POWGEN: rebuild of a third-generation powder diffractometer at the Spallation Neutron Source
Abstract not provided
Huq, Ashfia↗
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Pressure/temperature fluid cell apparatus for the neutron powder diffractometer instrument: Probing atomic structure in situ
This contribution describes a new local structure compatible gas/liquid cell apparatus for probing disordered materials at high pressures and variable temperatures in the Neutron Powder Diffraction instrument at the Lujan Neutron Scattering Center, Los Alamos National Laboratory. The new sample environment offers choices for sample canister thickness and canister material type. Finite element modeling is utilized to establish maximum allowable working pressures of 414 MPa at 15 K and 121 MPa at 600 K. High quality atomic pair distribution function data extraction and modeling have been demonstrated for a calibration standard (Si powder) and for supercritical and subcritical CO 2 measurements. As a result, the new sample environment was designed to specifically target experimental studies of the local atomic structures involved in geologic CO 2 sequestration, but will be equally applicable to a wide variety of energy applications, including sorption of fluids on nano/meso-porous solids, clathrate hydrate formation, catalysis, carbon capture, and H 2 and natural gas uptake/storage.
36 MATERIALS SCIENCE↗
Electronic angle focusing for neutron time-of-flight powder diffractometers
A neutron time-of-flight (TOF) powder diffractometer with a continuous wide-angle array of detectors can be electronically focused to make a single pseudo-constant wavelength diffraction pattern, thus facilitating angle-dependent intensity corrections. The resulting powder diffraction peak profiles are affected by the neutron source emission profile and resemble the function currently used for TOF diffraction.
electronic focusing↗
Note: An X-ray powder diffractometer with a wide scattering-angle range of 72° using asymmetrically positioned one-dimensional detectors
An X-ray powder diffractometer has been developed for a time-resolved measurement without the requirement of a scattering angle (2θ) scan. Six one-dimensional detector modules are asymmetrically arranged in a vertical line at a designed distance of 286.5 mm. A detector module actually covers a diffraction angle of about 12° with an angular resolution of 0.01°. A diffracted intensity pattern is simultaneously recorded in a 2θ angular range from 1.63° to 74.37° in a “one shot” measurement. We tested the performance of the diffractometer with reference CeO{sub 2} powders and demonstrated diffraction measurements from an operating lithium-air battery.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
X-Ray diffraction on large single crystals using a powder diffractometer
Information on the lattice parameter of single crystals with known crystallographic structure allows for estimations of sample quality and composition. In many cases it is sufficient to determine one lattice parameter or the lattice spacing along a certain, high- symmetry direction, e.g. in order to determine the composition in a substitution series by taking advantage of Vegard’s rule. Here we present a guide to accurate measurements of single crystals with dimensions ranging from 200 μm up to several millimeter using a standard powder diffractometer in Bragg-Brentano geometry. The correction of the error introduced by the sample height and the optimization of the alignment are discussed in detail. Finally, in particular for single crystals with a plate-like habit, the described procedure allows for measurement of the lattice spacings normal to the plates with high accuracy on a timescale of minutes.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Investigating Quantum Materials with Half-Polarized Diffraction and magnetic PDF analysis at the HB-2A Neutron Powder Diffractometer
Local magnetic ordering and anisotropy is often central to the emergent behavior and subsequent functional properties in quantum materials and beyond. Neutron powder diffraction provides a straightforward yet extremely powerful technique for quantitative measurements of microscopic magnetic properties. The HB-2A powder diffractometer located at the High Flux Isotope Reactor in ORNL is traditionally utilized for long-range magnetic structure determination. Recently these capabilities have been extended to include methods aimed at accessing local magnetism: Half- polarized neutron powder diffraction (pNPD) and magnetic pair distribution function (mPDF) analysis. These two distinct techniques are possible on HB-2A due to the versatility of the instrument’s reciprocal space coverage, resolution and novel ultra-low temperature multi-sample changers that operate down to dilution refrigerator temperatures. This provides unique capabilities not found on any powder diffraction instrument and is particularly well suited to investigations of magnetic quantum materials. The development and implementation of these techniques will be discussed with a series of science case examples ranging from geometric frustrated magnets to magnetic metal-organic frameworks. Data reduction and analysis tools will be presented that enable the extraction of the local site susceptibility tensor and local spin-spin correlations in real space. Finally, potential combinations of these techniques in the form of half-polarized magnetic pair distribution function (pmPDF) analysis will be considered. Looking forward, HB-2A is undergoing a detector upgrade that will be in the user program by 2026. This will offer an order of magnitude increase in count rates to further aid the development of these often low signal measurements and provide new scientific capabilities.
Neutron Scattering↗
Magnetic pair distribution function and half polarized neutron powder diffraction at the HB-2A powder diffractometer
Local magnetic order and anisotropy are often central for understanding fundamental behavior and emergent functional properties in quantum materials and beyond. Advances in neutron powder diffraction experiments and analysis tools now allow for quantitative determination. Here, we demonstrate this here with complementary total neutron scattering and polarized neutron measurements on the HB-2A neutron powder diffractometer at the High Flux Isotope Reactor (HFIR). In recent years, magnetic pair distribution function (mPDF) analysis has emerged as a powerful technique for probing local magnetic spin ordering of magnetic materials. This method can be broadly applied to any magnetic material but is particularly effective for studying systems with short-range magnetic order, such as materials with reduced dimensionality, geometrically frustrated magnets, thermoelectrics, multiferroics, and correlated paramagnets. Magnetic anisotropy often underpins the short-range order adopted. Half-polarized neutron powder diffraction (pNPD) can be used to determine the local susceptibility tensor on the magnetic sites to quantify the magnetic anisotropy. Combining the techniques of mPDF and pNPD can therefore provide valuable insights into local magnetic behavior. A series of measurements optimized for these techniques are presented as exemplar cases focused on frustrated materials where short-range order dominates, these include measurements to ultra-low temperature (<100 mK) not typically accessible for such experiments.
Half polarized neutron scattering↗
An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer
An electrochemical cell has been designed for powder X-ray diffraction studies of lithium ion batteries (LIB) and sodium ion batteries (SIB) in operando with high time resolution using a conventional powder X-ray diffractometer. The cell allows for studies of both anode and cathode electrode materials in reflection mode. The cell design closely mimics that of standard battery testing coin cells and allows obtaining powder X-ray diffraction patterns under representative electrochemical conditions. In addition, the cell uses graphite as the X-ray window instead of beryllium, and it is easy to operate and maintain. Test examples on lithium insertion/extraction in two spinel-type LIB electrode materials (Li{sub 4}Ti{sub 5}O{sub 12} anode and LiMn{sub 2}O{sub 4} cathode) are presented as well as first results on sodium extraction from a layered SIB cathode material (Na{sub 0.84}Fe{sub 0.56}Mn{sub 0.44}O{sub 2})
36 MATERIALS SCIENCE↗
Investigation of the response of a neutron-Hand monitor dedicated to the powder diffractometer at CENM-Maamora
Neutrons are used for the study of condensed matter. A neutron beam can indeed easily penetrate the solid material and undergo diffraction phenomena. Analysis of the diffused neutrons allows studying the atomic structure of crossed material. Their neutral electric charge makes them nondestructive probe of a great interest. In general, the size of the powder samples is very small and therefore the centering of the beam on these is very crucial. It is in this context we proceed to test a portable neutron monitor for centering and checking beam leak around the shielding to be installed around the diffractometer in TRIGA Mark II of CENM. It's consisting of a scintillation neutron detector NE426 ({sup 6}LiF + ZnS (Ag)) with electronic module and data acquisition system. The effect of radiation from radioactive neutrons source {sup 252}Cf is shown. Sensitivity and differential linearity are also performed. This study indicates several advantages of this detector with very good detection sensitivity and excellent stability during the counting time. (authors)
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
A high performance neutron powder diffractometer at 3 MW Triga Mark-II research reactor in Bangladesh
A high performance neutron diffractometer called Savar Neutron Diffractometer (SAND) was built and installed at radial beam port-2 of TRIGA Mark II research reactor at AERE, Savar, Dhaka, Bangladesh. Structural studies of materials are being done by this technique to characterize materials crystallograpohically and magnetically. The micro-structural information obtainable by neutron scattering method is very essential for determining its technological applications. This technique is unique for understanding the magnetic behavior in magnetic materials. Ceramic, steel, electronic and electric industries can be benefited from this facility for improving their products and fabrication process. This instrument consists of a Popovicimonochromator with a large linear position sensitive detector array. The monochromator consists of nine blades of perfect single crystal of silicon with 6 mm thickness each. The monochromator design was optimized to provide maximum flux on 3 mm diameter cylindrical sample with a relatively flat angular dependence of resolution. Five different wave lengths can be selected by orienting the crystal at various angles. A sapphire filter was used before the primary collimator to minimize the first neutron. The detector assembly is composed of 15 linear position sensitive proportional counters placed at either 1.1 m or 1.6 m from the sample position and enclosed in a air pad supported high density polythene shield. Position sensing is obtained by charge division using 1-wide NIM position encoding modules (PEM). The PEMs communicate with the host computer via USB. The detector when placed at 1.1 m, subtends 30° (2θ) at each step and covers 120° in 4 steps. When the detector is placed at 1.6 m it subtends 20° at each step and covers 120° in 6 steps. The instrument supports both low and high temperature sample environment. The instrument supports both low and high temperature sample environment. The diffractometer is a state-of-the art technology for diffraction study in our country.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Utilization of the High Flux Isotope Reactor at Oak Ridge National Laboratory
This paper addresses several aspects of the scientific utilization of the Oak Ridge National Laboratory High Flux Isotope Reactor (HFIR). Topics to be covered will include: 1) HFIR neutron scattering instruments and the formal instrument user program; 2) Recent upgrades to the neutron scattering instrument stations at the reactor, and 3) eMod a new tool for addressing instrument modifications and providing configuration control and design process for scientific instruments at HFIR and the Spallation Neutron Source (SNS). There are 15 operating neutron instrument stations at HFIR with 12 of them organized into a formal user program. Since the last presentation on HFIR instruments at IGORR we have installed a Single Crystal Quasi-Laue Diffractometer instrument called IMAGINE; and we have made significant upgrades to HFIR neutron scattering instruments including the Cold Triple Axis Instrument, the Wide Angle Neutron Diffractometer, the Powder Diffractometer, and the Neutron Imaging station. In addition, we have initiated upgrades to the Thermal Triple Axis Instrument and the Bio-SANS cold neutron instrument detector system. All of these upgrades are tied to a continuous effort to maintain a high level neutron scattering user program at the HFIR. For the purpose of tracking modifications such as those mentioned and configuration control we have been developing an electronic system for entering instrument modification requests that follows a modification or instrument project through concept development, design, fabrication, installation, and commissioning. This system, which we call eMod, electronically leads the task leader through a series of questions and checklists that then identifies such things as ES&H and radiological issues and then automatically designates specific individuals for the activity review process. The system has been in use for less than a year and we are still working out some of the inefficiencies, but we believe that this will become a very effective tool for achieving the configuration and process control believed to be necessary for scientific instrument systems.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Powder diffraction
Powder diffraction is a non-destructive technique, which is experimentally simple in principle. Because the physics behind diffraction is well understood, an exceptionally large amount of information can be obtained from a single measurement. The positions and relative intensities of the peaks yield a fingerprint that can be used for qualitative phase analysis. Quantitative phase analysis can be obtained by detailed analysis of the intensities. Unit cells can be derived from the peak positions. Crystal structures can be solved using powder diffraction data and refined by the Rietveld method. The peak profiles contain information about crystallite size, strain and nanostructure. Non-idealities in the intensities give information on texture. Abandoning the crystallographic model provides information about local structure, by pair distribution function analysis. For powder diffraction, everything is a sample; the technique is commonly applied to characterize minerals, ceramics, metals and alloys, catalysts, polymers, pharmaceuticals, organic compounds, environmental and forensic samples, among others. The major features of contemporary laboratory powder diffractometers are described. Methods for obtaining suitable powder specimens are summarized. Major applications of qualitative and quantitative phase analysis, structure solution, size/strain/nanostructure analysis using peak profiles, texture analysis and pair distribution function analysis are introduced.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Neutron Instruments for Research in Coordination Chemistry
Here, neutron diffraction and spectroscopies offer unique insight into structures and properties of solids and molecular materials. All neutron instruments located at the various neutron sources are distinct, even if their designs are based on similar principles, and thus, are usually less familiar to the community than commercial X–ray diffractometers and optical spectrometers. Major neutron instruments in the USA, which are open to scientists around the world, and examples of their use in coordination chemistry research are presented here, along with a list of similar instruments at main neutron facilities in other countries. The reader may easily and quickly find from this mini–review an appropriate neutron instrument for research. The instruments include single–crystal and powder diffractometers to determine structures, inelastic neutron scattering (INS) spectrometers to probe magnetic and vibrational excitations, and quasielastic neutron scattering (QENS) spectrometers to study molecular dynamics such as methyl rotation on ligands. Key and unique features of the diffraction and neutron spectroscopies that are relevant to inorganic chemistry are reviewed.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Pushing data quality for laboratory pair distribution function experiments
Over the past decade, some studies with laboratory pair distribution function (PDF) data emerged. Yet, limited Q max or instrumental resolution impeded in-depth structural refinements. With more advanced detector technologies, the question arose how to design novel PDF equipment for laboratories that will allow decent PDF refinements over r = 1–70 Å. It is crucial to reflect the essential requirements, namely, monochromatic X-rays, suppression of air scattering, instrumental resolution, and overall measurement times. The result is a novel PDF setup based on a STOE STADI P powder diffractometer in transmission-/Debye-Scherrer geometry with monochromatic Ag Kα 1 radiation, featuring a MYTHEN2 4K detector covering a Q range of 0.3–20.5 Å –1 . PDF data are collected in a moving PDF mode within 6 h. Structural signatures of liquids can be satisfactorily resolved in the PDF as shown for the ionic liquid hmimPF 6 . The high instrumental resolution is mirrored in low q damp values determined from LaB 6 measurements. PDF data from a powder sample of ca. 7 nm TiO 2 nanoparticles were successfully refined over up to 70 Å with goodness-of-fit values R w < 0.22 (respectively R w = 0.18 over 30 Å), thanks to the low background and high instrumental resolution, hereby enlarging the accessible r range by several tens of Angstroms compared to previous laboratory PDF studies.
47 OTHER INSTRUMENTATION↗
A suite-level review of the neutron powder diffraction instruments at Oak Ridge National Laboratory
The suite of neutron powder diffractometers at Oak Ridge National Laboratory (ORNL) utilizes the distinct characteristics of the Spallation Neutron Source and High Flux Isotope Reactor to enable the measurements of powder samples over an unparalleled regime at a single laboratory. Full refinements over large Q ranges, total scattering methods, fast measurements under changing conditions, and a wide array of sample environments are available. Here, this article provides a brief overview of each powder instrument at ORNL and details the complementarity across the suite. Future directions for the powder suite, including upgrades and new instruments, are also discussed.
47 OTHER INSTRUMENTATION↗
Enhancement in magnetic properties of magnesium substituted bismuth ferrite nanoparticles
We report a potential way to effectively improve the magnetic properties of BiFeO{sub 3} (BFO) nanoparticles through Mg{sup 2+} ion substitution at the Fe-sites of BFO lattice. The high purity and structural changes induced by Mg doping are confirmed by X-ray powder diffractometer and Raman spectra. Enhanced magnetic properties are observed in Mg substituted samples, which simultaneously exhibit ferromagnetic and superparamagnetic properties at room temperature. A physical model is proposed to support the observed ferromagnetism of Mg doped samples, and the superparamagnetic properties are revealed by the temperature dependent magnetization measurements. The improved magnetic properties and soft nature obtained by Mg doping in BFO nanoparticles demonstrate the possibility of BFO nanoparticles to practical applications.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Remote and automated high-throughput powder diffraction measurements enabled by a robotic sample changer at SSRL beamline 2-1
The general-purpose powder diffractometer beamline (BL2-1) at the Stanford Synchrotron Radiation Lightsource (SSRL) is described. The evolution of design and performance of BL2-1 are presented, in addition to current operating specifications, applications and measurement capabilities. Recent developments involve a robotic sample changer enabling high-throughput X-ray diffraction measurements, applicable to mail-in and remote operations. In situ and operando capabilities to measure samples with different form factors ( e.g. capillary, flat plate or thin film, and transmission) and under variable experimental conditions are discussed. Several example datasets and accompanying Rietveld refinements are presented.
43 PARTICLE ACCELERATORS↗
Impact of crystalline defects and size on X-ray line broadening: A phenomenological approach for tetragonal SnO{sub 2} nanocrystals
Nanocrystalline tin oxide (SnO{sub 2}) powders with different grain size were prepared by chemical precipitation method. The reaction was carried out by varying the period of hydrolysis and the as-prepared samples were annealed at different temperatures. The samples were characterized using X-ray powder diffractometer and transmission electron microscopy. The microstrain and crystallite size were calculated for all the samples by using Williamson-Hall (W-H) models namely, isotropic strain model (ISM), anisotropic strain model (ASM) and uniform deformation energy density model (UDEDM). The morphology and particle size were determined using TEM micrographs. The directional dependant young’s modulus was modified as an equation relating elastic compliances (s{sub ij}) and Miller indices of the lattice plane (hkl) for tetragonal crystal system and also the equation for elastic compliance in terms of stiffness constants was derived. The changes in crystallite size and microstrain due to lattice defects were observed while varying the hydrolysis time and the annealing temperature. The dependence of crystallite size on lattice strain was studied. The results were correlated with the available studies on electrical properties using impedance spectroscopy.
36 MATERIALS SCIENCE↗