Search NASA⌕ Search

SEARCH · Search NASA

Results for “AM Powder Characterization”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

A Thorium Metal‐Organic Framework with Outstanding Thermal and Chemical Stability

Abstract A new thorium metal‐organic framework (MOF), Th(OBA) 2 , where OBA is 4,4′‐oxybis(benzoic) acid, has been synthesized hydrothermally in the presence of a range of nitrogen‐donor coordination modulators. This Th‐MOF, described herein as GWMOF‐13, has been characterized by single‐crystal and powder X‐ray diffraction, as well as through a range of techniques including gas sorption, thermogravimetric analysis (TGA), solid‐state UV/Vis and luminescence spectroscopy. Single‐crystal X‐ray diffraction analysis of GWMOF‐13 reveals an interesting, high symmetry (cubic Ia d ) structure, which yields a novel srs‐a topology. Most notably, TGA analysis of GWMOF‐13 reveals framework stability to 525 °C, matching the thermal stability benchmarks of the UiO‐66 series MOFs and zeolitic imidazolate frameworks (ZIFs), and setting a new standard for thermal stability in f‐block based MOFs.

Carter, Korey P.↗
DOE OSTI2018

Magnetic Properties of Co-doped Bismuth Oxide (δ-Bi{sub 2}O{sub 3}) at Low Temperature

The (Bi{sub 2}O{sub 3}){sub 1−x−y}(Gd{sub 2}O{sub 3}){sub x}(Lu{sub 2}O{sub 3}){sub y} material compounds were prepared by using the solid-state reaction technique under normal air conditions. The heat treatments of the ternary samples were performed firstly at 800 °C for 48 h and then at 750 °C for 100 h. The structural, morphological, and magnetic properties of the materials were characterized by X-ray powder diffraction (XRD), scanning electron microscope, and a Quantum Design PPMS-9T system, respectively. From the XRD results, it was found that the phases of all of the samples consisted of the fluorite-type face-centered cubic δ-Bi{sub 2}O{sub 3} phase. It was observed that the microstructure of the samples is uniformly distributed on the samples’ surface. The temperature dependence of magnetization (M–T) measurements showed that the magnetization rose sharply at the critical temperature. The calculated critical temperature values vary from 22.19 to 56.61 K for the samples. All of the samples displayed the paramagnetic behavior. The paramagnetic behavior started from 300 K to very low temperature which varied from 22.19 to 56.61 K. The coercive rise on the magnetization below 22.19 K or 56.61 K with decreasing temperature causes a phase transformation in the δ-Bi{sub 2}O{sub 3} system. This sudden increment was considered as a ferromagnetic or ferrimagnetic phase transition.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Morphology, UV–visible and ellipsometric studies of sodium lithium orthovanadate

Sodium lithium orthovanadates were prepared by the classic ceramic method technique. Structure, phase purity, composition, and morphology were characterized by X-ray powder diffraction, infrared spectroscopy, energy dispersive spectroscopy, scanning-electron microscopy and atomic force microscopy. The optical properties of Na{sub x}Li{sub 1−x}CdVO{sub 4} (x = 0.5, 1) compounds prepared were recorded at room temperature using ultra-visible and ellipsometric spectroscopies in the spectral range (200–800) nm. The average reflectance of the pellets showed high reflectivity (over 80%) in the visible spectrum. The UV–Vis absorption bands are assigned to the charge transfer from the oxygen ligands to the central vanadium atom inside the [VO{sub 4}]{sup 3−} groups in the orthovanadate compounds. The optical band gaps E{sub g} of both samples are evaluated using Kubelka–Munk function. The analysis of the data revealed the existence of optical allowed direct transition for Na{sub x}Li{sub 1−x}CdVO{sub 4} (x = 0.5, 1). Spectroscopic ellipsometry measurements have been performed on Na{sub x}Li{sub 1−x}CdVO{sub 4} (x = 0.5, 1) specimens and their optical properties were analyzed using the Cauchy model.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
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 OSTI2018

Microstructural development of a C/C-ZrC-Cu composite prepared by reactive melt infiltration with Zr/Cu powder mixture

Highlights: • The composite was prepared by reactive melt infiltration with Zr/Cu powder mixture. • Some ZrC particles coalesced into a continuous layer around the pyrolytic carbon. • Nano-sized inclusions of Cu–ZrC were formed inside some ZrC particles. • Cu–rich phase gathered at the interface between the ZrC layer and pyrolytic carbon. - Abstract: Zirconium carbide (ZrC) was introduced into porous carbon/carbon(C/C) preforms by reactive melt infiltration (RMI) using Zr/Cu powder mixture as the infiltrator. Characterization results revealed that ZrC particles were present in the infiltration matrix in two forms, some of which coalesced into a continuous layer around the pyrolytic carbon (PyC) while the others were dispersed within Cu phase which was distributed throughout the matrix. Nano-sized inclusions of Cu-ZrC were detected inside some ZrC particles. Furthermore, Cu-rich phase was observed at the interface between the continuous ZrC layer and PyC. The formation of Cu-ZrC mixture and Cu-rich phase was attributed to the trapping mechanism that some Zr-Cu-based liquid remained during the coalescence of ZrC particles or the formation of the continuous ZrC layer.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Alternating current conduction mechanisms of RbMgPO4 compound

Highlights: • Two displacive reversible phase transitions located at T{sub 1} = 442/432 K and T{sub 2} = 460/445 K (heating/cooling). • The temperature dependence of conductivity was described in terms of Arrhenius relation. • The ac conductivity of this compound is proportional to ω{sup s} where the s values are between 0 and 2. • The (CBH) model was found to be the appropriate transport mechanism in RbMgPO{sub 4} compound. - Abstract: Rubidium magnesium monophosphate (RbMgPO{sub 4}) compound was prepared from highly pure constituents by solid state reaction. It was characterized by X-ray powder diffraction, IR, Raman, differential scanning calorimetry (DSC) and impedance spectroscopy. The infrared and Raman spectra were interpreted on the basis of PO{sub 4}{sup 3−} vibrations. DSC revealed two displacive and reversible phase transitions at T{sub 1} = 442/432 K and T{sub 2} = 460/445 K (heating/cooling). The electrical conductivity was measured in the frequency and temperature range 200 Hz-5 MHz and 423 K–523 K, respectively. The obtained results were analysed by fitting the experimental data to an equivalent circuit model. The temperature dependence of alternating and direct current conductivities (σ{sub ac}, σ{sub dc}) confirms the observed transitions in the calorimetric study; they were described in terms of Arrhenius relation. The activation energy’s values were determined in each phase. The AC conductivity behavior is ensured by a single process defined as a hopping transport mechanism. The conductivity frequency dependence was interpreted using the correlated barrier-hopping model (CBH) in all phases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Biogas reforming over Ni catalysts dispersed in different mixed oxides containing Zn2+, Al3+ and Zr4+cations

Highlights: • The oxides mixture containing NiO, ZnO, Al{sub 2}O{sub 3}, NiAl{sub 2}O{sub 4} and ZnAl{sub 2}O{sub 4} was detected. • The results exhibited intermediate interactions between Ni0 and other phases. • Dry reforming of methane was applied to production of synthesis gas. • Deposition of the carbon filamentous on the catalysts surface was observed. - Abstract: The active phase plays an important role in the catalytic activity. However, its applicability is directly associated with other present phases in the mixture. In view of this, we report the performance of Ni catalysts dispersed on mixed oxides containing Zn{sup 2+}, Al{sup 3+} and Zr{sup 4+}cations in biogas reforming. For this purpose, the samples were characterized by X-ray powder diffraction, which showed the formation of a homogeneous mixture of binary (NiO, ZnO, ZrO{sub 2} and Al{sub 2}O{sub 3}) and ternary (NiAl{sub 2}O{sub 4} and ZnAl{sub 2}O{sub 4}) oxides. The temperature-programmed reduction (H{sub 2}-TPR) provided information on the catalyst reduction. The performance of the catalysts was evaluated using two reduction temperatures (650 °C and 750 °C). The reactions were carried out at 750 °C, where the Ni/ZnAlZr catalyst presented the highest CO{sub 2} conversion attributed to the basic sites, which favored the CO{sub 2} adsorption. Otherwise, the Ni/ZnZr catalyst (reduced at 650 °C) showed a high CH{sub 4} conversion. The catalysts were also reduced at 750 °C and a lower conversion of both reactants (CH{sub 4} and CO{sub 2}) was observed. We argued that the agglomeration process during the reduction condition deteriorates the performance of the catalysts reduced at 750 °C.

09 BIOMASS FUELS↗
DOE OSTI2018

Preparation of graphene/WO3/TiO2 composite and its photocathodic protection performance for 304 stainless steel

Highlights: • TiO{sub 2} nanoparticles and WO{sub 3} nanorods were immobilized onto graphene by the hydrothermal method. • The composite can provide an effective protection for 304 stainless steel under visible light. • The composite can offer a sufficient cathodic protection even in the dark. • Possible photocathodic protection mechanism of graphene/WO{sub 3}/TiO{sub 2} composite was proposed. - Abstract: Graphene/WO{sub 3}/TiO{sub 2} composite (RGO/WO{sub 3}/TiO{sub 2}) was successfully fabricated via a two-step hydrothermal method. The structure, morphology and optical property of the as-prepared composite were characterized by X-ray powder diffraction, fourier transform infrared spectra, Raman spectra, transmission electron microscope, scanning electron microscope and ultraviolet-visible diffuse reflectance spectra, respectively. Results showed that the composite was incorporated by graphene nanosheets, WO{sub 3} nanorods and TiO{sub 2} nanoparticles. It exhibited favorable absorption ability in both UV and visible light region. The photocathodic protection performance for 304 stainless steel (304SS) was proven by photocurrent density, open circuit potential, Tafel polarization curves and electrochemical impedance spectroscopy. It was found that the composite could provide an efficient protection for 304SS under visible light irradiation and even in the dark compared to the pure TiO{sub 2}. The electrode potentials negatively shifted to −760 mV under visible light. The possible photocathodic protection mechanism of the composite was also proposed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Upconversion Er-doped TiO2 nanorod arrays for perovskite solar cells and the performance improvement

Highlights: • Er-doped TiO{sub 2} nanorod absorbs IR and converts into visible light. • The introduction of Er could make a positive shift in flat-band potential. • Er-doped TiO{sub 2} solar cells show a 20% increment in the current density. - Abstract: Upconversion erbium-doped rutile TiO{sub 2} nanorod arrays were synthesized by a facile process and applied in perovskite solar cells (PSCs). The structure was characterized by X-ray powder diffraction (XRD). Energy dispersive spectrometer (EDS) and Tauc plot indicated that Er was successfully introduced and changed TiO{sub 2} band gap from 3.00 eV to 3.07 eV. The incorporation of Er shifts the flat band potential positively and enhances the electron density. The Er-doped TiO{sub 2} nanorods have a broad absorption in the infrared light and up-convert it into visible light, which provides a possibility for PSCs to use NIR light for higher performance. A higher photocurrent density (J{sub sc}) of 22.97 mA/cm{sup 2} and a power conversion efficiency (PCE) of 10.6% were obtained, showing 20% and 16.5% increment in J{sub sc} and PCE, respectively, when compared with the un-doped device. The performance improvement was ascribed to the upconversion performance, enhanced electron-injection efficiency and reduced charge recombination.

14 SOLAR ENERGY↗
DOE OSTI2018

Preparation and investigation of Dy3+-doped Ca9LiGd2/3(PO4)7 single-phase full-color phosphor

Highlights: • A novel single-phased Ca{sub 9}LiGd{sub 2/3}(PO{sub 4}){sub 7}:xDy{sup 3+} phosphor was firstly synthesized. • Its structure, luminescent properties are well studied and characterized. • It was promising as a single-component white-light-emitting phosphor for w-LEDs. - Abstract: Novel single-phased white-light-emitting Ca{sub 9}LiGd{sub 2/3}(PO{sub 4}){sub 7}:xDy{sup 3+} (x = 0.02, 0.05, 0.10, 0.15, 0.20, 0.25, and 0.30) β-Ca{sub 3}(PO{sub 4}){sub 2}-type phosphate phosphors were synthesized. The phase structure, luminescence, and thermal stability of the phosphors were characterized by X-ray powder diffraction analysis, photoluminescence excitation and emission spectra, thermal quenching, and decay curves. XRD analysis confirmed the phase formation of Ca{sub 9}LiGd{sub 2/3}(PO{sub 4}){sub 7}:Dy{sup 3+} materials. Under the excitation of 352 nm, the emission of the Ca{sub 9}LiGd{sub 2/3}(PO{sub 4}){sub 7}:0.20Dy{sup 3+} sample centered at blue (488 nm) and yellow (580 nm), which corresponded to {sup 4}F{sub 9/2}–{sup 6}H{sub 15/2} transition and {sup 4}F{sub 9/2}–{sup 6}H{sub 13/2} transition. The optimum dopant concentration of Dy{sup 3+} ions was around 20 mol%, and the critical transfer distance of Dy{sup 3+} was calculated as 18 Å. The thermal-quenching temperature was above 500 K for Ca{sub 9}LiGd{sub 2/3}(PO{sub 4}){sub 7}:0.20Dy{sup 3+}. The developed phosphor has a great potential as a single-component white-light-emitting phosphor for UV-light-emitting diodes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Template-free cyclic hexavanadate: Synthesis, characterization, solid-state structure, and solution-state dynamics

A novel hexavanadate–organic hybrid material of the formula [NH 4 ] 2 [V 6 (µ 2 -O) 6 (O) 4 (PDC) 6 ] (PDC = 2,6-pyridinedicarboxylate) has been prepared in dilute nitric acid under hydrothermal reaction conditions. The product was characterized by single crystal and powder X-ray diffraction, FTIR, UV–Vis, Raman, and thermogravimetric analyses in the solid state, and small angle X-ray scattering, ESI-MS, NMR ( 1 H, 13 C, 51 V), and Raman spectroscopic techniques in aqueous solution. The crystal structure revealed a rare structure type in vanadium chemistry which crystallizes in the monoclinic space group P2 1/n and consists of a cyclic polyoxovanadate core with edge-capped tetrahedral and octahedral vanadium centers. The “hollow” polyoxovanadate is stabilized by a PDC ligand on each metal center, and ammonium ions charge balance the anionic core and form hydrogen bonding interactions with the hexavanadate units. Solution-state studies showed that the structural unit observed in the solid state hydrolyzes upon dissolution in water, resulting in a symmetric dimer bearing similar ligand sets. Finally, catalytic experiments on the photodecomposition of crystal violet, rhodamine B, methylene blue, and rhodamine 6G showed ≥93% degradation of the dyes under UV light irradiation upon addition of the vanadium complex.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Synthesis and characterization of Pt(Cu 0.67 Sn 0.33 )

Pt(Cu 0.67 Sn 0.33 ) has recently been found in a natural sample. In order to be able to characterize this new ternary compound, we synthesized it from the elements. Samples were characterized by X-ray powder diffraction, differential scanning calorimetry, thermal relaxation calorimetry, and scanning electron microscopy studies. Density functional theory-based model calculations complemented the experimental studies. Pt(Cu 0.67 Sn 0.33 )was already formed at a relatively low temperature of 773 K. Rietveld refinement of Pt(Cu 0.67 Sn 0.33 ) has been carried out in CuAu-type or L1 0 -type structure, space group P4/mmm, with Pt on 0,0,0 and disordered Cu and Sn on 1/2, 1/2, 1/2 and Z = 1. The lattice parameters are a = 2.823(1) Å, c = 3.64(1) Å, and V = 29.00(4) Å which are in good agreement with values obtained earlier on the natural sample and with the results of DFT calculations. The vibrational entropy for Pt(Cu 0.67 Sn 0.33 ) is $S_{298.15}^{vib}$ = 79.9(7) J mol -1 K -1 . The pressure dependence up to 36(2) GPa of the unit-cell volume and the lattice parameters and unit-cell volume have been obtained by synchrotron based powder diffraction using a diamond anvil cell. A fit of a 3rd-order Birch–Murnaghan equation of state to the Pt(Cu 0.67 Sn 0.33 )) (p,V)-data results in a bulk modulus of B 0 = 215(27) GPa and B' = 5(2).

36 MATERIALS SCIENCE↗
DOE OSTI2018

A Crystalline Polyimide Porous Organic Framework for Selective Adsorption of Acetylene over Ethylene

The separation of acetylene from ethylene is a crucial process in the petrochemical industry, as even small acetylene impurities can lead to premature termination of ethylene polymerization. Herein, we present the synthesis of a robust, crystalline naphthalene diimide porous aromatic framework via imidization of linear naphthalene-1,4,5,8-tetracarboxylic dianhydride and triangular tris(4-aminophenyl)amine. The resulting material, PAF-110, exhibits impressive thermal and long-term structural stability, as indicated by thermogravimetric analysis and powder X-ray diffraction characterization. Gas adsorption characterization reveals that PAF-110 has a capacity for acetylene that is more than twice its ethylene capacity at 273 K and 1 bar, and it exhibits a moderate acetylene selectivity of 3.9 at 298 K and 1 bar. Complementary computational investigation of each guest binding in PAF-110 suggests that this affinity and selectivity for acetylene arises from its stronger electrostatic interaction with the carbonyl oxygen atoms of the framework. As a result, to the best of our knowledge, PAF-110 is the first crystalline porous organic material to exhibit selective adsorption of acetylene over ethylene, and its properties may provide insight into the further optimized design of porous organic materials for this key gas separation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

The grain-size effect on thermal conductivity of uranium dioxide

We have investigated the grain-boundary scattering effect on the thermal transport behavior of uranium dioxide (UO 2 ). The polycrystalline samples having different grain-sizes (0.125, 1.8, and 7:2 µm) have been prepared by a spark plasma sintering technique and characterized by x-ray powder diffraction, scanning electron microscope, and Raman spectroscopy. The thermal transport properties (the thermal conductivity and thermoelectric power) have been measured in the temperature range of 2–300 K, and the results were analyzed in terms of various physical parameters contributing to thermal conductivity in these materials in relation to grain-size. We show that thermal conductivity decreases systematically with lowering grain-size in the temperatures below 30 K, where the boundary scattering dominates the thermal transport. At higher temperatures, more scattering processes are involved in the heat transport in these materials, making the analysis difficult. We determined the grain-boundary Kapitza resistance that would result in the observed increase in thermal conductivity with grain-size and compared the value with Kapitza resistances calculated for UO 2 using molecular dynamics from the literature.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Influence of cobalt substitution on the magnetism of NiBr 2

Co-substituted Ni 1-x Co x Br 2 (0≤x≤1) single crystals were synthesized using vapor transport. As a result, the physical properties of the crystals were characterized by x-ray powder diffraction, magnetization, and specific-heat measurements. Room-temperature x-ray powder diffraction data indicate that a change from the CdCl 2 structure type to the CdI 2 structure type occurs within 0.56 2 has a commensurate antiferromagnetic phase below T N ≈ 46 K and an incommensurate magnetic ground state below T IC ≈ 20 K. Both magnetic transitions are affected by cobalt substitution, and the incommensurate phase transition is present up to at least x=0.56. Here, the evolution of magnetism has been studied as a function of cobalt content and is summarized in the temperature-composition phase diagram.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The T 2 structure of polycrystalline cubic human insulin

The polymorphism of human insulin upon pH variation was characterized via X-ray powder diffraction, employing a crystallization protocol previously established for co-crystallization with phenolic derivatives. Two distinct rhombohedral ( R 3) polymorphs and one cubic ( I 2 1 3) polymorph were identified with increasing pH, corresponding to the T 6 , T 3 R 3 f and T 2 conformations of insulin, respectively. The structure of the cubic T 2 polymorph was determined via multi-profile stereochemically restrained Rietveld refinement at 2.7 Å resolution. This constitutes the first cubic insulin structure to be determined from crystals grown in the presence of zinc ions, although no zinc binding was observed. The differences of the polycrystalline variant from other cubic insulin structures, as well as the nature of the pH-driven phase transitions, are discussed in detail.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2018

Characterization Report on Fuels for NEAMS Model Variation

We have investigated the grain boundary scattering effect on the thermal transport behavior of uranium dioxide (UO 2 ). The polycrystalline samples having different grain sizes (0.125, 1.8, and 7.2 μm) have been prepared by spark plasma sintering technique and characterized by x-ray powder diffraction (XRD), scanning electron microscope (SEM), and Raman spectroscopy. The thermal transport properties (the thermal conductivity and thermoelectric power) have been measured in the temperature range 2-300 K and the results were analyzed in terms of various physical parameters contributing to the thermal conductivity in these materials in relation to grain-size. We show that thermal conductivity decreases systematically with lowering grain-size in the temperatures below 30 K, where the boundary scattering dominates the thermal transport. At higher temperatures more scattering processes are involved in the heat transport in these materials. We analyzed the results obtained using molecular dynamics (MD) calculations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗