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At least 1,009 records · Page 56

Pre- and post-annealing of mechanical damage in silicon wafers

Basic properties of mechanical damage in silicon consisting of cracks and abrasion were studied using transmission electron microscopy. The crystallographic structure of mechanical damage was determined before and after high temperature annealing. The main findings include that stresses in silicon around crack tips are not plastically relieved at room temperature and that abrasion at room temperature introduces shear loops into the silicon. It was also found that cracks of micron size can be annealed out, specifically, if cleavage occurs on 111 planes. The healing products of such cracks are 60 deg and 90 deg dislocations. Submicron cracks transform into stacking faults during annealing. Likewise high concentrations of shear loops due abrasion were found to anneal into stacking faults. A one to one correlation between surface areas containing small cracks and stacking faults was made. Measurements of damage removal on silicon surfaces through chemical-mechanical etching techniques are presented. It is shown that silicon dioxide repolishes damaged silicon surfaces most effectively.

Schwottke, G. H.↗

Cryogenic Electronics Being Developed for Space Operation

Planetary exploration missions and deep space probes require electrical power management and control systems that can operate efficiently and reliably in very low temperature environments. Presently, spacecraft operating in the cold environment of deep space carry a large number of radioisotope heating units to maintain the surrounding temperature of the onboard electronics at approximately 20 C. Electronics capable of operation at cryogenic temperatures would not only tolerate the hostile environment of deep space but also reduce system size and weight by eliminating or reducing the radioisotope heating units and their associate structures. Thereby, such electronics would reduce system development as well as launch costs. In addition, power electronic circuits designed for operation at low temperatures are expected to result in more efficient systems than those at room temperature. This improvement results because semiconductor and dielectric materials have better behavior and tolerance in their electrical and thermal properties at low temperatures. The Low Temperature Electronics Program at the NASA Glenn Research Center is focusing on the research and development of electrical components, circuits, and systems suitable for applications in the aerospace environment and in deep space exploration missions. Research is being conducted on devices and systems for reliable use down to cryogenic temperatures. Some of the commercial off-the-shelf as well as developed components that are being characterized include semiconductor switching devices, resistors, magnetics, and capacitors. Semiconductor devices and integrated circuits including digital-to-analog and analog-to-digital converters, dc-dc converters, operational amplifiers, and oscillators are also being investigated for potential use in low-temperature applications. For example, the output response of an advanced oscillator at room temperature and at -190 C is shown. Most oscillators can operate at temperatures down to only -55 C. It can be seen that, for this oscillator, the low temperature of -196 C changed the leading and trailing edges of the oscillator pulses by producing overshoot. The research and development efforts performed under the Low Temperature Electronics Program at Glenn are being carried out through collaboration with other Government agencies, industrial and aerospace companies, and academia. The program supports missions as well as technology development efforts at NASA's Goddard Space Flight Center and Langley Research Center, and the Jet Propulsion Laboratory.

Patterson, Richard L.↗

Develop low-temperature diffusional moisture outgassing model for silica-filled silicones

A universal outgassing model for all silica-filled silicones would allow researchers to make moisture outgassing predictions for many different silica-filled silicones using the same sets of kinetic parameters (but with different intensities for the outgassing constituents). In FY 2020, we succeeded in developing such a model for outgassing in a vacuum/dry environment after ~ 1-2 hours of room temperature vacuum pump. That means the FY2020 model does not account for the low temperature diffusional moisture outgassing during the first few hours under vacuum pump. In FY 2021, we have used the experimental technique of dynamic vapor sorption together with the modified Page diffusion model to measure and quantify the low temperature (i. e. room temperature) diffusional moisture release to complete our universal moisture outgassing model for silica-filled silicones from low temperatures to high temperatures.

36 MATERIALS SCIENCE↗

Optimization of the light detection system of the ICARUS detector

The ICARUS detector, a key component of the Short Baseline Neutrino (SBN) Program at Fermi National Acelerator Laboratory (FNAL), is a 600-ton Liquid Argon Time Projection Chamber (LArTPC) equipped with a Light Detection System (LDS) that uses 360 Hamamatsu R5912-MOD 8-inch photomultiplier tubes (PMTs), specifically designed to operate under cryogenic conditions ($\sim 87 \ K$). These PMTs feed the trigger signal to the readout, improve the spatial and timing resolution of the events, and contribute to cosmic rays mitigation. During operation at FNAL, a progressive degradation in the PMT gain was observed. We developed an experimental setup to investigate the temperature dependence of PMT performance. Gain measurements were carried out from room temperature to $-70 ^\circ C$ using an environmental chamber. The results show that, while the PMTs exhibit stable performance at room temperature, a significant and irreversible reduction in gain emerges at lower temperatures. Al though $-70 ^\circ C$ remains above the liquid argon temperatures, the trend clearly reveals a gain-sensitive degradation mechanism. A simplified physical model was developed to reproduce and interpret the observed behavior. Based on these findings, a series of mitigation strategies were implemented in the ICARUS detector to preserve PMT performance and ensure reliable operation under cryogenic conditions.

Saia, C. [Catania Astrophys. Observ.]↗

Demonstration of SiC Pressure Sensors at 750 C

We report the first demonstration of MEMS-based 4H-SiC piezoresistive pressure sensors tested at 750 C and in the process confirmed the existence of strain sensitivity recovery with increasing temperature above 400 C, eventually achieving near or up to 100% of the room temperature values at 750 C. This strain sensitivity recovery phenomenon in 4H-SiC is uncharacteristic of the well-known monotonic decrease in strain sensitivity with increasing temperature in silicon piezoresistors. For the three sensors tested, the room temperature full-scale output (FSO) at 200 psig ranged between 29 and 36 mV. Although the FSO at 400 C dropped by about 60%, full recovery was achieved at 750 C. This result will allow the operation of SiC pressure sensors at higher temperatures, thereby permitting deeper insertion into the engine combustion chamber to improve the accurate quantification of combustor dynamics.

Semiconductor↗

Delayed onset of discontinuous precipitation-based phase transformation in U10Mo alloys doped with Silicon

A uranium-10 wt% molybdenum (U-10Mo) alloy is one of the primary candidates for metallic fuels that would use low-enriched uranium in place of highly enriched uranium, to support nuclear nonproliferation efforts. Optimal performance of a U-based metallic nuclear fuel can be achieved by retaining the high-temperature, body-centered cubic (bcc) allotrope (γ-U) at room temperature, which can be accomplished in the U-10Mo alloy. However, presence of minor alloying elements can influence the final constitution of room-temperature phases in the U10Mo alloy, specifically, formation of α-U phase which results in anisotropic behavior of the fuel in reactor. Further, through a detailed transmission electron microscopy analysis, the present study reports the constituent phases that are present in a U10Mo alloy containing ~0.1 wt% Si after it is subjected to homogenization heat treatment and thermomechanical processing. For comparison, results from an undoped U10Mo alloy are also included. The experimental results reveal that γ-UMo solid solution is the major phase in a hot-rolled, Si-doped U10Mo alloy metallic fuel foil, along with U 2 MoSi 2 C, UC, and U 2 Mo, after isothermal annealing at 460 °C for 10h. In contrast, after the same heat treatment, the undoped U10Mo alloy metallic fuel had formed a noticeable amount of α-U along prior γ-UMo grain boundaries through discontinuous precipitation (DP, area fraction: ~27.9%) with characteristic lamellar morphology, together with γ-UMo, UC, and U 2 Mo. This result indicates that doping with Si could mitigate the DP reaction in U10Mo alloy and prevent formation of undesirable α-U. This work sheds light on optimizing Si-doping–dominated microstructure in U10Mo fuels and facilitates designing and tuning of microstructures of U10Mo alloys for tailoring the final designed performance of the fuel under irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Optimization of the light detection system of the ICARUS detector

The Short Baseline Neutrino (SBN) Program at Fermilab is designed to investigate short-baseline neutrino oscillations and test the hypothesis of sterile neutrinos, motivated by several experimental anomalies observed over the past decades. Within this program, the ICARUS experiment plays a key role. It employs the world’s largest Liquid Argon Time Projection Chamber (LArTPC) and serves as the farthest and most sensitive SBN detector for studying muon and electron neutrino oscillations. A crucial subsystem of the ICARUS detector is the Light Detection System (LDS), which captures the prompt scintillation light produced by neutrino interactions in the 600-ton active liquid Argon volume. This system provides precise timing information that is essential for event reconstruction, the trigger system, and cosmic background rejection. The LDS is composed of 360 Hamamatsu R5912-MOD 8-inch photomultiplier tubes (PMTs), operating under cryogenic conditions ($\sim 87 \ K$) inside the detector’s cryostats. During the detector’s operation at FNAL, a degradation in PMT gain has been observed, attributed to aging under low-temperature conditions. In collaboration with ICARUS teams from INFN Pavia and Catania, I developed an experimental setup to study the temperature-dependent behavior of the PMTs, performing gain measurements both at room temperature and down to $-70°C$ using a climatic chamber at INFN Catania. The results indicate that while the PMTs maintain stable gain at room temperature, a significant and permanent gain reduction occurs at low temperatures. Although $-70°C$ is still warmer than liquid Argon temperatures, the findings clearly demonstrate a gain-dependent performance degradation. The thesis also discusses mitigation strategies implemented in the ICARUS detector to address this issue and presents a simplified model to describe and simulate the observed behavior.

Saia, Clara [Catania U.] (ORCID:0009000464102417)↗

Syntheses of gold supported on metal oxides and their application in organic transformations

Herein, we report a general and straightforward synthesis method for gold supported on mesoporous and microporous metal oxides. Supported materials, in general, show higher crystallinity compare to unsupported systems as verified through powder X-ray diffraction (XRD). Also, through XRD, most of the metal is observed to be in its oxide form, whereas the gold support was found to be in its metallic state, which has been further confirmed from TEM. In terms of surface area, the catalyst was not found to follow any trend. Morphology wise, there are no changes observed after doping except in few cases. Combined results from XRD, X-ray fluorescence spectroscopy, Auger, and X-ray photoelectron spectroscopy suggest that gold is mainly in the bulk and very little (0.04% in case of gold doped calcium oxide) or non (in case of gold doped mixed manganese-cerium oxide) on the surface. The presence of Au (0) 4f peaks in XPS further confirms the metallic state of the gold. Oxides of indium, magnesium and calcium have been studied for the organic transformation reactions. An enhancement in activity and product selectivity was observed in the case of the gold supported catalysts. Indium serves as a great catalyst for C–C coupling and electrophilic aromatic substitution reactions and gives >99% conversion. Interestingly, 88% selectivity for C–C coupling and >99% selectivity for aromatic substitution have been achieved at 100 °C and room temperature respectively. Magnesium and calcium give Knoevenagel condensation products. At room temperature with very low catalyst loading, >99% conversion and selectivity were observed for the Knoevenagel reaction with as high as 35.30 TOF. Finally, a mechanism for the C–C coupling reaction has been proposed based on these results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The role of iron in magnetic damping of Mg(Al,Fe) 2 O 4 spinel ferrite thin films

© 2020 Author(s). We have investigated magnesium aluminum ferrite thin films with a range of iron concentrations and identified the optimal iron content to obtain high crystalline quality thin films with the low magnetic damping required for spin current-based applications. Epitaxial MgAl 2-x FexO4 films with 0.8 < x < 2.0 were grown by pulsed laser deposition on single crystal MgAl2O4 substrates and were characterized structurally and magnetically. We find that the x = 1.5 composition minimizes the room-temperature magnetic damping with a typical Gilbert damping parameter of α eff = 1.8 × 10-3. This minimized damping is governed by a competition between the more robust magnetic ordering with increased iron content, x, and the more defective structure due to larger film-substrate lattice mismatch with increased iron content. The temperature-dependent magnetization curves indicate that Tc is suppressed below room temperature for iron content x ≤ 1.2 and eventually suppressed entirely for x = 0.8. X-ray magnetic circular dichroism results indicate that for all x the magnetic moment is dominated by Fe 3 + cations distributed in a 60:40 ratio on the octahedral and tetrahedral sites, with minimal contribution from Fe 2 + cations. Films with x = 1.4-1.6 exhibit very strong ferromagnetic resonance and low Gilbert damping with α eff = (1.8-6) × 10-3, making them ideal candidates for microwave and spintronic applications.

36 MATERIALS SCIENCE↗

The effects of space radiation on a chemically modified graphite-epoxy composite material

The effects of the space environment on the engineering properties and chemistry of a chemically modified T300/934 graphite-epoxy composite system are characterized. The material was subjected to 1.0 x 10 to the 10th power rads of 1.0 MeV electron irradiation under vacuum to simulate 30 years in geosynchronous earth orbit. Monotonic tension tests were performed at room temperature (75 F/24 C) and elevated temperature (250 F/121 C) on 4-ply unidirectional laminates. From these tests, inplane engineering and strength properties (E sub 1, E sub 2, Nu sub 12, G sub 12, X sub T, Y sub T) were determined. Cyclic tests were also performed to characterize energy dissipation changes due to irradiation and elevated temperature. Large diameter graphite fibers were tested to determine the effects of radiation on their stiffness and strength. No significant changes were observed. Dynamic-mechanical analysis demonstrated that the glass transition temperature was reduced by 50 F(28 C) after irradiation. Thermomechanical analysis showed the occurrence of volatile products generated upon heating of the irradiated material. The chemical modification of the epoxy did not aid in producing a material which was more radiation resistant than the standard T300/934 graphite-epoxy system. Irradiation was found to cause crosslinking and chain scission in the polymer. The latter produced low molecular weight products which plasticize the material at elevated temperatures and cause apparent material stiffening at low stresses at room temperature.

Reed, S. M.↗

Demonstration of Oxygen and Carbon Monoxide Propellants for Mars Missions

Currently, proposed planetary exploration missions must be small, with low costs and a short development time. Relatively high-risk technologies are being accepted for such missions if they meet these guidelines. For a Mars sample-return mission, one of the higher risk technologies is the use of return propellants produced from indigenous materials such as the Martian atmosphere. This consists of 96 percent carbon dioxide, which can be processed into oxygen and carbon monoxide. This year, the NASA Lewis Research Center completed the experimental evaluation and subscale technology development of an oxygen/carbon monoxide propellant combination. Previous research included ignition characterization, combustion performance, and heat transfer characterization with gaseous propellants at room temperature. In this year s tests, we studied the ignition characteristics and combustion of oxygen and carbon monoxide at near liquid temperatures. The mixture ratio boundaries for oxygen and carbon monoxide were determined as a function of propellant temperature in a spark torch igniter. With both propellants at room temperature, the ignition range was between 0.50 and 1.44; and with both propellants chilled to near-liquid temperatures, it was between 2.4 and 3.1. Statistical analysis of the mean value of the ignition boundaries provided models that describe the combination of oxygen temperature, carbon monoxide temperature, and mixture ratio that resulted in ignition. This range is the larger boxed area shown in the figure. The smaller boxed area indicates the range at which there is a 90-percent confidence that ignition will occur. The relatively small range at only 90-percent confidence indicates that using the oxygen/carbon monoxide combination as its own ignition source may not be the best design for a remote engine operating on Mars. Tests also were performed in a simulated small rocket engine that used oxygen/hydrogen combustion gases as the ignition source for oxygen/carbon monoxide. In these experiments, the oxygen/carbon monoxide was successfully ignited in eight of eight tests at a mixture ratio of 0.52. In addition, the oxygen/carbon monoxide maintained steady combustion after the oxygen/hydrogen ignition source was removed, verifying that the oxygen/carbon monoxide rocket engine should continue to be included in mission plans as return propulsion from Mars.

Linne, Diane L.↗

Strong, Tough, and Pest Resistant MoSi2-Base Hybrid Composite for Structural Applications

Addition of about 30 to 50 vol % of Si3N4 particulate to MoSi2 improved resistance to low temperature accelerated oxidation by forming a Si2ON2 protective scale and thereby eliminating catastrophic 'pest failure'. The Si3N4 addition also improved the high temperature creep strength by nearly five orders of magnitude, doubled the room temperature toughness and significantly lowered the CTE of the MoSi2 and eliminated matrix cracking in SCS-6 reinforced composites even after thermal cycling. The SCS-6 fiber reinforcement improved the room temperature fracture toughness by seven times and impact resistance by five times. The composite exhibited excellent strength and toughness improvement up to 1400 C. More recently, tape casting was adopted as the preferred processing of MoSi2-base composites for improved fiber spacing, ability to use small diameter fibers, and for lower cost. Good strength and toughness values were also obtained with fine diameter Hi-Nicalon tow fibers. This hybrid composite remains competitive with ceramic matrix composites as a replacement for Ni-base superalloys in aircraft engine applications.

Hebsur, M. G.↗

Development and Characterization of SiC)/ MoSi2-Si3N4(p) Hybrid Composites

Intermetallic compound MoSi2 has long been known as a high temperature material that has excellent oxidation resistance and electrical/thermal conductivity. Also its low cost, high melting point (2023 C), relatively low density (6.2 g/cu cm versus 9 g/cu cm for current engine materials), and ease of machining, make it an attractive structural material. However, the use of MoSi2 has been hindered due to its poor toughness at low temperatures, poor creep resistance at high temperatures, and accelerated oxidation (also known as 'pest' oxidation) at temperatures between approximately 450 and 550 C. Continuous fiber reinforcing is very effective means of improving both toughness and strength. Unfortunately, MoSi2 has a relatively high coefficient of thermal expansion (CTE) compared to potential reinforcing fibers such as SiC. The large CTE mismatch between the fiber and the matrix resulted in severe matrix cracking during thermal cycling. Addition of about 30 to 50 vol % of Si3N4 particulate to MoSi2 improved resistance to low temperature accelerated oxidation by forming a Si2ON2 protective scale and thereby eliminating catastrophic 'pest failure'. The Si3N4 addition also improved the high temperature creep strength by nearly five orders of magnitude, doubled the room temperature toughness and significantly lowered the CTE of the MoSi2 and eliminated matrix cracking in SCS-6 reinforced composites even after thermal cycling. The SCS-6 fiber reinforcement improved the room temperature fracture toughness by seven times and impact resistance by five times. The composite exhibited excellent strength and toughness improvement up to 1400 C. More recently, tape casting was adopted as the preferred processing of MoSi2-base composites for improved fiber spacing, ability to use small diameter fibers, and for lower cost. Good strength and toughness values were also obtained with fine diameter Hi-Nicalon tow fibers. This hybrid composite remains competitive with ceramic matrix composites as a replacement for Ni-base superalloys in aircraft engine applications.

Hebsur, Mohan G.↗

MoSi2-Base Hybrid Composites from Aeroengine Applications

Addition of about 30 to 50 vol % of Si3N4 particulate to MoSi2 improved low temperature accelerated oxidation resistance by forming a Si2ON2 protective scale and thereby eliminated catastrophic 'pest failure'. The Si3N4 addition also improved the high temperature creep strength by nearly five orders of magnitude, doubled the room temperature toughness, and significantly lowered the CTE of the MoSi2 which eliminated matrix cracking in SCS-6 reinforced composites even after thermal cycling. The SCS-6 fiber reinforcement improved the room temperature fracture toughness by seven times and impact resistance by five times. The composite exhibited this excellent strength and toughness improvement up to 1673 K. More recently, tape casting was adopted as the preferred processing of MoSi2-base composites due to improved fiber spacing, ability to use small diameter fibers, and for lower cost. Good strength and toughness values were also obtained with fine diameter Hi-Nicalon tow fibers. These hybrid composites remain competitive with ceramic matrix composites as a replacement for Ni-base superalloys in aircraft engine applications.

Hebsur, Mohan G.↗

Correcting for digital image correlation speckle inversion at high temperature using color cameras

Digital image correlation (DIC) is a popular, noncontacting technique to measure full-field deformation by using cameras to track the motion of an applied surface pattern. Because it is noncontacting, DIC can be performed for extreme temperature applications (e.g., hot-fire rocket testing of carbon composite rocket nozzles) under harsh conditions during which bonded gauges are damaged. Speckle pattern inversion is a phenomenon that sometimes occurs while performing high-temperature DIC. During speckle pattern inversion, portions of the surface pattern that were initially darker at room temperature (e.g., graphite) may emit more light due to blackbody radiation than the portions that were initially paler, thereby producing images in which the pattern appears inverted at high temperature relative to the initial pattern at room temperature. This phenomenon can prevent the correlation algorithm from being able to resolve the displacements between images. This work compares three methods to mitigate speckle pattern inversion: (A) the subtraction method, a recently-published technique in which two high-temperature images are subtracted to remove unwanted light; (B) the filtering method, a popular technique in which optical bandpass filters screen out unwanted light; and (C) the histogram rescaling method, a proposed new method that pairs a color camera with a blue light source and uses information from the green sensor of the camera to correct against inversion in the blue sensor through postprocessing. The histogram rescaling method is shown to successfully eliminate speckle pattern inversion and has the added advantages that it does not require quasi-static loading to be able to compensate for speckle pattern inversion, nor does it impose thick-glass distortions caused by the optical filter.

Rowley, Lindsey J.↗

Characterization of Silicon Photomultiplier Photon Detection Efficiency at Liquid Nitrogen Temperature

The detection of individual photons at cryogenic temperatures is of interest to many experiments searching for physics beyond the Standard Model. Silicon photomultipliers (SiPMs) are often deployed in liquid argon or liquid xenon to detect scintillation light either directly or after it has been wavelength-shifted. Maximizing the photon detection efficiency (PDE) of the SiPMs used in these experiments optimizes the sensitivity to new physics; however, the PDEs of commercial SiPMs, although well known at room temperature, are not well characterized at the cryogenic temperatures at which many experiments operate them. Here we present results from an experimental setup that measures the photon detection efficiencies of silicon photomultipliers at liquid nitrogen temperature, 77 K. Results from a KETEK PM3325-WB-D0 and a Hamamatsu S13360-3050CS silicon photomultiplier — of R&D interest to the LEGEND experiment — exhibit a decrease in photon detection efficiency greater than 20% at liquid nitrogen temperature relative to room temperature for 562 nm light.

Cryogenic detectors↗

Feasibility study for the development of low temperature curing adhesives

The feasibility of a new approach for the development of stable, easily handled, room temperature (293 K - 311 K) curing adhesives was studied and demonstrated. The work concentrated on a family of unsaturated amide/ester resins. Twelve candidate resins were synthesized and tested for completeness of cure at room temperature, adhesion to aluminum and titanium, shear strength, moisture resistance and heat stability. The three most promising candidate resins were selected and recommended for further development.

Green, H. E.↗