- [Show abstract] [Hide abstract] ABSTRACT: We present the results of the study of the correlation between the electrical and structural properties of individual GaAs nanowires measured in their as-grown geometry. The resistance and the effective charge carrier mobility were extracted for several nanowires, and subsequently, the same nano-objects were investigated using X-ray nanodiffraction. This revealed a number of perfectly stacked zincblende and twinned zincblende units separated by axial interfaces. Our results suggest a correlation between the electrical parameters and the number of intrinsic interfaces.
- [Show abstract] [Hide abstract] ABSTRACT: In this work, we describe the synthesis of CdS nanocrystals in thin polymeric films by in-situ Grazing Incidence Diffraction (GID) and Grazing Incidence Small Angle Scattering (GISAXS). The 2D GISAXS patterns indicate how the precursor structure is altered as the temperature is varied from 25°C to 300°C. At 150°C, the CdS nanocrystals start to arrange themselves in a hexagonal lattice with a lattice parameter of 27 Å. The diffraction intensity from the hexagonal lattice reaches a maximum at 170°C and decreases steadily upon further heating above 220°C indicating loss of symmetry. Correspondingly, the GID scans at 170°C show strong crystalline peaks from cubic CdS nanocrystals that are about 2 nm size. The results indicate that a temperature of 170°C is sufficient to synthesize CdS nanocrystals without degradation of the polymer matrix (Topas) in thin films (about 30nm).
- [Show abstract] [Hide abstract] ABSTRACT: Thin films of the lead-free ferroelectric Na0.5Bi0.5TiO3 grown on thin-film Pt electrodes supported by SrTiO3 substrates have a complex microstructure consisting of crystalline grains with three distinct major crystallographic orientations. The piezoelectric response measured in spatially separated sub-micron grains using time-resolved synchrotron x-ray microdiffraction is highly inhomogeneous even among grains sharing the same major orientation. The piezoelectric coefficient d 33 varies by nearly a factor of two in a series of areas sharing the 〈001〉 orientation. The piezoelectric inhomogeneity is linked to the peculiar microstructure of the film, arising from local variations in the stress imposed by surrounding grains with different crystallographic orientations and differing directions of the ferroelectric remnant polarization. A systematic nonlinearity of the piezoelectric strain is observed in applied electric fields with small magnitudes in all regions, consistent with the coexistence of domains of differing polarization direction at zero applied electric field.
- [Show abstract] [Hide abstract] ABSTRACT: Polymers such as benzocyclobutene are commonly used as embedding materials for semiconductor nanostructures. During the curing process of the polymer up to 250 °C, a significant impact of strain can be induced on the embedded semiconductor material due to different thermal expansion coefficients. This strain has been revealed by X-ray diffraction in free-standing GaAs nanowires grown on a silicon substrate, embedded in a polymer matrix. It will be shown that this strain is released during the X-ray irradiation if additionally an external static electric field is applied.
- [Show abstract] [Hide abstract] ABSTRACT: Numerous imaging methods have been developed over recent years in order to study materials at the nanoscale. Within this context, scanning X-ray diffraction microscopy has become a routine technique, giving access to structural properties with sub-micrometre resolution. This article presents an optimized technique and an associated software package which have been implemented at the ID01 beamline (ESRF, Grenoble). A structural scanning probe microscope with intriguing imaging qualities is obtained. The technique consists in a two-dimensional quick continuous mapping with sub-micrometre resolution of a sample at a given reciprocal space position. These real space maps are made by continuously moving the sample while recording scattering images with a fast two-dimensional detector for every point along a rocking curve. Five-dimensional data sets are then produced, consisting of millions of detector images. The images are processed by the user-friendly X-ray strain orientation calculation software ( XSOCS ), which has been developed at ID01 for automatic analysis. It separates tilt and strain and generates two-dimensional maps of these parameters. At spatial resolutions of typically 200–800 nm, this quick imaging technique achieves strain sensitivity below Δ a / a = 10 −5 and a resolution of tilt variations down to 10 −3 ° over a field of view of 100 × 100 µm.
- [Show abstract] [Hide abstract] ABSTRACT: Strained semiconductors are ubiquitous in microelectronics and microelectromechanical systems, where high local stress levels can either be detrimental for their integrity or enhance their performance. Consequently, local probes for elastic strain are essential in analyzing such devices. Here, a scanning X-ray sub-microprobe experiment for the direct measurement of deformation over large areas in single-crystal thin films with a spatial resolution close to the focused X-ray beam size is presented. By scanning regions of interest of several tens of micrometers at different rocking angles of the sample in the vicinity of two Bragg reflections, reciprocal space is effectively mapped in three dimensions at each scanning position, obtaining the bending, as well as the in-plane and out-of-plane strain components. Highly strained large-area Ge structures with applications in optoelectronics are used to demonstrate the potential of this technique and the results are compared with finite-element-method models for validation.
- [Show abstract] [Hide abstract] ABSTRACT: A comprehensive overview of the possibilities and potential of X–ray scattering using nanofocused beams for probing matter at the nanoscale, including guidance on the design of nanobeam experiments. The monograph discusses various sources, including free electron lasers, synchrotron radiation and other portable and non–portable X–ray sources. For scientists using synchrotron radiation or students and scientists with a background in X–ray scattering methods in general.
- [Show abstract] [Hide abstract] ABSTRACT: We study by X-ray nanodiffraction the statistical distribution of the two possible twinned zinc-blende (ZB) orientations as well as the occurrence of the wurtzite structure within single GaAs nanowires (NWs) grown by molecular beam epitaxy on Si(111). A fast scanning scheme allowed to perform diffraction experiments on 160 individual NWs. We find that although on average the two ZB orientations show a similar abundance, in 90% of all NWs one ZB orientation dominates and little twinning is observed within each individual NW. ((c) 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)
- [Show abstract] [Hide abstract] ABSTRACT: We present here an unprecedented way of quantifying the number of dislocations in microcrystals. This method relies on a combination of several state-of-the-art techniques: coherent x-ray diffraction used as a local probe, together with the controlled compression of micro-objects. We demonstrate that by using this method, dislocations in the microcrystal can be detected and their number precisely quantified. This cannot be done with other techniques in a nondestructive way. Our method opens a route for the study of many small-scale systems with defect-dependent physical properties and it could become a critical tool for addressing future challenges in nanotechnology.
- [Show abstract] [Hide abstract] ABSTRACT: Instabilities caused during the erosion of a surface by an ion beam can lead to the formation of self-organized patterns of nanostructures. Understanding the self-organization process requires not only the in-situ characterization of ensemble averaged properties but also probing the dynamics. This can be done with the use of coherent X-rays and analyzing the temporal correlations of the scattered intensity. Here, we show that the dynamics of a semiconductor surface nanopatterned by normal incidence ion beam sputtering are age-dependent and slow down with sputtering time. This work provides a novel insight into the erosion dynamics and opens new perspectives for the understanding of self-organization mechanisms.
Article: Nanobeam X-ray Scattering
- [Show abstract] [Hide abstract] ABSTRACT: Ion beam sputtering is a widely used technique to obtain patterned surfaces. Despite the wide use of this approach on different materials to create surface nanostructures, the theoretical model to explain the time evolution of the erosion process is still debated. We show, with the help of simulations, that two-time correlation functions can serve to assess the validity of different models. These functions can be measured experimentally with the x-ray photon correlation spectroscopy technique.
- [Show abstract] [Hide abstract] ABSTRACT: A detailed characterization of the coherent x-ray wavefront produced by a partially illuminated Fresnel zone plate is presented. We show, by numerical and experimental approaches, how the beam size and the focal depth are strongly influenced by the illumination conditions, while the phase of the focal spot remains constant. These results confirm that the partial illumination can be used for coherent diffraction experiments. Finally, we demonstrate the possibility of reconstructing the complex-valued illumination function by simple measurement of the far field intensity in the specific case of partial illumination.
- [Show abstract] [Hide abstract] ABSTRACT: For advanced electronic, optoelectronic, or mechanical nanoscale devices a detailed understanding of their structural properties and in particular the strain state within their active region is of utmost importance. We demonstrate that X-ray nanodiffraction represents an excellent tool to investigate the internal structure of such devices in a nondestructive way by using a focused synchotron X-ray beam with a diameter of 400 nm. We show results on the strain fields in and around a single SiGe island, which serves as stressor for the Si-channel in a fully functioning Si-metal-oxide semiconductor field-effect transistor.
- [Show abstract] [Hide abstract] ABSTRACT: Three-dimensional reciprocal-space maps of a single SiGe island around the Si(004) Bragg peak are recorded using an energy-tuning technique with a microfocused X-ray beam with compound refractive lenses as focusing optics. The map is in agreement with simulated data as well as with a map recorded by an ordinary rocking-curve scan. The energy-tuning approach circumvents both the comparatively large sphere of confusion of diffractometers compared with nanostructures and vibrations induced by motors. Thus, this method offers new possibilities for novel combinations of three-dimensional micro- and nano-focused X-ray diffraction with complex in situ sample environments such as scanning probe microscopes.
- [Show abstract] [Hide abstract] ABSTRACT: We investigated the growth of CdS nanoparticles in polymer films by means of ex-situ and in-situ x-ray scattering experiments using synchrotron radiation. The CdS nanoparticles were synthesized by thermal decomposition of a Cd thiolate precursor dispersed in a cyclic olefin copolymer. The films were deposited by spin coating. Grazing incidence diffraction (GID) reveals the Bragg reflections of the CdS nanoparticles. In-situ diffraction and grazing incidence small angle scattering (GISAXS) experiments were recorded during the thermal treatment of the precursor/polymer films from room temperature up to 250°C. The diffraction curves show that the initial precursor structure is soon lost at 100°C Correspondingly, the GISAXS data show a peak at a momentum transfer value q - 0.2Å-1 that shifts towards smaller values with the temperature. Under UV excitation the films show photoluminescence in the range 400-700 nm.
- [Show abstract] [Hide abstract] ABSTRACT: SiGe islands are used to induce tensile strain in the Si channel of Field Effect Transistors to achieve larger transconductance and higher current driveabilities. We report on x-ray diffraction experiments on a single fully-processed and functional device with a TiN+Al gate stack and source, gate, and drain contacts in place. The strain fields in the Si channel were explored using an x-ray beam focused to 400 nm diameter combined with finite element simulations. A maximum in-plane tensile strain of about 1% in the Si channel was found, which is by a factor of three to four higher than achievable for dislocation-free tensile strained Si in state-of-the-art devices. Comment: The following article has been submitted to Applied Physics Letters. After it is published, it will be found at http://apl.aip.org/
- [Show abstract] [Hide abstract] ABSTRACT: We investigate the feasibility of applying coherent diffraction imaging to highly strained epitaxial nanocrystals using finite-element simulations of SiGe islands as input in standard phase retrieval algorithms. We discuss the specific problems arising from both epitaxial and highly strained systems and we propose different methods to overcome these difficulties. Finally, we describe a coherent microdiffraction experimental setup using extremely focused x-ray beams to perform experiments on individual nanostructures.
- [Show abstract] [Hide abstract] ABSTRACT: In this review we cover and describe the application of grazing incidence x-ray scattering techniques to study and characterize nanopattern formation on semiconductor surfaces by ion beam erosion under various conditions. It is demonstrated that x-rays under grazing incidence are especially well suited to characterize (sub)surface structures on the nanoscale with high spatial and statistical accuracy. The corresponding theory and data evaluation is described in the distorted wave Born approximation. Both ex situ and in situ studies are presented, performed with the use of a specially designed sputtering chamber which allows us to follow the temporal evolution of the nanostructure formation. Corresponding results show a general stabilization of the ordering wavelength and the extension of the ordering as a function of the ion energy and fluence as predicted by theory. The in situ measurements are especially suited to study the early stages of pattern formation, which in some cases reveal a transition from dot to ripple formation. For the case of medium energy ions crystalline ripples are formed buried under a semi-amorphous thick layer with a ripple structure at the surface being conformal with the crystalline/amorphous interface. Here, the x-ray techniques are especially advantageous since they are non-destructive and bulk-sensitive by their very nature. In addition, the GI x-ray techniques described in this review are a unique tool to study the evolving strain, a topic which remains to be explored both experimentally and theoretically.
European Synchrotron Radiation FacilityGrenoble, Rhône-Alpes, France
Johannes Kepler University Linz
Linz, Upper Austria, Austria
- Institute of Semiconductor and Solid State Physics