The properties of nanoscale materials vary with the size and shape of the building blocks, which can be measured by (grazing-incidence) small-angle X-ray scattering along with the mutual positions of the nanoparticles. The accuracy in the determination of such parameters is dependent on the signal-to-noise ratio of the X-ray scattering pattern and on the visibility of the interference fringes. Here, a first-generation-synchrotron-class X-ray laboratory microsource was used in combination with a new restoration algorithm to probe nanoscale-assembled superstructures. The proposed algorithm, based on a maximum likelihood approach, allows one to deconvolve the beam-divergence effects from data and to restore, at least partially, missing data cut away by the beam stopper. It is shown that the combination of a superbright X-ray laboratory microsource with the data-restoring method allows a virtual enhancement of the instrument brilliance, improving signal-to-noise ratio and fringe visibility and reaching levels of performance comparable to third-generation synchrotron radiation beamlines.

The paper shows how a table top superbright microfocus laboratory X-ray source and an innovative restoring-data algorithm, used in combination, allow to analyze the super molecular structure of soft matter by means of Small Angle X-ray Scattering ex-situ experiments. The proposed theoretical approach is aimed to restore diffraction features from SAXS profiles collected from low scattering biomaterials or soft tissues, and therefore to deal with extremely noisy diffraction SAXS profiles/maps. As biological test cases we inspected: i) residues of exosomes' drops from healthy epithelial colon cell line and colorectal cancer cells; ii) collagen/human elastin artificial scaffolds developed for vascular tissue engineering applications; iii) apoferritin protein in solution. Our results show how this combination can provide morphological/structural nanoscale information to characterize new artificial biomaterials and/or to get insight into the transition between healthy and pathological tissues during the progression of a disease, or to morphologically characterize nanoscale proteins, based on SAXS data collected in a room-sized laboratory.

The coupling and propagation of electromagnetic waves through planar X-ray waveguides (WG) with vacuum gap and Si claddings are analyzed in detail, starting from the source and ending at the detector. The general case of linearly tapered WGs (i.e. with the entrance aperture different from the exit one) is considered. Different kinds of sources, i.e. synchrotron radiation and laboratory desk-top sources, have been considered, with the former providing a fully coherent incoming beam and the latter partially coherent beams. It is demonstrated that useful information about the parameters of the WG can be derived, comparing experimental results with computer simulation based on analytical solutions of the Helmholtz equation which take into account the amplitude and phase matching between the standing waves created in front of the WG, and the resonance modes propagating into the WG

In this chapter, we will focus on a specific X-ray-based technique among those employed in surface science and which is especially suitable for the study of self-assembled nanocrystals: Grazing Incidence Small Angle X-ray Scattering (GISAXS). We will first introduce the main field of investigation considered herein, with basic notions of X-ray scattering from surfaces, and then address basic concepts about GISAXS. Finally, we will describe a few relevant examples of studies, of nanostructured architectures, through ex situ and in situ experiments of grazing incidence X-ray scattering. This manuscript is focused on the former, showing that they can be performed by using laboratory instruments. In situ investigations still need synchrotron radiation sources in most cases; therefore, only a few examples selected from the literature are reported here, for the sake of completeness. The experiments described are mainly performed in the small angle range, providing information on the size and shape of nanocrystals, together with their spatial arrangement. Both 2D and 3D architectures are considered. In particular, GISAXS measurements of 2D superlattices of nano-octapods, performed both at a third generation synchrotron beamline and with a table-top set-up, are compared; the employed table-top set-up is described in a dedicated paragraph. Further examples of grazing incidence studies as performed by the authors with a table-top set-up are reported: a GISAXS study of 3D iron oxide nanocrystal superlattices, showing the importance of modelling in order to obtain structural information from data; a combined small/wide angle scattering (GISAXS/GIWAXS) study of 3D PbS nanocrystal superlattices; and a GIWAXS study of P3HT nanofibres, showing how the ordering at the molecular and atomic length scales can be obtained by exploring different angular ranges in the same grazing incidence geometry. Finally, selected examples of in situ GISAXS studies, performed with synchrotron radiation sources, are described.

We performed reproducible atomic resolution Transmission Electron Microscopy and Wide Angle X-ray Scanning Microscopy experiments studying for the first time the nanoscale properties of a pristine fiber taken from the Turin Shroud. We found evidence of biologic nanoparticles of creatinine bounded with small nanoparticles of iron oxide. The kind, size and distribution of the iron oxide nanoparticles cannot be dye for painting but are ferrihydrate cores of ferritin. The consistent bound of ferritin iron to creatinine occurs in human organism in case of a severe polytrauma. Our results point out that at the nanoscale a scenario of violence is recorded in the funeral fabric and suggest an explanation for some contradictory results so far published.

Here we describe a new TEM-based coherent diffraction imaging (CDI) method to achieve sub-ångström resolution in lattice images of nanoparticles. The experiments were performed by using a TEM/STEM JEOL 2010F UHR (objective lens spherical aberration coefficient of (0.47±0.01) mm) with resolution at optimum defocus of 0.19nm and equipped by Schottky cathode. The experiments for CDI require the acquisition of HRTEM image and diffraction from the same region of the sample illuminated by a coherent electron probe. The experimental nano-diffraction must be recorded with the beam coherence length larger than the region to be imaged according to the oversampling requirements [1]. A new efficient iterative phase retrieval algorithm [2] based on pioneering work of Gerchberg and Saxton [3] has been developed and successfully applied. Figure 1 is an example of phase retrieval of a TiO2 particle at a resolution of 70 pm that allows to distinguish the O atoms appreciating subtle alterations in the unit cell structure of the nano-crystals, which would not be otherwise detectable by conventional HRTEM. Such structural deviations could be at the origin of peculiar size-dependent physical-chemical properties of the concerned oxide material in the nanoscale regime [2].

Purpose: In the hard x-ray region, the cross sections for the phase shift of low-Z elements are about 1000 times larger than the absorption ones. As a consequence, phase contrast is detectable even when absorption contrast is minimal or absent. Therefore, phase-contrast imaging could become a valid alternative to absorption contrast without delivering high dose to tissue/human body parts.

Herein, we demonstrate an EDI methodology, performed in a Jeol 2010F UHR microscope (spherical aberration coefficient Cs = 0.47±0.01 mm), by which the crystal structure of transition-metal oxide nanocrystals can be determined at 70 pm of resolution while unambiguously revealing the presence and location of light elements atomic columns in the relevant lattice. This approach, applied as a case study to TiO2 in the form of organic-capped nano-rods, also allows appreciating subtle alterations in the unit cell structure of the nano-crystals, relative to that inherent to the bulk material counterpart, which would not be otherwise detectable by conventional HRTEM. Such structural deviations could be at the origin of peculiar size-dependent physical-chemical properties of the concerned oxide material in the nanoscale regime. In addition, it is worthwhile to remark that this result has been achieved exposing the specimen to an electron dose as low as 106 e/nm2. The latter condition usually prevents the specimen against possible structural damages under exposure to 200 keV electrons, the induction of which remains one of the key issues in the ultimate accuracy achievable in the structural determination of materials [4].

We present a novel method to determine the projected atomic potential of a specimen directly from transmission electron microscopy coherent electron nano-diffraction patterns, overcoming common limitations encountered so far due to the dynamical nature of electron-matter interaction. The projected potential is obtained by deconvolution of the inverse Fourier transform of experimental diffraction patterns rescaled in intensity by using theoretical values of the kinematical atomic scattering factors. This novelty enables the compensation of dynamical effects typical of transmission electron microscopy (TEM) experiments on standard specimens with thicknesses up to a few tens of nm. The projected atomic potentials so obtained are averaged on sample regions illuminated by nano-sized electron probes and are in good quantitative agreement with theoretical expectations. Contrary to lens-based microscopy, here the spatial resolution in the retrieved projected atomic potential profiles is related to the finer lattice spacing measured in the electron diffraction pattern. The method has been successfully applied to experimental nano-diffraction data of crystalline centrosymmetric and non-centrosymmetric specimens achieving a resolution of 65 pm.

We present a method to treat spurious intensities in electron diffraction experiments. Coherent electron diffraction imaging requires proper data reduction before the application of phase retrieval algorithms. The presence of spurious intensities in the electron diffraction patterns makes the data reduction complicated and time consuming and jeopardizes the application of mathematical constraints to maximize the information that can be extracted from the experimental data. Here we show how the experimental diffraction patterns can be treated to remove the unwanted artifacts without corrupting the genuine intensities scattered by the specimen. The resulting diffraction patterns are suitable for the application of further processes and constraints aimed at deriving fundamental structural information by applying phase retrieval algorithms or other approaches capable of deriving quantitative atomic resolution information about the specimen structure.

Since its early days electron microscopy has represented a splendid way to study the interactions between charged particles and electromagnetic fields. These efforts produced a flexible and powerful tool to investigate the properties of the matter at the highest spatial resolution. One of the main reason for the high resolution achievable in electron microscopy is related to the small wavelength, l, associated to high-energy electrons, i.e. for 200 keV electrons l = 2.5pm. Unfortunately, the quality of the electron lenses is relatively poor and the diffraction limit is still unreached. The proof of Otto Scherzer in 1936 that skilful lens design could never eliminate the spherical and chromatic aberration of rotationally symmetric lenses [1] promote the efforts of the scientific community to find a gateway. Since that time many attempts were made from one side to find a way to correct spherical and chromatic aberrations via hardware and from the othe r to find different approaches to recovery the information lost in TEM imaging. In the latter approaches it might be mentioned, for example, the invention of Gabor of the holography [2] or the through focal reconstruction of the exit phase wave in high resolution TEM (HRTEM) [3]. Very recently, electron optical devices capable of correcting spherical aberration are available and sub-ångström resolution have been achieved by HRTEM [4] and incoherent imaging in scanning transmission electron microscopy (STEM) by using high angle annular dark field detector [5]. Nevertheless, the diffraction limit in electron microscopy is still not reached. Coherent diffraction imaging (CDI) is an approach combining real and reciprocal space information to achieve images in principle limited only by diffraction limit [6].

High-resolution imaging of low-atomic-number chemical elements using electron microscopy is challenging and may require the use of high doses of electrons. Electron diffractive imaging, which creates real-space images using diffraction intensities and phase retrieval methods, could overcome such issues, although it is also subject to limitations. Here, we show that a combination of electron diffractive imaging and high-resolution transmission electron microscopy can image individual TiO(2) nanocrystals with a resolution of 70 pm while exposing the specimen to a low dose of electrons. Our approach, which does not require spherical and chromatic aberration correction, can reveal the location of light atoms (oxygen) in the crystal lattice. We find that the unit cell in nanoscale TiO(2) is subtly different to that in the corresponding bulk.

Coherent Diffractive Imaging is a lensless technique that allows imaging of matter at a spatial resolution not limited by lens aberrations. This technique exploits the measured diffraction pattern of a coherent beam scattered by periodic and non-periodic objects to retrieve spatial information. The diffracted intensity, for weak-scattering objects, is proportional to the modulus of the Fourier Transform of the object scattering function. Any phase information, needed to retrieve its scattering function, has to be retrieved by means of suitable algorithms. Here we present a new approach, based on a memetic algorithm, i.e. a hybrid genetic algorithm, to face the phase problem, which exploits the synergy of deterministic and stochastic optimization methods. The new approach has been tested on simulated data and applied to the phasing of transmission electron microscopy coherent electron diffraction data of a SrTiO3 sample. We have been able to quantitatively retrieve the projected atomic potential, and also image the oxygen columns, which are not directly visible in the relevant high-resolution transmission electron microscopy images. Our approach proves to be a new powerful tool for the study of matter at atomic resolution and opens new perspectives in those applications in which effective phase retrieval is necessary.

The replacement of diseased tissues with biological substitutes with suitablebiomechanical properties is one of the most important goal in tissue engineering. Collagenrepresents a satisfactory choice for scaffolds. Unfortunately, the lack of elasticity represents arestriction to a wide use of collagen for several applications. In this work, we studied theeffect of human elastin-like polypeptide (HELP) as hybrid collagen-elastin matrices. Inparticular, we studied the biomechanical properties of collagen/HELP scaffolds ...

Bovine cornea was studied with scanning small-angle X-ray scattering (SAXS) microscopy, by using both synchrotron radiation and a microfocus laboratory source. A combination of statistical (adaptive binning and canonical correlation analysis) and crystallographic (pair distribution function analysis) approaches allowed inspection of the collagen lateral packing of the supramolecular structure. Results reveal (i) a decrease of the interfibrillar distance and of the shell thickness around the fibrils from the periphery to the center of the cornea, (ii) a uniform fibril diameter across the explored area, and (iii) a distorted quasi-hexagonal arrangement of the collagen fibrils. The results are in agreement with existing literature. The overlap between laboratory and synchrotron-radiation data opens new perspectives for further studies on collagen-based/engineered tissues by the SAXS microscopy technique at laboratory-scale facilities.Bovine cornea was studied with scanning small-angle X-ray scattering microscopy, by using both synchrotron radiation and a microfocus laboratory source. The supramolecular structure of the collagen fibers is explored thanks to the combination of statistical (adaptive binning and canonical correlation analysis) and crystallographic (pair distribution function analysis) approaches.

This paper describes the scientific aims and potentials as well as the preliminary technical design of IRIDE, an innovative tool for multi-disciplinary investigations in a wide field of scientific, technological and industrial applications. IRIDE will be a high intensity "particles factory", based on a combination of high duty cycle radio-frequency superconducting electron linacs and of high energy lasers. Conceived to provide unique research possibilities for particle physics, for condensed matter physics,chemistry and material science, for structural biology and industrial applications, IRIDE will open completely new research possibilities and advance our knowledge in many branches of science and technology. IRIDE is also supposed to be realized in subsequent stages of development depending on the assigned priorities.

Electron diffractive imaging (EDI) relies on combining information from the high-resolution transmission electron microscopy image of an isolated kinematically diffracting nano-particle with the corresponding nano-electron diffraction pattern. Phase-retrieval algorithms allow one to derive the phase, lost in the acquisition of the diffraction pattern, to visualize the actual atomic projected potential within the specimen at sub-ångström resolution, overcoming limitations due to the electron lens aberrations. Here the approach is generalized to study extended crystalline specimens. The new technique has been called keyhole electron diffractive imaging (KEDI) because it aims to investigate nano-regions of extended specimens at sub-ångström resolution by properly confining the illuminated area. Some basic issues of retrieving phase information from the EDI/KEDI measured diffracted amplitudes are discussed. By using the generalized Shannon sampling theorem it is shown that whenever suitable oversampling conditions are satisfied, EDI/KEDI diffraction patterns can contain enough information to lead to reliable phase retrieval of the unknown specimen electrostatic potential. Hence, the KEDI method has been demonstrated by simulations and experiments performed on an Si crystal cross section in the [112] zone-axis orientation, achieving a resolution of 71 pm.

In The Gospel as revealed to me, Maria Valtorta reports a lot of information on the Holy Land at the time of Jesus: historical, archaeological, astronomical, geographical, meteorological. She states she has written what seen "in vision". By a detailed astronomical analysis of explicit and implicit calendar information reported while she narrates detailed episodes concerning the three years of Jesus' public life-possible because of many references to lunar phases, constellations, planets visible in the night sky in her writings-it is ascertained that every event described implies a precise date-day, month, year-without being explicitly reported by her. For example, Jesus' crucifixion should have occurred on Friday April 23 of the year 34, a date proposed by Isaac Newton. She has also recorded the occurrence of rain so that the number of rainy days reported can be compared to the current meteorological data, supposing random observations and no important changes in rainfall daily frequency in the last 2000 years, the latter issue discussed in the paper. Unexpectedly, both the annual and monthly averages of rainy days deduced from the data available from the Israel Meteorological Service and similar averages deduced from her writings agree very well.

Nanocrystal superlattices are attracting significant interest due to novel and peculiar collective properties arising from the interactions of the nanocrystals forming the superlattice. A large variety of superlattice structures can be obtained, involving one or more types of nanocrystals, with different sizes and concentrations. Engineering of the superlattice properties relies on accurate structural and morphological characterization, able to provide not only a fundamental feedback for synthesis procedures, but also relevant insight into their structural properties for possible applications. Electron microscopy and X-ray based techniques are complementary approaches for nanoscale structural imaging, which however become challenging in the presence of building blocks only a few nanometers in size. Here, a structure solution for a three-dimensional (3D) self-assembly of PbS nanocrystals with bimodal size distribution is obtained, by exploiting small-angle X-ray diffraction, transmission electron microscopy, crystallographic procedures, and geometric constraints. In particular, analysis of small-angle X-ray diffraction data, based on the Patterson function and on the single crystal model, is shown to provide relevant information on the 3D superlattice structure as well as on particle size, the scattering signal being sensitive to particles as small as 1.5 nm. The combined approach here proposed is thus demonstrated to effectively overcome important resolution limitations in the imaging of superlattices including small nanocrystals.

PbS colloidal nanocrystal (NC) assemblies with monomodal and bimodal size distribution have been fabricated by slow evaporation of solvent on silicon substrates. The interparticle distances of the assembled structures have been carefully defined, both in the plane and in the z direction, perpendicular to the substrate, thanks to the combination of small and wide-angle X-ray diffraction and TEM measurements. The spectroscopic characteristics of PbS NCs, both in solution and organized in a superlattice, have been investigated by steady-state and time-resolved photoluminescence measurements. The optical results reveal the occurrence of a Forster resonant energy transfer (FRET) mechanism between closed-packed neighboring PbS NCs. The occurrence of FRET is dependent on NC assembly geometry, and thus on their interparticle distance, suggesting that only when NCs are close enough, as in the close-packed arrangement of the monomodal assembly, the energy transfer can be promoted. In bimodal assemblies, the energy transfer between large and small NCs is negligible, due to the low spectral overlap between the emission and absorption bands of the different sized nanoparticles and to the large interparticle distance. Moreover, recombination lifetimes on the microsecond time scale have been observed and explained in terms of dielectric screening effect, in agreement with previous findings on lead chalcogenide NC optical properties.

Ptychographic techniques are currently the subject of increasing scientific interest due to their capability to retrieve the complex transmission function of an object at very high resolution. However, they impose a substantial burden in terms of acquisition time and dimension of the scanned area, which limits the range of samples that can be studied. We have developed a new method that combines the ptychographic approach in one direction with Fresnel propagation in the other by employing a strongly asymmetric probe. This enables scanning the sample in one direction only, substantially reducing exposure times while covering a large field of view. This approach sacrifices ptychographic-related resolution in one direction, but removes any limitation on the probe dimension in the direction orthogonal to the scanning, enabling the scan of relatively large objects without compromising exposure times. (C) 2014 Optical Society of America

Until recently, the hard X-ray, phase-sensitive imaging technique called grating interferometry was thought to provide information only in real space. However, by utilizing an alternative approach to data analysis we demonstrated that the angular resolved ultra-small angle X-ray scattering distribution can be retrieved from experimental data. Thus, reciprocal space information is accessible by grating interferometry in addition to real space. Naturally, the quality of the retrieved data strongly depends on the performance of the employed analysis procedure, which involves deconvolution of periodic and noisy data in this context. The aim of this article is to compare several deconvolution algorithms to retrieve the ultra-small angle X-ray scattering distribution in grating interferometry. We quantitatively compare the performance of three deconvolution procedures (i.e., Wiener, iterative Wiener and Lucy Richardson) in case of realistically modeled, noisy and periodic input data. The simulations showed that the algorithm of Lucy Richardson is the more reliable and more efficient as a function of the characteristics of the signals in the given context. The availability of a reliable data analysis procedure is essential for future developments in grating interferometry. (C) 2013 Associazione Italiana di Fisica Medica. Published by Elsevier Ltd. All rights reserved.

Research on composite materials is facing, among others, the challenging task of incorporating nanocrystals, and their superstructures, in polymer matrices. Electron microscopy can typically image nanometre-scale structures embedded in thin polymer films, but not in films that are micron size thick. Here, X-ray Ptychography was used to visualize, with a resolution of a few tens of nanometers, how CdSe/CdS octapod-shaped nanocrystals self-assemble in polystyrene films of 24 ± 4 ?m, providing a unique means for non-destructive investigation of nanoparticles distribution and organization in thick polymer films.

The nanoscale structural order of air-dried rat-tail tendon is investigated using small-angle X-ray scattering (SAXS). SAXS fiber diffraction patterns were collected with a superbright laboratory microsource at XMI-LAB [Altamura, Lassandro, Vittoria, De Caro, Siliqi, Ladisa & Giannini (2012). J. Appl. Cryst. 45, 869-873] for increasing integration times (up to 10 h) and a novel algorithm was used to estimate and subtract background, and to deconvolve the beam-divergence effects. Once the algorithm is applied, the peak visibility improves considerably and reciprocal space information up to the 22nd diffraction order is retrieved (q = 0.21 angstrom(-1), d = 29 angstrom) for an 8-10 h integration time. The gain in the visibility is already significant for patterns collected for 0.5 h, at least on the more intense peaks. This demonstrates the viability of detecting structural changes on a molecular/nanoscale level in tissues with state-of-the-art laboratory sources and also the technical feasibility to adopt SAXS fiber diffraction as a future potential clinical indicator for disease.

Osteoarthritis (OA), among other bone pathologies, is expected to determine supramolecular changes at the level of the mineralized collagen fiber. In a proof-of-principle study, bone biopsies were collected from six coxarthritis-affected patients, aged 62-87 years, during hip prosthesis implant surgery, sliced down to 100 mm-thick tissues, and investigated using scanning small-angle and wide-angle X-ray scattering (SAXS and WAXS) transmission microscopy. A multimodal imaging evaluation of the SAXS and WAXS data, combined with principal component and canonical correlation analyses, allowed the transformation of the raw data into microscopy images and inspection of the nanoscale structure of the mineralized collagen fibers across mm 2 tissue areas. The combined scanning SAXS and WAXS microscopy is shown to be a suitable choice for characterizing and quantifying the nanostructural properties of collagen over extended areas. The results suggest the existence of a correlation between age and cross-linking-induced rigidity of collagen fibers.

Nanocomposites based on colloidal CdSe nanocrystals (NCs) and a poly(styrene-co-4-vinylpyridine), able to specifically coordinate the NC surface, have been designed and prepared. For first time, the polymer synthesis has been performed by using 2,2,5-tri-methyl-4-phenyl-3-azahexane-3-nitroxide as a mediator, increasing the percentage of 4-vinylpyridine monomeric unit, thus obtaining a random copolymer. The nanocomposite properties have been investigated as a function of NC surface chemistry and copolymer composition, by means of spectroscopic, morphological and structural characterization techniques. An improved uniformity of NC dispersion in the nanocomposite has been found at increased percentage of 4-vinylpyridine in the copolymer. The improved NC dispersion in the nanocomposite films has been discussed in terms of the ability of the copolymer to act as a multivalent ligand. The reported results offer a valuable contribution toward the design and the fabrication of innovative nanocomposite material, formed of copolymers and colloidal NCs, specifically suited for energy conversion applications.

Here the synthesis of distinct monomodal and bimodal PbS nanocrystal (NC) populations, with narrow size-distribution, is reported. The ability to achieve careful control of NC size and size distribution allowed the preparation, in one single synthetic step, of two distinct populations of PbS NCs, with tuneable size ratio. The NC growth was carefully studied in order to gain insight into the mechanism underlying the formation of the mono and bimodal PbS NC families. The synthesized PbS NCs were structurally and chemically characterized, and subsequently used as building blocks for fabricating solid crystal assemblies by solvent evaporation. In particular the role played by different parameters, namely NC size and concentration, dispersing solvent and substrate, on crystallinity, geometry and structure of the obtained solids was systematically investigated. Interestingly the assembly of bimodal PbS NC samples leads to the formation of diverse superlattice structures, with a final geometry dependent on the NC size and the size ratio in the bimodal population. The synthetic procedure was then ultimately responsible of the superlattice structures, through the control of the PbS NC size and size ratio in the bimodal population.

Three-dimensional binary superlattices were obtained by self-assembly of PbS nanocrystals (NCs) of size <= 4 nm, synthesized by colloidal chemistry routes and characterized by two distinct and narrow size distributions. The resulting binary superstructures have been imaged by small- and wide-angle X-ray diffraction (XRD), and by transmission electron microscopy (TEM). The combined use of such investigation techniques allowed retrieval of crystalline structure, size, and shape of the PbS NCs, along with their spatial arrangement in the 3D architecture. A detailed analysis of the wide-angle XRD data, based on the Debye approach, demonstrated an elongated shape of NCs even smaller than 2 nm and provided a lower limit for the effective NC size, to be compared with results from TEM. The careful interpretation of small-angle XRD data demonstrated the ordered arrangement of NCs perpendicularly to the substrate plane and, together with TEM observations, allowed retrieval of the 3D structure of the assembly. Moreover small-angle XRD is shown to contain peculiar features related to the size distribution of the NCs and the degree of order in the assembly. Such a highly detailed structural analysis, averaged over large volumes of the investigated material, can hardly be obtained even by sophisticated high-resolution TEM.

SUNBIM (Supramolecular & SUbmolecular Nano & Bio Materials X-ray IMaging Project) is a suite of integrated programs developed, in collaboration with Rigaku Innovative Technologies, to treat Small and Wide Angle X-ray Scattering data, collected either in transmission geometry (SAXS/WAXS) or in reflection geometry (GISAXS/GIWAXS). In addition, a specific routine to collect and analyze data in SAXS scanning transmission microscopy has been developed as additional tool to investigate tissues or material science samples through a focused X-ray beam which is used to raster scan a specimen while acquiring SAXS scattering patterns with a 2D detector. Indeed, a first-generation-synchrotron-class FrE+ SuperBright Rigaku microsource, coupled to a three pinhole S-MAX3000 camera, was recently installed at the X-ray MicroImaging Laboratory (XMI-L@b) and used with success in SAXS/WAXS/GISAXS/GIWAXS experiments (De Caro et al, 2012; 2013)and for SAXS scanning microscopy (Altamura et al, 2012; Giannini et al, 2013).

SUNBIM (supramolecular and submolecular nano- and biomaterials X-rayimaging) is a suite of integrated programs which, through a user-friendlygraphical user interface, are optimized to perform the following: (i) q-scalecalibration and two-dimensional ! one-dimensional folding on small- andwide-angle X-ray scattering (SAXS/WAXS) and grazing-incidence SAXS/WAXS (GISAXS/GIWAXS) data, also including possible eccentricity correctionsfor WAXS/GIWAXS data; (ii) background evaluation and subtraction,denoising, and deconvolution of the primary beam angular divergence onSAXS/GISAXS profiles; (iii) indexing of two-dimensional GISAXS frames andextraction of one-dimensional GISAXS profiles along specific cuts; (iv) scanningmicroscopy in absorption and SAXS contrast. The latter includes collection oftransmission and SAXS data, respectively, in a mesh across a mm2 area,organization of the as-collected data into a single composite image oftransmission values or two-dimensional SAXS frames, analysis of the composeddata to derive the absorption map and/or the spatial distribution, andorientation of nanoscale structures over the scanned area.

The progress of tomographic coherent diffractive imaging with hard X-rays at the ID10 beamline of the European Synchrotron Radiation Facility is presented. The performance of the instrument is demonstrated by imaging a cluster of Fe2P magnetic nanorods at 59 nm 3D resolution by phasing a diffraction volume measured at 8 keV photon energy. The result obtained shows progress in three-dimensional imaging of non-crystalline samples in air with hard X-rays.

The Turin Shroud is traditionally considered the burial cloth of Jesus Christ, but carbon-14 analysis indicated a medieval date. Here, a digital restoring of the hands' region of the Turin Shroud image has allowed to visualize anatomic details never seen before: the scrotum and part of the right hand's thumb. Additionally, the unnatural position of the right hand's thumb, adjacent to the palm of the hand, positioned below it and, consequently, almost fully hidden except for its protruding end, seems to denote a stress, which could be consequent to crucifixion. These results shed new light on the long-lasting scientific debate about the authenticity of the relic since the absence of the thumbs has been considered as one of the most important indirect proof that the Turin Shroud wrapped the body of a man who was crucified alive. (C) 2016 Elsevier Masson SAS. All rights reserved.

During recent decades innovative nanomaterials have been extensively studied, aiming at both investigating the structure-property relationship and discovering new properties, in order to achieve relevant improvements in current state-of-the art materials. Lately, controlled growth and/or assembly of nanostructures into hierarchical and complex architectures have played a key role in engineering novel functionalized materials. Since the structural characterization of such materials is a fundamental step, here we discuss X-ray scattering/diffraction techniques to analyze inorganic nanomaterials under different conditions: dispersed in solutions, dried in powders, embedded in matrix, and deposited onto surfaces or underneath them.

A first-generation-synchrotron-class X-ray laboratory microsource, coupled to a three-pinhole camera, is presented. It allows (i) small- and wide-angle X-ray scattering images to be acquired simultaneously, and (ii) scanning small- and wide-angle X-ray scattering microscopy to be carried out. As representative applications, the structural complexity of a biological natural material (human bone biopsy) and of a metamaterial (colloidal nanocrystal assembly) are inspected at different length scales, studying the atomic/molecular ordering by (grazing-incidence) wide-angle X-ray scattering and the morphological/structural conformation by (grazing-incidence) small-angle X-ray scattering. In particular, the grazing-incidence measurement geometries are needed for inspecting materials lying on top of surfaces or buried underneath surfaces.