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All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Probing the hydrolytic degradation of UF 4 in humid air

This manuscript describes the chemical transformations that occur during hydrolysis of uranium tetrafluoride (UF 4 ) due to its storage in humid air (85% and 50% relative humidity) at ambient temperatures. This hydrolysis was previously reported to proceed slowly or not at all (depending on the percent relative humidity); however, previous reports relied primarily on X-ray diffraction methods to probe uranium speciation. Here, we employ a battery of physiochemical probing techniques to explore potential hydrolysis, including Raman spectroscopy, powder X-ray diffraction, 19 F nuclear magnetic resonance spectroscopy, scanning electron microscopy, and focused ion beam microscopy with energy-dispersive X-ray spectroscopy. Of these, only Raman spectroscopy proved to be particularly useful at observing chemical changes to UF 4 . It was found that anhydrous UF 4 slightly oxidizes over the course of thirteen days to Schoepite-like uranium complexes and possibly UO 3 . In contrast, UF 4 exposed to 50% relative humidity slightly decomposes into UO 2 F 2 , Schoepite-like uranium complexes, and possibly a high order uranium oxide that eluded chemical assignment (U x O y ). Despite the rich chemical speciation observed in our Raman spectroscopy measurements, X-ray diffraction and 19 F NMR measurements on the same material showed no changes. Microscopy measurements suggest that the observed reactions between UF 4 and water occur primarily on the surface of UF 4 particulates via a method that is visually similar to surface corrosion of metals. Therefore, we postulate that NMR spectroscopy and X-ray diffraction, which are well-suited for bulk analysis, are less suited than Raman spectroscopy to observe the surface-based reactions that occur to UF 4 when exposed to humid air. Considering the importance of UF 4 in the production of nuclear fuel and weapons, the results presented herein are widely applicable to numerous nuclear science fields where uranium detection and speciation in humid environments is of value, including nuclear nonproliferation and nuclear forensics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Synthesis and crystal structure characterization of InGaZnO{sub 4} with a new defect structure

Single crystals of InGaZnO{sub 4} were synthesized in a sealed Pt-tube at elevated temperatures under normal pressure without flux. InGaZnO{sub 4} has a trigonal crystal system (R3{sup ¯}m; No. 166) deduced from convergent beam electron diffraction (CBED). Single crystal structure refinement from XRD data at −150 °C (a=3.275(1) Å; c=25.99(1) Å; Z=3) revealed an alternate stacking of InO{sub 6/3}{sup −} and (Ga,Zn)O{sub 4/4}{sup +} layers, iso-structural to YbFe{sub 2}O{sub 4}. The cell parameters at room temperature were refined from powder X-ray diffraction data (a=3.284(3) Å and c=26.037(3) Å). The transparent crystals have a gray-bluish color and exhibit an excess of Ga expressed by the cation ratio of In:Ga:Zn=30.2(9):39(1):31(1) determined by energy dispersive X-ray spectroscopy (EDXS). While the isovalent substitution of In{sup 3+} by Ga{sup 3+} is known, an additional aliovalent substitution of Zn{sup 2+} by Ga{sup 3+} is observed. This results in the formula (In{sub 0.9}Ga{sub 0.1})Ga{sub 1.06}Zn{sub 0.91}□{sub 0.03}O{sub 4} where 3% of the cations in 4+1 coordination are vacant due to aliovalent substitution. Further evidence of that defect structure is found in the lattice parameter a which is substantially smaller than in stoichiometric InGaZnO{sub 4}, as well as in the strong absorption in the near-IR from transitions correlated with the defect structure. The bluish color of the crystals is due to an enhanced absorption in the red of the visible spectrum. For the first time, we achieved to image InGaZnO{sub 4} at atomic resolution in the electron microscope proving a perfect periodic stacking of atomic layers. - Graphical abstract: Single crystals of InGaZnO{sub 4} have been synthesized at ambient pressure and analyzed with X-ray diffraction, electron microscopy, and optical absorption. Optical band gap and optical transmission have been determined. - Highlights: • Preparation of single crystals of InGaO{sub 3}(ZnO){sub 1} at ambient pressure for the first time. • Non-stoichiometric compound (In{sub 0.9}Ga{sub 0.1})Ga{sub 1.06}Zn{sub 0.91}□{sub 0.03}O{sub 4} with defect structure, excess of Ga, depletion of Zn. • Real structure of InGaO{sub 3}(ZnO){sub 1} imaged by high resolution TEM for the first time. • Optical band gap and transmission of InGaO{sub 3}(ZnO){sub 1} single crystal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Studies on 2-amino-5-nitropyridinium nitrate (2A5NPN): A semi-organic third order nonlinear optical single crystal

2-amino-5-nitropyridinium nitrate (2A5NPN) is a semi-organic nonlinear optical crystal and optically good quality 2A5NPN single crystals were successfully grown by slow evaporation solution growth technique (SEST) at ambient temperature. The crystallographic structure of the grown crystal was determined by single crystal X-Ray diffraction analysis and it belongs to Monoclinic crystal system with centro symmetric crystalline nature. The crystallinity of the grown crystal was confirmed by powder X-ray diffraction analysis. The other physical properties of grown crystals are also characterized using TG-DTA, UV-Visible NIR, chemical etching, photoconductivity and Z-scan measurements. The Z-scan method reveals that the 2A5NPN crystal possesses multi photon absorption behaviour and the significantly higher third order susceptibility and it is a promising potential NLO material.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Electron Paramagnetic Resonance and X-ray Diffraction of Boron- and Phosphorus-Doped Nanodiamonds

Powders of boron- and phosphorus-doped detonation nanodiamonds and sintered pellets of non-doped nanodiamond powders were studied using electron paramagnetic resonance and x-ray diffraction. Doping of detonation nanodiamond crystals with boron and phosphorus was demonstrated to be possible. These methods could be used to diagnose diamond nanocrystals doped during shock-wave synthesis.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

In situ synthesis and characterization of uranium carbide using high temperature neutron diffraction

Advances in neutron flux, neutron instrumentation, and sample environments over the past years allowed the development of unique techniques to characterize material synthesis and processing. The available infrastructure at LANL allows to apply these techniques to radioactive materials or materials containing actinides. Here, we present capabilities and results to characterize materials in situ at temperatures above 2000 Celsius degrees such as in loss-of-coolant accidents. Temperatures in excess of 2000 C. degrees are not readily achieved and neutrons are one of a few probes to characterize materials under these conditions. Research in refractory materials, phase diagram studies or accident scenarios for nuclear materials are research areas where such extreme conditions are required. As an example, we present the formation of UC{sub x} from UO{sub 2+x} and graphite in situ using high temperature neutron diffraction with particular focus on resolving the conflicting reports on the crystal structure of non-quenchable cubic UC{sub 2}. The ability to follow the reaction UO{sub 2}+C → UC{sub x}+CO{sub y} in situ with neutron diffraction allows us to conclude that the reaction occurs within minutes over a temperature range of 60 Celsius degrees. The initiation of the reaction is far below the reaction temperature of 2000 C. degrees reported for this reaction in standard text books on actinide chemistry. This may be due to the unusually small ∼100 nm grain size of our UO{sub 2} initial powder. Furthermore, the holding time of several hours reported in the literature would be unnecessary. The neutron diffraction data collected for the cubic high temperature UC{sub 2} phase unambiguously confirmed the disordered C-C dumbbells and excluded structures previously determined by X-ray diffraction.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

Residual stress induced crystalline to amorphous phase transformation in Nb{sub 2}O{sub 5} quantum dots

Nb{sub 2}O{sub 5} quantum dots (QDs) were grown using a simple technique of vacuum thermal evaporation. QDs were found to be crystalline in nature by selected area electron diffraction (SAED) in TEM. Samples with thickness up to 20 nm did not show any significant residual strain. Residual stress effect on band gap of crystalline Nb{sub 2}O{sub 5} was studied for films thicker than 20 nm. Residual strain was determined using SAED of the films with reference to powder X-ray diffraction (XRD). Films thicker than 45 nm become amorphous as analyzed by both SAED and XRD. The optical absorption of films in the range 25–60 nm indicates significantly varying optical band gap of films. The varying band gap with film thickness scales linearly very well with the variation of residual stress with film thickness. The residual stress dependence of band gap of crystalline films yields stress free band gap as 3.37 eV with pressure coefficient of band gap (∂E{sub g}/∂P){sub T} = −29.3 meV/GPa. From this study, the crystalline to amorphous transformation in tetragonal form of M-Nb{sub 2}O{sub 5} has been determined to be at about 14 GPa. Both pressure coefficient of band gap and crystalline to amorphous transition for tetragonal M-Nb{sub 2}O{sub 5} have been determined for the first time in the literature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Substitution effect on magnetic and electrical properties of half-Heusler alloy Ni{sub 1−x}Co{sub x}Mn{sub 1−y}Fe{sub y}Sb

We have studied the effects of Co and Fe doping on the magnetic and electrical properties of half-Heusler compound NiMnSb. The alloys were prepared by arc-melting method in the presence of Argon gas. The powder X-ray diffraction of the each alloy was performed in air at room temperature. The magnetic and electrical properties were performed in the temperature range 2–400 K and in magnetic field up to 1 T.

36 MATERIALS SCIENCE↗
DOE OSTI2014

A roadmap to uranium ionic liquids: Anti-crystal engineering

In the search for uranium-based ionic liquids, tris(N,N-dialkyldithiocarbamato)uranylates have been synthesized as salts of the 1-butyl-3-methylimidazolium (C 4 mim) cation. As dithiocarbamate ligands binding to the UO 2 2+ unit, tetra-, penta-, hexa-, and heptamethylenedithiocarbamates, N,N-diethyldithiocarbamate, N-methyl-N-propyldithiocarbamate, N-ethyl-N-propyldithiocarbamate, and N-methyl-N-butyldithiocarbamate have been explored. X-ray single-crystal diffraction allowed unambiguous structural characterization of all compounds except N-methyl-N-butyldithiocarbamate, which is obtained as a glassy material only. In addition, powder X-ray diffraction as well as vibrational and UV/Vis spectroscopy, supported by computational methods, were used to characterize the products. Differential scanning calorimetry was employed to investigate the phase-transition behavior depending on the N,N-dialkyldithiocarbamato ligand with the aim to establish structure–property relationships regarding the ionic liquid formation capability. Compounds with the least symmetric N,N-dialkyldithiocarbamato ligand and hence the least symmetric anions, tris(N-methyl-N-propyldithiocarbamato)uranylate, tris(N-ethyl-N-propyldithiocarbamato)uranylate, and tris(N-methyl-N-butyldithiocarbamato)uranylate, lead to the formation of (room-temperature) ionic liquids, which confirms that low-symmetry ions are indeed suitable to suppress crystallization. As a result, these materials combine low melting points, stable complex formation, and hydrophobicity and are therefore excellent candidates for nuclear fuel purification and recovery.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Growth and characterization of 4-chloro-3-nitrobenzophenone single crystals using vertical Bridgman technique

4-chloro-3-nitrobenzophenone (4C3N) has been grown by using vertical Bridgman technique. The grown crystal was confirmed by Powder X-ray diffraction analysis. The crystalline perfection of the grown crystal was examined by high-resolution X-ray diffraction study. The fluorescence spectra of grown 4C3N single crystals exhibit emission peak at 575 nm. The micro hardness measurements were used to analyze the mechanical property of the grown crystal.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Synthesis and optical properties of polycrystalline Li{sub 2}Al{sub 2}B{sub 2}O{sub 7} (LABO)

A polycrystalline lithium aluminum borate (Li{sub 2}Al{sub 2}B{sub 2}O{sub 7}, LABO) has been synthesized by using simple solid-state technique. The obtained LABO polycrystalline was characterized by powder X-ray diffraction; Fourier transform infrared (FT-IR) spectroscopy and second harmonic generation (SHG) efficiency measurement. The functional groups were identified using the FT-IR spectroscopic data. The SHG efficiency of the polycrystalline material was obtained by the classic Kurtz powder technique using a fundamental wavelength 1064 nm of Nd:YAG laser and it is found to be 1.4 times that of potassium dihydrogen phosphate (KDP).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Optical studies in Er{sup 3+} doped BaMoO{sub 4} downconverting phosphor for blue LEDs

Erbium ion (Er{sup 3+}) doped BaMoO{sub 4} phosphor has been synthesized via co-precipitation technique. Phase formation of the prepared phosphor has been recognized by powder X-ray diffraction analysis. The photoluminescence emission spectrum has been recorded in 400-800nm wavelength range under 380nm excitation. The observed photoluminescence peaks are explained with the help of energy level structure. The prepared phosphor seems capable to produce efficient blue colour emission which can be useful for making blue light emitting diodes (LEDs).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Particle Size and Specific Surface Area on the Determination of the Density of Nanocrystalline Silver Sulfide Ag{sub 2}S Powders

The effect of the particle size and specific surface area of silver sulfide powders on their density measured by the helium pycnometry method has been studied. Powders with different average particle sizes have been synthesized by hydrochemical deposition. The particle size of the silver sulfide powders has been determined by the Brunauer–Emmett–Teller method according to molecular nitrogen adsorption isotherms and, in the case of fine powders, by X-ray diffraction analysis according to diffraction reflection broadening. It has been shown that the density of the fine powders measured by helium pycnometry is underestimated compared with the true density, owing to the adsorption of helium by the highly developed surface of these powders.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Structural and electrical properties of T′-type Ln{sub 2}CuO{sub 4} (Ln = Pr, Nd, Sm, Eu and Gd) ceramics

T′-type Ln{sub 2}CuO{sub 4} (Ln = Pr, Nd, Sm, Eu and Gd) were successfully synthesized in phase pure form using conventional solid state reaction and sintering route. For all the Ln{sub 2}CuO{sub 4} samples, the solid state reaction temperature was found to be 950 °C and pure phase was realized only after 2-3 intermediate milling and solid state reaction cycles, irrespective of the lanthanide ion radius. Effect of lanthanide ion contraction on the structural properties was clearly revealed by the powder X-ray diffraction, with the XRD peaks observed to be shifting towards higher 2θ values with the decrease in Ln ionic radii. The optimum sintering temperature of these solid state reacted Ln{sub 2}CuO{sub 4} powder was found to be 1100 °C except for Pr{sub 2}CuO{sub 4} powder. The conductivity of these samples were tested over a wide temperature range (−100 to 150 °C), an anomaly was observed in the conductivity of all the Ln{sub 2}CuO{sub 4} samples near the antiferromagnetic ordering temperature of Cu (~ 30 °C), thus suggesting the bearing of ordering of magnetic moments on the electrical properties.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Morphologic and chemical characterization of products from hydrolysis of UF 6

Characterization of the chemical speciation and morphologies of products formed from hydrolysis of uranium hexafluoride (UF 6 ) is important for predicting dispersion and contamination of released material, or health consequences from inhalation of air-borne particles. Here, we report products of hydrolysis of UF 6 in which the quantity of water was insufficient for complete formation of UO 2 F 2 . Material was deposited onto carbon tape and aluminum. Scanning electron microscopy was employed to characterize textures and particle sizes, and powder X-ray diffraction analysis and μ-Fourier transform infrared absorption spectroscopy were used to characterize chemical speciation. These results revealed that the ratio of H 2 O to UF 6 , depository substrate composition, and storage conditions must be considered when evaluating chemical speciation, morphologic texture and particles size of UF 6 hydrolysis products. LA-UR-15-23846.

36 MATERIALS SCIENCE↗
DOE OSTI2024

PyFaults: A Python Toolkit for Stacking Fault Screening

PyFaults is an open-source Python library designed to model stacking fault disorder in crystalline materials and qualitatively assess the characteristic selective broadening effects in powder X-ray diffraction (PXRD). Here, the main capabilities of PyFaults are presented, including unit cell and supercell model construction, PXRD pattern calculation, assessment against experimental PXRD, and methods for rapid screening of candidate models within a set of possible stacking vectors and fault occurrence probabilities. This program aims to serve as a computationally inexpensive tool for identifying and screening potential stacking fault models in materials with planar disorder. Three diverse case studies, involving GaN, Li2MnO3 and Li3YCl6, are presented to illustrate the program functionality across a range of structure types and stacking fault modalities.

MATHEMATICS AND COMPUTING↗
DOE OSTI2014

Growth, structural and optical characterization of L-histidine 4-nitrophenolate (LHPNP) single crystals for NLO applications

Using slow evaporation solution growth technique, single crystals of L-histidine-4-nitro phenolate has been grown from the solution. Structural analyses were carried out by powder x-ray diffraction, FT-Raman, Fourier Transform Infrared and Nuclear Magnetic Resonance spectral methods to conform the grown crystals. Thermal stability of the grown crystals was studied by thermo-gravimetric (TG) and differential thermal analyses (DTA). UV-Vis spectral analysis has been carried out to find the transparency of the grown crystal. Nonlinear optical property has been confirmed by Kurtz powder technique. The PL measurements were carried out in Perkin Elmer LS 55 Luminescence spectrometer using 410 nm as excitation wavelength. The observed properties have confirmed that the grown crystal is suitable for nonlinear optical applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Low-temperature route to metal titanate perovskite nanoparticles for photocatalytic applications

MTiO 3 (M = Ca, Sr, Ba) nanoparticles were synthesized by a one-step room-temperature ultrasound synthesis in ionic liquid. The samples we gathered are characterized by X-ray diffraction, scanning electron microscopy, nitrogen adsorption, UV–vis diffuse reflectance, Raman and IR spectroscopy and their capability in photocatalytic hydrogen evolution and methylene blue degradation was tested. Powder X-ray diffraction and Raman spectroscopic investigations revealed the products to crystallize in the cubic perovskite structure. SEM observations showed that the obtained CaTiO 3 consists of nanospheres, BaTiO 3 of raspberry-like shaped particles of 20 nm in diameter. SrTiO 3 particles have cubic-like morphology with an edge length varying from 100 to 300 nm. SrTiO 3 exhibited the highest catalytic activity for photocatalytic H 2 evolution using only 0.025 wt.% Rh as co-catalyst and for the degradation of methylene blue under UV irradiation. The influence of parameters such as synthesis method, calcination temperature, and doping with nitrogen on the morphology, crystallinity, chemical composition, and photocatalytic acivity of SrTiO 3 was studied. Heating the as-prepared SrTiO 3 to 700 °C for extended time leads to a decrease in surface area and catalytic activity. Ionothermal prepared SrTiO 3 exhibits a higher activity than sonochemically prepared one without co-catalyst due to a synergistic effect of anatase which is present in small amount as a by-phase. Furthermore, after photodeposition of Rh, however, the activity is lower than that of the sonochemically prepared SrTiO 3 . Nitrogen-doped SrTiO 3 showed photocatalytic acivity under visible light irradiation.

36 MATERIALS SCIENCE↗