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C Argoud
Editorial
5 Advanced materials take centre stage
In Brief
6 European support for SESAME
6 ESRF reveals new human ancestor
6 Industry runs deep at the ESRF
7 A decade of success for biology partnership
7 Chemistry under pressure
7 Users’ corner
South Africa becomes the twentieth country to join the ESRF, p9.
FEATURES
A Goodwin
9 South Africa joins the ESRF
11 How to build an ultimate light source
UPGRADE NEWS
12 Experimental halls complete
12 NINA on track
13 MASSIF takes shape
13 ID08 magnet in place
13 ID20 welcomes first users
PORTRAIT
23 Aase Marie Hundere: a Norwegian perspective
INDUSTRY
24 ESRF attracts nanoelectronics firms
IRT Nanoelec programme further opens the ESRF to industry, p24. recruitment
25 Browse the latest vacancies
IEEE Trans. Appl. Supercond. 18 1754
Beauty OF science
Number 64 July 2013
26 Synchrotron reveals bioceramic jawbone
Inside materials
IN THE CORRIDORS
26 X-ray scanners reveal too much
26 Dutch firms visit Grenoble
On the cover: 26 What does the ESRF mean to you?
Porosity formed during 26 Windows 8 put on hold
the processing of a South Africa joins the ESRF
www.cosylab.com
Editorial
Mastering materials
Editor The development of existing technologies and the creation of new ones with reduced
Matthew Chalmers
Tel +44 (0)7857 866 457 environmental impact rely on advanced materials with specifically tailored properties. A deep
E-mail mdkchalmers@gmail.com knowledge of the structure of materials is crucial for understanding material properties and,
Editorial committee in the case of artificially engineered materials, for validating theoretical predictions.
Nick Brookes
Dominique Cornuéjols
Bauke Dijkstra
Complementary to static structure determination is the study of the structure and
Andy Fitch morphology of materials during their synthesis or under realistic working conditions. These
Claus Habfast
in situ studies provide fundamental information about different phases in a material’s lifecycle
Axel Kaprolat
Joanne McCarthy – the steps that underpin its formation or production. Synchrotron-based techniques provide
Sean McSweeney a deep understanding of each step at the atomic or molecular level, allowing researchers
Harald Reichert
Francesco Sette to optimise and control a material’s overall performance. In situ X-ray studies also provide
information about the intrinsic dynamics of a material’s structure during mechanical or
Subscription
Chantal Argoud
chemical degradation, offering ways to block or delay such processes.
For subscriptions to the digital version of
ESRFnews (print subscriptions are no longer
possible), visit http://go.esrf.eu/esrfnews
In recent years, ESRF staff and users have developed numerous new techniques to resolve
the structure of materials with superior spatial and temporal resolution. The coupling
ESRFnews is produced for the ESRF by of synchrotron probes with more standard laboratory techniques allows precise control
IOP Publishing
Temple Circus of sample conditions, making it possible to relate variations of a material’s properties to
Temple Way modifications in its underlying structure.
Bristol BS1 6HG, UK
Tel +44 (0)117 929 7481
www.iop.org The sample environment group at the ESRF has
Publisher
developed a broad range of instruments that allow “Advanced materials
users to alter the sample temperature from a few
Kelvin to a few thousand Kelvin, or to employ magnetic will continue to take
Susan Curtis
Group editor
Joe McEntee
Art director fields in excess of 30T, for example. Mobile infrared centre stage”
Andrew Giaquinto spectrometers are now available for installation at
Production
Alison Gardiner beamlines, as are scanning probe microscopes that are
Technical illustrator compatible with the electrically and mechanically noisy environment of an X-ray beamline.
Alison Tovey
Display-advertisement manager
These microscopes are not only able to image material surfaces in situ, but are valuable tools
Edward Jost with which to align nanosized X-ray beams with nanoscale objects. They also allow users to
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Mark Trimnell
apply a force on a nano-object in order to induce a mechanical response.
Marketing and circulation
Angela Gage This issue of ESRFnews is dedicated to advanced materials. The examples illustrate only
ISSN 1011-9310 a small subset of the full range of materials studied at the ESRF and the experimental
techniques on offer, but provide a snapshot of some of the latest advances in this important
©2013 ESRF
field. The commissioning of new facilities, such as the new electrochemistry and catalysis
laboratories, bear witness to the ESRF’s dedication to providing users with the best possible
support. These particular facilities will provide tools for controlling processes occurring at the
interface between a conducting solution and a conducting substrate, which are relevant for
many technological applications such as batteries, fuel cells and photovoltaics.
With new and upgraded beamlines becoming available to the user community that target
specifically the structure of materials down to the nanoscale, research on advanced materials
will continue to take centre stage at the ESRF.
ESRF/P Tafforeau
found has provided new insights
into our evolutionary past, thanks
CERN will provide the magnets to X-ray imaging at the ESRF. The
for SESAME’s storage ring. 55 million-year old fossil, which
represents a previously unknown
EC backs SESAME genus and species Archicebus
Achilles, is thought to have come
The European Commission is to from a pivotal “branch split” in
contribute €5 m towards SESAME, primate and human evolution
the third-generation light source that put monkeys, apes and
under construction in Jordan. humans (the anthropoids) on a
The agreement allows CERN to separate evolutionary lineage to
work with SESAME researchers to tarsiers.
develop magnets for the facility’s Archicebus differs radically
storage ring, paving the way for from any other primate known to
first beams in 2015. science, according to Christopher
SESAME’s injection systems Beard of the Carnegie Museum of
are based on hardware donated Natural History in Pittsburgh, one
from the BESSY source, but its of the authors of the research. “It
storage ring will be completely looks like an odd hybrid with the
new. “We are responsible for feet of a small monkey, the arms,
providing the magnets of the legs and teeth of a very primitive
new storage ring, namely 16 primate, and a primitive skull
bending magnets, 32 focusing bearing surprisingly small eyes.”
quadrupoles, 32 defocusing Archicebus belongs to a
quadrupoles, 64 sextupoles/ separate branch of the primate
correctors, plus spares,” says evolutionary tree that is closer to
CERN magnet engineer Attilio the lineage leading to modern
Milanese. “We’ve been working monkeys, apes and humans.
on this project with colleagues Team leader Xijun Ni of the
in Jordan since several months, Chinese Academy of Sciences in 3D image of Archicebus Achilles, which is 7m years older than the
so the technical work is well Beijing says the result represents oldest fossil primate skeletons previously known.
advanced.” The magnet designs a big step forward in our efforts
are now complete and CERN is to chart the course of the earliest allowed the team to piece “For several years the ESRF
ready to issue calls for tenders. phases of primate and human together the two separate parts has developed imaging facilities
“SESAME is one of the most evolution. “It will force us to and digitally reconstruct 3D enabling us to non-destructively
important projects in the world rewrite how the anthropoid images of the fragile creature study fossils buried in rock with a
right now,” said CERN director lineage evolved,” he said. (Nature 498 60). Extrapolating level of detail and contrast unique
general Rolf Heuer, “with its close The fossil was excavated by a from statistical analyses, in the world,” says coauthor
parallels to the origins of CERN, I local farmer from sedimentary Archicebus is thought to have Paul Tafforeau of the ESRF X-ray
am very happy that we are able to rock strata in an ancient lakebed weighed only about 20–30 g and imaging group. “We’ve been able
make this important contribution in central China’s Hubei Province. be smaller than today’s smallest to reveal microstructures that
to the young laboratory’s Computed tomography scanning living primates, overturning would normally require partial
success.” at the ESRF’s ID17 beamline conventional wisdom. destruction of the specimens.”
NASA
chemical reactions because their
outer electronic shells are fully
occupied. At high pressures and
temperatures, however, noble
A PSB technical platform. elements such as xenon exhibit
rich chemistry that provides
Biologists celebrate clues to the inner workings and
decade of success evolution of planets.
Using laser-heated diamond
The discovery of the 3D structure anvil cells at the ESRF’s ID27
of the flu virus polymerase has beamline, Chrystèle Sanloup
opened new possibilities for anti- of the University of Edinburgh
flu drugs, and is just one example and co-workers have discovered
of the successes of the Grenoble that xenon reacts with water
Partnership for Structural Biology ice at pressures above 50 GPa Understanding the composition of Jupiter and other “gas giants” sheds
(PSB) during the past decade. and temperatures of 1500 K – light on planetary evolution in the solar system and beyond.
In 2003, the ESRF joined forces conditions found in the interiors of
with nearby institutes EMBL and Uranus and Neptune. In situ X-ray witnessed amazing advances in depletion of elements such as
ILL along with three local research diffraction revealed the presence the last decade with over 100 neon in Jupiter’s atomsphere.
centres and universities to pool of a hexagonal lattice with four xenon compounds synthesised, The team now plans to explore
knowledge and equipment in xenon atoms per unit cell and essentially by UV photolysis. But the reactivity of xenon with other
structural biology. several possible distributions the pressure variable has seldom materials at extreme conditions.
On 4 June more than 150 of oxygen atoms. The team been used, with only a couple van “We have used the ESRF before to
specialists from across Europe combined the diffraction data der Waals compounds discovered study the reactivity of xenon with
gathered in Grenoble to mark with ab initio calculations in order so far.” silicon oxide to look for potential
the PSB’s tenth anniversary. to fully solve the crystallographic The discovery of a pure xenon xenon phases stable at depth in
Providing unique tools ranging structure of the compound (Phys. oxide phase extends the chemistry the Earth that could explain the
from sample expression and Rev. Lett. in press). of xenon in natural conditions atmospheric deficiency in xenon,”
crystallisation to structure “We wanted to see if pressure to pressures relevant for the Sanloup told ESRFnews. “The
resolution and imaging, the PSB could be used as a variable to giant planets, says Sanloup, and next step will be to target other
has helped drive the explosion synthesise xenon compounds,” adds further evidence for the light oxides and to try to map the
in structural biology research in explains Sanloup. “The field sequestration of noble gases at pressure-temperature-chemical
Grenoble in recent years. of noble gas chemistry has depth thought to explain the space of xenon.”
Users’ corner
At the last proposal submission data collected either entirely or a full XAFS scan to be taken submitting proposals. See p13 for
deadline on 1 March, 1011 new partially at ESRF are registered in a few seconds, with similar a detailed report.
proposals were received. It in our database via our easy- durations for full high-resolution l The nano-imaging beamline
marks another record number to-use interface: www.esrf.fr/ PD measurements thanks to a ID16A-NI and nano-analysis
of proposals received per UsersAndScience/Publications/ new 12 MP flat-panel CMOS. The beamline ID16B-NA will open
operational beamline. publication-notification-form. system is fully integrated for user for users during the scheduling
The next deadline for operation. period 2014-I (proposal deadline
submission of standard proposals News from the beamlines l ID02 will close down to be 1 September 2013). ID16A-NI
is 1 September for beam time l ID01 will be closed for upgraded in July 2013, with user will offer sub-50 nm beams with
during March–July 2014. users due to upgrade works operation expected to restart in mild monochromaticity (1%),
Proposers must use the most from December 2013, with Spring 2014. The new beamline while ID16B-NA will offer a multi-
recent “Experiment Methods” user operation to resume in with 30 m variable sample- modal approach designed to
template available on the user November 2014. Depending on detector separation will have accommodate different micro-
guide web pages and respect the their requirements, users may high-resolution and ultra small- analytical techniques combined
two-page length limit. Review consider ID13, ID03, ID10 or angle scattering capabilities. It with X-ray imaging. See p12 for a
panels will reject proposals that ID02 as alternative beamlines will be available for the next call detailed report.
do not respect the limit. Proposers and should discuss with the of proposals. l The high-resolution powder
should also ensure that they respective beamline scientist l ID08, which is being upgraded diffraction beamline ID31 will
submit experiment reports for all before submitting proposals. and moved to ID32, will be open close in December 2013 and will
relevant previous proposals. l Considerable progress has been for proposals for the XMCD be moved to ID22. It will re-enter
To confirm the status of open made at the Swiss Norwegian branch in the coming September user service in April 2014 with an
ESRF beamlines for the Beamline station BM01B in round. Partial user operation is energy range extended beyond
1 September deadline, proposers allowing users to follow chemical expected in the first half of 2014, the current limit of 63 keV.
are invited to check here and and catalytic processes in situ with the move towards full user Scientists wishing to submit
on the Beamline Status web using quasi-simultaneous XAFS, operation (including the opening proposals should remember
page. Users are also reminded powder diffraction (PD) and of the RIXS branch) for the March to request beamline ID22 for
to make sure that all new Raman spectrometry. The recent 2014 proposal round. Please proposals submitted from the
publications resulting from monochromator upgrade allows contact beamline staff before 1 September deadline onwards.
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Feature
C Argoud
the 20th country to join the
ESRF, and researchers there
are already planning new
experiments.
Scientists in South Africa have been involved
with the ESRF since the beginning of user
operation in 1994, when Trevor Derry of the
University of Witwatersrand carried out the
first synchrotron studies of diamond surfaces in
collaboration with teams from the ESRF and the
Netherlands. Derry hasn’t returned to the ESRF
since then but, like many researchers in South
Africa, he now expects to take full advantage of
the country’s newly agreed membership.
On 21 May, South Africa representatives ESRF director general Francesco Sette and secretary to the ESRF Council Itziar Echeverría tie
signed a medium-term arrangement that will the knot with Nithaya Chetty of the National Research Foundation of South Africa.
enable the country to participate in the ESRF
at a level of 0.3% for the next five years. “This facility’s research capabilities that on returning Subterranean treasure
agreement strengthens a relationship that home he immediately wrote to the then Diamonds (see box below) are not the only
has already produced numerous important president of the NRF suggesting that South treasure lying beneath South African soil. In
results – notably in palaeontology, materials Africa seek ESRF membership. “Just over a 2008 paleoanthropologist Lee Berger of the
science and macromolecular crystallography decade later it seems that ‘we have seen the University of Witwatersrand uncovered a new
– and builds ties between South Africa and light’, which has involved the tireless efforts of species of early human ancestor in the Malapa
the international synchrotron radiation our synchrotron research community,” he told Nature Reserve: Australopithecus sediba. In
community,” said ESRF director general ESRFnews. “I will obviously try to exploit this February 2010, he took the 1.9 million year-old-
Francesco Sette. Nithaya Chetty, group wonderful opportunity.” fossil to the ESRF, and the high-resolution X-ray
executive for astronomy at South Africa’s Fellow University of Johannesburg physicist scans at ID17 of the fossil’s brain case enabled
National Research Foundation (NRF) said the Bryan Doyle, who completed a post-doc at Berger and co-workers to shed light on the
agreement was “a solid achievement that the ESRF at the turn of the millennium, is transition from Autralopithecus to Homo.
makes us extremely happy”. also planning to submit proposals in light of Sasol, the South African energy company
the new arrangement. “I do not think that based in Johannesburg, has a long-standing
Proposal time the importance of us joining the ESRF can industrial partnership with the ESRF to
When physicist Giovanni Hearne of the be overstated,” he says. “It makes it much synthesise hydrocarbons via the Fischer-
University of Johannesburg undertook high- easier to convince people who have not Tropsch reaction. The ESRF allows Sasol
pressure experiments at the ESRF in 1999, yet discovered the enormous benefits of scientists to study the reaction under realistic
he recalls having been so impressed by the synchrotron radiation to become users.” conditions to gain a deeper understanding of
the company’s proprietary catalysts.
Diamond optics demand crystal perfection Africa is the only continent that does
not yet have a synchrotron, and the new
Most materials either absorb or transmit has remained a key player in the development agreement is part of a broader NRF plan to
X-rays, making it difficult to build components of diamond optical elements.” fund access to other synchrotrons worldwide.
that manipulate X-ray beams. Silicon’s high Lower quality diamonds have long been “For some years now, we have seen a new
degree of crystal perfection has made it used as windows, filters and polarising growth trajectory in science in South Africa,”
the material of choice, but diamond has elements, explains Connell. But it is only in the said Thomas Auf der Heyde of South Africa’s
several advantages including a higher heat last five years or so that diffracting elements Department of Science and Technology.
conductivity, lower thermal expansion and such as beam splitters and monochromators, “The agreement between the NRF and ESRF
lower absorption. Only synthetic materials especially those in imaging or coherent serves to further build human capital and
made using high-pressure high-temperature related applications, have been possible. “For research capacity for sustainable growth and
techniques can achieve the necessary single applications subjected to the highest intensity development.”
crystalline quality (pictured). radiation, in particular The new agreement is imperative if South
ELEMENT SIX TECHNOLOGIES
An industrial partnership initiated between for X-FELS, diamonds Africa is to become internationally competitive
Element Six Technologies in Johannesburg, may turn out to be the across a broad spectrum of disciplines,
the University of Johannesburg and the only solution,” he says. adds Hearne. “Not only do we now have
ESRF over a decade ago was the first source convenient access to one of Europe’s most
of high-quality diamonds for X-ray optical A synthetic diamond powerful research tools but it will likely lead to
elements, says physicist Simon Connell of of exceptional bulk new collaborations with European colleagues
University of Johannesburg. “The ESRF was quality and surface and students,” he told ESRFnews. “We are
certainly a very significant early player and finish. now limited only by our imagination.”
Matthew Chalmers
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The ESRF is at an advanced stage of an will be provided by lining the entire storage
“We are
ambitious upgrade. The first phase, based ring with non-evaporable getter coatings
on new and improved beamlines and developed at the ESRF. The increased number
instrumentation, is two-thirds complete. The of dipoles also means that we have to install
second phase, foreseen for 2015–2019, is
designed around a new storage ring lattice
working within more bending-magnet radiation absorbers
along the beam path.
that will reduce the horizontal spread of
emittance of the ESRF’s electron beam 4 nm to
very strong All this has to be achieved while also
leaving space to extract the X-rays from the
less than 0.2 nm – boosting the brilliance and
coherence of its X-rays to values never before constraints.” chamber. The strong dipoles in the existing
lattice make it relatively easy to separate
achieved at a synchrotron. the light from the path of the electron
Much progress has already been made beam, but the very small dipole angle of
towards this goal. The ultra-low vertical the new machine requires a much more
emittance and orbit stability provided by the emittance thanks to an increased number complicated chamber design. Moreover, the
new beam-positioning electronics and the of bending magnets (dipoles) and stronger lack of space restricts where we can install
fast orbit feedback system, for instance, are focusing magnets (quadrupoles and vacuum chamber hardware such as flanges,
fully compatible with the requirements of a sextupoles). It comprises 33 magnets per cell, bellows and pumps and also the diagnostic
next-generation storage ring. But a smaller which is about twice as many as are in the equipment. We therefore expect to have to
horizontal emittance is a recurrent request present machine, and the quadrupoles must design and build more complicated chambers
from the ESRF beamlines: highly brilliant have a very small magnet bore to achieve the than those in the present machine.
nanobeams allow users to extract maximal necessary magnetic gradients. The magnetic
information about materials. design of the high-gradient quadrupoles is Machine multitasking
Since December last year, when the well advanced and prototypes will be built These are just a few of the many exciting
ESRF Council endorsed the management’s during the second half of 2013. Sextupoles challenges involved in building the world’s first
proposal to launch the technical design study and the combined dipole-quadrupole magnet ultimate storage ring – which has to be carried
of the new machine lattice, members of the are presently under study. out while continuing actions from Phase I
Accelerator and Source Division have been The dipoles in the existing storage ring of the ESRF upgrade and, of course, while
working hard to ensure that a lattice that are electromagnetic, but the ESRF’s 20 years providing full access to users for experiments.
works perfectly on a computer can be built, of experience with permanent magnets Nine workflow packages have been identified
installed and operated reliably in practice. (for instance in insertion devices) allows to undertake the task. The ESRF’s plans are
us to design high-performance, compact based on pushing existing technologies to
Conceptual design permanent-magnet dipoles. Permanent their limits, but R&D will also be undertaken
The new design maximises the use of existing magnets take up less space on the lattice, into permanent-magnet designs, high-
infrastructure, with all insertion-device and and lead to significant savings in the cost of gradient quadrupoles and low-conductance
bending-magnet beamlines being kept in operating the machine. vacuum chambers.
addition to the present injector chain. The The magnet aperture defines the shape of The technical design study will be complete
storage ring itself will be rebuilt from scratch the vacuum chamber, which is another major by autumn next year. Should the green light
while preserving its 32-cell periodicity, challenge presented by the Phase II machine. for construction be given, the procurement
beamline positions and energy. Achieving Since the new lattice will pack more magnets and pre-assembly phase will begin in 2015
this within the same tunnel puts very closer together, in practice we will have just and the machine will then be stopped for
strong constraints on the lattice design and 3–4 m of “drift space” per cell compared approximately one year starting in August
engineering. to 8 m presently. The smaller magnet bore 2018 to install and commission the new ring.
The Phase II lattice – technically a “hybrid means a narrower vacuum chamber, requiring User access would begin late 2019, opening a
7-bend achromat” – achieves its record low distributed pumping, and additional pumping new chapter in synchrotron science.
R DIMPER
Construction work on the Belledonne and
Chartreuse experimental hall extensions (EX2
project) are complete. The two new halls were
delivered in mid-June, one month behind
schedule, with the laboratory and office
building expected to be ready at the end of July.
The inauguration of the new premises took
place on 24 June as ESRFnews went to press.
An important milestone was reached at
the end of April with the pouring of the final
layer of the high-quality concrete slabs in
the Belledonne and Chartreuse halls. This
layer, made out of a special concrete mix
and steel mesh, is 30 cm thick and required
3500 tons of concrete in total. Together with
precise temperature control in the halls, the
monolithic slabs will provide stable conditions
for the new nano-beam capabilities of the
ESRF Upgrade Programme.
“First measurements throughout May
confirm that the slabs are within specifications
concerning their planarity and vibration
stability,” says Rudolf Dimper, head of the
ESRF’s Technical Infrastructure Division.
“The drying process appears to generate
less shrinkage than expected and so far no
micro-cracking could be observed. This is
an important, successful and very promising
milestone indeed.”
C ARGOUD
The regionally funded CPER project (Contrat
Project Etat Region) is also proceeding well.
Completion of the new site entrance is
scheduled for the end of the year, while the
complete refurbishment of the site restaurant
is underway and the first floor of the
restaurant building is almost complete. The
new chalet located next to the guesthouse
is also finished and can be booked online for
social events.
“All works for the restaurant extension will
hopefully be finished this autumn, while the
science building, under the supervision of the
ILL, will be complete in the next few months,”
says Dimper. “The ESRF is looking forward
to relocating important laboratories into this
new building which, given the many common
activities between the ILL and ESRF, will play a The exterior of the new laboratory and office building and the high-quality concrete slab of the
pivotal role on the site.” Belledonne experimental hall extension.
P EVANS
the properties of the material with their
function,” says Martínez-Criado. “Our
work represents a step toward not only
the validation of theories of quantum
confinement, but also the realisation
of nanostructures with spectroscopic
properties that could prove advantageous in
nano-devices.” Multiferroic memory
In situ catalysis The magnetically driven memory inside
High-energy diffraction at the ESRF offers a hard-drives is extremely robust, but it
powerful tool for industry to track processes requires a lot of energy to write and erase
inside a working chemical reactor. A better data. Electrically driven “flash” memory
understanding of each step in reactions consumes less energy, but currently is not as
under industrial conditions can help chemical stable as magnetic memory and offers lower
manufacturers improve efficiency and reduce storage densities. Users of the ESRF’s XMaS
costs. beamline (BM28) are turning to advanced
Last year, users at ID15B undertook multiferroic materials – which couple electric
in operando studies of the zeolite catalyst and magnetic properties – to develop more
SAPO-34 in a custom built mini-reactor. This efficient data storage.
material is key to the methanol-to-olefin Philip Ryan of Argonne National
process, whereby inexpensive feeds such as Laboratory in the US and co-workers used
coal and biomass are converted into useful the unique sample environment at XMaS
hydrocarbons, but the build-up of coke to combine a high magnetic field and a
in its zeolite cavities causes the catalyst to high electric field at the extremely low
deactivate. Real-time structural data allowed temperatures at which europium titanate
the team to correlate growth in size of the unit reveals dual magneto-electric behaviour.
cell of the zeolite catalyst with its deactivation Nanometre-thin europium titanate was
at different positions in the reactor. Diffraction previously known to change from being
t the ESRF’s ID01 beamline. patterns were collected every second as the a paraelectric antiferromagnet to a
reactor setup was moved through the beam ferroelectric ferromagnet when stretched
Nanowires light up LEDs (Angew. Chem. Int. Ed. 51 7956). at temperatures close to absolute zero.
Nanowires are also In collaboration with several European Under strain, the two co-existing magnetic
promising materials with institutes, ESRF researchers are also carrying interactions compete, raising the possibility
which to exploit the out in situ studies of the catalytic reactions of switching between the two states by
counterintuitive occurring in car exhausts, in which applying a small electric field.
behaviour of noble-metal nanoparticles convert Ryan and colleagues observed such
quantum mechanics. unburned hydrocarbons and other a switch for the first time using X-ray
Compared to the planar exhaust gases into water, carbon dioxide resonant magnetic scattering, and could
semiconductor architecture of and nitrogen. These studies are carried out at explain the underlying intrinsic mechanism
LEDs, nanowires are more “area effective” different levels ranging from model systems using first principles calculations (Nature
and can fit within the building blocks of to the “real” reactor, explains Roberto Felici, Communications 4 1334).
nanophotonic devices such as light-emitting scientist in charge at ID03. For example, “XMaS gives you the freedom to measure
diodes (LEDs) and lasers, explains the ESRF’s experiments at ID03 have revealed that complicated diffraction geometries in
Gema Martínez-Criado. “Nanowires allow palladium nanoparticles under exposure to these very specific environments that
more sensitive control of parameters such carbon monoxide form a carbide phase that you can control and change,” said Ryan.
as the geometry and composition of the may play an important role in the reaction. At “From a potential application point of
quantum well.” ID15, the same phase has been observed in a view the results here suggest that the key
Core−multishell nanowires with a real car exhaust. requirements for the valuable coupling
hexagonal cross section are predicted “Nanoparticles exhibit a number of of these two properties might not be as
to confine charge carriers in 2D at the characteristics that are not present in unique and rare as first thought. This can
hexagon corners – a potentially bulk form, and these experiments give only increase the chances of being able to
useful property for LEDs that us the possibility to design nanoparticles replicate them together at higher, more
until now had never been with higher selectivity for a particular commercially appropriate temperatures.”
observed. Using energetic reaction and with a longer lifetime,” says The measurements were all done in
X-ray nanobeams at the ESRF’s Felici. “The in situ catalysis experiments situ with both electric and magnetic fields
ID22 beamline, Martínez-Criado now being undertaken at the ESRF have applied on the sample, adds XMaS beamline
sured (above) and and co-workers imaged such confinement never been done before, and they provide co-ordinator Laurence Bouchenoire. “Other
icted (top right) in gallium arsenide/indium gallium arsenide hugely important information about the examples of advanced materials research
er localisation at multi-quantum-well nanowires by combining numerous individual steps underpinning a carried out at XMaS include studies of liquid
exagonal corners optical luminescence with X-ray fluorescence working catalyst.” crystals and organic photovoltaic devices.”
nanowire. spectroscopy (Nano Letters 12 5829). Matthew Chalmers
www.luxel.com
Tel: 1-360-378-4137
info@luxel.com Friday Harbor, WA. USA
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3D crack-tip microscopy Novel composite materials such as titanium silicon carbide are lighter and can handle higher
Crack propagation in metallic materials is temperatures than traditional metals.
well understood. But aircraft manufacturers
are increasingly turning to more complicated a promising candidate for jet engine parts “I’d guess we’re talking 15 years before
composite materials that are lighter, stronger including new “bladed ring” designs. The such high-temperature composites could
and can operate at higher temperatures. Lower A380 and Boeing’s 787 Dreamliner already enter production,” says Withers. In the search
weight reduces fuel consumption, while higher employ polymer-based composites in the for tough ceramics that can operate at even
engine operating temperatures allow aero- fuselage frame and skin, but only metallic higher temperatures the team is also looking
engines to be more efficient. The challenge composites can handle the hostile conditions to natural systems – namely seashells, which
is to understand how cracks propagate inside an aero-engine. owe their toughness to multiple layers.
in such materials. Electron microscopy Composites typically contain three distinct Ceramics also show potential to be turned into
reveals the surface features of micro-cracks, phases: a metallic matrix, non-metallic fibres self-healing materials that repair themselves
but synchrotron X-rays penetrate tens of and the interface between them. In this upon damage.
millimetres into a sample where the behaviour system, cracks do not propagate in a planar
of cracks can be very different. manner, but instead divert along the interfaces. Nuclear issue
“The wonderful thing about the ESRF is that Provided the interfaces are not too strong Better knowledge of crack propagation
it provides two pieces of information: imaging, the fibres themselves don’t break, explains transfers directly to other industries in which
to see how the crack grows, and diffraction, Withers. Once the crack goes past the fibres, failure is unacceptable, says Withers, notably
which tells us about the local stresses that it they stop the crack from growing – just like the nuclear industry. Here, the team exploits
grows under,” Withers explains. “ID15 is one of extra stiches in a material stop it from tearing. the unique power of ID15’s X-rays to penetrate
the few beamlines in the world where you can “Understanding that sequence tells us how to up to 30 mm of steel. Such measurements
switch effortlessly between the two modes to engineer the material,” he explains. are used to support sophisticated model
form a kind of crack-tip microscope.” Withers and co-workers recently studied predictions in order to make advanced safety
In conjunction with Rolls-Royce, Withers cracking in titanium-silicon-carbide at ID15. cases for reactor systems.
and co-workers have been using the ESRF The ability to monitor cracks under load at “Engineers are always looking for devious
since the early 1990s to investigate novel high temperatures allowed the Manchester new ways to ensure that cracks don’t grow or,
composite materials such as titanium team to evaluate the potential of these if they do grow, to find new ways of stopping
reinforced with silicon carbide fibres. This materials under realistic conditions (Proc. R. them,” remarks Withers. “ID15 is so useful
material can operate at higher temperatures Soc. A 468 2722; Acta Materialia 60 958). because it allows you to both see how the
than titanium alone, making it cracks progress but also to map the local
stresses that causes them to grow. That
3D crack-tip microscopy allows you to make realistic estimates
shows a crack (purple) of the lifetime of existing components
growing in a composite and to design safer, more crack-
material containing resistant materials for the future.”
silicon carbide fibres. Matthew Chalmers
B POKROY
Opp
in it
(left
(rig
300
the
Spicules from the simple sea creature Herdmania momus contain large single crystals vaterite of higher quality than those in the synthetic
vaterite used in previous structure determinations.
J Stettner
makes it the material of choice for electrical
contacts. Not only can copper be drawn easily
into wires but by discharging copper ions
from solution under an applied voltage
(a process called electrodeposition) copper
can be fashioned into ultra-small connections
for chips and circuit boards.
The relentless miniaturisation of electronics
demands reliable electrical interconnects at
the nanoscale, which requires precise control
of the electrochemical deposition processes
and hence an improved understanding of
the underlying physics and chemistry. The
smallest features on today’s chips can be as
little as 100 atoms wide, so the slightest defect
can severely degrade or cause a loss of the
electrical contact.
In contrast to copper epitaxial growth under
vacuum conditions, however, a fundamental
understanding of electrodeposition from
solution under high voltages is largely lacking.
Specifically, the influence of the solid-liquid Mounting a copper sample in the ESRF’s ID32 beamline.
interface and the applied electrode potential
J Golks
on the elementary surface processes is unclear. grow rougher at higher voltages and this is
Industrial plating processes have long used also what current theory predicts.”
small amounts of chloride in the acidic plating The anomalous behaviour of copper, the
bath to optimise growth behaviour and team concludes, is due to the arrangement of
deposition properties, explains ESRF user Olaf the atomic layer of chloride ions present on
Magnussen of Kiel University in Germany, the surface. Copper atoms moving across the
but until now it has been a mystery how this surface have to push through this layer and
simple inorganic species influences copper they become more mobile at higher voltages,
growth at the atomic scale. where the chloride is more weakly bound.
“We suspect that it is due to the electrostatic
Growing on chloride energy resulting from the interaction of the
Last year, in collaboration with ESRF staff, charge chloride absorbates with the strong Graphical representation of the growth
Magnussen and co-workers used surface X-ray electric field at the electrochemical interface,” process, during which deposited copper
diffraction at ID32 to carry out in operando says Magnussen. atoms move across the surface through a layer
studies of electrochemical copper growth in The novel concept of a voltage dependent of chloride.
a chloride-containing acidic solution. They surface mobility mediated by absorbed
found that minute quantities of chloride in the adlayers, he explains, provides a simple implications, according to the team. For
electrolyte solution have a decisive influence conceptual framework that allows instance, knowledge about whether the
on the structure of the growing films, which microscopic physical growth theories to electrode surface transport is normal or
in turn determines their electrical behaviour be extended to liquid phase deposition anomalous allows manufacturers to assess
(Phys. Rev. Lett. 108 256101). processes. The results contribute to a better the roughness of the deposit that may be
The experiments were performed using an fundamental understanding of growth expected at certain deposition potentials.
electrochemical three-electrode cell in which and surface transport in electrochemical “Choride is the simplest additive and real
contact with the electrode was established environments, and have significant practical industrial additives are more complicated,”
by a droplet of electrolyte. The high-speed says Magnussen. “Our work is still at the
surface scattering setup at ID32 allowed very fundamental level but it provides insight
the researchers to study copper growth at into how these additives work.” The ESRF
a rate of several monolayers per second,
shedding light on how atoms attach to the
“Our results is important, he adds, because it allows
researchers to study deposition at high rates
growing surface during electrodeposition. By
increasing the voltage the team found that have significant in operando, approaching conditions in
industry. “We want to extend synchrotron
the copper films grew smoother, implying
reduced defects and cavities in the deposits. practical techniques to get the full 3D structures of the
additives. Such techniques may also be useful
implications.”
“This actually was a big surprise,” explains in other areas such as fuel cells.”
Magnussen. “Other metals, for example gold, Matthew Chalmers
POWERED BY
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C Argoud
has spanned academia, industry represented the research council
and, in her current role, science on the board of the SNBL. The
policy. But one thing has SNBL has become a “home
remained constant: an interest laboratory” to Norwegian
in advanced materials. Aase’s synchrotron users where they can
PhD research in the early 1990s build relationships and equipment
concerned the properties of with local contacts, she explains.
ceramics such as aluminium “It’s a very strategic way to carry
nitride, specifically how its out research.”
thermal conductivity changes Some of Norway’s 140 or so
due to different production synchrotron users travel to the
processes. It was a natural step nearby MAX-lab in Sweden to
from her undergraduate degree carry out experiments in areas
in inorganic chemistry, she such as surface science. Will more
explains. “I was interested in the use be made of the new MAX-IV
links between the fundamental machine when it comes online?
properties of materials and how “Of course MAX-IV will cover
they are synthesised.” a larger part of synchrotron
On finishing her PhD, Aase science, and it is much closer
became a research scientist for than Grenoble, but Norway’s
Elkem – one of Norway’s largest commitment to the ESRF and
companies – where she focused the SNBL will continue,” says
on silicon- and aluminium-based
materials for lining the furnaces
Aase Marie Hundere in brief Aase. “It’s also very important
for Norwegian researchers to
used in large-scale metal Born: Norway, 1966. Senior advisor at the Research collaborate in an international
production. Metal production Council of Norway. environment, because we find
is one of Norway’s biggest Education: PhD materials that researchers who do so are
industries, along with energy science, Norwegian University of Family: Married with two more successful.”
and fisheries, and materials Science and Technology, 1994. children.
science is one of the largest Materials for industry
areas of scientific research in the Career: 1995–2003 Research Interests: Skiing, running and Last year, Norway’s research
country. scientist, Elkem; 2003–present walking the dog. council launched a new
“Going from the laboratory 10-year-long programme in
where you focus very much on nanotechnology and advanced
the details into more applied materials, NANO2021, which is
settings was very interesting,” Aase’s main responsibility for
she recalls. “I came from a family
of engineers and I wanted to
“Long-term challenges the coming years. One of its
goals is to stimulate Norwegian
go from the academic world to
something more practical and in industry can be very industry to apply the knowledge
that is built up in universities in
relevant.”
Seeking a broader overview stimulating for academia.” new areas, which is something
Aase is looking forward to
of research, in 2003 Aase took focusing on. “Also, given the
up a position as an advisor to new infrastructure provided
the Research Council of Norway, by the ESRF upgrade, I want to
which had just launched a new Representing Norway via the “Nordsync” consortium, understand how we can take
programme in nanotechnology Since 2005 Aase has represented which contributes 4% of the full advantage to make industry
and advanced materials. “Also, Norway at the ESRF and total ESRF budget and also more aware.”
there was a lot of travel in my is the current chair of the includes Finland, Denmark and At the end of the day, she says,
previous job and I wanted to start ESRF’s Administrative and Sweden. The country also has research funding needs public
a family,” she says. “Norway Finance Committee (AFC). a 2.5% stake in the European acceptance. “It’s a balance with
is very good at supporting you The task of the AFC is to make Spallation Source currently under blue sky research, but we also
while you have small children, recommendations to the ESRF construction in Sweden and a know that long-term challenges
but you still are compared Council based on budgetary similar stake at CERN. in industry can be very stimulating
internationally so I think it’s tough and economic considerations. The ESRF’s Swiss-Norwegian for academia.”
to be a woman in science.” Norway participates at the ESRF beamline (SNBL) is funded Matthew Chalmers
“This is an important
the CEA established an eight- provides a unique tool to
year long ¤460 m public–private characterise large-area silicon
programme called Institut de wafers. “Thanks to the high
Recherche Technologique (IRT)
“Nanoelec” to develop 3D
project for us” brilliance provided by the ESRF,
X-ray based techniques allow
assembly for increasingly complex us to observe large embedded
chips, and silicon nanophotonics as possible for companies to Wolny of the CEA and Director features while maintaining state-
for faster communication within access beam time at large of IRT Nanoelec. “IRT will help of-the-art resolution.”
and between chips. IRT Nanoelec facilities. Based on experiments the ESRF to open its capabilities “This is an important project
is one of seven major programmes carried out by industrial partners to industry thanks to specific for us,” says Ed Mitchell of the
established in France to leverage and the ESRF, the programme investments and networking ESRF’s Business Development
high-tech industry through public will define preparation and among the 17 IRT partners.” Office. “Once we gain experience
and private sector research. The characterisation processes for and expertise in working with
ESRF together with the Institut specific materials and devices. Industry on board these firms we can apply it to
Laue-Langevin (ILL) and the “The ESRF allows characterisation IRT Nanoelec partner Soitec uses companies across Europe, thus
CEA are to share ¤6.5 m to help of microelectronic devices but X-ray diffraction and reflectivity extending the benefits to all ESRF
industry meet these goals. it’s still difficult for enterprises techniques to characterise funding states.”
The aim is to make it as simple to access the ESRF,” says Michel materials, but until now this has Matthew Chalmers
HOME RUN
Catch us at
ICXOM22,
booth number 28.
Also look out for our
industrial presentation.
beamline
instrumentation
In the corridors
X-ray scanners such as drugs or explosives.
External perception No Windows 8
US airports will use alternative
reveal too much full-body scanners based on The ESRF’s slogan Having weighed up the pros
The US millimetre-wave technology “A light for science” and cons of Microsoft’s latest
US TRANSPORTATION SECURITY ADMINISTRATION
Transportation with software that produces a is clear and operating system, Windows
Security generic outline of the body and understandable 8, the ESRF has decided to
Administration highlights suspicious material to those outside stick with Windows 7 until
has removed all using coloured boxes. the ESRF, but does not convey the release of Windows 8.1
“backscatter” enough about the ESRF’s mission. later this year. An ESRF team
X-ray scanners Netherlands at ESRF These are two conclusions to concluded that Windows 8 has
no added value for the ESRF
from its have emerged from a survey
airports More than of scientists and policy makers at present and would require
following 25 Dutch undertaken by communication both an upgrade of ESRF
criticism that companies specialist Marzena Lapka of infrastructure and extensive
the technique were CERN. The focus of the study was user training. Consequently, PCs
reveals too represented CERN, but Lapka also contacted running under Windows 8 are
much unnecessary detail to at the ESRF on 26–27 June as 13,720 ESRF staff and users (2.5% not supported and will not be
machine operators. Instead part of an industrial fair to bring of who responded). Her results connected to the ESRF network.
of relying on the absorption together high-tech industry suggest that surprisingly few CERN
and transmission of X-rays, and R&D partners from the scientists are familiar with the
backscatter screening maps GIANT Grenoble campus. The ESRF. “What’s interesting, though,
the patterns of X-rays scattered ESRF is one of eight members of is that once respondents who were
off elements within an object. GIANT, which groups more than unfamiliar with the ESRF visited the
Since elements with low atomic 10,000 industrial and academic ESRF website, they decided that it
numbers scatter X-ray photons researchers on one site and was an important organization,”
more strongly, the systems are generates some 5000 publications says Lapka. “So it might be a
good at imaging organic material and 500 patents every year. communication issue.”
Features
• Available
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