Abstract: We compare the magnetic properties of pure and oxidized Co nanoparticles embedded in an amorphous Al2O3 matrix. Nanoparticles with diameters of 2 or 3 nm were prepared by alternate pulsed laser deposition in high vacuum conditions, and some of them were exposed to O-2 after production and before being embedded. The nanoparticles are organized in layers, the effective edge-to-edge in-depth separation being 5 or 10 nm. The lower saturation magnetizations per Co atom for the samples containing oxidized nanoparticles provide evidence for the formation of antiferromagnetic CoO shells in the nanoparticles. None of the samples with Co/CoO nanoparticles show exchange bias, while vertical hysteresis loop shifts and enhanced coercivities (as compared to samples with pure Co nanoparticles) are observed. This constitutes evidence for the nanoparticles size being in all cases smaller than the critical size for exchange bias. The difference in coercivity versus temperature dependences for the samples with pure and oxidized Co nanoparticles shows that the exchange anisotropy in Co/CoO nanoparticles appears at temperatures lower than 50 K. (c) 2007 American Institute of Physics.

Abstract: Nanostripes are observed in melt-textured and single-crystalline samples of the ternary light rare earth (LRE)-compound (Nd0.33Eu0.33Gd0.33)Ba2Cu3Ox (NEG) by means of atomic force microscopy, scanning tunnelling microscopy at ambient conditions, combined with transmission electron microscopy and electron backscatter diffraction. This enables the observation of several important features: The nanostripes are formed by chains of nanoclusters, representing the LRE/Ba substitution. The dimensions of the nanostripes are similar for both types of NEG samples. The periodicity of the nanostripes is found to range between 40 and 60 nm; the shape of the nanoclusters is elliptic with a major axis length between 300 and 500 nm and a minor axis length of about 30150 nm. The stripes are filling effectively the space in between the twin boundaries. Concerning the flux pinning, the nanoclusters are the important pinning sites, not the nanostripes themselves.

Abstract: A hot dip aluminizing process to simulate the continuous galvanizing line (CGL) was carried out in three successive steps by a hot dip simulator: the pre-treatment for removing scales on the 200 x 250 mm(2) and 1mm in thickness cold rolled steel sheet, the dipping in 660 degrees C Al-Si melt for 3s and the cooling. In a pre-treatment, the steel specimen was partly coated by Au to confirm the mechanism of intermetallic compound (IMC) formation. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) analyses were followed to observe the cross-section and the distribution of the elements. The specimen was analyzed in the boundary of the dipped-undipped part to see the formation mechanism of the aluminized steel. An intermetallic compound (IMC) is rapidly developed and grown in the steel-liquid interface. It has been usually reported that the IMC was formed by the dissolution of iron in the steel substrate toward the melt and the diffusion of aluminum in an opposite direction. The specimen is covered with aluminum-10 wt.% silicon, forms the IMC in the part that was not Au coated. However, IMC is not formed in the Au-coated part. The interface of the dipped-undipped is also analyzed by EDX. At the interface of the steel-IMC, it is clearly shown that the IMC is only formed in the dipped part and exists in the steel substrate as well, and contributes by iron, aluminum and silicon. The result clearly shows that only aluminum diffuses into the steel substrate without the dissolution of iron and forms the IMC between the steel substrate and the melt. Au coating and the short dipping time prevent the iron from dissolving into the aluminum melt. By TEM combined with focused ion beam (FIB) sample preparation, the IMC is confirmed as Fe2SiAl8, a hexagonal structure with space group P6(3)/mmc.

Abstract: Occupancy of different structural positions in a crystal lattice often seems to play a key role in material prop-erties. Several experimental techniques have been developed to uncover this issue, all of them being mostly bulk sensitive. However, many materials including topological insulators (TIs), which are among the most intriguing modern materials, are intended to be used in devices as thin films, for which the sublattice occupancy may differ from the bulk. One of the possible approaches to occupancy analysis is X-ray Photoelectron Diffraction (XPD), a structural method in surface science with chemical sensitivity. We applied this method in a case study of Sb2(Te1-xSex)3 mixed crystals, which belong to prototypical TIs. We used high-angle annular dark field (HAADF) scanning transmission electron microscopy (STEM) as a reference method to verify our analysis. We revealed that the XPD data for vacuum cleaved bulk crystals are in excellent agreement with the reference ones. Also, we demonstrate that the anion occupancy near a naturally formed surface can be rather different from that of the bulk. The present results are relevant for a wide range of compositions where the system remains a topological phase, as we ultimately show by probing the transiently occupied topological surface state above the Fermi level by ultrafast photoemission.

Abstract: The crystalline and defect structure of epitaxial hexagonal RExMnyO3 (RE = Er, Dy) films with varying cationic composition was investigated by X-ray diffraction and transmission electron microscopy. The films are composed of a strained layer at the interface with the substrate and of a relaxed layer on top of it. The critical thickness is of 10 to 25 nm. For Mn-rich films (or RE deficient), an off-stoichiometric composition maintaining the hexagonal LuMnO3-type structure is stabilized over a large range of the RE/Mn ratio (0.72−1.00), with no Mn-rich secondary phases observed. A linear dependence of the out-of-plane lattice parameter with RE/Mn is observed in this range. Out-of-phase boundary (OPB) extended defects are observed in all films and exhibit a local change in stoichiometry. Such a large solubility limit in the RE deficient region points toward the formation of vacancies on the RE site (RExMnO3−δ, with 0.72 ≤ x < 1), a phenomenon that is encountered in perovskite manganites such as LaxMnO3−δ (x < 1) and that may strongly impact the physical properties of hexagonal manganites.

Abstract: Ptychography provides high dose efficiency images that can reveal light elements next to heavy atoms. However, despite ptychography having an otherwise single signed contrast transfer function, contrast reversals can occur when the projected potential becomes strong for both direct and iterative inversion ptychography methods. It has recently been shown that these reversals can often be counteracted in direct ptychography methods by adapting the focus. Here we provide an explanation of why the best contrast is often found with the probe focused to the middle of the sample. The phase contribution due to defocus at each sample slice above and below the central plane in this configuration effectively cancels out, which can prevent contrast reversals when dynamical scattering effects are not overly strong. In addition we show that the convergence angle can be an important consideration for removal of contrast reversals in relatively thin samples.

Abstract: The electrodeposition of nickel nanostructures on glassy carbon was investigated in 1:2 choline chloride urea deep eutectic solvent (DES) containing different amounts of water. By combining electrochemical techniques, with ex situ field emission scanning electron microscopy, high-angle annular dark field scanning transmission electron microscopy, and energy-dispersive X-ray spectroscopy, the effect of water content on the electrochemical processes occurring during nickel deposition was better understood. At highly negative potentials and depending on water content, Ni growth is halted due to water splitting and formation of a mixed layer of Ni/NiOx(OH)(2(1-x)(ads)). Moreover, under certain conditions, the DES components can also be (electro)chemically reduced at the electrode surface, blocking further three-dimensional growth of the Ni NPs. Hence, a two-dimensional crystalline Ni-containing network can be formed in the interparticle region.

Abstract: Intragranular amorphization shear lamellae are found in deformed olivine aggregates. The detailed trans-mission electron microscopy analysis of intragranular lamella arrested in the core of a grain provides novel information on the amorphization mechanism. The deformation field is complex and heteroge-neous, corresponding to a shear crack type instability involving mode I, II and III loading components. The formation and propagation of the amorphous lamella is accompanied by the formation of crystal defects ahead of the tip. These defects are geometrically necessary [001] dislocations, characteristics of high-stress deformation in olivine, and rotational nanodomains which are tentatively interpreted as disclinations. We show that these defects play an important role in dictating the path followed by the amorphous lamella. Stress-induced amorphization in olivine would thus result from a direct crystal-to -amorphous transformation associated with a shear instability and not from a mechanical destabilization due to the accumulation of high number of defects from an intense preliminary deformation. The pref-erential alignment of some lamellae along (010) is a proof of the lower ultimate mechanical strength of these planes.(c) 2022 The Authors. Published by Elsevier Ltd on behalf of Acta Materialia Inc. This is an open access article under the CC BY license ( http://creativecommons.org/licenses/by/4.0/ )

Abstract: The ordering for 11/20 alloys has been studied by high-resolution electron microscopy (HREM). The distribution of the intensity maxima in the HREM image have been statistically examined, which provides a profound basis for the image interpretation. Processing of the HREM images allows ''dark-field'' images to be obtained, exhibiting a two-dimensional distribution of those columns which contain the most information in order to interpret the short-range order correlations. Pair correlations and higher cluster correlations between projected columns can be visualised, providing unique information about the ordering as retrieved from an experimental result without any other assumption. The method has been applied to Au4Cr and to Au4Mn to interpret the quenched short-range order state and the transition to long-range order.

Abstract: Electrochemical oscillations accompanying the formation of anodic silica have been shown in the past to be correlated with rather abrupt changes in the mechanical stress state of the silica film, commonly associated with some kind of fracture or porosification of the oxide. To advance the understanding on the origin of such oscillations in fluoride-free electrolytes, we have revisited a seminal experiment reported by Lehmann almost two decades ago. We thereby demonstrate that the oscillations are not stress-induced, and do not originate from a morphological transformation of the oxide in the course of anodisation. Alternatively, the mechanical features accompanying the oscillations can be explained by a partial relaxation of the field-induced electrostrictive stress. Furthermore, our observations suggest that the oscillation mechanism more likely results from a periodic depolarisation of the anodic silica.