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A L I GH T FOR S CIE N C E

Number 77 December 2017

Extremely
Brilliant
Source

Green light for new beamlines


Algae turn fat to fuel
Cryo-EM arrives
X-Ray Spectroscopy

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Contents
T h e E u r o p e a n Sy n c h r o t r o n
ESRFnews Number 77 December 2017

EDITORIAL
5 A new record

IN BRIEF
6 ERC grant awarded
6 P&G sign collaboration agreement
6 Giant LEAPS for integration
6 Market call for detector tech
7 Tattoos affect lymph nodes
Tattoo nanoparticles reach lymph nodes, p7.
7 Earth’s inner carbon cycle probed
7 2018 User Meeting
7 SESAME staff exchanges begin

ESRF–EBS NEWS
8 Mock cell built
8 Girder assembly begins
9 Insight: the HMBA lattice

10 USER CORNER

FEATURES
12 The green way to turn fat to fuel
13 Cryo-EM platform launched
Cryo-electron microscopy comes to the ESRF, p13.
FOCUS ON: EXTREMELY BRILLIANT SOURCE
15 Extremely brilliant progress

BM23
ID24 16 ESRF–EBS layout unveiled
19 EBSL1: the ideal match
ID23 2 21 EBSL2: tilting the scales
EBSL3 (BM18) ID22 23
23 EBSL3: bigger and better
25 EBSL8: the serial approach
ID19 22
PORTRAIT
ID21 27 Titia Sixma on why she still comes to the ESRF
21

BM20
ID20 INDUSTRY
20

29 OCAS targets steel with dark-field microscopy


Green light for new EBS beamlines, p16.
MOVERS AND SHAKERS
29 Edith Heard; James Naismith; Paul Shearing and
Donal Finegan; Michael Hahn

A LIGHT FOR SCIENCE


BEAUTY OF SCIENCE
30 Finding a common ancestor
Number 77 December 2017

Extremely IN THE CORRIDORS


Brilliant
Source 30 First XFEL users; X-ray telescope launched; fastest
X-ray flash; X-rays help restore wind instruments

On the cover: Green light for new beamlines


Algae turn fat to fuel
Cryo-EM arrives
The new ESRF-EBS layout

December 2017 ESRFnews


O
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For up to o
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Editorial

A new record
Editor In September, a paper was published in the journal Science reporting a potentially
Jon Cartwright
Tel +44 (0)117 2303080 groundbreaking step towards sustainable sources of hydrocarbon fuels. Using ESRF data, the
E-mail jon.a.cartwright@icloud.com authors managed to uncover how a recently discovered enzyme has the seemingly unique
Editorial committee ability to convert fats into hydrocarbons, in the presence of sunlight. The results suggest that
Gary Admans the enzymes could be exploited to generate diesel, petrol or even jet fuel (p12).
Nick Brookes
Delphine Chenevier
Andy Fitch This Science paper was special in another way: it was one of those that inched the ESRF
Axel Kaprolat
past a milestone of 30,000 publications since our facility first opened its doors in 1994.
Michael Krisch
Gordon Leonard Among those publications are many that have since become regarded as breakthroughs
Joanne McCarthy – the discovery of the structure of the ribosome, for instance, won its authors Ada
Edward Mitchell
Pantaleo Raimondi Yonath and Venkatraman Ramakrishnan, both long-term ESRF users, a share of the 2009
Harald Reichert Nobel Prize in Chemistry. The publications reflect the diversity and vibrancy of the ESRF
Francesco Sette
Jean Susini
user community, too. Researchers from over the world, from all cultures and disciplines,
come to the ESRF to push back the frontiers of science, to unlock the secrets of materials
Subscription
Chantal Argoud
and to better understand living organisms. For over two decades this research has
For subscriptions to the digital version of enriched scientific culture, as well as furthering society by boosting the economies and
ESRFnews (print subscriptions are no competitiveness of ESRF member states and beyond.
longer possible), visit http://www.esrf.eu/
UsersAndScience/Publications/Newsletter
Such progress has been possible through a continuous
ESRFnews is produced for the ESRF by
IOP Publishing and dynamic research and development programme, “Many publications
Temple Circus which focuses on constantly improving the
Temple Way
Bristol BS1 6HG, UK
instrumentation and technology of the X-ray source have become
Tel +44 (0)117 929 7481
www.iop.org
and beamlines. Together with the constant support of regarded as
its international partners, the ESRF has become one of
Managing editor the leaders in the field of synchrotron and accelerator breakthroughs”
Susan Curtis physics and technology.
Art director
Andrew Giaquinto
Production One aspect of the ESRF R&D programme is the new cryo-electron microscopy (cryo-EM)
Alison Gardiner
Technical illustrator
platform, inaugurated in November this year. A collaborative initiative among the ESRF
Alison Tovey and its partners on the EPN science campus – the European Molecular Biology Laboratory,
Display-advertisement manager
Edward Jost
the Institut de Biologie Structurale and the Institut Laue-Langevin – this new state-of-the-
Advertisement production art cryo-EM facility will provide opportunities to the international community of structural
Mark Trimnell biologists. It will complement the ESRF macromolecular-crystallography beamlines and the
Marketing and circulation
Angela Gage other EPN campus structural biology facilities, and help us piece together the atomic details
of the molecular machines of life (p13).
ISSN 1011-9310

©2017 ESRF More broadly, the experimental programme of the ESRF’s Extremely Brilliant Source (EBS)
upgrade is entering a new operational phase, with the launching of the construction of four
new flagship EBSL beamlines (pp19–25) – identified by the ESRF Science Advisory Committee
and validated by the ESRF Council last June – complemented by important progress in the
detector-development and data-infrastructure programmes. The four new EBSL beamlines,
combined with a programme of refurbishment (pp16–17), will underpin research addressing
the major challenges facing our society today, including defining the next generation of
sustainable materials, developing new drugs, unravelling the complex mechanisms of living
organisms, unlocking the secrets of our planet and environment, and reconstructing historical
artefacts and fossils in 3D.

While all this is going on, the ESRF maintains its close involvement in European activities. It
plays an important role in the ATTRACT programme for shared progress in detectors and
imaging, in the SESAME programme for the Middle East’s light source, through collaboration
with Russia on the development of its fourth-generation synchrotron source, and with the new
LEAPS (League of Electron Accelerator-based Photon Sources) initiative aiming to strengthen
European leadership in X-ray science at synchrotron and XFEL facilities (pp6–7). The history
of the ESRF has shown that international scientific collaboration can create tremendous
breakthroughs and build bridges between nations: thanks to the constant support of our
community, we are looking forward to setting new records.

Francesco Sette, ESRF director-general

December 2017 ESRFnews


O
5
In brief
Giant LEAPS for
integration
Last month the ESRF, together
with 15 other facilities in
Europe, launched the League
of European Accelerator-based
Photon Sources (LEAPS), to offer
a “common vision” of using
scientific excellence to solve global
challenges, and boost European
competitiveness and integration.
One of the main aspects of
LEAPS is an agreed roadmap

MOLYNEUX
for the development of next-
generation light sources and
instrumentation, and tackling Kvashnina installs crystal analysers on ID26.
big data. Serving a combined
24,000-strong user community,
the initiative also aims to maximise
the strengths of individual
Kvashnina bags ERC grant
facilities through coordinated Kristina Kvashnina – a long- training, Kvashnina defended a prepared samples of lanthanide
specialisation, and to expand time ESRF user, a former ESRF PhD on soft X-ray spectroscopy and actinide nanomaterials for
industry services. Meanwhile, it will staff member and current of lanthanide and actinide Kvashnina’s research.
capture and map socioeconomic collaborating research group systems at Uppsala University in To study the samples,
impact, and improve training and beamline scientist – has Sweden, based on data taken Kvashnina has needed the
outreach programmes. “LEAPS received a prestigious starting at the Advanced Light Source ROBL beamline’s rare ability
will use the power of its combined grant from the European at Lawrence Berkeley National to safely handle radioactive
voice to ensure that member light- Research Council (ERC) to Laboratory in California, US. materials, its X-ray emission
source facilities continue to be pursue her work on actinide Afterwards, she moved to the spectrometer, and its
world-leading, to act as a powerful and lanthanide nanomaterials. ESRF, where she has studied the functioning with low-energy
tool for the development and The grant of €1.5 million is the same systems using the hard X-rays in the region of 3–7 keV,
integration of skills with a view maximum that can be awarded, X-rays at beamlines such as to reach the appropriate
to address 21st-century global and is designed to help early- BM20, the German Rossendorf actinide and lanthanide
challenges, and to consolidate career researchers in any (ROBL) beamline. Helmholtz- absorption edges.
Europe’s leadership in the field,” scientific field who show the Zentrum Dresden-Rossendorf “The ESRF is the only place in
reads the initiative’s mission potential for “excellence”. are the backers of the ROBL the world where we can carry
statement. A theoretical physicist by beamline, and have also out this research,” she says.

ATTRACTing tech P&G signs up with the ESRF and ILL


to the market
Large research facilities are home Procter and Gamble (P&G)
to swathes of cutting-edge signed a “master collaboration
technology, most of which is agreement” with the ESRF
never seen outside of the scientific and the Institut Laue-Langevin
community. A new pan-EU (ILL) in September, making the
initiative, ATTRACT, hopes to international consumer-goods
change that by helping to bring the company a strategic research
detector and imaging technology partner with the X-ray and
to market, to boost sectors such neutron facilities. The agreement
as information technology and establishes basic terms that will
sustainable materials. streamline future collaborations.
ATTRACT proposes a new P&G scientists first came
S CLAISSE

co-innovation paradigm among to the ESRF in 2004, when


industry, business, investors, they used its beamlines to
innovation specialists and European understand and optimise the Representatives from P&G, the ESRF and the ILL after signing the
research infrastructures. The ESRF, microstructure of Clairol Perfect agreement.
the European Molecular Biology 10, a hair colourant that worked
Laboratory, the Institut Laue- in a record-breaking 10 minutes. fundamental microstructure boundaries, to deliver even more
Langevin and CERN are among the Since then, the scientists have of our materials and products, breakthrough benefits.”
initiative’s nine partners, which will used the ESRF to investigate which helps the entire Francesco Sette, the ESRF
arrange for project proposals to be everything from fabric detergent development process, from director-general, applauded
reviewed by an independent panel and conditioner, to skin products, manufacturing to performance- the agreement. “The long-
in order to receive €100k each in nappies, polymer films and optimisation,” said Eric Robles, term partnership with P&G, a
seed funding. The first launch for toothpaste. a P&G research fellow. “Looking company that strongly invests in
open calls is in spring next year with “We have been working with forward, we will co-develop research for its development, is a
a final assessment in 2020. Details the ESRF and ILL for more than new capabilities that allow great example of commitment to
at attract-eu.org. a decade now to reveal the us to continue to push the innovation,” he said.

6 December 2017 O ESRFnews


In brief

Tattoo nanoparticle danger


Think before you ink.

C ARGOUD
User Meeting: 5–7 February.

ESRF gears up for


User meeting
The 2018 User Meeting is set to
take place from 5–7 February, and
is open to all ESRF users. According
to the User Organisation
Committee (UOC), the meeting
will include a “rich and diverse”
programme of events, including
keynote lectures, the Young
Scientist Award, a poster session
and director’s report, as well as
a range of scientific tutorials.
Microsymposia will be held on
the subjects of high-pressure
Nanoparticles present in Hiram Castillo-Michel, one of the author and ESRF postdoc (now science at the ESRF, metallurgy
tattoo ink can migrate to the authors of the work. “No one visiting scientist) Bernhard and materials processing, and the
lymph nodes, a critical part of checks the chemical composition Hesse, however, the discovery use of synchrotrons to understand
the body’s immune system, of the colours, but our study of tattoo nanoparticles in neurological diseases. For more
according to research performed shows that maybe they should.” lymph nodes is concerning information, see the UOC story
at the ESRF. The nanoparticles Previously, the chemical because particle behaviour on p10 or visit www.esrf.eu/
include pigments and titanium dangers of tattoos have been on that scale in the body is UM2018 .
dioxide, as well as chromium and studied only outside of the poorly understood. “That is
nickel, which are toxic. body, although it has long been the problem: we don’t know
“When someone wants to noted that the lymph nodes of how nanoparticles react,” he SESAME staff
get a tattoo, they are often tattooed people are sometimes says. The study was performed exchanges begin
very careful in choosing a enlarged and take on the using X-ray fluorescence
parlour where they use sterile tattoo’s colour, implying that measurements at ESRF The ESRF welcomed its first
needles that haven’t been used at least micro-sized particles beamlines ID21 and ID16B (Sci. scientist from the Synchrotron-
previously,” says ESRF scientist are present. According to study Rep. 7 11395). Light for Experimental Science
and Applications In the Middle
East (SESAME) in July, as part
Carbonates explain carbon’s descent of an EU project coordinated
by the ESRF, known as OPEN
Most people are familiar with SESAME, to help establish the
the carbon cycle above ground, new Jordan-based light source.
but tectonic movements Mahmoud Abdellatief is one
actually circulate a lot of the of 16 SESAME scientists who
carbon below ground. In fact, have either exchanged or have
recent estimates place some scheduled exchanges with
90% of the Earth’s carbon in the European facilities as part of the
mantle and core – though quite project. Ultimately, 65 staff will
how it is transported there has be exchanged.
been a mystery. A beamline scientist,
Valerio Cerantola of Bayreuth Abdellatief was at the ESRF
University in Germany (now for three weeks, during
a postdoc at the ESRF) and which he completed technical
others have shed some light specifications for a diffractometer
on the matter, by performing and decided what set-ups and
C ARGOUD

experiments on iron carbonate techniques his experimental


at pressures over 100 GPa and station will enable. He was
temperatures over 2500 K, Cerantola exploits the high-pressure lab at the ID18 beamline. mentored by Andy Fitch,
using the ESRF beamlines beamline scientist at ID22, among
ID27, ID18 and ID09A (now extreme conditions is poorly containing CO 4 tetrahedra are other ESRF staff. “This experience
ID15B). The carbonates are understood. preserved by reduction and will help me to figure out the
believed to exist in the lower The researchers found oxidation reactions, suggesting best design for our beamline
mantle because they are found that, at higher pressures and that these could be the lower so that we can exploit it to the
in diamonds originating in that temperatures, different phases mantle’s carbon-carriers (Nat. maximum with the scientists in
region, but their behaviour at of iron-bearing carbonates Commun. 8 15960). the community,” Abdellatief said.

December 2017 ESRFnews


O
7
ESRF–EBS news

Success for
mock-up cell
Engineers at the ESRF have and all the vacuum chambers
successfully built an entire were connected together and
EBS cell, consisting of girders, inserted in the magnets, and
magnets, vacuum chambers and pumped. “No major issues were
other components. The mock-up discovered,” says Eybert.
went entirely to plan, and paves
the way for the assembly of the
EBS proper (see story, right).
The EBS storage ring will consist
of thousands of components, all
“Many
of which have been designed in components have
three dimensions with computer
software. Experience from less than half
previous projects, however, has
demonstrated a possibility of a millimetre of
conflicts between components
during assembly due to design or
room for error.”
machining faults, especially when
space constraints are very high.
In the EBS, many components The mock-up was the first
have been designed with less time that engineers from the
than half a millimetre of room different groups and divisions –
for error. The Machine Advisory alignment and geodesy, technical
Committee recommended the infrastructure, vacuum, insertion
building of a mock-up cell at devices, power and so on – have
a meeting last year, and work worked together in the same place
began in February this year for the new EBS machine. “We’ve
in the ESRF’s Chartreuse Hall. had many meetings, but never
“The mock-up is the best tool to before have we all been working
anticipate and to tackle technical together, to do the assembly,”
issues before the busy assembly says Eybert. In fact, adds Eybert,
phase,” says Laurent Eybert, one working together allowed the
of the managers of the mock-up. team to get to know one another,
“It is also a demonstrator and a and to know precisely who was
useful training tool for all people responsible for what.
involved in the project.” The engineers baked the
The mock-up space was vacuum chambers at temperatures
divided into two zones: one of up to 150 °C for 48 hours to
for the assembly of vacuum achieve a level of vacuum better
vessels on dedicated tables, than 1 × 10 –10 mbar, and checked
and the other for four girders, that the main components still
anchored to the concrete remained within the alignment
floor in the alignment they will tolerances. In the next step, input
ultimately have in the tunnel. facilities such as piping and cabling
The engineers prepared a will be installed to fully validate
detailed procedure for assembly, their design, before issuing calls
outlining the necessary control for tender.
points, timescales, labour, tools
and layout configuration. By Right: ESRF engineers and
12 September, all the magnets technicians make adjustments to
were installed and aligned, the mock-up cell.

For more upgrade news,


check out the EBS blog:
http://ebs.esrf.fr

8 December 2017 O ESRFnews


ESRF–EBS news

Girder assembly begins


Assembly of the EBS has begun section and one arc. One arc is complete, real arc,” says Jean-
in earnest, as ESRF engineers composed of four girders, and Claude Biasci, the manager of
and technicians prepare the these have to support all the the assembly. “For us technical
machine’s 128 girders with all the components for maintaining people, it’s the opportunity to
components they need to form the electron beam – principally validate all of the components
the new storage ring. Working in magnets, magnet supports and and the assembly procedure,
a separate, dedicated building, vacuum chambers. There are including girder connections and
ESRF01, the engineers began last many steps to the assembly, bake-out.”
month and hope to complete up including the installation of The exact rate of girder
to four girders per week, so that pre-positioning templates, assembly will depend on the
the girders are ready to be moved alignment and checking of stock of components and the
into the location of the existing alignment. It takes engineers availability of labour. Once
storage ring by the shutdown at and technicians three weeks to assembled, the girders will be
the end of 2018. assemble the four girders in one ready to be moved into the ESRF
Like that of the existing ESRF, arc, although they are speeding tunnel, where they will only need
the EBS storage ring is made up the process by running to be aligned and have their
up of 32 cells, each of which three assembly lines in parallel. vacuum chambers connected
is composed of one straight “This assembly represents a together.

Insight: The hybrid multi-bend achromat lattice

One cell of the EBS’s HMBA lattice, supported on its four girders. There are four dipoles (blue) and three
dipole-quadrupoles (pink), making seven bending magnets in total. Also shown are quadrupoles (red) and
sextupoles (green).

What is the lattice? closely packed, and the resulting Will all this actually fit in
The hybrid multi-bend achromat synchrotron X-rays are brighter and the current ESRF tunnel?
(HMBA) lattice is the composition more coherent – in other words, Remarkably, yes. With roughly
of magnets that will guide and they approach the properties of a twice as many magnets in the
focus the EBS’s electron beam. laser beam. The HMBA will boost same space, each has had to be
Currently, the ESRF has a “double coherence by some two orders engineered to be more
bend achromat lattice”, so called of magnitude. Such properties compact and generate magnetic
because it relies on two bending are the driving force of the EBS fields up to three times stronger
magnets (dipoles) per cell, and upgrade, opening up new fields than existing models. The
because electrons of different of investigation in fundamental vacuum chambers have had to
energies are bent and focused in research, and allowing far better be redesigned for limited space
the same way – “achromatically” industry diagnostics to promote in and around the magnets, too,
– resulting in very collimated innovation. while the mechanical tolerances
and stable beams. There are also of some components have shrunk
achromat lattices based on three How will the HMBA make to just 100th of a millimetre. It
or four bending magnets: the these gains? is a complex and revolutionary
HMBA will have seven. Pioneered Having seven bending magnets design that has inspired the
by the ESRF, the HMBA will be key per cell gives far more control composition of other big light
to the EBS’s status as a “fourth- over the electron beam, but that sources around the world,
generation” synchrotron source, is just the start. Many magnets and won the ESRF’s Pantaleo
reducing horizontal emittance by are innovative: some dipoles are Raimondi the prestigious Gersch
a factor of 30 compared with the made of permanent magnets Budker Prize from the European
existing machine. (see ESRFnews July 2017, p9), for Physical Society Accelerator
example, while some magnets Group earlier this year. It “shows
Why is that so important? simultaneously bend and focus Raimondi’s ability to foster new
Emittance describes how tightly the beam. Compared with the ideas, his deep understanding
the electrons are confined in current lattice, there will also be of accelerator physics and [his]
the beam. If the emittance is 25 further magnets per cell to mastering of technological
smaller, the electrons are more enact subtle corrections. aspects,” the jury said.

December 2017 ESRFnews


O
9
User corner
News from the User Office News from the User Organisation Committee
In September, for the The next deadline (and last one The User Organisation (which we encourage you to
penultimate deadline before before the EBS shutdown) for Committee (UOC) met in circulate), can be found at
the shutdown for the ESRF’s submission of standard proposals September at the ESRF to finalise esrf.eu/UM2018. In particular,
Extremely Brilliant Source (EBS) is 1 March 2018, for beam time the organisation of the User we invite users to send
upgrade at the end of 2018, an between August and December Meeting. The 28th edition of the nominations for the Young
all-time record of more than 2018. There is no Long Term event will take place on 5, 6 and Scientist Award. This year,
1300 proposals was submitted, Project submission deadline in 7 February 2018 at the ESRF and besides receiving €1500, the
requesting a total of almost January 2018. all users are invited to attend. winner will also feature in a
18,000 shifts of beam time. Proposers are reminded by the Along with management short promotional video about
Despite this high submission, Beam Time Allocation Panels of and the User Office we have his or her research, produced by
faster and more efficient the importance of submitting prepared a diverse and rich a professional company.
experiments should still ensure experiment reports for all beam- programme including keynote We would like to remind
an acceptance rate of around time allocations previously used, lectures, the Young Scientist all users that the UOC has
40%. These proposals were and of citing these in the relevant Award, a poster session, the regular meetings over the
reviewed during the Beam Time section of the proposal form. Directors’ report and user- year, the agenda and minutes
Allocation Panel meetings on Resubmitted proposals should dedicated sessions with 12 of which are available upon
26 and 27 October, when 126 be clearly marked as such, and it tutorials on a range of different request. Users are welcome
external scientists met at the is mandatory to clearly indicate scientific topics and three to contact us at any time via
ESRF to evaluate them and what aspects of the proposal microsymposia. During the e-mail. Representatives of
provide recommendations for have been modified or improved. plenary session, an update on each user scientific community
beam-time allocation. We are Continuation proposals must have the EBS upgrade and the plan and their e-mail addresses
very grateful to our committee an experiment report submitted of future related activities will can be found at www.esrf.eu/
members for all their hard work for the original proposal. be given. Further information UsersAndScience/users_org.
in reviewing and discussing this Joanne McCarthy, Head of the on the 2018 User Meeting, and Paola Coan, chair of the User
very high number of proposals. User Office a download of the event poster Organisation Committee

News from the beamlines


O The ESRF has installed and angular dispersive diffraction. the fields of biology and cultural
commissioned a Titan Krios cryo In the Materials Chemistry heritage. The microscope will
electron microscope (cryo-EM) station (ID15A-EH3) the DRIFTS still be operational but using the
equipped with a GATAN K2 spectrometer has been installed internal Globar source, and the
detector for studies in Structural since the beginning of the hutch will be fully modified as
Biology (see p13). This new summer, allowing combined part of the refurbishment of the
facility, ESRF “beamline” CM01, XRD-DRIFTS measurements to ID21 X-ray platform. The X-ray
became operational in mid- be made. branches will be temporarily
November 2017 and has been O Additional laser PSS systems closed from December 2017 to
open for proposals since 28 have been installed on both March 2018 for the first parts of
September. Applications for ID19 and ID31 to allow shock as this refurbishment.
microscope access are made as well as additive manufacturing O The Structural Biology
Rolling Access Proposals and experiments to be performed. beamlines FIP-BM30A and
reviewed by the Beam Time O In addition to bulk XAFS ID30B hosted practical sessions
Allocation Panel C10 (Structural spectroscopy, the ROBL CRG as part of the MXIS 2017 training
Biology beamlines). Initially, beamline BM20 has now a course. MXIS is a practical course
only projects that have been Johann-type spectrometer with dedicated to in situ protein
previously evaluated using five analyser crystals available, crystallography, with a special
cryo-EM and for which suitable which can be used for high- emphasis on ligand screening.
proof of the sample quality is resolution XANES, XES and RIXS. The workshop was organised
available will be considered. This Anders Bank Blichfeld of the Furthermore, surface diffraction in two parts, each one lasting
proof has to be included in the NTNU using the new in situ (CTR, RAXR), powder diffraction for three days. Part 1 took place
application for access. heating setup on BM01. and single-crystal diffraction 8–10 November at the CNRS
O On the SNBL CRG beamline are currently being developed campus in Montpellier, with full
BM01, just prior to the summer working with piezoelectric thin and available to expert users lectures and practicals on the
shutdown, a group of users from films and hopes that the new in upon request. Note, however, topics of plate pre-coating for
the Department of Materials situ characterisation tool will help that ROBL will be closed from “dry” co-crystallisation and in
Science and Engineering at the to understand the nucleation the summer shutdown 2018 situ screening on a lab source.
Norwegian University of Science and growth mechanisms, onwards for the building of a Part 2 took place on the EPN
and Technology (NTNU) had the and improve the tuning and new radiochemical hutch. After Science Campus in Grenoble,
first beamtime using a new in designing of processing protocols the EBS upgrade, all techniques 29 November – 1 December,
situ heating setup for thin films to obtain better materials. will be available in an alpha- with full lectures at the Institut
(see photo, right). The setup is O On ID15A the new station lab environment dedicated to de Biologie Structurale and
designed to mimic the processing for Materials Engineering actinide research. practical sessions at the ESRF on
parameters typically used in thin- (ID15A-EH2) is ready for users. O The infrared station at ID21 the topics of in situ diffraction for
film production by the chemical Techniques available are ultra- stopped operation at the end crystal screening and structure
solution deposition method. fast imaging/tomography, of September after 13 years of resolution, and in situ data
The group has a long history of energy dispersive diffraction and successful activities, mainly in processing.

10 December 2017 O ESRFnews


Advertising feature

Positioning solution for analytical-methods: mechanical


system approaches limit of technical feasibility
At the X-ray light source PETRA III at the
DESY research centre (German Electron
Synchrotron) in Hamburg, Germany, the
Helmholtz-Zentrum Geesthacht Centre
for Materials and Coastal Research (HZG)
operates the Imaging Beamline P05,
which includes two experimental hutches,
one for nanotomography and one for
microtomography. In the nanotomography
hutch, X-ray optics for three-dimensional
micrographs with resolutions around
100 nm are used. The set-up also includes
microscopy optics for visible light, used
for further magnification of the X-ray
micrographs and their transfer to a camera.
With the aim to carry out as many different
experiments as possible, the HZG provides
two different X-ray optics configurations:
an imaging set-up, in which the sample
is positioned in front of the objective
optics, and a cone-beam set-up, in which
the sample is placed in the diverging
beam behind the optics. In both cases,
high mechanical stability and precision
positioning are essential to obtain Mounted on the combined tilt and Z stage (consisting of three differentially controlled lifting elements) is an air-bearing supported
rotation stage. It rotates at a velocity of up to 36$/s and works with flatness deviations of less than 100 nm at a resolution of 0.5 μrad
micrographs of high quality. (Image: PI / HZG)

However, thanks to the close co-operation


of the clients with the engineers and while maintaining a stable position as soon works with flatness deviations of less
developers from PI (Physik Instrumente), as the air flow is switched off. than 100 nm at a resolution of 0.5 μrad.
this complex task could be solved in a The air bearing does not produce any
practice-oriented manner. Complex sequences during sample
friction, which over time would lead to a
positioning
A particular challenge was how to deterioration of these values.
The basis of sample positioning is a
configure the control, which was based horizontal positioning unit that moves the Parallel kinematics for the sample holder
on an industrial controller. The challenge sample stage into the beam. It has a travel and the optics
consisted in controlling almost 50 axes range of 20 mm, can be subjected to a load The actual sample holder is located in
independently of one another while of 300 kg and works with a repeatability the aperture of the rotation stage on the
ensuring collision protection. The entire of 30 nm. moving platform of a six-axis parallel
system was finally integrated into the kinematic system. The samples are
TANGO interface customary for beamlines. This displacement unit is equipped with
positioned with six degrees of freedom.
three lifting elements that perform the
Essential features are the freely selectable
The base: granite platform supported by air height adjustment, tilt correction and
pivot point of the parallel-kinematic
bearings orthogonal alignment, relative to the
system and its high stiffness. A six-axis
To minimise the effect of vibrations and beam. It is based on three identical,
parallel-kinematic system of this type is
securely fasten the individual components symmetrically arranged and position-
also used for the positioning of the optics.
and stabilise them, relative to one another, controlled stepper motors, combined with
In nanotomography, which allows three-
a granite base 6.8 m in length forms the worm gears and spindle drives. Mounted
dimensional micrographs with resolutions
basis of the instrument. Another four on this Z stage is an air-bearing supported
below 100 nm, this machine is used to
moving granite platforms driven by linear rotation stage. In developing this stage,
align compound refractive lenses (CRL) in
motors are arranged on this base on the designers had to push the limits of
the beam with high precision.
air bearings. This makes it possible to technical feasibility: what was required
position all components with high speed was a really “pure” rotary motion of the
and precision: the sample stage, the X-ray sample with minimal wobble, radial runout
optics and the detector. The substructure or eccentricity. Only in this case can sharp
itself, which weighs several tonnes, is also pictures over 360$ be made that all refer
mounted on air bearings. This allows the to the same volume element and can all
entire assembly to be moved out of the be clearly assigned when reconstructing Contact
X-ray beam with minimal effort when the the picture. This is why the rotation stage, Web www.pi.ws
second experimental station is to be used, which rotates at a velocity of 36 $/s, Email d.knauer@pi.de
Feature

Algae turn fat into fuel


Fatty acids are chemically similar to found that, under blue light, the bacteria
The ESRF snapshots a hydrocarbons, except for the addition of a could indeed generate hydrocarbons from its
reaction that could provide pair of oxygen atoms at the end of the carbon
chain. Removing this carboxylic head normally
own membrane fatty acids. The protein was
a new photoenzyme, which the researchers
cleaner hydrocarbons. requires expensive and energy-intensive
processes, such as electrolysis, and corrosive
named fatty photodecarboxylase.

reactants, such as sodium hydroxide.


A lush carpet of algae stretches over a Since the 1970s, there have been hints
placid freshwater lake. In the environmental
movement, this is the kind of treasured picture
that some microalgae are able to remove the
carboxylic head, although it has been equally “Seeing is
the word “green” was intended to evoke. Yet possible that any hydrocarbons generated
it could prove to be a source of a product that came from contaminating bacteria, or even believing. The
usually brings to mind all the dirtiness of crude from organic solvents used in the analysis.
oil: hydrocarbon fuel.
That is the suggestion of a group of
Given the prospect of a clean source of fuel,
Beisson and colleagues wanted to find out
structure of the
biochemists led by Fred Beisson at the Institute
of Biosciences and Biotechnologies of Aix-
for sure. Last year, they performed controlled
tests on several pure cultures of microalgae,
complex was
Marseille (BIAM), a joint institute of the French
Atomic Energy Commission, the French
and found that a freshwater species, Chlorella
variabilis, could indeed convert fat to fuel, with
important.”
National Centre for Scientific Research and sunlight as an input (Plant Physiol. 171 2393).
the University of Aix-Marseille. Previously, To explore how the microalga does it,
the researchers discovered that certain algae, Beisson and colleagues filtered its proteins
when illuminated by sunlight, are able to into a number of fractions, and tested each The discovery was exciting: besides
convert fatty acids into hydrocarbons. Now, for an ability to convert fat. The researchers photosynthesis, reactions involving light-
with help from the ESRF, the researchers have then used a standard technique known as driven enzymes are incredibly rare in living
found out how – and they believe the answer proteomics to identify the proteins inside organisms. To confirm the enzyme activity,
could lead to a clean source of biofuels. “It’s the most highly active fractions. Among the Beisson and colleagues sent crystals of the
amazing to discover that microalgae might 10 proteins common to the active fractions photoenzyme in complex with a common
hold a key to the fuel of tomorrow, especially analysed, only one of them was unknown. fatty acid to the ESRF’s MASSIF-1, the only
as regular petroleum is in fact heavily derived The researchers therefore made a bacterium beamline in the world able to automatically
from ancient algal deposits,” says Beisson. express the gene encoding this protein, and screen crystals and probe a crystal’s best

12 December 2017 O ESRFnews


Feature

Cryo-EM launched
technology in the microscopes themselves
ESRF facility delivers high- (electron delivery, for example) and in
cryo-EM sample preparation.
resolution structures As a European leader in large-scale
without crystals. structural-biology infrastructure, the ESRF has
embraced this cutting-edge technique and
invested in a cryo-EM facility, CM01, that will
For 10 years, you have been investigating the be operated in a similar fashion to its regular
structure of a biological complex comprising X-ray beamlines. A collaboration with the
dozens of proteins and nucleic acids. Classical European Molecular Biology Laboratory, the
macromolecular crystallography has given Institut de Biologie Structurale and the Institut
you high-resolution structures for some of the Laue-Langevin, CM01 was inaugurated last
components, but only a three-dimensional month, and will remain operational during the
structure of the entire complex at close to long ESRF shutdown for the Extremely Brilliant
atomic resolution will reveal its detailed Source upgrade in 2019/2020. CM01 is a state-
function and interactions. Unfortunately, of-the-art Titan Krios G3 cryo-EM for the 3D
although you have a pure sample of the characterisation of single particles of biological
complex, it refuses to be crystallised. macromolecules. In addition to a GATAN K2
If this situation is anything like your own, direct detection detector, this most powerful
the ESRF’s new cryo-electron microscopy and flexible high-resolution microscope is also
(cryo-EM) facility could help. equipped with a Volta Phase Plate, delivering
In a cryo-EM experiment, a solution high-resolution imaging of macromolecules of
containing the biomolecule or complex less than 150 kDa in mass, and a GIF quantum
of interest is applied to a sample holder, LS energy filter to enhance the quality of the
or “grid”, as a thin layer. The grid is flash- images by producing less background noise
frozen in liquid ethane to vitrify the sample, and better contrast. The high frame-rate K2
which is then imaged by the cryo-EM with detector can record many images in a “movie
Chlorella variabilis lives in a freshwater environment. low doses of electrons to minimise radiation mode”, thereby correcting for electron beam-
damage. Because particles are imaged induced sample drifts and enhancing both low-
diffracting volume. The data revealed directly, there is no need for crystallisation and high-resolution frequencies.
the fatty acid wrapped around part of – although, if available, any high-resolution As with any ESRF “beamline”, CM01 was
the photoenzyme that leads to where crystal structures of the complex’s individual extensively characterised and tested prior to
a common biochemical, flavin adenine components can be used to guide the its inauguration. The first large biomolecule
dinucleotide (FAD), can be held. Beisson and interpretation of the cryo-EM image. studied with the microscope – the tobacco
colleagues believe that, under blue light, the In October this year, the Noble in Chemistry mosaic virus, which infects tobacco and other
photoenzyme helps FAD to steal an electron was awarded to three scientists, Jacques plants – produced an excellent description
from the fatty acid, which responds by Dubochet, Joachim Frank and Richard of its three-dimensional structure at a
detaching its carboxylic head to make a pure Henderson, for pioneering developments resolution better than 4 Å. The result augurs
hydrocarbon (Science 357 903). “If seeing is using cryo-EM. Over the last decade or so, the extremely well for the new facility and its aim
believing, then the structure of the complex average resolution that can be obtained using of producing structural information of high
was indeed important,” says BIAM’s Pascal this technique has dramatically improved scientific impact on the form and function of
Arnoux, who worked closely with the ESRF from 15–20 Å to around 8 Å, with many of large macromolecular complexes.
beamline operation manager Didier Nurizzo. the most recent depositions in the Protein OProposals for experiments on CM01 can
In nature, explains Beisson, C. variabilis Data Bank exhibiting atomic resolution of be submitted via a Rolling Access application
probably converts some of its fatty acids to 3–4 Å. This leap has been made possible by pathway. See tinyurl.com/ESRFcryoEM.
hydrocarbons for use as a hydrophobic barrier, an enormous progress in direct-detection Christoph Mueller-Dieckmann and Eaazhisai
or for signalling purposes. By engineering a technology for cryo-EM cameras, the Kandiah, ESRF O
photosynthetic microorganism to produce
STEF CANDÉ

more of the photoenzyme, this mechanism CM01 was


could be encouraged for the industrial inaugurated in
generation of hydrocarbons for fuel. This would November.
be an all-in-one solution in which a ready-to-
use fuel is effectively produced by a cell factory,
via photosynthesis, from carbon dioxide.
Alternatively, the photoenzyme itself could be
exploited to convert fatty acids derived from
plant oils, such as rapeseed and palm.
With regular plant or microalgal fatty acids,
the hydrocarbons that result would be 15–17
carbon atoms long, like diesel. But Beisson is
musing on the possibility of shortening the
fatty acids first, to generate hydrocarbons
more like petrol (6–10 carbon atoms) or jet fuel
(10–13 carbon atoms). “Jet fuel is of particular
interest, because cars can always be powered
by electricity, but not planes,” he says.

December 2017 ESRFnews


O
13
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Focus on: Extremely Brilliant Source

Extremely brilliant progress


The ESRF’s upgrade, the Extremely Brilliant Source, is on track to
deliver exciting new scientific and industrial opportunities.

This year has been an important one for the spectroscopy monochromators in order to
ESRF’s upgrade programme, the Extremely enable a maximum number of beamlines to
Brilliant Source (EBS). On 27 June the ESRF
Council, representing the 22 partner nations
take full advantage of the EBS source.
Meanwhile, there is a significant
“Scientists
of the synchrotron, gave the green light
for the construction and commissioning
investment in the third pillar of the ESRF-
EBS programme: experiment control, data
will carry out
of new beamlines, which together with
the new source and enabling technology
management and the development of
advanced data-analysis tools for our users.
experiments that
make up the ESRF–EBS programme’s three
pillars. Four new beamlines will be designed
At the heart of this initiative is the new
data policy endorsed by the ESRF Council are currently
for the full exploitation of the enhanced in November 2015, which guarantees
performance of the first fourth-generation data archival for 10 years (and metadata impossible.”
high-energy synchrotron. They will address indefinitely) as well as open access to data
major challenges facing our society, including after an embargo period of three years, enable scientists to carry out experiments
the development of the next generation of which can be extended upon request. The that are currently impossible. We will
drugs, biomaterials and sustainable materials, implementation of the new beamline control ensure that the ESRF beamlines and their
and provide deep insights into the complex system, BLISS, will take place throughout the performance continue to evolve after the
mechanisms governing living organisms. duration of the ESRF–EBS programme. EBS project, to capture all opportunities to
They will elucidate our recent and ancient After a 20-month shutdown, starting at optimise the science that can be developed
past, as manifested in historical artefacts the end of 2018, the ESRF will come back with the new source.
and fossils. What’s more, they will provide with an extremely brilliant source that will Harald Reichert and Jean Susini, ESRF O
unique opportunities for applied and
innovation-driven research.
The choice of the four EBS beamlines
(which are described in detail on pp19–
25 of this issue) was the result of an
l
extensive selection process. The entire
c tiona Scie
un
ESRF user community put forward 48
expressions of interest, and the ESRF f nce
/ extr
Science Advisory Committee then
ranked the final eight proposals for new
ral y and em at
log atter
tu

con
beamlines. The construction of the new
diti e
uc
bio

beamlines is planned such that it will


tm on
Str

minimise the disruption of user service.


f

First steps towards the implementation


so

of the new EBS beamlines will be


taken in spring 2018 with the delivery
of Technical Design Reports for the
construction of the two first beamlines,
at BM18 and ID29.
e d scie n ce
exp p-a n d -pro b e
e nts a n d

Just the start


The four EBS beamlines will
New, better
be complemented by a deep science
i m a gin

refurbishment of three more beamlines


X-r a y

considered during the selection


process – ID10, ID24 and ID27 – and the
ti m e r i m
s o lv

implementation of two user platforms:


m
g

the high-power laser facility (HPLF)


Pu

and the cryo-electron microscope


e -r e

(cryo-EM). Within the framework of


continuing beamline refurbishment,
further beamlines will be modernised
too, following the outcome of the
N a n o s cie n c e
regular beamline reviews: ID18,
ID21, ID23-2 and possibly more.
Furthermore, significant investment
and
is foreseen for the upgrade of na n ote ology
detectors and the replacement of the chn
December 2017 ESRFnews
O
15
Focus on: Extremely Brilliant Source

ESRF–EBS: the
The makeup of the Extremely Brilliant Source (EBS) has become cle
of the upgrade, including new beaml
EBS flagship beamlines
Four entirely new beamlines will be
built between 2018 and 2022:
HPLF BM25 ID26 BM
A+
EBSL1 Coherence applications (see p19) A+B
EBSL2 Hard X-ray diffraction microscopy (see p21)
EBSL3 Phase-contrast tomography (see p23)
EBSL8 Serial synchrotron crystallography (see p25) BM23
ID24
25
ID23 24
EBS refurbishment beamlines EBSL3 (BM18) ID22 23
Also over the 2018–2022 period, a refurbishment
programme will be carried out in parallel to the regular ID19 22
refurbishment, to exploit the high performance of the new
EBS storage ring for other beamlines (see details opposite): ID21

21
ID10 Surface science
ID24 High brilliance X-ray absorption spectroscopy BM20
ID27 Nano X-ray diffraction in extreme conditions
ID20

20
New platforms
ID17 19
Finally, as part of ongoing efforts to provide improved
services to users, the ESRF is strengthening its expertise
with two cutting-edge platforms:
18

Cryo-EM for determining structures of biological ID18


macromolecules without crystallisation (see p13)
High-power laser facility (HPLF) for the creation
of exotic states of matter at ultra-high pressures and
17

temperatures, such as those found in exoplanets, or for


ID16 A+B
the study of matter under very high strain, such as that in
BM16
demand by industry.
16

Instrumentation and data


15

Properly exploiting the EBS’s outstanding X-ray


ID15A+B
properties involves major upgrades to instrumentation: 14
faster and more efficient detectors; better optics; and BM14
new end-station designs integrating mechatronic
13
concepts. But upgrades to data handling are just as ID14 12
crucial. Users will need to visualise data in real time to
adapt their measurement strategies, and the wealth
of data they record means much of it will need to be
ID13
processed on site, at least in part. On top of cutting-edge ID12
data storage, backup and processing facilities, therefore,
will be a new beamline control system, BLISS, a new ESRF
data policy to systematically record metadata, and the ID11
extensive adoption of a common software library for
data analysis, SILX. In fact, the improvements are already
coming: SILX software was recently shown to cut the
analysis time of an experiment at the ID01 beamline from
10 hours down to two minutes.

16 December 2017 O ESRFnews


e future is near
earer now that the ESRF Council has approved several key aspects
ines. Jon Cartwright takes a look.
ID10 Surface science
The new ID10 will have two experimental hutches: one
with a multipurpose diffractometer and beam deflector
M26 ID27 for studies of liquid surfaces, and the other for developing
+B the work of the former ID03 beamline, performing surface
X-ray diffraction with a focus on surface chemical reactions

ID28 BM28 EBSL8 (ID29) and surface dynamics. Such dynamics data will now shrink
to the millisecond range, which will allow catalytic ignition
and electrochemical dissolution processes to be studied at
ID30 unprecedented time resolution, and which will open up new
26 BM29 fronts on the dynamics of nanoparticles at fluid interfaces and
27 A+B
macromolecules in model cell membranes. A new large-area
28 pixel detector means that determining surface and interface
BM30 A+B structures will get roughly 100 times faster. Meanwhile,
improved optics will open up new possibilities for in situ and
operando studies and sub-micron objects, as well as dynamic
BM31 ID31
1

studies of buried interfaces.


2

BM32 ID32 ID24 High brilliance X-ray absorption spectroscopy


Here, one branch of the existing ID24 beamline – used for
3

energy dispersive X-ray absorption spectroscopy (XAS) –


BM01 will be converted for use with scanning extended X-ray
ID01 absorption fine structure spectroscopy (EXAFS). Using a novel
double-crystal monochromator, which is challenging from
4

BM02 Cryo-EM an engineering point of view, the new EXAFS branch will
provide a variable spot size of 1 mm to 1 μm, a variable flux
ID02 of up to 4 × 1013 photons per second and a time resolution
down to a second. Today, in situ XAS applications in the
5

EBSL2 (ID03) geosciences are limited to conditions relevant to the Earth’s


lower mantle, but the new ID24 will allow investigation of
the local structure of melts at the inner core boundary, at
pressures and temperatures exceeding three megabars and
6

5000 K. Functional materials and natural samples will also be


explorable at unprecedented concentrations and timescales.
7

8 BM05 ID27 Nano X-ray diffraction in extreme conditions

9 Extending the existing ID27 beamline from 50 to 120 metres,


the new ID27 will be a sharper, more flexible nano-focussed
ID06
10 probe, unique in the world in terms of photon flux and
focussing capabilities. Coupled with the most advanced
11
tools to monitor the most extreme conditions of pressures
and temperatures, the upgraded capabilities will largely
EBSL1 (ID08) surpass current barriers and open unique routes to probe new
BM08 material properties. It will benefit many areas of research,
ID09 from planetary science to fundamental physics, including
ID10 solid-state chemistry, materials science and biology. For
example, the small beam size will allow scientists to probe
pressures higher than found at the centre of the Earth, while
fast signals will capture information from short-lived samples,
such as those held at above 3,000K in liquids. Materials
engineering and the pharmaceutical industry will be well
served.

December 2017 ESRFnews


O
17
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Focus on: Extremely Brilliant Source

The ideal 103


104 103
length scale (Å)
102 101 100

10–17

match 101
10–15
XPCS (present)
For XPCS, a technique 10–1
10–13
reliant on coherent X-rays,

time scale (s)

energy (eV)
the EBSL1 beamline is a 10–3
10–11
dream come true.
10–5
10–9
XPCS at EBS

The boost in coherent flux of the ESRF’s 10–7


Extremely Brilliant Source (EBS) upgrade 10–7
will directly benefit many X-ray techniques.
Perhaps none more so, however, than X-ray
10–9

FEDERICO ZONTONE, ESRF


photon correlation spectroscopy (XPCS).
With this technique, the smallest accessible 10–4 10–3 10–2 10–1 100 101
timescale improves with the square of the scattering vector Q (Å–1)
coherent flux. While the EBS coherence rises
100-fold, therefore, the key performance
In XPCS, coherent light scattering from a sample forms a speckle pattern that reveals information
factor of XPCS advances 10,000-fold. The EBS
about the intrinsic dynamics. Above: The dynamical range of XPCS before and after the EBS
is now set to exploit this potential with a new
upgrade. Below: With the new EBSL1 beamline, the acquisition time (o) between speckle patterns
XPCS beamline, EBSL1.
will be 10,000 times faster, allowing the observation of much more rapid dynamical processes.
The ESRF has always been an XPCS pioneer,
being the first synchrotron in Europe to open
a station for the technique in the 1990s. XPCS
is used to study slowly changing phenomena
o
(currently on the scale of 10 –2–104 seconds)
down to the nanometric and atomic scale.
“The key
It can track dynamics over time, and as a
function of external parameters, including
performance
temperature, illumination conditions, electric
and magnetic fields, and pressure. Scientists factor of
routinely use it to measure fluctuations in a
variety of colloidal, soft and hard condensed-
t
XPCS improves
matter systems on mesoscopic scales; at
the ESRF, scientists have led the way in
the observation of slow dynamics (lasting
10,000-fold.”
longer than 10 seconds) in alloys and glasses
on atomic length scales. XPCS is the only level. For the first time, it will be possible to thick specimens at nanometre resolution.
technique to observe atomic dynamics in explore microsecond fluctuations in biological CXDI at EBS promises three times higher
deeply supercooled melts and in structural systems (such as proteins and water-based resolution in tomographic imaging, bridging
glasses. soft matter) and in hard materials (such the gap between the atomic resolution of
as high-temperature superconductors, transmission electron microscopy and other
Massive boost piezoelectrics and magnetic systems). Thanks electronic techniques, and the sub-micron
Yet, XPCS at the ESRF is currently operating to the use of high energies, XPCS at the EBS resolution of optical microscopes. It will offer
during just half of the available beamtime at will unveil the particle motion of complex unique possibilities to study pathological
ID10, and it is strongly limited by the small materials under pressure (polyamorphism changes of bone structure, human cells and
fraction of coherent flux available from a in liquids and glasses), in confinement growth processes of bio-minerals and micro-
third-generation storage ring. Operating at and at buried interfaces. Many of these particles with 5–10 nm resolution.
low photon energies of around 8 keV also processes are characterised by spatial and Before EBSL1 is up and running, major
limits experiments with radiation-sensitive dynamical heterogeneities that evolve on technical challenges, including stability
samples, and sample environments requiring a the microsecond timescale. For the first time, requirements and detector development,
higher transmission power. these phenomena will be experimentally will have to be solved in order to exploit the
Situated at the ID08 port, the new EBSL1 accessible over a broad length scale, ranging extraordinary increase in coherent flux with
will easily surpass these former limitations. from single particles to particle clusters. small diffraction-limited X-ray beams. But
The EBS’s boost in coherence and its EBSL1 will be unique worldwide, but it one thing is for certain: the instrument will
extension into photon energies of 35 keV will not just be a platform for XPCS. It will open a new horizon in many disciplines across
will open the door to new groundbreaking also revolutionise coherent X-ray diffraction physics, material science and biology.
experiments, covering 11 orders of magnitude imaging (CXDI), a lensless microscopy Beatrice Ruta, Institut Lumiere Matière,
in timescales at both the nano and atomic technique for three-dimensional imaging of Université Lyon 1 and CNRS, France O

December 2017 ESRFnews


O
19
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Focus on: Extremely Brilliant Source

Tilting the scales


EBSL2 will allow users to track structural dynamics across length scales in real time.

Most hard materials – from rocks to metals, diffracted X-rays, we created a magnified,
to semiconductors and even bone – have full-field image of the individual dislocations
complex internal structures, often comprising
several layers of substructures interwoven
“We will capture within the crystal – a technique known
as dark field microscopy. Coordinated
across multiple length scales. What’s more,
these hierarchical structures define many of
real-time movies movements of the sample and optics then
enabled us to quantitatively map the local
the properties of the material. Bone is a classic
example: its unexpectedly high toughness
of structural crystal strain and symmetry with a resolution
of 100 nm. These maps showed how
stems from the way “hydroxyapatite”
nanoparticles self-assemble into highly dynamics.” dislocations and stacking faults self-organise
inside the material to create buried networks
oriented fibres up to the macroscopic characterised by long-range strain fields and
scale. Understanding the material means lattice distortions (see figure).
understanding the dynamics of how the jointly between the Technical University Now, however, this result is set to be just
individual sub-structures interact – but this of Denmark (DTU) and the ESRF as part the tip of the iceberg. One of the ESRF–EBS
requires direct access to every length scale, of an Advanced Grant from the European upgrade beamlines, EBSL2, located on the
within the same sample and at the same time. Research Council. Six years on, at the end ID03 port, will improve spatial resolution
This is the idea behind the hard X-ray of 2016, this collaboration resulted in a 10-fold, while making experiments hundreds
microscope: a single instrument offering prototype instrument at ID06. First results or even thousand of times faster. This
comprehensive full-field and time-resolved have provided new insights into some means we are no longer limited to seeing
imaging in two, three and four dimensions of longstanding and fundamental problems in static structures, but can capture real-
the phases, grains, domains, stress fields and metallurgy, energy and biological materials. time movies of structural dynamics as they
defects spanning length scales from 1 mm In one case, we visualised the multi- happen across multiple length scales. In the
to 10 nm. scale structure of dislocation networks in context of diamond, it could mean tracking
What makes hard X-ray microscopy unique diamond, an important industrial material the 3D motions of dislocations as they form
is the broad range of problems it can tackle. and, more recently, an ideal sandbox networks under stress. More broadly, it
Using high energy X-rays we can probe sub- for quantum-information technologies. allows us to pursue much more aggressive
structures within large samples or even Crucially, its photonic properties are dynamics problems, such as nucleation and
full devices. By combining complementary largely at the mercy of these defects – their material failure.
imaging techniques with the versatility intermingling networks, and the long-range The ability to extend 3D imaging into
of X-ray optics, we can seamlessly switch strains they create. the temporal regime is a game-changer
between fast overviews of microscopic At the coarse scale, we used diffraction for materials science, providing the
features and detailed images of individual X-ray topography to map the location of opportunity to truly guide and validate
defects. In this sense, the hard X-ray every dislocation in the crystal. This allowed multi-scale materials models. Such models
microscope is analogous to a transmission us to find a specific set of dislocation lines are essential to emerging approaches to the
electron microscope, albeit one that leverages of interest, in this case a group of three computational design of materials.
the penetrating power of X-rays to see orders containing kinks, including one with a clear Henning Friis Poulsen and Hugh Simons,
of magnitude further into the samples. stacking fault. Next, simply by inserting an Technical University of Denmark, and
Hard X-ray microscopy was developed X-ray objective lens into the beam of Bragg- Carsten Detlefs, ESRF O

X-ray topography Dark-field X-ray microscopy

DTU

200 μm 30 μm 4 μm

A multi-scale analysis of an artificial diamond shows the dislocation network, individual dislocation lines, and a single stacking
fault embedded deep within the crystal. After the EBS upgrade, with the EBSL2 beamline, it may be possible to track the
3D motions of these features with sub-second resolution as the material is stressed.

December 2017 ESRFnews


O
21
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Focus on: Extermely Brilliant Source

Bigger, faster, stronger, better


Thanks to EBSL3, microtomography could be targeting objects the size of car engines at
unprecedented speed and quality.
Synchrotron microtomography is one
of the primary three-dimensional
characterisation techniques at the
ESRF. Simple, non-destructive and
– compared with conventional X-ray
microtomography – fast and high-
quality, it has evolved steadily over
the past 20 years, and is now available
on several beamlines. Where once
there was a tool that could scan only small
samples using X-ray absorption, there is
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mechanisms and in times down to a

FRAUNHOFER
tenth of a second, even in complex
in situ or in operando environments.
Indeed, versatility has been key to the
success of the microtomography at
the ESRF, and explains the breadth
of applications covering material
science, cultural heritage, biology,
biomedical research, geology,
and notably industry.
Despite this success, however,
synchrotron microtomography
is reaching its limit. Industrial and
academic scientists want to scan even bigger
samples, at higher resolution and with better
phase-contrast capabilities at high energy; The application-oriented research organisation
they want to scan large series of samples, Fraunhofer, based in Germany, is able to detect
sometimes with multiple resolutions and with sub-millimetre defects in this aluminium
high throughput. experimental hutch will allow propagation engine cast using high-energy conventional
An entirely new beamline, EBSL3 – distances up to 35 metres, in order to X-ray tomography. With the EBS’s EBSL3
together with a refurbishment of the ESRF’s obtain high levels of phase contrast even beamline, it would be able to detect defects in
present iconic microtomography beamline, at maximum energy and low resolution. All the 20-micrometre range, and then examine
ID19 – will eclipse these limits. Making the this will be possible for samples 100 times them on a microscopic scale.
very best of the ESRF’s Extremely Brilliant bigger than today (up to 2.5 metres vertically
Source (EBS) upgrade, EBSL3 will be a 220 by 1.5 metres horizontally), for weights up samples, such as defects in aluminium engine
metre-long beamline that will perform to 300 kg. The whole beamline is designed casts (see figure), or the microscopic structure
hierarchical imaging (a voxel size of 100 μm to be rapid, versatile, easy to use, largely of large composite devices, with world-
down to 1 μm) of medium to large objects, automatic, and robust, to ensure high level of leading sensitivity and resolution.
using propagation phase contrast with reliability and high throughput. Academic fields, from cultural heritage to
high levels of automation. Thanks to the biomedical applications, will greatly benefit
EBS’s exceptional coherence, high-quality Parallel upgrade too. Today we can scan a Tyrannosaurus rex
propagation phase contrast of up to 350 While EBSL3 is being built, the upgrade of arm, a cat mummy, or a small human organ;
keV will be possible. A 40 metre-long the upgrade of ID19 will lead to it becoming tomorrow we will be able to scan a complete
an undulator-based beamline that reaches T. rex skull, a complete human mummy in its
higher resolutions with higher throughput, wooden sarcophagus, or even a complete
as well as at high energies in the sub-micron human body. Inside any of these we will see
“These range. X-ray imaging is one of the ESRF’s best
industrial tools, and so EBSL3 and ID19 have
things no one has ever seen before without
destroying the specimen, down to the
synchrotron been designed together with industrial needs
in mind. High throughput will allow rapid
micrometre scale.
This large-scale project will continue
microtomography surveys of, for example, pills and small metallic
devices on ID19, or batteries, mechanical
to make the ESRF’s synchrotron
microtomography capabilities truly unique,

abilities will be items and food products on EBSL3. On the


other hand, the large, high-energy beam
benefitting a host of industrial and academic
scientific topics – including many we are not
and hierarchical capabilities of EBSL3 makes yet even aware of.
truly unique.” it ideally suited to study small aspects of big Paul Tafforeau, ESRF O

December 2017 ESRFnews


O
23
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Focus on: Extremely Brilliant Source

The serial approach


With EBSL8, synchrotron
serial crystallography is
coming to the ESRF with
full force.
The harder you look, the more damage
you do: this unalterable truth of X-ray
crystallography has always prevented
crystals of biological macromolecules from
divulging all their structural information A schematic
before they are destroyed by radiation. Serial representation of
crystallography (SX), performed at either X-ray transmembrane
free electron lasers (XFELs) or synchrotron signalling in histidine
sources, helps overcome this limitation. The sensor kinases,
technique involves taking diffraction data reconstructed from
from numerous microcrystals – hundreds ESRF data. Effector
of thousands, in some cases – in order to (NO3) binding to the
assemble a complete dataset, piece by piece. receptor domain
SX was developed at XFELs, where just a outside the cell
single femtosecond pulse is usually enough produces a cascade
to destroy a crystal and where it is known as of conformational
serial femtosecond crystallography (SFX). changes (right)
The first successful applications involved that transmit the
sending crystals through the pulsed X-ray signal across the cell
beam in a liquid jet, at a density optimised for membrane where it
a maximum “hit rate” when crystal and X-ray will eventually reach
beam coincide. Later, investigators found that partner molecules in
less crystalline material was needed when the the signalling process.
crystals were contained in a viscous liquid, The new EBSL8
or even on a fixed target containing specially beamline could make a
designed crystal holders from which, in “molecular movie” of
favourable cases, multiple diffraction images this process.
could be collected per crystal.
Now, following successful proof-of- sources (Acta Cryst. D70 1248). Perhaps the programmes that should require lower
principle synchrotron experiments at the ESRF biggest advantage, however, is that SX allows consumption of both potential drug molecules
and elsewhere, the ID29 beamline is being time-resolved experiments to be carried out. and their biological targets. Moreover, SSX-
rebuilt for synchrotron serial crystallography The most exciting recent example of this derived room-temperature crystal structures
(SSX) as part of the ESRF’s Extremely Brilliant has been the SFX studies on photosystem will provide more information of the dynamics
Source (EBS) upgrade. Although an ESRF team II – the enzyme that splits water molecules of drug binding.
led by Daniele de Sanctis is still finalising the in photosynthesis – where researchers have Examples of other systems where SSX
technical details, the new beamline, EBSL8, obtained structures of different states in the can provide crucial structural information
promises to carry out entirely new types of photocycle (Nature 513 261). abound. These include bacterial sensor
experiment at a synchrotron source. histidine kinases, which play an important role
The beamline will have a variable focal Crucial timescale in signal transduction. This year, a group led
spot size of 0.5–10 μm, tuneable over the The EBSL8 SSX beamline will produce similar by Valentin Gordeliy at the Research Centre
energy range 10–30 keV, with a flux of some insights on many biological systems. While Jülich in Germany, including scientists at
1016 photons per second. That equates to a the exploration of femto- and nano-second the ESRF, determined crystal structures of a
brilliance many orders of magnitude higher timescales will remain the domain of XFELs, large fragment of the Escherichia coli nitrate/
than current macromolecular crystallography EBSL8 will take full advantage of the EBS nitrite sensor NarQ in its ligand-bound and
beamlines. The smallest beam size will allow upgrade to allow crystallographic studies at ligand-free states. The results revealed a
SSX data collection from micron or even sub- sub-millisecond time resolution, a timescale signalling mechanism based on a cascade of
micron sized crystals. on which many conformational changes in conformational changes that are transmitted
SX has several advantages over conventional biological macromolecules take place. from outside to inside the cell (Science 356
crystallography. One is that SX facilitates data Other potential experiments on the new 1043, see figure). EBSL8 will make it possible
collection at room temperature rather than beamline include optimised “mesh and to study this signalling mechanism in much
the usual cryogenic temperatures, which collect” experiments, in which a complete greater detail, including the production of
sometimes obscure functionally important data set is compiled from diffraction images a “molecular movie” of the conformational
conformations. Also, SSX at EBSL8 will allow from hundreds of crystals contained on changes involved.
exploration of the potentially mitigating the same sample support. EBSL8 will also Andrew Leslie, MRC Laboratory of Molecular
effects on radiation damage of very fast, very naturally expand industrial applications with Biology, Cambridge, UK, and Gordon
high dose rate data-collection at synchrotron microcrystal-based rational drug-design Leonard, ESRF O

December 2017 ESRFnews


O
25
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16-014
Portrait

The beauty of small things


Titia Sixma of the Netherlands Cancer Institute reveals how modern techniques
are helping us see life’s tiniest components in ever more detail.
A toxin that gives people stood out in three dimensions,”
traveller’s diarrhoea may not she says. Today, the structures of
sound like the most glamorous the mammalian receptors are only
topic for a PhD. For a true just being solved, although Sixma
structural biologist like Titia is no longer pursuing the topic.
Sixma, however, the interest Now head of biochemistry at
always lies in the finer details: the Netherlands Cancer Institute,
a molecular structure of Sixma is well aware of the strong
30 beta strands in five-fold collaboration between the
symmetry, within an asymmetric Netherlands and the ESRF. They
heterodimer. “It’s a beautiful share an ESRF block allocation
protein, it’s gorgeous,” she says. group with structural biologists
In fact, Sixma’s Escherichia in Belgium, and the two countries
coli protein structure revealed have a dedicated collaborating
valuable information as well as research group beamline at BM26,
beauty, for its unusual architecture DUBBLE. They have been coming
suggested ways in which it could regularly to ESRF for many years.
enter human cells. This was all Recently, however, Sixma has
the more important since the been “extremely pleased” with
diarrhoea toxin is closely related the ESRF’s automated MASSIF
to another that results in cholera, beamlines. “At the moment our
and so perhaps it was little surprise default is to send things to MASSIF
that the crystallography results, first. It’s really efficient. We got
taken at the European Molecular a couple of really nice structures
Biology Laboratory’s beamlines
Titia Sixma in brief back recently with minimal effort.”
at the Hamburg synchrotron Born: 1962, Utrecht, the Netherlands.
HASYLAB, found their way into Education: BSc chemistry, University Utrecht (1987); PhD structural Cool ideas
the journal Nature. That was way biology, University of Groningen (1992). With the advent of cryo-
back in 1991, three years before Career: Postdoc Yale University, New Haven, Connecticut, US electron microscopy (cryo-EM,
the ESRF was inaugurated – a time (1992–1994); group leader (1994–present) and division head see p13) at the ESRF, Sixma is
when structural biology was on (2008–present) Netherlands Cancer Institute; affiliate professor eager to further another of her
the cusp of a rapid expansion. (2004–present) of structural biology, Erasmus University Rotterdam. key research areas: ubiquitin
Sixma, a chemist by training, was conjugation, a process in which
lured by the prospect of hard data one or more ubiquitin proteins
in a field traditionally swamped by hang on to a target protein to
complexity.
“Having access to change its fate. In the last few
years, she and her colleagues
New horizons have determined a number of
Sixma continued to study the crystallography and cryo-EM structures of deubiquitinating
human process targeted by the enzymes to understand how they
toxin in her postdoc, before
quickly taking up a group-leader
is very powerful.” are regulated via “allostery”, or
the transmission of binding effects
position at the Netherlands everyone’s cells when they divide, transmission in the nervous from one site to another. This could
Cancer Institute in Amsterdam, to repair the few mistakes that system. In humans and other help in targeting them for cancer
where she has stayed since. “I occur during DNA replication. But mammals, these targets are or neurodegenerative drugs, but
was lucky because structural sufferers of Lynch syndrome have membrane proteins known as some of the latest proteins are
biology was expanding, and mutations in the genes encoding nicotinic acetylcholine receptors proving hard to crystallise. “We’ve
positions were appearing,” she the mismatch-repair proteins, and (nAChRs), and biochemists have been banging our heads against
recalls. There still are relatively therefore have a predisposition long tried to uncover how they the wall for too long, not getting
few structural biology groups in to colon cancer. Sixma has bind to important ligands. In the crystals of the larger and more
the Netherlands, yet Sixma has studied how the proteins work, to early 2000s, Sixma and others transient complexes, where we
come to be regarded as one of the understand how these enzymes used the ESRF to reveal how an want to capture the molecules
leading scientists in her field. find these very rare errors and then analogue of the nAChRs’ ligand- in action,” says Sixma. “With
One of the reasons for that is only repair the newly synthesised binding domain binds its ligand: cryo-EM we still have to trap the
her work on DNA mismatch repair, strand (Elife doi:10.7554/ so called acetylcholine-binding right transient state, but at least
for which she came to the ESRF eLife.06744) protein, found in snails (Neuron then we don’t need to crystallise
in the late 1990s to make use of Another high point in Sixma’s 41 907). “There were many them. Having access to both
its crystallography beamlines career has been the study of things known about the receptors crystallographic methods and
BM14 and (now decommissioned) the targets of molecules, such before, but with our structure cryo-EM is very powerful.”
ID14. Mismatch repair happens in as nicotine, that affect signal everything fell into place, and Jon Cartwright O

December 2017 ESRFnews


O
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Industry

Steel dives into dark-field microscopy


Research centre for the application of steel turns to
the ESRF to improve alloys.

In traditional metallurgy, Source upgrade of the ESRF.

JEFF WADE
microstructures can only be Yildirim’s model samples
studied in two dimensions in are used to design the
the finished product. “When methodology, and especially
I heard that we could follow the heat-treatment cycle
metallurgical reactions live management in alloys. In
and in 3D, I was immediately conventional steel processing,
convinced that this was the way nitrogen alloying is challenging
to go,” says Roger Hubert, the due to the element’s limited
chief scientific officer at OCAS, solubility during casting and
a metallurgical research centre solidification. Alternatively,
in Belgium. nitriding as thermochemical
Meanwhile, OCAS has funded treatment on the final material
a postdoctoral researcher, Can (also called case hardening) can
Yildirim, to investigate the be used to significantly improve
effects of nitrogen alloying in surface and bulk properties.
steel at the ESRF. Nitrogen can Thanks to dark-field X-ray
boost various steel properties microscopy, Yildirim and others
such as strength and hardness, can look inside the material,
but this strongly depends on whether it is inside a furnace
controlled nucleation and or other sample environment,
growth of nitride phases. Upon Yildirim at work on ID06. and see how the microstructure
cooling down, the solubility of evolves during processing. That is
nitrogen decreases and excess microscopy. Unlike bright-field crystalline materials from what makes it ideal for industrial
nitrogen precipitates as iron microscopy, where a sample is 100 nm to 1 mm, even at high clients such as OCAS.
nitrides. These precipitates are seen on a bright background temperatures. “We’re basically In July, Yildirim and his
desirable, so long as their phase, thanks to direct illumination, able to see the internal structure colleagues also conducted a
morphology and size can be dark-field microscopy detects of steel alloys and follow which first experiment on non-grain-
controlled. only light that is scattered from processes occur on a sub-micron oriented electrical steel samples,
To explore these iron-nitride Bragg diffraction. The result is scale in operando conditions,” and were moving on to a second
precipitates, Yildirim turned to a non-destructive technique says Yildirim. The technique will experiment at ID06 as this issue
ESRF beamline ID06, where he that allows 3D mapping of become even more powerful went to press.
could perform dark-field X-ray orientations and stresses within with the Extremely Brilliant Jon Cartwright O

Movers and shakers


Edith Heard James ESRF users Paul Michael Hahn,
has been Naismith has Shearing (left) former leader
selected to been appointed of University of the ESRF
be the fifth director of the College London vacuum group,
director new Research in the UK and has taken
general of the Complex Donal Finegan sabbatical
European Molecular Biology at Harwell (RCaH), a of the National Renewable leave to become section leader
Laboratory (EMBL). Currently multidisciplinary lab that has Energy Laboratory in Colorado, of vacuum technology at the
the director of the Genetics facilities for researchers in US, have won a coveted “Safety Paul Scherrer Institut (PSI) in
and Developmental Biology the life and physical sciences, and Security” award from The Villigen, Switzerland. At the PSI
Unit at Institut Curie in Paris, including those using the Engineer magazine for their he will be in charge of vacuum
and chair of epigenetics and adjacent Diamond Light Source. research on the failure of lithium- systems of large research
cellular memory at the Collège A long-standing member of ion batteries. Judged by a panel infrastructures, consisting of
de France, also in Paris, Heard Diamond’s board of directors, of leading UK engineers, the proton machines, a synchrotron
has research experience in Naismith is an expert in using awards draw attention to work light source and a free electron
epigenetics and developmental X-ray crystallography of proteins that is “innovative, collaborative laser under construction. He will
biology, as well as chromosome to investigate the pathways of and likely to have an impact in also work on the definition and
and RNA biology. She will take disease. He retains a position at their field of application”, and are preparation of the forthcoming
over from the EBML’s existing the University of Oxford, where designed to snapshot of some improved Swiss Light Source,
director general, Iain Mattaj, in he is also co-interim leader of the of the trends and technologies SLS-2, which is expected to be
January 2019. new Rosalind Franklin Institute. defining modern engineering. built over the period 2021–2024.

December 2017 ESRFnews


O
29
Beauty of science
Family resemblance:
Meet Alesi, a 13 million year-
old fossilised ape who –
thanks to research carried out
at the ESRF – has given strong
clues about the common
ancestor of all living apes and
humans. Alesi’s skull was dug
up in the Turkana basin of
northern Kenya three years
ago, and although it looks like
that of a gibbon, it is actually
that of a primate in the genus
Nyanzapithecus. Performing
X-ray microtomography at
ESRF beamline ID19 on Alesi’s
teeth, scientists revealed that
the primate was just one year
and four months old when it
died; meanwhile, in the inner
ears (highlighted green) the
microtomography revealed
cochleae (for hearing) and
semi-circular canals (for
balance). These structures,
and the size and shape of
the teeth, suggest that Alesi
was an ape, and specifically
an evolutionary cousin to
that line of ancestral apes
from which humans split off
some seven million years ago
(Nature 548 169).

In the corridors
China launches X-rays help restore
X-ray telescope wind instruments
China’s most recent foray Scientists at the Paul Scherrer
into space-based science is Institut (PSI) in Switzerland
an X-ray satellite, the Hard have used X-ray and neutron
X-ray Modulation Telescope tomography to guide the
First users at XFEL (HXMT), which launched in restoration of more than a
First experiments began at the June. Designed to study some dozen 16th-century Italian wind
European X-ray free-electron of the universe’s most energetic instruments. The resultant three-
laser (XFEL) in Hamburg, phenomena, such as gamma-ray Briefest X-ray flash dimensional images revealed
Germany, on 20 September, bursts, neutron stars and black the internal structure of the
nearly three weeks after the holes, HXMT actually carries A group led by Zenghu Chang at components made of wood,
facility was inaugurated. three X-ray telescopes operating the University of Central Florida metal and leather, in particular
Highlighting the range of at different energies, from 20 to in Orlando, US, has smashed its the shape of the finger holes
methods available at the XFEL, 200 keV. It is the latest of a series own record for the fastest X-ray and the borehole, and their
the experiments include the of instruments launched as part pulse. Lasting just 53 attoseconds deterioration over hundreds of
use of different spectroscopy of China’s highly active space (10 –18 seconds), the pulse was years. “Using this data, we can
methods to track ultrafast programme, including probes 14 attoseconds shorter than the now reconstruct for the first time
reactions and electron movement of dark matter, microgravity group’s previous record set in what they would have sounded
in model molecules, the probing and long-range quantum 2012, and is equivalent to the like when first played,” said
of organic light-emitting diodes, entanglement. time it takes light to travel one- Giulia Festa at the University of
and the investigation of nitrogen thousandth the diameter of a Rome Tor Vergata.
and oxygen recombination human hair. It was generated by
in the muscle tissue protein interacting an intense infrared
myoglobin. “This is a very laser with a noble gas, and is
important event, and we are thought to be important because
very happy that the first users it reaches the “water window”,
have now arrived,” said Robert where carbon atoms absorb
Feidenhans’l, the European XFEL’s strongly but water does not (Nat.
managing director. Comm. 8 186).

30 December 2017 O ESRFnews


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±5 A and ±10 A / ±20 V Bipolar Power Supply Series
Full-Bipolar operation, Digital Control Loop, Ethernet Connectivity
Device supported by Visual Easy-Driver software

FAST-PS-M
Digital Monopolar Power Supplies - up to 100 A
High-Precision Monopolar Power Converters with Gigabit Ethernet
Embedded Linux OS, device supported by Visual PS software

FAST-PS
Digital Bipolar Power Supplies - up to ±30 A and ±80 V
Full-Bipolar, Digital Control Loop, High-Bandwidth, 10/100/1000 Ethernet
Embedded Linux OS, device supported by Visual PS software

FAST-PS-1K5
Digital Bipolar Power Supplies - up to ±100 A and ±100 V
1.500 W, Paralleling via SFP/SFP+, 1 ppm/K TC, 10/100/1000 Ethernet
Embedded Linux OS, device supported by Visual PS software

NGPS
High-Stability 10-kW Power Supply - 200 A / 50 V
Digital Control Loop, Paralleling via SFP/SFP+, 10/100/1000 Ethernet
Embedded Linux OS, device supported by Visual PS software

www.caenels.com

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