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Facile synthesis of novel Ag/AgI/BiOI composites with highly enhanced visible light photocatalytic performances

Novel Ag/AgI/BiOI composites were controllably synthesized via a facile ion-exchange followed by photoreduction strategy by using hierarchical BiOI microflower as substrate. The as-prepared Ag/AgI/BiOI composites were studied by X-ray powder diffractometer (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller (BET) surface area analyzer and UV–vis diffuse reflectance spectroscopy (DRS). Under visible light (λ>420 nm), Ag/AgI/BiOI displayed highly enhanced photocatalytic activities for degradation of methyl orange (MO) compared to the pure hierarchical BiOI, which was mainly ascribed to the highly efficient separation of electrons and holes through the closely contacted interfaces in the Ag/AgI/BiOI ternary system. - Graphical abstract: Ag/AgI/BiOI displayed excellent photocatalytic activities for methyl orange degradation under visible light, which was mainly ascribed to the highly efficient separation of electrons and holes through Z-scheme pathway. Display Omitted - Highlights: • Novel Ag/AgI/BiOI composites were successfully synthesized. • Ag/AgI/BiOI displayed higher visible light activities than those of pure BiOI and AgI. • ·O{sub 2}{sup −} and h{sup +}, especially ·O{sub 2}{sup −}, dominated the photodegradation process of MO. • A Z-scheme pattern was adopted for Ag/AgI/BiOI activity enhancement.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Quantitative phase analysis of challenging samples using neutron powder diffraction. Sample #4 from the CPD QPA round robin revisited

Here, quantitative phase analysis (QPA) using neutron powder diffraction more often than not involves non-ambient studies where no sample preparation is possible. The larger samples and penetration of neutrons versus X-rays makes neutron diffraction less susceptible to inhomogeneity and large grain sizes, but most well-characterized QPA standard samples do not have these characteristics. Sample #4 from the International Union of Crystallography Commission on Powder Diffraction QPA round robin was one such sample. Data were collected using the POWGEN time-of-flight (TOF) neutron powder diffractometer and analysed together with historical data from the C2 diffractometer at Chalk River. The presence of magnetic reflections from Fe 3 O 4 (magnetite) in the sample was an additional consideration, and given the frequency at which iron-containing and other magnetic compounds are present during in-operando studies their possible impact on the accuracy of QPA is of interest. Additionally, scattering from thermal diffuse scattering in the high- Q region (<0.6 Å) accessible with TOF data could impact QPA results during least-squares because of the extreme peak overlaps present in this region. Refinement of POWGEN data was largely insensitive to the modification of longer d -spacing reflections by magnetic contributions, but the constant-wavelength data were adversely impacted if the magnetic structure was not included. A robust refinement weighting was found to be effective in reducing quantification errors using the constant-wavelength neutron data both where intensities from magnetic reflections were ignored and included. Results from the TOF data were very sensitive to inadequate modelling of the high- Q (low d -spacing) background using simple polynomials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An Easy‐to‐Use Custom‐Built Cell for Neutron Powder Diffraction Studies of Rechargeable Batteries

Abstract In operando powder diffraction remains one of the most powerful tools for non‐destructive investigation of battery electrode materials. While in operando X‐ray, especially synchrotron radiation, powder diffraction is by now a routine experimental technique, in operando neutron powder diffraction is still less established. We present a new electrochemical cell for in operando neutron powder diffraction, which is, first and foremost, easy to use, but can also cycle electrode materials under electrochemical conditions close to those achieved using standard laboratory cells. The cell has been designed in multiple sizes, and high‐quality electrochemical and neutron powder diffraction data is presented for sample sizes as low as 48 mg total active material. The cell handles lithium‐ion and sodium‐ion materials equally well, with no difference in how the cell is prepared and assembled. The cell is intended to be used as sample environment at powder diffractometers at the neutron facilities MLZ, ORNL and ACNS.

25 ENERGY STORAGE↗

Berberine and zinc oxide-based nanoparticles for the chemo-photothermal therapy of lung adenocarcinoma

Highlights: • Berberine (BER) and zinc oxide (ZnO)-based nanoparticles (NPs) were fabricated. • BER-ZnO NPs were prepared by simple blending method without pharmaceutical excipients. • BER-ZnO NPs exhibited improved chemo-photothermal therapeutic effects in A549 cells. Organic/inorganic hydrid nanoparticles (NPs) composed of berberine (BER) and zinc oxide (ZnO) were developed for the therapy of lung cancers. Without the use of pharmaceutical excipients, NPs were fabricated with only dual anticancer agents (BER and ZnO) by facile blending method. The mean weight ratio between BER and ZnO in BER-ZnO NPs was 39:61 in this study. BER-ZnO NPs dispersed in water exhibited 200–300 nm hydrodynamic size under 5 mg/mL concentration. The exposure of both BER and ZnO in the outer layers of BER-ZnO NPs was identified by X-ray photoelectron spectroscopy analysis. The amorphization of BER and the maintenance of ZnO structure were observed in the results of X-ray powder diffractometer analysis. Improved antiproliferation efficacy, based on the chemo-photothermal therapeutic efficacy, of BER-ZnO NPs in A549 (human lung adenocarcinoma) cells was presented. According to the blood tests in rats after intravenous administration, BER-ZnO NPs did not induce severe hepatotoxicity, renal toxicity, and hemotoxicity. Developed BER-ZnO NPs can be used efficiently and safely for the chemo-photothermal therapy of lung cancers.

60 APPLIED LIFE SCIENCES↗

New high pressure rare earth tantalates RE{sub x}Ta{sub 2}O{sub 5+1.5x} (RE=La, Eu, Yb)

Rare earth tantalates La{sub 0.075}Ta{sub 2}O{sub 5.113}, Eu{sub 0.089}Ta{sub 2}O{sub 5.134} and Yb{sub 0.051}Ta{sub 2}O{sub 5.077} have been prepared by solid state reaction at P=7.0 GPa and T=1050–1100 °C and studied by X-ray diffraction, thermal analysis and electron microscopy. Low hydrated amorphous tantalum, lanthanum, europium and ytterbium hydroxides were used as starting materials. Aqueous as well as anhydrous compounds were obtained. Title tantalates are crystallized in the structure type of F–Ta{sub 2}O{sub 5} [Zibrov et al. Russ. J. Inorg. Chem. 48 (2003) 464–471] [5]. The structure was refined by the Rietveld method from X-ray powder diffractometer data: La{sub 0.075}Ta{sub 2}O{sub 5.113}, a=10.5099(2), b=7.2679(1), c=6.9765(1) Å, V=532.90(1) Å{sup 3}, Z=6, space group Ibam; Eu{sub 0.089}Ta{sub 2}O{sub 5.134}, a=10.4182(3), b=7.2685(1), c=6.9832(1) Å, V=528.80(2) Å{sup 3}, Z=6, space group Ibam; Yb{sub 0.051}Ta{sub 2}O{sub 5.077}, a=10.4557(2), b=7.3853(1), c=6.8923(1) Å, V=532.21(1) Å{sup 3}, Z=6, space group Ibam. RE atoms do not replace the tantalum in its positions but the only water in the channels of the structure. Highly charged cations RE{sup +3} compress the unit cell so that its volume becomes less than that of F–Ta{sub 2}O{sub 5}. Significant decrease of the unit cell volume after water removal from the structure is possible due to the puckering of pentagonal bipyramid layers and change of the corrugation angle in the layer. - Graphical abstract: The structure of RE{sub x}Ta{sub 2}O{sub 5+1.5x} and its HRTEM image (“A” arrows show empty channel, “B” arrows show filled channel). - Highlights: • We synthesized new tantalates of RE under high pressure high temperature conditions. • RE atoms replace water molecules in the channels of the structure. • Aqueous as well as anhydrous tantalates were obtained. • Highly charged cations RE{sup +3} compress the unit cell decreasing RE–O distances.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Preparation of PbF2:Ho3+, Er3+, Yb3+ phosphors and its multi-wavelength sensitive upconversion luminescence mechanism

Highlights: • In this paper, PbF{sub 2}: Ho{sup 3+}, Er{sup 3+}, Yb{sup 3+} phosphors are prepared by a high-temperature solid-state method for the first time. • The crystal structure of the as-prepared phosphors is refined. • The upconversion luminescence properties and mechanism of the as-prepared phosphors are analyzed under excitation of 1064 nm, 1550 nm for the first time. - Abstract: In this paper, PbF{sub 2}: Ho{sup 3+}, Er{sup 3+}, Yb{sup 3+} phosphors are prepared by a high-temperature solid-state method. The crystal structure acquired by X ray powder diffractometer shows that the resultant phosphor is a pure cubic PbF{sub 2} crystal. The upconversion (UC) emission spectra of samples are performed by a fluorescence spectrophotometer coupled with lasers of 980 nm, 1064 nm and 1550 nm, presenting the green emission in the range of 541∼548 nm and red emission in the range of 653–667 nm, corresponding to the excitation path: Ho{sup 3+}: {sup 4}F{sub 9/2}→{sup 4}I{sub 15/2}, Er{sup 3+}: {sup 4}S{sub 3/2}→{sup 4}I{sub 15/2}, Er{sup 3+}: {sup 4}F{sub 9/2}→{sup 4}I{sub 15/2} and Ho{sup 3+}: {sup 5}F{sub 5}→{sup 5}I{sub 8}. Finally, the UC luminescence mechanism is analyzed under excitation of different wavelengths. The result shows that the phosphors have a promising prospect for application in anti-counterfeiting technologies and solar cell field.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Uniformity measurements and new positioning algorithms for wavelength-shifting fiber neutron detectors

Wavelength-shifting (WLS) fiber scintillator detectors were successfully installed at two neutron powder diffractometers at the Spallation Neutron Source (SNS). But, they have the following second-order disadvantages: (i). they cannot have both high efficiency and images free of ghosting (position misassignment) concomitantly; (ii). the apparent detection efficiency and spatial resolution are not uniform. These issues are related to the diffusion of scintillation photons and the fluctuation in the number of photons (quantum noise) collected by photo-multiplier tubes (PMTs). Therefore, to mitigate these two issues, we developed two statistics-based positioning algorithms, i.e., a centroid algorithm (CEA) and a correlation algorithm (CA). Compared with the generally used maximum-photon algorithm (MPA), CEA eliminates the ghosting with only about a 10% loss in detection efficiency, and provides better uniformity in detection efficiency and intrinsic background. CA can effectively eliminate ghosting too, but the loss of efficiency at the group boundaries of PMTs is large. Our results indicate that both algorithms can reduce the influence of quantum noise on the neutron positioning.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

PDFgetN3: Atomic Pair Distribution Functions From Neutron Powder Diffraction Data Using ad hoc Corrections

We describe PDFgetN3, a new software tool for the extraction of PDF from neutron powder diffraction intensity data. We demonstrate its use with constant wavelength neutron data measured at the new powder diffractometer PEARL at the Delft University of Technology (TU), Delft. PDFgetN3 uses an ad hoc data collection protocol similar to PDFgetX3. Here, the quality of the resulting PDFs is assessed by structure refinement and by comparison with established results from synchrotron x-ray scattering.

97 MATHEMATICS AND COMPUTING↗

Demonstration of neutron time-of-flight diffraction with an event-mode imaging detector

Neutron diffraction beamlines have traditionally relied on deploying large detector arrays of 3 He tubes or neutron-sensitive scintillators coupled with photomultipliers to efficiently probe crystallographic and microstructure information of a given material. Given the large upfront cost of custom-made data acquisition systems and the recent scarcity of 3 He, new diffraction beamlines or upgrades to existing ones demand innovative approaches. This paper introduces a novel Timepix3-based event-mode imaging neutron diffraction detector system as well as first results of a silicon powder diffraction measurement made at the HIPPO neutron powder diffractometer at the Los Alamos Neutron Science Center. Notably, these initial measurements were conducted simultaneously with the 3 He array on HIPPO, enabling direct comparison. Data reduction for this type of data was implemented in the MAUD code, enabling Rietveld analysis. Results from the Timepix3-based setup and HIPPO were benchmarked against McStas simulations, showing good agreement for peak resolution. With further development, systems such as the one presented here may substantially reduce the cost of detector systems for new neutron instrumentation as well as for upgrades of existing beamlines.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Neutron powder diffraction, Mossbauer Spectroscopy and Optical Spectroscopy to study magnetic and nuclear lattices in Fe-based oxychlorides Ca2FeO3Cl, Sr2FeO3Cl and Sr3Fe2O5Cl2

Data for Neutron Diffraction, Mossbauer Spectoscopy and Optical Spectroscopy are contained on all three samples (Ca2FeO3Cl, Sr2FeO3Cl, and Sr3Fe2O5Cl2). Mossbauer data are in the folder "MossbauerSpectroscopy". This contains details of files and examples to read the data. The Optical Spectroscopy are in the folder "AbsorptionData", this contains one file with explanatory headers. The neutron diffraction data are in the "NeutronDiffractionData" folder. The data was collected on the HB-2A powder diffractometer at HFIR. The autoreduced files are corrected using a vanadium standard and are in arbitrary intensity units. The RawData folder contains the uncorrected data with metadata for motor positions and temperature. All measurements were collected with a constant neuton wavelength of 2.41 Angstrom. An excel spreadsheet "NeutronDiffractionData_IPTS-29118_summary" contains details for each scan. Sr3Fe2O5Cl2 data were collected at only room temperature. Ca2FeO3Cl and Sr2FeO3Cl data were collected at 4K and room temperature. The autoreduced .dat fileformat is three columns corresponding to: Two-theta, Intensity and Intensity_error.

fe-based oxychlorides↗

Quantifying irradiation defects in zirconium alloys: a comparison between transmission electron microscopy and whole-pattern diffraction line-profile analysis - 2016-0089

Irradiation-induced dislocations significantly affect the mechanical properties of zirconium alloys, altering slip and influencing creep and growth. Thus, the quantitative characterization of irradiation defects as a function of fluence, cold work, and/or thermal treatments is important for models that attempt to predict their impact on properties. Whole-pattern diffraction line-profile analysis (DLPA) is a well-established modern tool for microstructure characterization based on first-principle physical models for dislocation density measurements in plastically deformed materials. However, applying these DLPA methods directly to irradiated materials yields higher than expected dislocation density values compared with historical transmission electron microscopy (TEM) measurements and past line-broadening analysis studies calibrated to TEM observations. In an effort to understand these differences, a new microstructural model was developed for DLPA to specifically address dislocation structures consisting of elliptical - and -component loops. To compare the refined DLPA method with TEM measurements, high-resolution neutron diffraction patterns on nonirradiated and irradiated Zr-2.5Nb samples were collected with the Neutron Powder Diffractometer instrument at the Los Alamos Neutron Science Center and were evaluated. High-resolution TEM measurements were performed at the Reactor Materials Testing Laboratory, Queen's University, for comparison with the DLPA results. The capabilities and inherent uncertainties of both the refined DLPA and TEM methods are compared and discussed in detail. We show that the differences between the density values provided by DLPA and TEM are inherent to the methods and can be reconciled with the interpretation of the data. (authors)

36 MATERIALS SCIENCE↗

A New Light Weight Structural Material for Nuclear Structures

Radiation shielding materials are commonly used in nuclear facilities to attenuate the background ionization radiations to a minimum level for creating a safer workplace, meeting regulatory requirements and maintaining high quality performance. The conventional radiation shielding materials have a number of drawbacks: heavy concrete contains a high amount of elements that are not desirable for an effective shielding such as oxygen, silicon, and calcium; a well known limitation of lead is its low machinability and toxicity, which is causing a major environmental concern. Therefore, an effective and environmentally friendly shielding material with increased attenuation and low mass density is desirable. Close-cell composite metal foams (CMFs) and open-cell Al foam with fillers are light-weight candidate materials that we have studied in this project. Close-cell CMFs possess several suitable properties that are unattainable by conventional radiation shielding materials such as low density and high strength for structural applications, high surface area to volume ratio for excellent thermal isolation with an extraordinary energy absorption capability. Open-cell foam is made up of a network of interconnected solid struts, which allows gas or fluid media to pass through it. This unique structure provided a further motive to investigate its application as radiation shields by infiltrating original empty pores with high hydrogen or boron compounds, which are well known for their excellent neutron shielding capability. The resulting open-cell foam with fillers will not only exhibit light weight and high specific surface area, but also possess excellent radiation shielding capability and good processability. In this study, all the foams were investigated for their radiation shielding efficiency in terms of X-ray, gamma ray and neutron. X-ray transmission measurements were carried out on a high-resolution microcomputed tomography (microCT) system. Gamma-emitting sources: 3.0mCi 60 Co, 1.8mCi 137 Cs, 13.5mCi 241 Am, and 5.0mCi 133 Ba were used for gamma-ray attenuation analysis. The evaluations of neutron transmission measurements were conducted at the Neutron Powder Diffractometer beam facility at North Carolina State University. The experimental results were verified theoretically through XCOM and Monte Carlo Z-particle Transport Code (MCNP). A mechanical investigation was performed by means of quasi-static compressive testing. Thermal characterizations were carried out through effective thermal conductivity and thermal expansion analyses in terms of high temperature guarded-comparative-longitudinal heat flow technique and thermomechanical analyzer (TMA), respectively. The experimental results were compared with analytical results obtained from, respectively, Brailsford and Major’s model and modified Turner’s model for verification. Flame test was performed in accordance with United States Nuclear Regulatory Commission (USNRC) standard. CMF sample and a 304L stainless steel control sample were subjected to a fully engulfing fire with an average flame temperature of 800°C for a period of 30 minutes. Finite Element Analysis was conducted to secure the credibility of the experimental results. This research indicates the potential of utilizing the light-weight close-cell CMFs and open-cell Al foam with fillers as shielding material replacing current heavy structures with additional advantage of high-energy absorption and excellent thermal characteristics.

36 MATERIALS SCIENCE↗

Investigation of Energy Selective Neutron Imaging at the PULSTAR Reactor

Neutron imaging is complementary to X-ray imaging where both are used to investigate the internal features of objects nondestructively. Historically, it only began three years after discovery of the neutron in 1932, however, neutron radiographs with reasonable quality were first made in the mid-fifties. Conventionally, the image is produced by placing the object between the neutron source and a two-dimensional position sensitive detector. The source commonly has a full energy spectrum (white beam) of thermal or cold neutrons to obtain high intensity in the sample and short exposure time. As a result, all neutron energies contribute to the obtained radiograph. Since the interaction of the neutron with matter is energy dependent, different energies produce different contrast on the radiographic image, hence, additional information about the object can be obtained. Neutron imaging that utilizes a narrow spectrum of energy instead of white beam is called energy selective neutron imaging. Many techniques have been explored to select a narrow band of neutron energy for the use in imaging such as the use velocity selectors, double crystal Monochromators, and time of flight techniques (at pulsed neutron sources). The PULSTAR reactor of North Carolina State University (1 MWth) currently has an operational neutron powder diffractometer (NPD) installed on beam tube no. 4, which was designed for neutron scattering experiments and can provide a monoenergetic beam of neutrons. The neutron energy could be selected by diffraction means using a Si bent perfect crystal as a Monochromator. In this work, an investigation of energy selective neutron imaging at the NPD is discussed in terms of the system performance and the ability of material discrimination on a test sample by observing the contrast variations of the neutron radiographs obtained using different neutron energies. Energy selective neutron imaging experiment was successfully tested at the PULSTAR reactor's NPD. Although, the uniform region is small and the exposure time is long in comparison with the NIF, both facilities exhibit similar spatial resolution which is a very important characteristic for any imaging facility. The contrast variation of neuron radiographs for the test sample obtained at different energies indicated a potential advantage for using energy selective neutron imaging over the white beam. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

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 3 He crisis in 2009, the authors promptly initiated the development of 3 He-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 50 g 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.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Axisymmetric and Focusing Analyzers to Enable Efficient Powder and Residual Stress Neutron Diffractometers

Project Summary: Company: Adelphi Technology, Inc., Redwood City, CA 94063-4121 DOE Phase 1 STTR PI: Dr. Jay Theodore Cremer, Jr. Chief Scientist at Adelphi Technology, Inc. DOE Phase 1 STTR with: Dr. Boris Khaykovich of Massachusetts Institute of Technology (MIT) MIT Nuclear Reactor Laboratory DOE Phase 1 STTR Title: Axisymmetric and Focusing Analyzers to Enable Efficient Powder and Residual Stress Neutron Diffractometers Statement of the problem or situation that is being addressed: Although thermal and cold neutron scattering is widely used, and is critical for success in many areas of materials science and engineering, relatively low neutron fluxes severely limit applications of not only laboratory neutrons generators, but also large national neutron facilities. State-of-the-art thermal and cold neutron sources are large expensive national facilities, which serve diverse community of scientific and industrial users. The constant need to improve the instruments performance, stems from the fact that neutron methods are gaining in popularity, and becoming more and more powerful, while new neutron sources are not being constructed, so as to keep pace with the developments and needs of the scientific community. Small research reactors at universities and National Labs, and laboratory-based neutron generators, are necessary not only for education and training, but also when samples cannot be transported to other facilities. However, the standard neutron techniques, which were developed for high-flux facilities, require much higher efficiencies to be used effectively with the low fluxes of small sources. Thus, the efficient use of neutron sources, such as with our proposed analyzer, is important for the progress and broader use of these neutron techniques. General statement of how this problem is being addressed: We strive to achieve the goal of efficient use of available thermal and cold neutrons, by introducing here, novel analyzers for powder diffraction and stress-strain measurements. These analyzers will enable polychromatic cold and thermal neutron diffractometers, which will have much higher throughput than existing instruments. At large national facilities, such as at Oak Ridge National Laboratory, these analyzers would enable very fast instruments for screening of multiple samples, for measuring kinetic processes, or for measuring residual stress tensors. Commercial Applications and Other Benefits: By combining the novel analyzers with the Adelphi thermal neutron generator, we will open a new market, which includes the testing of samples that cannot be transported, such as nuclear fuels, or the testing of parts during production. Given the reasonable cost and size of our proposed analyzer systems, along with the continuing development of more powerful thermal neutron generators, the proposed analyzers will be suitable for weak neutrons sources, which are installed at small to large university, industrial, and government laboratories. Key Words: Neutron powder diffraction, residual stress measurements, thermal neutron generators, TRIGA reactors, low flux thermal and cold neutron sources, neutron diffraction. Summary for Members of Congress: Thermal and cold neutron beams are a powerful materials science probe, which provide unique information about the structure of matter. The proposed innovations expand the reach of neutron-based investigations to new materials and industries by enabling new instrumentation capabilities, thereby greatly enhancing and expanding the role of small, laboratory-based neutron instrumentation, and improving education and training of neutron users.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Neutron diffraction studies for realtime leaching of catalytic Ni

The leaching of Al from intermetallic samples of Nickel Aluminium alloys to form Raney-type nickel catalysts is widely used in the hydrogenation industry, however, little is known of the leaching process itself. In this study, the leaching of Al was measured in realtime, in situ, using the high-flux powder neutron diffractometer, D20, at the Institut Laue-Langevin. Despite the liberation of hydrogen and effervescent nature of the reaction the transformation of the dry powder phases into Raney-type Ni was determined. Samples produced by gas-atomisation were found to leach faster than those produced using the cast and crushed technique. Regardless of processing route of the precursor powder, the formation of spongy-Ni occurs almost immediately, while Ni{sub 2}Al{sub 3} and NiAl{sub 3} continue to transform over longer periods of time. Small-angle scattering and broadening of the diffraction peaks is an evidence for the formation of the smaller Ni particles. Understanding the kinetics of the leaching process will allow industry to refine production of catalysts for optimum manufacturing time while knowledge of leaching dynamics of powders produced by different manufacturing techniques will allow further tailoring of catalytic materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

VERDI: VERsatile DIffractometer with wide-angle polarization analysis for magnetic structure studies in powders and single crystals

The VERsatile DIffractometer will set a new standard for a world-class magnetic diffractometer with versatility for both powder and single crystal samples and capability for wide-angle polarization analysis. The instrument will utilize a large single-frame bandwidth and will offer high-resolution at low momentum transfers and excellent signal-to-noise ratio. A horizontal elliptical mirror concept with interchangeable guide pieces will provide high flexibility in beam divergence to allow for a high-resolution powder mode, a high-intensity single crystal mode, and a polarized beam option. A major science focus will be quantum materials that exhibit emergent properties arising from collective effects in condensed matter. The unique use of polarized neutrons to isolate the magnetic signature will provide optimal experimental input to state-of-the-art modeling approaches to access detailed insight into local magnetic ordering.

36 MATERIALS SCIENCE↗