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We present a new protocol to grow large-area, high-quality single-layer graphene on Cu foils at relatively low temperatures. We use C60 molecules evaporated in ultra high vacuum conditions as carbon source. This clean environment results in a strong reduction of oxygen-containing groups as depicted by X-ray photoelectron spectroscopy (XPS). Unzipping of C60 is thermally promoted by annealing the substrate at 800 °C during evaporation. The graphene layer extends over areas larger than the Cu crystallite size, although it is changing its orientation with respect to the surface in the wrinkles and grain boundaries, producing a modulated ring in the low energy electron diffraction (LEED) pattern. This protocol is a self-limiting process leading exclusively to one single graphene layer. Raman spectroscopy confirms the high quality of the grown graphene. This layer exhibits an unperturbed Dirac-cone with a clear n-doping of 0.77 eV, which is caused by the interaction between graphene and substrate. Density functional theory (DFT) calculations show that this interaction can be induced by a coupling between graphene and substrate at specific points of the structure leading to a local sp3 configuration, which also contribute to the D-band in the Raman spectra., Financial support from EU Horizon 2020 research and innovation program under grant agreement No. 696656 (GrapheneCore1-Graphene-based disruptive technologies) and Spanish MINECO (grants MAT2014-54231-C4-1-P,MAT2014-52405-C2-2-R, CSD2009-00013, MAT2015-64110) is acknowledged. JA and NR are supported by the FPI program from MINECO (BES-2012-058600 and BES-2015-072642, respectively). CM and JIM acknowledge the financial support by the “Ramón y Cajal” Program of MINECO (RYC-2014-16626 and RYC-2015-17730, respectively). JIM and GS acknowledge funding from the ERC-Synergy Program (grant ERC-2013-SYG-610256 Nanocosmos). JIM thanks CTI-CSIC for use of computing resources. MK and VV acknowledge funding from ERC-CZ (LL1301) project. GO-I acknowledges FCT for his grant (SFRH/BPD/90562/2012).

Spray coating, a simple and low‐cost technique for large‐scale film deposition, is employed to fabricate mesoporous titania films, which are electron‐transporting layers in all‐solid‐state dye‐sensitized solar cells (DSSCs). To optimize solar cell performance, presynthesized crystalline titania nanoparticles are introduced into the mesoporous titania films. The composite film morphology is examined with scanning electron microscopy, grazing incidence small‐angle X‐ray scattering, and nitrogen adsorption–desorption isotherms. The crystal phase and crystallite sizes are verified by X‐ray diffraction measurements. The photovoltaic performance of all‐solid‐state DSSCs is investigated. The findings reveal that an optimal active layer of the all‐solid‐state DSSC is obtained by including 50 wt% titania nanoparticles, showing a foam‐like morphology with an average pore size of 20 nm, featuring an anatase phase, and presenting a surface area of 225.2 m2 g−1. The optimized morphology obtained by adding 50 wt% presynthesized crystalline titania nanoparticles yields, correspondingly, the best solar cell efficiency of 2.7 ± 0.1%., Financial support by TUM.solar in the context of the Bavarian Collaborative Research Project “Solar Technologies Go Hybrid” (SolTech), by the GreenTech Initiative (Interface Science for Photovoltaics – ISPV) of the EuroTech Universities and by the Nanosystems Initiative Munich (NIM) is gratefully acknowledged. V.K. thanks the Bavarian State Ministry of Sciences, Research and Arts for funding this research work via project “Energy Valley Bavaria.” L.S., W.W., and Y.Y. acknowledge the China Scholarship Council (CSC).

Crazes constitute one of the most common failure mechanisms in polymers. They act as fracture precursors, severely degrading the mechanical properties of the material. Thus, a deep understanding of the chain rearrangement occurring inside crazes is of utmost fundamental and practical importance. We have employed synchrotron infrared microspectroscopy (SIRMS) and Raman microspectroscopy to investigate the conformational changes inside micron-sized crazes in poly(ethylene terephthalate), PET. A promotion of the full-extended chain conformational structure at the expense of mainly the trans amorphous mesomorphic phase along with an increase in crystallinity of around 4% has been found. These results differ from what we observed across the deformation neck during PET cold drawing, where no promotion of the all-trans crystalline conformation occurred for slow drawing speeds at temperatures well below the glass transition. Our results show the tremendous capabilities of advanced vibrational microspectroscopy techniques to investigate microscale phenomena in polymer science.

Microfocus X-ray scattering and micro Raman spectroscopy have been applied to study the β-transcrystalline morphology in isotactic polypropylene. The transformation from the α- to the β-form through the so-called bifurcation of growth mechanism has been investigated with high spatial resolution. We found that the mixed α-β region does not present spatial correlation along the shearing direction, implying that there is no cooperative crystallization from the different β-nucleation centres. In addition, a strong change in the lamellar orientation of the α-form thin layer that induces the growth of the β-crystallites has been observed for the first time. Finally, changes in the relative intensities of some selected Raman bands allowed the observation of the α-β transformation process at the molecular level. (© 2014 WILEY-VCH Verlag GmbH &Co. KGaA, Weinheim) In fibre-reinforced materials the interaction between the fibre and the matrix strongly affects the final properties of the material. Therefore, a detailed analysis of the interface is of utmost importance. By applying a battery of different microscopic techniques, we investigate the transcrystalline polymorphic morphology of isotactic polypropylene with unprecedented spatial resolution.

Graphical abstractDisplay Omitted Gold nanowire gratings for organic photovoltaic cells were fabricated on, within and below ITO electrodes.The nanogratings have been fabricated by e-beam lithography and nano imprint lithography.The gratings were analyzed by SEM, AFM and GISAXS measurements.The tuneability of the plasmon resonance has been shown by white light extinction spectroscopy. Organic photovoltaic devices are interesting alternatives to conventional silicon based photovoltaic cells, due to potentially lower material costs and energy consumption during the fabrication process. However, the energy conversion efficiency of organic photovoltaic cells may still be improved. One possible approach is a combination with metallic nanostructures to improve light absorption properties in the active layer. We report on the fabrication and characterization of metallic nanogratings integrated with an indium tin oxide (ITO) electrode to be combined with small-molecule organic photovoltaic cells. With respect to geometry and extinction properties gratings fabricated by two different fabrication methods, conventional electron beam lithography and nanoimprint lithography, are presented. Furthermore, gratings fabricated on top of ITO are compared to gratings integrated both below and within ITO electrodes. Fabricating structures below or within electrodes is advantageous for organic thin film techniques to avoid compromising the crystallinity of the organic thin film and short-circuiting across the thin layer.

A simple, easily accessible solvent-free method for the dispersion of MWCNTs into PET is proposed, based on the preparation of a microparticulate polymer/nanotube masterbatch via cryogenic impact-milling and its subsequent melt blending with the bulk polymer. Thermal and mechanical properties of nanocomposites prepared using this method were evaluated as a function of nanotube concentration. Thermal stability was improved, and superior crystallization behavior of PET in the nanocomposites was observed. Significant improvements of around 25% in tensile strength and tensile modulus of the nanocomposites was achieved using this strategy, with only 0.25 wt.-% MWCNT, compared to previous literature data where 1wt.-% MWCNT was employed.

Titania nanoparticles are produced by laser ablation in liquid in order to initiate functionalization of titania with the polymer for the active layer. By combining these titania nanoparticles and water-soluble poly[3-(potassium-6-hexanoate)thiophene-2,5-diyl] (P3P6T) hybrid solar cells are realized., Financial support by TUM.solar in the frame of the Bavarian Collaborative Research Project “Solar technologies go Hybrid” (SolTec), by the GreenTech Initiative (Interface Science for Photovoltaics–ISPV) of the EuroTech Universities and by the Nanosystems Initiative Munich (NIM) is acknowledged. V.K. thanks the Bavarian State Ministry of Education, Science and the Arts for funding this research work via project “Energy Valley Bavaria”. L.S., W.W. and Y.Y. acknowledge the China Scholarship Council (CSC).

We describe the new experimental possibilities of the micro- and nanofocus X-ray scattering beamline P03 of the synchrotron source PETRA III at DESY, Hamburg (Germany), which arise from experiments with smaller beam sizes in the micrometer range. This beamline has been upgraded recently to perform new kinds of experiments. The use of an intermediate focus allows for reducing the beam size of microfocused hard X-rays while preserving a large working distance between the focusing elements and the focus position. For the first time, this well-known methodology has been employed to grazing incidence small- and wide-angle X-ray scattering (GISAXS/GIWAXS). As examples, we highlight the applications to in situ studies using microfluidic devices in GISAXS geometry as well as the investigation of the crystallinity of thin films in GIWAXS geometry.

Over the last decade the use of synchrotron infrared microspectroscopy to spatially discriminate chemical and structural features in many different types of materials has grown considerably and has made significant impact in numerous research areas, in particular, in biological sciences and medicine. Although the brightness advantage of the synchrotron infrared (IR) source is well accepted as the key to high spatial discrimination, little attention has been given to measure the polarization properties of the synchrotron light at the sample stage in IR microscopy. In this work the intrinsic polarization of the IR source and its consequences for the study of anisotropic materials are discussed. The polarization characteristics of predominantly bending magnet radiation and predominantly edge radiation sources were measured at the microscope focus and compared. To illustrate the direct use of the intrinsic polarization of these sources in microscopy, the orientation and conformational details of a drawn polymer sample are considered.

The crystallization process of isotactic polypropylene (iPP) was studied under both dynamic and isothermal conditions for a series of multiwall carbon nanotube (MWCNT) composites with nanotube concentrations between 0.1 and 1.0% by weight. The nucleation activity of the nanofillers was confirmed for both dynamic and isothermal crystallization, and was shown to be composition dependent. The effect of the nanofiller on the crystallization of iPP was discussed using the temperature coefficients obtained to determine the interfacial free energy and free energy of nucleation. The basal interfacial free energy decreased with respect to that of neat iPP by up to 15% for as little as 0.1% MWCNT, subsequently decreasing linearly with increasing nanotube concentration. This behavior is in line with the crystallization behavior of iPP with conventional nucleating agents. POLYM. COMPOS., 2011. © 2010 Society of Plastics Engineers

Solution-processed organic bulk heterojunction solar cells based on poly(3-hexylthiophene) (P3HT) blended with [6,6]-phenyl-C60-butyric acid methyl ester are doped with different concentrations of iron (II,III) oxide nanoparticles (Fe3O4). The power conversion efficiency of the devices doped at low concentrations is improved up to 11%. The improvement finds its origin in a lower recombination current, which is a consequence of an increased effective exciton lifetime according to the J–V characteristics and the optoelectronical analysis of the films. The increase in performance cannot be attributed to changes in morphology or crystallinity according to grazing-incidence X-ray scattering experiments. The evolution of the solar cell short-circuit current at low doping concentrations is related to variations in the arrangement of the crystalline regions of P3HT. For high doping concentrations (above 1.0 wt%) the performance of the solar cell decays rapidly, ascribed to the increased leakage currents in the device caused by the presence of nanoparticles.

Review of scientific instruments 84, 043901 (2013). doi:10.1063/1.4798544, HASE (Highly Automated Sputter Equipment) is a new mobile setup developed to investigate deposition processes with synchrotron radiation. HASE is based on an ultra-high vacuum sputter deposition chamber equipped with an in-vacuum sample pick-and-place robot. This enables a fast and reliable sample change without breaking the vacuum conditions and helps to save valuable measurement time, which is required for experiments at synchrotron sources like PETRA III at DESY. An advantageous arrangement of several sputter guns, mounted on a rotative flange, gives the possibility to sputter under different deposition angles or to sputter different materials on the same substrate. The chamber is also equipped with a modular sample stage, which allows for the integration of different sample environments, such as a sample heating and cooling device. The design of HASE is unique in the flexibility. The combination of several different sputtering methods like standard deposition, glancing angle deposition, and high pressure sputter deposition combined with heating and cooling possibil-ities of the sample, the large exit windows, and the degree of automation facilitate many different grazing incidence X-ray scattering experiments, such as grazing incidence small and wide angle X-ray scattering, in one setup. In this paper we describe in detail the design and the performance of the new equipment and present the installation of the HASE apparatus at the Micro and Nano focus X-ray Scattering beamline (MiNaXS) at PETRA III. Furthermore, we describe the measurement options and present some selected results. The HASE setup has been successfully commissioned and is now available for users., Published by American Institute of Physics, [S.l.]

The spatially resolved dichroic behaviour of a series of isothermally crystallised samples of isotactic polypropylene and polybutene-1 was investigated using polarization-modulated synchrotron infrared microspectroscopy (PM-SIRMS). The high brightness of the synchrotron source provides a good signal-to-noise performance at high spatial resolution in spite of the significant loss in infrared intensity through the photoelastic modulator. This technique gives access to information on average polymer chain orientation and crystalline morphology at the microscale, widening the possibilities for spatially resolved dichroic mapping of polymeric materials.

The last decade has seen a spectacular growth in the use of synchrotron-based IR sources for infrared microspectroscopy. The unique features of coupling synchrotron radiation into commercial IR microscopes at IR beamlines gives access to spatially resolved infrared spectra with superior signal-to-noise characteristics. Specific features of the technique are discussed with particular emphasis on its application to the study of polymeric materials, with examples from a series of heterogeneous polymeric systems, including semicrystalline polymers and blends, reinforced composites and microstructured polymer membranes.