notiziario neutroni e luce di sincrotrone - issue 18 n.1, 2013

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ESRF Users' Meeting 2013Shaping 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 featur-ing 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 OrganisationChiara Maurizio (chairperson)Physics DepartmentUniversity of Padovavia Marzolo, 835131 Padova, [email protected]

ESRF User Office,[email protected]. +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 investigationsE.H. Lehmann, A. Kaestner, P. Vontobel, C. Grünzweig, 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. Schröder

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 ISISS. 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 SourcesC.-K. Loong

Shull Fellows now launched on interesting and fulfilling careersA. Bardoel

n Call for proposal Neutron Sources

Synchrotron Radiation Sources

n Calendar

n Facilities Neutron Sources


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).

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

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

Volume 18 n. 1 Dicembre 2012Aut. Trib. Roma n. 124/96 del 22-03-96

EDITORC. Andreani

CNR - PROMOTION AND COLLABORATIONS M. Arata

CORRESPONDENTSF. Boscherini, L. Bove, C. Blasetti, A. Ekkebus,M. Forster, T. Guidi, C. Habfast, B. Palatini,L. Paolasini, H. Reichert, V. Rossi Albertini

ON LINE VERSIONV. Buttaro

CONTRIBUTORS TO THIS ISSUEI.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 SUBSCRIPTIONSS. FischerE-mail: [email protected]

GRAPHIC DESIGNStampa Sud S.p.A.

PRINTStampa Sud SpAVia P. Borsellino 7/974017 Mottola (TA) – Italye-mail: [email protected]

Editorial News 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 investigationsE.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 ISISS. 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 SourcesC.-K. Loong

33 Shull Fellows now launched on interesting and fulfilling careersA. Bardoel

Call for proposal 36 Neutron Sources

37 Synchrotron Radiation Sources

40 Calendar

Facilities 41 Neutron Sources

44 Synchrotron Radiation Sources

Summary

Finito di stampare nel mese di Gennaio 2013

Editorial News

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 1 2

A visit to ESRF, ILL and ISIS

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 cutting-edge 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

Luigi NicolaisPresident of CNR

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

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 CRG’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, – 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.

Scientific Reviews

3

Abstract

The study of material interaction with neutrons can provide essential informa-tion about the observed sample. On atom-ic and microscopic level, neutron diffrac-tion and scattering techniques are well established and structural information, quantum phenomena or lattice param-eters can be derived. The most prominent and powerful neutron sources are there-fore 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 impor-tant 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 frequen-cy was dramatically increased but mainly the options for more detailed studies of the neutron distributions inside and around the sample and the process un-der investigation. In this way, new imag-ing techniques have been developed and made available for a broad user commu-nity on routine basis. Similarly to X-ray techniques, neutron tomography enables the access to the third dimension, where-as phase contrast methods provide addi-tional and alternative information. New approaches are now the use of polarized neutrons, the observation in narrow en-ergy bands and the further improvement of the spatial resolution in neutron imag-ing. The study of real-time processes is an option close to the performance edge of neutron imaging, demanding and chal-lenging.

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

1. Introduction

Neutron Imaging started as “neutron radi-ography” about 50 years ago when strong enough neutron sources were made avail-able. 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 exploit-ed 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 di-mensions created only a small user com-munity in non-destructive testing, nu-clear 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

E.H. Lehmann, A. Kaestner, P. Vontobel,C. Grünzweig, D. Mannes, S. PeetermansNeutron Imaging and Activation Group, Paul Scherrer InstitutCH-5232 Villigen PSI, Switzerland

9th World Conference on Neutron Radi-ography was held in South Africa in 2010 [2]. A complementary series of expert’s meetings have been taken place regularly (International Topical Meetings on Neu-tron Radiography [3] and NEUWAVE [4]). Also IAEA managed to initiate some network and standards in neutron imag-ing [5] and gives further support, in par-ticular 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 pro-gram and broad application range. How-ever, 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 trans-mitting 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 attenua-tion properties of materials in this energy range, thermal and cold neutron beams have found to be most suitable for prac-tical 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 consider-ably high (see chapter 3.3.) and the expo-sure time is increasing much.Secondly, the beam collimation is very im-portant if a high spatial resolution is intend-ed. The geometric blurring ug is inversely

Figure 1

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

Neutron Imaging - status and prospects of a modern research toolFlexible non-invasive studies from plant-soil-interaction to magnetic material investigations

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:

2

DL

(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 neu-trons, the aperture dimensions w have to reduce further down to the millimeter range in order to fulfill the coherence con-ditions for the coherence length r in the micro-meter range (with the wavelength λ, the distance to the measurement posi-tion l) :

wlr

(2)

Because the intensity of even strongest neu-tron 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 scintilla-tion screen. Its efficiency and inherent spatial reso-lution 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 advan-tage 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.

3. Neutron imaging techniques

Here, we present a list of presently com-mon imaging techniques with neutrons without claim of full completeness. De-pending on the situation in the individ-ual institution, particular techniques are more or less pronounced or developed.

3.1. Transmission radiography mode

In this mode, neutron imaging can pro-vide similar performance like X-ray ra-diography (as common e.g. in hospitals) in respect to image size and resolution. However, the image contrast and there-fore 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 mate-rial itself. For e.g. Al or Pb a layer of 30 cm can be penetrated, but 1 cm of water is al-ready 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 sys-tems available with pixel sizes in the order of 15 micro-meters. The corresponding field-of-view is on the order of 30 mm.

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

Quantification:

The transmitted beam intensity I carries information about the sample content if it is compared to the initial intensity I0 with-out 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:

MLNd

II /)ln( 0 (3)

The attenuation coefficient Σ is just the multiplication of the material specific (and tabulated) microscopic cross-section and the density of nuclei N (L = Avoga-dro’s constant, M = atomic mass). In this way, a non-invasive determination of ma-terial distributions can be performed.

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

3.2. Neutron tomography

In order to investigate the third dimension of samples, it is necessary to take projec-tions over an angular range of at least 180°. Because the neutron source is fixed and given by the large scale facility, the sam-ples have to be rotated around their verti-cal or horizontal axis in the quasi-parallel neutron beam. This two-dimensional in-formation is needed to calculate the voxel-values for the volume by using reconstruc-tion tools, mainly based on filtered back-projection 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 sev-eral labs around the globe, but the number of installations is limited. The performance

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

3.3. Energy selective neutron imaging

The initially delivered beam spectra from the source are in most cases Maxwellian dis-tributions around the mean thermal energy of about 25 meV. Therefore, the obtained transmission data represent an energy-aver-aged value for the investigated material.Since the microscopic cross-sections σ are often strongly energy dependent the spec-tral dependency limits the quantification (see above) due to scattering and beam hardening effects. On the other hand, there is much micro-scopic 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 met-als). 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

1. Data acquisition300-1200 projections

Scan time 1-24h

2. CT reconstruction

Processing time ~1h

3. Data evaluationImage processing/analysis3D Visualization

Processing time: hours or days

Figure 3

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

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. Depend-ing 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 en-ergy – depending on the particular mate-rial – the crystal orientation and textured zones become directly visible by alternat-ing contrasts (see Fig. 6). In a later stage, by narrowing the energy even more, it will become possible to de-termine directly the stress distribution in structural materials. Future energy selective imaging will be per-formed in time-of-flight mode at the upcom-ing 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 sys-tems 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 ma-terial changes There are two directions for such kind of investi-gations: (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 de-fined which describes the direction of the outgoing wave front according to Snell’s law (N = nuclei density, bc = coherent scat-tering length):

62

1012

11

cbNn (4)

It is to mention that the deviation from 1 is very little (not com-parable 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 wave-length) 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 in-terferometer.

1 2 3 4 5 6 70

5

10

15

20

25

30

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Cu

Pb Zr Al

[b

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Ni

Figure 5

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

Figure 6

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])

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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 consid-ered misleading in the quantification (see 3.1). Now it has been proven that in the case of single crystals or poly-crystalline samples with large enough grains the diffracted neu-trons can be visualized and quantified in a second imaging detec-tor 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 orienta-tion can directly be observed by this method.

3.7. Neutron imaging with polarized neutrons

Neutrons carry a magnetic moment μn which is oriented anti-parallel to the spin. As the spin of the neutron exist in two states

(+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 as-sembly 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 supercon-ductor is described in a complete non-invasive way [13].

4. Neutron imaging user facilities world-wide

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 at-tributed 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 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

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].

Scientific Reviews


Many research reactors are operational in developing coun-tries, 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].

5. Main application fields

Due to new and more sophisticated methodical features and pos-sibilities, 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 ma-terial 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 in-dustrial applications. Here it complements the well established X-ray 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 di-mensions and timely resolved.

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 ac-cess program.

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

Figure 10

A radiograph showing the field lines around a bar magnet levitating over an yttrium–barium–copper-oxide(YBCO) superconductor due to the Meissner-effect [13]

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References

[1] J. Barton, Proc. 1st World Conference on Neutron Radi-ography, 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, El-sevier, 2012

[3] N. Takenaka et al. (ed.), Proceedings of the 6th In-ternational Topical Meeting on Neutron Radiogra-phy, 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-De-

structive Tool for Material Testing, Sept. 2008[6] E.H. Lehmann, A. Tremsin, C. Grünzweig, I. Johnson,

P. Boillat and L. Josic, Neutron imaging — Detector op-tions in progress, 2011 JINST 6 C01050

[7] A. B. Moradi, A. Carminati, D. Vetterlein, P. Vonto-bel, E. Lehmann, U. Weller, J. Hopmans, H.-J. Vogel, S. Oswald, Three-dimensional visualization and quan-tification of water content in the rhizosphere, New Phytologist (2011) 192: 653-663, doi: 10.1111/j. 1469-8137.2011.03826.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 imbibi-tion 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, Nu-clear 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 Visual-ized by Neutron Dark-Field Imaging, Applied Physics Letters 93 (2008) p. 112504

[13] N. Kardjilov et al., Three-dimensional imaging of mag-netic fields with polarized neutrons, nature physics Vo.4, 2008, doi:10.1038/nphys912

Scientific Reviews


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 con-centration for post-combustion CO2 capture, so called “amine-scrubbing 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, the-reby 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 pe-nalty, significantly limit their long-term applications. It is there-fore 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 en-vironment 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, defi-ning 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 ga-ses (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 bin-ding energy were obtained in this way. However, static crystal-lographic 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 fun-ctional 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 ther-mal 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 hydro-gen bonds, supplemented by weaker phenyl C-H···O supramole-cular 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 square-shaped 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. Impor-tantly, 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) mo-lecules and the NOTT-300 host is crucial to understanding the detailed binding mechanism and hence the observed high selec-tivities. Inelastic neutron scattering (INS) is a powerful neutron spectroscopy technique which has been used widely to investi-gate the H2 binding interactions within various storage systems by exploiting the high neutron scattering cross-section of hydro-gen (82.02 barns).5 However, this technique cannot directly de-tect 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

Sihai Yang,1 A.J. Ramirez-Cuesta,2 andMartin 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)

In situ Inelastic Neutron Scattering Study on aGas-Loaded Metal-Organic Framework

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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 La-boratory (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 addi-tion 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 hydro-gen is ten times more visible than other elements due to its high neutron cross-section; (ii) the technique is not subject to any op-tical 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 neu-trons 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 col-lected at below 10 K, where the thermal motion of the MOF ma-terial 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 oc-curs 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 NOTT-300·1.0CO2, indicating a stiffening of the motion of the NOTT-300 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 agre-ement 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

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(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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Scientific Reviews


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-to-weak hydrogen bonds and supramolecular interactions. Similar INS study and DFT analysis were also carried out on SO2-loaded NOTT-300, in order to probe the dynamics of the gas-loaded system. Comparison of the INS spectra below 5 K reveals two major increases in peak intensity on going from bare NOTT-300 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 stif-fening 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 interac-tions [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 pro-be 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. Signifi-cantly, 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 sug-gests 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 inte-ractions with adjacent C-H groups of benzene rings. The bin-ding 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 pro-mise not only for the efficient capture of CO2 and SO2, but also for their facile, low-energy and therefore economic release subse-quently; 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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e fFigure 2

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 SO2-loaded (f) NOTT-300 obtained from DFT analysis.

Scientific Reviews


Luca PasquiniDepartment of Physics and Astronomy, University of Bologna and CNISM

v.le C. Berti-Pichat 6/240127 Bologna, Italy

Application of synchrotron radiation techniquesto the study of hydrogen storage materials

AbstractMaterials 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 tech-niques, and on the design of in situ experiments which permit to follow phase transforma-tions 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 sys-tem 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 re-spect 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 °C tem-perature 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 liquefactionii) physisorption, i.e. adsorption of H2 molecule onto the

surface of highly porous materialsiii) formation of a chemical bond, e.g. metal hydrides, am-

monia. The reader interested in a critical discussion on the state

of the art of these H-storage categories and in a comparison be-tween them is referred to excellent reviews on the subject [1,2]. In particular, the third broad category, chemically bound hydro-gen, encompasses very different materials, like metal hydrides, complex hydrides, amines and amides, ammonia borane, and hydrocarbons. Some of these substances, like sodium borohy-dride 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 al-lowing reversible operation. In this case the mechanism of H-release 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 evo-lution 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 cor-responds to operating conditions appealing for mobile storage: 0-100 °C and 1-10 bar. Unfortunately, the elements or interme-tallic 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, mean-ing 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 re-versible 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, impres-sive improvements were obtained by employing nanocrystalline MgH2 with suitable dispersion of catalyst phases such as tran-sition 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 Bogdanovic´ and Schwickardi discovered that doping with small amounts of Ti compounds could significantly improve the kinetics of H evo-lution 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 materi-als 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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15

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 ther-modynamics of these nanomaterials does not simply result from a weighted average of the component phases, since new phys-ics emerges due to various interactions between them, and the local structure at the interfaces plays a very important role in this respect.

Motivation for experiments with the synchrotron probeSynchrotron radiation (SR) has the po-tential 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 com-plementary SR techniques. The study of how microstructure and phase composi-tion evolve during H-uptake and release can be undertaken by in situ X-ray diffrac-tion (XRD) experiments, which are also extremely helpful for determining the re-action 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 in-herently local and element-selective [5]. New hydride crystal structures can be de-termined by high-resolution XRD, some-times in combination with neutron dif-fraction due to the peculiar neutron scat-tering length of hydrogen and deuterium [6,7]. The distribution of particles sizes in a huge range is conveniently measured by

small-angle scattering techniques, includ-ing anomalous small angle x-ray scatter-ing (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 struc-ture, electron bonding states and transfor-mation pathways of advanced materials for SSHS based on reversible hydrides. Two examples constitute a combined approach that we have followed to investigate Mg-based nanostructured materials by means of complementary XRD and XAS experi-ments [10,11]. Another couple of illustra-tive case studies selected from recent lit-erature 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 H- uptake and release.

In situ X-ray diffractionThe 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 capil-lary 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-absorp-tion up to 5 MPa and H-desorption under rotary pump vacuum.

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.

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The first example is an investigation of Mg-based nanoparticles (NPs) [10]. Mag-nesium hydride MgH2 displays several at-tractive 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 interac-tion 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 nanoscaf-folds [16]. In Mg-based nanostructures, Pd is often employed as a capping layer to increase oxidation resistance and to pro-mote the dissociation/recombination of the H2 molecule at the surface. However, the occurrence of structural transforma-tions in Pd and in possible Mg-Pd com-pounds connected to H-sorption is gener-ally overlooked. Mg/MgO core/shell NPs were prepared by inert gas condensation and decorat-ed by Pd evaporation, as discussed in Ref. [17]. A shown in Figure 1, the first heating under vacuum causes the dis-appearance 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 ac-cording to the Mg-Pd phase diagram at low Pd concentration (13 wt% in this case), the importance of these experi-ments is to highlight a fast kinetics of alloy formation even at moderate tem-perature and in presence of a MgO bar-rier layer (5 nm thick). What is more interesting, is that the Mg6Pd phase plays an active role in subsequent H-sorption runs. In fact, Figure 2a shows that, upon H-absorption at 573 K / 5 MPa H2 pressure, not only Mg trans-forms into MgH2, but also Mg6Pd un-dergoes the reaction:

Mg6Pd+5H2 ↔ MgPd+5MgH2 (1)

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.

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17

mation of MgB2 is observed in the isothermal period. In summary, the useful-ness of in situ XRD experi-ments with synchrotron ra-diation 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.

X-ray SpectroscopyOn 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 differ-ent equilibrium states [11]. Figure 4 reports the magni-tudes of the Fourier Trans-forms (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 as-prepared 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 mi-croscopy observations [17]. EXAFS anal-ysis shows that the Pd-Pd interatomic dis-tance 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-ab-sorption at high temperature, fcc Pd dis-appears in favour of the MgPd phase. The corresponding EXAFS data (Figure 4c) were thus fitted using the crystallographic

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.

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 be-cause of the melting of this phase, and iii) at temperatures around 330 °C, desorp-tion of hydrogen from MgH2 occurs, to-gether with the formation of metallic Mg. Finally, after about 3 hours isothermal at 400 °C the formation of MgB2 is ob-served, correlated to the decomposition of LiBH4. An incubation time between the formation of metallic Mg and the for-

which is indeed reversible, i.e. when vac-uum is restored, MgPd transforms back into Mg6Pd as displayed in Figure 2b. The crystal structure of these two Mg-Pd in-termetallic compounds are illustrated in Figure 3: Mg6Pd has a huge cubic cell (lat-tice 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 pro-file at t=80s. These intermediate states were confirmed by further experiments at lower H2 pressure as discussed in de-tail in Ref. 10. In turn, reaction (1) cor-responds 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 calcula-tions [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 re-action with the formation of a new com-pound, 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

Scientific Reviews


information for the MgPd phase with only one Pd site. The Mg-Mg and Mg-Pd inter-atomic distances determined from the fit are larger than the ones quoted for bulk MgPd by about 2%. This result is impor-tant 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-de-sorption, 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 ob-tained in this case, supporting the idea that H does not enter into the Mg6Pd lat-tice in an appreciable amount. We emphasize that this XAS study repre-sents 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 dis-solved 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 com-pounds and the reversible transformation from MgPd to Mg6Pd which accompanies H-release [11].

X-ray spectroscopy is also an invalu-able 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 ex-perimental data are rather poor and the nature of Al-H bond is still controversial in the theoretical studies. Aluminum hy-dride 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 forma-tion is only slightly negative (−11.3 kJ/mol H2), meaning that extreme pressure conditions are required for its regen-eration. 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 experi-ments allow to measure the occupied and the unoccupied electronic states, respec-tively, 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 tar-get element. The sample for this study was obtained by hydrogenation of Al at 600 °C and 8.9 GPa. The measurements were per-formed 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 co-valent 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.

ConclusionsThe specific examples described here highlight the importance of SR techniques for the advanced structural characteriza-tion 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 Ac-tion focused on nanostructured hydrides was launched recently and currently counts 25 participating countries [20]. One of the Action’s working groups, de-voted to high resolution and high sensitiv-ity characterization of atomic level struc-ture 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 deep-er knowledge of materials’ structure and function at the nanoscale and to develop new materials in tight connection with theory and modeling.

Scientific Reviews

19

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.

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. Bonet-ti, 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. Bonet-ti, Appl. Phys. Lett. 94, 221905 (2009)[18] J.F. Fernandez, J.R. Ares, F. Cuevas, J. Bodega, F. Leardini, C. Sánchez, Interme-tallics 18, 233 (2010)[19] M. Dornheim et al., Scripta Mater. 56, 841 (2007)[20] http://www.cost-mp1103.eu/

Research Infrastructures

Notiziario Neutroni e Luce di Sincrotrone Volume 18 n. 120

ESRF Nano science beamline ID16 passes milestone

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 buil-ding 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 con-crete 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 tempera-ture 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 cur-rent 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 mate-rials 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 nano-analysis probe ID16NA for XRF, XAFS and XRD spectroscopy. In the bio-medical sciences, ID16 will play a key role in “metallo-mics”, 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 “metal-lome”. 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 riboso-me, 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 label-free 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 to-xicity of fine dust particles and aerosols, characterize the behavior of metals and metalloids in bio-geochemical systems, observe the inte-raction 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 Martinez-Criado, beamline responsible scientist for the nano-analysis end station, Peter Cloetens, beamline responsible scientist for the nano-imaging station and ID16 project coordinator.

Claus HabfastHead of Communication GroupEuropean Synchrotron Radiation Facility ESRF


21

New materials are the third science driver of ID16 which is an extremely broad field, ran-ging from electronics to healthcare. A parti-cular motivation comes from the evolution of micro-electronics towards miniaturiza-tion to the nano-scale which makes neces-sary to consider quantum size effects, tun-neling, exchange coupling, self-assembly, patterning etc. Understanding the structure of nano-objects enhances the ability to ma-nipulate 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) undersco-res this statement3.

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

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 im-possible 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 (1011-1012 ph/s) is optimized for tomography and low detection limits, and the complete set-up exhibits optimum mechanical stability and scanning precision.

Sample preparation will be routinely performed in a cryogenic environment to reduce ra-diation 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 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.

Figure 3

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

Figure 4

Simplified drawing of the nano-imaging end station

Figure 5

Simplified drawing of the nano-analysis end station



Engin-X is the world’s leading neutron diffractometer, purpose-built for materials science and engineering experiments. Its first neutrons were produced in 2002, and over the past 10 years Engin-X has continually redefined the frontier of stress measurement capability through investment in state-of-the-art equipment, at-tracting 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 disco-very 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 meta-morphosed 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.

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

such as temperature and external loads. In the early 1980s, residual strain measurement by neutron diffraction using conventional ge-neral purpose diffractometers was reported [1]. With increasing in-dustrial interest in the technique, the first dedicated pulsed neutron stress diffractometer, ENGIN, was born at the ISIS Facility at the Ru-therford 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 Engine-ering and Physical Sciences Research Council in 1999, at a cost of £2.5 million, and was completed in 2002. The principal inve-stigator 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 twin-ning. Secondly, experiments are focused on producing strain or stress maps as a function of position within components, possibly un-der a simulated service condition, often to provide data for the verification of finite ele-ment modelling predictions of engineering processes or for comparison with other me-thods of residual stress measurement. Measurements are typically carried out in collaborative experiments between univer-sities, industry and ISIS to address a wide

Shu Yan Zhang*, Joe Kelleher, Winfried KockelmannISIS Facility, Science and Technology Facilities Council,Rutherford Appleton Laboratory, Harwell Oxford, Didcot,Oxfordshire OX11 0QX, UK*email: [email protected]

Celebration of 10 years of ENGIN-X - Materials Science and Engineering research at ISIS

Figure 2

Schematic diagram of the Engin-X layout


23

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 sur-rounding 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 aeropla-ne 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 decom-missioning 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, Chi-nese 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



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 contri-buting to the measurement corresponds to the intersection of the incident and diffracted beams – the ‘gauge volume’, typically de-fined by incident slits and collimators. The gauge volume is typi-cally 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 measu-ring the elastic component of strain deep within crystalline ma-terials 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 measu-rement in crystalline materials relies on Bragg’s law (Eq. 1) that provides a means to determine the average interplanar lattice

spacing d within a small measurement volume of the sample. When a polycrystalline aggregate deforms elastically, the inter-planar spacing within the constituent grains changes, e.g. ten-sile 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 un-strained material (d0).

sin2d (Eq. 1)

00

0 )(dd

ddd

(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 me-thod 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

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) (b)


25

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)

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 in-tensities by allowing the intensity of individual reflections to vary freely, while the peak positions are determined in the usual man-ner from the unit cell dimensions. This approach provides an em-pirical 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 per-form real-time strain measurements during joining. An in-situ mountable servo-hydraulic stress rig can apply up to 100kN ten-sile 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 nor-mal atmosphere or under inert gas. The automation of experi-mental 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 measu-rement simulation software, SScanSS. [3]The following gives a summary of the sample environments equi-pement on ENGIN-X: • Furnaceequippedwithstressrig–providestemperaturesup

to 1100 oC within normal atmosphere or under inert gas• Vacuumfurnace–providestemperatureupto1800oC• Heatingpad–canbeusedforin-situheattreatmentexperi-

ment on complex-shaped or large objects• Cryogenic chamber–provides temperaturesdown to -200

oC. It can be used on its own or with the stress rig



• Servo-hydraulicStressrig–appliesloadsupto100kN• Laserscanninginspectionarms–providesautomationofex-

perimental setup for complex-shaped samples and used with virtual laboratory, SScanSS [4]

• CybamanManipulator(samplerotationrobot)• 2DTransmission detector – energy selective neutron ima-

ging and measurement of strain in the direction parallel to the beam

Experiment highlights Surface measurement - Nanostructured hydroxyapatite coa-tings for orthopaedic implantsThe 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 bon-ding 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 co-ated 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 co-

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 qua-lity 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 problemMagnesium Elektron, Manchester is a world leader in magne-sium technology and alloy development. Their alloys are exten-sively used in the aerospace and automotive industries. For ma-gnesium to be a financially viable alternative to aluminium, the company need to be able to mass produce it. However, a signifi-cant 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 re-sidual stress within the DC-cast slab. Measurements at Engin-X allowed the residual stress within the slab to be mapped in de-tail (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 bron-ze statuettes An attractive feature of neutron techniques is the ability to iden-tify hidden materials and structures inside engineering compo-nents and objects of art and archaeology. Having this in mind we are investigating a new technique, Tomography Driven Dif-fraction, which exploits tomography data to guide diffraction ex-periments 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 Re-naissance 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 No-bleman’, and provided an indication of different material compo-sitions. Incorporating the tomography model into the SScanSS software tool allowed many aspects of the experiment to be

Figure 6

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


27

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)(c)

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 compo-sitions of superficial and internal parts, but also showed small amounts of ferrite present, which until recently was not repor-ted 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 temperatureIn order to increase the operating temperature in turbine engi-nes, a new generation of nickel-base superalloys has been de-veloped 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 proper-ties alongside improved creep resistance. The deformation me-chanisms 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

that changes of the γ’ slip mode from {111} to {100} with incre-asing 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 indi-cating that the γ matrix is softer. At 400oC and 500oC, an instan-taneous 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 transfor-mation plasticity in carbon steelTRIP steels are becoming increasingly exploited for industrial applications because they show high strength and high uniform elongation (ductility). Despite this interest, the relative contri-butions of the different strengthening and straining mechanisms are often poorly understood. Neutron diffraction using Engin-x was employed to quantify the contribution of different mechani-sms to ductility and work hardening for a 0.25wt%C steel. Diffe-rences 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 tran-sformation is not complete even after 20% strain. By contrast, at -50oC straining quickly gives rise to significant transformation,



even during the macroscopically elastic regime. By approxima-tely 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]

In-situ machining – Stresses due to electro-discharge machi-ning Engin-x enables the stresses evolved in real engineering proces-ses 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 in-situ the strains generated by EDM. The results confirmed that al-though 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

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 pro-cess. 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]

Outlook After 10 years of operating, Engin-X continues to be in high de-mand. Engin-X has attracted wide interest beyond traditional materials engineering, and now the user community has expan-ded 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 ma-terial performance becomes more critical. Engin-X has conti-nuously 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 in-strument around the world has this capability yet.Industry involvement is essential for the future of neutrons scat-tering, and Engin-X is pursuing this approach. We have provi-

Figure 7

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.


29

ded a free initial ‘consultancy’ for many companies on the use of neutron facilities. ISIS has launched a new Industry Collabora-tive 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 econo-mic 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 con-sortium of railway companies, etc. Because of the increasing de-mand 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 neu-tron tomography instrument at a pulsed neutron source is being built for the ISIS second target station. The new instrument for ma-terials science & engineering imaging, IMAT [15], will be a state-of-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 medium-resolution 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 con-tinuing 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 wor-king 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 com-posites 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 po-sitioning systems. Nuclear Instruments and Methods in Physics Research A. (2007) 571, 709-718.[5] M.R. Daymond, M. Preuss and B. Clausen, Evidence of varia-tion in slip mode in a polycrystalline nickel-base superalloy with change in temperature from neutron diffraction strain measure-ments, 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 co-atings 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. Fitzpa-trick, K. A. Khor, ‘Neutron diffraction residual strain measure-ments in nanostructured hydroxyapatite coatings for Orthopa-edic 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 combi-ned 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 to-mography 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 diffrac-tion 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. Wi-thers, Work hardening induced by martensite during 3 transforma-tion-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 andJ.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 instrumenta-tion design and train them about the background knowledge behind the real-ization of neutron instrumentation. The school offered two weeks of full immer-sion about neutron scattering instrumen-tation. 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 tech-niques at international neutron facilities. Instrumentation lectures addressed ba-sics on design and construction concepts about neutron sources, diffractometers, three axis spectrometers, time of flight in-elastic instruments (instrumentation us-ing thermal and epithermal neutrons), re-flectometers, filter spectrometers, Larmor labelling and sample environment equip-ments. In addition there were lectures on data acquisition and treatment and con-structability. 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 exam-ples drawn from the course material and to share research experiences. The second week focused on a particular technical is-sue, a specialized course on neutron de-tectors. The latter choice is very timely given the worldwide shortage of helium-3 detectors coupled with a desire for ever-larger pixelated detectors. Thus the sec-ond week, organized by Erik Schooneveld

and Giuseppe Gorini, addressed technical issues about gaseous, solid state, scintil-lator 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 electron-ics, Digitizer Data processing, GEM de-tectors).

The welcome ceremony of the INSIS edi-tion 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/15-07-concert/.

The school welcomed a total of 42 stu-dents, 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. Stu-dents came from Asia, Europe and the Americas, almost equally distributed among the three continents. Most of the students had some background in neu-tron 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


31

the world’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 IN-SIS 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/de-fault.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 An-dreani (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 – Chair (University of Rome Tor Vergata and CNR-IPCF), Daniela Ferrucci (INFN), Giovanni Mazzitelli (INFN), Massimo Pistoni (INFN), Giovan-ni Romanelli, Roberto Senesi (University Rome Tor Vergata and CNR-IPCF)1School 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).



The Third Meeting of the Union forCompact Accelerator-driven Neutron Sources

Following Beijing in 2010 (UCANS-I see Neutron News 22(1), 2011) and Bloomington in 2011 (UCANS-II, Notiziario Neutroni e Luce di Sincrotrone 17(1), 2012), the city of Bilbao, Spain, wel-comed 60 scientists and engineers from 8 countries to convene the third meeting, UCANS-III, during July 31-August 3, 2012. The program, featuring nearly 50 talks and posters, covered the areas of accelerator and moderator-target systems for compact neutron sources, instrumentation, scientific and industrial appli-cations, and future development. Additionally, the participants toured the ESS-Bilbao facilities in Zamudio and a nearby indu-stry park where companies have undertaken engineering design and manufacture of scientific instruments including compo-nents for accelerators and neutron scattering. While keeping the tradition of reporting the status of on-going operation and con-struction of compact accele-rator-driven neutron sources (CANS) (e.g., the CPHS-Tsinghua U and PKUNIFTY of China, DAFNE of INFN-Rome of Italy, ESS-Bilbao of Spain, HUNS-Hokkaido U of Japan, and the small accelera-tor sources at Centro Atómico Bariloche of Argentina and at RIKEN of Japan), UCANS-III forwarded a dialogue betwe-en compact, low-to-medium power sources with the lar-ge, high-power sources such as the ESS, J-PARC, and SNS of synergetic roles on target, moderator, and scattering in-strumentation R&D. The in-creasing interest in compact neutron sources is reflected in the expanded coverage and update of scientific and indu-

strial applications of CANS (e.g., novel detectors, imaging and radiography, fast-neutron-induced single event effects, boron neutron capture therapy, neutron dosimetry by Bonner Sphere spectrometry, and procurement of nuclear data). Other presen-tations (e.g., on neutron generation by novel lasers, accelerator-driven system for transmutation, and outreach activities to em-brace the materials research community) added witness to the cross-disciplinary hallmark of UCANS, which undoubtedly will continue in the future meetings.The Proceedings of UCANS-III will be published in the Physics Proceedings series by Elsevier and UCANS-IV will be held at Hokkaido, Japan during September 23-26, 2013.

Chun-K. LoongSun Yat-Sen University, China

The Organizing Committee took the opportunity of the conference dinner to reflect on past activities and contemplate an expanding scope in future UCANS meetings.


33

Shull Fellows now launched on interesting andfulfilling careers

“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

The Neutron Sciences Directorate’s presti-gious Clifford G. Shull Fellowship, a two-year research appointment at Oak Ridge National Laboratory (ORNL), is now invi-ting applications from early career scien-tists.The next Fellow hired will be the ninth since the pro-gram’s inception in 2006. With the world’s most inten-se pulsed accelerator-based neutron source at the Spalla-tion 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 Ba-sic Energy Sciences. The Fellowship Program at-tracts new scientific talent, making it possible for outstan-ding early career scientists to launch their careers. The research areas that use neu-

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 scat-tering, a technique that reveals where atoms are and how they behave within a material.The first two Shull Fellowships were awar-ded in 2006 to Andrew Christianson, who received his PhD in Physics from Colora-do 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 Ten-nessee, 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) follo-wed 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, com-putation, and neutron scattering to cha-racterize the structure and dynamics of soft matter.“The Shull award at the beginning of my

Agatha BardoelNeutron Sciences Directorate, Oak RidgeNational Laboratory, USA

Photos by Genevieve MartinNeutron Sciences Directorate, Oak RidgeNational Laboratory, USA

During a visit to SNS in November 2012, Clifford Shull’s son Robert (right) met with several former and current Shull Fellows and showed them his father’s Nobel Prize (left to right): Andy Christianson, Chris Stanley, and Yongqiang Cheng. Robert Shull is also a recognized scientist and leads the Magnetic Materials Group at the National Institute of Standards and Technology.



career provided me with the critical de-gree 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 re-ading history in his spare time, says the freedom to choose his own research to-pics, 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 cha-racterize the earliest structures formed by the huntingtin protein implicated in Hun-tington’s disease, a genetic neurological disorder. Using the high flux of the small-angle neutron scattering (SANS) beam lines at HFIR, they measured normal and pathological peptides and are now begin-ning to identify structural differences that could be important in this disease.Stanley, now an instrument scientist on the EQ-SANS (Extended Q-Range SANS) in-strument at SNS, is also using EQ-SANS for his work, as its event mode of data collec-tion affords advantages for performing me-asurements on protein structural dynamics.Sylvia McLain, co-fellow with Stanley in 2007, has since settled in the UK, whe-re 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 stu-dent, and a master’s student, with ano-ther postdoc on the way,” McLain says. The East Tennessee native investigates

the structure and dynamics of biological molecules in solution on the atomic scale. She has recently published a high-impact paper in Ange-wandte Chemie on the association of peptides in solu-tion as a model for protein folding and another in PloSO-NE on the structure of a cellulose pre-cursor in solution. The 2007 Shull Fellowship helped McLain expand her research to include more computation, she says, and to investigate the bio-physics behind mo-lecule association, which is important in any life-giving process. “Fellowships of this type are always beneficial becau-se you are awar-ded funding to do your own research, which is essential in establishing a scientific career.” How is she fin-ding life abro-ad? “I don’t have many hobbies these days, other than eating, potte-ring around my garden, and reading in my spare time, though I do blog about science and science policy and write for a UK national newspaper. I am very interested in the history and philoso-phy of science, so I try to spend a lot

of time thinking and reading about this when I can,” McLain says. Olivier Delaire, the 2008 Shull Fellow,

is now a staff scientist in the Neutron and X-Ray Scattering Group in the Ma-terials Science and Technology Division at ORNL. “The Shull Fellowship was for me a wonderful opportunity to grow as an independent scientist and take advantage of the world-class resources

In the SNS Executive Conference Room, Robert Shull and Associate Laboratory Director for Neutron Sciences Kelly Beierschmitt look at photos of Clifford Shull and colleague Ernest


35

at ORNL,” says Delaire, who works on materials that can be used for energy technologies.

He investigates the fundamentals of ato-mic dynamics related to the transport of energy at the microscopic level. Quan-tum vibrations of atoms in crystalline lattices (phonons) are responsible for the transport of heat in semiconductors or insulators (such as thermoelectric mate-

rials, semiconductors for microelectro-nics, photovoltaics, and thermal barrier coatings).

“Phonons also in-teract with elec-trons and other elementary exci-tations in solids, resulting in intere-sting physics with useful applications for ferroelectrics, polarons, super-conductivity, and multiferroics,” he says.Having the Shull Fellowship meant having the free-dom to establish his own research directions, as well as the opportuni-ty to collaborate with outstanding scientists across different divisions at ORNL. “The interaction with scientists at SNS and HFIR also hel-ped me to quickly gain expertise with techniques that I had not previously been exposed to, such as working

with single-crystals.”Delaire says he developed collaborations both within ORNL and in the broader science community as a collaborating principal investigator for a DOE-funded Energy Frontier Research Center. The work has led to several high-impact rese-arch papers.

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 assi-stant professorship in the Department of Physics and Astronomy at Michigan State University. Ke works in experi-mental condensed matter physics and studies complex oxide materials, for which neutron scattering is a powerfully efficient tool. “The neutron is a uniquely powerful ‘mi-croscope’ 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 as-sistant professor in the Department of Nuclear, Plasma, and Radiological Engi-neering, University of Illinois at Urbana-Champaign.“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 op-portunity to unleash your imagination,” Zhang says.Zhang too continues his ties with ORNL from his new home in Illinois, with col-laborations on neutron scattering experi-ments at SNS and HFIR.Why should one apply for the Shull Fel-lowship? “SNS is the most intense pul-sed accelerator-based neutron source in the world, and HFIR is a world-class re-actor-based continuous source. ORNL also has the most powerful supercom-puter in the world. Finally, the Shull Fellowship is the most prestigious fel-lowship in the neutron scattering field,” Zhang says.For more information about the Shull Fellowship, see:neutrons.ornl.gov/shullfellowship

In the SNS Executive Conference Room, Robert Shull and Associate Laboratory Director for Neutron Sciences Kelly Beierschmitt look at photos of Clifford Shull and colleague Ernest

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.”

NeutronSources

Synchrotron Radiation

Call for proposal


Neutron Sourceshttp://nmi3.eu/about-nmi3/access-programme/facilities---submit-a-proposal.html

Call for proposal [Deadlines for proposal submission]

To be announced

May 15, 2013 (for August-December cycle)

March 1 and September 1, annually

Any time

January 25, 2013

March 6, 2013(for July-December cycle)

To be announced

To be announced

January 25, 2013

Twice a year, to be announced

Mai 1 and November 1, annually

Any time

Any time

May 15, 2013

March 6, 2013(for July-December cycle )

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

BNC – AEKI Budapest Neutron Centrehttp://www.bnc.hu/modules.php?name=News&file=article&sid=39

BER II – Helmholtz-Zentrum Berlinhttp://www.helmholtz-berlin.de/user/neutrons/user-info/call-for-proposals_en.html#c63361

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

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

HFIR – Oak Ridge National Laboratoryhttp://neutrons.ornl.gov/

ILL - Institut Laue-Langevinhttp://www.ill.eu/users/important-dates/

ISIS – Rutherford Appleton Laboratoryhttp://www.isis.stfc.ac.uk/apply-for-beamtime/apply-for-beamtime2117.html

JCNS - Jülich Centre for Neutron Science http://www.fz-juelich.de/jcns/DE/Leistungen/Userinfos3/_node.html

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

LLB - Laboratoire Léon Brillouinhttp://www-llb.cea.fr/en/Web/avr2000_e.php

NPL – Neutron Physics Laboratoryhttp://neutron.ujf.cas.cz/en/instruments/user-access/nmi3

RID - Reactor Institute Delft http://tnw.tudelft.nl/index.php?id=33195&L=1

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

SNS – Oak Ridge National Laboratoryhttp://neutrons.ornl.gov/

NeutronSources

Synchrotron Radiation

Call for proposal

37

Synchrotron Radiation Sourceswww.lightsources.org

ALS - Advanced Light Sourcehttp://www-als.lbl.gov/index.php/component/content/article/58.html

ANKA - Institute for Synchrotron Radiationhttp://ankaweb.fzk.de/website.php?page=userinfo_guide&id=1#subpart2

APS - Advanced Photon Sourcehttp://www.aps.anl.gov/Users/Calendars/GUP_Calendar.htm

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

BESSY II – Helmholtz-Zentrum Berlinhttp://www.helmholtz-berlin.de/user/beamtime/proposals/index_en.html

BSRF - Beijing Synchrotron Radiation Facilityhttp://english.ihep.cas.cn/rs/fs/srl/usersinformation/callforproposals/201203/t20120329_83307.html

CFN - Center for Functional Nanomaterialshttp://www.bnl.gov/cfn/user/User_Program_Overview.asp

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

CLS - Canadian Light Sourcehttp://www.lightsource.ca/uso/call_proposals.php

CNM - Center for Nanoscale Materialshttp://nano.anl.gov/users/call_for_proposals.html

Diamond - Diamond Light Sourcehttp://duo.diamond.ac.uk/propman/duo/main/home?execution=e1s1

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

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

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

March 6, 2013(General User Proposals for August–December cycle)

Any time(Rapid Access Proposals)

June 30 and January 15, annually(for the scheduling periods October-March

and April-September, respectively)

March 8, 2013(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)

June 5, 2013(for the period between September and December 2013)

March 1 and September 1, annually

Any time

January 31, 2013 (For the period between May and August 2013)

May 30, 2013(for the period between September and December 2013)

Proposals are accepted at any time

February 27, 2013(For the period between July and December 2013)

March 8, 2013

April 1, 2013

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)

Synchrotron Radiation Sources Calendar

Call for proposal



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

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

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

LCLS - Linac Coherent Light Sourcehttp://www-ssrl.slac.stanford.edu/lcls/users/

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

MAX-labhttps://www.maxlab.lu.se/calls

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

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

PALhttp://paleng.postech.ac.kr/

PF - Photon Factoryhttp://pfwww.kek.jp/users_info/users_guide_e/

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

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

SPring-8http://www.spring8.or.jp/en/users/proposals/

SRC - Synchrotron Radiation Centerhttp://www.src.wisc.edu/users/apply_for_beamtime_IR.htm

SSRL - Stanford Synchrotron Radiation Lightsourcehttp://www-ssrl.slac.stanford.edu/content/user-resources/ssrl-deadlines

To be announced

To be announced

To be announced

January 15, 2013

To be announced

To be announced

January 31, 2013 (for the period between May and August 2013)

To be announced

To be announced

Proposal submission system has been newly launched

To be announced

February 15, 2013For standard proposal for the period between July and December 2013

For the period between January 2014 and January 2015

To be announced

January and July, annually

January 22, 2013(Crystallography Proposals for March-May scheduling)

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)

Synchrotron Radiation Sources Calendar

39

Calendar

January 14 – 17, 2013

January 21 – 22, 2013

January 23 – 24, 2013

January 23 – 25, 2013

January 23 – 25, 2013

February 4 – 6, 2013

February 11 – 15, 2013

February 13 – 15, 2013

February 28 – March 8, 2013

March 5 – 14, 2013

March 12 – 14, 2013

March 18 – 19, 2013

March 18 – 22, 2013

March 25 – 27, 2013

April 1 – 5, 2013

Mumbai, IndiaInternational Symposium on Neutron Scatteringhttp://www.barc.gov.in/symposium/isns2013/

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

Gif-sur-Yvette, France8th SOLEIL Users’ Meeting http://www.synchrotron-soleil.fr/Soleil/ToutesActualites/Workshops/2013/SUM2013/Accueil

Grenoble, FranceFlipper 2013 - International Workshop on Single-Crystal Diffraction with Polarised Neutronshttp://www.ill.eu/news-events/events/flipper-2013/

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

Grenoble, FranceESRF Users’ Meeting 2013 & Associated Workshopswww.tinyurl.com/dy2q6r2

Vienna, AustriaThe 13th Vienna Conference on Instrumentationhttp://vci.hephy.at

Lund, SwedenIKON 4http://ess-scandinavia.eu/news/35-news/594-first-announcement-ikon3-and-ikon4

Berlin, Germany33rd Berlin School on Neutron Scatteringhttp://www.helmholtz-berlin.de/events/neutronschool/

Didcot, UKISIS Neutron Training Coursehttp://www.isis.stfc.ac.uk/learning/neutron-training-course/

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

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

Grenoble, FranceADD2013 - School and Conference on Analysis of Diffraction Data in Real Spacehttp://www.ill.eu/ADD2013/

Grenoble, FranceESS Science Symposium on Neutron Particle Physics at Long Pulse Spallation Sourceshttp://www.ill.eu/news-events/events/nppatlps-2013/

San Francisco, USAMRS Spring Meetinghttp://www.mrs.org/spring2013/

CalendarCalendar Calendar Neutron Scattering

Scattering

Calendar


April 2 – 5, 2013

April 7 – 20, 2013

May 13 – 17, 2013

May 26 – 29, 2013

June 20 – 21, 2013

July 2 – 5, 2013

July 08 – 12, 2013

August 17 – 23, 2013

September 9 – 12, 2013

Geneva, SwitzerlandProbing Macromolecules at Water-Solid Interfaces – School on Surface Analytical Techniqueshttp://cm1101.unige.ch/

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

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

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

Berlin, GermanyGeneral Assembly NMI3-II 2013http://nmi3.eu/about-nmi3/education.html?back=yes

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

Edinburgh, Scotland2013 International Conference on Neutron Scattering http://www.icns2013.org/

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

Garching, Germany1st International Conference on Neutron Imaging and Neutron Methods in Archaeology and Cultural Heritage Research http://www.frm2.tum.de/indico/conferenceDisplay.py?confId=3

CalendarCalendar Calendar Neutron Scattering

Scattering41

ANSTO Australian Nuclear Science and Technology Organization Phone: + 61 2 9717 3111 Fax: + 61 2 9543 5097httP://www.ansto.gov.au/home

BER II Helmholtz Zentrum Berlin tyPe: Swimming pool reactor. 10 MWPhone: +49-30 / 80 62 - 42778Fax: +49-30 / 80 62 – 42523email: [email protected] httP://www.helmholtz-berlin.de/user/neutrons/

BNC - Budapest Research reactor tyPe: Swimming pool reactor, 10MW Phone: +36 1 392 2222Fax: +36 1 395 9162 email: [email protected] httP://www.kfki.hu/brr/indexen.html

CAB - Centro Atómico BarilochePhone: +54 2944 44 5100, Fax: +54 2944 44 5299email: [email protected] httP://www.cab.cnea.gov.ar/

Centre for Energy Research, Hungarian Academy of SciencesPhone: +36-1-392-2539 Fax: +36-1-392-2533email: [email protected]://www.energia.mta.hu.

CSNSPhone: 86 10 68597289 Fax: 86 10 68512458email: [email protected]://english.cas.ac.cn/

ESS AB European Spallation Source Phone: +46 46 888 30 94mobile: +46 72 179 20 94email: [email protected]://www.esss.se/

FLNP Frank Laboratory of Neutron Physics Phone: (7-49621) 65-657Fax: (7-49621) 65-085email: [email protected]://flnp.jinr.ru/25/

FRM II Forschungs-Neutronenquelle Heinz Maier-Leibnitz tyPe: Compact 20 MW reactor Phone: +49 (0) 89 289 10794 Fax: +49 (0) 89 289 10799 email: [email protected]://www.frm2.tum.de/en/user-office

GEMS German Engineering Materials Science Centre Helmholtz Zentrum Geesthacht Phone: +49 4152 871254 Fax: +49 4152 871338 email: [email protected]://www.hzg.de/central_departments/gems/index.html.de

HANARO Center for Applications of Radioisotopes and Radiation Korea Atomic Energy Research InstitutePhone: +82 42 868-8120 Fax: +82 42 868-8448httP://hanaro.kaeri.re.kr/english/index.html

HFIR ORNL, Oak Ridge, USAPhone: 865-576-0214 Fax: 865-574-096email: [email protected]://neutrons.ornl.gov/facilities/HFIR/experiment.shtml

IBR-2 Frank Laboratory of Neutron PhysicsPhone: (7-49621) 65-657Fax: (7-49621) 65-085email: [email protected]:// flnp.jinr.ru/474/

Neutron SourcesWWW SERVERS IN THE WORLDhttp://nmi3.eu/neutron-research/where.html

Facilities

Neutron Scattering Neutron Scattering

Facilities


ILLtyPe: 58MW High Flux Reactor.Phone: + 33 (0)4 76 20 71 11Fax: + 33 (0)4 76 48 39 06 Phone: +33 4 7620 7179Fax: +33 4 76483906email: [email protected] and [email protected] httP://www.ill.eu

IPEN – Peruvian Institute of Nuclear ResearchPhone: 226-0030, 226-0033226email: [email protected]://www.ipen.gob.pe/site/index/index.htm

IPNS - Intense Pulsed Neutron at ArgonnePhone: 630/252-7820Fax: 630/252-7722 email: [email protected] mail (for proposal submission)httP://www.pns.anl.gov/

ISIS Didcot tyPe: Pulsed Spallation Source.Phone: +44 (0) 1235 445592Fax: +44 (0) 1235 445103email: [email protected] httP://www.isis.rl.ac.uk

JCNS Juelich Centre for Neutron Science Forschungszentrum Jülich Phone: +49 2461 614750 Fax: +49 2461 612610 email: [email protected] [email protected] (for JCNS-1) [email protected] (for JCNS-2)httP://www.fz-juelich.de/jcns/EN/Home/home_node.html

J-PARC Japan Proton Accelerator Research ComplexPhone: +81-29-284-3398Fax: +81-29-284-3286email: [email protected] httP://j-parc.jp/index-e.html

JRR-3MFax: +81 292 82 59227 Phoneex: JAERIJ24596Eemail: [email protected]://www.jaea.go.jp/jaeri/english/index.html

JEEP-II ReactortyPe: D2O moderated 3.5% enriched UO2 fuel. Phone: +47 63 806000, 806275Fax: +47 63 816356email: [email protected] httP://www.ife.no/index_html-en?set_language=en&cl=en

KENS Institute of Materials Structure ScienceHigh Energy Accelerator Research Organization1-1 Oho, Tsukuba-shi, Ibaraki-ken,?305-0801, JAPANemail: [email protected] httP://neutron-www.kek.jp/index_e.html

KUR Kyoto University Research Reactor InstituteKumatori-cho Sennan-gun, Osaka 590-0494,JapanPhone: +81-72-451-2300Fax: +81-72-451-2600httP://www.rri.kyoto-u.ac.jp/en/

LANSCE Phone: 505-665-1010Fax: 505-667-8830email: [email protected]: [email protected]://lansce.lanl.gov/

LENS Low Energy Neutron SourcePhone: +1 (812) 8561458email: [email protected]://www.indiana.edu/~lens/index.html

LLB tyPe: Reactor Flux: 3.0 x 1014 n/cm2/sSecrétariat Europe :Phone: 0169085417 Fax: 0169088261 email: [email protected] httP://www-llb.cea.fr

McMASTER NUCLEAR REACTORPhone: 905-525-9140httP://mnr.mcmaster.ca/

MIT - Nuclear reactor Laboratoryemail: [email protected] httP://web.mit.edu/afs/athena.mit.edu/org/n/nrl/www/

Neutron Scattering

Neutron Scattering Neutron Scattering

Facilities

43

SINQtyPe: Steady spallation sourcePhone: +41 56 310 4666 Fax: +41 56 3103294 email: [email protected] httP://sinq.web.psi.ch

SNS Spallation Neutron Source Phone: 865.241.5644 Fax: (865) 241-5177email: [email protected] httP://neutrons.ornl.gov

MURRPhone: 1.573.882.4211email: [email protected]://www.murr.missouri.edu/

NIST Center for Neutron Research Phone: (301) 975-6210Fax: (301) 869-4770email: [email protected] httP://www.ncnr.nist.gov/

NPL – NRItyPe: 10 MW research reactorPhone: +420 2 20941177 / 66173428Fax: +420 2 20941155email: [email protected] and [email protected] httP://neutron.ujf.cas.cz/

NPREPhone: 217/333-2295 Fax: 217/333-2906httP://npre.illinois.edu/

NRU - Chalk River LaboratoriesPhone: 613-584-8293Fax: 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) 46047Fax: +7(813-71) 36025, +7(813-71) 31347 httP://www.pnpi.spb.ru/

RIC Reactor Infrasctructure CentrePhone: +386 1 588 5450Fax: +386 1 561 2335httP://www.rcp.ijs.si/ric/index-a.htm

RID Reactor Institute Delft (NL)tyPe: 2MW light water swimming pool. Phone: +31 (0)15 278 5052Fax: +31 (0)15 278 6422email: [email protected] httP://www.rid.tudelft.nl/en/cooperation/facilities/reactor-instituut-delft/

RISØ DTU Phone: +45 4677 4677Fax: +45 4677 5688email: [email protected]://www.risoe.dtu.dk/


Facilities


CAMD Center Advanced Microstructures & DevicesPhone: +1 (225) 578-8887

Fax: +1 (225) 578-6954

email: [email protected]

httP://www.camd.lsu.edu/

CANDLE Center for the Advancement of Natural Discoveries using Light EmissionPhone/Fax : +(37 4-10) 629806


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

CESLAB Central European Synchrotron LaboratoryPhone: +420-541517500


httP://www.xray.cz/

CFN - Center for Functional Nanomaterials Phone: +1 (631) 344-6266

Fax: +1 (631) 344-3093


httP://www.bnl.gov/cfn/

CHESS Cornell High Energy Synchrotron Source Phone: 607-255-7163

Fax: 607-255-9001

httP://www.chess.cornell.edu/

CLIO Centre Laser Infrarouge d’Orsay email: [email protected]

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

ALBA Synchrotron Light FacilityPhone: +34 93 592 43 00

Fax: +34 93 592 43 01

httP://www.cells.es/

ALS Advanced Light Source Phone: 510.486.7745

Fax: 510.486.4773


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

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

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


httP://ankaweb.fzk.de/

APS Advanced Photon SourcePhone: (630) 252-2000

Fax: +1 708 252 3222


httP://www.aps.anl.gov/

AS - Australian SynchrotronPhone: +61 3 8540 4100

Fax: +61 3 8540 4200


httP://www.synchrotron.org.au/

BESSY II - Helmholtz Zentrum BerlinPhone: +49 30 - 80620

Fax: +49 30 8062 - 42181


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

BSRF - Beijing Synchrotron Radiation FacilityPhone: +86-10-68235125

Fax: 86-10-68186229


httP://www.ihep.ac.cn/bsrf/english/main/main.html

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


Facilities

45

DFELL Duke Free Electron Laser Laboratory Phone: 919-660-2681

Fax: 919-660-2671


httP://www.fel.duke.edu/

Diamond Light Source Phone: +44 (0)1235 778000

Fax: +44 (0)1235 778499


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

ELETTRA - Synchrotron Light Laboratory Phone: +39 40 37581

Fax: +39 (040) 938-0902

httP://www.elettra.trieste.it/

ELSA - Electron Stretcher Accelerator Phone: +49-228-735926

Fax: +49-228-733620


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

ESRF - European Synchrotron Radiation Lab.Phone: +33 (0)4 7688 2000

Fax: +33 (0)4 7688 2020


httP://www.esrf.eu/

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

Fax: +49 351 269 - 0461


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

FELIX Free Electron Laser for Infrared experimentsPhone: +31-30-6096999

Fax: +31-30-6031204


httP://www.rijnh.nl/felix/

CLS Canadian Light Source Phone: (306) 657-3500

Fax: (306) 657-3535


httP://www.lightsource.ca/

CNM Center for Nanoscale MaterialsPhone: 630.252.6952

Fax: 630.252.5739


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

CTST UCSB Center for Terahertz Science and TechnologyUniversity of California, Santa Barbara (UCSB), USA


httP://sbfel3.ucsb.edu/

DAFNE Light INFN-LNF Phone: +39 06 94031

Fax: +39 06 9403 2582

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

DELSY Dubna ELectron SYnchrotron Phone: + 7 09621 65 059

Fax: + 7 09621 65 891


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

DELTA Dortmund Electron Test Accelerator FELICITA I (FEL) Fax: +49-(0)231-755-5383

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


Facilities


ISI-800 Institute of Metal Physics - Ukraine Phone: +(380) 44 424-1005

Fax: +(380) 44 424-2561


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

Jlab - Jefferson Lab FEL Phone: (757) 269-7100

Fax: (757) 269-7848

httP://www.jlab.org/FEL

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

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

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

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

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

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

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

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

LCLS - Linac Coherent Light SourcePhone: +1 (650) 926-3191

Fax: +1 (650) 926-3600


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

LNLS - Laboratorio Nacional de Luz SincrotronPhone: +55 (0) 19 3512-1010

Fax: +55 (0)19 3512-1004


httP://www.lnls.br/site/home.aspx

MAX-LabPhone: +46-222 9872

Fax: +46-222 4710

httP://www.maxlab.lu.se/

Medical Synchrotron Radiation Facility Phone: +81-(0)43-251-2111

httP://www.nirs.go.jp/ENG/index.html

FOUNDRY The Molecular Foundry1 Cyclotron Road, Berkeley CA 94720, USA

Phone: +1 - 510.486.4088


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

HASYLAB Hamburger Synchrotronstrahlungslabor DORIS III, PETRA II / III, FLASH Phone: +49 40 / 8998-2304

Fax: +49 40 / 8998-2020


httP://hasylab.desy.de/

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

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

INDUS -1 / INDUS -2 Phone: +91-731-248-8003

Fax: 91-731-248-8000


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

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

IR FEL Research Center FEL-SUT Phone: +81 4-7121-4290

Fax: +81 4-7121-4298


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

ISA Institute for Storage Ring Facilities - ASTRID-1Phone: +45 8942 3778

Fax: +45 8612 0740


httP://www.isa.au.dk/



Facilities

47

PSLS - Polish Synchrotron Light SourcePhone: +48 (12) 663 58 20


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

RitS Ritsumeikan University SR Center Phone: +81 (0)77 561-2806

Fax: +81 (0)77 561-2859


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

SAGA-LS - Saga Light Source Phone: +81-942-83-5017

Fax: +81-942-83-5196

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

SESAME Synchrotron-light for Experimental Science and Applications in the Middle Eastemail: [email protected]

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

SLS - Swiss Light SourcePhone: +41 56 310 4666

Fax: +41 56 310 3294


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

SOLEILPhone: +33 1 6935 9652

Fax: +33 1 6935 9456


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

SPL Siam Photon LaboratoryPhone: +66-44-21-7040

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

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

SPring-8 Phone: +81-(0) 791-58-0961

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


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

MLS - Metrology Light SourcePhysikalisch-Technische Bundesanstalt

Phone: +49 30 3481 7312

Fax: +49 30 3481 7550


httP://www.ptb.de/mls/

httP://www.ptb.de/mls/

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

Fax: +1 (631) 344-7206


httP://www.nsls.bnl.gov/

NSRL National Synchrotron Radiation Laboratory Phone: +86-551-3601989

Fax: +86-551-5141078


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

NSRRC National Synchrotron Radiation Research Center Phone: +886-3-578-0281

Fax: +886-3-578-9816


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/

PAL - Pohang Accelerator Laboratory San-31 Hyoja-dong Pohang Kyungbuk 790-784, Korea


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

PF - Photon FactoryPhone: +81 (0)-29-879-6009

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


httP://pfwww.kek.jp/


Facilities


TSRF Tohoku Synchrotron Radiation Facility Laboratory of Nuclear SciencePhone: +81 (022)-743-3400

Fax: +81 (022)-743-3401


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


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

SRC Synchrotron Radiation CenterPhone: +1 (608) 877-2000

Fax: +1 (608) 877-2001

httP://www.src.wisc.edu/

SSLS Singapore Synchrotron Light Source - Helios IIPhone: (65) 6874-6568

Fax: (65) 6773-6734

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

SSRC Siberian Synchrotron Research Centre VEPP3/VEPP4 Phone: +7(3832)39-44-98

Fax: +7(3832)34-21-63


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

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

SSRL Stanford Synchrotron Radiation LaboratoryPhone: +1 650-926-3191

Fax: +1 650-926-3600


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

SuperSOR SuperSOR Synchrotron Radiation FacilityPhone: +81 (0471) 36-3405

Fax: +81(0471) 34-6041


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

Fax: +7(095) 531-4656


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

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

www.cnr.it/neutronielucedisincrotrone [email protected]@roma2.infn.it

notiziario neutroni e luce di sincrotrone - issue 18 n.1, 2013

Documents

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kockelmann n school

new coherent source