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The electrochemical growth of Au nanowires in a template of nano-porous anodic aluminum oxide was investigated in situ by means of grazing-incidence transmission small- and wide-angle x-ray scattering (GTSAXS and GTWAXS), x-ray fluorescence (XRF) and 2-dimensional surface optical reflectance (2D-SOR). The XRF and the overall intensity of the GTWAXS patterns as a function of time were used to monitor the progress of the electrodeposition. Furthermore, we extracted powder diffraction patterns in the direction of growth and in the direction of confinement to follow the evolution of the direction-dependent strain. Quite rapidly after the beginning of the electrodeposition, the strain became tensile in the vertical direction and compressive in the horizontal direction, which showed that the lattice deformation of the nanostructures can be artificially varied by an appropriate choice of the deposition time. By alternating sequences of electrodeposition to sequences of rest, we observed fluctuations of the lattice parameter in the direction of growth, attributed to stress caused by electromigration.. Furthermore, the porous domain size calculated from the GTSAXS patterns was used to monitor how homogeneously the pores were filled., Short communication manuscript. Four figures

Journal of alloys and compounds 895, 162657 (2022). doi:10.1016/j.jallcom.2021.162657, The surface chemistry and thickness of the native oxide, hydroxide, and modified sub-surface layer of three Ni superalloys (alloy 59, 625, and 718) were determined by synchrotron X-ray Photoelectron Spectroscopy (XPS) and X-ray Reflectivity (XRR). Taking advantage of the synchrotron radiation techniques, a procedure for normalizing the photoelectron intensity was employed, which allowed for accurate quantitative analysis revealing a total oxide thickness for all samples of 12���13 ��, a hydroxide layer of 2���3 ��, and a thickness of the sub-surface alloy layer of 20���35 ��. The thickness results were compared to structural atomic models suggesting that the oxide thickness corresponds to four planes of metal cations in the oxide matrix. The XPS data revealed that the native oxides were enriched in Cr$^{3+}$, Mo$^{(4,5,6)+}$, and Nb$^{5+}$, while no Ni oxide was detected. The hydroxide layer mainly contained Ni$^{2+}$ and Cr$^{3+}$ hydroxide. The sub-surface layer was enriched in Ni and depleted in Cr, Fe, Mo, and Nb. The obtained oxide composition can be explained using thermodynamics, and it was found that the oxide composition correlates with the enthalpy of oxide formation for the metal elements in the alloys. Finally, the advantages of synchrotron radiation for composition and thickness determination are discussed., Published by Elsevier, Lausanne

We have developed a microscope with a spatial resolution of 5 μm, which can be used to image the two-dimensional surface optical reflectance (2D-SOR) of polycrystalline samples in operando conditions. Within the field of surface science, operando tools that give information about the surface structure or chemistry of a sample under realistic experimental conditions have proven to be very valuable to understand the intrinsic reaction mechanisms in thermal catalysis, electrocatalysis, and corrosion science. To study heterogeneous surfaces in situ, the experimental technique must both have spatial resolution and be able to probe through gas or electrolyte. Traditional electron-based surface science techniques are difficult to use under high gas pressure conditions or in an electrolyte due to the short mean free path of electrons. Since it uses visible light, SOR can easily be used under high gas pressure conditions and in the presence of an electrolyte. In this work, we use SOR in combination with a light microscope to gain information about the surface under realistic experimental conditions. We demonstrate this by studying the different grains of three polycrystalline samples: Pd during CO oxidation, Au in electrocatalysis, and duplex stainless steel in corrosion. Optical light-based techniques such as SOR could prove to be a good alternative or addition to more complicated techniques in improving our understanding of complex polycrystalline surfaces with operando measurements.

A method for the electrochemical synthesis of palladium nanowires, using porous alumina templates with diameters of 25 nm and 40 nm, is presented. Through an electrochemical barrier layer thinning step, pulsed electrodeposition can take place directly into the anodized aluminum; without need for extra removal, pore opening, and metal contact coating steps. A digital oscilloscope is used to record and integrate the current, allowing the efficiency of the electrodeposition to be calculated. We discuss how using a large “off period” allows for the replenishment of the depleted diffusion layer. The nanowires are characterized by using a focused ion beam (FIB) to create cross-sections which can be accessed with a scanning electron microscope (SEM). With grazing-incidence X-ray diffraction (GI-XRD) we find that the nanowires have a slight compressive strain in the direction that they are confined by the pores (0.58% and 0.51% for the 25 nm and 40 nm pores respectively). Knowing the strain state of the nanowires inside the template is of importance for the use of templated nanowires in devices. Further characterization is made using high-resolution transmission electron microscopy (HR-TEM) and energy dispersive X-ray spectroscopy (EDS), after removal from the alumina templates.

Journal of physics / D 54(23), 235301 (2021). doi:10.1088/1361-6463/abeb3d, Templated electrochemical growth in nanoporous alumina can be used to fabricate nanowires with applications in magnetic storage devices, hydrogen sensors, and electrocatalysis. It is known that nanowires, grown in such templates, are strained. The strain in nanoscale materials can influence their performance in applications such as catalysts and electronic devices. However, it is not well established how the nanoporous template affects the lattice strain in the nanowires and how this develops during the growth process due to the lack of non-destructive in situ studies with spatial resolution. We have measured the strain and grain size of palladium nanowires in nanoporous templates during the growth process. For this, we performed in situ scanning x-ray diffraction with a submicron focused x-ray beam. We found a tensile strain in the nanowires and that it is more pronounced along the growth direction than in the confined direction of the templates. The tensile strain measured in situ is higher than previous ex situ reports, possibly due to hydrogen absorption during the growth. With the spatial information made possible with the focused synchrotron x-ray beam, we could observe local variations in the strain as a function of height. A region of local strain variation is found near the bottom of the nanowires where growth is initiated in branches at the pore bottoms. Knowledge of how nanoporous templates influences the strain of the nanowires may allow for atomic scale tailoring of the catalytic activity of such nanowires or minimizing strain to optimize electronic device performance., Published by IOP Publ., Bristol

The design and the experimental results of some prototypes of SiC X-ray detectors are presented. The devices have been manufactured on a 2’’ 4H-SiC wafer with 115 m thick undoped high purity epitaxial layer, which constitutes the detection’s active volume. Pad and pixel detectors based on Ni-Schottky junctions have been tested. The residual doping of the epi-layer was found to be extremely low, 3.7 x 1013 cm-3, allowing to achieve the highest detection efficiency and the lower specific capacitance of the detectors. At +22°C and in operating bias condition, the reverse current densities of the detector’s Schottky junctions have been measured to be between J=0.3 pA/cm2 and J=4 pA/cm2; these values are more than two orders of magnitude lower than those of state of the art silicon detectors. With such low leakage currents, the equivalent electronic noise of SiC pixel detectors is as low as 0.5 electrons r.m.s at room temperature, which represents a new state of the art in the scenario of semiconductor radiation detectors.

Gallium nitride (GaN) and related alloys (Al(x)Ga(1-x)N) are promising semiconductors For high-frequency and high-power devices applications. In particular, the growth of AlGaN/GaN heterostructures oil SiC Substrates, due to the high thermal conductivity of SiC, can lead to significant improvement in the device performances. Ail important issue in the fabrication of AlGaN/GaN devices is the influence of the required thermal budget (700-900 degrees C) on the properties of Ohmic contacts and device isolation. In this work, the influence of thermal annealing on the fabrication of AlGaN/GaN devices was studied. Ti/Al/Ni/Au multilayers led to ail Ohmic behavior with a specific resistance rho(c) in the 10(-5) Omega cm(2) range upon annealing between 750 degrees C and 850 degrees C. The electrical behavior of Ohmic contacts was correlated with the evolution of the formed phases and with the temperature behavior of rho(c). The stability of the inter-device isolation obtained by nitrogen-implantation during annealing at these temperatures was also monitored.

Cubic (111)-oriented silicon carbide (3C-SiC) heteroepitaxy on (110) silicon substrate was performed by low pressure chemical vapor deposition. A comparison with the previous work by Nishiguchi [Appl. Phy. Lett. 84, 3082 (2004)] shows that the relationship (110) Si parallel to(111) 3C-SiC could be misleading. Based on x-ray diffraction pole figures and numerical simulations, we prove that this relationship is due to the formation of second order twins during the initial stages of growth. This analysis also reveals that the crystal starts to grow with a misalignment of 3.5 degrees along the < 002 > Si direction to adapt the mismatch of lattice parameters. (c) 2008 American Institute of Physics.

The growth rate of 4H-SiC epitaxial layer has been increased by a factor 19 (up to 112 μm/h) with respect to the standard process with the introduction of HCl in the deposition chamber. The epitaxial layers grown with the addition of HCl have been characterized by electrical, optical and structural characterization methods. The effects of different deposition parameters on the epitaxial growth process have been described in detail. This process can be very promising for high power devices with a breakdown voltage of 10 kV.