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DOE OSTI2025

Deuteration Effects on the Physical and Optoelectronic Properties of Donor–Acceptor Conjugated Polymers

The significant differences in scattering cross sections between deuterium and protium are unique to neutron scattering techniques and have been a long-standing area of interest within the neutron scattering community. Researchers have explored selective deuteration to manipulate scattering contrast in soft matter systems, leading to the widespread use of deuterium labeling in materials development. As deuteration changes the atomic mass, it alters physical properties such as molecular volume, polarizability, and polarity, which in turn may affect noncovalent interactions and crystal ordering. Despite previous studies, there remains a limited understanding of how deuteration impacts donor–acceptor (DA) conjugated polymers. To address this, we synthesized deuterated DPP polymers and systematically investigated the effects of side-chain deuteration on their thermal stability, crystal packing, morphology, and optoelectronic properties. We found that deuteration increased the melting and crystallization temperatures of DPP polymers, although it did not significantly alter their morphology, molecular packing, or charge mobility. These properties were assessed by using atomic force microscopy (AFM), X-ray scattering, and thin-film transistor device measurements, respectively, for DPP polymers. Our work shows that deuterium labeling could be a powerful method for controlling scattering length density, enabling neutrons to study the structure and dynamics of conjugated polymers without impacting their electronic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Data Mining – Image Analysis of Radiography for Zr Redistribution

The research effort described in this report represents a first attempt to investigate the radial redistribution of Zr in ternary fuel alloys U-xPu-10Zr (x = 0, 8, 19) irradiated in the in-reactor fuel experiments during the operation of the U.S. Department of Energy’s (DOE’s) Experimental Breeder Reactor II (EBR-II) at Idaho National Laboratory (INL) using methods of image processing on post-irradiation neutron radiographs. Approximately 130,000 metal fuel pins were irradiated in EBR-II during its 30 years of operation to develop and characterize existing and prospective fuels. For many of the metal fuel irradiation experiments, neutron radiography imaging was performed historically now allowing application of modern image analysis techniques to characterize fuel behavior, such as fuel swelling, fluff formation, and now, fuel alloy constituent redistribution. The redistribution of fuel components depends on the temperature field, radially, within the fuel. Specifically, Zr is expected to redistribute radially towards the center of the pin, as well as towards the outer zones. Currently, direct imaging of a pin cross-section through optical methods or scanning electron microscopy (SEM) is used to study the constituents’ redistribution, which is very time-consuming and can only be applied to a limited number of pins. An automated image processing technique allowing for the investigation of fuel radial redistribution zones would significantly accelerate data analysis. In general, if the fuel temperature is hot enough, three redistribution zones are expected, corresponding to the main fuel components (e.g., U, Pu, Zr). While more assessment will be performed in fiscal year (FY)-2023, it seems possible to differentiate the pins according to their fuel composition using image analysis techniques on neutron radiographs of metallic fuel pins based on the analysis to date.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2022

Epitaxial intergrowths and local oxide relaxations in natural bixbyite Fe 2– x Mn x O 3

The scattering pattern of a crystal obeys the symmetry of the crystal structure through the corresponding Laue group. This is usually also true for the diffuse scattering, containing information about disorder, but here a case is reported where the diffuse scattering is of lower symmetry than the parent crystal structure. The mineral bixbyite has been studied by X-ray and neutron scattering techniques since 1928 with some of the most recent studies characterizing the low-temperature transition to a magnetically disordered spin-glass state. However, bixbyite also exhibits structural disorder, and here single-crystal X-ray and neutron scattering is used to characterize the different modes of disorder present. One-dimensional rods of diffuse scattering are observed in the cubic mineral bixbyite, which break the expected symmetry of the scattering pattern. It is shown that this scattering arises from epitaxial intergrowths of the related mineral, braunite. The presence of this disorder mode is found to be directly observable as well-defined residuals in the average structure refined against the Bragg diffraction. An additional three-dimensional diffuse scattering component is observed in neutron scattering data, which is shown to originate from the substitutional disorder on the Fe/Mn sites. This occupational disorder gives rise to local relaxations of the oxide sublattice, and the pattern of oxide displacements can be rationalized based on crystal-field theory. The combined use of neutron and X-ray single-crystal scattering techniques highlights their great complementarity. In particular, the large sample requirements for neutron scattering experiments prove to be an obstacle in solving the intergrowth disorder due to several growth orientations, whereas for X-ray scattering the one-dimensional nature of the intergrowth disorder renders solving this a more tractable task. On the other hand, the oxide relaxations cannot be resolved using X-rays due to the low Mn/Fe contrast. By combining the two approaches both types of disorder have been characterized.

36 MATERIALS SCIENCE↗

NASA NTRS2001

Proportional counter as neutron detector

A technique to separate out the dose, and lineal energy spectra of neutrons and charged particles is described. It is based on using two proportional counters, one with a wall, and the other with similar characteristics but wall made from a non-hydrogen containing material. Results of a calibration in a neutron field are also shown. c2001 Elsevier Science Ltd. All rights reserved.

NASA Center JSC↗

DOE OSTI2022

Neutron tagging following atmospheric neutrino events in a water Cherenkov detector

We present the development of neutron-tagging techniques in Super-Kamiokande IV using a neural network analysis. The detection efficiency of neutron capture on hydrogen is estimated to be 26%, with a mis-tag rate of 0.016 per neutrino event. The uncertainty of the tagging efficiency is estimated to be 9.0%. Measurement of the tagging efficiency with data from an Americium-Beryllium calibration agrees with this value within 10%. The tagging procedure was performed on 3,244.4 days of SK-IV atmospheric neutrino data, identifying 18,091 neutrons in 26,473 neutrino events. The fitted neutron capture lifetime was measured as 218±9 μs.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2026

Neutron Grating Interferometry at the High Flux Isotope Reactor

Neutron imaging is a non-destructive probe that can spatially resolve bulk materials’ internal features/structures. Neutron imaging spatial resolution is driven by detector technology, i.e., pixel size, and is currently on the order of 10–20 µm. This limitation can be alleviated by the use of neutron grating interferometry – an advanced neutron imaging technique – that enables simultaneous access to three contrast mechanisms: attenuation, differential phase, and small-angle neutron scattering. Recently, a Talbot-Lau neutron grating interferometry has been implemented at the Multimodal Advanced Radiography Station at the High Flux Isotope Reactor. In this work, the design, setup and performance of the grating apparatus are presented.

Zhang, Yuxuan [ORNL] (ORCID:0000000200831408)↗

DOE OSTI2023

Neutron Scattering (NS) Spectroscopy

A wide range of advanced experimental methods has been used in catalysis science to understand chemical transformations at molecular level. Among these, neutron scattering not only gives catalytic information that is highly complementary to other microscopic scattering techniques such as electrons (microscopy and diffraction) and photons from visible light to synchrotron X-rays but also often provides unique insights into catalysis. This chapter aims to provide a general overview of neutron scattering and its applications for heterogeneous catalysis, emphasizing chemistry at the gas/solid interface. It starts with an introduction to the theory of neutron scattering, with pros and cons for catalyst research, followed by a description of three main neutron scattering techniques: neutron diffraction (ND), inelastic neutron spectroscopy (INS), and quasi-elastic neutron scattering (QENS). It includes recent applications in each technique and then a short introduction of other neutron techniques that are less frequently used in the catalysis field. It ends with a summary and a future outlook.

Braatz, Jisue↗

NASA NTRS2012

Time-Resolved Data Acquisition for In Situ Subsurface Planetary Geochemistry

The current gamma-ray/neutron instrumentation development effort at NASA Goddard Space Flight Center aims to extend the use of active pulsed neutron interrogation techniques to probe the subsurface geochemistry of planetary bodies in situ. All previous NASA planetary science missions, that used neutron and/or gamma-ray spectroscopy instruments, have relied on a constant neutron source produced from galactic cosmic rays. One of the distinguishing features of this effort is the inclusion of a high intensity 14.1 MeV pulsed neutron generator synchronized with a custom data acquisition system to time each event relative to the pulse. With usually only one opportunity to collect data, it is difficult to set a priori time-gating windows to obtain the best possible results. Acquiring time-tagged, event-by-event data from nuclear induced reactions provides raw data sets containing channel/energy, and event time for each gamma ray or neutron detected. The resulting data set can be plotted as a function of time or energy using optimized analysis windows after the data are acquired. Time windows can now be chosen to produce energy spectra that yield the most statistically significant and accurate elemental composition results that can be derived from the complete data set. The advantages of post-processing gamma-ray time-tagged event-by-event data in experimental tests using our prototype instrument will be demonstrated.

Bodnarik, Julia Gates↗

NASA NTRS2013

Time-resolved Neutron-gamma-ray Data Acquisition for in Situ Subsurface Planetary Geochemistry

The current gamma-ray/neutron instrumentation development effort at NASA Goddard Space Flight Center aims to extend the use of active pulsed neutron interrogation techniques to probe the subsurface elemental composition of planetary bodies in situ. Previous NASA planetary science missions, that used neutron and/or gamma-ray spectroscopy instruments, have relied on neutrons produced from galactic cosmic rays. One of the distinguishing features of this effort is the inclusion of a high intensity 14.1 MeV pulsed neutron generator synchronized with a custom data acquisition system to time each event relative to the pulse. With usually only one opportunity to collect data, it is difficult to set a priori time-gating windows to obtain the best possible results. Acquiring time-tagged, event-by-event data from nuclear induced reactions provides raw data sets containing channel/energy, and event time for each gamma ray or neutron detected. The resulting data set can be plotted as a function of time or energy using optimized analysis windows after the data are acquired. Time windows can now be chosen to produce energy spectra that yield the most statistically significant and accurate elemental composition results that can be derived from the complete data set. The advantages of post-processing gamma-ray time-tagged event-by-event data in experimental tests using our prototype instrument will be demonstrated.

Pulsed neutrongenerator↗

NASA NTRS1992

Light curves of rotating, oscillating neutron stars

A technique has been developed for computing the light curve produced by a rotating, oscillating neutron star that emits radiation from circular polar cap regions, as are thought to exist in pulsars, X-ray binaries, and perhaps X-ray bursters. Several examples of light curves produced by single, low-order (l = 1, 2) oscillation modes are given. A Gaussian beaming function is used to simulate typical radio pulsar beam widths in order to investigate a neutron star oscillation model for subpulse drift in pulsars. X-ray bursts and X-ray pulsars have also been simulated to assess the possibility of detecting such oscillations in these sources with XTE and AXAF.

Strohmayer, T. E.↗

DOE OSTI2020

Phase evolution during lithium–indium halide superionic conductor dehydration

Select rare-earth alkali halides have demonstrated high lithium ion conductivity. The conductivity appears to be related to the stability of the crystal phase, ordering of the lithium sublattice and the amount of residual H 2 O. Li 3 InCl 6 can be synthesized from concentrated aqueous solution through controlled dehydration. In this work, we track Li 3 InCl 6 dehydration using a multimodal approach that combines thermogravimetric, spectroscopic, X-ray diffraction, and neutron scattering techniques. In situ X-ray diffraction suggests a single phase transition caused by dehydration, in disagreement with spectroscopic and thermodynamic measurements. Neutron scattering, being sensitive toward the H 2 O and Li sublattices, reveals multiple phase transitions. We show that the loss of the final trace H 2 O leads to strain and grain boundary formation. Thus, controlled dehydration may be a viable strategy for high-throughput processing for roll-to-roll manufacturing of REAH solid electrolytes.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Room temperature sodium diffusion in sodium iron phosphate investigated with neutron scattering

Sodium iron phosphate, Na x FePO 4 , is currently one of the most promising cathode materials for sodium ion batteries. Here we employ a systematic approach using three neutron scattering techniques to investigate temperature dependent properties with a focus on the charge transfer processes. Two distinct Na + diffusive motions are observed with quasielastic neutron scattering, including room temperature motion. These processes correspond to rapid double jumps through extrinsic vacancy sites of ∼6 Å along with the more fundamental nearest neighbor jumps of 3.1 Å. Experimental observations of room temperature ionic diffusion are highly desirable, as the diffusion pathways are naturally well suited for efficient transport. Inelastic neutron scattering was used to probe the vibrational density of states that assist in the ionic and electronic (polaronic) transport processes, which are further supported with density functional theory. Neutron diffraction examines the disordering of the sodium sublattice upon transition to the solid-solution phase, which is believed to enhance the overall kinetics during sodium insertion/extraction. Finally, 57 Fe Mössbauer spectroscopy measurements probes polaron hopping and the local structural evolution that modifies the electron density surrounding the redox active iron sites. This study sheds light on the temperature induced atomic scale dynamics that occur in olivine Na x FePO 4 .

Novak, Eric [Swarthmore College, Swarthmore, PA (U↗

DOE OSTI2020

Octupolar versus Néel Order in Cubic 5d 2 Double Perovskites

We report time-of-flight neutron spectroscopy and neutron and x-ray diffraction studies of the 5 d 2 double perovskite magnets, Ba 2 M OsO 6 ( M = Zn , Mg , Ca ). We find that these materials host antiferromagnetically coupled 5 d 2 Os 6 + ions decorating a face-centered cubic (fcc) lattice and are found to remain cubic down to the lowest temperatures. They all exhibit thermodynamic anomalies consistent with a single phase transition at a temperature T * , and a gapped magnetic excitation spectrum with spectral weight concentrated at wave vectors typical of type-I antiferromagnetic orders. However, while muon spin resonance experiments show clear evidence for time-reversal symmetry breaking below T * , we observe no corresponding magnetic Bragg scattering signal. These results are shown to be consistent with ferro-octupolar symmetry breaking below T * , and are discussed in the context of other 5 d double perovskite magnets and theories of exotic orders driven by multipolar interactions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Review of Direct Neutron Conversion and Detection Processes

Commercial and laboratory neutron detection systems use indirect neutron response of materials like pressurized helium-3 (via nuclear reaction 3He(n, p)3H) to measure and count neutrons emanating from a source. Recently a host of semiconductors, especially a ternary semiconductor of lithium indium diselenide (6LiInSe2) and a quaternary alloy of enriched lithium-6, indium, phosphorous, and selenium (6LiInP2Se6), have shown promising neutron counting possibilities by directly converting neutrons into charge-carrying elements within the body of the semiconductor. These semiconductors have high thermal neutron capture cross sections, suitable energy bandgaps (~2.0 electron volts) for room-temperature operations, and a favorable electronic band structure for efficient electron charge transport. The article examines the semiconductor properties of these compounds in terms of their neutron counting capabilities and possible ways to extract neutron energy information from them. Lithium-6 and boron-10 (with thermal neutron absorption cross sections of 938 ± 6 and 3855 ± 26 barns, respectively) produce charged particles to be measured via indirect neutron interactions. The efficiency of indirect conversion neutron detectors is limited because of the inefficiencies in conversion mechanism. In case of direct conversion, the neutrons create charged particles in a single material for neutron capture and charge collection, increasing detection efficiency. Unlike 3He proportional counters, which provide no neutron energy information, the semiconductors can be used as neutron energy spectrometer. Fully resolved neutron energy by 6LiInP2Se6 from a plutonium-beryllium source has been reported in the literature. We will discuss the influence of these multilayered semiconductors’ crystallographic structures and growth techniques on neutron energy determination.

61 RADIATION PROTECTION AND DOSIMETRY↗

DOE OSTI2022

Estimating β eff from static, late-time Feynman neutron noise measurements

The effective delayed neutron fraction, β eff , is a kinematic parameter describing the contribution of delayed neutrons to the effective multiplication factor, $\kappa$ eff , and is of great interest to the nuclear criticality safety community and beyond. In fact, $\kappa$ eff presently must be inferred (as opposed to directly measured) since variables like β eff must be obtained from simulation, reference tables, or a dynamic or pulsed measurement where the assembly of fissile material is perturbed and not in steady state. Several recent works have proposed neutron noise techniques to estimate β eff from static measurements (such as benchmark experiments). This work experimentally investigates an approach based on looking at late-time (up to thousands of seconds) correlated neutrons in Feynman histograms. This work utilizes measurements of weapons grade plutonium and highly enriched uranium to construct late-time Feynman histograms and investigate a proposed methodology of estimating β eff from a fit of the distribution. Data is shown from both He-3 detectors and an organic scintillator array. This work is preliminary in nature, demonstrating some experimental feasibility and proposing improvements for future investigations.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

NASA NTRS2000

Gravitational Waves from Rotating Neutron Stars and Evaluation of fast Chirp Transform Techniques

X-ray observations suggest that neutron stars in low mass X-ray binaries (LMXB) are rotating with frequencies from 300 - 600 Hz. These spin rates are significantly less than the break-up rates for essentially all realistic neutron star equations of state, suggesting that some process may limit the spin frequencies of accreting neutron stars to this range. If the accretion induced spin up torque is in equilibrium with gravitational radiation losses, these objects could be interesting sources of gravitational waves. I present a brief summary of current measurements of neutron star spins in LMXBs based on the observations of high-Q oscillations during thermonuclear bursts (so called 'burst oscillations'). Further measurements of neutron star spins will be important in exploring the gravitational radiation hypothesis in more detail. To this end I also present a study of fast chirp transform (FCT) techniques as described by Jenet and Prince in the context of searching for the chirping signals observed during X-ray bursts.

Strohmayer, Tod E.↗

DOE OSTI2021

Temperature Dependent Local Atomic Structure and Vibrational Dynamics of Barium Hydride and Calcium Hydride

Solid-state ionic conductors that exhibit pure ionic transport of hydride anions are rare. Here, we investigate two alkaline earth metal hydrides, barium hydride and calcium hydride, using neutron scattering techniques to understand how the local atomic environment plays a role in the diffusion of hydride ions. At high temperatures, barium hydride exhibits exceptional transport properties with ionic conductivities that are higher than those of many of the typical proton and oxide ion conductors in use today. Total neutron scattering and pair distribution function analysis reveal how a structural phase transition converts barium hydride from a modest ionic conductor into a fast ionic conductor through the introduction of disorder, deuterium site splitting, and dynamic structural fluctuations. Furthermore, neutron vibrational spectroscopy is employed to probe changes in the temperature evolution of the lattice dynamics and local energy landscape. These results improve our fundamental knowledge of the interplay between structure and dynamics governing a rare conduction process of hydride ions in solid-state materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Neutron scattering investigation of proposed Kosterlitz-Thouless transitions in the triangular-lattice Ising antiferromagnet TmMgGaO 4

In this study, we use a variety of neutron scattering techniques to investigate the nature of the unusual magnetism in the compound TmMgGaO 4 . The crystal structure of this material hosts a triangular lattice of Tm spins exhibiting strong geometrical frustration. Theoretical predictions have suggested an unusual topological magnetic phase transition known as a Kosterlitz-Thouless transition at low temperature. By combining and comparing the various neutron scattering results, we have compelling evidence that such a transition indeed occurs at temperatures around 4 K in TmMgGaO 4 . This establishes TmMgGaO 4 as a valuable system to study Kosterlitz-Thouless physics in a dense spin system.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗