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NASA NTRS2011

Reliability of Ceramic Column Grid Array Interconnect Packages Under Extreme Temperatures

A paper describes advanced ceramic column grid array (CCGA) packaging interconnects technology test objects that were subjected to extreme temperature thermal cycles. CCGA interconnect electronic package printed wiring boards (PWBs) of polyimide were assembled, inspected nondestructively, and, subsequently, subjected to ex - treme-temperature thermal cycling to assess reliability for future deep-space, short- and long-term, extreme-temperature missions. The test hardware consisted of two CCGA717 packages with each package divided into four daisy-chained sections, for a total of eight daisy chains to be monitored. The package is 33 33 mm with a 27 27 array of 80%/20% Pb/Sn columns on a 1.27-mm pitch. The change in resistance of the daisy-chained CCGA interconnects was measured as a function of the increasing number of thermal cycles. Several catastrophic failures were observed after 137 extreme-temperature thermal cycles, as per electrical resistance measurements, and then the tests were continued through 1,058 thermal cycles to corroborate and understand the test results. X-ray and optical inspection have been made after thermal cycling. Optical inspections were also conducted on the CCGA vs. thermal cycles. The optical inspections were conclusive; the x-ray images were not. Process qualification and assembly is required to optimize the CCGA assembly, which is very clear from the x-rays. Six daisy chains were open out of seven daisy chains, as per experimental test data reported. The daisy chains are open during the cold cycle, and then recover during the hot cycle, though some of them also opened during the hot thermal cycle..

Ramesham, Rajeshuni↗

NASA NTRS2007

Novel Nanotube Manufacturing Streamlines Production

Nanotubes have novel qualities that make them uniquely qualified for a plethora of uses, including applications in electronics, optics, and other scientific and industrial fields. The NASA process for creating these nanostructures involves using helium arc welding to vaporize an amorphous carbon rod and then form nanotubes by depositing the vapor onto a water-cooled carbon cathode, which then yields bundles, or ropes, of single-walled nanotubes at a rate of 2 grams per hour using a single setup. This eliminates costs associated with the use of metal catalysts, including the cost of product purification, resulting in a relatively inexpensive, high-quality, very pure end product. While managing to be less expensive, safer, and simpler, the process also increases the quality of the nanotubes. Goddard's Innovative Partnerships Program (IPP) Office promoted the technology, and in 2005, Boise-based Idaho Space Materials Inc. (ISM) was formed and applied for a nonexclusive license for the single-walled carbon nanotube (SWCNT) manufacturing technology. ISM commercialized its products, and the inexpensive, robust nanotubes are now in the hands of the scientists who will create the next generation of composite polymers, metals, and ceramics that will impact the way we live. In fact, researchers are examining ways for these newfound materials to be used in the manufacture of transistors and fuel cells, large screen televisions, ultra-sensitive sensors, high-resolution atomic force microscopy probes, supercapacitors, transparent conducting films, drug carriers, catalysts, and advanced composite materials, to name just a few of the myriad technologies to benefit.

Source record↗

DOE OSTI2021

Reliability Analysis of Large-Area, Low Pressure-Assisted Silver Sintering for Medium-Voltage Power Modules

Multi-layer insulating ceramic substrates can enable medium-voltage (MV) power modules with reduced peak electric field. This benefit is particularly important for MV silicon carbide (SiC) MOSFETs due to their higher operating voltages. Large-area, low-pressure assisted silver sintering is a potential solution for bonding substrates to create a multi-layer structure. The voiding content and defect density of the bond used to create the multi-layer substrate stack-up is critical to the reliability of the power module and the thermal performance, as this bond is in the primary path for heat dissipation in the power module structure. Here, samples of two-layer direct bonded aluminum (DBA) stacks have been fabricated and subjected to thermal cycling to analyze their reliability. Passive thermal cycling from -40 degrees C to 200 degrees C was performed. Cross-sections were cut at pre-determined intervals and imaged with Scanning Electron Microscopy (SEM). After 1000 thermal cycles, adhesive failures are observed between the sintered silver and the DBA surface. Cross-sections were cut and imaged via optical microscope and SEM. Thermal analyzer measurements are recorded on a 10-kV SiC power module utilizing the sintered DBA substrate stacks.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2021

Thermodynamically Stable, Plasmonic Transition Metal Oxide Nanoparticle Solar Selective Absorbers towards 95% Optical-to-Thermal Conversion Efficiency at 750 °C

Generation 3 (Gen) concentrating solar power (CSP) systems requires a high operation temperature ≥750°C to increase the power-cycle efficiency towards ≥50%. However, such a high operation temperature poses a notable challenge to high temperature materials. On the receiver side, a critical challenge is the lack of solar selective absorbers that demonstrate both high optical-to-thermal energy conversion efficiency η therm approaching 95% and long-term thermal stability at >750°C in air. Existing solar absorbers either have limited η therm ≤89% or deteriorate significantly within 500 h at 750°C; some of these also require costly vacuum deposition for stringent thickness control. Therefore, it is highly desirable to simultaneously achieve η therm ~95% AND high thermal stability at 750°C for future generations of CSP receivers. This project has investigated and developed low-cost, highly scalable spray-coated transition metal oxide nanoparticle (NP) pigmented solar selective coatings on various types of Inconel alloy tube sections that are thermodynamically stable at 750-800°C in air, maintaining η therm >94.3%(93.2%) under a solar concentration ratio of C=1000 after 60 simulated day-night cycles at 750ºC (800ºC) (1 cycle=12 h at 750 or 800°C and 12h ramping down to 25°C). We have also coated up to 48 inches long receiver tubes for preliminary solar testing under Norwich Technology’s parabolic trough systems, demonstrating notably improved performance in solar heating compared to benchmark Pyromark 2500 coatings. Two key innovations have been developed in this project: (1) We achieved an unprecedented high thermal efficiency >94% by optimizing the d-band optical absorption spectra of transition metal ions, engineering their valences and stoichiometry; (2) We were able to maintain or even slightly increase the efficiency when operating at 750°C in air by engineering the interdiffusion of transition metal ions between the coating and the Inconel substrate to our advantage. Featuring high-temperature solar spectral selectivity and thermodynamic stability in air, as well as low-cost, highly scalable solution-chemical synthesis and spray coating techniques, this innovation in solar selective absorber technology alone accounts for nearly 40% of the targeted reduction in the levelized cost of electricity (LCOE) from the receiver, thermal energy storage, and operation & maintenance combined by 2030, as proposed by the U.S. Department of Energy. For a 110 MWe CSP power plant, this LCOE reduction from the solar selective coating alone transfers to ~$\$ $1.9 M increase in annual profit based on a sales price of 10¢/kWh (or an annual sale of $50 M/year). The high solar absorptance (~98%) NP pigment materials developed in this project are equally applicable to volumetric receivers either as a coating or as bigger ceramic microspheres after sintering, potentially benefiting Gen3 falling particle CSP technologies. All these contributions facilitate the larger scale deployment of CSP systems with energy storage capability to address the intermittency issue of solar energy towards dispatchable solar electricity, bridging the temporal gap between peak solar electricity production and peak electricity consumption. The collaboration with Norwich Technologies and Brayton Energy in this project will also facilitate the future commercialization of this new solar selective coating technology developed in this SIPS project.

14 SOLAR ENERGY↗

NASA NTRS1997

Design of An Improved Miniature Ion Neutral Mass Spectrometer for NASA Applications

The ion optics of NASA's Ion Neutral Mass Spectrometer (INMS) sensor was simulated with three dimensional models of the open source, the quadrupole deflector, the exit lens system and the quadrupole mass analyzer to design more compact models with lower weight. Comparison of calculated transmission with experimental results shows good agreement. Transmission analyses with varying geometrical parameters and voltages throw light on possible ways of reducing the size of the sensor. Trajectories of ions of mass 1-99 amu were simulated to analyze and optimize transmission. Analysis of open source transmission with varying angle of attack shows that the angular acceptance can be considerably increased by programming the voltages on the ion trap/ collimator. Analysis of transmission sensitivity to voltages and misalignments of the quadrupole deflector rods indicate that increased transmission is possible with a geometrically asymmetrical deflector and a deflector can be designed with much lower sensitivities of transmission. Bringing the disks closer together can decrease the size of the quadrupole deflector and also increase transmission. The exit lens system can be redesigned to be smaller by eliminating at least one electrode entirely without loss of transmission. Ceramic materials were investigated to find suitable candidates for use in the construction of lighter weight mass spectrometer. A high-sensitivity, high-resolution portable gas chromatograph mass spectrometer with a mass range of 2-700 amu has been built and will be commercialized in Phase 3.

Swaminathan, Viji K.↗

DOE OSTI2024

Development and Application of In Situ Nanocharacterization to Photocatalytic Materials for Solar Fuel Generation

Photocatalytic materials offer an attractive approach for converting solar energy into chemical energy but the performance of the current generation of materials is insufficient to make a technology viable. To address this deficiency, it is necessary to develop a fundamental atomic level understanding of the functioning of such materials so that strategies can be developed to improve performance. This project was undertaken to explore the fundamental structure and properties of photocatalytic materials using atomic resolution imaging and spectroscopy techniques available on advanced transmission electron microscopy. Specifically, there is a need to develop an understanding of how atomic structures/defects and nanoparticle configurations regulate electronic, optical, and catalytic properties to facilitate the design of next generation photocatalysts for solar fuel production. The work focused on fundamental materials information that can be gained from advanced transmission electron microscopy study on novel and existing photocatalytic systems with an emphasis on the hydrogen evolution reaction (HER). Throughout the project, new instrumentation and microscopy characterization tools were developed. Two focus areas were: developing in situ TEM methods and advanced electron energy-loss spectroscopic for nanoscale analysis of catalysts. The work spanned a period of 12 years and for convenience, the report is divided into four phases, approximately corresponding to the four funding periods of the program. Most of the significant results are reported in archival journal publications.

36 MATERIALS SCIENCE↗

NASA NTRS1996

PICA Forebody Heatshield Qualification for the Stardust Discovery Class Mission

This paper presents the qualification of the light weight Phenolic Impregnated Carbon Ablators (PICA) as the forebody heatshield for the Stardust Discovery Class Mission. The Stardust spacecraft will be launched in early 1999 and fly by Comet Wild-2 to collect cometary and interstellar dust and return them back to earth in the Sample Return Capsule (SRC). This earth re-entry will be the fastest to date, at 12.6 km/s, and therefore requires a heatshield that can withstand very high heating rates and stagnation pressures, as well as provide the necessary insulation to the vehicle structure. The PICA material was developed as part of the Lightweight Ceramic Ablators program at NASA Ames Research Center, and was baselined as the forebody heatshield because of its low density and superior ablation and thermal performance at severe aerothermodynamic conditions. Under a Small Business Innovative Research (SBIR) program with NASA Ames, Fiber Materials, Inc. developed a process to manufacture a single-piece PICA heatshield for the forebody of the SRC, along with witness material for the fabrication of the test models. The test models were fabricated and instrumented by the staff of Lockheed Martin Astronautics in Denver, Colorado. Full body preliminary aerothermal CFD calculations were performed at NASA Ames to determine the heating and stagnation pressure conditions. The Heat shield sizing was also performed at NASA Ames by using a new material response code that accounts for the highly porous characteristics of the PICA material. The ablation and thermal performance of PICA was qualified in the NASA Ames Interaction Heating Arc Jet Facility. A total of 24 models and four test conditions were used to qualify PICA at the predicted peak heat flux, heat load, shear, and stagnation pressure conditions. Surface and in-depth temperatures were measured using optical pyrometers and thermocouples. Surface recession was measured by using a template and a height gage. Several models were tested to evaluate repair procedures, and two models were cold soaked in liquid nitrogen, prior th testing, to investigate the effect of the cold space environment on the performance of the material. In addition, material cored from a demonstration single-piece heatshield was tested to verify that the PICA process can be successfully completed on a large, complex heatshield shape.

Tran, Huy K.↗

DOE OSTI2021

Performance of Embedded Sensors in 3D Printed SiC

This report summarizes recent advances in embedding sensors in 3D printed silicon carbide (SiC) ceramic components under the Transformational Challenge Reactor (TCR) program. The additive manufacturing technologies developed under this program will enable fabrication of complex structures with embedded fuels and sensors. The sensors will be capable of characterizing fuel performance using spatially distributed measurements at the most strategic locations that would be otherwise inaccessible using conventional manufacturing techniques. While previous programmatic updates describe initial concepts for embedding sensors, materials selection, and initial characterization of the embedded sensors, the technology requires further demonstration, and quality-significant procedures must be established before the embedding technology is ready for adoption by industry. To this end, this report describes the most effective techniques that have been used to embed functional sensors in 3D printed components using a combination of binder-jet additive manufacturing and chemical vapor infiltration (CVI). A detailed procedure describes each step in the process and is available upon request. Molybdenum (Mo)-sheathed thermocouples have been successfully embedded in complex SiC components, and temperatures were monitored in situ during the embedding process. Post-embedding measurements showed no significant hysteresis, and characterization of the interface revealed qualitatively strong bonding around the entire perimeter of the sensor sheath. Distributed fiber-optic temperature sensors were able to briefly measure temperature profiles during CVI, but they ultimately failed prior to completion of the CVI run. The failure appears to be related to the fiber coating at temperatures close to 1,000°C. Future work will focus on irradiation testing of embedded thermocouples and other sheathed electrical sensors, as well as the identification of fiber-optic sensor coatings that can survive CVI.

42 ENGINEERING↗

NASA NTRS1997

First Single-Crystal Mullite Fibers

Ceramic-matrix composites strengthened by suitable fiber additions are being developed for high-temperature use, particularly for aerospace applications. New oxide-based fibers, such as mullite, are particularly desirable because of their resistance to high-temperature oxidative environments. Mullite is a candidate material in both fiber and matrix form. The primary objective of this work was to determine the growth characteristics of single-crystal mullite fibers produced by the laser-heated floating zone method. Directionally solidified fibers with nominal mullite compositions of 3Al2O3 2SiO2 were grown by the laser-heated floating zone method at the NASA Lewis Research Center. SEM analysis revealed that the single-crystal fibers grown in this study were strongly faceted and that the facets act as critical flaws, limiting fiber strength. The average fiber tensile strength is 1.15 GPa at room temperature. The mullite fibers exhibit superior strength retention (80 percent of their room temperature tensile strength at 1450 C). Examined by transmission electron microscopy, these mullite single crystals are free of dislocations, low-angle boundaries, and voids. In addition, they show a high degree of oxygen vacancy ordering. High-resolution digital images from an optical microscope furnish evidence of the formation of a liquid-liquid miscibility gap during crystal growth. These images represent the first experimental evidence of liquid immiscibility for these compositions and temperatures. Continuing investigation with controlled seeding of mullite single crystals is planned.

Source record↗

DOE OSTI2020

Coupling between interfacial charge and mechanical deformation at high temperatures in ceramics. Final report

Basic research, under this project, has led to new fundamental discoveries in the effect of electric field (and temperature) on diffusion kinetics, electroluminescence and electronic conductivity in ceramic materials. For example, yttria stabilized zirconia sinters in just seconds well below 1000°C, while, at the same time, exhibiting a highly non-linear rise in conductivity, and intense electroluminescence. The phenomenon has been shown to occur in nearly all ceramics whether they are ionic or electronic conductors, or insulators. The rise in conductivity leads to Joule heating but in-situ measurements with a platinum standard at APS and Brookhaven (NSLS-II) have shown that the temperatures are much below what would have been needed to sinter in a few seconds. We have explored the hypothesis that huge concentrations of Frenkel pairs of vacancies and interstitials are produced. While these point defects accelerate sintering (by the interstitials being transported to the pores and the vacancies to the grain boundaries), they may also produce electron-hole pairs which can impart high electrical conductivity or recombine to emit photons. Many measurements, including in-situ measurements of lattice expansion are consistent with this hypothesis. However, the energy barrier for generating Frenkels in zirconia for example is much larger than can be expected at temperature and electrical fields in these experiments. Most recent work suggests that short wavelength phonons play a critical role in the genesis of the “flash” phenomenon. For example, the Debye temperature has been shown to be the lower bound for initiating flash. Molecular dynamics simulations have shown that large concentrations of Frenkel pairs can form under the proliferation of “optical” phonons at the edge of the Brillouin zone, that is with a wavelength at or below the lattice parameter. This project has led to the development of new experimental techniques as well as a software hardware interface for process and control and data analysis in real time, with a time scale of less than one second. This approach spells a new paradigm in materials science research. It potential impact on high rate manufacturing is self evident.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Utilization of Novel (KNbO 3 ) 1− x (Ba 2 FeNbO 6 ) x ( x = 0.1, 0.2, 0.3) Solid Solutions for Efficient Photo‐Assisted Fenton Degradation of Methylene Blue Dye

Novel (KNbO 3 ) 1− x (Ba 2 FeNbO 6 ) x ( x = 0.1, 0.2, 0.3) solid solutions corresponding to K 0.82 Ba 0.18 Fe 0.09 Nb 0.91 O 3 , K 0.64 Ba 0.36 Fe 0.18 Nb 0.82 O 3 , and K 0.46 Ba 0.54 Fe 0.27 Nb 0.73 O 3 compounds have been synthesized via molten salt method. X‐ray diffraction confirms the formation of solid solutions, while transmission electron microscopy combined with energy‐dispersive spectroscopy results demonstrates a homogeneous distribution of elements. The obtained solid solutions crystallized in a cubic crystal structure, whereas the parent KNbO 3 possesses an orthorhombic structure. The wide bandgap semiconductor KNbO 3 transformed into a visible‐light‐active material, with its bandgap energy reduced from 3.56 eV to ≈2.4 eV. The substitution of K in KNbO 3 with Ba is responsible for structural modification from orthorhombic to cubic symmetry, whereas both structural modification and the substitution of Nb with Fe correlated with optical properties. The photocatalytic activities of all obtained solid solutions are improved compared with the parent KNbO 3 and Ba 2 FeNbO 6 compounds for photocatalytic degradation of methylene blue (MB) dye. Among the series of solid solutions, K 0.82 Ba 0.18 Fe 0.09 Nb 0.91 O 3 photocatalysts show the highest MB removal efficiency owing to its relatively higher surface area, suppressed charge carrier recombination, and more negative conduction band edge. Moreover, K 0.82 Ba 0.18 Fe 0.09 Nb 0.91 O 3 photocatalyst (0.1 g) combined with hydrogen peroxide (H 2 O 2 ) to form a novel photo‐Fenton system, achieving almost complete degradation of 100 mL of 10 mg L −1 MB dye in 30 min.

Avcıoğlu, Celal [Technische Universität Berlin, Fa↗

NASA NTRSDate not supplied

Passive Dust Mitigation Technologies Being Developed for Demonstration Under Patch Plate Materials Compatibility Analysis Task

With the Artemis program, we are planning longer stays on the surface, with more activities that have the potential to put the astronauts and equipment in contact with greater quantities of lunar dust. The success of these missions will depend on our understanding of material interactions with lunar dust and the development of ways to mitigate dust effects in cases where exposure to dust will lead to failure of components, unacceptable loss of power or thermal control, unacceptable loss of visibility, or health issues. Passive dust mitigation by coating or surface alteration is one method that is being developed and demonstrated under the Space Technology Mission Directorate’s Game Changing Technology, Dust Mitigation Program as part of the Patch Plate Materials Compatibility Assessment Task. The goal of the task is to alter the surfaces of materials in order to passively reduce the adhesion of dust, demonstrate their performance in relevant ground-based tests using lunar simulants, and prepare them for demonstration through experiment on the lunar surface. Optically transparent, sputter deposited, work function matching coatings are being developed to reduce adhesion of dust to windows, lenses and display panels by matching the minimum energy to remove an electron from the surface to that of lunar dust in order to reduce adhesion due to charge transfer. Low surface energy coatings and surfaces for thermal control are also being developed to reduce the bonding of dust with the surface enabling it to be removed more easily. Conductive coatings with the ability to shed dust more easily are being developed for use with the active Electrodynamic Dust Shield technology to help reduce the power needed to remove dust from the surface. Passive dust mitigation surfaces for metals such as aluminum, stainless steel, and titanium are being developed that reduce the area of dust contact with the surfaces through topographical modification using laser ablation patterning to impart hierarchical topographies with nanometer to micrometer length scales in a single step. Topographically modified polymeric materials, both those with extensive space heritage and those with lower technology readiness levels, are also being evaluated. Space suit fabric surfaces that can reduce dust penetration into and through the fabric are also being investigated as well as pristine and topographically modified ceramic materials that exhibit high wear resilience. An overview of the passive dust mitigation surfaces and coatings being developed under this task, ground testing being conducted using lunar simulants, characterization techniques, and materials preparation for flight sample delivery for integration into the Alpha Space Regolith Adherence Characterization experiment going to the lunar surface on a Commercial Lunar Payload Services (CLPS) lander in 2023 will be discussed.

Lunar dust, passive mitigation, lunar simulant, co↗

NASA NTRSDate not supplied

Evaluating Crystallinity in Thermoplastic Composites for Aerospace Applications

Polymer matrix composites (PMCs) offer many benefits for the aerospace industry due to their potential for weight reduction when compared to metal or ceramic based materials. Most PMCs currently in flight use thermoset matrices, however, thermoplastic resins are being explored as alternatives due to their ability to be remelted, which is of particular interest due to the potential for in-situ repair and faster production. Most thermoplastic resins are semicrystalline polymers. The properties of semicrystalline thermoplastics are directly influenced by their crystallinity, which can vary due to many factors including thermal treatments, environmental conditions, and mechanical deformation. Within thermoplastic PMC parts, crystallinity gradients can arise due to variations in part geometry, across part thicknesses, and along bonded joints. Monitoring the crystallinity of thermoplastic composites is key to ensuring these materials meet the high demands required for aerospace. Several different analytical techniques exist that can be used to characterize the bulk crystallinity of thermoplastic materials. However, many existing methods lack the specificity required to identify the subtle variations in crystallinity that may play a significant role in the performance and durability of PMC parts. Because of this, a significant amount of work is still required to fully characterize and understand the crystallinity profiles of thermoplastic PMCs and the resulting impact to material properties. This talk discusses the use of multiple techniques such as Differential Scanning Calorimetry, Polarized Light Optical Microscopy, and Fourier-Transform Infrared Spectroscopy to characterize the crystallinity in carbon fiber/thermoplastic composites. Samples of different crystallinity profiles were manufactured using various cooling procedures. This work aims to provide the fundamental data necessary to understand the effects of crystallinity on thermoplastic PMCs, which is key to advancing their use in aerospace applications.

Thermoplastics↗

NASA NTRS2003

Structural Anomalies Detected in Ceramic Matrix Composites Using Combined Nondestructive Evaluation and Finite Element Analysis (NDE and FEA)

Most reverse engineering approaches involve imaging or digitizing an object and then creating a computerized reconstruction that can be integrated, in three dimensions, into a particular design environment. The rapid prototyping technique builds high-quality physical prototypes directly from computer-aided design files. This fundamental technique for interpreting and interacting with large data sets is being used here via Velocity2 (an integrated image-processing software, ref. 1) using computed tomography (CT) data to produce a prototype three-dimensional test specimen model for analyses. A study at the NASA Glenn Research Center proposes to use these capabilities to conduct a combined nondestructive evaluation (NDE) and finite element analysis (FEA) to screen pretest and posttest structural anomalies in structural components. A tensile specimen made of silicon nitrite (Si3N4) ceramic matrix composite was considered to evaluate structural durability and deformity. Ceramic matrix composites are being sought as candidate materials to replace nickel-base superalloys for turbine engine applications. They have the unique characteristics of being able to withstand higher operating temperatures and harsh combustion environments. In addition, their low densities relative to metals help reduce component mass (ref. 2). Detailed three-dimensional volume rendering of the tensile test specimen was successfully carried out with Velocity2 (ref. 1) using two-dimensional images that were generated via computed tomography. Subsequent, three-dimensional finite element analyses were performed, and the results obtained were compared with those predicted by NDE-based calculations and experimental tests. It was shown that Velocity2 software can be used to render a three-dimensional object from a series of CT scan images with a minimum level of complexity. The analytical results (ref. 3) show that the high-stress regions correlated well with the damage sites identified by the CT scans and the experimental data. Furthermore, modeling of the voids collected via NDE offered an analytical advantage that resulted in more accurate assessments of the material s structural strength. The top figure shows a CT scan image of the specimen test section illustrating various hidden structural entities in the material and an optical image of the test specimen considered in this study. The bottom figure represents the stress response predicted from the finite element analyses (ref .3 ) for a selected CT slice where it clearly illustrates the correspondence of the high stress risers due to voids in the material with those predicted by the NDE. This study is continuing, and efforts are concentrated on improving the modeling capabilities to imitate the structural anomalies as detected.

Abdul-Aziz, Ali↗

DOE OSTI2020

Experimental system for studying temperature gradient-driven fracture of oxide nuclear fuel out of reactor

Temperature gradients in ceramic light water reactor (LWR) uranium dioxide (UO 2 ) nuclear fuel pellets generate thermal stresses that cause fractures in the fuel beginning early in the life of fresh fuel. The combination of heating due to fission and forced convective cooling on the exterior of LWR fuel rods generates a temperature profile that is difficult to replicate outside the reactor environment. In the present study, a state-of-the-art experimental set-up using electrical heating to replicate fission heating was built and surrogate fuel materials such as ceria (CeO 2 ) were used to validate the system. Cracking experiments were conducted on these surrogates by inducing reactivity-initiated-accident (RIA) like temperature gradients in the pellets via induction and direct resistance heating. Induction heating was done using copper coils and molybdenum susceptors which heated the surrogates to a threshold temperature that is sufficiently high for the fuel material to conduct current. Thereafter, direct resistance heating was used by a D.C. power supply to introduce volumetric heating to replicate LWR operating conditions analogous to fission heating. The pellets were held against nickel electrodes and mounted on a boron nitride test-stand. All the tests were carried out in a stainless-steel vacuum chamber. Simultaneous real-time dual imaging of the surrogate pellet surface has been implemented using an optical and infrared camera system which will be mounted along axial and perpendicular directions to the pellet surface respectively. A beam-splitter was used to split the incoming radiation from the sample into two halves. While one of the beams is transmitted from the splitter through a bandpass filter to obtain optical images, the other beam is reflected from the splitter to the thermal camera to capture full field temperature gradients of the as fabricated pellet surface during crack initiation and propagation. In the current series of tests, a 2-color pyrometer was used for recording and comparing the surface and centerline temperatures of the surrogate pellets in lieu of the thermal camera. A LabVIEW data acquisition system has been set up for collecting useful data during experiments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Structural Origins of High MoO 3 Solubility in Peraluminous Borosilicate Glasses

Molybdenum (Mo) imposes strict loading limits in conventional borosilicate nuclear waste glasses due to the tendency of tetrahedral molybdate [MoO 4 ] 2− species to phase-separate and crystallize as alkali molybdates. Here, we demonstrate an unprecedented 13.96 wt % (7.51 mol %) MoO 3 solubility in peraluminous sodium aluminoborosilicate glasses a ∼15× increase over their peralkaline counterparts. Using Raman spectroscopy, multinuclear and dipolarcorrelation magic angle spinning nuclear magnetic resonance (MAS NMR), electron paramagnetic resonance (EPR), and scanning transmission electron microscopy (STEM)-energy dispersive spectroscopy (EDS), we reveal that Nadeficient, low optical basicity conditions stabilize octahedral MoO 6 units, which polymerize into molybdite-like Mo−O clusters dispersed within the glass matrix. These Mo-rich clusters suppress the formation of depolymerized [MoO 4 ] 2− environments typically responsible for Na 2 MoO 4 precipitation and instead promote the formation of Na 2 Mo 2 O 7 as the saturation phase. Concurrently, Mo solubility drives the conversion of AlO 4 − to higher-coordination AlO 5 species, liberating Na + that is subsequently sequestered in molybdate-rich domains. The combined evolution of Mo coordination, modifier redistribution, and network depolymerization provides a mechanistic basis for the markedly enhanced Mo solubility in peraluminous compositions. These findings establish new structural guidelines for designing aluminoborosilicate waste forms with substantially greater capacity to incorporate Mo-rich nuclear waste streams.

Amorphous materials↗

NASA NTRS2007

NASA Tech Briefs, September 2007

Topics covered include; Rapid Fabrication of Carbide Matrix/Carbon Fiber Composites; Coating Thermoelectric Devices To Suppress Sublimation; Ultrahigh-Temperature Ceramics; Improved C/SiC Ceramic Composites Made Using PIP; Coating Carbon Fibers With Platinum; Two-Band, Low-Loss Microwave Window; MCM Polarimetric Radiometers for Planar Arrays; Aperture-Coupled Thin-Membrane L-Band Antenna; WGM-Based Photonic Local Oscillators and Modulators; Focal-Plane Arrays of Quantum-Dot Infrared Photodetectors; Laser Range and Bearing Finder With No Moving Parts; Microrectenna: A Terahertz Antenna and Rectifier on a Chip; Miniature L-Band Radar Transceiver; Robotic Vision-Based Localization in an Urban Environment; Programs for Testing an SSME-Monitoring System; Cathodoluminescent Source of Intense White Light; Displaying and Analyzing Antenna Radiation Patterns; Payload Operations Support Team Tools; Space-Shuttle Emulator Software; Soft Real-Time PID Control on a VME Computer; Analyzing Radio-Frequency Coverage for the ISS; Nanorod-Based Fast-Response Pressure-Sensitive Paints; Capacitors Would Help Protect Against Hypervelocity Impacts; Diaphragm Pump With Resonant Piezoelectric Drive; Improved Quick-Release Pin Mechanism; Designing Rolling-Element Bearings; Reverse-Tangent Injection in a Centrifugal Compressor; Inertial Measurements for Aero-assisted Navigation (IMAN); Analysis of Complex Valve and Feed Systems; Improved Path Planning Onboard the Mars Exploration Rovers; Robust, Flexible Motion Control for the Mars Explorer Rovers; Solar Sail Spaceflight Simulation; Fluorine-Based DRIE of Fused Silica; Mechanical Alloying for Making Thermoelectric Compounds; Process for High-Rate Fabrication of Alumina Nanotemplates; Electroform/Plasma-Spray Laminates for X-Ray Optics; An Automated Flying-Insect Detection System; Calligraphic Poling of Ferroelectric Material; Blackbody Cavity for Calibrations at 200 to 273 K; KML Super Overlay to WMS Translator; High-Performance Tiled WMS and KML Web Server; Modeling of Radiative Transfer in Protostellar Disks; Composite Pulse Tube; Photometric Calibration of Consumer Video Cameras; Criterion for Identifying Vortices in High- Pressure Flows; Amplified Thermionic Cooling Using Arrays of Nanowires; Delamination-Indicating Thermal Barrier Coatings; Preventing Raman Lasing in High-Q WGM Resonators; Procedures for Tuning a Multiresonator Photonic Filter; Robust Mapping of Incoherent Fiber-Optic Bundles; Extended-Range Ultrarefractive 1D Photonic Crystal Prisms; Rapid Analysis of Mass Distribution of Radiation Shielding; Modeling Magnetic Properties in EZTB; Deep Space Network Antenna Logic Controller; Modeling Carbon and Hydrocarbon Molecular Structures in EZTB; BigView Image Viewing on Tiled Displays; and Imaging Sensor Flight and Test Equipment Software.

Source record↗

NASA NTRS2013

Reliability of CCGA 1152 and CCGA 1272 Interconnect Packages for Extreme Thermal Environments

Ceramic column grid array (CCGA) packages have been increasing in use based on their advantages of high interconnect density, very good thermal and electrical performance, and compatibility with standard surface-mount packaging assembly processes. CCGA packages are used in space applications such as in logics and microprocessor functions, telecommunications, flight avionics, and payload electronics. As these packages tend to have less solder joint strain relief than leaded packages, the reliability of CCGA packages is very important for short- and long-term space missions. Certain planetary satellites require operations of thermally uncontrolled hardware under extremely cold and hot temperatures with large diurnal temperature change from day to night. The planetary protection requires the hardware to be baked at +125 C for 72 hours to kill microbugs to avoid any biological contamination, especially for sample return missions. Therefore, the present CCGA package reliability research study has encompassed the temperature range of 185 to +125 C to cover various NASA deep space missions. Advanced 1152 and 1272 CCGA packaging interconnects technology test hardware objects have been subjected to ex treme temperature thermal cycles from 185 to +125 C. X-ray inspections of CCGA packages have been made before thermal cycling. No anomalous behavior and process problems were observed in the x-ray images. The change in resistance of the daisy-chained CCGA interconnects was measured as a function of increasing number of thermal cycles. Electrical continuity measurements of daisy chains have shown no anomalies, even until 596 thermal cycles. Optical inspections of hardware have shown a significant fatigue for CCGA 1152 packages over CCGA 1272 packages. No catastrophic failures have been observed yet in the results. Process qualification and assembly are required to optimize the CCGA assembly processes. Optical inspections of CCGA boards have been made after 258 and 596 thermal cycles. Corner columns have started showing significant fatigue per optical inspection results.

Ramesham, Rajeshuni↗