Neutron Powder Diffractometer Research Articles

Comparison of the Numerical and Analytical Calculations of the Resolution Function for a Powder Neutron Diffractometer

Comparison of the Numerical and Analytical Calculations of the Resolution Function for a Powder Neutron Diffractometer

POWTEX visits POWGEN.

The high-intensity time-of-flight (TOF) neutron diffractometer POWTEX for powder and texture analysis is currently being built prior to operation in the eastern guide hall of the research reactor FRM II at Garching close to Munich, Germany. Because of the world-wide 3He crisis in 2009, the authors promptly initiated the development of 3He-free detector alternatives that are tailor-made for the requirements of large-area diffractometers. Herein is reported the 2017 enterprise to operate one mounting unit of the final POWTEX detector on the neutron powder diffractometer POWGEN at the Spallation Neutron Source located at Oak Ridge National Laboratory, USA. As a result, presented here are the first angular- and wavelength-dependent data from the POWTEX detector, unfortunately damaged by a 50g shock but still operating, as well as the efforts made both to characterize the transport damage and to successfully recalibrate the voxel positions in order to yield nonetheless reliable measurements. Also described is the current data reduction process using the PowderReduceP2D algorithm implemented in Mantid [Arnold et al. (2014). Nucl. Instrum. Methods Phys. Res. A, 764, 156-166]. The final part of the data treatment chain, namely a novel multi-dimensional refinement using a modified version of the GSAS-II software suite [Toby & Von Dreele (2013). J. Appl. Cryst.46, 544-549], is compared with a standard data treatment of the same event data conventionally reduced as TOF diffraction patterns and refined with the unmodified version of GSAS-II. This involves both determining the instrumental resolution parameters using POWGEN's powdered diamond standard sample and the refinement of a friendly-user sample, BaZn(NCN)2. Although each structural parameter on its own looks similar upon comparing the conventional (1D) and multi-dimensional (2D) treatments, also in terms of precision, a closer view shows small but possibly significant differences. For example, the somewhat suspicious proximity of the a and b lattice parameters of BaZn(NCN)2 crystallizing in Pbca as resulting from the 1D refinement (0.008 Å) is five times less pronounced in the 2D refinement (0.038 Å). Similar features are found when comparing bond lengths and bond angles, e.g. the two N-C-N units are less differently bent in the 1D results (173 and 175°) than in the 2D results (167 and 173°). The results are of importance not only for POWTEX but also for other neutron TOF diffractometers with large-area detectors, like POWGEN at the SNS or the future DREAM beamline at the European Spallation Source.

HRPD and TEM Study of P/M 58Fe17Cr25Ni Austenitic Stainless Steel Synthesized by Spark Plasma Sintering

58Fe17Cr25Ni austenite stainless steel has been fabricated using metal powder through sintering with a spark plasma at temperatures of 900 and 950°C for 5 minutes. High purity Fe, Ni and Cr powders were used as materials for this steel. Before sintering, the powder was mixed in a milling equipment which was processed for 5 hours, then it is formed into a coin by pressing it under a load of 25 tons. High resolution powder neutron diffractometer was used for identifying the crystal structure in the 58Fe17Cr25Ni austenitic stainless steel. The sintering process at temperatures of 900C and 950°C generally forms microstructure having matrix of equiaxed austenite grains, with a crystal structure of face-centered cubic which included in the Fm3m space group. Some particles with high Cr content, a'-Cr, are distributed in all austenite grains. The austenite grains seen in the 58Fe17Cr25Niaustenitic stainless steel sintered at 900°C are twin grains. Dislocations, slip planes and bands are also existed in those grains. These defects are expected to decrease with increasing sintering temperatures up to 950° C. This change was followed by the appearance of air bubbles and sub-grains as the dominant sub-structures in the 58Fe17Cr25Ni austenitic stainless steel sintered at 950°C.

Upgrade of Xuanwu: A dual-mode neutron powder diffractometer at CMRR

Neutron diffraction (ND) is a well-established technique of great significance in condensed physics and materials science. Although it has particular advantages against its brother X-ray diffraction (XRD), intensity is still a limiting factor counteracting its application. Herein, we report the upgrade of Xuanwu, a high-resolution neutron powder diffractometer at the China Mianyang Research Reactor (CMRR). A doubly focusing monochromator system made of Si blades is applied to enhance the intensity from 2 × 105n⋅cm−2⋅s−1 to 2.39 × 106n⋅cm−2⋅s−1 with changeable wavelength. The high-resolution mode with a best resolution 1.6‰ is reserved, which means the working style is optional between high-resolution and high-intensity, making Xuanwu more applicable in expanded scopes.

The neutron diffraction experiments under high pressure and high temperature on FENGHUANG diffractometer at CMRR

FENGHUANG diffractometer at CMRR, a high-intensity multi-section neutron powder diffractometer, has been constructed to in situ studies of materials under high pressure high temperature conditions. With development of anvils, high pressure high temperature cell assemblies, high pressure device and alignment system, we have been realized the angle-dispersive neutron diffraction data collect at the range of achievable pressures and temperatures of 0–30 GPa and 300–1500 K, with the sample size of millimeter scale. This paper describes the technical characteristics of diffractometer and related techniques for high pressure neutron diffraction experiments, and gives some scientific examples that have been recently performed on FENGHUANG. The experience gained experiments on FENGHUANG could help promote the development of high pressure techniques on neutron scattering facilities.

Effects of Plasma Sintering on the Post TIG Weld Joint of Fe-15Cr-25Ni Austenitic Stainless Steel

Arc-plasma sintering (APS) for 5 s has been applied to the post tungsten inert gas (TIG) weld joint of Fe–15Cr–25Ni austenitic stainless steel (ASS). The treatment is intended to observe the effect of heat generated by plasma on micro-crystal structures around the fusion zone (FZ), especially internal stress relief in steel after being subjected to welding. The effect of stress relief in weld was measured using the neutron diffraction technique. ASS that is predominantly composed of Fe, Cr, and Ni elements, with contents of 57%, 15%, and 25%wt. respectively, was cut into two parts. Both parts were then welded with TIG without filler with a current and voltage of 60 A and 50 V, respectively. After APS for 5 s, the sample was characterized and analyzed using high-resolution powder neutron diffractometer at a high-temperature laboratory facility. The results show that the tensile residual stress decreased with the APS heat input. The residual stresses significantly decreased from 82.40 MPa to 1.21 MPa in the FZ and continued almost evenly from 65.92 MPa to 1.24 MPa in the heat-affected zone (HAZ). The residual stress is a tensile stress that can reduce the mechanical strength of materials. This condition is also applicable to applied loads. A microstructure gives a confirmation that the C element migrates from the FZ to HAZ. The content was very high in dark traces. The C element reacts to Cr and O to form chromium carbide (Cr23C6) and chromium carbonyl (CrC6O6), respectively. It rapidly migrates among its grain boundaries. It may also weaken materials and probably initiate intergranular cracks.

Certification of SRM 640f line position and line shape standard for powder diffraction.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to be used to evaluate specific aspects of the instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 640f, the seventh generation of this powder diffraction SRM, which is designed to be used primarily for calibrating powder diffractometers with respect to line position; it also can be used for the determination of the instrument profile function. It is certified with respect to the lattice parameter and consists of approximately 7.5 g of silicon powder prepared to minimize line broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the Si powder. Both statistical and systematic uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.5431144 ± 0.000008 nm.

Neutron Diffraction Study on Ce-Doped Nickel Ferrite Nanoparticles

The NiCexFe2-xO4 polycrystalline spinel compound with composition x = 0.005, 0.010, 0.015, and 0.02 was synthesized by the solid reaction method using the high energy milling (HEM) apparatus. Measurement of the neutron diffraction patterns is carried out at room temperature using a high resolution powder neutron diffractometer (HRPD), wavelength λ = 1.8213 Å. The measured neutron diffraction data were analyzed by the Rietveld method utilizing the FullProf analysis code. The results of the neutron diffraction pattern refinement revealed that the sample has a cubic symmetry, the Fd-3m space group, mixed inverse spinel structure, A-site occupied by cation Fe3+, Ni2+, dan Ce3+. Whereas the B-site is only occupied by Fe3+ and Ni2+. The mole fraction of Fe3+ at the B-site is greater than the Fe3+ mole fraction at the A-site, whereas the mole fraction of Ni2+ at the B-site is smaller than the mole fraction of Ni2+ at the B-site. As a result of Ce3+ doping, oxygen position parameters increase, magnetic moments on B-site, and the net magnetic moments decrease. Ni2+ concentrations at the A-site and the B-site were not affected by the amount of Ce3+ substitutions. Without substitution and after Ce3+ substitution, the O-site occupancy factor is still oxygen deficient.

Neutron Guide Building instruments of the Brazilian Multipurpose Reactor (RMB) project

A growing community of scientists has been using neutrons in the most diverse areas of science. In order to meet the researchers demand in the areas of physics, chemistry, materials sciences, engineering, cultural heritage, biology and earth sciences, the Brazilian Multipurpose Reactor (RMB) will provide 3 thermal guides and 3 cold guides, with the installation of several instruments for materials characterization. In this study, we present a standard design requirement of two primordial instruments, namely Sabi'a and Araponga. They are, respectively, cold and thermal neutron instruments and correspond to a Small-Angle Neutron Scattering (SANS) and High-Resolution Powder Neutron Diffractometer (HRPND) to be installed in the Neutron Guide Building (N02) of RMB . To provide adequate flux for both instruments, we propose here an initial investigation of the use of simple and split guides to transport neutron beams to two different instruments on the same guide. For this purpose, we use Monte Carlo simulations utilizing McStas software to check the efficiency of thermal neutron transport for different basic configuration and sources. By considering these results, it is possible to conclude that the split guide configuration is, in most cases, more efficient than cases that use transmitted neutron beams independently of source. We also verify that the employment of different coating indexes for concave and convex surfaces on curved guides is crucial, at least on simulated cases, to optimise neutron flux (intensity and divergence) and diminish facility installation cost.

Neutron Diffraction Study of Multiferroic 0.6NiFe2O4/0.4BaTiO3 Composite

Neutron diffraction study on the 0.6NiFe2O4/0.4BaTiO3 multiferroic composite has been carried out. The 0.6NiFe2O4/0.4BaTiO3 multiferroic composites have been synthesized by solid reaction method. In this study, 20 g of BaTiO3 (BTO) and 20 g of NiFe2O4 (NFO) compounds were prepared from the powder raw materials of BaO3 and TiO2 for BTO, and NiO and Fe2O3 for NFO. Furthermore, both BTO and NFO were each crushed for 5 hours using High Energy Milling (HEM). Then the BTO and NFO were calcined in the furnace at 950°C/5 hours and 900°C/5 hours, respectively. Both NFO and BTO precursors were manually mixed with a weight percent ratio of NFO:BTO was 100:0, 60:40, and 0:100, hereinafter referred to NFO, NFO/BTO, and BTO, respectively. Then the three samples were pressed into pellets. The pellets were then sintered at 1150 °C/5 hours with a heating rate of about 44.8°C/min. Once cooled to room temperature within the furnace it was obtained NFO, BTO, and NFO/BTO multiferroic composite. The magnetic properties of the material were observed with the aid of the Vibrating Sample Magnetometer (VSM) instrument. The nuclear structure of BTO, and the magnetic structure of NFO, and NFO/BTO multiferroic composite were determined by neutron diffraction technique using the high resolution powder neutron diffractometer. The cations arrangement of NFO was obtained by whole pattern fitting with the Rietveld method based on neutron diffraction data using FullProf software. The cations arrangement was obtained by refining the occupancy of individual cation at tetrahedral and octahedral sites. The results of the analysis show that both NFO and 0.6NFO/0.4BTO samples have a mixed spinel structure, it means that there are cations of Ni2+ and Fe3+ on A-site and B-site. In NFO sample, the cations distribution among the A-site and B-site of NiFe2O4 is [Ni0.002Fe0.852][Ni0.006Fe0.862]2O4. The cations distribution among the A-site and B-site of NiFe2O4 in 0.6NFO/0.4BTO samples is [Ni0.0250Fe0.8975] [Ni0.012Fe0.950]2O4. So, the effect of adding BTO as a composite is to increase Ni2+ occupancy by 12.5 times on A-site and 2 times on B-site. The magnetic moment of multiferroic 0.6NFO/0.4BTO composite is 2.4(5) µB same as one of NFO. The BTO content in the composite has caused tensile strains induced into the NFO lattice, and at the same time, tensile strains of NFO caused the compressive strain on the c lattice of BTO even though the unit cell volume of BTO is also increasing from 64.100(5) to 64.374(6) A3.

Certification of Standard Reference Material 660c for powder diffraction.

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to evaluate specific aspects of instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 660c, the fourth generation of this powder diffraction SRM, which is used primarily for calibrating powder diffractometers with respect to line position and line shape for the determination of the instrument profile function (IPF). It is certified with respect to lattice parameter and consists of approximately 6 g of lanthanum hexaboride (LaB6) powder. So that this SRM would be applicable for the neutron diffraction community, the powder was prepared from an isotopically enriched 11B precursor material. The microstructure of the LaB6 powder was engineered specifically to yield a crystallite size above that where size broadening is typically observed and to minimize the crystallographic defects that lead to strain broadening. A NIST-built diffractometer, incorporating many advanced design features, was used to certify the lattice parameter of the LaB6 powder. Both Type A, statistical, and Type B, systematic, uncertainties have been assigned to yield a certified value for the lattice parameter at 22.5 °C of a = 0.415 682 6 ± 0.000 008 nm (95% confidence).

Molecular Dynamics and Neutron Scattering Studies of Potassium Chloride in Aqueous Solution.

Neutron diffraction with isotopic substitution (NDIS) experiments were done on both natural abundance potassium and isotopically labeled 41KCl heavy water solutions to characterize the solvent structuring around the potassium ion in water. Preliminary measurements suggested that the literature value for the coherent neutron scattering length (2.69 fm) for 41K was significantly in error. This value was remeasured using a neutron powder diffractometer and found to be 2.40 fm. This revision increases significantly the contrast between the natural abundance K and 41K by about 30% (from 1.0 to 1.3 fm). The experimentally determined structure factor of the potassium ion was then compared to that calculated from molecular dynamics (MD) simulations. Previous neutron scattering measurements of potassium gave a solvation number of 5.5 (see below). In this study, the NDIS and MD results are in good agreement and allowed us to derive a coordination number of 6.1 for water molecules and 0.8 for chloride ions around each K+ ion in 4 molal aqueous KCl solution.

The upgraded Polaris powder diffractometer at the ISIS neutron source.

This paper describes the design and operation of the Polaris time-of-flight powder neutron diffractometer at the ISIS pulsed spallation neutron source, Rutherford Appleton Laboratory, UK. Following a major upgrade to the diffractometer in 2010-2011, its detector provision now comprises five large ZnS scintillator-based banks, covering an angular range of 6° ≤ 2θ ≤ 168°, with only minimal gaps between each bank. These detectors have a substantially increased solid angle coverage (Ω ∼ 5.67 sr) compared to the previous instrument (Ω ∼ 0.82 sr), resulting in increases in count rate of between 2× and 10×, depending on 2θ angle. The benefits arising from the high count rates achieved are illustrated using selected examples of experiments studying small sample volumes and performing rapid, time-resolved investigations. In addition, the enhanced capabilities of the diffractometer in the areas of in situ studies (which are facilitated by the installation of a novel design of radial collimator around the sample position and by a complementary programme of advanced sample environment developments) and in total scattering studies (to probe the nature of short-range atomic correlations within disordered crystalline solids) are demonstrated.

POWGEN: rebuild of a third-generation powder diffractometer at the Spallation Neutron Source.

The neutron powder diffractometer POWGEN at the Spallation Neutron Source has recently (2017-2018) undergone an upgrade which resulted in an increased detector complement along with a full overhaul of the structural design of the instrument. The current instrument has a solid angular coverage of 1.2 steradians and maintains the original third-generation concept, providing a single-histogram data set over a wide d-spacing range and high resolution to access large unit cells, detailed structural refinements and in situ/operando measurements.

Weak Ferromagnetic Property and Electromagnetic Waves Absorption Characteristic of La(1-x)BaxMnO3

The weak ferromagnetic property and the electromagnetic waves absorption characteristic of La(1-x)BaxMnO3 (LBMO) compounds have been investigated. The samples of LBMO that are LaMnO3 (S0), La0.9Ba0.1MnO3 (S1); La0.8Ba0.2MnO3 (S2); and La0.7Ba0.3MnO3 (S3) were synthesized using high energy milling (HEM) method. Samples were characterized by means of XRD (X-ray diffractometer), HRPD (high-resolution powder neutron diffractometer), EDS (energy dispersive X-ray spectroscopy, VSM (vibrating sample magnetometer), and VNA (vector network analyzer). There is no magnetic ordering of ferromagnetic in S1 and S2 samples due to the Ba occupation factors of both less than 0.2. The Ba content in the S3 sample is greater than 0.2, hence the ferromagnetic property of the compound is not so visible with the VSM as well as the VNA. The absorption characteristics of electromagnetic waves using VNA indicated that there is an absorption of EM waves in the frequency range between 8-12 GHz with almost the same peak frequency for all four samples at 10.8 GHz with the absorption of around 5 dB. The existence of a weak ferromagnetic property can be detected clearly using HRPD. Neutron diffraction as a probe can observe the magnetic structure accurately even in a material having a weak ferromagnetic property.

Interplay between magnetic ion and amorphous carbon in Na3V2(PO4)3/C nanocomposite

The crystal structure, magnetic properties and electrical properties of Na3V2(PO4)3/C nanocomposite were investigated using neutron and x-ray powder diffractometer, Raman spectroscopy, and experiments on ac magnetic susceptibility and ac impendence. Na3V2(PO4)3 has a trigonal structure with an R-3c space group and the carbon film coating has an amorphous phase at temperatures between 5 K and 300 K. An external magnetic field enlarged the lattice constant size parallel to the c-axis but had no effect on that parallel to the a-axis. Short-range magnetic correlation was observed below 220 K. A magnetic field of 1 mT was equivalent to a 1.4(2) K thermal effect the c-axis. The carbon film yielded Raman peaks associated with D1-, D3-, D4-, and G-bands. The ac magnetic susceptibility curve is consistent with the Curie-Weiss law. The magnetic moment of V3+ and Curie temperature TC of the sample were 2.91(6) μB/f.u. and 15(4) K, respectively. Ac impedance (Z) experiments demonstrated that the external magnetic field had no any effect on Z at 300 K. This investigation reveals a possibility of lattice and phonon control by the application of an external magnetic field. Its findings may be useful in developing lithium or sodium ion batteries.

High-pressure neutron diffraction techniques based on Paris-Edingburgh press

Since the 1990s, with the benefit of available large-volumed samples, wide detector windows, and portability, Paris-Edinburgh press has been widely used in neutron facilities to study the structures and physical properties of condensed matter under high-pressure extreme conditions. In the present study, We perform high-pressure neutron diffraction experiments in neutron source of China using the Paris-Edinburgh press. The experiments are carried out on a high-pressure neutron diffraction spectrometer (Fenghuang) at China Mianyang Research Reactor (CMRR). Fenghuang is a high-intensity and moderate-resolution diffractometer which has been upgraded from a neutron powder diffractometer and can be used under ambient and extreme conditions. A single cylinder pump with a max load of 200 MPa provides a loading pressure for Paris-Edinburgh press, and a precise mobile platform is used to hang and to locate the Paris-Edinburgh press. Using the tungsten-carbide (WC) toroidal anvils with TiZr gasket, we obtain the neutron diffraction spectra of Fe samples at different pressures successfully. We also obtain the neutron diffraction spectra respectively at pressures of 9.7 GPa and 10.7 GPa by using a WC single-toroidal anvil and a WC double-toroidal anvil under load 100 MPa. The TiZr gasket blows out before the load reaches 100 MPa in the WC single-toroidal anvil assembly, while it remains good in the WC double-toroidal anvil assembly under the same load. The WC single-toroidal anvil assembly becomes unstable under load about 80 MPa, and the WC double-toroidal anvil assembly is still stable under load 100 MPa. Thus, the stability of the double-toroidal anvil assembly is much higher than that of the single-toroidal anvil assembly. It is found that the thickness of the gasket edge is very important for the stability of the assembly during loading. The thicker the edge of the gasket, the more stable the assembly is. The main reason is that the groove of the double concave anvil can enhance the lateral support ability of the gasket, thereby making the double concave surface assembly more stable than the single concave surface assembly.

ECHIDNA: a decade of high-resolution neutron powder diffraction at OPAL

The ECHIDNA high-resolution neutron powder diffractometer at the 20 MW OPAL research reactor in Australia produces high-quality data for a broad spectrum of crystal and magnetic structural studies. The paper presents an overview of the current status of the hardware, latest developments in data-reduction software, statistics on instrument usage and the user programme, and instrument limitations.

Fenghuang: High-intensity multi-section neutron powder diffractometer at CMRR

Fenghuang has been upgraded to be the first neutron powder diffractometer at the China Mianyang Research Reactor (CMRR) dedicated to research on the microstructure of materials. It was firstly built in 2005 at the Swimming Pool Research Reactor-300 (SPRR-300) in Mianyang, and then moved to CMRR in 2013. Through the combination of a horizontally focusing neutron guide and a vertically focusing monochromator, the neutron flux at the sample position is up to 2.84 × 106 n s−1cm−2. The resolution of the diffractometer can be adjusted by a horizontal slit for different sample. The superposition scan mode enables each detector to measure the complete diffraction pattern and simplifies the correction of the efficiency of the counting channels. This diffractometer is equipped with temperature and pressure devices, and can be used for research at ambient and extreme conditions.

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. 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.