Bollettino della Comunità Scientifica in Australasia. Ambasciata d Italia CANBERRA. Agosto 2006

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1 Trieste - Melbourne cooperation in advanced imaging with synchrotron radiation Kaulich B.1, Kiskinova M.1, Mancini L.1, Menk R.H.1, Rigon L.1,2, Tuniz C.2, Tromba G.1, Wilkins S.W.3, Zanini F.1 The International Centre for Theoretical Physics (ICTP) in Trieste and Sincrotrone Trieste, together with the ARC Centre of Excellence in Coherent X-Ray Science based in Melbourne (involving Universities of Melbourne, Monash, Swinburne & La Trobe as well as the Commonwealth Scientific and Industrial Research Organisation, CSIRO), are establishing an International Consortium for Coherent Diffractive X-ray Imaging (I<CCDX>I) at ICTP. The Consortium will support and promote international cooperation in synergy to current ICTP programs, particularly those related to applied physics and condensed matter. It will focus on areas opening new frontiers of research in (1) Coherent diffractive imaging (CDI); (2) All methods of X-ray phase-contrast imaging and microscopy; (3) Related methods of tomography; (4) Full-field and related scanning X-ray microscopy (including soft X-ray); (5) 2D and 3D quantitative elemental mapping using X-ray fluorescence induced by a scanning micron size beam (μxrf); (6) Related fundamental physics aspects; (7) Related X-ray optics and instrument development such as detectors; (8) Associated software development and sharing; (9) Access to major imaging facilities and data processing facilities via remote access. Absorption contrast has been the principal X-ray imaging mode for over 100 years, and only recently has considerable progress been made in developing and implementing novel methods of X-ray imaging based on phase contrast, thanks to the high brightness and high level of coherence of 3rd generation synchrotron sources, the development of high performance microfocus sources and the development of novel x-ray detectors. Several phase-sensitive imaging approaches have been employed and tested in the last decades, such as differential phase and interference contrast, diffraction enhanced contrast, interferometric techniques, phase retrieval techniques etc. (Fitzgerald, 2000). Such techniques are expected to become greatly aided and expanded by the availability of X-ray free-electron lasers (XFELs), also called 4th generation sources, in the near future. A simple case is afforded by the propagation-based phase-contrast imaging (PB-PCI), see Snigirev et al. 1995; Wilkins et al. 1996, and Cloetens et al If the source transverse spatial coherence is high enough, free-space propagation transforms the phase modulation of the transmitted beam into an amplitude modulation on the detector. According to the choice of the sample-to-detector distance d (typically ranging from a few centimeters up to a few meters) with respect to the size a of the feature to be identified, one may discriminate between two different regimes: the edge-detection regime (d << a2/λ, where λ is the X-ray wavelength) and the holography regime (d a2/λ) (Cloetens et al. 1997). The former enhances the edges of the sample, improving the image contrast and can benefit from application of phase retrieval techniques to give quantitative information (Nugent et al, 1996). Fig. 1 shows an example with a nylon air-bubble wrap imaged using; a) conventional (absorption-based) imaging and b) PB-PCI. In the holographic regime the edges are modulated so strongly that the image cannot be interpreted directly, but a precise map of the phase shift can be obtained by use of phase retrieval algorithms. Figure 1 Images of a nylon air bubble wrap in: a) conventional (absorption) X-ray imaging and b) phase contrast imaging, edge detection regime. The edge-enhancement in b) allows the visualization of details not visible in a). 12

2 So-called Diffraction Enhanced Imaging (DEI) or Analyzer-Based phase-contrast imaging (AB-PCI) is based on the use of a perfect crystal analyser crystal placed between the sample and the imaging detector (Ingal and Beliaevskaya 1995, Davis et al 1995, Chapman et al. 1997). The analyser acts as an angular filter, selectively accepting or rejecting the photons deviated in the sample at very small angles. Thus, in addition to X-ray absorption, also refraction and ultra-small angle scattering (which continuously evolves from refraction) may be exploited for imaging. Fig. 2 shows a set of three DEI images of a dandelion (taraxacum officinale). They were collected with three different analyzer settings, collecting mostly: a) very-small-angle scattering; b) refraction, and c) absorption and extinction (i.e. rejection of very small angle scattering) signal. Figure 2 Images of a dandelion (taraxacum officinale) collected with different analyzer settings (see text). Other phase contrast techniques applied for X-ray microscopy require special detectors and/or special tailoring optics (Kaulich et al. 2002; Wilhein et al. 2001; Di Fabrizio et al. 2003; Morrison et al. 1998). Fig. 3 shows one example of differential phase contrast. The images were taken with the TwinMic station at ELETTRA using a configured EMCCD camera, which allows simultaneous acquisition of brightfield images and a center of gravity differential phase contrast images (Kaulich et al. 2006). Figure 3: Marine planktonic diatom Coscinodiscus sp., encased in an intricately patterned pillbox-like skeleton of amorphous biosilicate. The ornate of the biosilicate shell consisting of a double hexagonal layer are observed. The brightfield image (left) and the differential phase contrast image (right) are acquired simultaneously. Photon energy: 718 ev. Dwell time per pixel: 80 ms. In X-ray computed micro-tomography (µ-ct) the sample is rotated in front of the detector, and several different projections are acquired. A 3D image is then reconstructed by back-projecting the profiles collected in this way with specific mathematical recipes. As for planar imaging, µ-ct can be performed both in absorption or phase-sensitive modality (in edge detection or in holography regime), depending on the sample-to-detector distance d. An example of phase sensitive µ-ct (edge detection regime) of polystyrene can be seen in figure 4. Of note is that both macro- and micro-structures are visualized, even if the absorption of polystyrene is negligible, due to edge enhancement. 13

3 Figure 4 Phase sensitive micro tomographic volume reconstructions of polystyrene foam, obtained at 10 kev, d=18 cm with a 14 micron pixel size. Left: reconstruction from 33 slices. Right: reconstruction from 199 slices. Moreover, three-dimensional elemental imaging can be obtained by combining microtomography with x-ray fluorescence induced by a scanning micron size beam (μxrf) (Tuniz et al. 1990). An example is given in figure 5, where the Uranium (U) and Plutonium (Pu) distributions in a hot particle are mapped. Figure 5 Example of 3D elemental imaging using XRF μct. (courtesy of D. Wegrzynek, A. Markowicz, E. Chinea-Cano, S. Bamford, M. Bogovac, Seibersdorf IAEA Laboratories). The main advantages of phase-sensitive X-ray imaging techniques are basically three : (i) new and improved contrast, (ii) the applied X-ray dose may be reduced dramatically, and (iii) the exposure time (and hence radiation damage) is less, because the phase shift cross-section dominates the absorption cross-section (Sayre et al. 1995). One exciting new area of activity in phase-sensitive X-ray imaging which is making rapid progress is that of Coherent Diffractive Imaging and which relies on the inversion of far-field (diffraction) data to obtain high spatial resolution structural information on non-periodic objects. The original idea and approach was due to Sayre (1980). More recently important new demonstrations of this technique have been obtained e.g. by Miao et al (1999), Shapiro et al (2005) and Quiney et al (2006). The technique of CDI offers the opportunity for very high spatial resolution structure determination of non-periodic objects, not limited by the need for 14

4 corresponding high resolution X-ray optics. A major goal of various consortia recently established around the world, including those linked to the I<CCDX>I is to push these techniques to molecular and ultimately atomic resolution. Key frontier challenges here are problems such as the determination of the structure of membrane proteins in their functional form in situ. Several areas of materials science, medicine, biology, environmental science, food science, geology, archaeology etc have already benefited from applying phase contrast imaging techniques. At ELETTRA, important results have been obtained studying shape memory alloys (Besseghini et al. 2004), highperformance sail fabrics (Tesei et al. 2005a), endodontic obturations (Contardo et al. 2005), oral implants (Tesei et al. 2005b), bone and cartilage in healthy and arthritic joints (Majumdar et al. 2004, Muehleman et al. 2004), mammography (Arfelli et al. 2000), anatomy and embryology of insects (Hönnicke et al. 2005), metal intake in plants (Kaiser et al. 2005), bread porous structure (Falcone et al. 2004), detection of microdiamonds in kimberlitic rocks (Schena et al. 2005), environmental marine and soil samples (Kaulich et al. 2006, Thieme et al. 2006), archaeological glasses (Gerlach et al. 2003) and other archeometric investigations (Zanini et al 2006). In mid-march 2006, the first clinical mammography studies using SR and involving phase-contrast were carried out at the SYRMEP beamline at ELETTRA. The ICCDXI aims at fostering international cooperation and understanding in the area, for instance promoting image processing software development, evaluation and sharing among members; supporting research into fundamental aspects of CDI and on advanced X-ray detectors and X-ray optics; pursuing funding opportunities in connection with consortium members who are eligible and wish to combine together on such proposals; running conferences, workshops and training courses. Moreover, the Consortium will especially promote and support opportunities for the involvement of people from developing countries, both via remote access to advanced X-ray imaging techniques and facilities, and supporting them for extended study visits at ICTP. Scientists from Developing Countries will also benefit through schools and courses in advanced imaging, including experimental activities at the ICTP Laboratory and at ELETTRA. In particular, India and Brazil are developing capabilities in advanced imaging with synchrotron radiation and, with the support of the proposed Consortium, could act as regional resource centres for less developed countries. An imaging beamline is also being planned for SESAME, the synchrotron facility being built in Jordan with the support of UNESCO and of the European Union. The second international meeting on this topic will be held in Trieste on May 20-22, focusing on the performance required from future imaging systems to solve critical problems in life and material sciences. New funding sources for this enterprise are being identified. References: Arfelli F. et al., Radiology, 215 (2000) Besseghini S. et al., Mat. Sci. Eng. A 378 (2004) 125 Chapman D. et al., Phys. Med. Biol. 42 (1997) Cloetens, P. Barrett, R. Baruchel, J. Guigay, J-P and Schlenker,M. J.Phys.D: Appl.Phys. 29, (1996). Cloetens P. et al., J. Appl. Phys. 81 (1997) Contardo L. et al., Nucl. Instrum. and Meth. A 548 (2005) Davis T. J. et al., Nature 373 (1995) Di Fabrizio E. et al., Microelectron. Eng (2003) 87 Falcone P. M. et al., Journal of Food Science 69 (2004) FEP38-FEP43 Fitzgerald R., Phys. Today 53 (2000) Gerlach S. et al., Elettra Highlights (2003) Hönnicke M. G. Et al., Nucl. Instrum. and Meth. A 548 (2005) Kaiser J. et al., European Physical Journal D 32 (2005) Kaulich B. et al., J. Opt. Soc. Am 19 (2002) Kaulich B. et al., IPAP Conf. Series (2006) in press Ingal V.N. and Beliaevskaya E. A., J. Phys. D: Appl. Phys. 28 (1995) Majumdar S. et al., Eur Radiol. 14 (2004) Miao, J. et al Nature 400 (1999) Morrison G. R. et al., in X-ray microscopy and spectromicroscopy, J. Thieme, G. Schmahl, D. Rudolph, and E. Umbach, eds. (Springer Verlag Berlin, 1998), pp. I-85-I-94 Muehleman C. et al., Osteoarthr. Cartilage, 12 (2004) Nugent, K.A. et al, Phys. Rev. Letts. 77, (1996) Quiney, H.M. et al Nature Physics, 2 (2006), Sayre, D. in Imaging Processes and Coherence in Physics (eds Schlenker, J. et al) (Springer, Berlin 1980). Sayre D. et al., Ultramicroscopy 2 (1995)

5 Schena G. et al., International Journal of Mineral Processing 75 (2005) Shapiro, D. et al (2005) Proc. Natl. Acad. sci. 102, Snigirev A. et al., Rev. Sci. Instrum. 66 (1995) Tesei L. et al., Advanced Engineering Materials 7 (2005a) Tesei L. et al., Nucl. Instrum. and Meth. A 548 (2005b) Thieme J. et al., Syn. Rad. News, (2006) in press Tuniz C. et al., Nucl. Instrum. and Meth. B 50 (1990) Wilhein T. et al., Appl. Phys. Lett. 78 (2001) 2082 Wilkins S. W. et al., Nature 384 (1996) Zanini F. et al., J. Neutron Res. (2006) in press Kaulich B. 1, Kiskinova M. 1, Mancini L. 1, Menk R.H. 1, Rigon L. 1,2,, Tuniz C. 2, Tromba G. 1, Wilkins S.W. 3, Zanini F Sincrotrone Trieste, Trieste, Italy 2. The Abdus Salam International Centre for Theoretical Physics, Trieste, Italy 3. Commonwealth Scientific and Industrial Research Organisation, Melbourne, Australia Original manuscript in English 16

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