Nanostructures of Titanium oxide (TiO2) are being studied for many promising applications, e.g., solar photovoltaics, solar water splitting for H2 fuel generation etc., due to their excellent photo-catalytic properties. We have synthesized low-dimensional TiO2 nanoparticles by gas phase CW CO2 laser pyrolysis. The laser synthesis process has been optimized for the deposition of highly pure, nearly mono-dispersed TiO2 nanoparticles on silicon substrates. Hard x-ray standing wave-field (XSW) measurements in total reflection geometry were carried out on the BL-16 beamline of Indus-2 synchrotron radiation facility in combination with x-ray reflectivity and grazing incidence x-ray fluorescence measurements for the determination of surface morphology of the deposited TiO2 nanostructures. The average particle size of TiO2 nanostructure estimated using transmission electron microscopy (TEM) was found to closely agree with the XSW and grazing incidence x-ray diffraction (GIXRD) results.
The non-uniform standing spin-wave modes in thin magnetic films and nanostructures provide important information about surfaces and buried interfaces. Very often they are lacking in the recorded ferromagnetic resonance spectra for symmetry reasons. In this work we experimentally demonstrate that by direct injection of microwave currents into an array of Permalloy nanostripes using a microscopic microwave coaxial to coplanar adaptor one can efficiently excite non-uniform standing spin wave modes with odd symmetry. The proposed method is quick and allows easy spatial mapping of magnetic properti…
Here, we demonstrate an approach that provides a precise control of the dimension of InAs from one-dimensional nanowires to wafer-scale free-standing two-dimensional nanosheets, which have a high degree of crystallinity and outstanding electrical and optical properties, using molecular-beam epitaxy by controlling catalyst alloy segregation. In our approach, two-dimensional InAs nanosheets can be obtained directly from one-dimensional InAs nanowires by silver-indium alloy segregation, which is much easier than all previously reported method, such as traditional buffering technique and select ar…
Fine structure analysis of core electron excitation spectra is a cornerstone characterization technique across the physical sciences. Spectra are most commonly measured with synchrotron radiation and X-ray spot sizes on the μm to mm scale. Alternatively, electron energy loss spectroscopy (EELS) in the (scanning) transmission electron microscope ((S)TEM) offers over a 1000 fold increase in spatial resolution, a transformative advantage for studies of nanostructured materials. However, EELS applicability is generally limited to excitations below ~2 keV, i.e., mostly to elements in just the first…
In the present work we investigate the photocatalytic hydrogen production (water splitting) activity of different Pt loaded TiO2 nanotube layers. Therefore, we fabricate free standing membranes and fix them in four different configurations: top up (with initiation layer grass or without) and bottom up (bottom closed or open), then decorate the tubes with various amounts of Pt and measure the open-circuit photocatalytic H2 production rate. We find a strong influence of the configuration with the open top morphology showing the highest photocatalytic hydrogen production efficiency, these nanotub…
We demonstrate spatial mapping of the local and nano-scale structure of thin film objects using spatially resolved PDF analysis of synchrotron x-ray diffraction data. This is demonstrated in a lab-on-chip combinatorial array of sample spots containing catalytically interesting nanoparticles deposited from liquid precursors using an ink-jet liquid handling system. We present a software implementation of the whole protocol including an approach for automated data acquisition and analyis using the atomic pair distribution function (PDF) method. The protocol software can handle semi-automated data…
The ability to non-destructively measure the structural properties of devices, either in situ or operando, are now possible using an intense X-ray synchrotron source combined with specialized equipment. This tool attracted researchers, in particular metallurgists, to attempt more complex and ambitious experiments aimed at answering unresolved questions in formation mechanisms, phase transitions, and magnetism complex alloys for industrial applications. In this paper, we introduce the diffraction diffusion anomale multi-longueur d'onde (D2AM) beamline, a French collaborating research group (CRG…
We present a unified elucidation for the role temporal coherence properties of x-rays in surface x-ray standing wave analysis, under total external reflection condition. Analytical formulas have been derived that provide a direct relation between the intensity distribution of x-ray standing wave (XSW) pattern and complex degree of coherence of the incoming x-rays. The novelty of the proposed method has been demonstrated experimentally together with the theoretical results for a real application by analyzing the distribution of metal nanoparticles on a Si mirror surface. Our results demonstrate…
Micro-focused X-ray beams produced by third generation synchrotron sources offer new perspective of studying strains and processes at nanoscale. Atomic force microscope setup combined with a micro-focused synchrotron beam allows precise positioning and nanomanipulation of nanostructures under illumination. In this paper, we report on integration of a portable commercial atomic force microscope setup into a hard X-ray synchrotron beamline. Details of design, sample alignment procedure and performance of the setup are presented.
The formation of a 3D network composed of free standing and interconnected Pt nanowires is achieved by a two-step method, consisting of conformal deposition of Pt by atomic layer deposition (ALD) on a forest of carbon nanotubes and subsequent removal of the carbonaceous template. Detailed characterization of this novel 3D nanostructure was carried out by transmission electron microscopy (TEM) and electrochemical impedance spectroscopy (EIS). These characterizations showed that this pure 3D nanostructure of platinum is self-supported and offers an enhancement of the electrochemically active sur…
Free-standing nanoribbons of InAs quantum membranes (QMs) transferred onto a (Si/Mo) multilayer mirror substrate are characterized by hard x-ray photoemission spectroscopy (HXPS), and by standing-wave HXPS (SW-HXPS). Information on the chemical composition and on the chemical states of the elements within the nanoribbons was obtained by HXPS and on the quantitative depth profiles by SW-HXPS. By comparing the experimental SW-HXPS rocking curves to x-ray optical calculations, the chemical depth profile of the InAs(QM) and its interfaces were quantitatively derived with angstrom precision. We det…
Surface diffusion has an impact on the lateral resolution of nanostructures in bottom-up atom nanofabrication. In this paper we study the effects of the gallium atoms self-assembled on silicon surfaces (100) patterned with trenches at different slopes. These particular substrate morphologies have been made to enable an effective deposition rate variation along the surface. In this way we experimentally mimic the effect of the atomic flux modulation created by standing wave during an atom nanofabrication experiment. Even if we observe self organization of gallium atoms on the surface, we conclu…
Investigation of Fe-Ag and Ag-Fe Interfaces in Ag-57Fe-Ag trilayer Using Nuclear Resonance Scattering under X-ray Standing Wave Conditions
UGC-DAE Consortium for Scientific Research（UGC-DAE 科学研究联合体）；Deutsches Elektronen-Synchrotron DESY（德国电子同步加速器中心）；Department of Physics, University of Petroleum and Energy Studies（石油与能源大学物理系）；Elettra Sincrotrone Trieste（的里雅斯特电子同步加速器）；Raja Ramanna Centre for Advanced Technology（拉贾·拉曼纳先进技术中心）
Vanadium tetracyanoethylene (V[TCNE]$_\text{x}$) is an organic-based ferrimagnet that exhibits robust magnetic ordering (T$_\text{C}$ of over 600 K), high quality-factor (high-Q) microwave resonance (Q up to 3,500), and compatibility with a wide variety of substrates and encapsulation technologies. Here, we substantially expand the potential scope and impact of this emerging material by demonstrating the ability to produce engineered nanostructures with tailored magnetic anisotropy that serve as a platform for the exploration of cavity magnonics, revealing strongly coupled quantum confined sta…
Dynamic evolution of internal stress, grain growth, and crystallographic texture in arc-evaporated AlTiN thin films using in-situ synchrotron x-ray diffraction
Vitrimers - a class of polymer networks which are covalently crosslinked and insoluble like thermosets, but flow when heated like thermoplastics - contain dynamic links and/or crosslinks that undergo an associative exchange reaction. These dynamic crosslinks enable vitrimers to have interesting mechanical/rheological behavior, self-healing, adhesive, and shape memory properties. We demonstrate that vitrimers can self-assemble into complex meso- and nanostructures when crosslinks and backbone monomers strongly interact. Vitrimers featuring polyethylene (PE) as the backbone and dioxaborolane mal…
X-ray standing-wave photoemission experiments involving multilayered samples are emerging as unique probes of the buried interfaces that are ubiquitous in current device and materials research. Such data require for their analysis a structure optimization process comparing experiment to theory that is not straightforward. In this work, we present a new computer program for optimizing the analysis of standing-wave data, called SWOPT, that automates this trial-and-error optimization process. The program includes an algorithm that has been developed for computationally expensive problems: so-call…
Topological insulator surface properties are strongly correlated to structural properties, requiring high-resolution techniques capable of probing both surface and bulk structures at once. In this work, high flux of synchrotron source, recursive equations for fast X-ray dynamical diffraction simulation, and genetic algorithm for data fitting are combined to reveal the detailed structure of bismuth telluride epitaxic films with thickness ranging from 8 to 168 nm. It includes stacking sequences, thickness and composition of layers in model structures, interface coherence, surface termination and…
We demonstrate a technique of broadband spin torque ferromagnetic resonance (ST-FMR) with magnetic field modulation for measurements of spin wave properties in magnetic nanostructures. This technique gives great improvement in sensitivity over the conventional ST-FMR measurements, and application of this technique to nanoscale magnetic tunnel junctions (MTJs) reveals a rich spectrum of standing spin wave eigenmodes. Comparison of the ST-FMR measurements with micromagnetic simulations of the spin wave spectrum allows us to explain the character of low-frequency magnetic excitations in nanoscale…
Mapping reaction mechanism during overcharge of a LiNiO2/Graphite-silicon lithium-ion battery: a correlative operando approach by simultaneous gas analysis and synchrotron scattering techniques
Magnetic anisotropy is a key parameter of magnetic materials as it decides the response in the presence of an external magnetic field. The artificial tailoring of magnetic anisotropy by manipulating surface and interface morphology is attracting widespread interest for its application in spintronic and magnetic memory devices. In this perspective, the primary focus of this thesis has been inducing and tailoring magnetic anisotropy in thin film-based systems via the engineering of structure and surface/interfacial morphology. For this purpose, instead of multistep, expensive lithographic techni…
The increasing demand for ultrahigh data storage densities requires development of 3D magnetic nanostructures. In this regard, focused electron beam induced deposition (FEBID) is a technique of choice for direct-writing of various complex nano-architectures. However, intrinsic properties of nanomagnets are often poorly known and can hardly be assessed by local optical probe techniques. Here, we demonstrate spatially resolved spin-wave spectroscopy of individual circular magnetic elements with radii down to 100 nm. The key component of the setup is a microwave antenna whose microsized central p…
