nnls_vol18_n1_13 by Notiziario nnls

School and Meeting Reports

Research Infrastructures

ISSN 1592-7822 - Vol. 18 n. 1 Gennaio 2013 Aut. Trib. Roma n. 124/96 del 22-03-96 - Sped. Abb. Post. 70% Filiale di Roma - C.N.R. p.le A. Moro 7, 00185 Roma

Scientific Reviews

Volume 18 n. 1 www.cnr.it/neutronielucedisincrotrone

ESRF Users' Meeting 2013 Shaping the Next Decade of Research

On 4-6 February 2013, the next ESRF Users’ Meeting will exceptionally include large room for discussions about the future of the ESRF. Four years after the launch of the Upgrade Programme, the ESRF is currently engaged in the definition of its second phase to start after 2015. These discussions centre around the proposal to build a new, low-emittance, high-brilliance storage ring in the existing tunnel featuring a novel lattice. This would allow the brilliance of the source to be boosted by a factor of 30-40. The ESRF is inviting all Users to a series of five workshops coinciding with the next Users’ Meeting, to discuss the scientific opportunities such a new source would offer. The five Upgrade Phase II workshops will be held on Monday 4 February 2013, with the following topics: • • • • •

X-ray Cinematography with the New Coherent Source Seeing is believing: the future of Structural Biology Phase II: Prospects for Materials & Chemistry From Functional Soft Matter to Biology - Future Challenges Science at Extreme Conditions with an Ultimate Source

The plenary meeting on 5-6 February 2013 will feature: • • • • • •

Six plenary lectures by world leading scientists covering a large spectrum of ESRF activities; A presentation on the status of the facility and on the progress of the Upgrade Programme; A talk by the winner of the prestigious “ESRF Young Scientist Award”; A session dedicated to feedback from the Phase II workshops and further discussion; A poster session; A banquet, with awards to the ESRF Young Scientist Award and for the best poster.

ESRF User Organisation Chiara Maurizio (chairperson) Physics Department University of Padova via Marzolo, 8 35131 Padova, Italy chiara.maurizio@unipd.it ESRF User Office, useroff@esrf.fr Tel. +33 4 76 88 25 52 For more information and to register, go to www.esrf.eu or directly to www.tinyurl.com/dy2q6r2.

n Editorial News

A visit to ESRF, ILL and ISIS L. Nicolais

n Scientific Reviews

Neutron Imaging - status and prospects of a modern research tool Flexible non-invasive studies from plant-soil-interaction to magnetic material investigations E.H. Lehmann, A. Kaestner, P. Vontobel, C. GrĂźnzweig, D. Mannes and S. Peetermans

In situ Inelastic Neutron Scattering Study on a Gas-Loaded Metal-Organic Framework S. Yang, A. J. Ramirez-Cuesta and M. SchrĂśder

Application of synchrotron radiation techniques to the study of hydrogen storage materials L. Pasquini

n Research Infrastructures

ESRF Nanoscience beamline ID16 passes milestone C. Habfast

Celebration of 10 Years of Engin-X - Materials Science and Engineering research at ISIS S. Y. Zhang, J. Kelleher and W. Kockelmann

n School and Meeting Reports

International Neutron Scattering Instrumentation School (INSIS) I.S. Anderson, C. Andreani, M. Arai, A. Harrison, R. McGreevy , R. Pynn

The Third Meeting of the Union for Compact Accelerator-driven Neutron Sources C.-K. Loong

Shull Fellows now launched on interesting and fulfilling careers A. Bardoel

n Call for proposal Neutron Sources

Synchrotron Radiation Sources

n Calendar

n Facilities

Neutron Sources Synchrotron Radiation Sources

Volume 18 n. 1 www.cnr.it/neutronielucedisincrotrone

Summary

Published by CNR (Publishing and Promotion of Scientific Information) in collaboration with the Centro NAST of the University of Rome Tor Vergata

Editorial News Volume 18 n. 1 Dicembre 2012 Aut. Trib. Roma n. 124/96 del 22-03-96 EDITOR C. Andreani CNR - PROMOTION AND COLLABORATIONS M. Arata CORRESPONDENTS F. Boscherini, L. Bove, C. Blasetti, A. Ekkebus, M. Forster, T. Guidi, C. Habfast, B. Palatini, L. Paolasini, H. Reichert, V. Rossi Albertini ON LINE VERSION V. Buttaro CONTRIBUTORS TO THIS ISSUE I.S. Anderson, M. Arai, A. Bardoel, R. McGreevy, C. Grünzweig, C. Habfast, A. Harrison, A. Kaestner, J. Kelleher, W. Kockelmann, E.H. Lehmann, C.K. Loong, D. Mannes, L. Nicolais, L. Pasquini, S. Peetermans, R. Pynn, A.J. Ramirez-Cuesta, Martin Schröder, P. Vontobel, Sihai Yang, S.Y. Zhang EDITORIAL INFORMATION AND SUBSCRIPTIONS S. Fischer E-mail: nnls@roma2.infn.it GRAPHIC DESIGN Stampa Sud S.p.A. PRINT Stampa Sud SpA Via P. Borsellino 7/9 74017 Mottola (TA) – Italy e-mail: info@stampa-sud.it www.stampa-sud.it

Finito di stampare nel mese di Gennaio 2013

2 A visit to ESRF, ILL and ISIS L. Nicolais

Scientific Reviews 3 Neutron Imaging - status and prospects of a modern research tool Flexible non-invasive studies from plant-soil-interaction to magnetic material investigations E.H. Lehmann, A. Kaestner, P. Vontobel, C. Grünzweig, D. Mannes and S. Peetermans

10 In situ Inelastic Neutron Scattering Study on a Gas-Loaded Metal-Organic Framework S. Yang, A. J. Ramirez-Cuesta and M. Schröder

14 Application of synchrotron radiation techniques to the study of hydrogen storage materials L. Pasquini

Research Infrastructures

20 ESRF Nanoscience beamline ID16 passes milestone C. Habfast

22 Celebration of 10 Years of Engin-X - Materials Science and Engineering research at ISIS S. Y. Zhang, J. Kelleher and W. Kockelmann

School and Meeting Reports 30 International Neutron Scattering Instrumentation School (INSIS) I.S. Anderson, C. Andreani, M. Arai, A. Harrison, R. McGreevy , R. Pynn

32 The Third Meeting of the Union for Compact Accelerator-driven Neutron Sources C.-K. Loong

33 Shull Fellows now launched on interesting and fulfilling careers A. Bardoel

Call for proposal

Cover photo The picture shows an example of metallomics from beamline ID22: Fe fluorescence measured in a malaria infected red blood cell to localise the distribution of a drug target in the cell. (Image courtesy of C. Habfast, European Synchrotron Radiation Facility ESRF).

36 Neutron Sources

37 Synchrotron Radiation Sources

40 Calendar Facilities 41 Neutron Sources 44 Synchrotron Radiation Sources

Editorial News

A visit to ESRF, ILL and ISIS Luigi Nicolais President of CNR

I recently visited the European Synchrotron Radiation Facility (ESRF) and the Institut Laue-Langevin (ILL), both hosted at the European Photon & Neutron (EPN) science campus of Grenoble (France), as well as the ISIS spallation neutron source hosted at the Rutherford Appleton Laboratory in UK. These facilities, each of them in highly successful partnership agreement with CNR, play a central role in promoting high-level research at European and international level. CNR investments continue to offer our scientific community access to experimental methods of tackling some of the most fundamental scientific questions and cuttingedge technologies in the fields of advanced materials, biology, chemistry, physics with applications for example to cultural heritage, environment, energy, health, engineering, geosciences, new materials and sustainable energy research. I could experience first-hand the achievements of the Italian neutron science community in collaboration with scientists of these facilities and it was an opportunity for exploratory discussions on how to stimulate industrial innovation from state-funded research. Italian researchers regularly succeed in winning a significantly greater share of the time available at these facilities, through competitive international peer review and the strong impact of the Italian community in developing advanced

neutron instrumentation. Within the international agreements CNR secures with ILL, ISIS and ESRF several beamlines have been developed over the years as well as the instrumentation R&D activities driven by Italian researchers, often operated by Italian scientists on behalf of their community. CNR scientists are currently taking a strong lead with the operation of the CRG beamline Gilda BM08 at ESRF, the CRGâ&#x20AC;&#x2122;s BRISP and IN13 beamlines at ILL and INES beamline at ISIS, in order to support the development of new beamlines for Chip irradiation and imaging of materials detectors and detector concepts at ISIS for the benefit of the wider community. A team of ISIS-CNR scientists - the PANAREA project - is currently developing the CHIPIR and IMAT beamlines at ISIS Second Target Station (TS2) within the current agreement; in addition, â&#x20AC;&#x201C; the DANTE project is developing new technologies for detection and neutron polarization for the ESS project. A significant experience was the meeting with the community of Italian researchers at both Grenoble and Chilton who contribute daily to the implementation of projects. During the meetings with the leaders of these infrastructure I had the opportunity of discussing how to further expand our mutual collaborating research activities, highly successful for all partners, and how to optimize and exploit them to their full potential. A science-driven organization such as CNR is naturally committed to continue to enable Italian researchers to access leading national and international science facilities by funding membership of international bodies such as ILL, ISIS and ESRF.

From left to right: L. Nicolais (CNR), R. McGreevy (ISIS), T. Guidi (ISIS)

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

Scientific Reviews

Abstract The study of material interaction with neutrons can provide essential information about the observed sample. On atomic and microscopic level, neutron diffraction and scattering techniques are well established and structural information, quantum phenomena or lattice parameters can be derived. The most prominent and powerful neutron sources are therefore equipped with families of neutron scattering devices. On the macroscopic level we mainly deal with neutron transmission imaging where a 1:1 “shadow image” contains the important information about the inner features of the observed objects. With the availability of digital neutron imaging systems (starting in the 90ies of last century) not only the image frequency was dramatically increased but mainly the options for more detailed studies of the neutron distributions inside and around the sample and the process under investigation. In this way, new imaging techniques have been developed and made available for a broad user community on routine basis. Similarly to X-ray techniques, neutron tomography enables the access to the third dimension, whereas phase contrast methods provide additional and alternative information. New approaches are now the use of polarized neutrons, the observation in narrow energy bands and the further improvement of the spatial resolution in neutron imaging. The study of real-time processes is an option close to the performance edge of neutron imaging, demanding and challenging.

Unfortunately, the number of facilities providing a state-of-the-art research infrastructure for neutron imaging is still limited. The article will discuss this point and gives some guidelines how to overcome the current situation.

1. Introduction Neutron Imaging started as “neutron radiography” about 50 years ago when strong enough neutron sources were made available. Using film techniques combined with a neutron converter, a single image was ready after exposure and processing within about 1 hour. The essential differences and advantages compared to X-rays were already exploited at that time: a higher penetrability for heavy materials and the better visibility for light elements, in particular hydrogen. The limitation on static imaging in two dimensions created only a small user community in non-destructive testing, nuclear engineering, pyrotechnics and some further industrial applications. Nevertheless, a series of conferences of a world-wide connected community was initiated in 1981 by J. Barton [1] and the Figure 1

Simplified sketch of an (neutron) imaging setup – not to scale

9th World Conference on Neutron Radiography was held in South Africa in 2010 [2]. A complementary series of expert’s meetings have been taken place regularly (International Topical Meetings on Neutron Radiography [3] and NEUWAVE [4]). Also IAEA managed to initiate some network and standards in neutron imaging [5] and gives further support, in particular for developing countries. This is a clear indication of the increased importance of neutron imaging methods while their abilities and their potential are further increased. In some institutions, neutron imaging is already an equally accepted technique with a clear user program and broad application range. However, several conditions have to be fulfilled to declare to be a “user facility”.

2. Neutron imaging today The basic setup for neutron imaging is shown in Fig. 1: the collimated beam from a neutron source is observed by a suitable two-dimensional area detector after transmitting the object under investigation. There are several parameters defining the quality of the obtained neutron image. First of all, the source properties have to be considered. Due to the high contrast and the large differences in the attenuation properties of materials in this energy range, thermal and cold neutron beams have found to be most suitable for practical use. The utilization of fast neutrons provides a higher penetration but much lower contrast and resolution, given by the detection process. In the best case, only mono-energetic neutrons are used. However, the effort to limit the neutron energy band is considerably high (see chapter 3.3.) and the exposure time is increasing much. Secondly, the beam collimation is very important if a high spatial resolution is intended. The geometric blurring ug is inversely

Scientific Reviews

linked to the inherent beam divergence (calculated via the ratio of the collimator length L and the aperture opening D) and directly to the sample - detector distance d. On the other hand, the beam intensity φ is decreasing with this collimation ratio in the following manner:

L    D

2

(1)

Therefore, a compromise has to be found between the beam intensity and its best possible collimation. Because neutron sources are generally limited in intensity a high degree in the flexibility is needed to tune the beam for the particular setting and application. In order to obtain spatially coherent neutrons, the aperture dimensions w have to reduce further down to the millimeter range in order to fulfill the coherence conditions for the coherence length r in the micro-meter range (with the wavelength λ, the distance to the measurement position l) :

r

 l w

(2)

Because the intensity of even strongest neutron sources is quite limited, the work with mono-chromatic and coherent neutrons in imaging mode is still not very common. Third, the detector performance plays an essential role in order to define which techniques are possible today in neutron imaging. As digital imaging is performed exclusively at modern facilities, the result of a transmission analysis is provided as pixel matrix with 1000 … 4000 pixels in one direction and a wide dynamic range (e.g. 16 bits). While the detector is in most cases camera based (CCD or CMOS), the primary sensor for neutrons is a scintillation screen. Its efficiency and inherent spatial resolution is defined by the layer thickness (10 to 300 micro-meters). Compared to other detection systems (imaging plates,

amorphous silicon flat panels, pixilated detectors) [6] the camera has the advantage to be flexible in the field-of-view and pixel size, has a fixed position in respect to the beam (an option needed for referencing and tomography), high dynamic range and a high signal/noise performance.

Figure 2

Aluminium based plant container filled with soil are used for the observation of root growing [6]: only the neutron image (bottom) enables the root inspection while the X-ray image (top) suggest empty space in the root region

3. Neutron imaging techniques Here, we present a list of presently common imaging techniques with neutrons without claim of full completeness. Depending on the situation in the individual institution, particular techniques are more or less pronounced or developed.

3.1. Transmission radiography mode In this mode, neutron imaging can provide similar performance like X-ray radiography (as common e.g. in hospitals) in respect to image size and resolution. However, the image contrast and therefore the inherent information are quite different. As shown in the example in Fig. 2, a high sensitivity for small amounts of organic materials (here: plant roots) is given in a metallic container and wet soil environment. The dimensions of objects to investigate are less limited by the size of the beam (which can have a diameter up to 40 cm) but more by the attenuation of the material itself. For e.g. Al or Pb a layer of 30 cm can be penetrated, but 1 cm of water is already nearly “black”. The attenuation data in respect to thermal neutrons are well known and can be used for estimates [7]. In respect to the spatial resolution, the main limitation is given by the detection system. For the moment, there are systems available with pixel sizes in the order of 15 micro-meters. The corresponding field-of-view is on the order of 30 mm.

Quantification: The transmitted beam intensity I carries information about the sample content if it is compared to the initial intensity I0 without the sample (open beam image). In first order, the Beer-Lambert’s law is valid for the attenuation of the beam intensity. Than it is possible to derive for each pixel in the sample region the material density ρ by inverting the attenuation law:

I L ln( 0 ) / d    N        (3) I M The attenuation coefficient Σ is just the multiplication of the material specific (and tabulated) microscopic cross-section and the density of nuclei N (L = Avogadro’s constant, M = atomic mass). In this way, a non-invasive determination of material distributions can be performed.

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Figure 3

Procedures in neutron tomography in order to get the volume data of the observed objects and to access the third dimension

1. Data acquisition 300-1200 projections Scan time 1-24h

2. CT reconstruction Processing time ~1h

Processing time: hours or days

For thicker material layers there are deviations from the exponential law and some corrections have to be included for multiple scattering and changes in the spectral neutron distribution [8].

of the systems differs due to the various beam conditions and detection systems. The results of studies are competitive to Xray tomography data and complement them in several cases very well (e.g. Fig. 4).

3.2. Neutron tomography

3.3. Energy selective neutron imaging

In order to investigate the third dimension of samples, it is necessary to take projections over an angular range of at least 180°. Because the neutron source is fixed and given by the large scale facility, the samples have to be rotated around their vertical or horizontal axis in the quasi-parallel neutron beam. This two-dimensional information is needed to calculate the voxelvalues for the volume by using reconstruction tools, mainly based on filtered backprojection algorithms (e.g. [9]). Depending on the detectors performance in respect to the number of pixels (typical 1000 to 4000) the size of the reconstructed data volume is in the order of several GBytes per object, what is still demanding in respect to the visualization, processing and storing. Neutron tomography in established in several labs around the globe, but the number of installations is limited. The performance

3. Data evaluation Image processing/analysis 3D Visualization

The initially delivered beam spectra from the source are in most cases Maxwellian distributions around the mean thermal energy of about 25 meV. Therefore, the obtained transmission data represent an energy-averaged value for the investigated material. Since the microscopic cross-sections σ are often strongly energy dependent the spectral dependency limits the quantification (see above) due to scattering and beam hardening effects. On the other hand, there is much microscopic information in the cross-sections due to the crystalline structure and the scattering at lattice planes in the case of solid crystalline materials (as many metals). Fig. 5 shows this behavior in the cold energy range very pronounced. The access to this information is only possible by limiting the energy range of the incoming neutrons. The reduction of the energy band

can be done by selection device, either based on a turbine with tilted blades or by single crystals which scatter out the suitable (or the misleading) parts of the spectrum. Depending on the devices performance, the energy resolution is between 5% and 15%. There are two aspects for experiments near Bragg edges: (1) two measurements – one below and another above the strong edge helps to increase the contrast among the involved materials; (2) at a suitable energy – depending on the particular material – the crystal orientation and textured zones become directly visible by alternating contrasts (see Fig. 6). In a later stage, by narrowing the energy even more, it will become possible to determine directly the stress distribution in structural materials. Future energy selective imaging will be performed in time-of-flight mode at the upcoming beam imaging lines at pulsed sources [4], where the energy band can be chosen more flexible and nearly with arbitrary width.

3.4. Time-dependent neutron imaging Only with modern digital imaging systems it has become possible to work effi-

Scientific Reviews

Figure 4

Slices of a tomography study of a concrete sample (photo – middle) with X-rays (120 kV, left) and thermal neutrons (right); in this case, a higher contrast is given in the neutron study and the profile is more uniform

ciently in the time domain in order to study processes and material changes There are two directions for such kind of investigations: (1) to monitor a process in real-time (mainly without any delay by the readout); (2) to use stroboscopic procedures for repetitive processes in order increase the image quality by the superposition of frames at identical settings. Generally, the limiting factor for the time resolution is the source intensity. Because the neutron flux is typically of the order of 108 cm-2 s-1 a single frame needs exposure time in the milli-second range and often even more, depending on the detection system. Stroboscopic imaging has been performed up to repetition rates of 8000 rpm without blurring by the motion. As shown in Fig. 7, clear images can be obtained which are nearly the same in quality compared to static images.

3.5. Phase-sensitive neutron imaging As neutrons can be considered not only as free particles but also as waves with a wavelength λ according to the de Broglie relation, their interaction with matter can induce some phase

shift next to the amplitude reduction (which describes the common attenuation). Accordingly, a refraction index n is defined which describes the direction of the outgoing wave front according to Snell’s law (N = nuclei density, bc = coherent scattering length):

n  1   1

It is to mention that the deviation from 1 is very little (not comparable to light optics) and the angular changes are very small therefore. Nevertheless, refraction becomes directly visible in high resolution neutron imaging using cold neutrons (long wavelength) as edge enhancements (Fig. 8). On the other hand, it is really challenging to derive the phase shift δ as an additional signal, complementary to the absorption data. Grating based interferometers have been building for this purpose. It has been shown with such a device that magnetic interactions at domain walls can be made visible in the bulk structure by using the "dark field image" from the grating interferometer.

Figure 5

Figure 6

Total cross-sections of structural materials in the energy/wavelength range where Bragg edges are pronounced due to the scattering at crystalline lattice planes 30 25

 [barn]

2  N  bc  1  10 6 (4) 2

Part of a stainless steel weld (photo – top) was investigated by neutron tomography in the “white beam” (middle) and with neutrons around 3.5 Å (bottom): the needle type structure become visible over the whole volume of the weld material verifying a preferred crystal orientation (data from [11])

Pb Zr Al

5 0

Neutron wavelength [Å]

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

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Figure 7

Neutron images of a two-stroke combustion engine: top – static image obtained within 10s; bottom – 1000 stacked frames with 50 micro-seconds exposure each

(+1/2 and -1/2) the orientation of the neutrons in respect to a magnetic field can be either “up” or “down”. It is possible by experimental means to separate the two spin states and to produce a beam of polarized neutrons with only one orientation. Because magnetic fields and magnetic structures interact with neutrons via its magnetic moment the polarized beam can be used for a direct imaging of magnetic properties. It is required to analyze the beam after passing the magnetic assembly in respect to the depolarization by an analyzer device which is aligned in front of the detector. A result of studies with polarized neutrons is given in Fig. 10 where the distribution of the magnetic field around a superconductor is described in a complete non-invasive way [13].

4. Neutron imaging user facilities world-wide

3.6. Diffractive neutron imaging In the neutron transmission imaging the majority of the neutrons get attenuated by scattering processes, e.g. the scattering cross-sections are for most of the materials larger than the absorption cross-sections. However, the scattering component of the attenuated beam has been ignored in neutron imaging mainly until know or considered misleading in the quantification (see 3.1). Now it has been proven that in the case of single crystals or polycrystalline samples with large enough grains the diffracted neutrons can be visualized and quantified in a second imaging detector which is set aside the sample (about 90° apart). This setup and some of the first results are shown in Fig. 9. There is a high potential for material research in the future with this method because the crystalline structure of samples can be studies in one overview run semi-quantitatively, in conjunction with the transmission data, before more specific investigations can follow at specialized facilities. As high performance parts of engines and turbines are produced as signal crystals, the spatial distribution of the crystal orientation can directly be observed by this method.

Neutron imaging on a high performance level can only be performed at strong sources, mainly reactor based, and with only few exceptions at accelerator based sources. Mobile sources have never the needed intensity to get the suitable image quality. In a world-wide overview, only about 15 facilities could be attributed to this standard. It is mainly the in-house acceptance, competition and funding which limits to establish a real neutron imaging competence in the individual institutions. Figure 8

Phase effects in neutron imaging: top – edge enhancement by refraction (sample: diesel injection nozzle); bottom – visualization at magnetic domain walls in the dark field image [12].

3.7. Neutron imaging with polarized neutrons Neutrons carry a magnetic moment μn which is oriented antiparallel to the spin. As the spin of the neutron exist in two states

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Many research reactors are operational in developing countries, but with limited utilization yet. Presently, support is given by IAEA to start neutron imaging activities. In the developed countries, projects at the powerful pulsed spallation sources are started and installations with high performance will be available around 2015 [4].

Figure 9

Simultaneous observation of the transmission image in the direct beam (microbox) and the diffracted signal (Laue diffraction spots) at a selected wavelength (midibox): it can be attributed directly which regions in the sample contribute to the signals

5. Main application fields Due to new and more sophisticated methodical features and possibilities, the user community around neutron imaging facilities has been extended and new scientific and technical approaches were realized. Traditionally, geosciences, soil physics, biology and nuclear material research are among the users profiles for neutron imaging. New request are coming from paleontology, electro-chemistry, cultural heritage research and wood science. However, also the study of building materials has a very high economic impact and relevance of growing cities. Other new fields like magnetism research, structural material studies and environmental research will follow as soon as the suitable performance can be provided at the different neutron imaging facilities. Neutron imaging methods have of course a high potential for industrial applications. Here it complements the well established Xray methods in non-destructive testing and material inspection. The distribution of lubricants, fluids, glues and of inner defects are some prominent examples to be studied in two or three dimensions and timely resolved.

Figure 10

A radiograph showing the field lines around a bar magnet levitating over an yttriumâ&#x20AC;&#x201C;bariumâ&#x20AC;&#x201C;copper-oxide(YBCO) superconductor due to the Meissner-effect [13]

6. Conclusions Neutron imaging techniques are today tools for material research with high flexibility in spatial, time and energy resolution. They are clearly useful advantageously on the macroscopic scale due to the high penetration ability. The high contrast of light elements within bulk metallic structures provides many new approaches for investigations. The more sophisticated methods in phase contrast imaging and the utilization of polarized neutrons has to be promoted to the users by further successful pilot experiments. Many of the existing facilities can be used on request in their access program.

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

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References [1]

J. Barton, Proc. 1st World Conference on Neutron Radiography, San Diego, USA, Gordon and Breach Science Publisher, 1983 [2] F. de Beer et al. (ed.), Proc. 9th World Conference on Neutron Radiography, Kwai Maritane. South Africa, Elsevier, 2012 [3] N. Takenaka et al. (ed.), Proceedings of the 6th International Topical Meeting on Neutron Radiography, Kobe (Japan), Sept. 2008, Elsevier, doi:10.1016/j. nima.2009.01.115 [4] http://neutrons.ornl.gov/conf/neuwave4/ [5] IAEA-TECDOC-1604, Neutron Imaging: A Non-Destructive Tool for Material Testing, Sept. 2008 [6] E.H. Lehmann, A. Tremsin, C. Grünzweig, I. Johnson, P. Boillat and L. Josic, Neutron imaging — Detector options in progress, 2011 JINST 6 C01050 [7] A. B. Moradi, A. Carminati, D. Vetterlein, P. Vontobel, E. Lehmann, U. Weller, J. Hopmans, H.-J. Vogel, S. Oswald, Three-dimensional visualization and quantification of water content in the rhizosphere, New Phytologist (2011) 192: 653-663, doi: 10.1111/j. 14698137.2011.03826.x [8] http://www.ncnr.nist.gov/resources/n-lengths/ [9] Hassanein R., Meyer H.O., Carminati A., Estermann M., Lehmann E., Vontobel P.,Investigation of water imbibition in porous stone by thermal neutron radiography JOURNAL OF PHYSICS D: Appl. Phys. 39 4284-4291, 2006 http://dx.doi.org/10.1088/0022-3727/39/19/023 [10] http://www.ugct.ugent.be/software.php [11] Josic, L., Lehmann, E., Kaestner, A., Energy selective neutron imaging in solid state materials science, Nuclear Instruments and Methods in Physics Research, Section A: Accelerators, Spectrometers, Detectors and Associated Equipment 651 (2011) , pp. 166-170 [12] C. Grünzweig, C. David, O. Bunk, M. Dierolf, G. Frei, G. Kühne, R. Schäfer, S. Pofahl, H.M.R. Rønnow, and F. Pfeiffer, Bulk Magnetic Domain Wall Structures Visualized by Neutron Dark-Field Imaging, Applied Physics Letters 93 (2008) p. 112504 [13] N. Kardjilov et al., Three-dimensional imaging of magnetic fields with polarized neutrons, nature physics Vo.4, 2008, doi:10.1038/nphys912

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In situ Inelastic Neutron Scattering Study on a Gas-Loaded Metal-Organic Framework Sihai Yang,1 A.J. Ramirez-Cuesta,2 and Martin Schröder1 [1] School of Chemistry, University of Nottingham, University Park, Nottingham, NG7 2RD (UK) [2] ISIS Facility, Rutherford Appleton Laboratory, Chilton, Oxfordshire, OX11 0QX (UK)

Selective capture of harmful flue gases, such as carbon dioxide (CO2) and sulphur dioxide (SO2), represents a major challenge in mitigating the global climate change.1 Current state-of-the-art technology uses aqueous solutions organic amines at high concentration for post-combustion CO2 capture, so called “aminescrubbing mechanism”.2 Capture systems functionalised with amine groups dominate this area, due to potential formation of carbamates via H2N(δ-)···C(δ+)O2 electrostatic interactions, thereby trapping CO2 covalently.3 However, the considerable costs of this process due to the substantial energy input required for the regeneration of the amine solutions as well as their highly corrosive and toxic nature, and their negative environmental penalty, significantly limit their long-term applications. It is therefore important to develop alternative carbon capture systems that base on environmental-friendly materials. Porous metal-organic framework (MOF) complexes are a sub-class of coordination polymers with high surface area and tuneable functional pore environment and show great promise for application in gas storage and separation.4 Optimising the interactions between MOF hosts and the adsorbed gas molecules can lead to the discovery of new functional materials with better capture properties. Thus, defining and the direct visualisation of binding interactions within these host-guest systems represent important methodologies for the understanding of mechanisms for the selective capture of gases (CO2 and SO2). The extended 3D crystalline nature of MOF materials allows the study of material function via advanced diffraction techniques, and enormous invaluable structural rationale for their high binding energy were obtained in this way. However, static crystallographic studies cannot provide insights into the dynamics of the crystal lattice and gas molecules upon gas loading. Thus it is a major challenge to understand the dynamics during the CO2 capture process. Herein we report the novel application of in situ

inelastic neutron scattering (INS) combined with density functional theory (DFT) calculations to permit direct visualisation of the dynamics of the binding interaction between adsorbed XO2 (X = C, S) molecules and a metal-hydroxyl-functionalised porous solid (NOTT-300) exhibiting high chemical and thermal stability, and high selectivity and uptake capacity for CO2 and SO2. These dynamic study suggests that the active hydroxyl groups within the pore channels interact directly with CO2 and SO2 via the formation of moderate Al-OH···O=C(S)=O hydrogen bonds, supplemented by weaker phenyl C-H···O supramolecular contacts surrounding the pore. The solvated framework complex [Al2(OH)2(C16O8H6)] (H2O)6 (NOTT-300-solvate) was prepared via hydrothermal reaction of H4L1 (biphenyl-3,3’,5,5’-tetracarboxylic acid) and Al(NO3)3·9H2O in water containing HNO3. Crystal structural determination suggests that NOTT-300-solvate exhibits an open structure comprising chains of [AlO4(OH)2] moieties bridged by tetracarboxylate ligands L4-. This overall connectivity affords a porous 3D framework structure with 1D channels (Fig. 1a). An important consequence of this MOF is the formation of squareshaped channels with hydroxyl groups protruding into them, endowing the pore environment with free hydroxyl groups over four different directions. Fully desolvated material NOTT-300 was prepared by heating the as-synthesised sample at 120 oC and under high vacuum (10-9 bar) for 1 day. NOTT-300 shows very high uptake capacities for CO2 (7.0 mmol g-1) and SO2 (8.1 mmol g-1) adsorption at 273 K and 1.0 bar (Fig. 1b). Significantly, the SO2 uptake represents the highest value observed within this type of materials so far. In contrast, under the same conditions the isotherms for CH4, CO, N2, H2, O2, and Ar show only surface adsorption by NOTT-300, with very low uptake of gas. Importantly, comparison of the gas adsorption isotherms clearly shows ultra-high selectivities for CO2 and SO2, indicating the potential of NOTT-300 for the selective capture of these harmful gases. Direct visualisation of the interaction between XO2 (X=S, C) molecules and the NOTT-300 host is crucial to understanding the detailed binding mechanism and hence the observed high selectivities. Inelastic neutron scattering (INS) is a powerful neutron spectroscopy technique which has been used widely to investigate the H2 binding interactions within various storage systems by exploiting the high neutron scattering cross-section of hydrogen (82.02 barns).5 However, this technique cannot directly detect the CO2 or SO2 binding interaction within a carbon capture system because the scattering cross-sections for carbon (5.551 barns), sulphur (1.026 barns) and oxygen (4.232 barns) are too small to obtain a clear neutron scattering signal. In this study, we

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have successfully combined INS and DFT to visualise captured CO2 and SO2 molecules within NOTT-300 by investigating the change in the dynamics of the hydrogen atoms of the local MOF structure, including those of the hydroxyl groups and benzene rings of the ligand. INS spectra were recorded on the TOSCA spectrometer at the ISIS Facility at the Rutherford Appleton Laboratory (UK) for energy transfers between ~-2 and 500 meV. Calculation of the INS spectra from DFT vibrational analysis can be readily achieved, and the DFT calculations relate directly to the INS spectra, and, in the case of solid state calculations, there are no approximations other than the use of DFT eigenvectors and eigenvalues to determine the spectral intensities.6 In addition to the straight forward DFT analysis, INS spectroscopy also has other unique advantages, in particular when comparing with traditional IR or Raman spectroscopy: (i) INS spectroscopy is ultra-sensitive to the vibrations of hydrogen atoms, and hydrogen is ten times more visible than other elements due to its high neutron cross-section; (ii) the technique is not subject to any optical selection rules. All vibrations are active and, in principle, measurable; (iii) neutrons penetrate deeply into materials and pass readily through the walls of metal containers making neutrons ideal to measure bulk properties of this material; (iv) INS spectrometers cover the whole range of the molecular vibrational

spectrum, 0-500 meV (0-4000 cm-1); (v) INS data can be collected at below 10 K, where the thermal motion of the MOF material and adsorbed CO2 molecules can be significantly reduced. Combining these features, INS spectra of gas-loaded material can provide key insight into the binding interactions. Comparison of INS spectra, measured at temperatures below 5 K to minimise the thermal motion of the adsorbed CO2 and the framework host, reveals two major increases in peak intensity on going from bare NOTT-300 to NOTT-300·1.0CO2: peak I occurs at low energy transfer (30 meV) and peak II at high energy transfer (125 meV) (Fig. 2a). Moreover, the peaks in the range 100-160 meV are slightly shifted to higher energies in NOTT300·1.0CO2, indicating a stiffening of the motion of the NOTT300 host upon CO2 adsorption. To understand these changes, DFT calculations have been used to simulate the INS spectra and optimise the structures for NOTT-300 and NOTT-300·1.0CO2. The INS spectra derived from these calculations show good agreement with experimental spectra and confirm that the adsorbed CO2 molecules interact end-on to the hydroxyl groups. The O···H distance between the CO2 molecule and the hydroxyl group is 2.335 Å, indicating a moderate-to-weak hydrogen bond. Each adsorbed CO2 molecule is also surrounded by four aromatic C-H groups, forming weak cooperative supramolecular interactions

Figure 1 (a) Views of the structure for NOTT-300 showing 1D channels; (b) the comparison of the gas adsorption isotherms for NOTT-300 at 273 K and 1.0 bar.

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between O(δ-) of CO2 and H(δ+) from -CH [O···H = 3.029, 3.190 Å, each occurring twice]. Specifically, peak I can be assigned to the O-H groups wagging perpendicular to the Al-O-Al direction, attributed to the presence of the CO2, and peak II to the wagging of the four aromatic C-H groups on four benzene rings adjacent to each CO2 molecule in conjunction with the wagging of the OH group along the Al-O-Al direction (Fig. 2e). Thus, a total of five hydrogen atoms H(δ+) interact cooperatively with the O(δ-) charge centres of CO2 molecules in the channel via moderate-toweak hydrogen bonds and supramolecular interactions. Similar INS study and DFT analysis were also carried out on SO2loaded NOTT-300, in order to probe the dynamics of the gasloaded system. Comparison of the INS spectra below 5 K reveals two major increases in peak intensity on going from bare NOTT300 to NOTT-300·2SO2 (or NOTT-300·3SO2): peak I occurs at low energy transfer (30–50 meV) and peak II at high energy transfer (125 meV), similar to that observed in the INS spectra for CO2-loaded NOTT-300 (Fig. 2b). Moreover, immediate stiffening of the motion of the NOTT-300 host was observed upon SO2 inclusion, as evidenced by the slight shift in INS peak to higher energies in NOTT-300·2SO2 and NOTT-300·3SO2. DFT simulation has also been performed to optimise the structures of both NOTT-300 and NOTT-300·2SO2 materials. The simulated INS spectra show good agreement with the experimental spectra and are consistent with the adsorbed SO2 molecules interacting end-on to the hydroxyl groups via the hydrogen bond interactions [O···H = 2.338 Å] with additional supramolecular contacts with the adjacent aromatic C-H groups [O···H = 2.965–3.238 Å]. The INS/DFT results also suggest the formation of this weak hydrogen bond interaction. In order to understand why low uptakes are observed for some gases while high selectivity for CO2 is achieved, we sought to probe the interactions between H2 and NOTT-300 (Fig. 3). The INS spectra of NOTT-300·1.0H2 show an overall increase in signal upon H2 loading, indicating adsorption of H2 by NOTT-300 at below 40 K. The difference INS spectra, measured at below 5 K, between bare NOTT-300 and NOTT-300·1.0H2 show a series of features that resemble the signal of liquid molecular H2. Significantly, the sharp rotational peak usually observed around 14.7 meV as a prominent feature in the INS of molecular H2 in the solid state or adsorbed on surface is not observed here. This suggests a 1D fluid-like recoil motion of the H2 along the channel consistent with extremely weak interactions and low uptake of H2 in NOTT-300. Thus, in situ INS study on the non-amine-containing capture material NOTT-300 has suggested that the Al-OH groups in the

pore cavity can participate in moderate interactions with CO2 and SO2, and that these are supplemented by cooperative interactions with adjacent C-H groups of benzene rings. The binding energy of these moderate-to-weak hydrogen bonds can be viewed as soft binding interactions, quite distinct from the direct bond formation between the N-centre of amine groups and the electro-positive C-carbon centre of CO2. This offers great promise not only for the efficient capture of CO2 and SO2, but also for their facile, low-energy and therefore economic release subsequently; moreover this “easy-on”/“easy-off ” soft binding model is achieved without any reduction in either selectivity or capacity.

References 1. D. W. Keith, Science, 2009, 325, 1654-1655. 2. G. T. Rochelle, Science, 2009, 325, 1652-1654. 3. C. Villiers, J. P. Dognon, R. Pollet, P. Thuery and M. Ephritikhine, Angew. Chem. Int. Ed., 49, 3465-3468. 4. J. R. Long and O. M. Yaghi, Chem. Soc. Rev., 2009, 38, 1201-1507. 5. P. C. H. Mitchell, S. F. Parker, A. J. Ramirez-Cuesta and J. Tomkinson, Vibrational spectroscopy with neutrons with applications in chemistry, biology, material sciences and catalysis, World Scientific, Singapore, 2005. 6. A. J. Ramirez-Cuesta, Comput. Phys. Commun., 2004, 157, 226-238.

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Comparison of the experimental (top) and DFT simulated (bottom) INS spectra for bare and CO2-loaded (a) and SO2-loaded (b) NOTT-300. Difference plot for experimental INS spectra of bare and CO2-loaded NOTT-300 (c) or SO2 loaded NOTT-300 (d). View of the optimised structure of CO2-loaded (e) and SO2loaded (f) NOTT-300 obtained from DFT analysis.

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Application of synchrotron radiation techniques to the study of hydrogen storage materials Luca Pasquini Department of Physics and Astronomy, University of Bologna and CNISM v.le C. Berti-Pichat 6/2 40127 Bologna, Italy

Abstract Materials for reversible hydrogen storage in the solid state constitute a subject of intensive research. In this article, after an introductory discussion on hydrogen storage materials, specific examples of their investigation by means of synchrotron radiation are presented. Emphasis is given to the complementary use of X-ray diffraction and absorption techniques, and on the design of in situ experiments which permit to follow phase transformations and microstructure changes induced by hydrogen uptake and release.

The Hydrogen Storage Challenge The realization of a safe and efficient way to store hydrogen (H) remains a key challenge for the advent of H-fuelled light vehicles. The main figures that describe the performance a H-storage system relate to its gravimetric (rm) and volumetric (rV) capacities (expressed as H mass per mass or volume of the system) and to the temperature range for its operation. Based on the idea that customers would hardly accept reduced performances with respect to fossil fuel-powered cars, the US Department of Energy (DOE) has developed targets that a H-storage tank should meet in order to be successful in the market. For the year 2015, the targets are rm = 5.5 wt%, rV = 40 kg H2 m-3, and -40/60 Â°C temperature range, with the ambition to reach rm = 7.5 wt% and rV =70 kg H2 m-3 as ultimate figures. The different strategies which are currently being explored to solve the H-storage problem can be generally subdivided into three main categories: i) physical containment, e.g. compression or liquefaction ii) physisorption, i.e. adsorption of H2 molecule onto the surface of highly porous materials iii) formation of a chemical bond, e.g. metal hydrides, ammonia. The reader interested in a critical discussion on the state of the art of these H-storage categories and in a comparison between them is referred to excellent reviews on the subject [1,2]. In particular, the third broad category, chemically bound hydrogen, encompasses very different materials, like metal hydrides, complex hydrides, amines and amides, ammonia borane, and hydrocarbons. Some of these substances, like sodium borohydride NaBH4, easily release H2 upon reaction with water, but the reaction products are too thermodynamically stable to be easily refueled. The most interesting systems are instead those in which the release (desorption) and uptake (absorption) of hydrogen can occur under mild pressure/temperature conditions, thus allowing reversible operation. In this case the mechanism of Hrelease is an entropy-driven endothermal decomposition which

takes place at sufficiently high temperature, more precisely when TDS>DH, where DS is the entropy increase associated with evolution of the H2 gas and DH is the decomposition enthalpy. The reverse process is then an enthalpy-driven exothermal refueling by H-uptake at low temperature/high pressure. Since the term DS mainly arises from the entropy of the gas itself (130 J K-1 mol-1 at a pressure of 1 bar) and therefore varies little from one material to another, the decomposition / refueling temperature T=DH/DS is largely determined by the reaction enthalpy. The sought ideal enthalpy value lies between 30 and 48 kJ/mol H2, which corresponds to operating conditions appealing for mobile storage: 0-100 Â°C and 1-10 bar. Unfortunately, the elements or intermetallic compounds, like Pd, LaNi5, TiFe, which fulfill this enthalpy requirement, are far away from the desired gravimetric capacity. Conversely, metal or complex hydrides based on light materials, which display appealing rm values, are either too stable, meaning that the decomposition requires too high temperatures (e.g. MgH2, LiBH4), or too unstable, i.e. the refueling requires only occurs at very high pressures (e.g. AlH3, Mg(AlH4)2). In addition to the thermodynamic issue, the kinetics of the reversible transformation often poses severe problems. However, in many cases valid solutions have been found by proper materials engineering. For example, in the Mg-H system, which in its basic form suffers from sluggish kinetics of H-uptake/release, impressive improvements were obtained by employing nanocrystalline MgH2 with suitable dispersion of catalyst phases such as transition metals and their oxides. These materials can be prepared rather easily in a single step by means of simple and scalable techniques like ball milling. Another significant step forward was achieved with sodium alanate NaAlH4, where BogdanovicÂ´ and Schwickardi discovered that doping with small amounts of Ti compounds could significantly improve the kinetics of H evolution and uptake. Given such a rich scenario where the holy grail of H-storage is still missing, it is clear why the research on advanced materials for solid-state H-storage (SSHS) represents a hot topic. On one hand, the synthesis and characterization of novel bulk com-

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pounds is explored, along with chemical routes to make their H-sorption reactions reversible at practical temperature and pressure, which leads to the advanced concept of reactive hydride composites, an example of which will be discussed later. On the other hand, the research focuses on nanostructures in which two or more phases with different DH values coexist on a nanometric length scale. The thermodynamics of these nanomaterials does not simply result from a weighted average of the component phases, since new physics emerges due to various interactions between them, and the local structure at the interfaces plays a very important role in this respect.

Figure 1

In situ XRD study of the phase transformations in Mg/MgO core/shell NPs decorated with Pd during the first heating ramp in vacuum. The heating rate was 5K/min. The main peaks of each phase are marked and the colors serve to identify different regimes of phase coexistence. Magenta: starting

composition with Mg and Pd; blue: the Mg-Pd intermetallics Mg5Pd2 and Mg6Pd appear; orange: Pd disappears while a significant formation of MgO is detected; green: Mg5Pd2 transforms completely into Mg6Pd. Details on the quantitative phase analysis are given in Ref. 10.

Motivation for experiments with the synchrotron probe Synchrotron radiation (SR) has the potential to address most of the challenging requirements posed by the investigation of SSHS materials. In fact, a number of studies have been published in the last years, employing different and often complementary SR techniques. The study of how microstructure and phase composition evolve during H-uptake and release can be undertaken by in situ X-ray diffraction (XRD) experiments, which are also extremely helpful for determining the reaction pathways in complex systems [3,4]. X-ray Absorption Spectroscopy (XAS) is suitable for investigating the structure of diluted catalysts, often in form of ultrafine particles, since the physical phenomenon upon which the technique is based is inherently local and element-selective [5]. New hydride crystal structures can be determined by high-resolution XRD, sometimes in combination with neutron diffraction due to the peculiar neutron scattering length of hydrogen and deuterium [6,7]. The distribution of particles sizes in a huge range is conveniently measured by

small-angle scattering techniques, including anomalous small angle x-ray scattering (ASAXS) [8] and small-angle neutron scattering (SANS) [9]. In the next sections, we will discuss specific examples on the use of SR to probe structure, electron bonding states and transformation pathways of advanced materials for SSHS based on reversible hydrides. Two examples constitute a combined approach that we have followed to investigate Mgbased nanostructured materials by means of complementary XRD and XAS experiments [10,11]. Another couple of illustrative case studies selected from recent literature on the subject will be also reviewed [9,12]. Particular emphasis in given to in situ experiments because of their unique ability to shed light on the structural trans-

formations and microstructural evolution which take place during the processes of Huptake and release.

In situ X-ray diffraction The experiments presented here were performed at the beamline I711 of the synchrotron MAX-II in Lund. Data were collected using a Marresearch MarCCD 165 detector. The powder samples were inserted in a single crystal sapphire capillary tube mounted in an airtight sample holder. A tungsten wire wrapped around a quartz rod and placed 0.5 mm under the capillary provided radiation heating to the sample. The capillary was also connected to a gas control manifold for H-absorption up to 5 MPa and H-desorption under rotary pump vacuum.

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The first example is an investigation of Mg-based nanoparticles (NPs) [10]. Magnesium hydride MgH2 displays several attractive features like low cost, high rm = 7.6 wt%, non toxicity, but unfortunately also a high stability (DH = 75 kJ/mol H2) and a poor catalytic activity. The interaction of H with Mg-based nanostructures has been characterized in many different morphologies, including thin films and layered materials [13], nanowires [14], NPs [15], and MgH2-loaded nanoscaffolds [16]. In Mg-based nanostructures, Pd is often employed as a capping layer to increase oxidation resistance and to promote the dissociation/recombination of the H2 molecule at the surface. However, the occurrence of structural transformations in Pd and in possible Mg-Pd compounds connected to H-sorption is generally overlooked. Mg/MgO core/shell NPs were prepared by inert gas condensation and decorated by Pd evaporation, as discussed in Ref. [17]. A shown in Figure 1, the first heating under vacuum causes the disappearance of fcc Pd and the formation of Mg-Pd alloys: first Mg5Pd2 around 470 K and finally Mg6Pd. While Mg6Pd is the expected equilibrium phase according to the Mg-Pd phase diagram at low Pd concentration (13 wt% in this case), the importance of these experiments is to highlight a fast kinetics of alloy formation even at moderate temperature and in presence of a MgO barrier layer (5 nm thick). What is more interesting, is that the Mg 6Pd phase plays an active role in subsequent Hsorption runs. In fact, Figure 2a shows that, upon H-absorption at 573 K / 5 MPa H 2 pressure, not only Mg transforms into MgH2, but also Mg6Pd undergoes the reaction:

Figure 2

In situ XRD profiles taken at selected times during (a) H-absorption at 573 K and p(H2)=5 MPa, admitting H2 at time t=0+ s, and (b) H-desorption at 573 K under dynamic vacuum, pumping away H2 at time t=0+ s. The symbols

mark the main reflections of the identified phases. The gray circles superposed to the last pattern represent the Rietveld fit, the residual being shown below. The results of the quantitative phase analysis are given in Ref. 10.

Mg6Pd+5H2 ↔ MgPd+5MgH2 (1)

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mation of MgB2 is observed in the isothermal period. In summary, the usefulness of in situ XRD experiments with synchrotron radiation is to simultaneously determine the H-sorption kinetics and to provide a structural viewpoint on the ongoing reactions and transformations pathways as a function of pressure and temperature.

Figure 3

Crystal structures of the Mg-Pd intermetallic compounds which characterize the equilibrium state after H-desorption (Mg6Pd) and after H absorption at 573 K under 5 MPa H2 pressure (MgPd). Pd is represented in green color.

which is indeed reversible, i.e. when vacuum is restored, MgPd transforms back into Mg6Pd as displayed in Figure 2b. The crystal structure of these two Mg-Pd intermetallic compounds are illustrated in Figure 3: Mg6Pd has a huge cubic cell (lattice parameter a=20.108 Å, space group F-43m) while MgPd has a simple CsCl structure (space group Pm3m). Figure 2b suggests the existence of other equilibrium states, revealed by the peaks of the Mg5Pd2/Mg3Pd phases in the profile at t=80s. These intermediate states were confirmed by further experiments at lower H2 pressure as discussed in detail in Ref. 10. In turn, reaction (1) corresponds to a H-storage capacity of 3.96 wt% specific of the Mg6Pd phase and to a H-desorption enthalpy of 69 kJ/mol H2 on the basis of thermodynamic calculations [18], i.e. 9% lower than for pure MgH2. A second illustrative example deals with reactive hydride composites (RHCs), i.e. composites in which the value of the endothermal H-desorption enthalpy is effectively lowered by an exothermic reaction with the formation of a new compound, and vice versa for the exothermal H-absorption [19]. A very prominent and promising system is: 2LiBH4+MgH2 ↔ 2LiH+MgB2+4H2 (2) with a storage capacity of 11.5 wt%. In (2), it is the exothermic formation of MgB2 which lowers the enthalpy of the

X-ray Spectroscopy

H-releasing reaction. While heating an as-milled LiBH4+MgH2 RHC doped with NbF3 to a final temperature of 400 °C, three distinct events were observed [9]: i) at about 110 °C, LiBH4 transforms from orthorhombic to hexagonal; ii) at 275 °C, the LiBH4 diffraction peaks fade out because of the melting of this phase, and iii) at temperatures around 330 °C, desorption of hydrogen from MgH2 occurs, together with the formation of metallic Mg. Finally, after about 3 hours isothermal at 400 °C the formation of MgB2 is observed, correlated to the decomposition of LiBH4. An incubation time between the formation of metallic Mg and the for-

On the same Mg-Pd NPs discussed previously, we used Pd K – edge EXAFS, at the GILDA beamline of the European Synchrotron Radiation Facility (ESRF), to quantitatively describe the local structure of Pd -containing phases in different equilibrium states [11]. Figure 4 reports the magnitudes of the Fourier Transforms (FT) of the EXAFS functions for the following samples: reference Pd foil, as-prepared NPs, NPs after H-absorption, and NPs after H-desorption. In the asprepared NPs shown in Figure 4b, Pd is in form of ultrafine fcc crystals (diameter ≈ 3 nm) on top of the NPs’ outer MgO shell, as suggested by transmission electron microscopy observations [17]. EXAFS analysis shows that the Pd-Pd interatomic distance is the same as for bulk Pd, while the average coordination number is reduced due to surface effects. According to the XRD results, after H-absorption at high temperature, fcc Pd disappears in favour of the MgPd phase. The corresponding EXAFS data (Figure 4c) were thus fitted using the crystallographic

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information for the MgPd phase with only one Pd site. The Mg-Mg and Mg-Pd interatomic distances determined from the fit are larger than the ones quoted for bulk MgPd by about 2%. This result is important because it suggests that H enters in solid solution into the MgPd lattice: if this is so, an expansion between 2 and 3 Å3 per H atom absorbed can be expected. Conversely, XRD tells us that, after H-desorption, Pd is bound to Mg in the Mg6Pd phase, in which 4 different Pd sites can be identified. The details of EXAFS analysis are given in Ref. 11. Figure 4d shows that by properly taking into account single and multiple scattering paths for each Pd site, the experimental data can be fitted quite satisfactorily. No indication in favour of expanded interatomic distances is obtained in this case, supporting the idea that H does not enter into the Mg6Pd lattice in an appreciable amount. We emphasize that this XAS study represents a very useful complement to the in situ XRD investigation, since it allows a deeper characterization of Pd-containing nanostructured phases. It also points out that reaction (1) should be corrected into a form which takes into account H dissolved into MgPd; Mg6Pd+(5+d/2)H2 ↔ MgPdHd + 5MgH2 (1´) with d in the range 0.4 – 0.6. In situ XANES measurements during a heating ramp were also performed on as-prepared and on hydrogenated NPs, to investigate the irreversible formation of Mg-Pd compounds and the reversible transformation from MgPd to Mg6Pd which accompanies H-release [11]. X-ray spectroscopy is also an invaluable tool for the study of the electronic states and bond nature in bulk hydrides. Among these, the electronic structure and

the bonding state of α-AlH3 have been an important subject of research, but experimental data are rather poor and the nature of Al-H bond is still controversial in the theoretical studies. Aluminum hydride α-AlH3 is an appealing H-storage material due to its large gravimetric and volumetric capacities (10.1 wt% and 149 kgm−3, respectively). However, it suffers from the opposite drawback with respect to MgH2: in fact, its enthalpy of formation is only slightly negative (−11.3 kJ/ mol H2), meaning that extreme pressure conditions are required for its regeneration. In a recent study, the electronic structure of AlH3 was investigated by an insightful combination of XAS and X-ray Emission Spectroscopy (XES) in the soft x-ray regime [12]. XES and XAS experiments allow to measure the occupied and the unoccupied electronic states, respectively, and to obtain the whole feature of the electronic states by combination of their spectra. In addition, it is possible to extract a partial density of states (PDOS) for a specific element by tuning photon energy to the excitation energy of the target element. The sample for this study was obtained by hydrogenation of Al at 600 °C and 8.9 GPa. The measurements were performed at the experimental station of soft x-ray beamline BL27SU of SPring-8. By comparing the electronic structures of α-AlH3 with reference Al metal, it emerged that α-AlH3 has an energy gap of a few eV and that the spectral intensity of the Al 3p PDOS in the occupied states of α-AlH3 is larger. The authors conclude that the Al-H bond in α-AlH3 has a covalent like nature. We remark here that these kind of experimental data are vital to the theoretical modeling of hydrides and to the development of chemical and physical strategies aimed at tuning their stability.

Conclusions The specific examples described here highlight the importance of SR techniques for the advanced structural characterization of H-storage materials, from bulk new compounds to nanostructures where two or more phases coexist on a small scale. At the European level, a COST Action focused on nanostructured hydrides was launched recently and currently counts 25 participating countries [20]. One of the Action’s working groups, devoted to high resolution and high sensitivity characterization of atomic level structure and microstructural features, sees the participation of several groups from the SR and neutron community. In the future it will be important to integrate SR-based investigations with electron and scanning probe microscopy, in order to gain a deeper knowledge of materials’ structure and function at the nanoscale and to develop new materials in tight connection with theory and modeling.

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References [1] A.J. Churchard et al., Phys. Chem. Chem. Phys. 13, 16955 (2011) [2] U. Eberle, M. Felderhoff, F. Schüth, Angew. Chem. Int. Ed. 48, 6608 (2009) [3] M.D. Riktor et al., J. Mater. Chem. 17, 4939 (2007) [4] U. Bösenberg et al., Acta Mater. 55, 3951 (2007) [5] R. Checchetto et al., Appl. Phys. Lett. 87, 061904 (2005) [6] A. Fossdal, H.W. Brinks, M. Fichtner, B.C. Hauback, J. Alloys Compd. 387, 47 (2001) [7] Y. Filinchuk et al. Angew. Chem. Int. Ed. 50, 11162 (2011) [8] U. Bösenberg et al., Nanotechnology 20, 204003 (2009) [9] P.K. Pranzas et al., Adv. Eng. Mat. 13, 730 (2011) [10] E. Callini, L. Pasquini, L.H. Rude, T.K. Nielsen, T.R. Jensen, E. Bonetti, J. Appl. Phys. 108, 073513 (2010) [11] L. Pasquini et al., Phys. Rev. B 83, 184111 (2011) [12] Y. Takeda et al., Phys. Rev. B 84, 153102 (2011) [13] A. Baldi, M. Gonzalez-Silveira, V. Palmisano, B. Dam, R. Griessen, Phys. Rev. Lett. 102, 226102 (2009) [14] W.Y. Li, C.S. Li, H. Ma, J. Chen, J. Am. Chem. Soc. 426, 316 (2007) [15] L. Pasquini, E. Callini, E. Piscopiello, A. Montone, M. Vittori Antisari, E. Bonetti, Appl. Phys. Lett. 94, 041918 (2009) [16] A.F. Gross, C.C. Ahn, S. L. Van Atta, P. Liu, J.J. Vajo, Nanotechnology 20, 204005 (2009) [17] E. Callini, L. Pasquini, E. Piscopiello, A. Montone, M. Vittori Antisari, E. Bonetti, Appl. Phys. Lett. 94, 221905 (2009) [18] J.F. Fernandez, J.R. Ares, F. Cuevas, J. Bodega, F. Leardini, C. Sánchez, Intermetallics 18, 233 (2010) [19] M. Dornheim et al., Scripta Mater. 56, 841 (2007) [20] http://www.cost-mp1103.eu/

Figure 4

Magnitude of the FT of raw EXAFS spectra (open circles). The continuous lines represent the fit performed with the package ARTEMIS. In(c), the dashed and dotted lines represent the fit contributions coming from the 1st shell of MgPd and from a shell of 8 Mg atoms. In (d),

the 1st shell-like contributions from the four different Pd sites in the Mg6Pd structure are displayed as thin solid lines marked by one symbol. The details of the data analysis are discussed in Ref. 11.

Research Infrastructures

ESRF Nano science beamline ID16 passes milestone Claus Habfast Head of Communication Group European Synchrotron Radiation Facility ESRF

On 18 October 2012, the large satellite building for the new ESRF beamline ID16 was inaugurated in the company of members of its Administrative and Finance Committee (figure 1). The building occupies a floor surface of some 700 square metres, of which 400 sqm are for the actual experimental hall and about 200 sqm for the 100-metre long tunnel linking the satellite building to the main experimental hall. A particular feature of the building is the high stability of the concrete slab in the experimental hall. High stability means absence of vibrations added to the level already present from sources outside the ESRF, and that absence of curling or shrinkage due to temperature gradients across the slab. A close-to-perfect floor is needed for the nanoscience beamline ID16 to meet its design performances. To date, the measured slab parameters look promising. ID16 is one of eight ESRF Upgrade Beamlines, to replace the current beamline ID221. Its development is driven by three key scientific fields, all linked together by the need for studies at the nano-scale: 1 G. Martínez-Criado et al., Status of the hard X-ray microprobe beamline ID22 of the European Synchrotron Radiation Facility, J. Synchrotron Rad. 19, 10-18 (2012)

bio-medical research, environmental and earth sciences, and materials sciences. Such a wide field cannot be addressed with a single end station, which is why ID16 includes two independent end stations, each fed by one of two canted undulators: a nano-imaging station ID16NI for fluorescence analysis and nano-tomography, and a nanoanalysis probe ID16NA for XRF, XAFS and XRD spectroscopy. In the bio-medical sciences, ID16 will play a key role in “metallomics”, a new frontier field where cells are not only characterized by genome and proteome, but also by the distribution of metals among the different species and cell compartments, the “metallome”. Nano-X-ray-fluorescence will elucidate the distribution of trace metals in cellular organelles (typical sizes are about 2-5μm for the nucleus, 0.5-1μm for mitochondria, 25nm for the ribosome, and 20nm for chromatin fibers), and nano-X-ray-absorption spectroscopy will identify their chemical state. Recent work on ID22, the pre-cursor beamline of ID16, on the sub-cellular labelfree localization of anti-malaria drugs has shown the timeliness and relevance of such research2 (figure2). In the Earth and environmental sciences, ID16 will make possible studying how minerals and particles react with their environment at the sub-grain level: for example, establish the mechanisms of toxicity of fine dust particles and aerosols, characterize the behavior of metals and metalloids in bio-geochemical systems, observe the interaction of bacteria with contaminants, and understand the toxicity and bio-geochemistry of manufactured and natural nanoparticles.

2 F Dubar et al., Chem. Commun. 48, 910 (2012)

Figure 1

Happy faces at the inauguration of the ID16 building. From left to right: Francesco Sette, Director General, Bauke Dijkstra, Director of Research, Gema MartinezCriado, beamline responsible scientist for the nano-analysis end station, Peter Cloetens, beamline responsible scientist for the nano-imaging station and ID16 project coordinator.

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Figure 2

An example of metallomics from beamline ID22: Fe fluorescence measured in a malaria infected red blood cell to localise the distribution of a drug target in the cell.

The key feature of the nano-analysis end station (see figure 4) is its multi-modal concept allowing to using a monochromatic hard (5 - 65 keV) X-ray beam (50 nm) for many different techniques (XRF, XRD, XAS, XEOL, 2D/3D XRI). A free distance of > 35 mm and a high photon flux (1010-1011 ph/s) make possible to incorporate in-situ sample environments. The satellite building will host both a high-end optical microscope and a compact SEM to support sample visualization, manipulation & mounting. A drying oven, ultrasonic bath, precision scale, binocular viewer etc. along with a stock of standard materials, chemicals & consumables will make possible finishing sample preparation on site in many cases where this is impossible before traveling to the ESRF. Clean and secure storage space for samples and equipment is therefore also foreseen in the ID16 building. The nano-imaging end station (see figure 5) is designed for X-ray fluorescence microscopy and coherent imaging with a 15 nm nanofocused pink beam. The high photon flux (10111012 ph/s) is optimized for tomography and low detection limits, and the complete set-up exhibits optimum mechanical stability and scanning precision.

Figure 4

Simplified drawing of the nanoimaging end station

Sample preparation will be routinely performed in a cryogenic environment to reduce radiation damage, and the preparation room includes a cryo-plunger, a cryo-cartridge loading area, a freeze-drier and an inverted fluorescence microscope. For biological samples, also a class II cabinet and a CO2 incubator are available. Finally, an animal biomedical facility is located in the immediate vicinity. Hutch construction in the new building has started in mid-November 2012, and the first users are expected to arrive early in 2014.

Figure 3

New materials are the third science driver of ID16 which is an extremely broad field, ranging from electronics to healthcare. A particular motivation comes from the evolution of micro-electronics towards miniaturization to the nano-scale which makes necessary to consider quantum size effects, tunneling, exchange coupling, self-assembly, patterning etc. Understanding the structure of nano-objects enhances the ability to manipulate them and fosters the development of new models to describe their behavior at this scale. Recent work on ID22NI on the quantum states of nano-wires used as novel light-emitting devices (figure 3) underscores this statement3.

An example of research into nano-materials: quantum confinement inside a nanowire probed at beamline ID22, and a comparison with theory.

Figure 5

Simplified drawing of the nanoanalysis end station

3 Nano Lett., 2012, 12 (11), pp. 5829-5834

Research Infrastructures

Celebration of 10 years of ENGIN-X - Materials Science and Engineering research at ISIS Shu Yan Zhang*, Joe Kelleher, Winfried Kockelmann ISIS Facility, Science and Technology Facilities Council, Rutherford Appleton Laboratory, Harwell Oxford, Didcot, Oxfordshire OX11 0QX, UK *email: shu-yan.zhang@stfc.ac.uk

Engin-X is the world’s leading neutron diffractometer, purposebuilt for materials science and engineering experiments. Its first neutrons were produced in 2002, and over the past 10 years EnginX has continually redefined the frontier of stress measurement capability through investment in state-of-the-art equipment, attracting academic and industrial users from 24 countries. "The 10th anniversary of Engin-X operation coincides with the centenary of Max von Laue's demonstration of X-ray crystallography and the 80th anniversary of Chadwick's discovery of the neutron. The diverse applications of Engin-X, some of which are described in this paper, illustrate beautifully how, over the years, these academic research discoveries have metamorphosed into a specialised technique for materials science and engineering which has significant impact on fundamental knowledge (for the next generation of techniques) and on the technical decisions and developments with major economic consequences." - Prof. Robert McGreevy, ISIS Director.

Overview Neutron stress measurement is a non-destructive technique that has the unique ability to measure strain and stress deep within engineering components, including under representative service conditions

such as temperature and external loads. In the early 1980s, residual strain measurement by neutron diffraction using conventional general purpose diffractometers was reported [1]. With increasing industrial interest in the technique, the first dedicated pulsed neutron stress diffractometer, ENGIN, was born at the ISIS Facility at the Rutherford Appleton Laboratory, UK in the mid 1990s. In response to demands from users, major developments and upgrades were made. ENGIN was replaced by Engin-X (Figure 1), providing an order of magnitude increase in performance [2]. Engin-X is a world leading neutron diffractometer for materials science and engineering, with high resolution and versatile capabilities. The success of Engin-X has also led to dedicated engineering instruments being built at neutron sources in other countries. The construction of the instrument was funded by the Engineering and Physical Sciences Research Council in 1999, at a cost of £2.5 million, and was completed in 2002. The principal investigator was Lyndon Edwards at the Open University, along with co-investigators Mark Daymond (ISIS), Mike Johnson (ISIS), Noel O’Dowd (Imperial), Peter Webster (Salford), Phil Withers (Cambridge/Manchester), Mike Fitzpatrick (Open University) and George Webster (Imperial). Engineering measurements are based on Bragg diffraction, yielding information on the distortion of the atomic lattice, typically as a function of position, or applied thermal and/or mechanical loads. This information is used to shed light on deformation mechanisms, processing and manufacturing routes, and failure mechanisms both in real components and in test samples. The applications cover two main basic areas. First, studies of fundamental material behaviour including investigations of basic deformation mechanisms in metals, including phase transformations and twinning. Secondly, experiments are focused on producing strain or stress maps as a function of position within components, possibly under a simulated service condition, often to provide data for the verification of finite element modelling predictions of engineering processes or for comparison with other methods of residual stress measurement. Measurements are typically carried out in collaborative experiments between universities, industry and ISIS to address a wide Figure 2

Schematic diagram of the Engin-X layout

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Figure 1

Preparations for a collaborative ENGIN-X experiment between The Open University, Airbus UK and ISIS, aimed at optimising the fabrication of large aluminium alloy wing components. A wingbox typical of that which may be used on the very large aircraft is being loaded on to the instrument.

range of engineering problems: manufacturing challenges surrounding magnesium alloys for the automotive industry, thermal deformation characteristics of nickel-base superalloys for aero engines, structural integrity of welds for nuclear power plants, fabrication stresses in a range of samples from complex aeroplane parts to steel wires, ancient steel making techniques and the development of strain measurement standards. User from EDF Energy says: "The collaborative experiment between EDF Energy, Open University and ISIS to study critical welded components, helped demonstrate that the welds retained their structural integrity, and supported 5 year life-extensions to be made for these power plants, deferring the need for decommissioning and replacement of two nuclear power stations at a cost of a round £1.5 billion each". After 10 years of operation, the instrument continues to be in high demand. The user community is drawn from:

• 24 countries • 22 UK universities • Multinational companies including Rolls-Royce, Airbus, Boeing, TWI, Tata Steel, QinetiQ, EDF Energy, Magnesium Elektron • Major international museums including the Rijksmuseum Amsterdam, Wallace Collection London, Natural History Museum London • Government agencies from the UK and overseas, including AWE, CNR (Italy), Atomic Energy of Canada Limited, Chinese Academy of Sciences, Japan Atomic Energy Agency •

Instrument description and capabilities

A schematic of the instrument layout is shown in Figure 2. A pulsed beam of neutrons with a wide energy range travels to the sample, where a small fraction of the diffracted beam is collected with the two sets of detectors at an angle of 90o either side of

Research Infrastructures

Figure 3

(a) Schematic of implant (b) Residual stress profile of HA coating and Ti-6Al-4V substrate (as-sprayed; heat treated; and heat treated then soaked in simulated body fluid)

(a) the incident beam. The bisection of the incident and diffracted beam is the neutron ‘scattering vector’, which is the direction of the strain component that the diffracted neutrons will measure. With two sets of detectors, two perpendicular strain directions can be measured simultaneously. The volume of material contributing to the measurement corresponds to the intersection of the incident and diffracted beams – the ‘gauge volume’, typically defined by incident slits and collimators. The gauge volume is typically of the order of cubic millimetres and defines the location of the measurement. On ENGIN-X, the gauge volume is at a fixed position in the instrument, so strain measurement at different locations across the sample is accomplished using a translation stage to move the sample itself. A diffraction pattern will be obtained for each detector bank during the measurement. The particular significance of neutron diffraction methods is that they offer a direct method of measuring the elastic component of strain deep within crystalline materials through the precise characterisation of the crystal lattice’s interplanar spacing. Diffraction uses the atomic lattice itself as a deformation gauge. The principle of diffraction strain measurement in crystalline materials relies on Bragg’s law (Eq. 1) that provides a means to determine the average interplanar lattice

(b) spacing d within a small measurement volume of the sample. When a polycrystalline aggregate deforms elastically, the interplanar spacing within the constituent grains changes, e.g. tensile stress will cause an increase in the lattice spacing within the lattice planes normal to the loading direction. The strain is then calculated by comparing this measurement with that of the unstrained material (d0).

2d sin    (Eq. 1)



(d  d 0 ) d  d0 d0

(Eq. 2)

with 2θ being the angle between incident beam and diffracted beam, and λ being wavelength of neutron beam. There are two data analysis methods that can be used: Single peak fitting and whole pattern refinement. The single peak fitting method normally fits the experimental data using peak profiles such as Gaussian, Pseudo-Voigt, etc. Each single peak is characterized by its position, amplitude and peak width; there’s no need to input the crystal structure information into the program. As single peak fitting analyses individual hkl reflections, the elastic lattice strain

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for each lattice plane is determined independently. In addition to fitting the single peaks, it is possible to perform a whole pattern refinement on the data. Pawley refinement is a similar approach to Rietveld refinement that accommodates the variation in peak intensities by allowing the intensity of individual reflections to vary freely, while the peak positions are determined in the usual manner from the unit cell dimensions. This approach provides an empirical average of the different reflections and potentially includes physics that describes the overall deformation of the polycrystal. The lattice unit cell parameters a, b and c are determined from the refinement, and lattice strain is hence calculated from these lattice parameters instead of the individual d spacings. Engin-X has a very user friendly data analysis program, where no prior knowledge of diffraction is required. Measurement data can be analyzed online during the experiment, meaning results can be taken away as soon as the experiment is finished. Engin-X has consistently pushed forward the frontier of stress measurement capability through investment in state-of-the-art equipment to alter the conditions under which experiments are carried out. These include a rotation robot, furnaces, cryostat, and hydraulic stress-rigs for testing material performance under simulated in-service loading. A sample mounting stage allows samples weighing up to one tonne to be accurately positioned around the measurement vo-

lume with an accuracy better than 10 micrometres. Moving and rotating the sample within the neutron beam allows spatial and directional maps of strain to be built up. With the large sample mounting space, Engin-X provides the flexibility for the users to bring their own ancillary devices, such as welding rigs to perform real-time strain measurements during joining. An in-situ mountable servo-hydraulic stress rig can apply up to 100kN tensile or compressive cyclic loads. The rig can be equipped with a furnace or a cryogenic chamber that allow the sample to be maintained at temperatures from -200 oC to 1100 oC within normal atmosphere or under inert gas. The automation of experimental setup for complex-shaped samples can be addressed via the use of the coordinate measurement machine (CMM), laser scanning inspection arms, a robotic arm and the virtual measurement simulation software, SScanSS. [3] The following gives a summary of the sample environments equipement on ENGIN-X: • Furnace equipped with stress rig– provides temperatures up to 1100 oC within normal atmosphere or under inert gas • Vacuum furnace – provides temperature up to 1800 oC • Heating pad – can be used for in-situ heat treatment experiment on complex-shaped or large objects • Cryogenic chamber – provides temperatures down to -200 oC. It can be used on its own or with the stress rig

Figure 4

(a) DC-cast slab being positioned at ENGIN-X (b)Map of the residual strain measured using neutron diffraction within the DC-cast slab. The map is supermposed with estimated position of the crack in the measurement plane. The unit display is in microstrain.

(a)

(b)

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• Servo-hydraulic Stress rig – applies loads up to 100kN • Laser scanning inspection arms – provides automation of experimental setup for complex-shaped samples and used with virtual laboratory, SScanSS [4] • Cybaman Manipulator (sample rotation robot) • 2D Transmission detector – energy selective neutron imaging and measurement of strain in the direction parallel to the beam

Experiment highlights Surface measurement - Nanostructured hydroxyapatite coatings for orthopaedic implants The use of surface coatings in orthopaedic and dental implants has significantly improved the quality of human life (Figure 3). Early implants were expensive, and often failed because the bonding between the implant and the bone was poor. Several designs have been formulated to date but many failed to achieve a strong enough bond. Implants are commonly made using titanium coated in hydroxyapatite (HA), which is the main constituent of human bone. One of the main reasons of failure is the residual stress developed at the metal-HA interface. The hydroxyapatite coFigure 6

Axial and trasverse elastic strain response of γ and γ’ of polycrystalline nickel-base superalloy at 20oC, 400oC, 500oC, 650oC and 750oC

ating is typically 220 micrometres thick. The residual stress at the titanium-HA interface is mainly due to differences in the thermal and mechanical properties of the two materials. The orthopaedic implant industry can use stress profile model to monitor the quality of the HA coating. The experiment at Engin-X was used to validate their model. It was also concluded that the heat-treatment and simulated body fluid exposure had a significant effect on the residual strain profiles in the top layers of the HA coating. Further information: [6] [7] Large scale engineering component – Helping UK magnesium producer with casing problem Magnesium Elektron, Manchester is a world leader in magnesium technology and alloy development. Their alloys are extensively used in the aerospace and automotive industries. For magnesium to be a financially viable alternative to aluminium, the company need to be able to mass produce it. However, a significant level of cold cracking has been observed within direct chill (DC) cast, high-strength magnesium alloy Elecktron WE43 in production of large slabs. These cracks have been attributed to the formation of significant residual stresses during casting. A finite-element modelling code has been used to predict the residual stress within the DC-cast slab. Measurements at Engin-X allowed the residual stress within the slab to be mapped in detail (Figure 4). The information is used to refine the computer simulation of DC casting. Magnesium Elektron is now able to successfully cast the slabs without cracks. Further information: [8] Tomography driven diffraction – Studying Renaissance bronze statuettes An attractive feature of neutron techniques is the ability to identify hidden materials and structures inside engineering components and objects of art and archaeology. Having this in mind we are investigating a new technique, Tomography Driven Diffraction, which exploits tomography data to guide diffraction experiments on samples with complex structures and shapes. This technique has been successfully applied for the measurements on engineering (e.g. turbine blades) and art objects (e.g. a Renaissance bronze statuette). As shown in Figure 5, neutron tomography at the Paul Scherrer Institut in Switzerland was used to reveal the internal structure of a Renaissance statuette from the Rijksmuseum, a ‘Striding Nobleman’, and provided an indication of different material compositions. Incorporating the tomography model into the SScanSS software tool allowed many aspects of the experiment to be

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Figure 5

(a) Contrabas Spelende Man (Striding Nobleman), Rijksmuseum Amsterdam, Inv. BK-16083. The statuette is about 35 cm high. (b) Slices of neutron tomography data of the Striding Nobleman. (c) Neutron analysis points selected within the SScanSS virtual model.

(b)

planned in advance, including the accurate specification of the measurement locations. Diffraction measurements on Engin-x can be made to study the material compositions and crystalline structures of the bronze with a millimetre-sized gauge volume placed at any selected point within the object. Analysis of the statuette gave evidence of the different copper alloy compositions of superficial and internal parts, but also showed small amounts of ferrite present, which until recently was not reported for Renaissance bronzes. A combined application of neutron techniques thus provided a better understanding of the sculpture production methods, thereby advancing the analytical studies of these museum objects. Further information: [9][10][11] In-situ loading at high temperature – Evidence of variation in slip mode in a polycrystalline nickel-base superalloy with change in temperature In order to increase the operating temperature in turbine engines, a new generation of nickel-base superalloys has been developed for disk applications containing a significantly higher volume fraction of γ’ than previous superalloys. Understanding the deformation mechanisms is critical in these alloys, since it is necessary to ensure good tensile strength and fatigue properties alongside improved creep resistance. The deformation mechanisms under tensile loading in a 45 vol.% c γ’ polycrystalline nickel-base superalloy have been studied using Engin-X at 20oC, 400oC, 500oC, 650oC and 750oC (Figure 6). The data demonstrate

(c)

that changes of the γ’ slip mode from {111} to {100} with increasing temperature. Between room temperature and 500oC there is load transfer from γ’ to γ, indicating that γ’ is the softer phase. At higher temperatures, opposite load transfer is observed indicating that the γ matrix is softer. At 400oC and 500oC, an instantaneous yielding increment of about 2% was observed, after an initial strain of 1.5%. This instantaneous straining coincided with zero lattice misfit between γ and γ’ in the axial direction. Further information: [5] In-situ loading at low temperature – The origins of transformation plasticity in carbon steel TRIP steels are becoming increasingly exploited for industrial applications because they show high strength and high uniform elongation (ductility). Despite this interest, the relative contributions of the different strengthening and straining mechanisms are often poorly understood. Neutron diffraction using Engin-x was employed to quantify the contribution of different mechanisms to ductility and work hardening for a 0.25wt%C steel. Differences in the stress-strain response at different temperatures are related to the extent of the transformation of metastable austenite into martensite during deformation. In Figure 7, the fraction of austenite during tensile deformation is plotted against stress and strain at the three test temperatures. For room temperature, 10% strain decreases the amount of austenite by half, while the transformation is not complete even after 20% strain. By contrast, at -50oC straining quickly gives rise to significant transformation,

Research Infrastructures

even during the macroscopically elastic regime. By approximately 7% strain, the transformation is complete. The response to straining at -100oC is essentially the same as at -50oC. At the low plastic strains, the transformation contributes almost half to the total strain for deformation at low temperature, explaining the relatively low work hardening compared to room temperature straining. Subsequent deformation at room temperature after pre-straining at -50oC results in larger work hardening than for solely room temperature straining due to the higher martensite levels formed at -50oC. This load sharing effect is similar to work hardening in a composite containing a strong constituent in a soft matrix. Further information: [12]

the part, particularly during quenching. Annealing is often used on each component in order to relax these stresses. However it is not known how quickly stresses relax during the annealing process. The experiment carried out at Engin-X is to study ‘in-situ’ the effect of annealing on relaxing residual stresses generated during quenching. The experiment required heating and then holding the sample at an ageing temperature while measuring strain using neutron diffraction. It was found that the initial stress relaxation was rapid, approximately 200 MPa in 15–30 min, with a slower linear relaxation continuing after this for the rest of the ageing heat treatment. This behaviour suggests creep may be the means by which stress relaxation takes place in this material during ageing. Further information: [14]

Figure 7

In-situ machining – Stresses due to electro-discharge machining Engin-x enables the stresses evolved in real engineering processes to be studied in –situ and often in real time. Electro-discharge machining (EDM) is such a process which is important in a wide range of engineering applications. These applications assume that EDM process is itself stress free. It is important to test this assumption. To this end, Engin-X has been used to measure insitu the strains generated by EDM. The results confirmed that although the EDM process introduced high elastic thermal strains, it did not generate any additional residual stresses. Further information: [13] In-situ heat treatment – Stress relaxation through ageing heat treatment In forgings, the residual stresses develop due to the component geometry setting up significant variations of cooling rates across

Change in the austenite fraction during straining at room temperature, -50°C and -100°C determined by neutron diffraction displayed as a) a function of strain and b) a function of applied stress.

Outlook After 10 years of operating, Engin-X continues to be in high demand. Engin-X has attracted wide interest beyond traditional materials engineering, and now the user community has expanded to include geology, biomechanics and cultural heritage. As the demand for new materials and techniques increases to meet the global energy challenge, the in-depth understanding of material performance becomes more critical. Engin-X has continuously defined the frontier of stress measurements through investment in state-of-the-art equipment to alter the conditions under which experiments are carried out. For example, EdF Energy and its university partners, Open University and Bristol University together with ISIS have started a project to build a creep rig for long time-base experiments, which none of the instrument around the world has this capability yet. Industry involvement is essential for the future of neutrons scattering, and Engin-X is pursuing this approach. We have provi-

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ded a free initial ‘consultancy’ for many companies on the use of neutron facilities. ISIS has launched a new Industry Collaborative R&D scheme in October 2011. The aim of the scheme is to widen the use of ISIS by industry in order to increase the economic benefit that ISIS contributes to the UK. This scheme has also become one of the important funding sources for ISIS. Engin-X has also become the most popular instrument for the scheme. Within one year, ISIS has signed Collaborative R&D agreements with Rolls Royce (three different projects), EdF Energy, Boeing, Tata Steel, TWI, a consortium of oil and gas companies, a consortium of railway companies, etc. Because of the increasing demand for Engin-X from industry and the user community, the experiment proposal over-subscription rate has been increasing and is now at the highest rate for the last 10 years. In order to enhance the neutron imaging capabilities at ISIS and to complement the existing materials analysis facilities, the first neutron tomography instrument at a pulsed neutron source is being built for the ISIS second target station. The new instrument for materials science & engineering imaging, IMAT [15], will be a stateof-the-art combined instrument for cold neutron radiography and diffraction analysis for materials science, materials processing, and engineering studies. The instrument will provide the largest possible neutron flux available for imaging at ISIS and will allow mediumresolution neutron “colour” imaging and diffraction. The ability to perform imaging and diffraction studies on the same beamline with a single sample set-up will offer unprecedented opportunities for a new generation of neutron studies. With IMAT being built, and continuing research, development and investment, ISIS will continue to be at the forefront of material science and engineering research.

Acknowledgements The success of the 10 years operation of Engin-X is owned to all the instrument scientists that have worked on the instrument especially those who have built and developed the instrument: Mike Johnson, Mark Daymond, Jude Dunn, Ed Oliver, Javier Santisteban and Ania Paradowska, all the support stuff at ISIS and more importantly the user community, who have been working with us to produce science of the highest quality.

References [1] M. T. Hutchings, P. J Withers, T. M. Holden and T. Lorentzen, Introduction to the Characterization of Residual Stress by Neutron Diffraction. Boca Raton: CRC Press, Taylor and Francis (2005). [2] J. R. Santisteban, M. R. Daymond, J. A. James and L. Edwards, ENGIN-X: a third-generation neutron strain scanner, J. Appl. Cryst. 39, 812–825 (2006).

[3] S. Y. Zhang, et al. “Materials engineering - High-tech composites to ancient metals”, Materials Today 12 (7-8) 78-84 (2009) [4] J.A. James and L. Edwards, Application of robot kinematics methods to the simulation and control of neutron beam line positioning systems. Nuclear Instruments and Methods in Physics Research A. (2007) 571, 709-718. [5] M.R. Daymond, M. Preuss and B. Clausen, Evidence of variation in slip mode in a polycrystalline nickel-base superalloy with change in temperature from neutron diffraction strain measurements, Acta Materialia 55 (2007) 3089–3102 [6] R. Ahmed, N. H. Faisal, R. L. Reuben, A. M. Paradowska, M. E. Fitzpatrick, ‘Residual strain and fracture response of Al2O3 coatings deposited via APS and HVOF techniques’, J. Thermal Spray Technol:2012:21(1):23-40. DOI: 10.1007/s11666-011-9680-7 [7] R. Ahmed, N. H. Faisal, A. M. Paradowska, M. E. Fitzpatrick, K. A. Khor, ‘Neutron diffraction residual strain measurements in nanostructured hydroxyapatite coatings for Orthopaedic Implants’, J. Mechanical Behaviour of Biomedical Materials: 2011:4(8):2043-2054.doi:10.1016/j.jmbbm.2011.07.003 [8] M Turski, A Paradowska, S. Y. Zhang, D Mortensen, H Fjaer, J Grandfield, et al, Validation of Predicted Residual Stresses within Direct Chill Cast Magnesium Alloy Slab, Metall Mater Trans A 43A (5) 1547-1557 (2012) [9] R van Langh, J. James, G. Burca, W. Kockelmann, S. Y. Zhang, E. Lehmann, M. Estermann, A. Pappot, New insights into alloy compositions: studying Renaissance bronze statuettes by combined neutron imaging and neutron diffraction techniques, Journal of Analytical Atomic Spectrometry, 2011,26, 949-958 [10] G Burca, J James, W Kockelmann, M Fitzpatrick, S. Y. Zhang, J Hovind, et al, A new bridge technique for neutron tomography and diffraction measurements, Nucl Instrum Meth A Volume 651, Issue 1, Pages 229–235 [11] S. Pierret, A. Evans, A.M. Paradowska, A. Kaestner, J. James, T. Etter and H. VanSwygenhoven, Combining neutron diffraction and imaging for residual strain measurements in a single crystal turbine blade, NDT&E International 45 (2012) 39–45 [12] R.J. Moat, S. Y. Zhang, J. Kelleher, A.F. Mark, T. Mori and P.J. Withers, Work hardening induced by martensite during 3 transformation-induced plasticity in plain carbon steel, Acta Materialia, in press [13] S Hossain, et al., Mat. Sc. And Eng. A 373 (2004) 339 [14] J. Rolph, A. Evans, A. Paradowska, M. Hofmann, M. Hardy and M. Preuss, Stress relaxation through ageing heat treatment – a comparison between in situ and ex situ neutron diffraction techniques, C. R. Physique 13 (2012) 307–315 [15] W. Kockelmanna, SY. Zhang, J.F. Kelleher, J.B. Nightingale, G. Burca and J.A. James, IMAT – a new imaging and diffraction instrument at ISIS, Physics Procedia, in press (2012)

School and Meeting Reports

International Neutron Scattering Instrumentation School (INSIS) Beyond the several neutron scattering schools held around the world every year the core business of the INSIS school is the training of young researchers about neutron scattering instrumentation. The school aims to educate students in some of the nuances of neutron instrumentation design and train them about the background knowledge behind the realization of neutron instrumentation. The school offered two weeks of full immersion about neutron scattering instrumentation. In the first week students gained a comprehensive grounding in modern instrumentation issues at both steady state and pulsed neutron sources and had the opportunity to hear about the latest research being carried out with the techniques at international neutron facilities. Instrumentation lectures addressed basics on design and construction concepts about neutron sources, diffractometers, three axis spectrometers, time of flight inelastic instruments (instrumentation using thermal and epithermal neutrons), reflectometers, filter spectrometers, Larmor labelling and sample environment equipments. In addition there were lectures on data acquisition and treatment and constructability. The topics were backed up by hands-on Monte Carlo tutorials using McStas. These also represented a unique opportunity to discuss the course material with the lecturers, to work through examples drawn from the course material and to share research experiences. The second week focused on a particular technical issue, a specialized course on neutron detectors. The latter choice is very timely given the worldwide shortage of helium-3 detectors coupled with a desire for everlarger pixelated detectors. Thus the second week, organized by Erik Schooneveld

and Giuseppe Gorini, addressed technical issues about gaseous, solid state, scintillator detectors as well as signal read out, acquisition and processing. In addition to lectures, students followed practical work, detailed examination of a number of pieces of radiation detection hardware (High Purity Germanium, Single-crystal Diamond Detector, Scintillators, Light sensors, 3He tube resistive wire electronics, Digitizer Data processing, GEM detectors). The welcome ceremony of the INSIS edition was held in the concert hall at the Pontificio Istituto di Musica Sacra where participants were invited to attend the concert of Maestro Adolfo Barabino, http://silo.lnf.infn.it/pub/INSIS/1507-concert/.

The school welcomed a total of 42 students, 36 attended the first week of the school, a total of 25 attended the second week. A total number of 19 students stayed for both weeks of the school, the others came for only one week. Students came from Asia, Europe and the Americas, almost equally distributed among the three continents. Most of the students had some background in neutron scattering either because they were graduate students using the technique or because they were young scientists or PhD’s at a neutron facility. We had about 10 more applicants than we were not able to accommodate. This first year’s school was held at the INFN in Frascati, near Rome (Italy), in the period July 15 – 27, 2012. The school was supported by directors of

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

School and Meeting Reports

the worldâ&#x20AC;&#x2122;s major neutron facilities, which agreed to support the travel costs of lecturers from their facilities, by NMI3, NSF (US) and CNR (I) and INSN(I). A daily streaming service and record of all lectures was provided during both weeks of INSIS school. Most of the participants were housed in lodgings belonging to the INFN that are used for visiting scientists carrying out experiments there. Lunches and dinners were a vibrant opportunity for participants and lecturers to interact daily and informally. An exhaustive list of topics along with files containing the viewgraphs used by the lecturers can be found on the school website http://info.ornl.gov/sites/insis/default.aspx. Videos of the lectures will be added soon. In future INSIS schools, the structure of the first week will be maintained more or less the same while the content of the second week might change from year to year. Based on the student survey, posted on the INSIS web site, we have decided to continue to offer this school

in future, with the next school to be organized by ISIS, possibly as early as next year. I. S. Anderson (ORNL), Carla Andreani (University of Rome Tor Vergata and CNR-IPCF), M. Arai (J-PARK), R. McGreevy (ISIS), A. Harrison (ILL), R. Pynn (Chair, Indiana University of Bloomington)

International Committee: Ian Anderson (ORNL), Carla Andreani (University of Rome Tor Vergata and CNR-IPCF), Masa Arai (J-PARC), G. Gorini (University of Milano Bicocca and CNR-IFP), Andrew Harrison (ILL), Robert McGreevy (ORNL), Roger Pynn - Chair (University of Indiana). Local Organizers: Carla Andreani â&#x20AC;&#x201C; Chair (University of Rome Tor Vergata and CNR-IPCF), Daniela Ferrucci (INFN), Giovanni Mazzitelli (INFN), Massimo Pistoni (INFN), Giovanni Romanelli, Roberto Senesi (University Rome Tor Vergata and CNR-IPCF)1 School Office: Sandra Fischer Sponsored The school was supported by CNR (I), ILL (F), ISIS (UK), INFN (I), J-PARC (J), NMI3 (EU), NSF (US), ORNL (US), SoNS (I). The school was hosted by the INFN in Frascati (Rome, I).

School and Meeting Reports

The Third Meeting of the Union for Compact Accelerator-driven Neutron Sources Chun-K. Loong Sun Yat-Sen University, China

Following Beijing in 2010 (UCANS-I see Neutron News 22(1), strial applications of CANS (e.g., novel detectors, imaging and 2011) and Bloomington in 2011 (UCANS-II, Notiziario Neutroni radiography, fast-neutron-induced single event effects, boron e Luce di Sincrotrone 17(1), 2012), the city of Bilbao, Spain, wel- neutron capture therapy, neutron dosimetry by Bonner Sphere comed 60 scientists and engineers from 8 countries to convene spectrometry, and procurement of nuclear data). Other presenthe third meeting, UCANS-III, during July 31-August 3, 2012. tations (e.g., on neutron generation by novel lasers, acceleratorThe program, featuring nearly 50 talks and posters, covered the driven system for transmutation, and outreach activities to emareas of accelerator and moderator-target systems for compact brace the materials research community) added witness to the neutron sources, instrumentation, scientific and industrial appli- cross-disciplinary hallmark of UCANS, which undoubtedly will cations, and future development. Additionally, the participants continue in the future meetings. toured the ESS-Bilbao facilities in Zamudio and a nearby indu- The Proceedings of UCANS-III will be published in the Physics stry park where companies have undertaken engineering design Proceedings series by Elsevier and UCANS-IV will be held at and manufacture of scientific instruments including compo- Hokkaido, Japan during September 23-26, 2013. nents for accelerators and neutron scattering. While keeping the tradition of reporting the status of on-going operation and construction of compact accelerator-driven neutron sources (CANS) (e.g., the CPHSTsinghua U and PKUNIFTY of China, DAFNE of INFNRome of Italy, ESS-Bilbao of Spain, HUNS-Hokkaido U of Japan, and the small accelerator sources at Centro At贸mico Bariloche of Argentina and at RIKEN of Japan), UCANS-III forwarded a dialogue between compact, low-to-medium power sources with the large, high-power sources such as the ESS, J-PARC, and SNS of synergetic roles on target, moderator, and scattering instrumentation R&D. The increasing interest in compact neutron sources is reflected in the expanded coverage and The Organizing Committee took the opportunity of the conference dinner to reflect on past activities and contemplate an update of scientific and induexpanding scope in future UCANS meetings.

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

School and Meeting Reports

Shull Fellows now launched on interesting and fulfilling careers Agatha Bardoel Neutron Sciences Directorate, Oak Ridge National Laboratory, USA Photos by Genevieve Martin Neutron Sciences Directorate, Oak Ridge National Laboratory, USA

“Unique power of neutrons” opened a new window on proteins, materials “The beauty of the Shull Fellowship is the freedom to explore and develop your own scientific interests.” Chris Stanley, 2007 Shull Fellow

tron scattering include condensed matter physics, chemistry, materials science and engineering, and biology. The award was named for ORNL neutron scientist and Massachusetts Institute of Technology (MIT) professor Clifford Shull, who with Bertram Brockhouse of Canada was awarded the 1994 Nobel Prize in Physics. Shull won the award for his pioneering work in neutron scattering, a technique that reveals where atoms are and how they behave within a material. The first two Shull Fellowships were awarded in 2006 to Andrew Christianson, who received his PhD in Physics from Colorado State University, and Wei-Ren Chen, a PhD graduate in Nuclear Science and Engineering from MIT. Both completed their terms and became staff research scientists at ORNL. The 2007 Fellowships were awarded to

Christopher Stanley, a PhD graduate in Polymer Science and Engineering from the University of Massachusetts, Amherst, and Sylvia McLain, a PhD graduate in Chemistry from the University of Tennessee, Knoxville. Olivier Delaire, a PhD in Materials Science from the California Institute of Technology was the 2008 Shull Fellow; Xianglin Ke (PhD in Physics, University of Wisconsin-Madison) followed in 2009; Yang Zhang (PhD, Nuclear Science and Engineering, MIT) was the Shull Fellow in 2010; and in 2011, ORNL welcomed Yongqiang Cheng (PhD, Johns Hopkins University). Wei-Ren Chen, the 2006 winner, went on to win a national Early Career Award in 2012 for his proposal to use theory, computation, and neutron scattering to characterize the structure and dynamics of soft matter. “The Shull award at the beginning of my

The Neutron Sciences Directorate’s prestigious Clifford G. Shull Fellowship, a twoyear research appointment at Oak Ridge National Laboratory (ORNL), is now inviting applications from early career scientists. The next Fellow hired will be the ninth since the program’s inception in 2006. With the world’s most intense pulsed accelerator-based neutron source at the Spallation Neutron Source (SNS) and a world-class continuous neutron source at the High Flux Isotope Reactor (HFIR), ORNL aims to be among the world leaders in neutron science. Both facilities are funded by the US Department of Energy (DOE) Office of Basic Energy Sciences. The Fellowship Program attracts new scientific talent, making it possible for outstanding early career scientists During a visit to SNS in November 2012, Clifford Shull’s son Robert (right) met with several former and current Shull Fellows to launch their careers. The and showed them his father’s Nobel Prize (left to right): Andy Christianson, Chris Stanley, and Yongqiang Cheng. Robert Shull research areas that use neu- is also a recognized scientist and leads the Magnetic Materials Group at the National Institute of Standards and Technology.

School and Meeting Reports

career provided me with the critical degree of freedom for my research of soft colloids,” Chen says. “It greatly helped me to obtain the Early Career Award funding from the Department of Energy this year.” Chen, who enjoys classical music and reading history in his spare time, says the freedom to choose his own research topics, the neutron scattering beam time, and ORNL’s immense computational resources have been key to his research success. “The beauty of the Shull Fellowship is the freedom to explore and develop your own scientific interests,” says 2007 Fellow Chris Stanley. Stanley developed a collaboration with Valerie Berthelier at the University of Tennessee Medical Center in Knoxville. The two researchers use neutrons to characterize the earliest structures formed by the huntingtin protein implicated in Huntington’s disease, a genetic neurological disorder. Using the high flux of the smallangle neutron scattering (SANS) beam lines at HFIR, they measured normal and pathological peptides and are now beginning to identify structural differences that could be important in this disease. Stanley, now an instrument scientist on the EQ-SANS (Extended Q-Range SANS) instrument at SNS, is also using EQ-SANS for his work, as its event mode of data collection affords advantages for performing measurements on protein structural dynamics. Sylvia McLain, co-fellow with Stanley in 2007, has since settled in the UK, where she is a UK Engineering and Physical Sciences Career Acceleration Fellow at the University of Oxford. “At Oxford, I work in the Department of Biochemistry, where I have a research group that includes a postdoc, a PhD student, and a master’s student, with another postdoc on the way,” McLain says. The East Tennessee native investigates

the structure and dynamics of biological of time thinking and reading about this molecules in solution on the atomic scale. when I can,” McLain says. She has recently published a high-impact Olivier Delaire, the 2008 Shull Fellow, paper in Angewandte Chemie on the association of peptides in solution as a model for protein folding and another in PloSONE on the structure of a cellulose precursor in solution. The 2007 Shull Fellowship helped McLain expand her research to include more computation, she says, and to investigate the biophysics behind molecule association, which is important in any life-giving process. “Fellowships of this type are always beneficial because you are awarded funding to do your own research, which is essential in establishing a scientific career.” How is she fin- In the SNS Executive Conference Room, Robert Shull and Associate Laboratory Director for ding life abro- Neutron Sciences Kelly Beierschmitt look at photos of Clifford Shull and colleague Ernest ad? “I don’t have many hobbies is now a staff scientist in the Neutron these days, other than eating, potteand X-Ray Scattering Group in the Maring around my garden, and reading in my spare time, though I do blog about terials Science and Technology Division science and science policy and write at ORNL. “The Shull Fellowship was for for a UK national newspaper. I am very me a wonderful opportunity to grow interested in the history and philoso- as an independent scientist and take phy of science, so I try to spend a lot advantage of the world-class resources

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

r t

School and Meeting Reports

at ORNL,” says Delaire, who works on

rials, semiconductors for microelectronics, photovoltaics, and thermal barrier coatings). technologies. “Phonons also interact with electrons and other elementary excitations in solids, resulting in interesting physics with useful applications for ferroelectrics, polarons, superconductivity, and multiferroics,” he says. Having the Shull Fellowship meant having the freedom to establish his own research directions, as well as the opportunity to collaborate with outstanding scientists across different divisions at ORNL. “The interaction with scientists at SNS and HFIR also helped me to quickly gain expertise with techniques that I had not previously Wollan as they worked at the Oak Ridge Graphite Reactor circa 1945. Nobel Laureate Clifford Shull is often referred to in the scientific community as the “father of neutron scattering.” been exposed to, such as working He investigates the fundamentals of ato- with single-crystals.” mic dynamics related to the transport of Delaire says he developed collaborations both within ORNL and in the broader energy at the microscopic level. Quanscience community as a collaborating tum vibrations of atoms in crystalline principal investigator for a DOE-funded lattices (phonons) are responsible for the Energy Frontier Research Center. The transport of heat in semiconductors or work has led to several high-impact reseinsulators (such as thermoelectric mate- arch papers. materials that can be used for energy

When he is not working, Delaire enjoys the proximity of the Smoky Mountains for photography, hiking, and kayaking. Xianglin Ke, the 2009 Shull Fellow, has moved on to a tenure-track assistant professorship in the Department of Physics and Astronomy at Michigan State University. Ke works in experimental condensed matter physics and studies complex oxide materials, for which neutron scattering is a powerfully efficient tool. “The neutron is a uniquely powerful ‘microscope’ that allows us to ‘see’ the atoms and molecules,” comments Yang Zhang, the 2010 Shull Fellow, whose field is soft and disordered matter. He is now an assistant professor in the Department of Nuclear, Plasma, and Radiological Engineering, University of Illinois at UrbanaChampaign. “Many of the amazing discoveries in the microscopic world are yet to come. It is a golden time for neutron scattering. The Shull Fellowship provides you with an opportunity to unleash your imagination,” Zhang says. Zhang too continues his ties with ORNL from his new home in Illinois, with collaborations on neutron scattering experiments at SNS and HFIR. Why should one apply for the Shull Fellowship? “SNS is the most intense pulsed accelerator-based neutron source in the world, and HFIR is a world-class reactor-based continuous source. ORNL also has the most powerful supercomputer in the world. Finally, the Shull Fellowship is the most prestigious fellowship in the neutron scattering field,” Zhang says. For more information about the Shull Fellowship, see: neutrons.ornl.gov/shullfellowship

Call for proposal

Call for proposal [Deadlines for proposal submission]

Neutron Sources

Neutron Sources Sy http://nmi3.eu/about-nmi3/access-programme/facilities---submit-a-proposal.html To be announced

ANSTO

http://www.ansto.gov.au/research/bragg_institute/users/call_for_proposals

May 15, 2013

(for August-December cycle)

March 1 and September 1, annually

BNC – AEKI Budapest Neutron Centre

http://www.bnc.hu/modules.php?name=News&file=article&sid=39

BER II – Helmholtz-Zentrum Berlin

http://www.helmholtz-berlin.de/user/neutrons/user-info/call-for-proposals_en.html#c63361

Any time

CINS - Canadian Institute for Neutron Scattering http://www.cins.ca/beam.html#apply

January 25, 2013

FRM-II – Forschungs-Neutronenquelle Heinz Maier Leibnitz http://www.frm2.tum.de/en/user-office

March 6, 2013

(for July-December cycle)

To be announced

HFIR – Oak Ridge National Laboratory http://neutrons.ornl.gov/

ILL - Institut Laue-Langevin

http://www.ill.eu/users/important-dates/

To be announced

ISIS – Rutherford Appleton Laboratory

http://www.isis.stfc.ac.uk/apply-for-beamtime/apply-for-beamtime2117.html

January 25, 2013

JCNS - Jülich Centre for Neutron Science

http://www.fz-juelich.de/jcns/DE/Leistungen/Userinfos3/_node.html

Twice a year, to be announced

LANSCE – Los Alamos National Laboratory http://lansce.lanl.gov/uresources/proposals.shtml

Mai 1 and November 1, annually Any time

LLB - Laboratoire Léon Brillouin

http://www-llb.cea.fr/en/Web/avr2000_e.php

NPL – Neutron Physics Laboratory

http://neutron.ujf.cas.cz/en/instruments/user-access/nmi3

Any time

RID - Reactor Institute Delft

http://tnw.tudelft.nl/index.php?id=33195&L=1

May 15, 2013

SINQ - Swiss Spallation Neutron Source http://www.psi.ch/sinq/call-for-proposals

March 6, 2013 (for July-December cycle )

SNS – Oak Ridge National Laboratory http://neutrons.ornl.gov/

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

Call for proposal

Synchrotron Radiation Sources

n s ynchrotro Radiatio www.lightsources.org

March 6, 2013

(General User Proposals for August–December cycle)

ALS - Advanced Light Source

http://www-als.lbl.gov/index.php/component/content/article/58.html

Any time

(Rapid Access Proposals)

June 30 and January 15, annually

(for the scheduling periods October-March

ANKA - Institute for Synchrotron Radiation

http://ankaweb.fzk.de/website.php?page=userinfo_guide&id=1#subpart2

and April-September, respectively)

APS - Advanced Photon Source

March 8, 2013

http://www.aps.anl.gov/Users/Calendars/GUP_Calendar.htm

(2013-2: for the period between May and August 2013)

July 12, 2013

(2013-3: for the period between October and December 2013)

February 13, 2013

(for the period between May and September 2013)

AS - Australian Synchrotron

http://www.synchrotron.org.au/index.php/features/applying-for-beamtime/proposal-deadlines

June 5, 2013

(for the period between September and December 2013)

March 1 and September 1, annually

BESSY II – Helmholtz-Zentrum Berlin

http://www.helmholtz-berlin.de/user/beamtime/proposals/index_en.html

Any time

BSRF - Beijing Synchrotron Radiation Facility

http://english.ihep.cas.cn/rs/fs/srl/usersinformation/callforproposals/201203/ t20120329_83307.html

January 31, 2013

(For the period between May and August 2013)

CFN - Center for Functional Nanomaterials

http://www.bnl.gov/cfn/user/User_Program_Overview.asp

May 30, 2013

(for the period between September and December 2013)

Proposals are accepted at any time

CHESS - Cornell High Energy Synchrotron Source http://www.chess.cornell.edu/prposals/index.htm

February 27, 2013

(For the period between July and December 2013)

March 8, 2013

CLS - Canadian Light Source

http://www.lightsource.ca/uso/call_proposals.php

CNM - Center for Nanoscale Materials

http://nano.anl.gov/users/call_for_proposals.html

April 1, 2013

Diamond - Diamond Light Source

http://duo.diamond.ac.uk/propman/duo/main/home?execution=e1s1

March 15, 2013

(For the period between July and December 2013)

March 1, 2013

(for the period between August 2013 and February 2014)

January 15, 2013

(for Long-Term Project (LTP) applications)

ELETTRA

https://vuo.elettra.trieste.it/pls/vuo/guest.startup

ESRF - European Synchrotron Radiation Facility http://www.esrf.eu/UsersAndScience/UserGuide/Applying

FELIX - Free Electron Laser for Infrared experiments http://www.rijnhuizen.nl/felix/beamtime/

Call for proposal Synchrotron Radiation Sources

To be announced

FOUNDRY - The Molecular Foundry https://isswprod.lbl.gov/TMF/login.aspx

To be announced

HASYLAB – Hamburger Synchrotronstrahlungslabor at DESY http://hasylab.desy.de/user_info/write_a_proposal/2_deadlines/index_eng.html

To be announced

ISA - Institute for Storage Ring Facilities http://www.isa.au.dk/user/access.asp

Synchro Radiatio Ca January 15, 2013

LCLS - Linac Coherent Light Source

http://www-ssrl.slac.stanford.edu/lcls/users/

To be announced

LNLS - Laboratório Nacional de Luz Síncrotron http://www.lnls.br/blog/category/news/

To be announced

MAX-lab

https://www.maxlab.lu.se/calls

January 31, 2013

(for the period between May and August 2013)

To be announced

NSLS - National Synchrotron Light Source https://pass.nsls.bnl.gov/deadlines.asp

NSRRC - National Synchrotron Radiation Research Center http://portal.nsrrc.org.tw/index.php

To be announced

PAL

http://paleng.postech.ac.kr/

Proposal submission system has been newly launched To be announced

PF - Photon Factory

http://pfwww.kek.jp/users_info/users_guide_e/

SLS - Swiss Light Source http://www.psi.ch/sls/calls

February 15, 2013

For standard proposal for the period between July and December 2013

SOLEIL

http://www.synchrotron-soleil.fr/portal/page/portal/Recherche/SUN

For the period between January 2014 and January 2015

To be announced

SPring-8

http://www.spring8.or.jp/en/users/proposals/

January and July, annually

SRC - Synchrotron Radiation Center

http://www.src.wisc.edu/users/apply_for_beamtime_IR.htm

January 22, 2013

(Crystallography Proposals for March-May scheduling)

SSRL - Stanford Synchrotron Radiation Lightsource

http://www-ssrl.slac.stanford.edu/content/user-resources/ssrl-deadlines

February 15, 2013

(Xray/VUV Proposals for May-July scheduling)

April 20, 2013 (Crystallography Proposals for June-July scheduling) August 15, 2013

(Xray/VUV Proposals for November-February scheduling)

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

Calendar January 14 – 17, 2013

Mumbai, India International Symposium on Neutron Scattering http://www.barc.gov.in/symposium/isns2013/

January 21 – 22, 2013

Gif-sur-Yvette, France SYREES 2013: Synchrotron Radiation for Electrochemical Energy Storage  http://www.synchrotron-soleil.fr/Soleil/ToutesActualites/Workshops/2013/SYREES-2013/Welcome

otron on Source Calendar January 23 – 24, 2013

Gif-sur-Yvette, France 8th SOLEIL Users’ Meeting

http://www.synchrotron-soleil.fr/Soleil/ToutesActualites/Workshops/2013/SUM2013/Accueil

January 23 – 25, 2013

Grenoble, France Flipper 2013 - International Workshop on Single-Crystal Diffraction with Polarised Neutrons http://www.ill.eu/news-events/events/flipper-2013/

January 23 – 25, 2013

Hamburg, Germany European XFEL Users’ Meeting 2013 http://www.xfel.eu/2013-users-meeting/

February 4 – 6, 2013

Grenoble, France ESRF Users’ Meeting 2013 & Associated Workshops www.tinyurl.com/dy2q6r2

February 11 – 15, 2013

Vienna, Austria The 13th Vienna Conference on Instrumentation http://vci.hephy.at

February 13 – 15, 2013

Lund, Sweden IKON 4

http://ess-scandinavia.eu/news/35-news/594-first-announcement-ikon3-and-ikon4

February 28 – March 8, 2013

Berlin, Germany 33rd Berlin School on Neutron Scattering

http://www.helmholtz-berlin.de/events/neutronschool/

March 5 – 14, 2013

Didcot, UK ISIS Neutron Training Course

http://www.isis.stfc.ac.uk/learning/neutron-training-course/

March 12 – 14, 2013

Oak Ridge, USA High Resolution Neutron Scattering to Measure Slow Dynamics (MELODY) http://neutrons.ornl.gov/calendar/

March 18 – 19, 2013

Oxford, UK The Impact and Future Directions of Scattering Techniques in Soft Matter http://www.rsc.org/ConferencesAndEvents/conference/alldetails.cfm?evid=111563

March 18 – 22, 2013

Grenoble, France ADD2013 - School and Conference on Analysis of Diffraction Data in Real Space http://www.ill.eu/ADD2013/

March 25 – 27, 2013

Grenoble, France ESS Science Symposium on Neutron Particle Physics at Long Pulse Spallation Sources http://www.ill.eu/news-events/events/nppatlps-2013/

April 1 – 5, 2013

San Francisco, USA MRS Spring Meeting http://www.mrs.org/spring2013/

Calen dar alendar N Calendar

April 2 – 5, 2013

Geneva, Switzerland Probing Macromolecules at Water-Solid Interfaces – School on Surface Analytical Techniques http://cm1101.unige.ch/

April 7 – 20, 2013

Oak Ridge and Argonne, USA National School on Neutron and X-Ray Scattering (tentative) http://jins.tennessee.edu/events/

May 13 – 17, 2013

Shanghai, China 2013 International Particle Accelerator Conference (IPAC’13) http://www.aps.org/meetings/meeting.cfm?name=IPAC13

May 26 – 29, 2013

Nagoya, Japan 4th International Symposium on Diffraction Structural Biology http://www.sbsp.jp/ISDSB2013/homepage/index.html

June 20 – 21, 2013

Berlin, Germany General Assembly NMI3-II 2013

http://nmi3.eu/about-nmi3/education.html?back=yes

July 2 – 5, 2013

Munich, Germany International Workshop on Neutron Optics and Detectors http://www.iucr.org/news/notices/meetings/meeting_2012_299

July 08 – 12, 2013

Edinburgh, Scotland 2013 International Conference on Neutron Scattering http://www.icns2013.org/

August 17 – 23, 2013

Zuoz, Switzerland 12th PSI summer school on condensed matter physics http://www.psi.ch/summerschool

September 9 – 12, 2013

Garching, Germany 1st International Conference on Neutron Imaging and Neutron Methods in Archaeology and Cultural Heritage Research http://www.frm2.tum.de/indico/conferenceDisplay.py?confId=3

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

ndar Facilities

Neutron Sources

WWW SERVERS IN THE WORLD http://nmi3.eu/neutron-research/where.html ANSTO Australian Nuclear Science and Technology Organization

FLNP Frank Laboratory of Neutron Physics

Phone: + 61 2 9717 3111

Fax: (7-49621) 65-085

Fax: + 61 2 9543 5097

Email: belushk@nf.jinr.ru

Http://www.ansto.gov.au/home

Http://flnp.jinr.ru/25/

BER II Helmholtz Zentrum Berlin

FRM II Forschungs-Neutronenquelle Heinz Maier-Leibnitz

Type: Swimming pool reactor. 10 MW Phone:

+49-30 / 80 62 - 42778

Phone: (7-49621) 65-657

Type: Compact 20 MW reactor

Fax: +49-30 / 80 62 – 42523

Phone: +49 (0) 89 289 10794

Email: neutrons@helmholtz-berlin.de

Fax: +49 (0) 89 289 10799

Http://www.helmholtz-berlin.de/user/neutrons/

Email: userinfo@frm2.tum.de Http://www.frm2.tum.de/en/user-office

Neutron Scatte BNC - Budapest Research reactor Fax: +36 1 395 9162

GEMS German Engineering Materials Science Centre Helmholtz Zentrum Geesthacht

Email: tozser@sunserv.kfki.hu

Phone: +49 4152 871254

Http://www.kfki.hu/brr/indexen.html

Fax: +49 4152 871338

Type: Swimming pool reactor, 10MW Phone: +36 1 392 2222

CAB - Centro Atómico Bariloche Phone: +54 2944 44 5100, Fax:

+54 2944 44 5299

Email: info@cab.cnea.gov.ar

Http://www.cab.cnea.gov.ar/

Centre for Energy Research, Hungarian Academy of Sciences Phone: +36-1-392-2539 Fax: +36-1-392-2533

Email: tamas.BELGYA@energia.mta.hu Http://www.energia.mta.hu.

CSNS

Email: klaus.pranzas@hzg.de

Http://www.hzg.de/central_departments/gems/index.html.de

HANARO Center for Applications of Radioisotopes and Radiation Korea Atomic Energy Research Institute Phone: +82 42 868-8120 Fax: +82 42 868-8448

Http://hanaro.kaeri.re.kr/english/index.html

HFIR ORNL, Oak Ridge, USA Phone: 865-576-0214 Fax: 865-574-096

Phone: 86 10 68597289

Email: burnettese@ornl.gov

Fax: 86 10 68512458

Http://neutrons.ornl.gov/facilities/HFIR/experiment.shtml

Email: cas_en@stimes.cn

Http://english.cas.ac.cn/

ESS AB European Spallation Source

IBR-2 Frank Laboratory of Neutron Physics Phone: (7-49621) 65-657 Fax: (7-49621) 65-085

Phone: +46 46 888 30 94

Email: belushk@nf.jinr.ru

Mobile: +46 72 179 20 94

Http:// flnp.jinr.ru/474/

Email: sindra.petersson@esss.se Http://www.esss.se/

Facilities Neutron Scattering

ILL

JEEP-II Reactor

Type: 58MW High Flux Reactor.

Type: D2O moderated 3.5% enriched UO2 fuel.

Phone: + 33 (0)4 76 20 71 11

Phone: +47 63 806000, 806275

Fax: + 33 (0)4 76 48 39 06

Fax: +47 63 816356

Phone: +33 4 7620 7179

Email: kjell.bendiksen@ife.no

Fax: +33 4 76483906

Http://www.ife.no/index_html-en?set_language=en&cl=en

Neutron Neutr S Email: cico@ill.fr and sco@ill.fr Http://www.ill.eu

IPEN – Peruvian Institute of Nuclear Research Phone: 226-0030, 226-0033226 Email: ceid@ipen.gob.pe

Http://www.ipen.gob.pe/site/index/index.htm

IPNS - Intense Pulsed Neutron at Argonne Phone: 630/252-7820 Fax: 630/252-7722

Email: cpeters@anl.govor mail (for proposal submission) Http://www.pns.anl.gov/

ISIS Didcot

KENS Institute of Materials Structure ScienceHigh Energy Accelerator Research Organization 1-1 Oho, Tsukuba-shi, Ibaraki-ken,?305-0801, JAPAN Email: kens-pac@nml.kek.jp Http://neutron-www.kek.jp/index_e.html

KUR Kyoto University Research Reactor Institute Kumatori-cho Sennan-gun, Osaka 590-0494,Japan Phone: +81-72-451-2300 Fax: +81-72-451-2600 Http://www.rri.kyoto-u.ac.jp/en/

Type: Pulsed Spallation Source.

LANSCE

Phone: +44 (0) 1235 445592

Phone: 505-665-1010

Fax: +44 (0) 1235 445103

Fax: 505-667-8830

Email: uls@isis.rl.ac.uk

Email: lansce_users@lanl.gov

Http://www.isis.rl.ac.uk

Email: tichavez@lanl.gov

JCNS Juelich Centre for Neutron Science Forschungszentrum Jülich

Http://lansce.lanl.gov/

LENS Low Energy Neutron Source

Phone: +49 2461 614750

Phone: +1 (812) 8561458

Fax: +49 2461 612610

Email: pesokol@indiana.edu

neutrons@fz-juelich.de d.richter@fz-juelich.de (for JCNS-1) t.brueckel@fz-juelich.de (for JCNS-2) Http://www.fz-juelich.de/jcns/EN/Home/home_node.html

Http://www.indiana.edu/~lens/index.html

Email:

J-PARC Japan Proton Accelerator Research Complex Phone: +81-29-284-3398 Fax: +81-29-284-3286

Email: j-uo@ml.j-parc.jp

Http://j-parc.jp/index-e.html

JRR-3M

Fax: +81 292 82 59227

Phoneex: JAERIJ24596E

LLB

Type: Reactor

Flux: 3.0 x 1014 n/cm2/s

Secrétariat Europe : Phone: 0169085417 Fax: 0169088261 Email: experience@llb.cea.fr Http://www-llb.cea.fr

McMASTER NUCLEAR REACTOR Phone: 905-525-9140

Http://mnr.mcmaster.ca/

Email: www-admin@www.jaea.go.jp

MIT - Nuclear reactor Laboratory

Http://www.jaea.go.jp/jaeri/english/index.html

Email: nrl-rrs@mit.edu Http://web.mit.edu/afs/athena.mit.edu/org/n/nrl/www/

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

Facilities

MURR

SINQ

Phone: 1.573.882.4211

Type: Steady spallation source

Email: MURRCustomerService@missouri.edu

Phone:

Http://www.murr.missouri.edu/

Fax: +41 56 3103294

+41 56 310 4666

n Scatteri ron Scatterin NIST Center for Neutron Research

Email: sinq@psi.ch

Http://sinq.web.psi.ch

Fax: (301) 869-4770

SNS Spallation Neutron Source

Email: Robert.dimeo@nist.gov

Phone: 865.241.5644

Http://www.ncnr.nist.gov/

Fax: (865) 241-5177

Phone: (301) 975-6210

NPL – NRI

Email: ekkebusae@ornl.gov Http://neutrons.ornl.gov

Type: 10 MW research reactor

Phone: +420 2 20941177 / 66173428 Fax: +420 2 20941155

Email: krz@ujv.cz and brv@nri.cz Http://neutron.ujf.cas.cz/

NPRE

Phone: 217/333-2295 Fax: 217/333-2906

Http://npre.illinois.edu/

NRU - Chalk River Laboratories Phone: 613-584-8293 Fax: 613-584-4040

Http://neutron.nrc-cnrc.gc.ca/home_e.html

PIK - Petersburg Nuclear Physics Institute Phone: +7(813-71) 46025, +7(813-71) 46047 Fax: +7(813-71) 36025, +7(813-71) 31347 Http://www.pnpi.spb.ru/

RIC Reactor Infrasctructure Centre Phone:

+386 1 588 5450

Fax: +386 1 561 2335

Http://www.rcp.ijs.si/ric/index-a.htm

RID Reactor Institute Delft (NL)

Type: 2MW light water swimming pool. Phone: +31 (0)15 278 5052 Fax: +31 (0)15 278 6422

Email: secretary-rid@tudelft.nl

Http://www.rid.tudelft.nl/en/cooperation/facilities/reactor-

instituut-delft/

RISØ DTU Phone: +45 4677 4677 Fax: +45 4677 5688 Email: risoe@risoe.dtu.dk Http://www.risoe.dtu.dk/

Facilities

Synchrotron Radiation Sources WWW SERVERS IN THE WORLD www.lightsources.org/cms/?pid=1000098

Sync Radiatio S ALBA Synchrotron Light Facility

CAMD Center Advanced Microstructures & Devices

Phone: +34 93 592 43 00

Phone: +1 (225) 578-8887

Fax: +34 93 592 43 01

Fax: +1 (225) 578-6954

Http://www.cells.es/

Email: leeann@lsu.edu

ALS Advanced Light Source

Http://www.camd.lsu.edu/

Fax: 510.486.4773

CANDLE Center for the Advancement of Natural Discoveries using Light Emission

Email: alsuser@lbl.gov

Phone/Fax : +(37 4-10) 629806

Http://www-als.lbl.gov/als

Email: baghiryan@asls.candle.am

Phone: 510.486.7745

ANKA

Http://www.candle.am/index.html

Fax: +49-(0)7247 / 82-8677

CESLAB Central European Synchrotron Laboratory

Email: info@fzk.de

Phone: +420-541517500

Http://ankaweb.fzk.de/

Email: kozubek@ibp.cz

Phone: +49 (0)7247 / 82-6188

APS Advanced Photon Source

Http://www.xray.cz/

CFN - Center for Functional Nanomaterials

Phone: (630) 252-2000

Phone: +1 (631) 344-6266

Fax: +1 708 252 3222

Fax: +1 (631) 344-3093

Email: fenner@aps.anl.gov

Email: cfnuser@bnl.gov

Http://www.aps.anl.gov/

Http://www.bnl.gov/cfn/

AS - Australian Synchrotron Phone: +61 3 8540 4100

CHESS Cornell High Energy Synchrotron Source

Fax: +61 3 8540 4200

Phone: 607-255-7163

Email: info@synchrotron.org.au

Fax: 607-255-9001

Http://www.synchrotron.org.au/

Http://www.chess.cornell.edu/

BESSY II - Helmholtz Zentrum Berlin Phone: +49 30 - 80620

CLIO Centre Laser Infrarouge dâ&#x20AC;&#x2122;Orsay

Fax: +49 30 8062 - 42181

Email: accueil-clio@lcp.u-psud.fr

Email: info@helmholtz-berlin.de

Http://clio.lcp.u-psud.fr/clio_eng/clio_eng.htm

Http://www.helmholtz-berlin.de/

BSRF - Beijing Synchrotron Radiation Facility Phone: +86-10-68235125 Fax: 86-10-68186229 Email: houbz@mail.ihep.ac.cn Http://www.ihep.ac.cn/bsrf/english/main/main.html

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

Facilities

chrotron on Sources CLS Canadian Light Source

DFELL Duke Free Electron Laser Laboratory

Phone: (306) 657-3500

Phone: 919-660-2681

Fax: (306) 657-3535

Fax: 919-660-2671

Email: clsuo@lightsource.ca

Email: beamtime@fel.duke.edu

Http://www.lightsource.ca/

Http://www.fel.duke.edu/

CNM Center for Nanoscale Materials

Diamond Light Source

Phone: 630.252.6952

Fax: +44 (0)1235 778499

Fax: 630.252.5739

Email: useroffice@diamond.ac.uk

Email: carrieclark@anl.gov

Http://www.diamond.ac.uk/default.htm

Phone: +44 (0)1235 778000

Http://nano.anl.gov/facilities/index.html

CTST UCSB Center for Terahertz Science and Technology

ELETTRA - Synchrotron Light Laboratory Phone: +39 40 37581

Fax: +39 (040) 938-0902

Http://www.elettra.trieste.it/

University of California, Santa Barbara (UCSB), USA Email: ramian@sbFEL3.ucsb.edu

ELSA - Electron Stretcher Accelerator

Http://sbfel3.ucsb.edu/

Phone: +49-228-735926 Fax: +49-228-733620

DAFNE Light INFN-LNF

Phone: +39 06 94031

Email: roy@physik.uni-bonn.de

Http://www-elsa.physik.uni-bonn.de/elsa-facility_en.html

Fax: +39 06 9403 2582

ESRF - European Synchrotron Radiation Lab.

Http://www.lnf.infn.it/acceleratori/btf/

Phone: +33 (0)4 7688 2000 Fax: +33 (0)4 7688 2020

DELSY Dubna ELectron SYnchrotron Phone: + 7 09621 65 059 Fax: + 7 09621 65 891 Email: post@jinr.ru

Http://wwwinfo.jinr.ru/delsy/variant-21june.htm

Email: useroff@esrf.fr Http://www.esrf.eu/

FELBE Free-Electron Lasers at the ELBE Radiation Source at the HZDR Dresden-Rossendorf Phone: +49 351 260 - 0

DELTA Dortmund Electron Test Accelerator FELICITA I (FEL)

Fax: +49 351 269 - 0461 Email: m.helm@hzdr.de

Http://www.hzdr.de/db/Cms?pNid=471

Fax: +49-(0)231-755-5383

Http://usys.delta.uni-dortmund.de/

FELIX Free Electron Laser for Infrared experiments Phone: +31-30-6096999 Fax: +31-30-6031204 Email: B.Redlich@rijnh.nl Http://www.rijnh.nl/felix/

Facilities Synchrotron Radiation Sources

Synchrotr Rad Sources FOUNDRY The Molecular Foundry

ISI-800 Institute of Metal Physics - Ukraine

1 Cyclotron Road, Berkeley CA 94720, USA

Phone: +(380) 44 424-1005

Phone: +1 - 510.486.4088

Fax: +(380) 44 424-2561

Email: rjkelly@lbl.gov

Email: metall@imp.kiev.ua

Http://foundry.lbl.gov/index.html

Http://www.imp.kiev.ua/ (Russian)

HASYLAB Hamburger Synchrotronstrahlungslabor DORIS III, PETRA II / III, FLASH

Jlab - Jefferson Lab FEL

Phone: +49 40 / 8998-2304

Http://www.jlab.org/FEL

Fax: +49 40 / 8998-2020

Email: HASYLAB@DESY.de Http://hasylab.desy.de/

Phone: (757) 269-7100 Fax: (757) 269-7848

Kharkov Institute of Physics and Technology Pulse Stretcher/Synchrotron Radiation Phone: +38 (057) 335-35-30

HSRC Hiroshima Synchrotron Radiation Center HiSOR Phone: +81 82 424 6293 Fax: +81 82 424 6294

Http://www.hsrc.hiroshima-u.ac.jp/english/index-e.htm

Fax: +38 (057) 335-16-88

Http://www.kipt.kharkov.ua/.indexe.html

KSR - Nuclear Science Research Facility Accelerator Laboratory Fax: +81-774-38-3289

Ifel

Phone: +81-(0)72-897-6410

Http://www.fel.eng.osaka-u.ac.jp/english/index_e.html Http://www.eng.osaka-u.ac.jp/en/index.html

Http://wwwal.kuicr.kyoto-u.ac.jp/www/index-e.htmlx

KSRS - Kurchatov Synchrotron Radiation Source Siberia-1 / Siberia-2 Phone: 8-499-196-96-45

INDUS -1 / INDUS -2

Http://www.lightsources.org/cms/?pid=1000152

Phone: +91-731-248-8003

Http://www.kiae.ru/ (Russian)

Fax: 91-731-248-8000

Email: rvn@cat.ernet.in

LCLS - Linac Coherent Light Source

Http://www.cat.ernet.in/technology/accel/indus/index.htm

Phone: +1 (650) 926-3191

Http://www.cat.ernet.in/technology/accel/atdhome.htm

Fax: +1 (650) 926-3600

Email: knotts@ssrl.slac.stanford.edu

IR FEL Research Center FEL-SUT

Http://www-ssrl.slac.stanford.edu/lcls/

Phone: +81 4-7121-4290

LNLS - Laboratorio Nacional de Luz Sincrotron

Fax: +81 4-7121-4298

Phone: +55 (0) 19 3512-1010

Email: felsut@rs.noda.sut.ac.jp

Fax: +55 (0)19 3512-1004

Http://www.rs.noda.sut.ac.jp/~felsut/english/index.htmI

Email: sau@lnls.br Http://www.lnls.br/site/home.aspx

ISA Institute for Storage Ring Facilities - ASTRID-1

MAX-Lab

Phone: +45 8942 3778

Phone: +46-222 9872

Fax: +45 8612 0740

Fax: +46-222 4710

Email: fyssp@phys.au.dk

Http://www.maxlab.lu.se/

Http://www.isa.au.dk/

Medical Synchrotron Radiation Facility Phone: +81-(0)43-251-2111 Http://www.nirs.go.jp/ENG/index.html

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1

Facilities

tron diation s MLS - Metrology Light Source

PSLS - Polish Synchrotron Light Source

Physikalisch-Technische Bundesanstalt

Phone: +48 (12) 663 58 20

Phone: +49 30 3481 7312

Email: mail@synchrotron.pl

Fax: +49 30 3481 7550

Http://www.if.uj.edu.pl/Synchro/

Email: Gerhard.Ulm@ptb.de Http://www.ptb.de/mls/

RitS Ritsumeikan University SR Center

Http://www.ptb.de/mls/

Phone: +81 (0)77 561-2806 Fax: +81 (0)77 561-2859

NSLS National Synchrotron Light Source Phone: +1 (631) 344-7976

Email: d11-www-adm@se.ritsumei.ac.jp

Http://www.ritsumei.ac.jp/se/re/SLLS/newpage13.htm

Fax: +1 (631) 344-7206

SAGA-LS - Saga Light Source

Email: nslsuser@bnl.gov

Phone: +81-942-83-5017

Http://www.nsls.bnl.gov/

Fax: +81-942-83-5196

NSRL National Synchrotron Radiation Laboratory

Http://www.saga-ls.jp/?page=173

Fax: +86-551-5141078

SESAME Synchrotron-light for Experimental Science and Applications in the Middle East

Email: zdh@ustc.edu.cn

Email: hhelal@mailer.eun.eg

Http://www.nsrl.ustc.edu.cn/en/

Http://www.sesame.org.jo/index.aspx

NSRRC National Synchrotron Radiation Research Center

SLS - Swiss Light Source

Phone: +886-3-578-0281

Fax: +41 56 310 3294

Fax: +886-3-578-9816

Email: slsuo@psi.ch

Email: user@nsrrc.org.tw

Http://sls.web.psi.ch/view.php/about/index.html

Phone: +86-551-3601989

Http://www.nsrrc.org.tw/

NSSR Nagoya University Small Synchrotron Radiation Facility Phone: +81-(0)43-251-2111

Http://www.nagoya-u.ac.jp/en/

Phone: +41 56 310 4666

SOLEIL

Phone: +33 1 6935 9652 Fax: +33 1 6935 9456

Email: frederique.fraissard@synchrotron-soleil.fr

Http://www.synchrotron-soleil.fr/portal/page/portal/Accueil

PAL - Pohang Accelerator Laboratory

SPL Siam Photon Laboratory

San-31 Hyoja-dong Pohang Kyungbuk 790-784, Korea

Phone: +66-44-21-7040

Email: ilguya@postech.ac.kr

Fax: +66-44-21-7047, +66-44-21-7040 ext 211

Http://pal.postech.ac.kr/eng/index.html

Http://www.slri.or.th/new_eng/

PF - Photon Factory

SPring-8

Phone: +81 (0)-29-879-6009

Phone: +81-(0) 791-58-0961

Fax: +81 (0)-29-864-4402

Fax: +81-(0) 791-58-0965

Email: users.office2@post.kek.jp

Email: sp8jasri@spring8.or.jp

Http://pfwww.kek.jp/

Http://www.spring8.or.jp/en/

Facilities

Synchrotr Rad Sources SRC Synchrotron Radiation Center Phone: +1 (608) 877-2000

TSRF Tohoku Synchrotron Radiation Facility Laboratory of Nuclear Science

Fax: +1 (608) 877-2001

Phone: +81 (022)-743-3400

Http://www.src.wisc.edu/

Fax: +81 (022)-743-3401

SSLS Singapore Synchrotron Light Source - Helios II Phone: (65) 6874-6568 Fax: (65) 6773-6734

Http://ssls.nus.edu.sg/index.html

SSRC Siberian Synchrotron Research Centre VEPP3/VEPP4

Email: koho@LNS.tohoku.ac.jp

Http://www.lns.tohoku.ac.jp/index.php

UVSOR Ultraviolet Synchrotron Orbital Radiation Facility Phone: +81-564-55-7418 (Receptionist's office) Fax: +81-564-54-2254

Email: webmaster@ims.ac.jp

Http://www.uvsor.ims.ac.jp/defaultE.html

Phone: +7(3832)39-44-98 Fax: +7(3832)34-21-63

Email: G.N.Kulipanov@inp.nsk.su

Http://ssrc.inp.nsk.su/english/load.pl?right=general.html

SSRF Shanghai Synchrotron Radiation Facility Http://ssrf.sinap.ac.cn/english/

SSRL Stanford Synchrotron Radiation Laboratory Phone: +1 650-926-3191 Fax: +1 650-926-3600

Email: knotts@ssrl.slac.stanford.edu

Http://www-ssrl.slac.stanford.edu/index.html

SuperSOR SuperSOR Synchrotron Radiation Facility Phone: +81 (0471) 36-3405 Fax: +81(0471) 34-6041

Email: kakizaki@issp.u-tokyo.ac.jp

Http://www.issp.u-tokyo.ac.jp/labs/sor/project/MENU.html

SURF Synchrotron Ultraviolet Radiation Facility Phone: +1 (301) 975-4200 Http://physics.nist.gov/MajResFac/SURF/SURF/index.html

TNK - F.V. Lukin Institute

Information

Phone: +7(095) 531-1306 / +7(095) 531-1603

on Conference Announcements and Advertising for Europe and US, rates and inserts can be found at:

Fax: +7(095) 531-4656 Email: admin@niifp.ru

www.cnr.it/neutronielucedisincrotrone

Http://www.niifp.ru/index_e.html

segreteria@centronast.it nnls@roma2.infn.it

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1