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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

The First Neptunium Dioxide Neutron Diffraction Experiment at HFIR

Here we present the first neutron diffraction experiment of a 50 mg sample of neptunium(IV) dioxide (NpO 2 ) powder at the High Flux Isotope Reactor (HFIR) using the wide-angle neutron diffractometer (WAND 2 ) HB-2C. We also provide a brief literature survey to pinpoint gaps in the crystal, electronic, and magnetic structure of NpO 2 to determine the optimum experiment to be pursued in the next HFIR user proposal cycle. Characterizing actinide materials with neutron diffraction, inelastic scattering, neutron imaging, polarized neutron studies, and small-angle neutron scattering techniques will increase our understanding of 5f electron behavior and elucidate atomic and magnetic structural properties. This strategy will help fill gaps in the literature and provide theoretical physicists with the data needed to build physical and chemical models to guide and validate computational methods. These methods may be used for predicting structural and chemical features of actinide-based materials. This proof-of-principle effort begins to uncover how to advance actinide science and technology at Oak Ridge National Laboratory (ORNL) using neutron capabilities. This effort has already sparked collaborative discussions between researchers outside the Radioisotope Science and Technology Division, including theoretical physicists from the Nuclear Nonproliferation Division and beamline scientists in the Neutron Scattering Division. We intend to continue pursuing neutron experiments and develop a scientific strategy focused on studying transuranium elements (e.g., Np, Pu, Am, and Cm) using the advanced neutron capabilities at ORNL.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2024

Microstructural and Hall–Petch Analysis of Additively Manufactured Ferritic Alloy Using 2507 Duplex Stainless Steel Powder

The powder bed fusion–laser beam (PBF-LB) process, a method of additive manufacturing (AM), was used to print duplex stainless steel (DSS) using commercial-grade 2507 powders. While conventionally processed DSS has a two-phase microstructure consisting of 50% austenite and 50% ferrite, the PBF-LB-printed 2507 alloy was nearly 100% ferrite. Optimal processing conditions that minimized porosity were determined to be 290 W laser power and 1000 mm/s scan speed, and grain size, texture, and phases were characterized as a function of laser power and scan speed. Grain size increased with increasing laser power but decreased with increasing scan speed. A <100> texture diminished with increasing scan speed from 1000 mm/s to 1400 mm/s. No austenite phase was detected. Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) characterization revealed nanoscale chromium nitride precipitates in the ferritic matrix (incoherent hexagonal close-packed (HCP) precipitates at grain boundaries and coherent body-centered cubic (BCC) precipitates within the grains) and a high density of tangled dislocations. Tensile tests of as-printed alloys showed a yield strength of 570 MPa, an ultimate tensile strength of 756 MPa, and an elongation to failure of 10%. The tensile properties were analyzed based on the observed microstructure considering grain size, nanoscale precipitates, and the high density of dislocations.

Crystallography↗
DOE OSTI2024

Nonoxidative dehydrogenation of propane using boron-incorporated silica-supported Pt Sites synthesized by atomic layer deposition

Nonoxidative dehydrogenation of propane to propylene using Pt-based supported catalysts is an active research area in catalysis because catalyst attributes of Pt sites can be controlled by careful design of active sites. One way to achieve this is by the addition of a second metal that may impart a change in the electron density of active sites, which in turn affects catalytic performance. In this study, bimetallic Pt and B sites were deposited on powder SiO2 using atomic layer deposition (ALD). Boron was first deposited on SiO2 via half-cycle ALD using triisoproplyborate as the B source. Following calcination, Pt deposition was performed via half-cycle ALD using trimethyl(methylcyclopentadienyl)platinum(IV) as the Pt source. The synthesized catalysts were reduced under H2 at 550 °C and characterized using inductively coupled plasma optical emission spectroscopy for elemental analysis, diffuse reflectance infrared Fourier transform spectroscopy of adsorbed CO to examine the properties of Pt, and time-resolved X-ray absorption near edge structure spectroscopy to examine the changes in the reducibility of Pt sites. The samples were then tested for nonoxidative dehydrogenation of propane at 550 °C using a fixed-bed plug-flow reactor to examine the role of B on the catalytic performance. Characterization results showed that the addition of B imparted an increase in electron density and affected the reducibility of Pt sites. In addition, incorporating B on SiO2 created anchoring sites for Pt ALD. The amount of Pt deposited on B/SiO2 was 2.2 times that on SiO2. Catalytic activity results revealed the addition of B did not change the initial activity of Pt sites significantly, but improved propylene selectivity from 80% to 87% and stability almost threefold. The enhanced selectivity and stability of PtB/SiO2 is most presumably due to favored desorption of propylene and mitigating coke formation under reaction conditions, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

An Alternative Low-Cost Process for Deposition of MCrAlY Bond Coats for Advanced Syngas/Hydrogen Turbine Applications

The objective of this project was to develop and optimize MCrAlY bond coats for syngas/hydrogen turbine applications using a low-cost electrolytic codeposition process. Prealloyed CrAlY-based powders were codeposited into a metal matrix of Ni, Co or Ni-Co during the electroplating process, and a subsequent post-deposition heat treatment converted it to the MCrAlY coating. Our research efforts focused on: (1) investigation of the effects of electro-codeposition configuration and parameters on the CrAlY particle incorporation in the NiCo-CrAlY composite coatings; (2) development of the post-deposition heat treating procedure; (3) characterization of coating properties and evaluation of coating oxidation performance; (4) exploration of a sulfurfree electroplating solution; (5) cost analysis of the present electrolytic codeposition process. Different electro-codeposition configurations were investigated, and the rotating barrel system demonstrated the capability of depositing NiCo-CrAlY composite coatings uniformly on the entire specimen surface, with the CrAlY particle incorporation in the range 37-42 vol.%. Post-deposition heat treatment at 1000-1200 °C promoted interdiffusion between the CrAlY particles and the Ni-Co metal matrix, resulting in β/γ’/γ or β/γ’ phases in the heat-treated coatings. The results also indicate that the post-deposition heat treatment should be conducted at temperatures ≤1100 °C to minimize Cr evaporation and outward diffusion of Ti. The electro-codeposited NiCrAlY coatings in general showed lower hardness and surface roughness than thermal spray MCrAlY coatings. Coating oxidation performance was evaluated at 1000-1100 °C in dry and wet air environments. The initial electro-codeposited NiCoCrAlY coatings containing relatively high sulfur did not show good oxidation resistance. After modifications of the coating process, the cleaner NiCoCrAlY coating exhibited good oxidation performance at 1000 °C during the 2,000 1-h cyclic oxidation test. A sulfur-free fluoboratebased plating solution was explored in order to reduce the sulfur level in the electro-codeposited MCrAlY coatings. However, chemical reactions occurred between the CrAlY powder and the fluoborate plating solution, resulting in dark powdery coatings. The fluoborate-based plating bath can thus only be used to codeposit more inert particles (e.g., oxides or carbides) instead of the present Al-containing metallic particles.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Optimization of direct aging temperature of Ti free grade 300 maraging steel manufactured using laser powder bed fusion (LPBF)

Maraging steels are of interest to the tool and die industry owing to their high strength, toughness and machinability. Additive manufacturing technologies like laser powder bed fusion (LPBF) can result in a paradigm shift in the design of maraging steel tools. Here, the lack of precipitates, in combination with solute segregation and non-equilibrium microstructure in Grade 300 maraging steel fabricated via LPBF makes the steel amenable to strengthening via direct aging post fabrication instead of the conventional solution treatment and aging. In this study we have focused on optimizing the direct aging temperature for a Ti-free Grade 300 maraging steel fabricated via LPBF for two different aging times. Through strain hardening analysis and detailed microstructural characterization, we show that direct aging at a temperature of 440 °C for 6 h resulted in the best strength-ductility combination. Aging samples at a lower temperature or shorter time resulted in no strain hardening prior to necking as a result of lower fraction of reverted austenite, whereas aging samples at a higher temperature resulted in extensive recrystallization of martensite, coarsening of precipitates, and extensive austenite reversion, resulting in softening of the fabricated parts.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Neutron Characterization of 3D Printed Gas Turbine Alloy With Internal Cooling Structure

The objective of this research work is to investigate the residual strains induced by the presence of a exit hole and internal hollow geometry present in a 3D printed IN718 similar to that seen in a gas turbine blade. The specimens were manufactured with an internal hollow structure that ended with an exit hole, and fabricated by direct metal laser sintering additive manufacturing technique. Using this technique, metal powder was melted by a laser source and rapidly cooled to form the part layer by layer. Rapid heating and cooling generate large thermal gradients and residual stresses in the 3D printed material. To be aligned with industry standards, specimens were heat-treated to relieve most of the residual stresses as well as to investigate whether IN718 still preserved a nonhomogeneous stress state after the thermal treatment. Roughness and microstructure analysis was performed to understand the heat-treated sample properties. To investigate the volumetric residual strain, the neutron diffraction technique was used with a definite neutron wavelength. Bragg’s law was used to determine lattice spacing. Interplanar lattice spacing and stress-free state lattice spacings were measured to calculate the strains. Residual strains were measured in the x and y direction to understand the impact of the presence of a exit hole and internal hollow geometry. The results of volumetric residual strain in the x and y directions showed no significant variations in the distribution of the strain due to the presence of a hollow structure as well as the exit hole. Overall, no significant stress concentration was observed in the heat treated sample. Sample geometry, instrumentation for neutron diffraction, and material properties are discussed in detail in this paper.

Raju, Nandhini↗
DOE OSTI2022

Novel processing route for design and manufacturing of metal toughened nanoceramics: Al–Al 2 O 3 nanocermets

Monolithic alumina is a highly brittle ceramic with a very low fracture toughness, making it an unreliable material for mechanical and structural applications. Ceramic-metal composites (cermets) are the subject of intensive interest to obtain materials which can address the intrinsic brittleness of ceramics without compromising their high strength and light weight. In the present investigation, aluminium-alumina (Al–Al 2 O 3 ) nanocermets were developed. The nanocermets possessed the toughness of Al phase and the strength of reinforced nano Al 2 O 3 particles. Here, the nanocermets green bodies were prepared such that upon sintering each adjacent Al 2 O 3 grain was conformally coated with a continuous Al film. Mechanical milling via a combination of cryo-milling and ball-milling was used to prepare Al–Al 2 O 3 nano-powder mixture. Spark plasma sintering was used to consolidate the green nanocermets. Results show that specimens prepared from 35 h milled powders exhibited superior mechanical properties as compared to other nanocermets, with an improvement in microhardness, elastic modulus, compressive strength, and flexural strength by 88%, 78%, 69% and 40% with respect to sintered pure Al. The indentation toughness of 35 h milled nanocermet showed an increment of 12.5% with respect to sintered pure Al 2 O 3 . Characterization techniques such as XRD, SEM, HR-TEM, X-ray tomography were employed to investigate the phase evolution and structural morphology, while FEM simulations were performed for understanding the crack propagation mechanisms in nanocermets.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Characterization of nickel laterite reduction from Pomalaa, Sulawesi Tenggara

The effect of using different reductors in the reduction process of nickel laterite was investigated. In this work, the author conducted the reduction of nickel laterite ores by anthracite coal, lamtoro charcoal, and carbon raiser, in air and CO{sub 2} atmosphere, within the temperature ranged from 800°C and 1000°C. The results indicate that at higher temperatures, the reduction reactions proceed more complete. According to the X-ray powder diffraction (XRD) analysis, the type of carbon used greatly influence the rate of the reduction of nickel laterite. The order of reactivity is anthracite coal, lamtoro charcoal, and carbon raiser, respectively. The reduction atmospheric condition also greatly influences the reduction process. The reduction process in CO{sub 2} atmospheric condition gives a lot of significant decrease in hematite and magnetite presence, means that the reduction reactions proceed more complete compared to the reduction process in the air atmospheric condition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

High-resolution Compton spectroscopy using x-ray microcalorimeters

X-ray Compton spectroscopy is one of the few direct probes of the electron momentum distribution of bulk materials in ambient and operando environments. Herein, we report high-resolution inelastic x-ray scattering experiments with high momentum and energy transfer performed at a storage-ring-based high-energy x-ray light source facility using an x-ray transition-edge sensor (TES) microcalorimeter detector. The performance was compared with a silicon drift detector (SDD), an energy-resolving semiconductor detector, and Compton profiles were measured for lithium and cobalt oxide powders relevant to lithium-ion battery research. Spectroscopic analysis of the measured Compton profiles demonstrates the high-sensitivity to the low- Z elements and oxidation states. The line shape analysis of the measured Compton profiles in comparison with computed Hartree–Fock profiles is usually limited by the resolution of the semiconductor detector. We have characterized an x-ray TES microcalorimeter detector for high-resolution Compton scattering experiments using a bending magnet source at the Advanced Photon Source with a double crystal monochromator, providing monochromatic photon energies near 27.5 keV. The momentum resolution below 0.16 atomic units (a.u.) was measured, yielding an improvement of more than a factor of 7 over a state-of-the-art SDD for the same scattering geometry. Furthermore, the lineshapes of narrow valence and broad core electron profiles of sealed lithium metal were clearly resolved using an x-ray TES compared to smeared and broadened lineshapes observed when using the SDD. High-resolution Compton scattering using the energy-resolving area detector shown here presents new opportunities for spatial imaging of electron momentum distributions for a wide class of materials with applications ranging from electrochemistry to condensed matter physics.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

Synthesis of platinum single-site centers through metal-ligand self-assembly on powdered metal oxide supports

Developing single-site metal catalysts has been regarded as a promising strategy to improve activity and selectivity in heterogeneous catalysis. Here, we report a metal-ligand self-assembly method to create Pt single-site centers on powdered oxide supports. Impregnating Pt and a ligand 3,6-di-2-pyridyl-1,2,4,5- tetrazine (DPTZ) simultaneously (one-step) creates Pt-DPTZ single-sites on powdered MgO, Al 2 O 3 , and CeO 2 . MgO has the most uniform single-sites due to a strong, non-competitive support-ligand interaction, and a support-metal interaction of appropriate strength. Pt(II) centers are stabilized between the N binding pockets of DPTZ, with minimal metallic nanoparticle formation. This system was characterized by XAS, XPS, TEM, XRD, and CO adsorption. Sequential impregnation of Pt and DPTZ (two-step) was also tested on Al 2 O 3 and CeO 2 , but is not as effective as the one-step method due to limited Pt accessibility and mobility. These oxide-supported Pt-DPTZ single-sites were found to be effective catalysts in hydrosilylation reactions. In conclusion, this work demonstrates a metal-ligand self-assembly strategy to create metal singlesite centers on high surface area catalyst supports.

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

Crystal structures of the new ternary stannides La{sub 3}Mg{sub 4−x}Sn{sub 2+x} and LaMg{sub 3−x}Sn{sub 2}

Synthesis and structural characterization of the two new lanthanum–magnesium–stannides La{sub 3}Mg{sub 4−x}Sn{sub 2+x} (0.12≤x≤0.40) and LaMg{sub 3−x}Sn{sub 2} (0.33≤x≤0.78) are reported. The crystal structures of these intermetallics were determined by single crystal X-ray diffraction analysis and confirmed by Rietveld refinement of powder X-ray diffraction patterns of the corresponding samples. The La{sub 3}Mg{sub 4−x}Sn{sub 2+x} phase crystallizes in the hexagonal Zr{sub 3}Cu{sub 4}Si{sub 2} structure type (P6¯2m, hP9, Z=3, x=0.12(1), a=7.7974(7), c=4.8384(4) Å), which represents an ordered derivative of the hP9-ZrNiAl prototype, ubiquitous among equiatomic intermetallics. The LaMg{sub 3–x}Sn{sub 2} phase is the second representative of the trigonal LaMg{sub 3−x}Ge{sub 2} type, which is a superstructure of the LaLi{sub 3}Sb{sub 2} structure type (P3¯1c, hP34-0.12, Z=6, x=0.35(1), a=8.3222(9), c=14.9546(16) Å). The scheme describing the symmetry reduction/coloring with respect to the parent type is reported here with the purpose to discuss the LaMg{sub 3−x}Sn{sub 2} off-stoichiometry from the geometrical point of view. Structural relationships between the La–Mg–Sn ternary phases, including the already known equiatomic LaMgSn compound (oP12-TiNiSi), are presented in the framework of the AlB{sub 2}-related compounds family and discussed with the aid of group-subgroup relations in the Bärnighausen formalism. - Graphical abstract: Crystal structure of LaMg{sub 3−x}Sn{sub 2} viewed along the (001) direction together with the puckered layer of Mg and Sn atoms hosting Mg2, Mg3 and vacancy □. - Highlights: • Crystal structures of the new La{sub 3}Mg{sub 4−x}Sn{sub 2+x} and LaMg{sub 3−x}Sn{sub 2} phases were determined. • The off-stoichiometry of LaMg{sub 3−x}Sn{sub 2} was discussed from geometrical point of view. • Structural relations between the known La–Mg–Sn phases were established. • The studied compounds are related to the AlB{sub 2} type by symmetry reduction.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructure and mechanical behavior of laser remelted amorphous Al-Ni-La welds

To explore the feasibility of using laser powder bed fusion systems to print bulk amorphous Al alloys, a single autogenous weld produced by laser remelting on a cast Al-5La-9Ni (at.%) alloy was studied for its microstructure and mechanical behavior. The solidification rates experienced by material within the welds were high enough to produce entirely amorphous regions within the welds. Welds were characterized using SEM, STEM, and APT and were found to contain Ni-rich amorphous clusters. Micropillar compression tests were used to assess mechanical properties of the welds and found that all of the amorphous regions exhibited yield strengths around 1 GPa. In conclusion, these results are discussed in the context of diffusivity of Ni and rare earth elements in liquid, glass forming ability, thermodynamic driving force for phase formation during solidification, free volume concentrations in bulk metallic glasses, and cluster-related softening.

APT↗
DOE OSTI2019

Characterization of shielding materials used in neutron scattering instrumentation

The nuclear cross-sections of certain isotopes make some materials excellent candidates for neutron shielding. We have performed a series of measurements examining the transmission, reflection, and nuclear Bragg scattering of a series of common materials used for neutron shielding. Here, we concentrate on characterizing the materials most likely to be used in neutron scattering instrumentation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

Microstructure evolution and electrical characterization of Lanthanum doped Barium Titanate (BaTiO{sub 3}) ceramics

In the current work, we investigated the structural and dielectric properties of Lanthanum oxide (La{sub 2}O{sub 3}) doped Barium Titanate (BaTiO{sub 3}) ceramics and established a correlation between them. Solid state sintering method was used to dope BaTiO{sub 3} with 0.3, 0.5 and 0.7 mole% La{sub 2}O{sub 3} under different sintering parameters. The raw materials used were La{sub 2}O{sub 3} nano powder of ~80 nm grain size and 99.995% purity and BaTiO{sub 3} nano powder of 100 nm grain size and 99.99% purity. Grain size distribution and morphology of fracture surface of sintered pellets were examined by Field Emission Scanning Electron Microscope and X-Ray Diffraction analysis was conducted to confirm the formation of desired crystal structure. The research result reveal that grain size and electrical properties of BaTiO{sub 3} ceramic significantly enhanced for small amount of doping (up to 0.5 mole% La{sub 2}O{sub 3}) and then decreased with increasing doping concentration. Desired grain growth (0.80-1.3 µm) and high densification (<90% theoretical density) were found by proper combination of temperature, sintering parameters and doping concentration. We found the resultant stable value of dielectric constant was 10000-12000 at 100-300 Hz in the temperature range of 30°-50° C for 0.5 mole% La{sub 2}O{sub 3} with corresponding shift of curie temperature around 30° C. So overall this research showed that proper La{sup 3+} concentration can control the grain size, increase density, lower curie temperature and hence significantly improve the electrical properties of BaTiO{sub 3} ceramics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Microstructural features underpinning the mechanical behavior of powder metallurgy Cr-based alloys

Refractory materials such as Cr-based alloys offer the potential of enhanced elevated temperature performance but have been limited by their poor formability. However, powder metallurgy has been shown to be a viable pathway to fabricate these alloys. Nanophase separation sintering (NPSS) in particular has been used in the literature to accelerate the densification of powder metallurgy Cr- and W-based alloys. Here, we explore microstructure evolution during NPSS in a binary Cr 85 Ni 15 alloy consolidated via (i) cold pressing & pressureless sintering and (ii) hot isostatic pressing followed by hot extrusion & hot upsetting, and the role of these different processing routes on resulting material properties. The alloy lacked room temperature tensile ductility regardless of consolidation process, with multi-length scale characterization, including scanning electron microscopy, transmission electron microscopy, atom probe tomography, X-ray diffraction, and uniaxial tensile testing, revealing that brittleness was due to intrinsically poor Cr grain boundary cohesion. Tensile testing conducted at 760 °C showed marked strength reduction for the extruded & upset (94 %) condition compared to the pressed & sintered (18 %). The formation of orthorhombic CrNi 2 intermetallics functioned as precipitate strengtheners and prevented elevated temperature softening in the pressed and sintered condition. The findings offer foundational insights into aiding the future development of Cr-based alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Increased Thermal Conductivity in Metal-Organic Heat Carrier Nanofluids

Metal organic heat carriers (MOHCs) are recently developed nanofluids containing metal organic framework (MOF) nanoparticles dispersed in various base fluids including refrigerants (R245Fa) and methanol. MOHCs utilize the MOF properties to improve the thermo-physical properties of base fluids. Here, we report the synthesis and characterization of MOHCs containing nanoMIL-101(Cr) and graphene oxide (GO) in an effort to improve the thermo-physical properties of various base fluids. MOHC containing MIL-101(Cr)/GO nanocomposites showed enhanced surface area, porosity, and nitrogen adsorption compared with the intrinsic nano MIL-101(Cr) and the properties depend on the amount of GO added. Powder X-ray diffraction (PXRD) confirmed the preserved crystallinity of MIL-101(Cr) in all nanocomposites with the absence of any unreacted GO. Scanning electron microscopy images confirmed the presence of near spherical MIL-101(Cr) nanoparticles in the range of 40-80 nm in diameter. MOHC nanofluids containing MIL-101(Cr)/GO in methanol exhibited significant enhancement in the thermal conductivity (by approxi-mately 50%) relative to that of the intrinsic nano MIL-101(Cr) in methanol. The thermal conductivity of base fluid (methanol) was enhanced by about 20 %. The enhancement in the thermal conductivity of nanoMIL-101(Cr) MOHCs due to graphene oxide functionalization is explained using a classical Maxwell model.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2016

Effect of oxidizer to fuel molar ratio on particle size and DC conductivity of CeO{sub 2} nanoparticles

Cerium oxide nanoparticles were synthesized by solution combustion method with varying the oxidizer (cerium nitrate hexa hydrate) to fuel (Glycine) molar ratio. The prepared samples were characterized by UV-visible spectrometer, X-ray diffractometer (XRD), Scanning electron microscope (SEM) and Energy dispersive X-Ray analysis (EDAX). XRD pattern reveals the formation of cubic fluorite structure of CeO{sub 2}. It was observed that finest crystallites were found at extreme fuel-deficient condition and it is good enough to produce favorable powder characteristics. The average crystallite size was found to be 14.46 nm to 21.57 nm. The temperature dependent dc conductivity was carried out using Keithley source meter between the temperature range from 300 K to 573 K. From this study it was found that the conductivity increases with increase of temperature due to semiconducting behavior of CeO{sub 2} and it decreases with particle size due to increase in the energy band gap.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

Crystal electric field excitations in the quasicrystal approximant TbCd 6 studied by inelastic neutron scattering

Here, we have performed inelastic neutron scattering measurements on powder samples of the quasicrystal approximant, TbCd 6 , grown using isotopically enriched 112 Cd. Both quasielastic scattering and distinct inelastic excitations were observed below 3 meV. The intensity of the quasielastic scattering measured in the paramag- netic phase diverges as T N ~ 22 K is approached from above. The inelastic excitations, and their evolution with temperature, are well characterized by the leading term, B$0\atop{2}$O$0\atop{2}$, of the crystalline electric field (CEF) level scheme for local pentagonal symmetry for the rare-earth ions [1] indicating that the Tb moment is directed primarily along the unique local pseudo-five-fold axis of the Tsai-type clusters. We also find good agreement between the inverse susceptibility determined from magnetization measurements using a magnetically diluted Tb 0.05 Y 0.95 Cd 6 sample and that calculated using the CEF level scheme determined from the neutron measurements.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗