Browsing by Author "Booth, N"
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- ItemACNS sample environment update(Australian Nuclear Science and Technology Organisation, 2021-11-25) White, R; Davidson, G; D'Adam, TM; Booth, N; Baldwin, C; Shumack, ASince the last ANSTO User Meeting the sample environment group at ACNS has supported our facility users with a range of unique developments and set ups. We have had a change in structure with the laboratory group forming and working alongside us. We will report on the progress on our ongoing projects on Direct Laser Melting (DLM) deposition system co-funded by a NSW RAAP grant. Also underway are LIEF grants with equipment for use at ACNS, one includes a rheometer for use on ACNS beam instruments. This presentation will also cover our new equipment projects funded by the NCRIS RIIP scheme. This includes new cryofurnaces, a new type of furnace, a universal testing machine and other equipment. This funding will maintain and improve our existing capabilities and increase the redundancy across the SE suite to better service competing requests. © The Authors
- ItemAdvanced sample environment support for neutron instruments at the Bragg Institute, ANSTO(Australian Institute of Physics, 2016-02-04) Imperia, P; Booth, N; Lee, S; D'Adam, TM; Manning, AGOver the last few years a number of advancements have been made in sample environments available to scientists visiting the Neutron Beam Facility run by the Bragg institute at ANSTO (Lucas Heights). Conventional sample environment equipment allows experiments to be carried out from 35mK to 1700K, magnetic fields up to 12T and electric fields up to 10kV. These extremes are not available on all neutron instruments nor with one piece of equipment. However combinations of temperature, magnetic and electric fields are also possible. These conventional sample environments will not be covered here. This presentation will outline advances made in the gas handling, vapour delivery, differential scanning calorimetry (DSC) and spectroscopy at extreme temperatures all carried out simultaneously with neutron data collection. Some examples of the complimentary data collected are also presented. Our automated gas handling system allows gas mixing (up to 4 gases), dosing (volumetric Sievert analysis) up to 200Bar, gas flow and molecular analysis with a dedicated mass spectrometer for kinetics investigations. The Hiden Isochema system is based on their commercial IMI system with the standard reaction chamber removed and replaced by thermalised capillary lines to allow the gas delivery to a sample reactor placed within a cryostat or furnace on the sample stage of our neutron instruments. Two options are available for vapour delivery. For samples that do not outgas a static system can be used where computer controlled valves control the vapour pressure. One valve is used to lower the pressure using a turbo pump and the second one to allow the vapour from the reservoir to increase the vapour pressure. Any non-corrosive liquid can be used in this system. The second vapour system, dynamically controls the vapour and dry gas flow allowing mixing of two vapours and a dry stream of gas or the recirculation of a saturated vapour through a sample reactor The DSC system is based on A Mettler Toledo model DSC1. The furnace has been moved to allow the passage of the neutron beam and Bragg designed crucibles are used to allow scattering experiments to be carried out while DSC data are collected. Quartz and Aluminium crucibles are available and temperature range of 550C to -100C is achievable. Using Ocean Optics spectrometer equipment we have successfully carried out NIR spectroscopy down to 4K while collecting Neutron diffraction data. The use a standard NIR reflection probe and modification of the cryostat sample stick allows the probe to be introduced into the cryostat. A second spectrometer is available for UV-Vis spectroscopy and can be used in a similar method. These spectrometers are also available for use on other scattering instruments over a limited temperature range.
- ItemAustralian centre for neutron scattering: sample environment report(Australian Institute of Nuclear Science and Engineering (AINSE), 2018-11-19) Manning, AG; Wakeham, D; Davidson, G; Booth, N; Imperia, P; White, R; Lee, S; D'Adam, TMIn the past 2 years since the 2016 AANSS symposium, the sample environment group of the Australian Centre for Neutron Scattering (ACNS) has continued to facilitate neutron experiments and expand sample environment capability. This report will present the current sample environment and laboratory facilities and recent developments. We have made progress in light irradiation and spectroscopy developments; on a new temperature controlled multi-sample changer with tumbling capability; on a rotational PE Cell; and on new sample probes made from composite materials. Other improvements include new high pressure couplings for helium compressors and modifications to a dilution insert to allow larger samples and use in other cryostats extending the capability. Ongoing major projects are a new superconducting split-coil magnet dedicated to SANS and TOFPAS, two new cryostats (1.5 K to 800 K temperature range) with the aim of halving the system and sample cooling time and a new dilution fridge that will allow top-loading of samples and the ability to take much larger samples than the existing dilution insert. There have also been staffing changes with previous Sample Environment Group Leader, Paolo Imperia moving into the Operations Manager position. The new group leader, Rachel White, was recently appointed. Our Laboratory Manager, Deborah Wakeham, joined us in July 2017. © The Authors.
- ItemBlack hydrogenated titanium dioxide(Australian Institute of Physics, 2013-02-06) Imperia, P; Aldus, RJ; Booth, N; Muir, J; Jovic, V; Waterhouse, GNot available
- ItemCalibration of temperature controllers and sensors(Australian Institute of Nuclear Science and Engineering, 2016-11-29) Manning, AG; Booth, N; Imperia, PReliable temperature measurements are a key part of many sample environment setups for neutron scattering experiments. This typically requires the use of both a temperature sensor and temperature controller. It is often desirable to be able to perform a continuous measurement spanning a wide range of temperatures, however the choice of suitable sensors is limited. Rhodium iron (RhFe) resistive thermometers are best suited to the temperature range of our cryofurnaces (1.5 to 800 K), however their calibration is known to drift when exposed to elevated temperatures. Here, we will present procedures to ensure that both the controller and sensor used in such experiments are performing optimally. Calibrated resistors, which can mimic the behavior of a temperature sensor fixed at a particular temperature, can be used to check the calibration of the readings given by temperature controllers such as Lake Shore 336/340 or Oxford Instruments iTC units. If the controllers are known to be operating to the tolerances specified by their manufacturer, then we can have confidence in the measurements that they make. We can then use our newly verified controllers to assess the performance of RhFe sensors over a range of temperatures from 4 to 800 K in a custom-built calibration rig. This allows us to quantify the behavior of the sensors after they are subject to high temperatures, and to account for shifts in their readings. Using this procedure, we can ensure that the sensors remain reliable after prolonged operational use.
- ItemCurrent high-pressure capabilities at ACNS and future plans(Australian Institute of Nuclear Science and Engineering (AINSE), 2020-11-11) Maynard-Casely, HE; Booth, N; Shumack, A; Baldwin, C; White, R; Rule, KC; McIntyre, GJ; Novelli, GHigh-pressure (>1 Kbar) is a marvellous variable, which can reveal mechanical properties, structural transitions and exotic behaviours. This pairs very well with neutron scattering, where the highly penetrating nature of neutron beams is idea for accessing sample within complex sample environments. The Australian Centre for Neutron Scattering (ACNS) has developed a number of capabilities for high-pressure experiments, mainly revolving around the use of our Paris-Edinburgh press but more recently with miniature diamond-anvil cells. Some of these, such as our ability to compress radioactive samples as well as combining high-pressure and high-electric fields are unique in the world. Here we review the high pressure capabilities at ACNS, and outline some directions for capabilities and measurements.
- ItemDesign and implementation of a differential scanning calorimeter for the simultaneous measurement of small angle neutron scattering(IOP Science, 2014-04-08) Pullen, SA; Booth, N; Olsen, SR; Day, B; Franceschini, F; Mannicke, F; Gilbert, EPFor almost 30 years, at synchrotron facilities, it has been possible to perform small-angle x-ray scattering experiments whilst simultaneously measuring differential scanning calorimetry (DSC). However, a range of challenges exist to enable the collection of simultaneous small-angle neutron scattering (SANS) and DSC data associated not only with intrinsic flux limitations but also scattering geometry and thermal control. The development of a DSC (temperature range ca. −150 ◦C to 500 ◦C) suitable for SANS is detailed here and its successful use is illustrated with combined measurements on a binary blend of normal alkanes in which one component has been deuterium labelled. © 2014, IOP Publishing Ltd
- ItemDevelopment of Direct Laser Melting (DLM) deposition system for in-situ use on neutron beam instruments(Australian Institute of Nuclear Science and Engineering (AINSE), 2020-11-11) Baldwin, C; White, R; Paradowska, AM; Booth, N; Davidson, G; D’Adam, TM; Shumack, A; Darmann, FDirect Laser Melting (DLM) deposition is an additive manufacturing technique in which a high power laser is used to create a melt pool on a workpiece while a jet of metal powder is applied, resulting in localised material deposition. This technique is used in industry for additive repairs, cladding with dissimilar metals, or, in conjunction with a CNC milling machine, as a full-fledged 3D additive fabrication platform. As the prominence of this technology rises, so too does interest in characterising deposition dynamics over a vast parameter space. Neutron beam instruments offer unique capabilities for such characterisation. As part of the NSW Research Attraction and Acceleration Program, ACNS is developing world first sample environment capabilities enabling in-situ laser metal deposition, for use on KOWARI and DINGO beamline. The system will utilise a self-contained motion stage and laser cladding head which will construct a thin wall structure on a user specified substrate, utilising up to two metal powders at a time. Neutron studies of the melt pool or heat affected zone can then be performed during and after printing. This paper will present the technical specifications and capabilities of the system, which will be available to the user community in late 2021. © The authors.
- ItemFirst application of simultaneous sans and differential scanning calorimetry: microphase separated alkane blends(International Conference on Neutron Scattering, 2017-07-12) Pullen, SA; Booth, N; Olsen, SR; Franceschini, F; Mannicke, D; Gilbert, EPThe combination of small-angle x-ray scattering experiments with simultaneous measurement of phase transitions using differential scanning calorimetry (DSC) has become common-place. However, no such facility existed, until recently to enable the simultaneous measurement of DSC and small angle neutron scattering (SANS). DSC data complements SANS by providing first and second order phase transition temperatures and, with appropriate calibration, the magnitude and sign of associated enthalpy changes due to these phase transitions. A range of challenges have been addressed to enable the collection of simultaneous SANS and DSC data associated not only with intrinsic flux limitations but also scattering geometry, thermal control and synchronisation of the DSC and SANS data. The development of a DSC suitable for SANS is detailed here which, to our knowledge, is the first and only one of its kind. The resulting instrument has a temperature range of -50?C to 500?C and a furnace geometry that allows access to the full q range of QUOKKA, at the OPAL reactor to be reached. The DSC-SANS was first used to investigate the behaviour of binary mixtures of normal alkanes which is presented here although several further successful experiments have been carried out since on range of soft and hard condensed matter samples.
- ItemIntegration of polarised 3He infrastructure with sample environment equipment(Australian Institute of Physics, 2017-01-31) D'Adam, TM; Booth, N; Davidson, G; Lee, S; Manning, AG; Timperon, N; Imperia, PMany challenges exist when attempting to integrate polarised 3He infrastructure with neutron beam instruments. This is often due to its sensitivity to the magnetic environment and also due to the compact geometry of many beam lines. One additional consideration is the effect that Sample Environment equipment can have on the functionality of a particular polarised neutron setup. We have been able to provide incident beam polarisation with two separate magnets providing fields at the sample position of up to 2 T. In addition, full polarisation analysis is possible over a temperature range of 30 mK to 800 K. To enable this, some pieces of Sample Environment equipment must be designed specifically for use with polarised 3He and in many cases modifications are necessary to accommodate the sensitive gas. We are also in the process of procuring an 8 T shielded asymmetric magnet suitable for use with polarised 3He infrastructure.
- ItemNeutron optics upgrades to the residual stress diffractometer, KOWARI(Materials Research Forum LLC, 2016-07-03) Reid, M; Olsen, SR; Luzin, V; New, M; Booth, N; Clowes, D; Nguyen, T; Franceschini, F; Ogrin, A; Pangelis, S; Paradowska, AM; Larkin, N; Pan, Z; Hoye, N; Suzuki, HIn the last 5 years a number of significant enhancements have been implemented on the neutron beam strain scanner Kowari at the OPAL reactor in Sydney Australia. These changes have resulted in reduced beam time losses when conducting experiments due to sample and stage alignment, and optics and sample changes. There have been 3 projects, starting in 2011 with a new manual slit system design and collision recovery system, in 2013 with a series of radial collimators and finally with the delivery. © The Authors
- ItemNeutron scattering quantification of unfrozen pore water in frozen mud(Elsevier, 2021-09) Gates, WP; Bordallo, HN; Bouazza, A; Carnero-Guzman, GG; Aldridge, LP; Klapproth, A; Iles, GN; Booth, N; Mole, RA; Seydel, T; Yu, DH; de Souza, NRThe Earth's polar regions are experiencing a greater frequency of freeze-thaw events throughout the polar summer, contributing to atmospheric methane and destabilising clay-rich sediments. Clays in soils tightly bind pore water and thus substantially modify freeze-thaw events. While temperatures of phase transitions for confined pore water may be precisely assessed using calorimetric or thermal analyses to −30 or −40 °C, neutron scattering directly probes how pores in clay minerals control ice formation and melting to lower temperatures. We apply elastic neutron scattering to accurately quantify the unfrozen water content of clay gels and unambiguously identify different pore-water environments by their freezing temperatures. Using this approach, we conclude that cryosuction controls water mobility in frozen soils in the absence of soluble salts to much lower temperatures than observed by other techniques. Dyanmics determined from neutron scattering indicates that water in clay gel pores thaws at much lower temperatures than currently considered, and thus pose potential risks for contaminant migration at sub freezing temperatures. The general poor strength of wet clays can significantly impact infrastructure in cold regions undergoing an increased frequency of freeze-thaw events. © 2021 Elsevier Inc.
- ItemNew sample environment projects and developments at the Australian Centre for Neutron Scattering(Australian Institute of Physics, 2019-02-05) White, R; Imperia, P; Booth, N; D'Adam, TM; Davidson, G; Lee, S; Manning, AG; Tobin, SSince the 2018 meeting the sample environment team at the Australian Centre for Neutron Scattering (ACNS) has progressed the design and construction of the new superconducting split-coil magnet, a fast cooling closed cycle cryostat and a new type of closed cycle dilution refrigerator. The first of the two fast cooling cryostats (compact closed cycle dry cryostats, 1.5 K to 800 K) will arrive in early 2019, with a tested sample cool down of 30 minutes. The new magnet is in the final stages of design, including a sample well for our time-of-flight spectrometer PELICAN. The new magnet will have active magnetic shielding and an asymmetric coil design to allow experiments with polarised neutrons. The expected arrival for the magnet is mid-2019. The closed cycle dilution refrigerator will have high cooling power and a very large sample space allowing a new class of experiments with neutrons at ultra-low temperature, arriving in March 2019. Also presented is the development of carbon fibre sample probes to enable faster cooling and quicker sample changes.
- ItemNew sample environment projects and developments at the Australian Centre for Neutron Scattering(International Conference on Neutron Scattering, 2017-07-12) Imperia, P; Booth, N; D'Adam, TM; Davidson, G; Lee, S; Manning, AGThe sample environment team at the Australian Centre for Neutron Scattering (ACNS) has been recently awarded funding for a new superconducting split-coil magnet, a fast closed cycle cryostat and a closed cycle dilution refrigerator of the latest generation. The new magnet design is of particular interest; the brief is complicated by the request to serve two separate classes of instruments: small angle scattering and time of flight. The magnet will have low fringe field, active shield design, and specific requirements for the asymmetric field gradient to allow experiments with polarised neutrons. Low fringe field values are combined with a minimum central field of 7 Tesla, wide “clean” scattering angle and dimensional and weight constraints. The design challenges and possible solutions will be detailed, together with a time frame for delivery and commissioning. The new compact closed cycle cryostat (1.5 K to 800 K) with a small He dump, aims to halve the system and sample cooling time, generating performances comparable to that of wet type “orange” cryostats without the necessity to refill with cryogenic liquids. The closed cycle dilution refrigerator will have high cooling power and large sample space, allowing new class of experiments with neutrons at ultra-low temperature. The most recent equipment built in-house and unique to the ACNS, such as the Peltier sample changer and the thermalised sample tumblers for SANS and USANS, will also be discussed.
- ItemNew sample environment projects and developments at the Australian Centre for Neutron Scattering.(Australian Institute of Physics, 2018-01-30) Imperia, P; Booth, N; D'Adam, TM; Davidson, G; Lee, S; Manning, AG; Tobin, S
- ItemNovel non destructive sample analysis techniques using neutron scattering(Engineers Australia, 2014-01-01) Olsen, SR; Gilbert, EP; Booth, N; Pullen, SA; Imperia, P; Peterson, VK; Garbe, U; Luzin, V; Paradowska, AM; Studer, AJ; Liss, KDIn late 2006 the new 20MW Open Pool Australian Light Water Reactor (OPAL) went critical for the first time. Since 2007 thousands of scientists and engineers have used the neutron beam instruments to perform a wide range of non-destructive studies of samples covering physics, chemistry, biology, engineering and materials science. Neutrons provide a wealth of information about the state of materials including structure, residual stress, magnetic properties and dynamic properties. As neutrons scatter from nuclei and not electrons, they are highly penetrating, capable of travelling tens of millimeters into most metals. Neutrons behave, for to some extent, like tiny bar magnets and therefore can be used to investigate the magnetic properties of materials such as superconductors and computor memories. Recent engineering studies - often undertaken in situ at industrially relevant conditions - include railway sleepers, turbine blades, polymer processing, lithium battery testing, and titanium alloys. © 2021 Informit
- ItemA peltier controlled sample changer for SANS(Australian Institute of Nuclear Science and Engineering, 2016-11-29) Lee, S; Booth, N; Imperia, P; Davidson, GA twelve position sample changer for SANS instruments at ACNS has been developed and will be available for users in the near future. The design philosophy for this project was to make the system as modular and scalable as possible with an emphasis on ease of use for the user and reduced background. The Peltier control system allows each sample to be controlled at different temperatures and allows the possibility of producing very fast temperature changes over a limited range. The system can be controlled via a local Watlow™ touchscreen and remotely via the SICS based neutron instrument control system used at ACNS. The liquid cooled heatsink for the Peltiers provides the support for the spring loaded sample holders, allowing rapid sample changes. The width of the sample changer has been reduced compared to the existing 20 position and with Borated aluminium shielding the background with blocked beam has been improved. The temperature sensors used are K-type thermocouples. Performance and stability tests will be presented. A design for uSANS is being developed.
- ItemRheo-ND: temperature and shear induced crystal transformation of a model triglyceride observed using neutron diffraction(Australian Institute of Nuclear Science and Engineering (AINSE), 2018-11-19) Maynard-Casely, HE; Stuart, BH; Booth, N; Thomas, PSRheo-SANS (rheology and small angle neutron diffraction) is now a well-established technique to probe the shape and size of particles under different shear and temperature regimes [1]. Recent work on WOMBAT [2], the high intensity neutron diffraction instrument at the Australian Centre for Neutron Scattering, has successfully combined rheology and neutron diffraction. This was used to follow the crystalline phase transformations in a model (deuterated) triglyceride. The initial impetus for this work was part of a forensic investigation [3] linking the crystallisation of triglycerides under high shear rates that are encountered in motor vehicle accidents. However now the technique has been demonstrated it may be of interest to investigate crystallization due to shear in other organic systems. Figure 1 - Diffraction data collected from the shear cell during cooling and shearing at 1000 s-1, colours give the intensity of the diffraction pattern (left axis) and the black squares chart the measured viscosity (right axis). This demonstrates the ability to track crystallisation in situ under high shear rates. The high neutron flux and detector efficiency available at WOMBAT is instrumental in allowing diffraction patterns to be collected from the small sample volumes available in the Couette cell geometry. The Couette cell used has a sample gap of 1mm and was mounted tangentially to the neutron beam. The shear rate applied to the sample can be varied over a range of 10-2500 s-1 and the temperature can be controlled using an external water jacket from between -10 and 80 ⁰C. We invite other researchers who are interested in this capacity to contact us about possible experiments. © The Authors.
- ItemSmall punch test of LC4/SiCP metal matrix composites(Trans Tech Publications, 2010-09-17) Mak, J; Wuhrer, R; Humphries, SR; Booth, N; Heness, G; Yeung, WY; Wei, T; Qin, JN; Ouyang, QB; Zhang, DThere have been growing demands of high performance metal matrix composites in advanced engineering applications in virtue of their high specific strengths. This paper is to report an assessment of the mechanical properties of LC4/SiCp metal matrix composites using an innovative testing technique, small punch test. The composite materials of this study were produced by stir casting method with particulate reinforcements of 7wt.% and 14wt.% of SiC respectively. Small punch testing was performed on the LC4 base alloy and the two composites materials. The small punch test is a relatively new mechanical testing technique capable of utilizing small disk-shaped samples to determine the mechanical properties of the test materials. In this study, the equivalent fracture strain, εqf of the LC4/SiCp MMCs was characterised and compared with the base alloy. The fracture mechanism of the test samples was examined using scanning electron microscopy. © Trans Tech Publications Ltd.
- ItemThree impossible things before lunch - the task of a sample environment specialist(IOS Press, 2017-11-16) Booth, N; Davidson, G; Imperia, P; Lee, S; Stuart, BH; Thomas, PS; Komatsu, K; Yamane, R; Prescott, SW; Maynard-Casely, HE; Nelson, A; Rule, KCIn the course of their day, sample environment professionals can be confronted by numerous technical challenges applicable to a range of scientific questions. This paper presents three successful outcomes from user-posed sample environment challenges for in situ neutron scattering experiments undertaken at the Australian Centre for Neutron Scattering (formerly the Bragg Institute). The sample environments presented here have nothing in common other than their novelty. They may not be the best solution but have been constrained by time, resources and ability. The questions the users posed were: Can we mount a cylinder in cylinder (CIC) rheometer, more regularly used on a small angle scattering instrument, on a diffraction instrument and obtain usable data? Can we supply high-voltage (up to 10 kV) across a sample within the Paris–Edinburgh press while mounted on a powder diffraction instrument? And finally can a Lakeshore 340 and an in-house built liquid conductivity cell do the job of a commercial liquid conductivity meter? This paper presents the engineering and equipment solutions that were used to answer these questions, and in each case the scientific users left with useful, intriguing and, hopefully, publishable data. © 2017 IOS Press