Synchrotron radiation imaging and diffraction for industrial applications

Europhysics News, Jul 2018

José Baruchel, Åke Kvick

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Synchrotron radiation imaging and diffraction for industrial applications

Synchrotron radiation imaging and diffraction for industrial applications Jose Baruchel 0 Ake Kvick ESRF 0 Grenoble 0 France 0 0 About the author Massimo Altarelli was trained at the University of Rome as a con­ densed matter theorist. At the ESRF in Grenoble, he was Research Director (1987-1993), and Head ofthe Theory Group (1994-1998). Since 1999 he has been in Trieste on the staff of the International Centre for Theoretical Physics, and Director of the Elettra Syn­ chrotron Light Source ious laboratories around the world. Clearly the technical difficulties connected with the requirements on the quality of the electron bunches (emittance, peak current, etc.) grow dramatically as the required wavelength decreases towards the range of the hard xrays. In the pursuit of the higher brilliance of fourth generation sources there is an alternative road to the Linac FEes. This is the approach based on recirculating Linacs, as exemplified by the 4GLS ("4th Generation Light Source") project being designed at Daresbury Laboratory in the UK. The idea is to combine the "few passes" strategy to lower emittance with the advantage of the ring geometry in which a large number of tangential beam lines and experimental stations can be exploited by users in parallel. It consists of a Linac that feeds electrons into one or several arc-shaped sections on which undulators, wigglers and even FEes can be inserted (Fig. 4). At the end of the (last) arc, electrons are either dumped or fed back into the Linac, where they can return part of their energy to the RF fields in the accelerating cavities (this latter version is called "energy-recovery Linac"). The Linac is preferably of the superconducting type, one of the reasons being that it can support a much higher repetition rate (a much smaller time mterval between successive bunches). - [2] See http://www-ssrl.slac.stanford.eduljhhorne.htrnlforashort description of the state of the project he use of the modern synchrotron radiation (SR) sources for T X-ray imaging and diffraction provides new possibilities for applied science and technology. They include an enhanced resolu­ tion (spatial and/or temporal), the possible use of the coherence of the beam, in-situ experiments and accurate quantitative measure­ ments of local density or strain. Selected applications showing the improved capabilities in absorption or phase microtomography, time-resolved diffraction experiments showing the way a lithium­ based battery works, or strain measurements on stir-welding materials, are presented as examples. The combination of diffrac­ tion and imaging (i.e. diffraction with micron spatial resolution) allows further applications, such as the study of grain growth, or the X-ray topographic investigation of defects responsible for spu­ rious modes in single crystal resonators. The aim of the present paper is to highlight the contribution of synchrotron radiation X-ray imaging and diffraction to the inves­ tigation of industrial topics. These techniques, which allow the visualization of the volume of systems opaque for other probes and the determination of their structure, have been dramatically renewed by the use of modern, "third generation" , synchrotron radiation (SR) facilities beams. Real timelhigh-resolution experi­ ments are performed for both X-ray imaging and diffraction. The high energy of the available beams allows the deformation within bulk materials to be investigated. The high coherence of the beam allows phase contrast imaging to be exploited, the contrast arising from phase variations across the transmitted beam. Absorption and phase microtomography provide three-dimensional informa­ tion on features like cracks, porosities or inclusions, which are of high interest for applied topics such as metallurgy, polymers, or reservoir rocks containing fuel. The spatial resolution of these tech­ niques is now in the 1 flm range. Lastly the combination of diffraction and imaging, through the new tracking techniques, or the use of Bragg diffraction imaging (X-ray topography) provides additional information on industrially interesting materials. <Ol Fig. 1: 3D image of the distribution of holes (in white) within a copper target (transparent), 269*284*201 pixels, 2 J.lm voxel size so a b c 4 Fig. 2: Reconstruction of an open-cell flexible polyurethane foam at several levels of compressive strain. (a) 0%, (b) 10%, (c) 23%, these percentages being the ratio ofthe variation of vertical length of the foam over the original, unstrained, length.The 30 renditions represent volumes of 7mm x 7mm x 1.4 mm. The original features of third generation synchrotron radiation facilities such as the APS, ESRF, or Spring 8, for imaging and dif­ fraction applications, are: a) the very high intensity of the X-ray beam (factor 106 with respect to usual X-ray generators); both white and monochro­ matic beams can be used b) the availability of photons spanning the whole range from the infrared to hard X-rays (up to 300-400 keV) c) the design ofbeamlines optimised for a given set of techniques d) the small size of the electron beam cross-section « 100 Jlm), which leads to high brilliance, and to a sizeable lateral coherence of the X-ray beam. Absorption and phase microtomography The principle of microtomography is very similar to that of the well-known medical scanner. When applied to materials investi­ gation, it consists in recording a series of radiographs (typically of the order of 1000) for different angular positions of the sample, which rotates around an axis perpendicular to the beam. Several laboratory microtomographs have been commercially produced over the last years (Riiegsegger et al., 1996, Sasov and Van Dyck, 1998) . But the best images, in terms of spatial resolution, signal­ to-noise ratio and quantitative exploitation, are obtained using synchrotron radiation. This results from the high intensity, practi­ cally parallel and monochromatic incoming beam. In this approach there is no image magnification, and the spatial resolu­ tion mainly results from the effective pixel size of the detector. The range of pixel sizes available at the ESRF goes from 0.3 Jlffi to 30 !lm, and a big effort is being produced to enhance the spatial reso­ lution down to the 100 nm range. The total acquisition time is in the 10-2 ("fast tomography") to1 hour range, and the recorded data is often several Gigabytes. An increasing number of applied or industrial research labora­ tories require the use of microtomography to solve some of the problems they encounter. To achieve this requirement they either buy beamtime and expertise, or have access to the synchrotron facilities through collaboration with Universities or research groups and peer-reviewed proposals. The industrial requirements include, most of the time, confidentiality, rapid access and full ser­ vice. Most facilities, and in particular the ESRF, propose such a service, going from the experiment to the data analysis (volume .reconstruction, extraction of relevant parameters ... ). Figure 1 is an example of such application-oriented investigation. A strong impact on a copper target creates porosity within the bulk metal. The investigation of the pore sizes and distribution is of high importance for applications. The only way to image these pores inside such a sample is X-ray microtomography (Bontaz-Carion et al., 2001) . The spatial distribution of pores within one of these copper samples was determined (figure 1), and shown to be less homogeneous, both from the point of view of size and oflocation, than what was expected from theoretical models. Another example of absorption tomography, which implies a specially designed sample environment cell, is the in-situ investiga­ tion of an open-cell polyurethane foam at several levels of compressive strain (figure 2). This work, performed by a research group from ICI Polyurethane in collaboration with a group of the University of Cambridge, correlates the macroscopic behaviour (stress/strain curve) with the local structure modifications. It shows that the initial phase of compression, which is associated with a linear elastic response, corresponds to a bending of the struts, whereas the plateau in the stress/strain curve is linked to the collapse a whole band of cells (Elliott et al., 2002). This result was known from surface observations, but no volume evidence was available. The X-ray beams produced at third generation synchrotron radiation facilities exhibit a high degree of coherence. This results from the small source size 0' (in the 50 Jlffi range) and the large source to sample distance L (in the 100 m range). The transverse coherence length de= 'A-L/2 0', is in the 100 Jlm range, and allows "phase images" to be recorded by just varying the sample-to-detec­ tor distance ("propagation technique", reviewed for instance by Cloetens et al., 1999a). The great advantage of this new type of imaging is the increased sensitivity it provides, either for light materials such as polymers, or for composites made up of materi­ als with neighbouring densities (for example AI and SiC). A first use of the phase images relies on the visualisation of the phase jumps that occur at the edges of a particle or porosity imbedded in a matrix having a different index of refraction. Phase microto­ mography based on the visualisation of the edges was used, for instance, to understand the mechanisms of degradation in AI-SiC composites. It was possible not only easily to visualize the SiC reinforcing particles, but also to observe the nucleation and prop­ agation of cracks when the material is submitted, in situ, to tensile stress. The cracks appear first in the elongated particles, and their number is 50% more than suggested by surface investigations (Buf­ fiere et al. 1999). 4 Fig. 3: Tomographic images of an AI-Si alloy, quenched from the"semi-solid" state a) Detector to sample distance D= 0.7 cm b) 0=60 cm c) "holotomographic"image, d) 3D rendering shOWing the former"liquid" phase (courtesy L. Salvo and P. C1oetens). d Phase imaging based on the detection of the edges does not allow the local phase to be extracted quantitatively, and its spatial resolution is limited by the occurrence of the fringes used to visu­ alize the borders. A more quantitative approach of phase imaging and tomography was developed. It is based on the combination of several images recorded at different distances. An algorithm, ini­ tially developed for electron microscopy by the Antwerp group, was successfully adapted to the X-ray case, and allows the "holo­ graphic" reconstruction of the local phase, well beyond the images of edges (Cloetens et al., 1999a). Once the phase maps are obtained through holographic reconstruction, there is no conceptual diffi­ culty in bringing together many maps corresponding to different orientations of the sample, and in producing the tomographic, three-dimensional, reconstruction procedure. For each of the angular positions of the sample, the phase map is retrieved using images recorded at several (typically four) distances. The highest accessible spatial frequency is determined by the resolution of the detector. This combined quantitative phase mapping and tomog­ raphy procedure, called holotomography (Cloetens et al.,1999b), provides a very useful approach to the characterization of materi­ als on the micrometer scale. The "holotomographic" procedure was applied to an AI-Si alloy; quenched from a temperature where a "mainlyAI" solid phase is surrounded by an AI-Si liquid one. This is an important indus­ trial material because in the "semi-solid" state it is possible to give a desired shape to the alloy, this shape being retained when cooled to room temperature. The density difference between the two phases is in the 1-2% range. For each angular position of the sam­ ple 4 images were recorded at different distances, yielding 3D quantitative images that show, with a voxel edge size of 1 filll' the distribution of electron density, hence of mass density, in the sam­ ple. The highest accessible spatial frequency is determined by the maximum resolution of the detector (-1-2 flm). Fig 3 compares the possibilities of absorption microtomography (fig. 3a, where the phases are indistinguishable, and only iron-rich metallic inclusions are visible) with edge-enhancement phase microtomography (fig. 3b, where the phase boundaries are outlined by a black-white line) and with holotomography (fig. 3c, where the two phases are clear­ ly observable through their grey level), and shows in 3d) a 3D rendering of what was the ''liquid'' phase. Diffraction experiments on industrially related topics The accessibility of hard penetrating X rays that can be focussed into sub micron spots while retaining extremely high probe inten­ sity has opened up the field of diffraction to industrially interesting fields. New experiments with millisecond time-resolution, sub micron spatial resolution with bulk probing capability of several tens of centimetres in high Z materials can now be performed to map out stress/strain fields, to follow reactions in real time or to study in situ processes in complex environments such as inside reaction vessels or even in working devices like batteries or other electrochemical cells. Time resolution Time-resolved studies tend to fall into three categories: the second to several minute processes, millisecond to microsecond processes and extremely fast pico-second reactions. The last category can only be studied at present by "stroboscopic" experiments were the process is repeated many times to obtain sufficient counting statis­ tics. Most industrial reactions however fall into the first two categories and are usually irreversible ruling out stroboscopic mea­ surements. The present synchrotron facilities provide sufficient x-ray flux: to perform one-shot experiments well down in time to - --_... ----- _.12 16 the microsecond regime. The 2 dimensional diffraction data is recorded by fast read-out detectors such as large CCD cameras. An example is given by the in-situ study of an electrochemical reaction experiment on a working LixCo02battery (Morcrette et al. 2002). Strong diffraction spots from higWy crystalline current col­ lectors and packaging material have in the past compromised the weaker diffraction from the material under study. In order to de­ emphasise the strong diffraction it is now possible to use micro beams and combine diffraction rapidly collected from many dif­ ferent areas. In the case of the LixCo0 2 battery 16 different orientations were collected in less than 2 secs and the pixel by pixel medians of the images collected by the CCD camera could be used to reduce the influence of the electrodes. One-dimensional powder patterns from 2 D images can thus be produced with suf­ ficient precision to obtain accurate time-resolved behaviour of the phase fractions during the working cycle of the battery. The struc­ tures of the phases that are stable only under applied voltage a ,........................""""'".......................,.............................. b • 6 1) 10 A.gIe(~) 12 lJ I~ TiC+TtH; TI+U: Ti .. '}+ltC Tj··l ... Fig. 5: (a) The diffraction pattern during the reaction between A (anatase),G (graphite) and M (magnesium).The timeresolution is 0.65 msec. (b) The diffraction patterns captured while the reaction between the metals take place.The time interval is 0.65 ms. investigated volume 50mm -950mm .... Fig.6: Schematic of the experimental setup with spiral sUt and online image plate scanner on 1015B. showed the existence of intermediate phases as well as the termi­ nallayered Co02 structure. Figure 4 gives the diffraction phases during in situ reduction of the LixCo02 battery with the different rhombohedral, monoclinic and triclinic phases indicated. The highest time-resolution for irreversible reactions so far (l0-30ms) has been obtained in the study of self-propagating high temperature synthesis (SHS). SHS is based on the characteristic of highly exothermic reactions to sustain themselves following an ini­ tiation by relatively mild conditions. These reactions typically proceed as reaction fronts with speeds of up to 25cm/sec under temperatures up to 5000e. An example is given by Contreras et al. 2004 where the production of TiC and TiB2 was studied via two routes: from elements and from oxides. The reactions were moni­ tored by 0.2601 A X rays in situ. The starting powders were compacted to cylindrical pellets and the reaction was started by external ignition at the bottom of the pellets. The X-ray beam was focused on the central part of the pellet and the reaction process was recorded as the reaction front passed the probing X-ray beam. The bulk process was followed by recording the diffraction in transmission by a CCD camera. The detailed process could be recorded and showed that the entire process took place during less than 0.1 second. The different synthesis routes produced different final microstructures that depended on the starting conditions. The particle size when pure elements were used was 10 flIll where­ as the reaction using oxides and Mg had sub-flIll microstructure. Fig. 5 gives the diffraction patterns during the critical phases of the reactions. Combined diffraction and imaging High spatial resolution The mapping of residual stresses in components is essential in pro­ viding a roadmap for future failure modes in materials and a detailed knowledge of their distribution can indicate potential alle­ viating processes, which may lengthen component lifetime and avert catastrophic failures such as fractures in railroad tracks or air­ plane turbine blades. Until recently only destructive methods or europhysics news MARCHI APRIL 2004 methods with large measuring gauges have been employed. Recent deVelopments at the high energy synchrotron facilities have now produced highly penetrating micro-focus beams with mea­ suring gauges down to -5*5*50 flm3• The experimental set-ups with CCD cameras or narrow receiving slits and micro-precision translation tables now give spatial resolution on the flm scale. High precision lattice parameters with 6.d/d -10'6 can thus be determined with the small measuring gauge and excellent spatial resolution. A recent example of a novel strain and phase-mapping technique is given by Martins et al. 2003 in their depth resolved investigation of friction stir welding. Friction stir welding is a new method for solid welding using a spinning tool forced along a joint line. This new method can overcome problems such as weld poros­ ity; use of filler materials and cracking in the heat-affected zone. In this study the bulk investigation of several mm thick AI plates was performed, and the depth resolution was obtained by a spiral slit assembly. The experimental set up is illustrated in Fig. 6 and the resulting distribution of the Si phase and the residual micro strain is given in Fig. 7 for this weld of a single phase AI alloy and an AISilOMg phase. Multi-crystal techniques The excellent spatial resolution now available opens up entirely new opportunities for studying dynamical phenomena at the mesoscopic level. Surprisingly theoretical understanding of many fundamental materials processes, such as recrystallisation and deformation, relies on models that have built in assumptions such as sample homogeneity and absence of grain-grain interactions. The new experimental facilities can now test these assumptions. An example is given by Offerman et al. 2002 in their study of grain growth following phase transformations in a steel sample. Using the spatial resolving power of the synchrotron beam it was shown a) long~udinal strain map 2000 '00l C '"C';:~~:::;:~...,-=;;'::::;;;::::;;;::::~ _ ·'000 ~ 1 ~ ~ 0 "'6 ··i5 c~lt...n_"",re(lmml b) through thickness longitudinal reSidual stress q~2Olf'','~''---'--''-;'~., ,y. , , :~ " S}'SI<,!r-..c e.m>.r. i l r],*~r: ~,--,>,_ .1 -.1 -","~~"_~A...A_~L_'_.-...-....-~; c) r....··..e~i~;~:d view for Ph~;';;;~P'''''''l 1 d - [ f: · J_ , 1.'- , ,~ 1 _"o,,! AA2Il24 .....""'9.<10_ . ~o _tro·5m_ete~._r mSml 10 "IS 1()(JlA M2G24 ... Fig. 1: (a) Depth resolved residual macrostrains in longitudinal direction (parallel to weld). (b) through thickness long.itudInal residual stress component, calculated from the strain measurements in three dimensions. (c) enlarged view of the distribution of the plate. material (AA60B2 and AA2024) in the stirring zone. ,'"' .~ .' that four different growth mechanisms were present in ferrite and these were correlated with the local environment of the grains indi­ cating that the present models are far from adequate. Fig. 8 shows the integrated intensity of 5 grains near the cube orientation shown as a function of annealing time. At present several hundred differ­ ent grains can be monitored simultaneously. This method of simultaneous determination of orientation within a bulk sample (Lauridsen et al. 2000) gives interesting access to the mesoscale. It is now possible, via tracking techniques, to map out grain bound­ aries with resolutions down to 5 flm and to follow kinetics and . dynamics of groups of individual grains during processes such as heating, torsion etc. Industrial application of Bragg diffraction imaging (X-ray topography) Figure 9 shows the image recorded using the 444 Bragg diffracted beam from a flux-grown platelet-shaped gallium-substituted yttri­ um iron garnet crystal (Y3GaxFes-xO12, with x-I, Ga-YIG). These Ga-YIG crystals are grown to produce hyper-frequency resonators. It was observed that some of these crystals exhibit spurious modes, which are very detrimental to their performance. This X-ray dif­ fraction topographic investigation was therefore performed to identify the crystal defects present on some of the resonators, pro­ duced during growth, which are responsible for these spurious modes. Many types of defects are observable on the topographs, and one of them, the dissolution bands, appeared to be the origin, through the occurrence of "closure-like" magnetic domains, of these modes. Future developments The above examples give only a few insights of possible studies of industrial phenomena using diffraction and imaging at the syn­ chrotrons. X-raymicrotomography is an invaluable tool to obtain 3D data on a large variety of materials. The use of modern synchrotron radi­ ation sources opens up new possibilities, with "fast tomography" to investigate the evolution of a system when varying an external para­ meter (time, temperature, stress, etc.) and/or improved spatial resolution, going down to the 100 nm range. In addition phase images reveal phenomena hardly visible by other means. Other areas include the rapidly expanding field ofhigh-pressure diffraction where micro- focussed beams and laser-heating capa­ bilities open up new experimental routes to studies of synthesis ~ fOAl •.5 j. ~ c ~ 3.5 S ~o 3 I 25 e .!'; 2 2> ~~ 1.5 .s ." ~ ~ I 0.5 0 ·20 .. Fig. 8:The integrated intensity of five grains near the cube in steel as a function of annealing time '" ~Topograph of a flux grown Ga-YIG crystal. and equation of states under non-ambient conditions such as megabars of pressure and several thousands of degrees of temper­ ature. High-resolution powder diffraction is advancing rapidly and ab initio structure determinations ofvery large structures can now be performed on materials, which cannot be obtained as single crystals. The current trend in instrumentation development will in the near future give access to nanometre size beams. This leads to another type of image through the use of X-ray microbeam-based scanning imaging approaches, probing for instance the fluores­ cence or the absorption near absorption edges. The diffraction experiments will more and more be combined with complemen­ tary techniques such as imaging or Raman spectroscopy, by performing simultaneous observations. Development in detector technology will further advance the time- and space-resolving aspects of the experiments. About the authors Ake Kvick graduated from Uppsala University in 1974. Work on hydrogen bonded systems, zeolites and time-resolved studies with neutrons and X-rays. Scientist at Brookhaven National Lab. 1980­ 1989. From 1989 work at the ESRF on synchrotron radiation diffraction; presently Head of Materials Science Group and editor of J. Synch.Rad. Jose Baruchel graduated in Physics at the University of Greno­ ble. From 1971 to 1991, work on magnetic domains and nearly perfect crystals, with X-rays and neutrons. From 1991, work at the ESRF on synchrotron radiation imaging (topography and tomog­ raphy); presently Head of the X-ray Imaging Group. @/j EDP sClr,,'\fCES EDP Sciences' journals All the information on EDP Sciences' journals for authors and institutions and access to the ~Iectronic versions for readers is available at: http://www. e dpsciene.:e$~org europhysics news MARCH!APRIL 2004 What is your strategy for Framework 6? Sean McCarthy, Managing Director ofHyperion Ltd. ow many research organisations have a formal written strat­ H egy for Framework 6? How many individual researchers have a personal strategy for Framework 6? This article presents a checklist for the writing of a simple but practical strategy for Framework 6. An organisation's strategy for Framework 6 The following are examples of statements of objectives that could be used in a research organisation's strategy for Framework 6. They are based on actual discussions with research organisations on their Framework 6 strategies. (The comments in brackets are actual quotations from research managers) To access European Union Funding for research activities. One of the problems with this simple objective is that the researchers may concentrate on obtaining any contracts rather than focussing on the research priorities of the organisation. To establish the research group as the European (or Internation­ al) scientific leader in a scientific area ('to be the best in our field'). It is important that the scientific areas are well defined (a niche within an niche). For example, , to be the world leader in the simulation and design of photovoltaic (solar) systems'. To access new technologies relevant to the organisation's areas of excellence ('to avoid missing the train'). To work with the best research partners in the European Union. ('to be the preferred partner of the best scientists in our field') To provide better education and training to graduates and post-graduates. ('We want our graduates to excel in any inter­ view, anywhere in the world') • To promote the organisation's scientific and technical excellence to the scientific/technical community ('more conferences, more publications, more website hits.. :) To ensure the research results are used by enterprises and soci­ ety ('getting value from our research efforts') To provide relevant support to researchers ('To streamline the process of proposal writing, contract negotiation and contract management/administration') . Bontaz-Carion J. , Nicollet M. , Manczur P. , Pellegrini Y.-P. , Boiler E. , Baruchel J . Dynamic damage in metal: porosity as a testfor damage models, in A . Chiba, S. Tanimura and K. Okamoto eds., Impact Engineering and Application, Proc. 4th Int. Symp. on Impact Engineering , pp. 633 - 638 , Elsevier, Oxford ( 2001 ). Buffiere J.Y. , Maire E. , Cloetens P. , Lormand G. and Fougeres R. , Characterization ofinternal damage in a MMCp using synchrotron phase contrast microtomography , Acta Mater . 47 , 1613 - 1625 ( 1999 ) Cloetens P. , Ludwig w., Baruchel J. , Guigay J.P. , Rejmankova-Pernot P. , Salome-Pateyron M. , Schlenker M. , Buffiere J.Y. , Maire E. , Peix G. , Hard X-ray phase imaging using simple propagation ofa coherent synchrotron radiation beam . J. Phys. D: Appl. Phys . 32 , A145-A151 (1999a) Cloetens E , Ludwig W , Baruchel J" Van Dyck D. , Van Landuyt J. , Guigay J.P. , Schlenker M. , Holotomography: quantitative phase tomography with micrometer resolution using hard synchrotron radiation X-rays , Appl. Phys. Lett. 75 , 2912 - 2914 ( 1999b ) Contreras 1 ., Turillas X. , Vaughan G.B.M. , Kvick A. , Rodriguez M.A. Time-resolved XRD study ofTiC- TiBl composites obtained by SHS . To be published ( 2004 ) Elliott J.A. , Windle A.H. , Hobdel J.R. , Eeckhaut G. , Oldman R.J. , Ludwig W , Boiler E. , Cloetens E , Baruchel J. , Foam compression by microtomography , J. Mat. Science , 37 , 1547 - 1555 ( 2002 ). Lauridsen E.M , Juul Jensen D. , Poulsen H.P. Lienert U , Kinetics of individual grains a during crystallisation ., Scripta Materialia , 43 , 5561 - 566 ( 2000 ). Martins R.V , Honkirnaki v., Depth resolved investigation offriction stir welds using a novel strain and phase mapping technique , Texture and Microstructure , 35 , 145 - 152 ( 2003 ). Morcrette M. , Chahre Y. , Vaughan G.B.M. , Amatucci G. , Leriche J.B. , Patoux 5 ., Masquelier c., Tarascon J.M. In situ x-ray diffraction techniques as a powerful tool to study battery electrode materials . ElectrochirnicaActa , 47 , 3137 - 3149 ( 2002 ) Offerman S.E, van Dijk N.H , Sietsma J. , Grigull 5 ., Lauridsen E.M, Margulies 1 ., Poulsen H.P. , Rekveldt M. Th ., van der Zwaag S. Grain nucleation and growth during phase transformations . Science , 298 , 1003 - 1005 ( 2002 ). Riiegsegger E , Koller Rand Miiller R ,. A microtomographic system for the non destructive evaluation of bone architecture, Calcif . Tiss.lnt., 58 , 24 - 29 ( 1996 ). Sasov A. and Van Dyck D. , Desk-top microtomography: gateway to the 3D world , European Microscopy and Analysis , pp. 17 - 19 ( 1998 ).

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José Baruchel, Åke Kvick. Synchrotron radiation imaging and diffraction for industrial applications, Europhysics News, 50-55, DOI: 10.1051/epn:2004205