analyse the higher-order Laue zones (HOLZ) line splitting. The influence of surface strain relaxation on the broadening of HOLZ lines is confirmed. The quantitative fit of the observed HOLZ line profiles is successfully achieved using a formalism particularly well-adapted to the case of a z-dependent crystal potential (z being the zone axis). This formalism, based on a time-dependent perturbation theory approach, proves to be much more efficient than a classical Howie-Whelan approach, to reproduce the complex HOLZ lines profile in this heavily strained test sample.

The Geometrical phase analysis, which is a very efficient method to measure deformation from High resolution transmission electron microscopy images, is studied from a theoretical point of view. We point out that the basic property of this method is its ability to measure local reciprocal lattice parameters with a high level of accuracy. We attempt to provide some insights into (a) different formula used in the geometrical phase analysis such as the well-known relation between phase and displacement: Pg(r)=-2pi g.u(r), (b) the two different definitions of strain, each of which corresponding to a different lattice reference and (c) the meaning of a continuous displacement in a dot-like high resolution image. The case of one-dimensional analysis is also presented. Finally, we show that the method is able to give the position of the dot that is nearest to a given pixel in the image.