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At least 235 records · Page 13

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↗

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↗

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↗

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↗

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↗

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↗

Understanding Microstructural Effects on Dynamic Performance Towards the Development of Shock Metamaterials

With the recent advances in additive manufacturing (AM), long-range periodic lattice assemblies are being developed for vibration and shock mitigation components in aerospace and military applications with unique geometric and topological structures. There has been extensive work in understanding the static properties associated with varying topology of these lattice architectures, but there is almost no understanding of microstructural affects in such structures under high-strain rate dynamic loading conditions. Here we report the shock behavior of lattices with varying intrinsic grain structures achieved by post process annealing. High resolution 316L stainless steel lattices were 3D printed by a laser-powder bed fusion machine and characterized by computed tomography. Subsequent annealing resulted in stress-relieved and recrystallized lattices. Overall the lattices had strong cubic texture aligning with the x-, y- and z-directions of the build with a preference outside the build direction (z). The recrystallized sample had more equiaxed polygonal grains and a layer of BCC ferrite at the surface of the structure approximately 1 grain thick. Upon dynamic compression the as-deposited lattice showed steady compaction behavior while the heat-treated lattices exhibit negative velocity behavior indicative of failure. We attribute this to the stiffer BCC ferrite in the annealed lattices becoming damaged and fragmenting during compression.

36 MATERIALS SCIENCE↗

New NDA Methods for Thorium Fuel Cycle Safeguards (Mid-Project Report)

This project is developing new Non-Destructive Assay (NDA) safeguards techniques for emergent thorium fuel cycles based on Neutron Resonance Transmission Analysis (NRTA), which can assay 233 U and 235 U when they are present together in a sample with potentially high gamma-ray backgrounds from fission products and 232 U. Existing passive techniques face large challenges for this task so new active interrogation methods are needed. This effort is also exploring how gamma-ray signatures can complement NRTA for enhanced assayed performance. This project leverages an NRTA system being developed at PNNL in collaboration with MIT, which uses a commercially available deuterium-tritium neutron generator at short standoff (~2 m). We aim to assess the feasibility and performance of these new NDA techniques for the range of relevant samples in thorium fuel cycles. Key advancements described in this mid-project report include NRTA system design for thorium safeguards measurements, characterization of 233 U oxide powder at PNNL, a survey of detector technologies suitable for NRTA in high gamma background environments, successful preliminary demonstration of a quantitative isotopic estimation algorithm, and first NRTA measurements of a thorium sample.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A&L Annual Report: GRM-MAPS

Exploding Bridge Wire (EBW) is an important design for initiating detonators relevant to several LLNL systems. In such designs, a metal bridge wire is in direct contact with a porous secondary high explosive (HE), typically pressed to around 50% of its crystalline density. Initiation is believed to occur through shock waves generated when the bridge wire is made to explode via the rapid passing of a strong current pulse. Permeametry is an important characterization tool for the porous powdered HE (PETN, HMX, etc.) component in such devices. Such powders are well known to coarsen with age, with an accompanying deterioration in performance, which includes increased function time and sensitivity. Among various material characteristics, one that has been shown to correlate the most with such performance parameters is the flow-permeable surface area (FSSA), measured using air-permeametry. Commercially available permeametry apparatuses, such as that from Fisher Scientific or a more modern version from Micromeritics suffer from a few drawbacks, most notably as related to monitoring age-related changes in FSSA. This is because it requires re-compaction of the aged powder into the permeametry tube, which in most cases leads to an unwanted increase in FSSA. To address this and a few other shortcomings, we have been developing a modern version of the permeameter, Gee-Reinstein-Maiti Modern Air-Permeametry System (GRM-MAPS). In this report, we summarize progress made in FY25 toward perfecting and calibrating the instrument, which we aim at deploying within surveillance in FY26.

36 MATERIALS SCIENCE↗

Interaction of hydrogen chloride with alumina

The influence of outgas conditions and temperature on the adsorptive properties of two aluminas Alon-c and Al6sG were studied using adsorption isotherm measurements. Alon-C and Al6SG were characterized using X-ray powder diffraction, thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and BET nitrogen surface areas. Some of these techniques were applied to two other aluminas but no isotherm data was obtained. Isotherm data and techniques applied to each alumina are summarized in tabular form.

Bailey, R. R.↗

Advanced powder metallurgy aluminum alloys via rapid solidification technology

Aluminum alloys containing 10 to 11.5 wt. pct. of iron and 1.5 to 3 wt. pct. of chromium using the technique of rapid solidification powder metallurgy were studied. Alloys were prepared as thin ribbons (.002 inch thick) rapidly solidified at uniform rate of 10(6) C/second by the melt spinning process. The melt spun ribbons were pulverized into powders (-60 to 400 mesh) by a rotating hammer mill. The powders were consolidated by hot extrusion at a high reduction ratio of 50:1. The powder extrusion temperature was varied to determine the range of desirable processing conditions necessary to yield useful properties. Powders and consolidated alloys were characterized by SEM and optical metallography. The consolidated alloys were evaluated for (1) thermal stability, (2) tensile properties in the range, room temperature to 450 F, and (3) notch toughness in the range, room temperature to 450 F.

Ray, R.↗

Composition dependence of superconductivity in YBa2(Cu(3-x)Al(x))Oy

Eleven different compositions in the system YBa2(Cu(3-x)Al(x))O(y) (x = 0 to 0.3) have been synthesized and characterized by electrical resistivity measurements, powder x-ray diffraction, and scanning electron microscopy. The superconducting transition temperature T sub c (onset) was almost unaffected by the presence of alumina due to its limited solubility in YBa2Cu3O(7-x). However, T sub c(R = 0) gradually decreased, and the resistive tails became longer with increasing Al2O3 concentration. This was probably due to formation of BaAl2O4 and other impurity phases from chemical decomposition of the superconducting phase by reaction with Al2O3.

Bansal, Narottam P.↗

Composition dependence of superconductivity in YBa2(Cu(3-x)Al(x))O(y)

Eleven different compositions in the system YBa2(Cu(3-x)Al(x))O(y) (x = 0 to 0.3) have been synthesized and characterized by electrical resistivity measurements, powder X-ray diffraction, and scanning electron microscopy. The superconducting transition temperature T sub c (onset) was almost unaffected by the presence of alumina due to its limited solubility in YBa2Cu3O(7-x). However, T sub c(R = 0) gradually decreased, and the resistive tails became longer with increasing Al2O3 concentration. This was probably due to formation of BaAl2O4 and other impurity phases from chemical decomposition of the superconducting phase by reaction with Al2O3.

Bansal, N. P.↗

Applications of diamond films and related materials; Proceedings of the 1st International Conference, Auburn, AL, Aug. 17-22, 1991

The present conference discusses the nucleation and growth of diamond from hydrocarbons, the cutting tool performance of CVD thick-film diamond, the characterization of CVD diamond grinding powder, industrial applications of crystalline diamond-coated tools, standardized SEM tribometry of diamond-coated substrates, residual stress in CVD diamond films, the optical properties of CVD diamond films, polycrystalline diamond films for optical applications, and diamond growth on ferrous metals. Also discussed are ion beam-irradiation smoothing of diamond films, electronic circuits on diamond substrates, diamond-laminated surfaces for evaporative spray cooling, electron devices based on the unique properties of diamond, diamond cold cathodes, thin-film diamond microstructure applications, Schottky diodes from flame-grown diamond, diamond films for thermionic applications, methods of diamond nucleation and selective deposition, high-rate/large-area diamond film production, halogen-assisted diamond growth, the economics of diamond technology, and the optical and mechanical properties of diamondlike films.

Tzeng, Yonhua↗

Characterization of two germania gels of different coordination

Two germania gels were synthesized by hydrolytic condensation of germanium ethoxide and by dissolution of germanium dioxide powder in ammonium hydroxide solution. The two gels were characterized using differential scanning calorimetry, X-ray powder diffraction, surface area and weight loss data, and infrared spectroscopy. The results indicate that, in gels, germanium is capable of tetragonal as well as hexagonal coordination, resulting in different crystallization behaviors.

Mukherjee, Shyama P.↗

Comparison of Electron Beam and Laser Beam Powder Bed Fusion Additive Manufacturing Process for High Temperature Turbine Component Materials, Phase II. CRADA Final Report

The evolving additive manufacturing (AM) technology is now at the point where some metallic turbine components are being fabricated for both development and production purposes. The goal of this phase II project is to continue the evaluation of AM Nickel Alloy X fabricated by electron beam (EB) or laser beam (LB) powder bed fusion (PBF) process for gas turbine applications. Microstructure, mechanical and oxidation properties characterization was conducted on test specimens produced with powders of different chemistries within the typical material specification range. Powders with high Silicon (Si) content for the LB-PBF and low Si content for the EB-PBF displayed significant cracking levels in the AM Nickel Alloy X material. Accordingly, optimum fatigue performance would require careful control of powder chemistry, optimization of the fabrication parameters for a given powder and use of hot isostatic pressing (HIP) post treatment. Oxidation testing conducted at 1472°F (800ºC) in air showed that the roughness of the EB-PBF specimens led to an increase in specimen mass change, but overall the AM specimens exhibited oxidation behavior at 1472°F (800ºC) that is appropriate for applications in gas turbine engines. Assessment of the geometric capability of the LB-PBF and EBPBF systems using artifacts representative of turbine component geometries revealed that the LB-PBF process is well-suited for the fabrication of intricate geometries needed for turbine engine fuel injector components, but further process development is required to improve the EB-PBF system feature resolution.

36 MATERIALS SCIENCE↗

Nanostructured Powders Made from Flame Spray Pyrolysis for Li-Ion Cathode

Flame processes are the most economic ones to produce fine powders and have been used to produce pigment titanium oxide and fused silica in large volumes. In this work a flame spray pyrolysis (FSP) process is used to make positive electrode materials for Li-ion battery, which is made of complex metal oxide powders, such as Li(Ni1/3Mn1/3Co1/3)O2. In particular, the work was focused on making the NMC materials with stoichiometric compositions and desired morphologies. During the pyrolysis process different morphologies can be formed, involving often powders with primary nanoparticles. Such nanostructures were found to have affected the battery performance. Detailed results of the synthesis, characterization, and battery testing of the NMC powder materials will be presented.

25 ENERGY STORAGE↗

Lithography-based Ceramics Manufacturing Technologies

In this work, surrogate powders were prepared with lithography-based ceramic printing. Lanthanum oxide, a powder from Oak Ridge National Laboratory (ORNL), was prepared by milling, characterizing, and printing of coupon samples. The printing resulted in net-shaped green parts. Alumina, a more developed powder, was also printed and characterized at ORNL, and these parts were surrogate geometries larger than coupons that were sintered to net shape within 0.3% of the desired geometry.

36 MATERIALS SCIENCE↗