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All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Two new helical compounds based on Keggin clusters and N-donor multidentate ligand: Syntheses, structures and properties

Two isostructural polyoxometalate-based inorganic–organic hybrids with 1D helical chain, [CuH{sub 3}L{sub 2}(GeMo{sub 12}O{sub 40})]·2H{sub 2}O (1) and [CuH{sub 3}L{sub 2}(SiMo{sub 12}O{sub 40})]·2H{sub 2}O (2), where L=2,4,5-tri(4-pyridyl)-imidazole have been synthesized under hydrothermal conditions. It is the first time to use the L ligand to synthesis the Keggin-type polyoxometalate-based inorganic–organic hybrids. The two compounds possess the left- and right-handed helical chains and the POMs as pendants attach in the helical chains through Cu–O bonds. The two compounds have been characterized by elemental analyses, infrared (IR) spectroscopy, powder X-ray diffraction (PXRD), X-ray photoelectron spectra (XPS), thermogravimetric analysis (TGA) and photoluminescent spectroscopy. Moreover, nitrogen adsorption−desorption measurement, electrochemical and photocatalysis properties for degradation of methylene blue (MB) upon a UV irradiation of compound 1 have been examined. - Graphical abstract: Two new compounds, [CuH{sub 3}L{sub 2}(GeMo{sub 12}O{sub 40})]·2H{sub 2}O (1) and [CuH{sub 3}L{sub 2}(SiMo{sub 12}O{sub 40})]·2H{sub 2}O (2) have been synthesized under hydrothermal conditions. The two compounds possess the left- and right-handed helical chains. - Highlights: • The tridentate L ligand is first used to synthesis Keggin-type polyoxometalates. • The two compounds possess the left- and right-handed Cu–L helical chains. • Relationship between surface properties and photocatalytic activity was studied. • Two compounds exhibit photoluminescence of ligand-to-metal charge transfer.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Photoluminescence properties of AlN-doped BaMgAl{sub 10}O{sub 17}:Eu{sup 2+} phosphors

Highlights: ► Ideal hexagonal shape particle size in 5 μm and 2.5–3 μm in thickness are obtained. ► The growth mechanism is studied by a computer simulation. ► The influence of introduced AlN on the sites of Eu{sup 2+} and photoluminescence properties was investigated. - Abstract: The AlN-doped BaMgAl{sub 10}O{sub 17}:Eu{sup 2+} phosphors were synthesized by conventional solid-state reaction. Powder X-ray diffraction (XRD), scanning electron microscope (SEM) and photoluminescence spectrum (PL) were used for characterization. The growth mechanism was carried out by computer simulation with CASTEP application, and revealed that an ideal hexagonal shape, particle size in 5 μm and 2.5–3 μm in thickness, could be obtained by AlN doping. Additionally, due to the low electronegativity of N{sup 3−}, the AlN-doped sample showed 35% increase in PL intensity and improvement of thermal stability. These fine particle size and better photoluminescence properties are expected to be applicable to industrial production of BaMgAl{sub 10}O{sub 17}:Eu{sup 2+} phosphors.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Efficient extraction of inorganic selenium from water by a Zr metal–organic framework: investigation of volumetric uptake capacity and binding motifs

Strict monitoring and control of selenium concentrations in freshwater supplies is critical to safeguarding human health and aquatic life. A handful of previously investigated sorbents exhibit noteworthy gravimetric (mg g -1 ) Se uptake capacities; however, often display insufficient volumetric (mg cm -3 ) capacities, thereby requiring large volumes of material for commercial implementation. In this paper, in pursuit of mitigating this material inefficiency, we investigated the selenite (SeO 3 2- ) and selenate (SeO 4 2- ) affinity of MOF-808, a Zr-based metal–organic framework with a high density of potential Se oxyanion binding sites. MOF-808 recorded exceptional volumetric and gravimetric Se oxyanion capacities of 133 mg g -1 (127 mg cm -3 ) and 118 mg g -1 (112 mg cm -3 ) for aqueous selenite and selenate, respectively. Single-crystal X-ray diffraction studies revealed that selenite and selenate can bind at the MOF node via two distinct binding motifs, an η 2 μ 2 motif in which the oxyanion coordinates to two different metal atoms in a single node, and a μ 2 motif in which the oxyanion interacts with only a single metal atom. Finally and furthermore, powder X-ray diffraction (PXRD) patterns and N 2 adsorption/desorption isotherms confirm the retention of bulk crystallinity and porosity after the uptake of Se oxyanions.

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

Blue emission of Eu{sup 2+} doped LaMgAl{sub 11}O{sub 19} phosphor prepared by combustion synthesis method

Blue-emitting phosphor LaMgAl{sub 11}O{sub 19}:Eu{sup 2+} has been synthesized successfully at 500 °C by one step combustion synthesis method. The as-synthesized materials were characterized by powder x-ray diffraction (XRD) and photoluminescence (PL) techniques. Upon 365 nm excitation, emission spectra of the LaMgAl{sub 11}O{sub 19}:Eu{sup 2+} phosphors show a blue band at 450 nm. The excitation spectra corresponding to 4f{sup 7}-4f{sup 6}5d transition of Eu{sup 2+} cover the spectral range of 280–430 nm. The concentration quenching of Eu{sup 2+} in the LaMgAl{sub 11}O{sub 19} host was determined to be 3 mol%. The CIE chromaticity of LAM: Eu{sup 2+} phosphors was compared with the commercial BAM.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Anion-controlled assembly of metal 3,5-bis(benzimidazol-1-ylmethyl) benzoate complexes: Synthesis, characterization and property

Hydrothermal reactions of 3,5-bis(benzimidazol-1-ylmethyl)benzoic acid (HL) with Cd(II), Cu(II) and Zn(II) salts provide eight new metal complexes which were characterized by single crystal and powder X-ray diffraction, IR, elemental and thermogravimetric analyses. Two cadmium frameworks [Cd(L){sub 2}]·2H{sub 2}O (1) and [Cd(L)Cl] (2) have 3D structures with (4{sup 2}.6{sup 5}.8{sup 3})(4{sup 2}.6) and rtl (4.6{sup 2}){sub 2}(4{sup 2}.6{sup 10}.8{sup 3}) topologies, respectively. Structural diversity of four copper complexes [Cu{sub 3}(L){sub 2}]·NO{sub 3}·0.5H{sub 2}O (3), [Cu{sub 2}(HL){sub 2}(SO{sub 4})]·3.5H{sub 2}O (4), [Cu(L)(bdc){sub 0.5}]·1.5H{sub 2}O (5) and [Cu{sub 2}(L)(HL)(Hbdc)] (6) (H{sub 2}bdc=1,4-benzenedicarboxylic acid) is achieved through the alteration of copper salts and addition of auxiliary ligand. As a result, 3 has a 1D ladder structure, 4 is a discrete dinuclear complex, 5 displays a (3,4)-connected 2-nodal 3-fold interpenetrating framework with (4{sup 2}.6.10{sup 2}.12)(4{sup 2}.6) topology, 6 exhibits a 4-connected uninodal 2D sql (4{sup 4}.6{sup 2}) network. Within the zinc series, ZnCl{sub 2} and ZnSO{sub 4} were used for the syntheses of [Zn(L)Cl] (7) and [Zn(L)(SO{sub 4}){sub 0.5}]·2H{sub 2}O (8), respectively. 7 shows a 3-connected uninodal 2D hcb network with (6{sup 3}) topology and 8 is a (3,6)-connected 2-nodal 3D framework with (4{sup 2}.6){sub 2}(4{sup 4}.6{sup 2}.8{sup 8}.10) topology. The luminescent properties of the Cd(II) and Zn(II) complexes were investigated. - Graphical abstract: Eight new complexes have been successfully synthesized from the hydrothermal reactions of Cd(II), Cu(II) and Zn(II) salts with 3,5-bis(benzimidazol-1-ylmethyl)benzoic acid. The complexes exhibited anion-controlled structural diversity. - Highlights: • Metal complexes have diverse structures of 1D chains, 2D networks and 3D frameworks. • Anion-controlled assembly of the complexes is reported. • The luminescent properties of the Cd(II) and Zn(II) complexes were investigated.

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

Novel mixed hydroxy-carbonate precursor assisted synthetic technique for LiNi{sub 1/3}Mn{sub 1/3}Co{sub 1/3}O{sub 2} cathode materials

Highlights: • MHC method used to overcome drawbacks of solid state synthesized materials. • Least cation mixing, phase purity, good reversibility and rate capability achieved. • XRD I {sub 0} {sub 0} {sub 3}/I{sub 1} {sub 0} {sub 4} factor, indicating electrochemical reactivity is maximum at 1.6984. • Li/LiNi{sub 1/3}Mn{sub 1/3}Co{sub 1/3}O{sub 2} cell delivered an initial discharge capacity of 175 mAh g{sup −1}. - Abstract: Novel mixed hydroxy-carbonate (MHC) precursors were used to synthesis technique of LiNi{sub 1/3}Mn{sub 1/3}Co{sub 1/3}O{sub 2} cathode material. The powder X-ray diffraction (XRD) pattern of the synthesized LiNi{sub 1/3}Mn{sub 1/3}Co{sub 1/3}O{sub 2} cathode materials exhibited a hexagonal cell with a = 2.8535 Å and c = 14.2040 Å. Fourier transform infrared spectroscopy (FT-IR) spectrum of MHC and LiNi{sub 1/3}Mn{sub 1/3}Co{sub 1/3}O{sub 2} consistent with vibration modes of functional group. Presence of sub-micrometer particle size (200 nm) and highly crystalline morphology confirmed using scanning electron microscopy (SEM). X-ray photoelectron spectroscopy (XPS) suggested that oxidation state of the transition metals; Ni in +2, Mn in +4 and Co in +3 states, respectively in LiNi{sub 1/3}Mn{sub 1/3}Co{sub 1/3}O{sub 2} cathode materials. Cyclic voltammograms (CV) revealed only one major redox couple at 4 V and suggested the absence of structural transitions from hexagonal to monoclinic structure. The Li vs. LiNi{sub 1/3}Mn{sub 1/3}Co{sub 1/3}O{sub 2} cell delivered an initial discharge capacity of 175 mAh g{sup −1} in the voltage range 2.5–4.6 V @ 0.1 C.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Structural and magnetic investigation of In{sub 2}Fe{sub 2−x}Ga{sub x}CuO{sub 7}

The solid solution of In{sub 2}Fe{sub 2−x}Ga{sub x}CuO{sub 7} (space group P6{sub 3}/mmc) was synthesized and investigated through X-ray diffraction and magnetic susceptibility studies. Limited changes to the lattice parameters were observed as a result of the similar ionic radii for Fe{sup 3+} and Ga{sup 3+} in the trigonal bipyramidal (TBP) crystallographic site. An increase in the Weiss temperature, along with spin glass behavior are observed from x=0 to x=2, but irregularities in the trend are apparent for x=0.75 and 1. With the highest concentration in magnetic ions, In{sub 2}Fe{sub 2}CuO{sub 7} appears to have competing nearest neighbor interactions that produce a suppression of the Curie tail and the experimental magnetic moment. In comparison to InFe{sub 1−x}Ga{sub x}CuO{sub 4}, both solid solutions show an invariable progression of the lattice parameters, but the magnetic properties are greatly affected by the distinct TBP layering schemes. - Graphical abstract: Solid solution of In{sub 2}Fe{sub 2−x}Ga{sub x}CuO{sub 7} has been synthesized and analyzed with powder X-ray diffraction and DC magnetic susceptibility studies. The magnetic ground state has been investigated through cation substitution and compared to that of InFe{sub 1−x}Ga{sub x}CuO{sub 4}. Highlights: • The complete solid solution of In{sub 2}Fe{sub 2−x}Ga{sub x}CuO{sub 7} has been synthesized. • Limited changes in the lattice parameters were observed through XRD refinements. • Spin glass magnetic interactions were found to depend on Fe{sup 3+} content. • The layering of the TBP greatly affects the observed magnetic interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Low-temperature synthesis, structural and magnetic properties of self-dopant LaMnO{sub 3+δ} nanoparticles from a metal-organic polymeric precursor

Graphical abstract: Monophasic and highly crystalline Self-dopant LaMnO{sub 3+δ} nanoparticles (72 nm) have been successfully synthesized at low temperature (773 K) by metal citrate complex method based on Pechini-type reaction route which showed ferromagnetic interaction. Surface areas of LaMnO{sub 3+δ} nanoparticles were found to be 157.4 and 153 m{sup 2} g{sup −1} for the samples annealed at 773 K and 1173 K, respectively. - Highlights: • Self-dopant LaMnO{sub 3+δ} nanoparticles using Pechini-type reaction route at 773 K. • Size range varies from 72 to 80 nm. • Surface area varies from 153 to 157 m{sup 2} g{sup −1}. • Extensive characterization using sophisticated techniques. - Abstract: Self-dopant LaMnO{sub 3+δ} nanoparticles have been successfully synthesized by metal citrate complex method based on Pechini-type reaction route, at low temperature (773 K). Powder X-ray diffraction and transmission electron microscope revealed pure and nanostructured phase of LaMnO{sub 3+δ} (δ = 0.125) with an average grain size of ∼72 nm (773 K) and ∼80 nm (1173 K). DC-magnetization measurements under an applied magnetic field of H = ±60 kOe showed an increase in the magnetization with the increase of calcination temperature. Ferromagnetic nature shown by non-stoichiometric LaMnO{sub 3+δ} was verified by well-defined hysteresis loop with large remanent magnetization (M{sub r}) and coercive field (H{sub c}). Surface areas of LaMnO{sub 3+δ} nanoparticles were found to be 157.4 and 153 m{sup 2} g{sup −1} for the samples annealed at 773 K and 1173 K, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Crystal structure and dielectric properties of layered perovskite-like solid solutions Bi{sub 3–x}Y{sub x}TiNbO{sub 9} (x = 0, 0.1, 0.2, 0.3) with high Curie temperature

The structural and electrophysical characteristics of a number of solid solutions of layered perovskite-like oxides Bi{sub 3–x}Y{sub x}TiNbO{sub 9} (x = 0, 0.1, 0.2, 0.3) have been studied. According to the data of powder X-ray diffraction, all the compounds are single-phase with the structures of two-layer Aurivillius phases (m = 2) with the orthorhombic crystal lattice (space group A2{sub 1}am). The temperature dependence of the relative permittivity ε/ε0(T) compounds have been measured and showed that the Curie temperature of the perovskite-like oxides Bi{sub 3–x}YxTiNbO{sub 9} linearly increases with the substituting parameter x up to T{sub C} = 965°C.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Synthesis, structure and photoluminescence properties of Sm{sup 3+}-doped BiOBr phosphor

Well-crystallized tetragonal layered BiOBr and Bi{sub 0.95}Sm{sub 0.05}OBr phosphors were prepared by the solid state method. These compounds were characterized using powder X-Ray diffraction and photoluminescence technique. In PL spectra, the electric dipole transitions dominate than other transitions which indicate that the Sm{sup 3+} ions occupy a site with an inversion center of BiOBr. CIE chromaticity diagram confirmed that these phosphors can be useful in the fabrication of red component in white light emitting diodes (WLEDs) for display device applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Combustion synthesis of MgO nanoparticles using plant extract: Structural characterization and photoluminescence studies

Magnesium oxide nanoparticles (MgO Nps) have been successfully synthesized via solution combustion method using Parthenium plant extract as fuel for the first time. Powder X-ray diffraction (PXRD) pattern reveal that product belongs to the cubic phase (Periclase). FTIR spectrum shows the band at 822 cm{sup −1} indicates the formation of cubic periclase MgO. The optical band gap of MgO Nps estimated from UV –Vis spectrum was found to be in the range 5.40–5.45 eV. SEM images showed that, the product is agglomerated and particle in nature. Photoluminescence (PL) studies shows violet emission at 390 nm, blue emission at 470 nm and green emission at 550 nm. MgO Nps shows good photocatalytic activity for the degradation of methylene blue (MB) dye under UV/Sun light irradiation.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
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↗
NASA NTRS1989

Mechanical alloying, characterization and consolidation of Ti-Al-Ni alloys

Mechanical alloying is being investigated as a processing route for the production of aluminide intermetallics. This program involves powder production and characterization, consolidation and thermal treatments and determination of microstructure-property relationships. An attritor mill is being used to produce powder in lots up to 1000 grams and the processing parameters are being systematically varied to establish the optimum milling conditions. The mill is being instrumented to generate data related to the processing to provide a basis for theoretical modeling. Powder is being characterized using thermal analysis, optical and electron microscopy and X-ray diffraction. Particle size distributions and powder density are being determined. Consolidation of the powder is being approached in several different ways including, cold isostatic pressing, sintering, extrusion and hot pressing. The results of the program so far will be presented and future directions discussed.

Nash, P.↗
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↗