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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Nuclear fuel irradiation testbed for nuclear security applications

The nuclear security community has long been interested in the identification and quantification of nuclear material signatures to understand a material’s provenance, use, and ultimate application. New forensics signatures and methods intended for non-traditional or advanced nuclear fuel applications require fuel irradiation experiments to demonstrate viability and validity. Integral fuel irradiations have historically required significant costs and long timelines to design, irradiate, and characterize. This paper describes how a recently developed nuclear fuel irradiation testbed can be used to provide a low cost, rapid turnaround, modular test environment for irradiation and evaluation of nuclear fuel specimens for nuclear security applications. The irradiation testbed houses six small ‘MiniFuel’ samples within hermetically sealed capsules inside targets that can be removed in between each ∼25-day operating cycle of the High Flux Isotope Reactor (HFIR). As many as nine targets can be irradiated using a single irradiation position (reflector region) in HFIR, allowing for varying irradiation temperatures and burnups. A suite of hot cell capabilities have been established to perform post-irradiation examination for measuring performance (e.g., fuel swelling, fission gas release) and facilitating experiment disassembly for subsequent property measurements, microstructural analysis, or chemical assay. This new testbed allows fuel irradiations to be conducted on an accelerated timeframe to enable rapid proof of concept testing and to provide reference material for nuclear fuel security applications. Recent applications using this testbed include the testing of isotopic taggants in UO 2 fuel (intentional forensics), testing of U-10Mo fuel for down-conversion of highly enriched uranium–fueled reactors, and the production of irradiated UO 2 fuel material for signature analysis of its isotopic composition (plutonium, fission gases, etc.).

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2022

All-Ceramic Passive Wireless Temperature Sensor Realized by Tin-Doped Indium Oxide (ITO) Electrodes for Harsh Environment Applications

In this work, an all-ceramic passive wireless inductor–capacitor (LC) resonator was presented for stable temperature sensing up to 1200 °C in air. Instead of using conventional metallic electrodes, the LC resonators are modeled and fabricated with thermally stable and highly electroconductive ceramic oxide. The LC resonator was modeled in ANSYS HFSS to operate in a low-frequency region (50 MHz) within 50 × 50 mm geometry using the actual material properties of the circuit elements. The LC resonator was composed of a parallel plate capacitor coupled with a planar inductor deposited on an Al2O3 substrate using screen-printing, and the ceramic pattern was sintered at 1250 °C for 4 h in an ambient atmosphere. The sensitivity (average change in resonant frequency with respect to temperature) from 200–1200 °C was ~170 kHz/°C. The temperature-dependent electrical conductivity of the tin-doped indium oxide (ITO, 10% SnO2 doping) on the quality factor showed an increase of Qf from 36 to 43 between 200 °C and 1200 °C. The proposed ITO electrodes displayed improved sensitivity and quality factor at elevated temperatures, proving them to be an excellent candidate for temperature sensing in harsh environments. The microstructural analysis of the co-sintered LC resonator was performed using a scanning electron microscope (SEM) which showed that there are no cross-sectional and topographical defects after several thermal treatments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1987

Study of the production of some superconducting and magnetic materials by solidification in the drop tube and drop tower

A systematic study on the relationship between the microstructure and physical properties of several superconducting materials prepared by solidification in low gravity was conducted. Further study of the materials, such as the applications of hydrostatic pressure which is known to be an effective mean to vary the electronic structure of materials, in conjunction with the detailed microstructure analysis of the samples was also performed to better understand the low gravity effects on the enhancement of the electronic properties. Results of the studies on the directionally solidified AlInSn alloys processed in the KC-135 aircraft and immiscible GaBi alloy prepared during free fall in the Marshall Space Flight Center Drop Tower are presented.

Wu, M. K.↗
NASA NTRS1991

Microstructural and magnetic characterization of rapidly solidified and annealed Pt-Co-B alloys

Significant increases in intrinsic coercivity (Hic) of Pt-Co alloys have been obtained by the addition of boron and the application of rapid solidification processing. After rapid solidification by double anvil splat quenching with subsequent annealing at 650 C for 30 min, an alloy of Pt42Co45B13 exhibits an Hic as high as 14 kOe. Annealing of the Pt-Co-B influences the L1(0) superlattice structure and grain size of the matrix, the crystal structure and size of Co-boride precipitate, and the distribution of magnetic domain walls. A microstructural analysis shows that the maximum H(ic) occurs when Co borides, having the Co3B structure, are within the single magnetic domain size. The magnetic hardening mechanism in Pt-Co-B is believed to be a combination of inhibited magnetic domain nucleation and difficult reverse magnetic domain growth caused by the interaction of the magnetically anisotropic Co borides with the L1(0) Pt-Co matrix.

Qiu, N.↗
NASA NTRS1991

Long discontinuous fiber composite structure: Forming and structural mechanics

Cost effective composite structure has motivated the investigation of several new approaches to develop composite structure from innovative material forms. Among the promising new approaches is the conversion of planar sheet to components of complex curvature through sheet forming or stretch forming. In both cases, the potential for material stretch in the fiber direction appears to offer a clear advantage in formability over continuous fiber systems. In the present study, the authors have established a framework which allows the simulation of the anisotropic mechanisms of deformation of long discontinuous fiber laminates wherein the matrix phase is a viscous fluid. The initial study focuses upon the establishment of micromechanics models for prediction of the effective anisotropic viscosities of the oriented fiber assembly in a viscous matrix. Next, the developed constitutive relation is employed through an analogy with incompressible elasticity to exercise the finite element technique for determination of local fiber orientation and laminate thickness after forming. Results are presented for the stretch bending of a curved beam from an arbitrary composite laminate and the bulging of a clamped sheet. Structural analyses are conducted to determine the effect of microstructure on the performance of curved beams manufactured from long discontinuous fiber composites. For the purposes of this study, several curved beams with ideal and non-ideal microstructures are compared for response under pure bending. Material parameters are determined from a separate microstructural analysis.

Pipes, R. B.↗
NASA NTRS1992

Solidification kinetics and metastable phase formation in binary Ti-Al

Electromagnetic levitation was used to solidify near-equiatomic alloys of Ti-Al at various bulk undercoolings. Detailed thermal histories were acquired during experiments using optical pyrometry with sampling rates as fast as 500 KHz. Solidification and other high-temperature transformation pathways were deduced from the thermal data and microstructural analysis. Recalescence rise times were employed to determine semiquantitative primary solidification kinetics for the different phases. Primary beta solidification was observed at compositions well into the equilibrium alpha regime; this is presented as part of a near-equiatomic nucleation domain diagram that shows the primary solidification phase that results for each combination of nucleation temperature and composition. Solidification kinetics are faster for primary beta than they are for primary alpha. For undercoolings less than about 150 K, the primary solidification kinetics are about an order of magnitude slower for gamma than for alpha.

Anderson, C. D.↗
NASA NTRS1995

Thermal Stability of Hi-Nicalon SiC Fiber in Nitrogen and Silicon Environments

The room temperature tensile strength of uncoated and two types of pyrolytic boron nitride coated (PBN and Si-rich PBN) Hi-Nicalon SiC fibers was determined after 1 to 400 hr heat treatments to 1800 C under N2 pressures of 0.1, 2, and 4 MPa, and under 0.1 Mpa argon and vacuum environments. In addition, strength stability of both uncoated and coated fibers embedded in silicon powder and exposed to 0.1 MPa N2 for 24 hrs at temperatures to 1400 C was investigated. The uncoated and both types of BN coated fibers exposed to N2 for 1 hr showed noticeable strength degradation above 1400 C and 1600 C, respectively. The strength degradation appeared independent of nitrogen pressure, time of heat treatment, and surface coatings. TEM microstructural analysis suggests that flaws created due to SiC grain growth are responsible for the strength degradation. In contact with silicon powder, the uncoated and both types of PBN coated fibers degrade rapidly above 1350 C.

Bhatt, R. T.↗
NASA NTRS1996

Parabolic aircraft solidification experiments

A number of solidification experiments have been utilized throughout the Materials Processing in Space Program to provide an experimental environment which minimizes variables in solidification experiments. Two techniques of interest are directional solidification and isothermal casting. Because of the wide-spread use of these experimental techniques in space-based research, several MSAD experiments have been manifested for space flight. In addition to the microstructural analysis for interpretation of the experimental results from previous work with parabolic flights, it has become apparent that a better understanding of the phenomena occurring during solidification can be better understood if direct visualization of the solidification interface were possible. Our university has performed in several experimental studies such as this in recent years. The most recent was in visualizing the effect of convective flow phenomena on the KC-135 and prior to that were several successive contracts to perform directional solidification and isothermal casting experiments on the KC-135. Included in this work was the modification and utilization of the Convective Flow Analyzer (CFA), the Aircraft Isothermal Casting Furnace (ICF), and the Three-Zone Directional Solidification Furnace. These studies have contributed heavily to the mission of the Microgravity Science and Applications' Materials Science Program.

Workman, Gary L.↗
NASA NTRS1995

Failure Mechanisms During Isothermal Fatigue of SiC/Ti-24Al-11Nb Composites

Failure mechanisms during isothermal fatigue of unidirectional SiC/Ti-24Al-11Nb (at.%) composites have been determined by microstructural analysis of samples from tests interrupted prior to the end of life and from tests conducted to failure. Specimens from three regions of life were examined based on the maximum strain from a fatigue life diagram: Region 1 (high strain), Region 2 (mid-strain) and Region 3 (low strain). Crack lengths were also measured from interrupted samples and compared based on temperature (23-815 C), region of life and numbers of cycles. Region 1 was controlled by fiber-dominated failure. A transition zone was observed between Regions 1 and 2 due to competition between failure mechanisms. Failure in Region 2 was generally described as surface-initiated cracking with varying amounts of fiber bridging. However, the specific descriptions of crack propagation through the fibers and matrix varied with strain and temperature over this broad region. Region 3 exhibited endurance behaviour at 23 C with no cracking after lO(exp 6) cycles. However at 425 C, surface-initiated cracking was observed after 10(exp 6) cycles with fractured fibers in the crack wake. If endurance behaviour exists for conditions of isothermal fatigue in air at temperatures of greater than or equal to 425 C, it may only be found at very low strains and at greater than 10(exp 6) cycles.

Brindley, P. K.↗
NASA NTRS1997

Stressed Oxidation of C/SiC Composites

Constant load, stressed oxidation testing was performed on T-300 C/SiC composites with a SiC seal coat. Test conditions included temperatures ranging from 350 C to 1500 C at stresses of 69 MPa and 172 MPa (10 and 25 ksi). The coupon subjected to stressed oxidation at 550 C/69 MPa for 25 hours had a room temperature residual strength one-half that of the as-received coupons. The coupon tested at the higher stress and all coupons tested at higher temperatures failed in less than 25 hr. Microstructural analysis of the fracture surfaces, using SEM (scanning electron microscopy), revealed the formation of reduced cross-sectional fibers with pointed tips. Analysis of composite cross-sections show pathways for oxygen ingress. The discussion will focus on fiber/matrix interphase oxidation and debonding as well as the formation and implications of the fiber tip morphology.

Halbig, Michael C.↗
NASA NTRS1998

Effects of HF Treatments on Tensile Strength of Hi-Nicalon Fibers

Tensile strengths of as-received Hi-Nicalon fibers and those having a dual BN/SiC surface coating, deposited by chemical vapor deposition, have been measured at room temperature. These fibers were also treated with HF for 24 h followed by tensile strength measurements. Strengths of uncoated and BN/SiC coated Hi-Nicalon fibers extracted from celsian matrix composites, by dissolving away the matrix in HF for 24 h, were also determined. The average tensile strength of uncoated Hi-Nicalon was 3.19 +/- 0.73 GPa with a Weibull modulus of 5.41. The Hi-Nicalon/BN/SiC fibers showed an average strength of 3.04 q 0.53 GPa and Weibull modulus of 6.66. After HF treatments, the average strengths of the uncoated and BN/SiC coated Hi-Nicalon fibers were 2.69 +/- 0.67 GPa and 2.80 +/- 0.53 GPa and the Weibull moduli were 4.93 and 5.96, respectively. The BN/SiC coated fibers extracted from the celsian matrix composite exhibited a strength of 2.38 +/- 0.40 GPa and a Weibull modulus of 7.15. The strength of the uncoated Hi-Nicalon fibers in the composite was so severely degraded that they disintegrated into small fragments during extraction with HF. The uncoated fibers probably undergo mechanical surface damage during hot pressing of the composites. Also, the BN layer on the coated fibers acts as a compliant layer which protects the fibers from mechanical damage during composite processing. The elemental composition and thickness of the fiber coatings were deten-nined using scanning Auger analysis. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy and transmission electron microscopy. Strengths of fibers calculated using average and measured fiber diameters were in good agreement. Thus, the strength of fibers can be evaluated using an average fiber diameter instead of the measured diameter of each filament.

Bansal, Narottam P.↗
NASA NTRS1999

Oxygen Diffusion and Reaction Kinetics in Continuous Fiber Ceramic Matrix Composites

Previous stressed oxidation tests of C/SiC composites at elevated temperatures (350 C to 1500 C) and sustained stresses (69 MPa and 172 MPa) have led to the development of a finite difference cracked matrix model. The times to failure in the samples suggest oxidation occurred in two kinetic regimes defined by the rate controlling mechanisms (i.e. diffusion controlled and reaction controlled kinetics). Microstructural analysis revealed preferential oxidation along as-fabricated, matrix microcracks and also suggested two regimes of oxidation kinetics dependent on the oxidation temperature. Based on experimental results, observation, and theory, a finite difference model was developed. The model simulates the diffusion of oxygen into a matrix crack bridged by carbon fibers. The model facilitates the study of the relative importance of temperature, the reaction rate constant, and the diffusion coefficient on the overall oxidation kinetics.

Halbig, Michael C.↗
NASA NTRS1999

Containerless, Low-Gravity Undercooling of Ti-Ce Alloys in the MSFC Drop Tube

Previous tests of the classical nucleation theory as applied to liquid-liquid gap miscibility systems found a discrepancy between experiment and theory in the ability to undercool one of the liquids before the L1-L2 separation occurs. To model the initial separation process in a two-phase liquid mixture, different theoretical approaches, such as free-energy gradient and density gradient theories, have been put forth. If there is a large enough interaction between the critical liquid and the crucible, both models predict a wetting temperature (T(sub w)) above which the minority liquid perfectly wets and layers the crucible interface, but only on one side of the immiscibility dome. Materials with compositions on the other side of the dome will have simple surface adsorption by the minority liquid before bulk separation occurs when the coexistence (i.e., binoidal) line in reached. If the interaction between the critical liquid and the crucible were to decrease, T(sub w) would increase, eventually approaching the critical consolute temperature (T(sub cc)). If this situation occurs, then there could be large regions of the miscibility gap where non-perfect wetting conditions prevail resulting in droplets of L1 liquid at the surface having a non-zero contact angle. The resulting bulk structure will then depend on what happens on the surface and the subsequent processing conditions. In the past several decades, many experiments in space have been performed on liquid metal binary immiscible systems for the purpose of determining the effects that different crucibles may have on the wetting and separation process of the liquids. Potard performed experiments that showed different crucible materials could cause the majority phase to preferentially wet the container and thus produce a dispersed microstructure of the minority phase. Several other studies have been performed on immiscibles in a semi-container environment using an emulsion technique. Only one previous study was performed using completely containerless processing of immiscible metals and the results of that investigation are similar to some of the emulsion studies. In all the studies, surface wetting was attributed as the cause for the similar microstructures or the asymmetry in the ability to undercool the liquid below the binoidal on one side of the immiscibility dome. By removing the container completely from the separation process, it was proposed that the loss of the crucible/liquid interaction would produce a large shift in T(sub w) and thus change the wetting characteristics at the surface. By investigating various compositions across the miscibility gap, a change in the type and amount of liquid wetting at the surface of a containerless droplet should change the surface nucleating behavior of the droplet - whether it be the liquid-liquid wetting or the liquid-to-solid transition. Undercooling of the liquid into the metastable region should produce significant differences in the separation process and the microstructure upon solidification. In this study, we attempt to measure these transitions by monitoring the temperature of the sample by optical pyrometry. Microstructural analysis will be made to correlate with the degree of undercooling and the separation mechanisms involved.

Robinson, M. B.↗
NASA NTRS2000

Intermediate Temperature Stress Rupture of Woven SiC Fiber, BN Interphase, SiC Matrix Composites in Air

Tensile stress-rupture experiments were performed on woven Hi-Nicalon reinforced SiC matrix composites with BN interphases in air. Modal acoustic emission (AE) was used to monitor the damage accumulation in the composites during the tests and microstructural analysis was performed to determine the amount of matrix cracking that occurred for each sample. Fiber fractograph), was also performed for individual fiber failures at the specimen fracture surface to determine the strengths at which fibers failed. The rupture strengths were significantly worse than what would have been expected front the inherent degradation of the fibers themselves when subjected to similar rupture conditions. At higher applied stresses the rate of rupture "?as larger than at lower applied stresses. It was observed that the change in rupture rate corresponded to the onset of through-thickness cracking in the composites themselves. The primary cause of the sen,ere degradation was the ease with which fibers would bond to one another at their closest separation distances, less than 100 nanometers, when exposed to the environment. The near fiber-to-fiber contact in the woven tows enabled premature fiber failure over large areas of matrix cracks due to the stress-concentrations created b), fibers bonded to one another after one or a few fibers fail. i.e. the loss of global load sharing. An@, improvement in fiber-to-fiber separation of this composite system should result in improved stress- rupture properties. A model was den,eloped in order to predict the rupture life-time for these composites based on the probabilistic nature of indin,idual fiber failure at temperature. the matrix cracking state during the rupture test, and the rate of oxidation into a matrix crack. Also incorporated into the model were estimates of the stress-concentration that would occur between the outer rim of fibers in a load-bearing bundle and the unbridged region of a matrix crack after Xia et al. For the lower stresses, this source of stress-concentration was the likely cause for initial fiber failure that would trigger catastrophic failure of the composite.

Morscher, Gregory N.↗
NASA NTRS1996

A microstructural approach to cytoskeletal mechanics based on tensegrity

Mechanical properties of living cells are commonly described in terms of the laws of continuum mechanics. The purpose of this report is to consider the implications of an alternative approach that emphasizes the discrete nature of stress bearing elements in the cell and is based on the known structural properties of the cytoskeleton. We have noted previously that tensegrity architecture seems to capture essential qualitative features of cytoskeletal shape distortion in adherent cells (Ingber, 1993a; Wang et al., 1993). Here we extend those qualitative notions into a formal microstructural analysis. On the basis of that analysis we attempt to identify unifying principles that might underlie the shape stability of the cytoskeleton. For simplicity, we focus on a tensegrity structure containing six rigid struts interconnected by 24 linearly elastic cables. Cables carry initial tension ("prestress") counterbalanced by compression of struts. Two cases of interconnectedness between cables and struts are considered: one where they are connected by pin-joints, and the other where the cables run through frictionless loops at the junctions. At the molecular level, the pinned structure may represent the case in which different cytoskeletal filaments are cross-linked whereas the looped structure represents the case where they are free to slip past one another. The system is then subjected to uniaxial stretching. Using the principal of virtual work, stretching force vs. extension and structural stiffness vs. stretching force relationships are calculated for different prestresses. The stiffness is found to increase with increasing prestress and, at a given prestress, to increase approximately linearly with increasing stretching force. This behavior is consistent with observations in living endothelial cells exposed to shear stresses (Wang & Ingber, 1994). At a given prestress, the pinned structure is found to be stiffer than the looped one, a result consistent with data on mechanical behavior of isolated, cross-linked and uncross-linked actin networks (Wachsstock et al., 1993). On the basis of our analysis we concluded that architecture and the prestress of the cytoskeleton might be key features that underlie a cell's ability to regulate its shape.

NASA Discipline Cell Biology↗
NASA NTRS2000

Formation of Leading-Edge Pinholes in the Space Shuttle Wings Investigated

The space shuttle wing leading edge and nose cap are composed of a carbon/carbon composite that is protected by silicon carbide. The coefficient of thermal expansion mismatch leads to cracks in the silicon carbide. The outer coating of the silicon carbide is a sodium-silicate-based glass that becomes fluid at the shuttles high reentry temperatures and fills these cracks. Small pinholes roughly 0.1 mm in diameter have been observed on these materials after 12 or more flights. These pinholes have been investigated by researchers at the NASA Johnson Space Center, Rockwell International, the Boeing Company, Lockheed Martin Corporation, and the NASA Glenn Research Center at Lewis Field to determine the possible sources and the extent of damage. A typical pinhole is illustrated in the photomicrographs. These pinholes are found primarily on the wing leading edges and not on the nose cap, which is covered when the orbiter is on the launch pad. The pinholes are generally associated with a bead of zincrich glass. Examination of the orbiter and launch structure indicates that weathering paint on the launch structure leads to deposits of zinc-containing paint flakes on the wing leading edge. These may become embedded in the crevices of the wing leading edge and form the observed zinc-rich glass. Laboratory experiments indicate that zinc oxide reacts vigorously with the glass coating on the silicon carbide. Thus, it is likely that this is the reaction that leads to pinhole formation (Christensen, S.V.: Reinforced Carbon/Carbon Pin Hole Formation Through Zinc Oxide Attack. Rockwell International Internal Letter, RDW 96 057, May 1996). Cross-sectional examination of pinholes suggests that they are enlarged thermal expansion mismatch cracks. This is illustrated in the photomicrographs. A careful microstructural analysis indicates that the pinhole walls consist of layers of zinc-containing glass. Thus, pinholes are likely formed by zinc oxide particles lodging in crevices and forming a corrosive zinc-rich glass that enlarges existing cracks. Having established the likely source of the pinholes, we next needed to model the damage. Our concern was that if a pinhole went through the silicon carbide to the carbon/carbon substrate, oxygen would have a clear path to oxidize the carbon at high temperatures. This possibility was examined with studies in a laboratory furnace. An ultrasonic drill was used to make artificial pinholes in a sample of protected carbon/carbon. After exposure, the specimens were weighed and cross-sectioned to quantify the extent of oxidation below the pinhole. The results at higher temperatures showed good agreement with a simple diffusion-control model. This model is based on the two-step oxidation of carbon to carbon monoxide and carbon dioxide. The fluxes are illustrated in the final figure. The model indicates a strong dependence on pinhole diameter. For smaller diameters and short times, the oxidation of carbon is very limited.

Jacobson, Nathan S.↗
NASA NTRS2004

Active Metal Brazing of Carbon-Carbon Composites to Titanium

The Ti-metal/C-C composite joints were formed by reactive brazing with three commercial brazes, namely, Cu-ABA, TiCuNi, and TiCuSil. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). The results of the microstructure analysis indicate solute redistribution across the joint which led to good wetting, spreading, and metallurgical bond formation via interdiffusion.

Singh, M.↗
NASA NTRS2004

Reactive Brazing of Carbon-Carbon Composites to Titanium

The Ti-metal/C-C composite joints were formed by reactive brazing with three commercial brazes, namely, Cu-ABA, TiCuNi, and TiCuSil. The joint microstructures were examined using optical microscopy, and scanning electron microscopy (SEM) coupled with energy dispersive spectrometry (EDS). The results of the microstructure analysis indicate solute redistribution across the joint and possible metallurgical bond formation via interdiffusion, which led to good wetting and spreading.

Shpargel, Tarah↗