KMC-2: an X-ray beamline with dedicated diffraction and XAS endstations at BESSY II

The KMC-2 beamline is dedicated to provide X-ray radiation with high energy stability and resolution. The experimental setup is optimized towards offering a wide range of methods and sample environments. Two permanent endstations can be used in alternation. DIFFRACTION is a flexible multi-purpose diffractometer, based on a Huber six circle diffractometer in psi geometry. XANES provides the possibility for EXAFS, XANES and X-ray fluorescence measurements at-air

The use of anomalous x ray diffraction as a tool for the analysis of compound semiconductors

We provide a review about the current and previous use of anomalous diffraction of x rays in the analysis of compound semiconductors. Among the large number of available techniques, those that have been used in successful experiments on this class of compounds are identified. An exhaustive overview of the compound semiconductor systems that have been studied successfully is provided and the kind of results derived from experiments is discusse

Uncovering cation disorder in ternary Zn1+xGe1−x(N1−xOx)2 and its effect on the optoelectronic properties

Ternary nitride materials, such as ZnGeN2, have been considered as hopeful optoelectronic materials with an emphasis on sustainability. Their nature as ternary materials has been ground to speculation of cation order/disorder as a mechanism to tune their bandgap. We herein studied the model system Zn1+xGe1−x(N1−xOx)2 including oxygen – which is often a contaminant in nitride materials – using a combination of X-ray and neutron diffraction combined with elemental analyses to provide direct experimental evidence for the existence of cation swapping in this class of materials. In addition, we combine our results with UV-VIS spectroscopy to highlight the influence of disorder on the optical bandgap

Unraveling the properties of sharply defined submicron scale FeCu and FePd magnetic structures fabricated by electrodeposition onto electron-beam-lithographed substrates

In this work, Fe–X (X = Cu, Pd) submicron-scale structures were electrodeposited onto pre-patterned substrates prepared by e-beam lithography. The FeCu and FePd (with reduced Pd content) systems were investigated as attractive candidates for a variety of potential applications in magnetic data storage and biomedicine. Confined growth in the restricted cavities resulted in a nanoscale grain size leading to well-defined geometries with sharp edges and corners and an average height of up to 215 nm. Specifically, nine 100 μm × 100 μm arrays of three geometries (cylindrical, rectangular and cruciform) in three different sizes were created. In addition, the total deposition time ranged from 3.5 s (FeCu) to 200 s (FePd), i.e. much faster than by traditional physical vapor deposition approaches and was performed at ambient conditions. Magnetic force microscopy for the cylindrical and cruciform structures revealed virtually no contrast at zero field, suggesting magnetic curling effects (instead of coherent rotation) during magnetization reversal. These curling effects result in low values of remanent magnetization, which is advantageous in minimizing dipolar interactions between the structures either when they are deposited onto the substrate or eventually dispersed in a liquid (e.g. in biomedical applications, as drug delivery carriers, where particle agglomeration is undesirable)

Electromechanical Behavior of Al/Al2_{2}O3_{3} Multilayers on Flexible Substrates: Insights from In Situ Film Stress and Resistance Measurements

A series of Al and Al/Al$_{2}$O$_{3}$ thin-film multilayer structures on flexible polymer substrates are fabricated with a unique deposition chamber combining magnetron sputtering (Al) and atomic layer deposition (ALD, Al$_{2}$O$_{3}$, nominal thickness 2.4–9.4 nm) without breaking vacuum and thoroughly characterized using transmission electron microscopy (TEM). The electromechanical behavior of the multilayers and Al reference films is investigated in tension with in situ X-ray diffraction (XRD) and four-point probe resistance measurements. All films exhibit excellent interfacial adhesion, with no delamination in the investigated strain range (12%). For the first time, an adhesion-promoting naturally forming amorphous interlayer is confirmed for thin films sputter deposited onto polymers under laboratory conditions. The evolution of Al film stresses and electrical resistance reveal changes in the deformation behavior as a function of oxide thickness. Strengthening of Al is observed with increasing oxide thickness. Significant embrittlement can be avoided for oxide layer thicknesses ≤2.4 nm

Crystal and magnetic structure transitions in bimno3+δ ceramics driven by cation vacancies and temperature

The crystal structure of BiMnO$_{3+δ}$ ceramics has been studied as a function of nominal oxygen excess and temperature using synchrotron and neutron powder diffraction, magnetometry and differential scanning calorimetry. Increase in oxygen excess leads to the structural transformations from the monoclinic structure (C2/c) to another monoclinic (P2$_{1}$/c), and then to the orthorhombic (Pnma) structure through the two-phase regions. The sequence of the structural transformations is accompanied by a modification of the orbital ordering followed by its disruption. Modification of the orbital order leads to a rearrangement of the magnetic structure of the compounds from the long-range ferromagnetic to a mixed magnetic state with antiferromagnetic clusters coexistent in a ferromagnetic matrix followed by a frustration of the long-range magnetic order. Temperature increase causes the structural transition to the nonpolar orthorhombic phase regardless of the structural state at room temperature; the orbital order is destroyed in compounds BiMnO$_{3+δ}$ (δ ≤ 0.14) at temperatures above 470 °C

Cooperative light-induced breathing of soft porous crystals via azobenzene buckling

Although light is a prominent stimulus for smart materials, the application of photoswitches as light-responsive triggers for phase transitions of porous materials remains poorly explored. Here we incorporate an azobenzene photoswitch in the backbone of a metal-organic framework producing light-induced structural contraction of the porous network in parallel to gas adsorption. Light-stimulation enables non-invasive spatiotemporal control over the mechanical properties of the framework, which ultimately leads to pore contraction and subsequent guest release via negative gas adsorption. The complex mechanism of light-gated breathing is established by a series of in situ diffraction and spectroscopic experiments, supported by quantum mechanical and molecular dynamic simulations. Unexpectedly, this study identifies a novel light-induced deformation mechanism of constrained azobenzene photoswitches relevant to the future design of light-responsive materials

Crystal Growth and the Structure of a New Quaternary Adamantine Cu☐GaGeS₄

Single crystals of quaternary adamantine-type Cu☐GaGeS4 were grown using the chemical vapor transport technique, with iodine as the transport agent. Dark red transparent crystals were grown in a temperature gradient of ΔT = 900–750 °C. Chemical characterization by X-ray fluorescence showed the off-stoichiometric composition of Cu☐GaGeS4 crystals—in particular, a slight Ge deficiency was observed. By X-ray diffraction, Cu☐GaGeS4 was found to adopt the chalcopyrite-type structure with the space group I4¯2d. Cation distribution in this structure was analyzed by multiple energy anomalous synchrotron X-ray diffraction, and it was found that Cu and vacancies occupied the 4a site, whereas Ga and Ge occupied the 4b site. The band gap energies of several off-stoichiometric Cu☐GaGeS4 crystals were determined by UV-Vis spectroscopy and ranged from 2.1 to 2.4 eV. A non-linear correlation of the band gap energy with the Ge content of the compound was shown to follow the usual bowing behavior of semiconductor alloys, with a bowing parameter of b = −1.45 (0.08)

The electro-chemo-mechanical coupling in lithium alloy electrodes and its origins

A method to identify and separate the influence of changes in the surface stress from the bulk stress in a model lithium-ion battery electrode during electrochemical cycling was developed. The strategy for this separation is based on the different influence of surface and bulk stresses on the coupling between electrode potential and mechanical strain as measured by dynamic electro-chemo-mechanical analysis and the coupling between the transferred electric charge and the elastic strain as determined by wide angle X-ray scattering. Using both methods, it was possible to uncover the behavior of an apparent surface stress evoked by the bulk stress due to grain boundary alloying of lithium in a gold film. Additionally, the analysis allowed for a determination of a range in surface stress due to underpotential deposition of one monolayer of lithium as the interval between -3.1 to -1.9 N/m