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DOE OSTI2025

In Situ Diffraction and Ex Situ Transmission X‐Ray Microscopy Studies of Solid‐State Upcycling for NMC Cathodes

Upcycling of recycled LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) cathodes offers an economical route to produce cathode materials with increased energy density (i.e., LiNi 0.8 Mn 0.1 Co 0.1 O 2 , NMC811) that meet the performance needs of present-day electric vehicles. In this work, solid-state upcycling of NMC622 via calcination with Ni(OH) 2 and LiOH was monitored using in situ synchrotron powder X-ray diffraction measurements. Sequential Rietveld refinements indicate that the calcination proceeds by initially converting Ni(OH) 2 to a rocksalt NiO phase followed by lithiation of NiO to form LiNiO 2 (LNO), with both NMC and LNO phases present in nearly equal proportions at the calcination endpoint. Variable-energy transmission X-ray microscopy tomograms of upcycled samples reveal that the NMC and LNO domains are intermixed at sub-micron length scales. Depth-dependent analysis of multi-elemental fitting maps matches the expected NMC811 composition at the secondary particle level and indicates that transition metal diffusion is not limited by the secondary particle size.

cathode upcycling↗

DOE OSTI2015

Synthesis, characterization and photo luminescence studies of uranyl doped SrBPO{sub 5}

SrBPO{sub 5}: UO{sub 2}{sup 2+} was synthesized using solid state reaction method and characterized using powder X-ray diffraction. PXRD data showed the formation of single phase confirming successful doping of UO{sub 2}{sup 2+}. Photo luminescence investigation informed stabilization of Uranium as Uranyl (UO{sub 2}{sup 2+}) in SrBPO{sub 5} matrix. Luminescence decay time data suggested two possible environments for UO{sub 2}{sup 2+} with two different life time values.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2022

Thermal behavior of ammonium octafluorodirhenate(III)

The thermal behavior of (NH 4 ) 2 [Re 2 F 8 ]·2H 2 O salt was studied in the temperature range 150–700 °C under flowing nitrogen gas. The decomposition products were studied by powder X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. Results are consistent with the formation of (NH 4 ) 2 [Re 2 F 8 ] salt at 150 °C, amorphous rhenium metal at 300 and 400 °C, and crystalline rhenium metal at 500 and 700 °C. A mechanism of formation of rhenium metal from (NH 4 ) 2 [Re 2 F 8 ]·2H 2 O was proposed. Here, the effect of crystallite size and lattice strain was evaluated at 500 and 700 °C from powder XRD peak broadenings using both Williamson–Hall and the modified Scherrer methods.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Synthesis and characterization of CuO nano particles using precipitation method

A simple and efficient synthesis of CuO nanoparticles was carried out by precipitation method using copper metal chips as precursor and sodium hydroxide as a stabilizing agent at different calcinations temperatures (100°C, 150°C, and 175°C). The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier Transform Infrared Spectroscopy (FTIR). XRD indicated monoclinic structure of CuO. SEM indicated the variation in nanostructures with the heating temperatures and FTIR inidcated Cu-O stretching frequencies. The CuO nanostructures with the average particle size of about 16.52 nm were prepared at 100°C for 3 hr. When the calcinations temperature was increased to 150°C and 175°C, CuO nanostructures with the particle size of about 17.41 nm, and 18.44 nm were obtained respectively. This aqueous precipitation method can give a large scale production of CuO nanoparticles easily.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2017

A Novel Coordination Polymer Based on Trinuclear Cobalt Building Blocks Cluster: Synthesis, Crystal Structure, and Properties

The title compound {[Co_3(μ_3-OH)(μ_2-H_2O)2(H_2O)_5(BTC)_2] · 6H_2O}{sub n} (H{sub 3}BTC is a 1,3,5-benzenetricarboxylic acid) was prepared and characterized by single crystal and powder X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric and elemental analyses. The single crystal X-ray diffraction reveals that the title compound consists of 1D infinite zigzag chains which were constructed by trinuclear cobalt cluster and BTC{sup 3–} ligand. Neighbouring above-mentioned 1D infinite zigzag chains are further linked by intermolecular hydrogen bonding to form a 3D supermolecular structure. In addition, the luminescent properties of the title compound were investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Synthesis and characterization of Ca{sup 2+} substituted barium niobate nanopaticles for photocatalytic and luminescence applications

Highlights: • Nanoparticles of Ca{sup 2+} (30 mol%) substituted BaNb{sub 2}O{sub 6} were synthesized. • Ca{sup 2+} ions occupy newer 8d Wyckoff positions rather than 4c. • Self-activated photoluminescence was observed. • Excellent H{sub 2} generation tendency from pure water under UV light was also observed. - Abstract: Ca{sup 2+} substituted barium niobate i.e. Ca{sub x}Ba{sub 1-x}Nb{sub 2}O{sub 6} (x = 0.3) compound in nanoparticles form was synthesized by a simple co-precipitation method for the first time and its structural characterization has been done by using powder X-ray diffraction data. Other characterizations were done by using transmission electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy and ultraviolet-visible spectroscopy. It was found that the Ca{sub x}Ba{sub 1-x}Nb{sub 2}O{sub 6} (x = 0.3) compound stabilizes in the orthorhombic phase (Pbcn space group) with the lattice parameters a = 14.984 Å, b = 5.761 Å and c = 5.216 Å. A representative TEM image shows the irregular sphere like morphology of the synthesized particles with the size ranging from 70 to 120 nm. The optical band gap energy was found to be 3.74 eV. It was observed that the synthesized nanoparticles exhibit excellent H{sub 2} evolution tendency and self–activated photoluminescence under the excitation of UV light. These activities were assigned to the nanocrystalline nature of the synthesized material.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Development of silver and zinc oxide decorated nanoclay containing polymeric composites for water disinfection applications

Contaminated drinking water has serious implications to the human health that could lead to death. The rapid growth of bacterial contamination in drinking water is alarming, and yet a robust and cost effective method with less limitation has not been developed. The current study is aimed at evaluating the performance of nanoclay composites dispersed in chitosan biopolymer as an antibacterial material. The performances of the composites were evaluated using the batch kinetic studies. Three composites of Ag-CtsB, ZnO-CtsB and Ag/ZnO-CtsB were prepared and evaluated against gram negative Escherichia coli and gram positive Enterococcus faecalis bacteria. The composites were characterized by powder X-ray diffraction, scanning electron microscope, energy dispersive spectroscopy and BET surface area measurements. Antibacterial activity results showed that the composites can be a potent bactericide material for water disinfection as they are highly effective against both gram negative and gram positive bacteria tested. Whereas both Ag-CtsB and ZnO-CtsB composites showed good antibacterial activity against bacteria with removal efficiency from 51%, best antibacterial activity was observed with Ag/ZnO-CtsB composite with removal efficiency from 78%. The results revealed that Ag/ZnO-CtsB composite is a promising bactericide that is highly effective against both gram negative and gram positive bacteria tested.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Effects of Co doping on the structure and physicochemical properties of hausmannite (Mn 3 O 4 ) and its transformation during aging

Hausmannite is a common low-valence manganese oxide mineral with a distorted spinel structure in surficial sediments. Although natural Mn oxides often contain various transition metal (TM) impurities, few studies have addressed the substitution mechanisms of TMs, such as cobalt (Co), with hausmannite and induced changes in the mineral physicochemical properties. In this study, Co-doped hausmannites with final Co/Mn molar ratios of 0.05 and 0.11 were synthesized and characterized by wet chemical analysis, powder X-ray diffraction (XRD), Fourier transformed infrared spectra (FTIR), high resolution transmission electron microscope (HRTEM), X-ray photoelectron spectroscopy (XPS) and X-ray absorption fine structure spectroscopy (XAFS). Co-doped samples have larger crystallite sizes and smaller specific surface areas than those of the hausmannite without Co. The Co cations exist in a mixed-valence of +3 and + 2. Powder XRD and acid dissolution experiments indicate that Co incorporates into the mineral structures, and increases the mineral structural stability. Co K-edge extended X-ray adsorption fine structure (EXAFS) analysis demonstrates that Co likely substitutes for lattice Mn(III). After aging at room temperature for three years, 14.1 ± 1.9% of pure hausmannite is transformed to manganite while only 2.6 ± 0.7% of manganite appears in the aged Co-doped sample with an initial Co/Mn molar ratio of 0.10. Finally, these results provide new insights into the incorporation mechanisms of TMs into low valence Mn oxides, and the stability of these minerals in natural environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Structural and photoluminescence studies of TiO{sub 2} nanoparticles synthesized by solution combustion method

In this study titanium dioxide nanoparticle is prepared by simple solution combustion method. The powder X-ray diffraction pattern indicates the prepared titanium dioxide nanoparticles crystalline nature with tetragonal structure. Also it shows the nanoparticle is anatase and rutile mixed phase. The Field Emission Scanning Electron Microscopy image shows the nanostructure of particles in the size range about 50 nm. Room temperature photoluminescence shows intrinsic defects of oxygen vacancies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2016

Photocatalytic properties of h-WO{sub 3} nanoparticles obtained by annealing and h-WO{sub 3} nanorods prepared by hydrothermal method

In the present study, two different methods for preparing hexagonal WO{sub 3} (h-WO{sub 3}) photocatalysts were used - controlled thermal decomposition and hydrothermal synthesis. WO{sub 3} nanoparticles with hexagonal structure were obtained by annealing (NH{sub 4}){sub x}WO{sub 3-y} at 500 °C in air. WO{sub 3} nanorods were prepared by a hydrothermal method using sodium tungstate Na{sub 2}WO{sub 4}, HCl, (COOH){sub 2} and NaSO{sub 4} precursors at 200 °C. The formation, morphology, structure and composition of the as-prepared nanoparticles and nanorods were studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy combined with energy-dispersive X-ray spectroscopy (SEM-EDX). The photocatalytic activity of the h-WO{sub 3} nanoparticles and nanorods was studied by decomposing methyl orange in aqueous solution under UV light irradiation.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Structure and physical properties of RT{sub 2}Cd{sub 20} (R=rare earth, T=Ni, Pd) compounds with the CeCr{sub 2}Al{sub 20}-type structure

Eleven new compounds, R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Sm, Gd, Tb) and R Pd{sub 2}Cd{sub 20} (R=Ce, Pr, Sm), were grown as single crystals in high temperature cadmium-rich solutions. They crystallize in the cubic CeCr{sub 2}Al{sub 20}-type structure (Fd3{sup ¯}m, Z=8) as characterized by measurements of powder X-ray diffraction. Electrical resistivity, magnetization, and specific heat measurements were performed on R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Sm, Gd, Tb) single crystals. Whereas YNi{sub 2}Cd{sub 20} and LaNi{sub 2}Cd{sub 20} exhibit unremarkable metallic behavior, when magnetic moments from localized 4f electron states (Gd{sup 3+}–Tb{sup 3+}) are embedded into this host, they exhibit ferromagnetic order with values of the Curie temperature T{sub C} for R Ni{sub 2}Cd{sub 20} (R=Gd, and Tb) which scale with the de Gennes factor. - Graphical abstract: Specific heat divided by temperature C/T vs. T for single crystals of R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Gd, and Tb). Left inset: Low temperature C/T vs. T{sup 2} for LaNi{sub 2}Cd{sub 20}. The solid line represents a linear fit of the data. Right inset: Low-temperature C/T data vs. T for R=Ce–Nd, Gd, and Tb; magnetic ordering temperatures are indicated by arrows. - Highlights: • R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Sm, Gd, Tb) single crystals synthesized for the first time. • R Pd{sub 2}Cd{sub 20} (R=Ce, Pr, Sm) single crystals synthesized for the first time. • Single crystals are of good metallurgical quality (large RRR values). • NdNi{sub 2}Cd{sub 20} orders antiferromagnetically at T{sub N}=1.5 K. • R Ni{sub 2}Cd{sub 20} (R=Sm, Gd, Tb) order ferromagnetically.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Early age hydration and application of blended magnesium potassium phosphate cements for reduced corrosion of reactive metals

Highlights: • Magnesium potassium phosphate cements were studied for nuclear waste encapsulation. • The optimised formulation in this study was determined to be 0.24 w/s ratio. • Different reaction kinetics were discovered for the FA/MKPC and BFS/MKPC binders. • Struvite-K was the only crystalline reaction product observed via in-situ SXPD. • Uranium trials revealed MKPC corrosion was reduced compared to a UK nuclear grout. Magnesium potassium phosphate cements (MKPC) were investigated to determine their efficacy towards retardation of reactive uranium metal corrosion. Optimised low-water content, fly ash (FA) and blast furnace slag (BFS) blended MKPC formulations were developed and their fluidity, hydration behaviour, strength and phase assemblage investigated. In-situ time resolved synchrotron powder X-ray diffraction was used to detail the early age (~60 h) phase assemblage development and hydration kinetics, where the inclusion of BFS was observed to delay the formation of struvite-K by ~14 h compared to FA addition (~2 h). All samples set within this period, suggesting the possible formation of a poorly crystalline binding phase prior to struvite-K crystallisation. Long-term corrosion trials using metallic uranium indicated that MKPC systems are capable of limiting uranium corrosion rates (reduced by half), when compared to a UK nuclear industry grout, which highlights their potential application radioactive waste immobilisation.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Enhancing the photovoltaic performance of CdTe/CdS solar cell via luminescent downshifting using K{sub 2}SiF{sub 6}:Mn{sup 4+} phosphors

The efficiency of CdTe/CdS solar cell can be significantly improved by using luminescent down-shifting material on their front surface. Taking this into account a red emitting phosphor K{sub 2}Si{sub 1-x}F{sub 6}:xMn{sup 4+} (x=10 to 25 mol %) has been synthesized through wet chemical method. The as-synthesized materials were characterized by powder x-ray diffraction (XRD) and photoluminescence (PL) techniques. The photoluminescence studies of K{sub 2}SiF{sub 6}:Mn{sup 4+} revealed enhancement in the emission intensity, when Mn{sup 4+} concentration was increased from 10 mol % to 25 mol %. This red emitting phosphor efficiently absorbs the photons typically in the region 300-500 nm and re-emits in the region where the photovoltaic device exhibits significantly better response. The results show the possibility of enhancing the photovoltaic conversion efficiency of CdTe thin film solar cell by modifying the absorption spectra and utilising the energy in the UV-blue part of the solar spectrum.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Phase evolution studies in CaZrTi{sub 2}O{sub 7}−RE{sub 2}Ti{sub 2}O{sub 7} (RE = Nd{sup 3+}, Sm{sup 3+}) system: Futuristic ceramic host matrices for nuclear waste immobilization

Series of compositions with general stoichiometry as Ca{sub 1−x}Zr{sub 1−x}RE{sub 2x}Ti{sub 2}O{sub 7} (RE = Nd{sup 3+}, Sm{sup 3+}) were prepared by solid state reaction and characterized by powder x-ray diffraction technique to unravel the phase fields in the title systems. The phase fields in CaZrTi{sub 2}O{sub 7−}Nd{sub 2}Ti{sub 2}O{sub 7} and CaZrTi{sub 2}O{sub 7−}Sm{sub 2}Ti{sub 2}O{sub 7} systems differed significantly at the rareearth rich regions. The common phase fields like zirconolite-2M, zirconolite-4M, cubic perovskite are observed at the zirconolite rich regions of both systems. Depending on the structure of RE{sub 2}Ti{sub 2}O{sub 7} phase, the cubic pyrochlore or monoclinic RE{sub 2}Ti{sub 2}O{sub 7} phases are observed in the studied system. The observed phase fields in these two systems indicate ionic radius of the rare-earth ion has a dominating role in the phase relations. Further details of the phases and their homogeneity are explained in the text of the manuscript.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Scaling spin–phonon and spin–spin interactions in magnetoelectric Gd{sub 1−x}Y{sub x}MnO{sub 3}

We present a systematic study of the structure and lattice dynamics at room temperature, and the phonon behavior at low temperatures in orthorhombic Gd{sub 1−x}Y{sub x}MnO{sub 3} manganites, with 0≤x≤0.4. Powder x-ray diffraction and Raman scattering at ambient conditions reveal that the Jahn–Teller distortion is composition-independent, while the Mn–O1–Mn bond angle increases by about 0.5° from x=0 to x=0.4. The spin–phonon coupling was ascertained from the relation between the renormalized wavenumber of the in-plane O2 stretching mode, associated with the spin–spin correlation function. The balance between competitive magnetic interactions is discussed based on the temperature dependence of the phonon frequency renormalization. - Graphical abstract: Wavenumber of the in-plane O2 stretching mode as a function of the spin–spin correlation function, for GdMnO{sub 3} (a), and Gd{sub 0.8}Y{sub 0.2}MnO{sub 3} (b). - Highlights: • Crucial role of structural distortions induced by ion substitution. • Tuning of magnetic interactions through ion substitution. • Facing spin–phonon coupling and competitive exchange magnetic interactions. • Scaling of spin–phonon and spin–spin mechanisms.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Impact of temperature on zinc oxide particle size by using sol-gel process

Zinc oxide (ZnO) nanoparticles were prepared and synthesized via sol-gel method, by using citric acid as a precursor. The impact of annealing on the particle size was investigated. Based on the results from the Thermogravimetric Analysis (TGA), three different annealing temperature which is 500, 600 and 700 °C were chosen followed by the characterization of the ZnO nanoparticle by using Powder X-Ray Diffraction (PXRD), Transmission Electron Microscopy (TEM) and Field Emission Scanning Electron Microscopy (FESEM). Results showed that the crystallite size estimated from PXRD increased with the annealing temperature which was hexagonal structure for ZnO. TEM further revealed the same tendency which the Zn NPs size also increased with the annealing temperature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

In situ high-temperature X-ray diffraction study of Sc-doped titanium oxide nanocrystallites

Titanium dioxide is an inexpensive wide-gap highly ionic semiconductor with striking photocatalytic capabilities in several heterogeneous photoredox reactions. A small crystal size is desirable to maximize the surface area, since photocatalytic reactions occur at the surface of a photocatalyst. Presented in this work are the synthesis and microstructural characterization of 4 at.% Sc-doped TiO 2 (4SDT) prepared by water-based co-precipitation. The crystal structure of 4SDT was examined via in situ high-temperature powder X-ray diffraction experiments from 25 to 1200°C. Rietveld analysis revealed single-phase anatase up to 875°C, while at 900°C the anatase-to-rutile phase transformation occurred and at higher temperatures additional reflections of Sc-rich phases (Sc 2 TiO 5 from 975°C and Ti 3 Sc 4 O 12 or Sc 2 O 3 at 1200°C) were observed. Debye function analysis (DFA) was applied to model the total scattering pattern directly in reciprocal space, allowing the reconstruction of Ti vacancies. Both Rietveld and DFA methods were applied to estimate the nanocrystallite size and shape with consistent growth in crystallite size with temperature: an ellipsoid shape with equatorial ~4.7 nm / axial (001) ~6.9 nm at 25°C to equatorial ~27.9 nm / axial (001) ~39.6 nm at 900°C refined by Rietveld analysis, versus a cylinder shape with D a , b = 4.3 nm and size dispersion σ ab = 1.5 nm, L c = 4.9 nm and σ c = 2.3 nm at 25°C to D a , b = 21.4 nm, σ ab = 8.3 nm, L c = 23.9 and σ c = 10.9 nm at 900°C estimated by DFA. The microstructural changes obtained by Rietveld and DFA methods were supported by high-resolution transmission electron microscopy image analysis, as well as by the less direct nitrogen sorption techniques that provide information on the size of non-agglomerated and dense particles. The Ti site-occupancy factor showed a linear increase from 0.6–0.8 at 25°C to unity at 900°C for anatase, and from ~0.7 at 900°C to unity at 1200°C for rutile, via Rietveld analysis and DFA.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Nanorods and nanoparticles of titanium dioxide and their use in dye sensitized solar cells

Mesoporous TiO{sub 2} nanorods/nanorods were successfully synthesized by hydrothermal process at 170 °C for 72 hr. The powder X-ray diffraction pattern shows large fraction of anatase phase with good crystalline behavior of the prepared materials. The specific surface area and pore volume of the synthesized material are about 84.83 m{sup 2}/g and 0.1316 cc/g respectively. The morphological results show that the TiO{sub 2} nanorods had diameter of ~ 25 nm and the length of ~ 80 nm. The nanoparticles have 20 nm in size. The current-voltage curve shows that the synthesized TiO{sub 2} nanostructure results in 36.7 % higher solar cell efficiency than commercial P25.

77 NANOSCIENCE AND NANOTECHNOLOGY↗