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DOE OSTI2023

Determining Stress in Metallic Conducting Layers of Microelectronics Devices Using High Resolution Electron Backscatter Diffraction and Finite Element Analysis

Delayed failure due to stress voiding is a concern with some aging microelectronics, as these voids can grow large enough to cause an open circuit. Local measurements of stress in the metallic layers are crucial to understanding and predicting this failure, but such measurements are complicated by the fact that exposing the aluminum conducting lines will relieve most of their stress. In this study, we instead mechanically thin the device substrate and measure distortions on the thinned surface using high resolution electron backscatter diffraction (HREBSD). These measurements are then related to the stresses in the metallic layers through elastic simulations. This study found that in legacy components that had no obvious voids, the stresses were comparable to the theoretical stresses at the time of manufacture (≈300 MPa). Distortion fields in the substrate were also determined around known voids, which may be directly compared to stress voiding models. In conclusion, the technique presented here for stress determination, HREBSD coupled with finite element analysis to infer subsurface stresses, is a valuable tool for assessing failure in layered microelectronics devices.

HREBSD↗

NASA NTRS2013

Atomic Force Microscope Mediated Chromatography

The atomic force microscope (AFM) is used to inject a sample, provide shear-driven liquid flow over a functionalized substrate, and detect separated components. This is demonstrated using lipophilic dyes and normal phase chromatography. A significant reduction in both size and separation time scales is achieved with a 25-micron-length column scale, and one-second separation times. The approach has general applications to trace chemical and microfluidic analysis. The AFM is now a common tool for ultra-microscopy and nanotechnology. It has also been demonstrated to provide a number of microfluidic functions necessary for miniaturized chromatography. These include injection of sub-femtoliter samples, fluidic switching, and sheardriven pumping. The AFM probe tip can be used to selectively remove surface layers for subsequent microchemical analysis using infrared and tip-enhanced Raman spectroscopy. With its ability to image individual atoms, the AFM is a remarkably sensitive detector that can be used to detect separated components. These diverse functional components of microfluidic manipulation have been combined in this work to demonstrate AFM mediated chromatography. AFM mediated chromatography uses channel-less, shear-driven pumping. This is demonstrated with a thin, aluminum oxide substrate and a non-polar solvent system to separate a mixture of lipophilic dyes. In conventional chromatographic terms, this is analogous to thin-layer chromatography using normal phase alumina substrate with sheardriven pumping provided by the AFM tip-cantilever mechanism. The AFM detection of separated components is accomplished by exploiting the variation in the localized friction of the separated components. The AFM tip-cantilever provides the mechanism for producing shear-induced flows and rapid pumping. Shear-driven chromatography (SDC) is a relatively new concept that overcomes the speed and miniaturization limitations of conventional liquid chromatography. SDC is based on a sliding plate system, consisting of two flat surfaces, one of which has a recessed channel. A fluid flow is produced by axially sliding one plate past another, where the fluid has mechanical shear forces imposed at each point along the channel length. The shear-induced flow rates are very reproducible, and do not have pressure or voltage gradient limitations. SDC opens up a new range of enhanced separation kinetics by permitting the sample confinement with submicron dimensions. Small, highly confined liquid is advantageous for chromatographic separation because the separation rate is known to scale according to the square of the confined sample diameter. In addition, because shear-driven flows are not limited by fluid velocity, shear-driven liquid chromatography may provide up to 100,000 plate efficiency.

Anderson, Mark S.↗

NASA NTRS2005

Unraveling the Material Processing Conditions for Optimizing FSW Process

In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. This environmentally friendly, solid-state technique has been successfully used in the joining of materials that are difficult to fusion weld. To determine optimal processing parameters for producing a defect free weld a better understanding of the resulting metal deformation flow path and velocity is required. In this study the metal flow fields are marked by the use of thin (0.001? tungsten) wires embedded in the weld seam at various locations. X-ray radiographs record the position and segmentation of the wire and are used to elucidate the flow field. Microstructures observed in a FSW cross-section in an aluminum alloy are related to their respective strain-strain rate-temperature histories along their respective flow trajectories. Two kinds of trajectories, each subjecting the weld metal to a distinct thermomechanical process and imparting a distinct microstructure, can be differentiated within the weld structure.

Schneider, Judy↗

NASA NTRS2005

Quantifying the Material Processing Conditions for an Optimized FSW Process

In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edgs of the seam together. This environmentally friendly, solid-state technique has been successfully used in the joining of materials that are difficult to fusion weld. To determine optimal processing parameters for producing a defect free weld, a better understanding of the resulting metal deformation flow path and velocity is required. In this study the metal flow fields are marked by the use of thin (0.001 in. tungsten) wires embedded in the weld seam at various locations. X-ray radiographs record the position and segmentation of the wire and are used to elucidate the flow field. Microstructures observed in a FSW cross-section in an aluminum alloy are related to their respective strain-strain rate-temperature histones along their respective flow trajectories. Two kinds of trajectories, each subjecting the weld metal to a distinct thermomechanical process and imparting a distinct microstructure, can be differentiated within the weld structure.

Schneider, Judy↗

NASA NTRS2016

Elaborated Odor Test for Extended Exposure

Concerns were raised when incidental exposure to a proprietary bonding material revealed the material had an irritating odor. The NASA-STD-6001B document describes a supplemental test method option for programs to evaluate materials with odor concerns (Test 6, Odor Assessment). In addition to the supplemental standard odor assessment with less than 10 seconds of exposure, the NASA White Sands Test Facility (WSTF) Materials Flight Acceptance Testing section was requested to perform an odor test with an extended duration to evaluate effects of an extended exposure and to more closely simulate realistic exposure scenarios. With approval from the NASA Johnson Space Center Industrial Hygienist, WSTF developed a 15-minute odor test method. WSTF performed this extended-duration odor test to evaluate the odor and physical effects of the bonding material configured between two aluminum plates, after the safety of the gas was verified via toxicity analysis per NASA-STD-6001B Test 7, Determination of Offgassed Products. During extended-duration testing, odor panel members were arranged near the test material in a small room with the air handlers and doors closed to minimize dilution. The odor panel members wafted gas toward themselves and recorded their individual assessments of odor and physical effects at various intervals during the 15-minute exposure and posttest. A posttest interview was conducted to obtain further information. Testing was effective in providing data for comparison and selection of an optimal offgassing and odor containment configuration. The developed test method for extended exposure is proposed as a useful tool for further evaluating materials with identified odors of concern if continued use of the material is anticipated.

Buchanan, Vanessa D.↗

NASA NTRS1998

Low-Temperature Friction-Stir Welding of 2024 Aluminum

Solid state friction-stir welding (FSW) has been demonstrated to involve dynamic recrystallization producing ultra-fine, equiaxed grain structures to facilitate superplastic deformation as the welding or joining mechanism. However, the average residual, equiaxed, grain size in the weld zone has ranged from roughly 0.5 micron to slightly more than 10 micron, and the larger weld zone grain sizes have been characterized as residual or static grain growth as a consequence of the temperatures in the weld zone (where center-line temperatures in the FSW of 6061 Al have been shown to be as high as 480C or -0.8 T(sub M) where T(sub M) is the absolute melting temperature)). In addition, the average residual weld zone grain size has been observed to increase near the top of the weld, and to decrease with distance on either side of the weld-zone centerline, an d this corresponds roughly to temperature variations within the weld zone. The residual grain size also generally decreases with decreasing FSW tool rotation speed. These observations are consistent with the general rules for recrystallization where the recrystallized grain size decreases with increasing strain (or deformation) at constant strain rate, or with increasing strain-rate, or with increasing strain rate at constant strain; especially at lower ambient temperatures, (or annealing temperatures). Since the recrystallization temperature also decreases with increasing strain rate, the FSW process is somewhat complicated because the ambient temperature, the frictional heating fraction, and the adiabatic heating fraction )proportional to the product of strain and strain-rate) will all influence both the recrystallization and growth within the FSW zone. Significantly reducing the ambient temperature of the base metal or work pieces to be welded would be expected to reduce the residual weld-zone grain size. The practical consequences of this temperature reduction would be the achievement of low temperature welding. This study compares the residual grain sizes and microstructures in 2024 Al friction-stir welded at room temperature (about 30C and low temperature (-30C).

Benavides, S.↗

NASA NTRS2000

Development and Application of Tools to Characterize the Oxidative Degradation of AP/HTPB/Al Propellants in a Propellant Reliability Study

The oxidative thermal aging of a crosslinked hydroxyl-terminated polybutadiene (HTPB)/isophorone diisocyanate (IPDI) polyurethane rubber was studied at temperatures between 25 C and 125 C. Changes in tensile elongation, mechanical hardening, polymer network properties, density, O2 permeation, and molecular chain dynamics were investigated as a function of age. The techniques used include solvent swelling, detailed modulus profiling, and NMR relaxation measurements. The Arrhenius methodology, which normally assumes a linear extrapolation of high temperature aging data, is critically evaluated by using extensive data superposition and highly sensitive oxygen consumption measurements. Significant curvature in the Arrhenius diagram of these oxidation rates is observed to be similar to previous results found for other rubber materials that have been evaluated by this technique. Preliminary gel/network properties suggest that crosslinking is the dominant process at higher temperatures. The effect on the oxidation rate of the binder when other constituents found in propellants are present, such as ammonium perchlorate, plasticizer and aluminum powder, is presented.

Celina, Mathew↗

DOE OSTI2024

Enabling in-situ LIBS measurements of liquids and slurries

The aim of this work was to explore the use of, and further develop, a in-situ and near-real time LIBS (Laser Induced Breakdown Spectroscopy) instrument to measure liquids relevant to the Hanford site. Specifically, we investigated the feasibility of using LIBS to measure the cation composition of HLW (High Level Waste) streams. In addition, we focused on enabling continuous interrogation of those liquids using the LIBS system. For the first part, we investigated simple (sodium nitrate) solutions as well as various Hanford tank waste surrogate slurries. We showed that relevant cations (such as sodium, aluminum, magnesium, potassium) can be measured via LIBS under good conditions but the results – both quantitative and qualitative (aka reproducibility) – strongly depend on the kind and concentration of the material used. The dependence of signal intensity on concentration was also confirmed by other measurements conducted (sodium chloride and sodium nitrate in water). For the second part, we investigated the influence of varying depth and concentration of a liquid sample. We observed that for the concentrations and fill depths investigated, the liquid fill depth did not impact the emission intensity of the analyte, while concentration is confirmed to have significant effects. The results of the sample depth experiments influenced testing of waste surrogates. In addition, we focused on further developing and adapting data fitting tools in order to efficiently, accurately, and reproducibly identify the elements and materials present in a LIBS spectrum.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2015

Composite Cryotank Technologies and Development 2.4 and 5.5M out of Autoclave Tank Test Results

The Composite Cryotank Technologies and Demonstration (CCTD) project substantially matured composite, cryogenic propellant tank technology. The project involved the design, analysis, fabrication, and testing of large-scale (2.4-m-diameter precursor and 5.5-m-diameter) composite cryotanks. Design features included a one-piece wall design that minimized tank weight, a Y-joint that incorporated an engineered material to alleviate stress concentration under combined loading, and a fluted core cylindrical section that inherently allows for venting and purging. The tanks used out-of-autoclave (OoA) cured graphite/epoxy material and processes to enable large (up to 10-m-diameter) cryotank fabrication, and thin-ply prepreg to minimize hydrogen permeation through tank walls. Both tanks were fabricated at Boeing using automated fiber placement on breakdown tooling. A fluted core skirt that efficiently carried axial loads and enabled hydrogen purging was included on the 5.5-m-diameter tank. Ultrasonic inspection was performed, and a structural health monitoring system was installed to identify any impact damage during ground processing. The precursor and 5.5-m-diameter tanks were tested in custom test fixtures at the National Aeronautics and Space Administration Marshall Space Flight Center. The testing, which consisted of a sequence of pressure and thermal cycles using liquid hydrogen, was successfully concluded and obtained valuable structural, thermal, and permeation performance data. This technology can be applied to a variety of aircraft and spacecraft applications that would benefit from 30 to 40% weight savings and substantial cost savings compared to aluminum lithium tanks.

Jackson, Justin R.↗

DOE OSTI2024

Mu2e experiment: Simulation of the Production Target

The Mu2e experiment will search for coherent, neutrinoless conversion of muons to elections in an aluminum stopping target. A simulation program is used to experiment and design the production target of the Mu2e experiment. The module uses programing languages and libraries to work. The program called the Offline uses C++ as the programing language in the module. To construct the simulation, the Geant4 library constructs shapes and uses them in the simulation program, ROOT. The offline program simplifies the creation of the tube by organizing them into parameter objects and nesting them with other variables required to construct the tube-like center point, material, or if it is allowed to conflict with other solids. The parameter varies for every solid tube. The geometry file uploads the parameters by declaring and organizing the parameters in C++ using the configuration tools. The author describes the development and the future of this project.

43 PARTICLE ACCELERATORS↗

NASA NTRS1995

The Effect of Propellant Variables on Slag in Subscale Spin Motors: Design and Qualification of a Slag Discrimination Motor - Part 1

The formation, collection, and expulsion of aluminum oxide slag is known to affect the performance of many solid rocket motor systems. Slag expulsion, in particular, is believed to be capable of causing pressure and thrust perturbations. Propellant combustion studies, performed and documented by many investigators, have shown that variations in propellant raw materials and processing affect the nature of alumina droplets at the burning propellant surface, and hence, may affect the quantity of slag retained in the motor chamber, available for expulsion. Thiokol has completed an experimental and analytical evaluation to determine the effects of several material and process variables on Space SHuttle propellant and its propensity to 'slag'. This paper describes the test article, a small scale spin motor with special nozzle, designed and qualified as a slag discriminating tool for use in the evaluation.

Perkins, F. M.↗

NASA NTRS2010

Development of Weld Inspection of the Ares I Crew Launch Vehicle Upper Stage

NASA is designing a new crewed launch vehicle called Ares I to replace the Space Shuttle after its scheduled retirement in 2010. This new launch vehicle will build on the Shuttle technology in many ways including using a first stage based upon the Space Shuttle Solid Rocket Booster, advanced aluminum alloys for the second stage tanks, and friction stir welding to assemble the second stage. Friction stir welding uses a spinning pin that is inserted in the joint between two panels that are to be welded. The pin mechanically mixes the metal together below the melting temperature to form the weld. Friction stir welding allows high strength joints in metals that would otherwise lose much of their strength as they are melted during the fusion welding process. One significant change from the Space Shuttle that impacts NDE is the implementation of self-reacting friction stir welding for non-linear welds on the primary metallic structure. The self-reacting technique differs from the conventional technique because the load of the pin tool pressing down on the metal being joined is reacted by a nut on the end of the tool rather than an anvil behind the part. No spacecraft has ever flown with a self-reacting friction stir weld, so this is a major advancement in the manufacturing process, bringing with it a whole new set of challenges for NDE to overcome. The metal microstructure and possible defects are different from other weld processes. Friction plug welds will be used to close out the hole remaining in the radial welds when friction stir welded. This plug welding also has unique challenges in inspection. The current state of development of these inspections will be presented, along with other information pertinent to NDE of the Ares I.

Russell, Sam↗

DOE OSTI2024

Mu2e experiment: Simulation of the Production Target

Szewczyk, Albert↗

NASA NTRS2017

Ti Isotopes: Echoes of Grain-Scale Heterogenaity in the Protoplanetary Disk

Calcium-aluminum-rich inclusions (CAIs) are the oldest surviving solids to have formed in the Solar System. Their chemical and isotopic compositions provide a record of the conditions present in the protoplanetary disk where they formed and can aid our understanding of how solids formed in the solar nebula, an important step in the eventual process of planet building. The isotopic compositions of CAIs are primarily controlled by volatility. Evaporation/sublimation are well understood through both theory and experimental work to produce an enrichment in the heavy isotopes of an element, but less is understood about the effects of condensation. Mass-dependent fractionation can potentially provide a record of nebular condensation. Ti is not likely to experience evaporation due to its refractory nature, making it a useful tool for assessing the effects of condensation. We have undertaken a study of the stable isotope fractionation of Ti isotopes as a tracer of processes that predate the last evaporation events affecting CAIs. We compare the 49Ti/47Ti stable isotope ratio with excess 50Ti common in CAIs. We have collected Ti, Mg, Si, and Ca isotope data for a suite of CAIs in order to search for heterogeneity in each of these isotope systems, and for potential correlations among them. We compare our results to expectations for condensation.

Jordan, M. K.↗

NASA NTRS1989

Making on-orbit structural repairs to Space Station

One of the key factors dictating the safety and durability of the proposed U.S. Space Station is the ability to repair structural damage while remaining in orbit. Consequently, studies are conducted to identify the engineering problems associated with accomplishing structural repairs on orbit, due to zero gravity environment and exposure to extreme temperature variations. There are predominant forms of structural failure, depending on the metallic or composite material involved. Aluminum is the primary metallic material used in space vehicle applications. Welding processes on aluminum alloy structures were tested, resulting in final selection of electron beam welding as the primary technique for metallic material repair in Space. Several composite structure repair processes were bench-tested to define their applicability to on-orbit EVA requirements: induction heating prevailed. One of the unique problems identified as inherent in the on-orbit repair process is that of debris containment. The Maintenance Work Station concept provides means to prevent module contamination from repair debris and ensure the creation of a facility for crew members to work easily in a microgravity environment. Different technologies were also examined for application to EVA repair activities, and the concept selected was a spring-loaded, collapsible, box-like Debris Containement and Collection Device with incorporated fold-down tool boards and handholes in the front panel.

Haber, Harry S.↗

NASA NTRS1974

Effects of porosity on weld-joint tensile strength of aluminum alloys

Tensile properties in defect-free weldments of aluminum alloys 2014-T6 and 2219-T87 (sheet and plate) are shown to be related to the level or concentration of induced simulated porosity. The scatter diagram shows that the ultimate tensile strength of the weldments displays the most pronounced linear relationship with the level of porosity. The relationships between yield strength or elongation and porosity are either trivial or inconsequential in the lower and intermediate levels of porosity content. In highly concentrated levels of porosity, both yield strength and elongation values decrease markedly. Correlation coefficients were obtained by simple straight line regression analysis between the variables of ultimate tensile strength and pore level. The coefficients were greater, indicating a better correlation, using a pore area accumulation concept or pore volume accumulation than the accumulation of the pore diameters. These relationships provide a useful tool for assessing the existing aerospace radiographic acceptance standards with respect to permissible porosity. In addition, these relationships, in combination with known design load requirements, will serve as an engineering guideline in determining when a weld repair is necessary based on accumulative pore level as detected by radiographic techniques.

Lovoy, C. V.↗

NASA NTRS2009

Using FLUKA to Calculate Spacecraft: Single Event Environments: A Practical Approach

The FLUKA nuclear transport and reaction code can be developed into a practical tool for calculation of spacecraft and planetary surface asset SEE and TID environments. Nuclear reactions and secondary particle shower effects can be estimated with acceptable accuracy both in-flight and in test. More detailed electronic device and/or spacecraft geometries than are reported here are possible using standard FLUKA geometry utilities. Spacecraft structure and shielding mass. Effects of high Z elements in microelectronic structure as reported previously. Median shielding mass in a generic slab or concentric sphere target geometry are at least approximately applicable to more complex spacecraft shapes. Need the spacecraft shielding mass distribution function applicable to the microelectronic system of interest. SEE environment effects can be calculated for a wide range of spacecraft and microelectronic materials with complete nuclear physics. Evaluate benefits of low Z shielding mass can be evaluated relative to aluminum. Evaluate effects of high Z elements as constituents of microelectronic devices. The principal limitation on the accuracy of the FLUKA based method reported here are found in the limited accuracy and incomplete character of affordable heavy ion test data. To support accurate rate estimates with any calculation method, the aspect ratio of the sensitive volume(s) and the dependence must be better characterized.

Koontz, Steve↗

NASA NTRS2011

Vehicle Shield Optimization and Risk Assessment for Future Human Space Missions

As the focus of future human space missions shifts to destinations beyond low Earth orbit such as Near Earth Objects (NEO), the moon, or Mars, risks associated with extended stay in hostile radiation environment need to be well understood and assessed. Since future spacecrafts designs and shapes are evolving continuous assessments of shielding and radiation risks are needed. In this study, we use a predictive software capability that calculates risks to humans inside a spacecraft prototype that builds on previous designs. The software uses CAD software Pro/Engineer and Fishbowl tool kit to quantify radiation shielding provided by the spacecraft geometry by calculating the areal density seen at a certain point, dose point, inside the spacecraft. Shielding results are used by NASA-developed software, BRYNTRN, to quantify organ doses received in a human body located in the vehicle in case of solar particle event (SPE) during such prolonged space missions. Organ doses are used to quantify risks on astronauts health and life using NASA Space Cancer Model. The software can also locate shielding weak points-hotspots-on the spacecraft s outer surface. This capability is used to reinforce weak areas in the design. Results of shielding optimization and risk calculation on an exploration vehicle design for missions of 6 months and 30 months are provided in this study. Vehicle capsule is made of aluminum shell that includes main cabin and airlock. The capsule contains 5 sets of racks that surround working and living areas. Water shelter is provided in the main cabin of the vehicle to enhance shielding in case of SPE.

Nounu, Hatem N.↗