Over the last two decades, three-dimensional (3D) imaging by transmission electron microscopy or “electron tomography” has evolved into a powerful tool to investigate a variety of nanomaterials in different fields, such as life sciences, chemistry, solid-state physics, and materials science. Most of these results were obtained with nanometer-scale resolution, but different approaches have recently pushed the resolution to the atomic level. Such information is a prerequisite to understand the specific relationship between the atomic structure and the physicochemical properties of (nano)materials. We provide an overview of the latest progress in the field of atomic-resolution electron tomography. Different imaging and reconstruction approaches are presented, and state-of-the-art results are discussed. This article demonstrates the power and importance of electron tomography with atomic-scale resolution.

Conventional glass-ionomer cements (GICs) are popular restorative materials, but their use is limited by their relatively low mechanical strength. This paper reports an attempt to improve these materials by incorporation of 10 wt% of three different types of nanoparticles, aluminum oxide, zirconium oxide, and titanium dioxide, into two commercial GICs (ChemFil® Rock and EQUIA™ Fil). The results indicate that the nanoparticles readily dispersed into the cement matrix by hand mixing and reduced the porosity of set cements by filling the empty spaces between the glass particles. Both cements showed no significant difference in compressive strength with added alumina, and ChemFil® Rock also showed no significant difference with zirconia. By contrast, ChemFil® Rock showed significantly higher compressive strength with added titania, and EQUIA™ Fil showed significantly higher compressive strength with both zirconia and titania. Fewer air voids were observed in all nanoparticle-containing cements and this, in turn, reduced the development of cracks within the matrix of the cements. These changes in microstructure provide a likely reason for the observed increases in compressive strength, and overall the addition of nanoparticles appears to be a promising strategy for improving the physical properties of GICs.

Focused ion beam (FIB) induced damage in nanocrystalline Al thin films has been characterized using advanced transmission electron microscopy techniques. Electron tomography was used to analyze the three-dimensional distribution of point defect clusters induced by FIB milling, as well as their interaction with preexisting dislocations generated by internal stresses in the Al films. The atomic structure of interstitial Frank loops induced by irradiation, as well as the core structure of Frank dislocations, has been resolved with aberration-corrected high-resolution annular dark-field scanning TEM. The combination of both techniques constitutes a powerful tool for the study of the intrinsic structural properties of point defect clusters as well as the interaction of these defects with preexisting or deformation dislocations in irradiated bulk or nanostructured materials.

The three-dimensional (3D) distribution of carbon nanotubes (CNTs) grown inside semiconductor contact holes is studied by electron tomography. The use of a specialized tomography holder results in an angular tilt range of ±90°, which means that the so-called “missing wedge” is absent. The transmission electron microscopy (TEM) sample for this purpose consists of a micropillar that is prepared by a dedicated procedure using the focused ion beam (FIB) but keeping the CNTs intact. The 3D results are combined with energy dispersive X-ray spectroscopy (EDS) to study the relation between the CNTs and the catalyst particles used during their growth. The reconstruction, based on the full range of tilt angles, is compared with a reconstruction where a missing wedge is present. This clearly illustates that the missing wedge will lead to an unreliable interpretation and will limit quantitative studies.

Nanocrystalline diamond films have generated much interested due to their diamond-like properties and low surface roughness. Several techniques have been used to obtain a high re-nucleation rate, such as hydrogen poor or high methane concentration plasmas. In this work, the properties of nano-diamond films grown on silicon substrates using a continuous DC bias voltage during the complete duration of growth are studied. Subsequently, the layers were characterised by several morphological, structural and optical techniques. Besides a thorough investigation of the surface structure, using SEM and AFM, special attention was paid to the bulk structure of the films. The application of FTIR, XRD, multi wavelength Raman spectroscopy, TEM and EELS yielded a detailed insight in important properties such as the amount of crystallinity, the hydrogen content and grain size. Although these films are smooth, they are under a considerable compressive stress. FTIR spectroscopy points to a high hydrogen content in the films, while Raman and EELS indicate a high concentration of sp2 carbon. TEM and EELS show that these films consist of diamond nano-grains mixed with an amorphous sp2 bonded carbon, these results are consistent with the XRD and UV Raman spectroscopy data.

Application of SiC substrates instead of the most commonly used sapphire for the heteroepitaxial growth of III-Nitrides offers advantages as better lattice matching, higher thermal conductivity, and electrical conductivity. This namely offers interesting perspectives for the development of vertical III-Nitride devices for switching purposes. For example, an AlGaN/SiC heterojunction could improve the performance of SiC bipolar transistors. In this work, n-type GaN layers have been grown by MOVPE on p-type 4H-SiC substrates using Si doped Al0.08Ga0.92N or Al0.3Ga0.7N nucleation layers. They have been characterized with temperature dependent current-voltage (I-V-T), capacitance-voltage (C-V) techniques and transmission electron microscopy (TEM).

The performance of AlGaN/GaN High Electron Mobility (HEMT) transistors is directly related to the electrical characteristics of the two-dimensional electron gas formed at the interface thanks to the piezoelectric field. Modification of the Al content or thickness of the AlGaN layer can within a certain limit modify the carrier density and mobility in the 2DEG. However, further reduction of the sheet resistance requires strain engineering of the heterostructure. An effective way to reduce the sheet resistance, as well as to lower the threading dislocation (TD) density, is to perform strain engineering through the use of low temperature AlN interlayers inserted in the GaN buffer layer. From correlation of AFM, TEM and HRXRD mapping of the HEMT layers, the strain modification, as well as the mechanism reducing the TD density, can be explained by the highly defected nature of the AlN interlayer grown at low temperature, as well as its very small thickness. The LT AlN acts as a second nucleation layer for the GaN grown on top. Contrarily, when the AlN interlayer is grown at 1050°C, its high crystalline quality and the possibility to grow pseudomorphic and abrupt interfaces, allows its use at the AlGaN/GaN interface. Optimal combination of the AlGaN and AlN layer thickness leads to record values of the mobility at room temperature of 2050 cm2/Vs, for heterostructures grown on sapphire, which is approaching state-of-the-art for HEMT grown on SiC.

We have determined the structure of the paraelectric phase of BaAl2O4, which is a stuffed tridymite, by different TEM techniques and we will describe the phase transition between the ferroelectric room temperature phase and the paraelectric high temperature phase. We have also obtained HREM images of the higly radiation sensitive acristobalite phase of (Si0,9 Ge0,1)O2 and analysed the extended defects in this material.

The stuffed tridymite BaAl2O4 is ferroelectric at room temperature and undergoes a paraelectric-ferroelectric (PEFE) phase transition. The transition is reversible, takes place over a wide temperature range (400K-670K) and has a dynamical character. BaAl2O4 is easily obtained by solid state reaction of BaCO3, and A12O4,. The stoichiometric amounts of the initial reagents were mixed, grinded in an agate mortar under acetone and pressed into a pellet. The pellet was annealed in alumina crucibles at 1000 °C and 1300 °C for 40 h in air and furnace cooled.