LABEC, the INFN ion beam laboratory of nuclear techniques for environment and cultural heritage.

The LABEC laboratory, the INFN ion beam laboratory of nuclear techniques for environment and cultural heritage, located in the Scientific and Technological Campus of the University of Florence in Sesto Fiorentino, started its operational activities in 2004, after INFN decided in 2001 to provide our applied nuclear physics group with a large laboratory dedicated to applications of accelerator-related analytical techniques, based on a new 3 MV Tandetron accelerator. The new accelerator greatly improved the performance of existing Ion Beam Analysis (IBA) applications (for which we were using since the 1980s an old single-ended Van de Graaff accelerator) and in addition allowed to start a novel activity of Accelerator Mass Spectrometry (AMS), in particular for 14C dating. Switching between IBA and AMS operation became very easy and fast, which allowed us high flexibility in programming the activities, mainly focused on studies of cultural heritage and atmospheric aerosol composition, but including also applications to biology, geology, material science and forensics, ion implantation, tests of radiation damage to components, detector performance tests and low-energy nuclear physics. This paper describes the facilities presently available in the LABEC laboratory, their technical features and some success stories of recent applications.

Refractive index variation in a free-standing diamond thin film induced by irradiation with fully transmitted high-energy protons.

Ion irradiation is a widely employed tool to fabricate diamond micro- and nano-structures for applications in integrated photonics and quantum optics. In this context, it is essential to accurately assess the effect of ion-induced damage on the variation of the refractive index of the material, both to control the side effects in the fabrication process and possibly finely tune such variations. Several partially contradictory accounts have been provided on the effect of the ion irradiation on the refractive index of single crystal diamond. These discrepancies may be attributable to the fact that in all cases the ions are implanted in the bulk of the material, thus inducing a series of concurrent effects (volume expansion, stress, doping, etc.). Here we report the systematic characterization of the refractive index variations occurring in a 38 µm thin artificial diamond sample upon irradiation with high-energy (3 MeV and 5 MeV) protons. In this configuration the ions are fully transmitted through the sample, while inducing an almost uniform damage profile with depth. Therefore, our findings conclusively identify and accurately quantify the change in the material polarizability as a function of ion beam damage as the primary cause for the modification of its refractive index.

Complex refractive index variation in proton-damaged diamond.

An accurate control of the optical properties of single crystal diamond during microfabrication processes such as ion implantation plays a crucial role in the engineering of integrated photonic devices. In this work we present a systematic study of the variation of both real and imaginary parts of the refractive index of single crystal diamond, when damaged with 2 and 3 MeV protons at low-medium fluences (range: 10(15) - 10(17) cm(-2)). After implanting in 125 × 125 µm(2) areas with a scanning ion microbeam, the variation of optical pathlength of the implanted regions was measured with laser interferometric microscopy, while their optical transmission was studied using a spectrometric set-up with micrometric spatial resolution. On the basis of a model taking into account the strongly non-uniform damage profile in the bulk sample, the variation of the complex refractive index as a function of damage density was evaluated.

Iterative retrieval of one-dimensional x ray wave field using a single intensity measurement.

The problem of retrieving a complex function from the modulus of its Fourier transform has non-unique solutions in one dimension. Therefore iterative phase retrieval methods cannot in general be confidently applied to one-dimensional problems, due to the presence of ambiguities. We present a method for a posteriori reduction of the ambiguities based on the correlation analysis of the solution of a large number of runs of an iterative phase retrieval algorithm with different random starting phases. The method is applied to experimentally measured diffraction patterns from an x ray waveguide illuminated by hard x rays. We demonstrate the possibility of retrieving the complex wave field at the exit face of the waveguide and compare the result with theoretical prediction.

Early stage mineralization in tissue engineering mapped by high resolution X-ray microdiffraction.

The specific routes of biomineralization in nature are here explored using a tissue engineering approach in which bone is formed in porous ceramic constructs seeded with bone marrow stromal cells and implanted in vivo. Unlike previous studies this model system reproduces mammalian bone formation, here investigated at high temporal resolution. Different mineralization stages were monitored at different distances from the scaffold interface so that their spatial analysis corresponded to temporal monitoring of the bone growth and mineralization processes. The micrometer spatial resolution achieved by our diffraction technique ensured highly accurate reconstruction of the different temporal mineralization steps and provided some hints to the challenging issue of the mineral deposit first formed at the organic-mineral interface. Our results indicated that in the first stage of biomineralization organic tissue provides bioavailable calcium and phosphate ions, ensuring a constant reservoir of amorphous calcium phosphate (ACP) during hydroxyapatite (HA) nanocrystal formation. In this regard we suggest a new role of ACP in HA formation, with a continuous organic-mineral transition assisted by a dynamic pool of ACP. After HA nanocrystals formed, the scaffold and collagen act as templates for nanocrystal arrangement on the microscopic and nanometric scales, respectively.

Evidence of light guiding in ion-implanted diamond.

We demonstrate the feasibility of fabricating light-waveguiding microstructures in bulk single-crystal diamond by means of direct ion implantation with a scanning microbeam, resulting in the modulation of the refractive index of the ion-beam damaged crystal. Direct evidence of waveguiding through such buried microchannels is obtained with a phase-shift micro-interferometric method allowing the study of the multimodal structure of the propagating electromagnetic field. The possibility of defining optical and photonic structures by direct ion writing opens a range of new possibilities in the design of quantum-optical devices in bulk single-crystal diamond.

Bulk and interface investigations of scaffolds and tissue-engineered bones by X-ray microtomography and X-ray microdiffraction.

This review is presented of recent investigations concerning the structure of ceramic scaffolds and tissue-engineered bones and focused on two techniques based on X-ray radiation, namely microtomography (microCT) and microdiffraction. Bulk 3D information, with micro-resolution, is mainly obtained by microCT, whereas microdiffraction provides useful information on interfaces to the atomic scale, i.e. of the order of the nanometer. Since most of the reported results were obtained using synchrotron radiation, a brief description of the European Synchrotron Radiation Facility (ESRF) is presented, followed by a description of the two techniques. Then examples of microstructural investigations of scaffolds are reported together with studies on bone architecture. Finally, studies on ex vivo tissue-engineered bone and on bone microstructure in vivo are presented.

Wave-field formation in a hollow x-ray waveguide.

Diffraction and refraction phenomena at the entrance of a hollow x-ray waveguide with weakly absorbing dielectric cladding layers are investigated using two independent approaches: (a) analytical and (b) numerical solutions of the wave equation in the paraxial (parabolic) approximation. It is shown that the wave penetrating through the cladding material substantially modifies the wave field near the waveguide entrance. It results in a significant increase of the total energy flux inside the guiding layer and in additional spatial modulation of the electromagnetic field.

Improvements in CVD diamond properties for radiotherapy dosimetry.

The goal of this work was to compare the behaviour of a chemical vapour deposited (CVD) diamond sample, grown at the University of Florence using a local procedure, with that of a commercial CVD diamond. The comparison was performed exposing both systems to 25 MV photons and measuring the current response during irradiation. Properties of dosimetric interest such as stability of response, dose rate dependence and rise time were investigated. After a preliminary study, which evidenced better performances of the commercial device with respect to the local CVD diamond, the latter was irradiated with a high fluence of fast neutrons. As a result of the neutron treatment, the quality of the CVD home-made diamond has been improved to match with that of the commercial dosemeter.

Dispersion properties of x-ray waveguides.

We study the propagation of ultrashort pulses in x-ray waveguides (WGs) by addressing the problem of the temporal dispersion. Starting from basic equations, by means of numerical calculation we demonstrate that far from the absorption edges of the WGs the cladding's material dispersion is negligible. However, close to the absorption edge significant dispersion can take place. This behavior could in principle be exploited to manipulate incoming chirped beams. Moreover, using the two coherent beams produced by the WG in the second (and higher) order of resonance suggests the use of the WC as a dispersion-free beam splitter, which can facilitate x-ray pump-probe experiments in the femtosecond temporal range without the need for external sources.

Engineered bone from bone marrow stromal cells: a structural study by an advanced x-ray microdiffraction technique.

The mechanism of mineralized matrix deposition was studied in a tissue engineering approach in which bone tissue is formed when porous ceramic constructs are loaded with bone marrow stromal cells and implanted in vivo. We investigated the local interaction between the mineral crystals of the engineered bone and the biomaterial by means of microdiffraction, using a set-up based on an x-ray waveguide. We demonstrated that the newly formed bone is well organized inside the scaffold pore, following the growth model of natural bone. Combining wide angle (WAXS) and small angle (SAXS) x-ray scattering with high spatial resolution, we were able to determine the orientation of the crystallographic c-axis inside the bone crystals, and the orientation of the mineral crystals and collagen micro-fibrils with respect to the scaffold. In this work we analysed six samples and for each of them two pores were studied in detail. Similar results were obtained in all cases but we report here only the most significant sample.

Large-distance refocusing of a submicrometre beam from an X-ray waveguide.

Among the several available X-ray optics for synchrotron radiation producing micrometre and submicrometre beams with high intensity, the X-ray waveguide (WG) can provide the smallest hard X-ray beam in one direction. A drawback of this optics is that, owing to the divergence at the exit, a nanometre-sized spot on the sample can only be obtained if this is within a few micrometres of the WG exit. Another limitation is that in planar WGs the beam is compressed in only one direction. Here, using a dynamically bent elliptical Si/Pt mirror, the guided X-ray beam has been refocused at approximately 1 m from the waveguide exit. The large working distance between the device and the submicrometre focus leaves some space for sample environment (vacuum chamber, furnace, cryostat, magnets, high-pressure device etc.) and allows cross-coupled geometries with two WGs for efficient compression in two directions.

X-ray micro-diffraction analysis of reconstructed bone at Zr prosthetic surface with sub-micrometre spatial resolution.

The purpose of the present investigation is to demonstrate the power of the x-ray micro-diffraction technique in biological studies. In particular the reported experiment concerns the study of the interface between a Zr prosthetic device implanted in a rat femur and the newly-formed bone, with a spatial resolution of 0.5 microm. The obtained results give interesting information on the Zr deformation and on the crystallographic phase, the grain size and the orientation of the new bone. Moreover the study reveals a marked difference in the structure of the reconstructed bone with respect to the native bone, which cannot be appreciated with other techniques.

Non-destructive determination of local strain with 100-nanometre spatial resolution

Structure sizes of approximately 180 nm are now standard in microelectronics, and state-of-the-art fabrication techniques can reduce these to just a few tens of nanometres. But at these length scales, the strain induced at interfaces can locally distort the crystal lattice, which may in turn affect device performance in an unpredictable way. A means of non-destructively characterizing such strain fields with high spatial resolution and sensitivity is therefore highly desirable. One approach is to use Raman spectroscopy, but this is limited by the intrinsic approximately 0.5-microm resolution limit of visible light probes. Techniques based on electron-beam diffraction can achieve the desired nanometre-scale resolution. But either they require complex sample preparation procedures (which may alter the original strain field) or they are sensitive to distortional (but not dilational) strain within only the top few tens of nanometres of the sample surface. X-rays, on the other hand, have a much greater penetration depth, but have not hitherto achieved strain analysis with sub-micrometre resolution. Here we describe a magnifying diffraction imaging procedure for X-rays which achieves a spatial resolution of 100nm in one dimension and a sensitivity of 10(-4) for relative lattice variations. We demonstrate the suitability of this procedure for strain analysis by measuring the strain depth profiles beneath oxidized lines on silicon crystals.

Submicrometre resolution phase-contrast radiography with the beam from an X-ray waveguide.

Experimental data with unprecedented submicrometre resolution obtained in a phase-contrast radiography experiment in a magnifying configuration are presented. The term 'phase contrast' here indicates that the phase retardation of coherent light in matter was utilized as the contrast mechanism. The coherent and divergent beam exiting an X-ray waveguide was used in a lensless configuration to magnify spatial variations in optical path length up to several hundred times. The defocused image of a nylon fibre was measured with a resolution of 0.14 micro m at the object. Sufficient contrast was found for exposure times of 0.1 s, i.e. in the regime for real-time studies.

Submicrometre beams from a hard X-ray waveguide at a third-generation synchrotron radiation source.

The use of an X-ray waveguide for scattering experiments at an undulator of a third-generation synchrotron radiation source is discussed. The performance with a perfect crystal monochromator, multilayer monochromator and focusing mirror is explored. A maximum flux of 8 x 109 photons s(-1) at lambda = 0.083 nm was obtained for a 0.15 (V) x 600 (H) micron(2) beam at the exit of the waveguide with a multilayer monochromator. The combination of an Si (111) monochromator and ellipsoidal mirror resulted in a flux of approximately 10(9) photons s(-1) but with a horizontal compression of the beam to approximately 30 micron. The use of the waveguide in diffraction experiments is addressed.