Browsing by Author "McIntyre, GJ"

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    18O isotope substitution on the multiferroic compound DyMnO3
    (Australian Institute of Physics, 2013-02-06) Narayanan, N; Li, F; Hutchison, WD; Reynolds, NM; Rovillain, P; Ulrich, C; Hester, JR; McIntyre, GJ; Mulders, AM
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    The 1st ANSTO-AINSE Workshop on Nuclear Techniques for Cultural Heritage
    (Taylor & Francis Online, 2019-05-24) Salvemini, F; White, R; McIntyre, GJ; Bevitt, JJ; Cubbin, K
    No abstract available.
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    2nd Asia-Oceania Instrument Scientist Workshops, Manly, July 19, 2015
    (Taylor & Francis Online, 2015-11-17) Hester, JR; Holt, SA; Imperia, P; Piltz, RO; Rehm, C; Rule, KC; Mole, RA; McIntyre, GJ
    No abstract available
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    A (3 + 3)-dimensional “hypercubic” oxide-ionic conductor: type ii bi2o3–nb2o5
    (ACS Publications, 2013-04-09) Ling, CD; Schmid, S; Blanchard, PER; Petříček, V; McIntyre, GJ; Sharma, N; Maljuk, A; Yaremchenko, AA; Kharton, VV; Gutmann, MJ; Withers, RL
    The high-temperature cubic form of bismuth oxide, δ-Bi2O3, is the best intermediate-temperature oxide-ionic conductor known. The most elegant way of stabilizing δ-Bi2O3 to room temperature, while preserving a large part of its conductivity, is by doping with higher valent transition metals to create wide solid-solutions fields with exceedingly rare and complex (3 + 3)-dimensional incommensurately modulated ?hypercubic? structures. These materials remain poorly understood because no such structure has ever been quantitatively solved and refined, due to both the complexity of the problem and a lack of adequate experimental data. We have addressed this by growing a large (centimeter scale) crystal using a novel refluxing floating-zone method, collecting high-quality single-crystal neutron diffraction data, and treating its structure together with X-ray diffraction data within the superspace symmetry formalism. The structure can be understood as an ?inflated? pyrochlore, in which corner-connected NbO6 octahedral chains move smoothly apart to accommodate the solid solution. While some oxide vacancies are ordered into these chains, the rest are distributed throughout a continuous three-dimensional network of wide δ-Bi2O3-like channels, explaining the high oxide-ionic conductivity compared to commensurately modulated phases in the same pseudobinary system. © 2013, American Chemical Society.
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    37th Annual Condensed Matter and Materials Meeting Wagga 2013
    (Australian Institute of Physics, 2013-02-05) McIntyre, GJ; Mole, RA
    The 37th Annual Condensed Matter and Materials Meeting was held at Charles Sturt University, Wagga Wagga, NSW from 5th – 8th February, 2013. There were 88 attendees, including international visitors from Singapore, Brazil, Turkey and Germany. A total of 11 invited and 18 contributed oral papers were presented during the two and one half days of scientific sessions. There were also two sessions with a total of 53 poster presentations. All presenters were invited to submit a manuscript for publication in the conference proceedings. Each manuscript was refereed by at least two anonymous reviewers who worked to a set of guidelines made available by the editors. Each accepted publication therefore satisfies the requirements for classification as a refereed conference publication (E1). The organizers would like to thank the 25 reviewers for their time and effort in reviewing manuscripts, which resulted in 14 papers being accepted for publication. The accepted manuscripts are available at the on-line publication section of the Australian Institute of Physics national web site (http://www.aip.org.au/).
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    4-phenoxyphenol: a porous molecular material
    (American Chemical Society, 2012-04-01) Thomas, LH; Cheung, E; Jones, AOF; Kallay, AA; Lemée-Cailleau, MH; McIntyre, GJ; Wilson, CC
    4-Phenoxyphenol is a simple organic molecule that crystallizes as a porous material with channels running throughout the structure. The channels are constructed by a 6-fold hydrogen bonded ring and can host solvent molecules incorporated during crystal growth, with a minimum channel diameter of 5.8-5.9 angstrom; each channel usually contains a single solvent molecule per unit cell. The hydrogen bonded ring shows surprising flexibility, being able both to breathe and to sustain its crystalline integrity even when grown with empty pores. This is particularly surprising given that the remainder of the interactions within the crystal structure are C-H center dot center dot center dot pi interactions and are weak in nature. It is also possible to grow "dry" porous 4-phenoxyphenol crystals by using a bulky solvent in the recrystallization. © 2012, American Chemical Society.
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    Accurate H-atom parameters for the two polymorphs of L-histi­dine at 5, 105 and 295 K
    (International Union of Crystallography, 2021-10-01) Novelli, G; McMonagle, CJ; Kleemiss, F; Probert, MR; Puschmann, H; Grabowsky, S; Maynard-Casely, HE; McIntyre, GJ; Parsons, S
    The crystal structure of the monoclinic polymorph of the primary amino acid L-histi­dine has been determined for the first time by single-crystal neutron diffraction, while that of the orthorhombic polymorph has been reinvestigated with an untwinned crystal, improving the experimental precision and accuracy. For each polymorph, neutron diffraction data were collected at 5, 105 and 295 K. Single-crystal X-ray diffraction experiments were also performed at the same temperatures. The two polymorphs, whose crystal packing is interpreted by intermolecular interaction energies calculated using the Pixel method, show differences in the energy and geometry of the hydrogen bond formed along the c direction. Taking advantage of the X-ray diffraction data collected at 5 K, the precision and accuracy of the new Hirshfeld atom refinement method im­ple­mented in NoSpherA2 were probed choosing various settings of the functionals and basis sets, together with the use of explicit clusters of molecules and enhanced rigid-body restraints for H atoms. Equivalent atomic coordinates and aniso­tropic displacement parameters were com­pared and found to agree well with those obtained from the corresponding neutron structural models.© International Union of Crystallography
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    Accurate hydrogen parameters for the amino acid L-leucine
    (International Union of Crystallography, 2016-01) Binns, J; Parsons, S; McIntyre, GJ
    The structure of the primary amino acid L-leucine has been determined for the first time by neutron diffraction. This was made possible by the use of modern neutron Laue diffraction to overcome the previously prohibitive effects of crystal size and quality. The packing of the structure into hydrophobic and hydrophilic layers is explained by the intermolecular interaction energies calculated using the PIXEL method. Variable-temperature data collections confirmed the absence of phase transitions between 120 and 300 K in the single-crystal form. © International Union of Crystallography
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    The antiferromagnetic structures of IrMn3 and their influence on exchange-bias
    (Nature Publishing Group, 2013-08-12) Kohn, A; Kovács, A; Fan, R; McIntyre, GJ; Ward, RCC; Goff, JP
    We have determined the magnetic structures of single-crystal thin-films of IrMn3 for the crystallographic phases of chemically-ordered L12, and for chemically-disordered face-centred-cubic, which is the phase typically chosen for information-storage devices. For the chemically-ordered L12 thin-film, we find the same triangular magnetic structure as reported for the bulk material. We determine the magnetic structure of the chemically-disordered face-centred-cubic alloy for the first time, which differs from theoretical predictions, with magnetic moments tilted away from the crystal diagonals towards the face-planes. We study the influence of these two antiferromagnetic structures on the exchange-bias properties of an epitaxial body-centred-cubic Fe layer showing that magnetization reversal mechanism and bias-field in the ferromagnetic layer is altered significantly. We report a change of reversal mechanism from in-plane nucleation of 90° domain-walls when coupled to the newly reported cubic structure towards a rotational process, including an out-of-plane magnetization component when coupled to the L12 triangular structure. © 2013, Nature Publishing Group.
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    Area detectors in single-crystal neutron diffraction
    (IOP Science, 2015-12-01) McIntyre, GJ
    The introduction of area detectors has brought about a gentle revolution in the routine application of single-crystal neutron diffractometry. Implemented first for macromolecular crystallography, electronic detectors subsequently gradually spread to chemical and physics-oriented crystallography at steady-state sources. The volumetric surveying of reciprocal space implicit in the Laue technique has required area detectors right from the start, whether using film and more recently image plates and CCD-based detectors at reactors, or scintillation detectors at spallation sources. Wide-angle volumetric data collection has extended application of neutron single-crystal diffractometry to chemical structures, sample volumes, and physical phenomena previously deemed impossible. More than 30 of the dedicated single-crystal neutron diffractometers at steady-state reactor and neutron spallation sources worldwide and accessible via peer-review proposal mechanisms are currently equipped with area detectors. Here we review the historical development of the various types of area detectors used for single crystals, discuss experimental aspects peculiar to experiments with such detectors, highlight the scientific fields where the use of area detectors has had a special impact, and forecast future developments in hardware, implementation, and software.© 2015 IOP Publishing Ltd
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    Bi(III)-containing lanthanum germanium apatite-type oxide ion conductors and their structure-property relationships
    (Australian Institute of Physics, 2016-02-04) Tate, ML; McIntyre, GJ; Evans, IR
    Oxide ion conductors are used in a wide variety of applications, including oxygen sensors and separation membranes, but are undergoing significant study for their use in solid oxide fuel cells (SOFCs), which allow for the direct conversion of chemical to electrical energy. Apatite-type silicates and germanates, La9.33+x(TO4)6O2+3x/2 (T = Si, Ge), have exhibited high oxide ion conductivities, potentially allowing for their use in SOFCs. Apatite-type compounds have the general formula, [AI4][AII6][TO4]6X2±δ, (A = alkaline or rare earth metal, or Pb; T = Ge, Si, P, V; X = O, OH, halides) and can be thought of as comprised of a framework of AI4(TO4)6 with flexible cavities containing AII6X2 units. The structures of apatite-type materials are primarily hexagonal, with the remainder being monoclinic, with several triclinic examples known. The origin of the triclinic structure is thought to be partly due to the size differences between the units comprising the framework and those within the cavities. The inclusion of interstitial oxide ions have been shown to promote the triclinic distortion, potentially caused by further expansion of the framework. Three novel Bi(III)-containing lanthanum germanium apatite compounds (Bi2La8[(GeO4)6]O3, Bi4Ca4La2[(VO4)2(GeO4)4]O2, and Bi4Ca2La4[(GeO4)6]O2) were synthesised by a solid state synthetic method, before undergoing AC impedance spectroscopy experiments to study their electrical properties. The Bi2La8[(GeO4)6]O3 compound has been identified as being the first bismuth containing apatite with a triclinic structure, whilst the Bi4-containing compounds possess hexagonal structures. All samples show high levels of conductivity, with the triclinic sample possessing higher conductivity values than the hexagonal samples at high temperature.
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    Bi1−xNbxO1.5+x (x=0.0625, 0.12) fast ion conductors: structures, stability and oxide ion migration pathways
    (Elsevier, 2015-05) Tate, ML; Hack, J; Kuang, X; McIntyre, GJ; Withers, RL; Johnson, MR; Evans, IR
    A combined experimental and computational study of Bi1−xNbxO1.5+x (x=0.0625 and 0.12) has been carried out using laboratory X-ray, neutron and electron diffraction, impedance measurements and ab-initio molecular dynamics. We demonstrate that Bi0.9375Nb0.0625O1.5625, previously reported to adopt a cubic fluorite-type superstructure, can form two different polymorphs depending on the synthetic method: a metastable cubic phase is produced by quenching; while slower cooling yields a stable material with a tetragonal √2×√2×1 superstructure, which undergoes a reversible phase transition into the cubic form at ~680 °C on subsequent reheating. Neutron diffraction reveals that the tetragonal superstructure arises mainly from ordering in the oxygen sublattice, with Bi and Nb remaining disordered, although structured diffuse scattering observed in the electron diffraction patterns suggests a degree of short-range ordering. Both materials are oxide ion conductors. On thermal cycling, Bi0.88Nb0.12O1.62 exhibits a decrease in conductivity of approximately an order of magnitude due to partial transformation into the tetragonal phase, but still exhibits conductivity comparable to yttria-stabilised zirconia (YSZ). Ab-initio molecular dynamics simulations performed on Bi0.9375Nb0.0625O1.5625 show that oxide ion diffusion occurs by O2− jumps between edge- and corner-sharing OM4 groups (M=Bi, Nb) via tetrahedral □M4 and octahedral □M6 vacancies. © 2015 Elsevier Inc.
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    Carbon molecules in space: a thermal equation of state study of solid hexamethylenetetramine
    (Australian Institute of Physics, 2020-02-04) Novelli, G; McIntyre, GJ; Maynard-Casely, HE; Marshall, WG; Kamenev, KV; Parsons, S
    Properties such as compressibility, thermo-elasticity and the energy landscape remain unknown for many organic compounds under conditions encountered on extraterrestrial planets and moons and in space. In this study, a thermal Equation of State (EoS) for the crystalline solid hexamethylenetetramine was determined by neutron powder diffraction in the temperature and pressure ranges of 113-480 K and 0-5 GPa, respectively. The material was chosen as a molecular model for its high symmetry and its property of remaining in the same phase throughout the experimental conditions selected to simulate the planetary environments. Equations of States (EoSs) show how the thermodynamic variables of temperature (T), pressure (P) and volume (V) are inter-related. The ideal gas law, PV = nRT, is an example of an EoS which is used as a simple but effective model to explain the properties of gases. More complex EoSs, where the assumption of ideality is relaxed, can be applied to solids in order to describe how the geometry and energy transform when they experience dramatic changes in their environment. Such information acquires enormous importance in planetary materials science, where scientists are trying to understand the fate of carbon, the fourth most abundant element in our galaxy, in the context of the origin of life and planetary environments. Despite the large heterogeneity of galactic and interstellar regions, the organic chemistry of the universe seems to follow common pathways. Molecules of high astrobiological and astrophysical relevance such as amino acids, polyaromatic hydrocarbons, and N-heterocycles have been identified across the solar system, but how they behave under such varied conditions is a question yet to be answered. Key to our approach was the determination of how the internal energy (U), entropy (S) and the Gibbs free energy (G) vary with pressure not only computationally, but also, and for the first time, experimentally. A new method has been developed, able to transform directly variable-PT crystallographic data into thermodynamic information. Although it is quite common to model thermal expansion at ambient pressure with a VTEoS, and compression at ambient temperature using a PV-EoS, determinations of PVT-EoSs are much less common, particularly for organic materials. This paucity of PTV-EoSs reflects the difficulty of varying pressure and temperature simultaneously in crystallographic experiments, especially at reduced temperatures. The task was addressed in this study by the variable-temperature insert for the Paris-Edinburgh press available on the PEARL instrument at the ISIS Neutron Spallation Source (UK). The results were successfully combined with periodic DFT (Figure 1) and other semiempirical calculations, where pressure and temperature can be included at little time cost, enabling the stability profile of the material to be understood, right down to the level of individual intermolecular interactions.
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    Chemical pressure effects on crystal and magnetic structures of bilayer manganites PrA2Mn2O7 (A = Sr or Ca)
    (AIP Publishing, 2016-06-03) Deng, G; Sheptyakov, D; Pomjakushin, V; Medarde, M; Pomjakushina, E; Conder, K; Kenzelmann, M; Studer, AJ; Gardner, JS; McIntyre, GJ
    The crystal and magnetic structures of the bilayer manganites PrSr2Mn2O7 (PSMO) and PrCa2Mn2O7 (PCMO) have been studied by neutron powder diffraction. It was found that PSMO crystallizes in space group I4/mmm, while PCMO adopts space group Cmc21 at room temperature. The difference in the structure arises from chemical pressure induced by the Ca substitution for Sr on the A sites, which causes different Jahn-Teller distortions. In PSMO, the MnO6 octahedra suffer a small elongated distortion, while those in PCMO adopt strong compressed distortion along the axial direction. In addition, the octahedra in PCMO show a+b0c0 rotation and a0b+c+ tilting in the Glazer notation in comparison to PSMO. As a result, these two compounds adopt very different magnetic structures: The magnetic structure of PSMO is an A-type magnetic structure (Im'm'm) with propagation vector k = (0, 0, 1) and magnetic moments in the ab plane. In contrast, a C-type antiferromagnetic magnetic structure (Cm'c2′1) with the multiple propagation vectors (k = (0, 12, 12) and (0, 12, 0)) and magnetic moments mainly along the b axis is found in PCMO. The critical exponent of the magnetic phase transition is around 0.345 for PSMO and 0.235 for PCMO, indicating 3D and 2D XY transitions, respectively. The strong Jahn-Teller distortion induced by the chemical pressure is believed to suppress the double exchange and favour super-exchange in PCMO, leading to the dramatic difference in the magnetic structure. © 2016 Author(s). Published by AIP Publishing.
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    The cold-neutron triple-axis spectrometer SIKA at OPAL
    (Australian Institute of Physics, 2018-01-31) Deng, G; Yano, SI; Wu, CM; Peng, JC; Gardner, JS; Imamovic, E; Vorderwisch, P; Li, WH; McIntyre, GJ
    SIKA is a high-flux cold-neutron triple-axis spectrometer funded by Ministry of Science and Technology of Taiwan and currently being operated by National Synchrotron Radiation Research Center. It is located on the OPAL reactor face at the Australian Nuclear Science and Technology Organization (ANSTO). Its incident energy ranges from 2.6meV to 30meV with the highest flux at ~8meV. SIKA is equipped with a multiplexing analyzer consisting of an array of 13 PG crystal blades, a multi-wire detector, a single detector and a diffraction detector. The most frequently-used single-detector mode and the multi-Q constant-Ef mode are demonstrated by using the standard samples, namely, MnF2 and Pb single crystals, respectively. The spin-wave excitation of MnF2, the phonon dispersion of thermoelectric material SeSn, the spin dynamics of the spin-glass system (Ni0.40Mn0.60)TiO3, and other experimental data from SIKA are demonstrated as examples of SIKA’s capabilities and performance. The spin-wave excitation was observed in the quasi-one-dimensional spinladder compound SrCa13Cu24O41, indicating the low background of SIKA. These results indicate that SIKA is a highly-flexible cold triple-axis spectrometer with reasonably low background.
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    Comparison of the magnetic and crystal field excitations in orthorhombically distorted vanadates and multiferroic manganites
    (Australian Institute of Nuclear Science and Engineering, 2012-11-15) Reynolds, N; Rovillain, P; Narayanan, N; Fujioka, F; Tokura, Y; Danilkin, SA; Mulders, AM; McIntyre, GJ; Ulrich, C
    Magnetism and ferroelectricity are both exciting physical properties and are used in everyday life in sensors and data storage. In multiferroic materials both properties coexist. They offer a great potential for future technological applications like the increase of data storage capacity or in novel senor applications. We have performed a comparative inelastic neutron scattering (INS) investigation on a series of vanadates, in particularly TbV0{sub 3} DyV0{sub 3}, PrV0{sub 3}, and CeV0{sub 3}, with their multiferroic Mn-counterparts. The Vanadates are isostructural to the multiferroic materials TbMnO{sub 3} and DyMn0{sub 3}, but posses a collinear antiferromagnetic spin arrangement below TN ≈110 K instead of a cycloidal spin structure below TFE 28 ≈K. By using inelastic neutron scattering we have obtained the spin wave dispersion relation and the crystal field excitations of the V-sublattice and the rare earth ions, respectively. The data will be compared with previously obtained INS data of D. Senff on TbMnO{sub 3} and our INS data on DyMnO{sub 3} with the intention of uncovering information about the complex interplay between the magnetic moments of the rare earth ions its role in the formation of the multiferroic phase.
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    A crystal chemical investigation of armenite, BaCa2Al6Si9O30·H2O: the behavior of extra framework Ca cations and H2O molecules in microporous silicates
    (European Geosciences Union, 2012-04-22) Geiger, CA; Gatta, GD; Xue, X; McIntyre, GJ
    The crystal chemistry of armenite, ideally BaCa2Al6Si9O30·H2O, from Wasenalp, Valais, Switzerland was studied. Armenite typically forms in relatively low-temperature hydrothermal veins and fissures and has small pores containing Ca cations and H2O molecules as extra-framework species. Single-crystal neutron and X-ray diffraction measurements were made on armenite from Wasenalp for the first time. IR powder spectroscopic measurements were made from room temperature (RT) down to 10 K. 1H and 29Si NMR measurements were made at RT. Attention was given to investigating the behavior of the extra-framework species and hydrogen bonding. The neutron results also give the first static description of the protons, allowing bond distances and angles relating to the H2O molecules and H-bonds to de determined. The diffraction results indicate complete Al-Si order in the framework and four crystallographically independent Ca and H2O molecule sites. Both sites appear to have partial occupancies such that locally a Ca atom can have only a single H2O molecule bonded to it through an ion-dipole interaction. The Ca cation is further bonded to six O atoms of the framework forming a quasi cluster. The IR spectrum of armenite is characterized in the OH-stretching region at RT by two broad bands at roughly 3470 and 3419 cm−1 and by a single H2O bending mode at 1654 cm−1 and four intense OH bands at 10 K. The 1H MAS spectra contain a single main resonance near 5.3 ppm and a smaller one near 2.7 ppm. The extra-framework “Ca-oxygen-anion-H2O-molecule quasi-clusters” and the nature of H-bonding in the microporous zeolites scolecite, wairakite and epistilbite were also analyzed. The average OH stretching wavenumbers shown by the IR spectra of armenite and scolecite are, for example, not far removed from that observed in liquid H2O, but greater than that of ice. What remains poorly understood in microporous silicates is how the ion-dipole interaction in quasi clusters affects H-bonding strength between the H2O molecules and the aluminosilicate framework. © Author(s) 2012
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    Crystal chemistry of boron-containing minerals by single-crystal neutron diffraction
    (Australian Institute of Nuclear Science and Engineering, 2012-11-15) Gatta, GD; McIntyre, GJ
    Many natural and highly stable minerals contain a significantly high amount of boron which makes their synthetic counterparts of interest as potential neutron absorbers or hosts for storage of nuclear waste. Examples include londonite, with ideal formula (Cs,K)Al4Be4(B,Be)12O28, and hambergite, with formula Be2BO3(OH)0.96F0.04. Single-crystal neutron diffraction is well suited to determining the B/Be distribution and the presence or location of H atoms in these minerals but the high neutron attenuation of B requires very short neutron wavelengths and/or crystal volumes that are considerably smaller than those traditionally desired for neutron diffraction. Here we describe the principal novel neutron diffraction techniques that we used to determine the complete crystal structures of londonite and hambergite. For londonite, neutron Laue diffraction on OrientExpress at the Institut Laue-Langevin (ILL), Grenoble, was an efficient way to select a good quality small crystal for further study on the monochromatic diffractometer D9, also at the ILL, at the short wavelength of 0.7058 A from the hot neutron source. For hambergite, neutron Laue diffraction using KOALA at the OPAL reactor at ANSTO, yielded excellent diffraction data within 36 hours from two small crystals, 2 mm3 in volume.
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    Crystallography at ANSTO’s jewel, the OPAL reactor
    (Australian Institute of Physics, 2014-09-01) Maynard-Casely, HE; McIntyre, GJ
    Australian neutron scattering leapt into the 21st century with the start up of the OPAL reactor at ANSTO in 2006. The major part of the initial success has been in crystallography, carrying on the excellent tradition established since the late 1950s at the HIFAR reactor. 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, and has trained numerous students who are now highly respected ambassadors for neutron scattering. Here we give an overview of highlights in crystallography that have come from the capabilities offered by and around OPAL, and hint at further developments in the field. © 2014 Australian Institute of Physics Inc.
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    Current 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, G
    High-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.