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Novel electrospun materials for bone tissue engineering were obtained by blending biodegradable polyhydroxybutyrate (PHB) or polyhydroxybutyrate valerate (PHBV) with the anionic sulfated polysaccharide κ-carrageenan (κ-CG) in varying ratios. In both systems, the two components phase separated as shown by FTIR, DSC and TGA. According to the contact angle data, κ-CG was localized preferentially at the fiber surface in PHBV/κ-CG blends in contrast to PHB/κ-CG, where the biopolymer was mostly found within the fiber. In contrast to the neat polyester fibers, the blends led to the formation of much smaller apatite crystals (800 nm vs 7 μm). According to the MTT assay, NIH3T3 cells grew in higher density on the blend mats in comparison to neat polyester mats. The osteogenic differentiation potential of the fibers was determined by SaOS-2 cell culture for 2 weeks. Alizarin red-S staining suggested an improved mineralization on the blend fibers. Thus, PHBV/κ-CG fibers resulted in more pronounced bioactive and osteogenic properties, including fast apatite-forming ability and deposition of nanosized apatite crystals.

This article reports on surface density variations that are accompanied by ion-beam-induced pattern formation processes on Si. The density profiles perpendicular to Si(100) surfaces were investigated after off-normal implantation with 5 keV Fe+ions at fluences ranging from 1 × 1016to 5 × 1017 ions cm−2. Ripple formation was observed for ion fluences above 1 × 1016 ions cm−2. X-ray reflectivity (XRR) revealed the formation of a nanometre subsurface layer with incorporated Fe. Using XRR, no major dependence of the surface density on the ion fluence could be found. In order to improve the surface sensitivity, extremely asymmetric X-ray diffraction was applied. Depth profiling was achieved by measuring X-ray rocking curves as a function of the decreasing incidence angle down to 0° using this noncoplanar scattering geometry. The density information was extracted from the dynamical Bragg shift of the diffraction peak caused by refraction of the X-ray beam at the air–sample interface. Simulations based on the dynamical theory of X-ray diffraction revealed a decrease of density for increasing ion fluence in a region close to the surface, caused by the amorphization and surface roughening.

We investigate the incorporation of iron atoms during nano-patterning of Si surfaces induced by 2 keV Kr + ion beam erosion under an off-normal incidence angle of 15°. Considering the low penetration depth of the ions, we have used X-ray reflectivity (XRR) and X-ray absorption near edge spectroscopy (XANES) under grazing-incidence angles in order to determine the depth profile and phase composition of the incorporated iron atoms in the near surface region, complemented by secondary ion mass spectrometry and atomic force microscopy. XRR analysis shows the accumulation of metallic atoms within a near surface layer of a few nanometer thickness. We verify that surface pattern formation takes place only when the co-sputtered Fe concentration exceeds a certain limit. For high Fe concentration, the ripple formation is accompanied by the enhancement of Fe close to the surface, whereas no Fe enhancement is found for low Fe concentration at samples with smooth surfaces. Modeling of the measured XANES spectra reveals the appearance of different silicide phases with decreasing Fe content from the top towards the volume.

Journal of applied physics 120(14), 145703 (2016). doi:10.1063/1.4964600, Unique electronic properties of semiconductor heterostructured nanowires make them useful for future nano-electronic devices. Here, we present a study of the band bending effect at the heterointerface of GaAs/InAs core/shell nanowires by means of synchrotron based X-ray photoelectron spectroscopy. Different Ga, In, and As core-levels of the nanowire constituents have been monitored prior to and after cleaning from native oxides. The cleaning process mainly affected the As-oxides and was accompanied by an energy shift of the core-level spectra towards lower binding energy, suggesting that the As-oxides turn the nanowire surfaces to n-type. After cleaning, both As and Ga core-levels revealed an energy shift of about −0.3 eV for core/shell compared to core reference nanowires. With respect to depth dependence and in agreement with calculated strain distribution and electron quantum confinement, the observed energy shift is interpreted by band bending of core-levels at the heterointerface between the GaAs nanowire core and the InAs shell., Published by American Inst. of Physics, Melville, NY

In this paper, we reported the preparation of non-stoichiometric copper sulfide Cu 7 S 4 nanocrystalline by ultrasonic irradiation in ethylenediamine solvent system mixed with a complexing agent of 1-decanthiol, using sulfur powder and copper nitrate as reactants under normal laboratory conditions. X-ray diffraction (XRD) pattern indicates that the products are nanocrystallites in monoclinic structure. Scanning electron microscope (SEM) images display that the product consists of nanocrystallites of about 20 nm which aggregated in the form of polydispersive nanoclusters with sizes in the range of 150–300 nm. Energy-dispersive X-ray analysis (EDAX) shows that the products are absolutely pure and atomic percentage ratio of Cu to S is about 60:40. UV–vis absorption spectroscopy of the as-prepared particles reveal an energy band gap of about 2.54 eV; compared to 2 eV corresponding to its bulk value; a blue shift of about 0.54 eV has been observed, which is understood as quantum size effect due to three-dimensional confinement of electrons and holes in a small volume.

CdS nanoparticles of about 5 nm in size have been prepared with the aid of ultrasound irradiation to ethylenediamine solution of cadmium acetate dehydrate and elemental S in presence of 1-decanthiol under air and normal laboratory conditions. X-ray diffraction (XRD) and selected area electron diffraction (SAED) studies indicate that the products are nanocrystallites in hexagonal structure. High resolution transmission electron microscopy (HRTEM) image reveals that lattice fringes are clearly visible, conforming their crystallinity with lattice space of 0.27 nm corresponding to (1 0 2) plane of hexagonal CdS. Energy-dispersive X-ray analysis (EDAX) shows that the product are entirely pure and atomic percentage ratio of Cd to S is about 53:47. UV–vis absorption spectroscopy of the as prepared nanoparticles reveals an energy band gap of about 3.8 eV compared to 2.42 eV corresponding to its bulk value; a blue shift of about 1.38 eV, which is understood as quantum size effect due to confinement of electron and hole in a small volume.

ZnS nanorods of approximately 1 μm in length and 20 nm in diameter have been prepared by sonicating ethylenediamine solution of elemental S and zinc acetate in presence of 1-decanthiol under air. The nanorods were characterized using techniques such as X-ray powder diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray analysis (EDAX) and UV–vis absorption spectroscopy. The as-prepared nanorods have regular shape, narrow size distribution and high purity, having band gap of 4.56 eV compared to 3.54 eV corresponding to its bulk single-crystal.

Defect engineering is an effective and powerful tool to control the existing material properties and produce completely new ones, which are symmetry-forbidden in a defect-free crystal. For example, the application of a static electric field to a single crystal of SrTiO3 forms a strained near-surface layer through the migration of oxygen vacancies out of the area beneath the positively charged electrode. While it was previously shown that this near-surface phase holds pyroelectric properties, which are symmetry-forbidden in centrosymmetric bulk SrTiO3, this paper reports that the same phase is strongly piezoelectric. We demonstrate the piezoelectricity of this phase through stroboscopic time-resolved X-ray diffraction under alternating electric field and show that the effective piezoelectric coefficient d33 ranges between 60 and 100 pC/N. The possible atomistic origins of the piezoelectric activity are discussed as a coupling between the electrostrictive effect and spontaneous polarization of this near-surface phase.

In this work, we report on correlations between surface density variations and ion parameters during ion beam-induced surface patterning process. The near-surface density variations of irradi- ated Si(100) surfaces were investigated after off-normal irradiation with 5 keV Fe ions at different fluences. In order to reduce the x-ray probing depth to a thickness below 5 nm, the extremely asym- metrical x-ray diffraction by variation of wavelength was applied, exploiting x-ray refraction at the air-sample interface. Depth profiling was achieved by measuring x-ray rocking curves as function of varying wavelengths providing incidence angles down to 0°. The density variation was extracted from the deviations from kinematical Bragg angle at grazing incidence angles due to refraction of the x-ray beam at the air-sample interface. The simulations based on the dynamical theory of x-ray diffraction revealed that while a net near-surface density decreases with increasing ion fluence which is accompanied by surface patterning, there is a certain threshold of ion fluence to surface density modulation. Our finding suggests that the surface density variation can be relevant with the mechanism of pattern formation.

We report on formation of non-crystalline Fe-silicides of various stoichiometries below the amorphized surface of crystalline Si(001) after irradiation with 5 keV Fe+ ions under off-normal incidence. We examined samples prepared with ion fluences of 0.1 × 1017 and 5 × 1017 ions cm−2 exhibiting a flat and patterned surface morphology, respectively. Whereas the iron silicides are found across the whole surface of the flat sample, they are concentrated at the top of ridges at the rippled surface. A depth resolved analysis of the chemical states of Si and Fe atoms in the near surface region was performed by combining X-ray photoelectron spectroscopy and X-ray absorption spectroscopy (XAS) using synchrotron radiation. The chemical shift and the line shape of the Si 2p core levels and valence bands were measured and associated with the formation of silicide bonds of different stoichiometric composition changing from an Fe-rich silicides (Fe3Si) close to the surface into a Si-rich silicide (FeSi2) towards the inner interface to the Si(001) substrate. This finding is supported by XAS analysis at the Fe K-edge which shows changes of the chemical environment and the near order atomic coordination of the Fe atoms in the region close to surface. Because a similar Fe depth profile has been found for samples co-sputtered with Fe during Kr+ ion irradiation, our results suggest the importance of chemically bonded Fe in the surface region for the process of ripple formation.