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158 records · Page 9

Experimental Testing and Modeling of a Pneumatic Regolith Delivery System for ISRU

Excavating and transporting planetary regolith are examples of surface activities that may occur during a future space exploration mission to a planetary body. Regolith, whether it is collected on the Moon, Mars or even an asteroid, consists of granular minerals, some of which have been identified to be viable resources that can be mined and processed chemically to extract useful by-products, such as oxygen, water, and various metals and metal alloys. Even the depleted "waste" material from such chemical processes may be utilized later in the construction of landing pads and protective structures at the site of a planetary base. One reason for excavating and conveying planetary regolith is to deliver raw regolith material to in-situ resource utilization (ISRU) systems. The goal of ISRU is to provide expendable supplies and materials at the planetary destination, if possible. An in-situ capability of producing mission-critical substances such as oxygen will help to extend the mission and its success, and will greatly lower the overall cost of a mission by either eliminating, or significantly reducing, the need to transport the same expendable materials from the Earth. In order to support the goals and objectives of present and future ISRU projects, NASA seeks technology advancements in the areas of regolith conveying. Such systems must be effective, efficient and provide reliable performance over long durations while being exposed to the harsh environments found on planetary surfaces. These conditions include contact with very abrasive regolith particulates, exposure to high vacuum or dry (partial) atmospheres, wide variations in temperature, reduced gravity, and exposure to space radiation. Regolith conveying techniques that combine reduced failure modes and low energy consumption with high material transfer rates will provide significant value for future space exploration missions to the surfaces of the moon, Mars and asteroids. Pneumatic regolith conveying has demonstrated itself to be a viable delivery system through testing under terrestrial and reduced gravity conditions in recent years. Modeling and experimental testing have been conducted at NASA Kennedy Space Center to study and advance pneumatic planetary regolith delivery systems in support of NASA's ISRU project. The goal of this work is to use the model to predict solid-gas flow patterns in reduced gravity environments for ISRU inlet gas line allowing the eductor inlet gas flow to vary and depend on the flow pattern developed at the eductor as inferred by the experimental observations.

Santiago-Maldonado, Edgardo↗

Spin Reorientation in Antiferromagnetic Layered FePt 5 P

FePt 5 P, a substitutional variant of the anti-CeCoIn 5 structure type in the space group P4/mmm, was synthesized by a high-temperature solid-state method and structurally characterized by X-ray diffraction. FePt 5 P contains layers of FePt 12 clusters formed by magnetically active Fe and heavy Pt with strong spin-orbit coupling (SOC); the layers are separated by P atoms. The various Fe–Pt distances in FePt 12 clusters generate complex magnetic orders in FePt 5 P. According to temperature-dependent magnetic and specific heat measurements, FePt 5 P shows a stripe-type antiferromagnetic order at T N ≈ 90 K, which is also confirmed by resistivity measurements. Furthermore, a spin reorientation occurs at ~74 and ~68 K in and out of the ab plane based on the specific heat measurements. The temperature-dependent neutron powder diffraction patterns demonstrate the antiferromagnetic order in FePt 5 P, and the spins orientate up to 58.4° with respect to the c axis at 10 K. First-principles calculations of FePt 5 P show the band splitting at the Fermi level by strong SOC and the s–d hybridization between P and Fe/Pt electrons enhances the structural stability and affects the magnetic ordering.

36 MATERIALS SCIENCE↗

Multifunctional Cu 2 TSiS 4 (T = Mn and Fe): Polar Semiconducting Antiferromagnets with Nonlinear Optical Properties

In this work, Cu 2 TSiS 4 (T = Mn and Fe) polycrystalline and single-crystal materials were prepared with high-temperature solid-state and chemical vapor transport methods, respectively. The polar crystal structure (space group Pmn2 1 ) consists of chains of corner-sharing and distorted CuS 4 , Mn/FeS 4 , and SiS 4 tetrahedra, which is confirmed by Rietveld refinement using neutron powder diffraction data, X-ray single-crystal refinement, electron diffraction, energy-dispersive X-ray spectroscopy, and second harmonic generation (SHG) techniques. Magnetic measurements indicate that both compounds order antiferromagnetically at 8 and 14 K, respectively, which is supported by the temperature-dependent (100–2 K) neutron powder diffraction data. Additional magnetic reflections observed at 2 K can be modeled by magnetic propagation vectors k = (1/2,0,1/2) and k = (1/2,1/2,1/2) for Cu 2 MnSiS 4 and Cu 2 FeSiS 4 , respectively. The refined antiferromagnetic structure reveals that the Mn/Fe spins are canted away from the ac plane by about 14°, with the total magnetic moments of Mn and Fe being 4.1(1) and 2.9(1) μ B , respectively. Both compounds exhibit an SHG response with relatively modest second-order nonlinear susceptibilities. Density functional theory calculations are used to describe the electronic band structures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Magnetic Properties and Large Second-Harmonic Generation Response of a Chiral Ternary Chalcogenide: Eu 2 SiSe 4

Eu(II)-containing chalcogenides are an emerging class of materials that are of great interest due to their high optical activity and intriguing magnetism. Here, we synthesized Eu 2 SiSe 4 as red-colored single crystals and characterized its structure with single-crystal X-ray diffraction, confirming the reported chiral monoclinic P2 1 symmetry at room temperature. The crystal structure of Eu 2 SiSe 4 comprises distorted SiSe 4 tetrahedral units and charge-balancing Eu(II) cations. Here, we develop a two-step solid-state synthesis method for Eu 2 SiSe 4 and compare it to the known boron chalcogenide method. We find the second-harmonic generation (SHG) activity of polycrystalline Eu 2 SiSe 4 to be ∼7 × AgGaS 2 , placing it among the highest-known SHG-active chalcogenides. No symmetry lowering is observed down to 100 K in single-crystal X-ray diffraction, although an anomalous expansion in the b-axis lattice parameter occurs and may be correlated to lattice modes of the SiSe 4 tetrahedra. We investigate the physical properties of Eu 2 SiSe 4 using magnetometry and heat capacity measurements and find a transition to an antiferromagnetic ground state at T N ≈ 5.5 K. The low-temperature transition releases less entropy than expected, which may be due to the complex crystal electric field effects of Eu(II).

36 MATERIALS SCIENCE↗

Methods for Determining the Infrared Complex Refractive Indices n (λ) and k (λ) from Organic Solid Powders: Comparison of a Sucrose Single Crystal and a Pressed Pellet

There exists a need to measure optical constants n and k for many materials, especially organic solids in the infrared spectral region, but at present, there are only two established methods for making such measurements: single-angle (SA) reflectance and infrared spectroscopic ellipsometry (IRSE). The former derives the n/k vectors via measurement of the change in the amplitude of light reflected from the sample and then uses the Kramers–Kronig transform, while the latter measures the change in polarization of the reflected light from the sample to derive n/k. Here we make a direct comparison between the n/k vectors derived from SA measurements of a sucrose single crystal and the n/k values obtained after the crystal had been crushed, ground to powder, and pressed into a pellet form. The pellet was measured not only by SA but also via the IRSE method, and we found that pressing specular-quality pellets was critical, especially for the SA data. The n/k values of this typical organic molecule all agree to within 0.04 root-mean-square error, confirming that a pressed pellet can be used instead of a crystal to derive the intrinsic n/k vectors. In conclusion, this result is important for the many organic materials that, unlike sugar, do not have centimeter-sized crystals readily available.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Development of a Cold-Walled Molten Regolith Electrolysis Reactor for Lunar Oxygen Production

On the lunar surface, production of commodi-ties to support human presence, such as water, food and oxygen, and sustain the growth of a per-manent outpostwill likely require the use oflocal resources. The moon is covered almost entirely withfragmented oxide minerals known as regolithhundreds of meter thick.As a resource, it is rich in oxygen (> 42 wt.%) bound in a solid state with a variety of metals. The molten regolith electrolysis (MRE)reactor is a promising technology for the production of gaseous oxygen from the lunar reg-olithin a simple, single-stepreaction that requires minimalconsumable materials, produces oxygen and metals with high electrical efficiency and high yields from any regolithcomposition.This process involvesmelting regolith to~1600°C then electro-lyzing the molten pool to separate metal and oxy-gen ions that are then collected as liquid metal and gaseous oxygen at the respective electrodes. Lab-scale demonstrations of the MRE technology have previously reliedon external heating sources to bring the entirety of the reactor up to the operating temperaturewhich creates corrosive interfaces be-tween the molten regolith and the containment ma-terial in the reactor, limiting the overall lifespan of a reactor[1]. The Gaseous Lunar Oxygen from Regolith Electrolysis (GaLORE) project is focused on the development of a “cold-walled” or “Joule-heated” reactor design in which an internal heating source is used to selectively melt a pool of regolith between the electrodes of the reactor, leaving a shell of solidified regolith between the molten pool and the containment vessel of the reactor. This next generation reactor concept has been under development as molten oxide electrolysis (MOE) by MIT and Boston Metal for the production of iron from pure ores for terrestrial application [2]. The GaLORE project in engaged in early development of the technology for use with varying lunar regolith compositionsin the lunar environment. Thermal modelling of a proposed cold-walledreac-tor design were used as a scaffold to develop pa-rameters for a feasible reactor shape and size as well as target energy consumption[3]. The current development effort for the cold-walled reactor de-sign will be presented as a trade study of the most promising techniques for melting regolithwithin the constraints imposed by the lunar environment.Heater devices are designed to accommodate lim-ited electrical power availabilityon the moon, a wide range of regolith compositions that may be seen on the moon, limited metals available for re-placing consumed parts,and the low thermal con-ductivity of granular regolith in vacuum.Heater de-vices will be down-selectedbased on performance measurements within the above operationalcon-straints,and selected devices will be integrated into a reactor with electrodes to begin producing oxygen. [1]Sibille,L.,Sadoway, D.R.,Sirk, A., Tripathy,P.,Melendez, O., Standish, E., Dominguez, J. A., Stefanescu, D.M.,Curreri, P.A., Poizeau,S.,2009. “Recent Advancesin Scale-up Development of Molten Regolith Electrolysis for Oxygen Production in support of a Lunar Base.”AIAA 2009-659, 47th AIAA Aerospace Sciences Meeting, 5 -8 January 2009, Orlando, FL. [2] Boston Metal, https://www.boston-metal.com/moe-technology/#moe-process[3]Schreiner, S.S.,Sibille, L., Dominguez, J.A., Hoffman, J.A., 2016. "A parametric sizing model for Molten Regolith Electrolysis reactors to pro-duce oxygen on the Moon." Advances in Space Research 57.,7,1585-1603.

K D Grossman↗

Cs X Si 15 P 21 ( X = Sn or Pb): Polar Noncentrosymmetric Si–P Frameworks Stabilized by Covalent X –P Bonding

Metal silicon phosphides composed of earth-abundant Si and P tend to exhibit semiconducting properties and adopt diverse crystal structures with relatively small additions of structure-directing elements. The potential of silicon phosphide materials in nonlinear optical applications has been hindered by the inability to systematically produce noncentrosymmetric structures with such a flexible framework. Here, in this work, two isostructural compounds with a novel noncentrosymmetric structure were made possible by the inclusion of elements with stereochemically active lone pairs (Sn 2+ and Pb 2+ ). The structures were determined through single-crystal and synchrotron powder X-ray diffraction. Analysis of chemical bonding in real space through the electron localization function revealed stereochemically active Pb 2+ and Sn 2+ species in a trigonal pyramidal coordination with {Pb/Sn}–P bonds. Such covalent bonding between Pb and P is quite uncommon in extended solids and has been reported in a few rare instances. Band structure calculations and linear optical measurements confirm the semiconducting nature of Cs X Si 15 P 21 ( X = Sn or Pb). The synthesis was optimized to yield high-purity polycrystalline samples. The nonlinear optical properties show promising second-harmonic generation (SHG) coefficients from the Kurtz–Perry method. First-principles calculations of the nonlinear optical properties support the experimentally determined SHG values and provide moderate values of birefringence, suggesting Cs X Si 15 P 21 could be phase-matchable and practical nonlinear optical materials in the mid-IR region.

crystal structure↗

Timing Performance of the CMS High Granularity Calorimeter Prototype

This paper describes the experience with the calibration,reconstruction and evaluation of the timing capabilities of the CMSHGCAL prototype in the beam tests in 2018. The calibrationprocedure includes multiple steps and corrections ranging from tensof nanoseconds to a few hundred picoseconds. The timing performanceis studied using signals from positron beam particles with energiesbetween 20 GeV and 300 GeV. The performance is studied as afunction of particle energy against an external timing reference aswell as standalone by comparing the two different halves of theprototype. The timing resolution is found to be 60 ps forsingle-channel measurements and better than 20 ps for full showersat the highest energies, setting excellent perspectives for theHGCAL calorimeter performance at the HL-LHC.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Interfacial defect reduction enhances universal power law response in Mo–SiNx granular metals

Granular metals (GMs), consisting of metal nanoparticles separated by an insulating matrix, frequently serve as a platform for fundamental electron transport studies. However, few technologically mature devices incorporating GMs have been realized, in large part because intrinsic defects (e.g., electron trapping sites and metal/insulator interfacial defects) frequently impede electron transport, particularly in GMs that do not contain noble metals. Here, we demonstrate that such defects can be minimized in molybdenum–silicon nitride (Mo–SiN x ) GMs via optimization of the sputter deposition atmosphere. For Mo–SiN x GMs deposited in a mixed Ar/N 2 environment, x-ray photoemission spectroscopy shows a 40%–60% reduction of interfacial Mo-silicide defects compared to Mo–SiN x GMs sputtered in a pure Ar environment. Electron transport measurements confirm the reduced defect density; the dc conductivity improved (decreased) by 10 4 –10 5 and the activation energy for variable-range hopping increased 10×. Since GMs are disordered materials, the GM nanostructure should, theoretically, support a universal power law (UPL) response; in practice, that response is generally overwhelmed by resistive (defective) transport. Here, the defect-minimized Mo–SiN x GMs display a superlinear UPL response, which we quantify as the ratio of the conductivity at 1 MHz to that at dc, Δσ ω ⁠. Remarkably, these GMs display a Δσ ω up to 10 7 , a three-orders-of-magnitude improved response than previously reported for GMs. By enabling high-performance electric transport with a non-noble metal GM, this work represents an important step toward both new fundamental UPL research and scalable, mature GM device applications.

36 MATERIALS SCIENCE↗

Measurement of the fractional radiation length of a pixel module for the CMS Phase-2 upgrade via the multiple scattering of positrons

High-luminosity particle collider experiments such as theones planned at the High-Luminosity Large Hadron Collider requireever-greater vertexing precision of the tracking detectors,necessitating reductions in the material budget of the detectors.Traditionally, the fractional radiation length (x/X$_{0}$) ofdetectors is either estimated using known properties of theconstituent materials, or measured in dedicated runs of the finaldetector. In this paper, we present a method of direct measurementof the material budget of a CMS prototype module designed for thePhase-2 upgrade of the CMS detector using a 40–65 MeV positronbeam. A total of 630 million events were collected at the PaulScherrer Institut PiE1 experimental area using a three-planetelescope consisting of the prototype module as the central plane,surrounded by two MALTA monolithic pixel detectors. Fractionalradiation lengths were extracted from scattering angle distributionsusing the Highland approximation for multiple scattering. Astatistical technique recovered runs suffering from triggerdesynchronisation, and several corrections were introduced tocompensate for local inefficiencies related to geometric and beamshape constraints. Two regions of the module were surveyed andyielded average x/X$_{0}$ values of (0.72 ± 0.05)% and(0.95 ± 0.09)%, which are compatible with empirical estimatesfor these regions computed from known material properties of 0.753%and 0.892%, respectively. Two types of higher-granularity maps ofthe fractional radiation length were produced, subdivided eitherinto rectangular regions of uniform size, or polygonal-shapedregions of uniform material composition. The results bode well forthe CMS Phase-2 upgrade modules, which will play a key role in theminimisation of the material of the upgraded detector.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Exploring the Links between Structural Distortions, Orbital Ordering, and Multipolar Magnetic Ordering in Double Perovskites Containing Re(VI) and Os(VII)

A combination of high-resolution powder diffraction techniques and solid-state NMR has been employed to explore the links between crystal structure, orbital ordering, and magnetism in three isostructural double perovskites containing transition metal ions with a 5d 1 configuration. In Ba 2 ZnReO 6 , both neutron and synchrotron X-ray powder diffraction data reveal a cubic-to-tetragonal transition at 23 K that breaks the degeneracy of the t 2g orbitals and leads to a pattern of orbital ordering that stabilizes magnetic ordering when the sample is cooled below 16 K. Similar behavior is observed in Ba 2 MgReO 6 , with an orbital ordering temperature of 33 K and a magnetic ordering temperature of 18 K. Prior theoretical works suggest that the pattern of orbital order seen in the P42/mnm space group is needed to stabilize the heavily canted antiferromagnetism of these compounds. Unfortunately, powder diffraction data is not sensitive enough to differentiate between the I4/mmm and P42/mnm structural models, as the distortions are too subtle to be unambiguously identified from either neutron or synchrotron X-ray powder diffraction methods. In contrast, both diffraction and 7 Li NMR data indicate that Ba 2 LiOsO 6 retains the cubic structure down to 1.7 K. The antiferromagnetic ground state and lack of any sign of orbital ordering in Ba 2 LiOsO 6 provide compelling evidence that the electronically driven tetragonal distortion seen in Ba2ZnReO6, and Ba2MgReO6 is intimately linked to the magnetic ordering seen in those compounds. The absence of magnetic reflections in high intensity neutron powder diffraction data collected on Ba 2 MgReO 6 strongly suggests ordering of multipolar moments on Re(VI), likely ferro-octupolar ordering.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Intercalation-Induced Topotactic Phase Transformation of Tungsten Disulfide Crystals

Recent research has demonstrated the potential for topological superconductivity, anisotropic Majorana bound states, optical nonlinearity, and enhanced electrochemical activity for transition metal dichalcogenides (TMDs) with a 2M structure. These unique TMD compounds exhibit metastability and, upon heating, undergo a transition to the thermodynamically stable 2H phase. The 2M phase is commonly made at high temperatures using traditional solid-state methods, and this metastability further complicates the growth of large 2M WS 2 crystals. Herein, a novel synthetic method was developed, focusing on a molten salt reaction to synthesize large 2H crystals and then inducing transformation to the 2M phase through intercalation and thermal treatment. The 2H crystals were intercalated via a room-temperature sodium naphthalenide solution, producing a previously unreported Na-intercalated 2H WS 2 phase. Thermal heating was required to facilitate the phase transition to the intercalated 2M crystal structure. This phase transition was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), electron dispersive X-ray spectroscopy (EDS), and Raman spectroscopy, which confirmed the synthesis of the intercalated 2M phase. Upon deintercalation, crystal and powder samples showed superconductivity with a T c of 8.6–8.7 K, similar to previously reported values. The generality of this process was further demonstrated using alkali metal triethyl borohydride to intercalate 2H WS 2 and produced the desired 2M phase. This novel synthetic method has broad implications for discovering metastable phases in other TMD families and layered materials. Furthermore, separation of the intercalation and phase transition also has the potential to allow for large-scale synthesis of this technologically important phase with greater control over each step of the reaction.

36 MATERIALS SCIENCE↗

Neutron irradiation and electrical characterisation of the first 8” silicon pad sensor prototypes for the CMS calorimeter endcap upgrade

As part of its HL-LHC upgrade program, the CMS collaboration is replacing its existing endcap calorimeters with a high-granularity calorimeter (CE). The new calorimeter is a sampling calorimeter with unprecedented transverse and longitudinal readout for both electromagnetic and hadronic compartments. Due to its compactness, intrinsic time resolution, and radiation hardness, silicon has been chosen as active material for the regions exposed to higher radiation levels. The silicon sensors are fabricated as 20 cm (8”) wide hexagonal wafers and are segmented into several hundred pads which are read out individually. As part of the sensor qualification strategy, 8” sensor irradiation with neutrons has been conducted at the Rhode Island Nuclear Science Center (RINSC) and followed by their electrical characterisation in 2020-21. The completion of this important milestone in the CE's R&D program is documented in this paper and it provides detailed account of the associated infrastructure and procedures.The results on the electrical properties of the irradiated CE silicon sensors are presented.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Pixel response characterization of the ARCADIA fully depleted MAPS

Monolithic Active Pixel Sensors (MAPS) achieved widespread use in several scientific applications, thanks to their properties, such as low material budget and high granularity. The ARCADIA INFN project developed a Fully-Depleted MAPS (FD-MAPS), using a modified LFoundry 110 nm CIS process. This work presents the first laboratory characterization of the ARCADIA MD3 prototype. Measurements include threshold uniformity studies using both test-pulse injection and a 55 Fe source, as well as threshold and noise calibration achieved thanks to monochromatic X-ray sources. Ultimately, charge-collection efficiency is evaluated using an infrared laser setup.

Particle tracking detectors↗