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VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
Neutron scattering at the OPAL research reactor
Garry J. McIntyre and Peter J. Holden
Bragg Institute, Australian Nuclear Science and Technology Organisation, New Illawarra
Road, Lucas Heights NSW 2234, Australia
E-mail: garry.mcintyre@ansto.gov.au
Abstract. The current suite of 14 neutron scattering instruments at the multipurpose OPAL
research reactor is described. All instruments have been constructed following best practice,
using state-of-the-art components and in close consultation with the regional user base. First
results from the most recently commissioned instruments match their design performance
parameters. Selected recent scientific highlights illustrate some unique combinations of
instrumentation and the regional flavour of topical applications.
1. Introduction
Australian neutron scattering leapt into the 21st century with the start up of the 20 MW
OPAL nuclear research reactor at the Australian Nuclear Science and Technology Organisation
(ANSTO) in 2006. OPAL is unique amongst modern high-power research reactors in that it is
multipurpose, being used to produce medical isotopes and exploited for neutron transmutation
doping and neutron activation analysis, as well as being used to provide beams for neutron
scattering. While the multipurpose nature led to some compromises in the core design for
the neutron-beam instruments, it brought with it valuable political and economic security. Both
OPAL and its cold-neutron source, the running of which is not linked intimately to the operation
of the reactor unlike at most research reactors, now operate consistently for around 300 days
per year - an impressive statistic amongst modern research reactors.
The major part of the initial success at OPAL has been in crystallography, carrying on the
excellent tradition established since the late 1950s at the HIFAR reactor at Lucas Heights.
HIFAR had an illustrious career in itself. As well as providing a materials research capability
for the (then) projected nuclear power programme in Australia, it was also the training ground
for many young scientists that went on to distinguished careers in Australia and abroad. Hugo
Rietveld and Alan Hewat of neutron powder diffraction (NPD) fame were just two of these,
although it is noteworthy that their first neutron experiments were in single-crystal diffraction
[1] and triple-axis spectrometry [2] respectively, since the power of NPD in materials discovery
was yet to be realised, much less appreciated.
As befits a national facility, the neutron-scattering science at OPAL is largely driven by the
external user programme, through a peer-review proposal system for access to the neutron-
beam instruments. Fee-for-service commercial use is growing with the present target being 5%
averaged over the full suite. Certain scientific themes, where neutrons offer distinct advantages as
a research tool, are also promoted within the Bragg Institute, the entity that runs the neutron-
scattering programme. These themes currently include energy materials, thermo-mechanical
processes, magnetism, food science, biomolecules, and cultural heritage.
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Published under licence by IOP Publishing Ltd 1
VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
Figure 1: Schematic of the layout of the neutron-beam instruments at OPAL. DINGO, SIKA,
and TAIPAN are located close to the reactor face, the other instruments are on neutron guides.
Green text denotes the instruments on thermal neutron beams, blue text those on cold neutron
beams. Also indicated is the convenient location of the 3He spin-filter filling station atop the
neutron guide bunker.
Here we introduce the OPAL neutron-beam facility, show the first results from the instruments
most recently brought on-line, and describe recent scientific highlights allied closely to the new
or unique instrumentation.
2. Neutron-beam instruments at OPAL
The construction of the neutron-beam instruments at OPAL has proceeded in three main
tranches. The first, called Neutron Beam Instrument Project - 1 (NBI-1), produced the first
seven instruments [3] as part of the full funding for the reactor construction. The second,
denoted Major Capital Works with funding from various internal and external sources, yielded
four further instruments. Most recently, the Neutron Beam Instrument Project - 2 (NBI-2)
funded as part of the Super Science Initiative of 2009, has added three more [4], to bring the
total number of instruments to 14. Figure 1 shows the layout of the current suite of neutron-
beam instruments at OPAL, and table 1 describes each instrument with its key features and the
year that it entered user operation.
Based largely on user wishes, the suite of instruments is fairly conventional and
constructed using proven components following best practice elsewhere, to produce state-of-
the-art instruments, but occasionally in unique combinations of components and with unique
applications. One example is the time-of-flight spectrometer PELICAN, which has been designed
from the outset to offer a full polarisation analysis capability using a supermirror polariser before
the sample, a PASTIS insert [5] around the sample, and a wide-angle 3He spin-filter cell after the
sample, a worthy successor to the long-wavelength polarised-neutron spectrometer LONGPOL
[6], which gave HIFAR a unique capability for several decades.
The cold-neutron triple-axis spectrometer, SIKA, constructed by National Central University,
Taiwan, and just recently awarded its operating licence, has been presented elsewhere at
2
VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
Table 1: Neutron-scattering instruments at OPAL in 2015.
Instrument Description Features In user Referencea
program
Diffraction
ECHIDNA High-resolution powder 128-element multi-tube 2008 [7]
diffractometer detector, robot sample
changer
JOEYb Neutron Laue camera for Fast-read-out CCD detec- - [8]
single-crystal alignment tor; precision sample ta-
ble that supports 200 kg
KOALA Thermal neutron Laue Sample volumes of typi- 2008 [9]
diffractometer cally 0.1 mm3
WOMBAT High-intensity (powder) Large area detector, op- 2008 [10]
diffractometer tional radial oscillating
collimator
Inelastic scattering
EMU High-resolution backscat- Nearly exact back- 2016c
tering spectrometer scattering at low Q
PELICAN Time-of-flight spectrome- Designed at the outset 2014 [11]
ter for optional polarisation
analysis
SIKA Cold-neutron three-axis Choice of single or multi- 2015
spectrometer analyser
TAIPAN Thermal-neutron three- Optional Be-filter mode 2010 [12]
axis spectrometer
Small-angle scattering
BILBY Time-of-flight small- Large Q range for kinetic 2016c
angle neutron-scattering studies
(SANS) instrument
KOOKABURRA Ultra-small-angle Bonse-Hart geometry 2014 [13]
neutron-scattering in- with choice of two wave-
strument lengths
QUOKKA Pinhole SANS instrument Large area detector; re- 2009 [14]
fractive lens; polarised-
neutron options
Nano- to macro-scale imaging
DINGO Neutron imaging instru- High-flux and high- 2014 [15]
ment resolution modes
KOWARI Strain scanner Large-volume samples up 2008 [16]
to 1 t; texture studies
PLATYPUS Neutron reflectometer Polarised-neutron options 2009 [17] [18]
aAdditional details of each instrument can be found at [19]; bAccessible on an ad hoc basis;
cAnticipated
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VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
ECNS 2015 by Dr Jason Gardner. SIKA is now operated by the National Synchrotron
Radiation Research Center (NSRRC), Taiwan. The NSRRC team [20] at ANSTO is not just
an outstation but is in many respects an integral part of the neutron-scattering program at
ANSTO. A polarised-neutron capability using 3He spin filters is currently being introduced
on five instruments - PELICAN, QUOKKA, SIKA, TAIPAN, and WOMBAT - and added as
an option to the capability already possible using polarising super-mirrors on PLATYPUS.
Observation of the first scattered neutrons is an exciting time for the instrument construction
teams, and figure 2 shows the first results from the most recently commissioned instruments or
capabilities.
The high-resolution powder diffractometer, ECHIDNA, with 51 papers in 2014, has now
achieved a publication rate amongst the world’s best comparable instruments, and several other
OPAL instruments are not far behind in such comparisons.
There is space for several additional instruments in the present guide hall, mostly by
installation or extension of one each of additional thermal and cold neutron guides, the exact
number of instruments depending on the types finally installed. There is also space directly
opposite the present guide hall for a second guide hall, and for installation of a hot source if user
demand warrants it. Just as for the first suite of instruments, the choice of additional instruments
will be made in close consultation with the potential user base [21]. Such an approach has been
fully vindicated by the consistent over-demand for beam time on the existing instruments.
The Bragg Institute currently includes the National Deuteration Facility (NDF), which
produces a range of deuterated molecules, including lipids, proteins, biopolymer, aromatics,
detergents, and sugars, principally for diffraction, SANS, and reflectometry experiments. The
NDF also produces samples for other research techniques, such as NMR, and to study the effect
of isotopic substitution itself on properties [24]. There is also a small computing cluster and
limited atomistic-modelling support, as well as X-ray small-angle scattering and reflectometry
instruments to complement the neutron user program, and most recently a Physical Properties
Measurement System (Quantum Design Inc.).
The main commercial use of neutron beam time is for strain scanning of large pipes,
rail components, and welds in general, with a growing interest in strain analysis of additive
manufacturing, and radiography of cement samples. An interesting observation from our
industrial program is that smaller companies are keen to advertise their use of the neutron-
beam instruments to validate their work or process. The Bragg Institute Industrial Liaison
Office [23] coordinates industrial activities, including products like deuteration at the NDF and
software, in addition to neutron beam time.
3. Recent scientific highlights
Each set of authors of overviews of the OPAL neutron-beam instruments brings their own slant.
Being the current research leaders in the Bragg Institute we focus on a small selection of the
science that the new capabilities explore with emphasis on the instrumentation where OPAL is
at the forefront and on topical regional applications.
3.1. ’Dynamic’ sample environment
WOMBAT was the scene for the world’s first in situ operando experiments on a functioning
battery just five years ago [25], and ANSTO continues to play a leading role in in situ neutron
diffraction on Li-ion batteries, producing 46% of the publications worldwide in this area since
then.
’Dynamic’ in situ experiments of a softer kind have also been pioneered by adapting a Rapid
ViscoTM analyser to QUOKKA to study simultaneously structural and viscosity changes during
cooking of starch[26], diffraction studies of crystallisation of the triglyceride, tripalmitin, under
shear force using a rheometer on WOMBAT, and simultaneous differential scanning calorimetry
4
VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
(a) (b) (c)
(d) (e) (f)
(g) (h) (i)
Figure 2: First results from the latest tranche of neutron-beam instruments or capabilities at
OPAL: a) Quasi-elastic neutron scattering from 9.1% proline in H2O/D2O on PELICAN [22];
b) Laue pattern from TbMn2O5 on JOEY; c) Crystal-field excitation from PrFeO3 recorded on
SIKA; d) Radiograph of an alarm clock on DINGO; e) Extension of the Q range in small-angle
scattering to 4 x 10−5 Å−1 enabled by KOOKABURRA; f) Small-angle scattering from silver
behenate on BILBY; g) Energy-transfer resolution on EMU determined by an energy scan from
polyvinyl chloride; h) Vibrational density-of states spectrum for octane from the Be-filter option
on TAIPAN; i) Polarisation analysis in the magnetic phase of a multiferroic single-crystal sample
using a 3He spin filter on WOMBAT.
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VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
(DSC) and SANS on QUOKKA [27]. The signal in the last experiments, which monitored the
periodicity of generally incommensurate lamellar structures of a binary blend of alkane molecules
of different length, was enhanced by deuteration of one of the alkanes to give a considerable
contrast advantage over similar studies with X-rays.
3.2. Chemical crystallography
With the regrettable withdrawal of the pioneering thermal-neutron Laue diffractometer,
VIVALDI [28], from the user program at the Institut Laue-Langevin, KOALA, essentially a
clone of VIVALDI, is now the sole reactor-based thermal-neutron Laue diffractometer accessible
to external users, yet is leading the world in application of neutron diffraction to the study of
challenging hydrides [9]. One surprising recent example is the 28 copper 15 hydride Chinese
puzzle molecule found to form when certain copper compounds are mixed with a hydride of
boron [29]. This new structure has alternating layers of hydride and copper wrapped in an outer
shell of protecting dithiocarbamate molecules, and is much more stable than many other hydride
compounds, which has promising implications for nanoparticle formation.
3.3. Spintronics
Not surprisingly, magnetism is a common theme on the majority of instruments, with transition-
metal and rare-earth magnetism in bulk samples being strong favourites. There is also a
growing effort in studies of thin-film magnetism, exploiting the tunability allowed by doping,
strain, and proximity effects, of properties of importance for real applications. Reflectometry on
PLATYPUS and diffraction on TAIPAN are the favoured techniques, often aided by structural
characterisation using the in-house X-ray reflectometer. Recently, diffraction experiments
on TAIPAN revealed that thin films of SrCoO3−δ on a DySrO3 substrate, which provides
large epitaxial linear strain, undergo a strain-induced ferromagnetic-to-antiferromagnetic phase
transition unlike similar films on the better-lattice-matched SrTiO3 substrates [30]. Films as
thin as 20 nm, a new record for successful neutron diffraction experiments, were necessary to
maintain the strain through the film.
3.4. Granular materials
Granular materials are a unique form of matter that can act in a similar manner to a solid,
liquid, or gas, depending on the circumstances. In quasi-static systems their ability to flow and
support static shear stress provides for interesting physical behaviour. The constitutive response
of granular materials is highly non-linear and incremental (historical) and has provided an active
area of study for physicists and engineers for hundreds of years. Far from being of purely
academic interest, the ability to model the response of granular materials is of high relevance
to the handling of bulk commodities such as coal (4.72 tonnes ’flow’ through Newcastle in New
South Wales, Australia, each second), cereal grains, and mineral sands.
The full triaxial stress state within individual particles in a monodisperse spherical granular
assembly has recently been measured for the first time [31]. This was made possible by
neutron imaging and computed tomography on DINGO combined with neutron diffraction strain
measurement techniques and associated stress reconstruction using KOWARI. The assembly in
question consisted of 549 precision steel ball bearings under an applied load of 85 MPa in a
cylindrical die. Clear evidence of force chains was observed in terms of both the shape of the
probability distribution function for normal stresses and the network formed by highly loaded
particles.
3.5. Imaging ancient Australian fauna
One could be forgiven for thinking that Australian fauna still hark back to the days of dinosaurs,
but it is little appreciated that real dinosaurs did roam the southern continent and that there
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VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
exist several quite important dig sites. The most significant of these are around Winton in
outback Queensland, where the first bones were unearthed just 12 years ago. Ada Klinkhamer
and David Elliot of the Australian Age of Dinosaurs Museum in Winton have been working
with the DINGO scientist, Joseph Bevitt, to explore the possibilities of neutron radiography for
non-invasive examination of rocks from the Winton area to detect ancient fossils. It can be hit
or miss, but occasionally beautiful images like that in figure 3 can be teased out.
4. Instruments of communication: Public outreach
ANSTO is very conscious of the need to communicate our scientific and commercial activities
to the general public. The external-communications group and our Discovery Centre are very
proactive in outreach to the general public, having stalls at local fairs and celebration days,
sponsoring groups from ANSTO in local charity sporting events, and conducting tours of the
site including visits to the viewing platform overlooking the reactor guide hall. Figure 4 shows
a recent billboard advertisement, and similar advertisements were posted on local bus shelters
and on buses themselves.
Figure 3: Non-invasive neutron radiogra- Figure 4: A Sutherland Shire billboard
phy on DINGO reveals the outline of To- inviting the general public to visit ANSTO
rynomma quadrata, a cretaceous crab. and the neutron-beam facilities.
Several groups of school classes, or community groups such as senior citizens, visit the site
each week day, and the general public can register for guided tours on Saturdays. Annually,
there are over 15,000 such visitors, with 11,000 in school excursions. The net result is that the
nuclear-based activities at ANSTO are predominantly seen in a favourable light by the general
public, and with considerable pride by the citizens of Sutherland Shire, where ANSTO is located.
The communications group also aids ANSTO scientists to create media and demonstration
tools, such as the recent video that shows how EMU works [32] and a LEGO robotics model of
TAIPAN [33], the latter in collaboration with Macquarie University.
5. Conclusions
The combination of state-of-the-art instrumentation, support facilities, expert scientific staff,
and enthusiastic users of OPAL has yielded an impressive series of scientific results, as
well as a fledgling industrial programme. The Bragg Institute’s scientific projects are
effective interfaces with the user community, have international impact, and often local public
appeal. With currently 13 neutron-scattering instruments in the user programme, including a
radiography/tomography instrument, all run by very expert, talented scientists and engineers,
ANSTO is well on the way to achieving its commitment to make OPAL one of the top three
research reactors for neutron scattering in the world.
7
VI European Conference on Neutron Scattering (ECNS2015) IOP Publishing
Journal of Physics: Conference Series 746 (2016) 012001 doi:10.1088/1742-6596/746/1/012001
Acknowledgments
We gratefully acknowledge the skill and commitment of all ANSTO staff, especially those in the
Bragg Institute, that have led to the success of the neutron-scattering program at OPAL. We
especially thank the researchers, whose work we have highlighted here, as well as the staff of the
ANSTO external communications group, in particular Chris Wensrich (University of Newcastle,
NSW), Wei Kong Pang (University of Wollongong), Rod Dowler (ANSTO communications), and
Anna Paradowska and Joseph Bevitt (both ANSTO, Bragg Institute) who generously provided
material for presentation at ECNS 2015. We also acknowledge partial funding of the NDF
and part of the neutron instrument suite by the National Collaborative Research Infrastructure
Strategy of the Australian Government.
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