The composition and phase fraction of the intergranular phase of 94ND10 ceramic is determined and fabricated ex situ. The fraction of each phase is 85.96 vol% Al2O3 bulk phase, 9.46 vol% Mg-rich intergranular phase, 4.36 vol% Ca/Si-rich intergranular phase, and 0.22 vol% voids. The Ca/Si-rich phase consists of 0.628 at% Mg, 12.59 at% Si, 10.24 at% Ca, 17.23 at% Al, and balance O. The Mgrich phase consists of 14.17 at% Mg, 0.066 at% Si, 0.047 at% Ca, 28.69 at% Al, and balance O. XRD of the ex situ intergranular material made by mixed oxides consisting of the above phase and element fractions yielded 92 vol% MgAl2O4 phase and 8 vol% CaAl2Si2O8 phase. The formation of MgAl2O4 phase is consistent with prior XRD of 94ND10, while the CaAl2Si2O8 phase may exist in 94ND10 but at a concentration not readily detected with XRD. The MgAl2O4 and CaAl2Si2O8 phases determined from XRD are expected to have the elemental compositions for the Mg-rich and Ca/Si-rich phases above by cation substitutions (e.g., some Mg substituted for by Ca in the Mg-rich phase) and impurity phases not detectable with XRD.
Mechanical strength of a 94 wt% debased alumina was measured using ASTM-C1161 specimens fabricated via conventional and lithography-based ceramic manufacturing (LCM) methods. The effects of build orientation and a 1500°C wet hydrogen fire added to the LCM firing sequence on strength were evaluated. A Weibull fit to the conventional flexural specimen data yielded 20 and 356 MPa for the modulus and characteristic strength, respectively. Weibull fits of the data from the LCM specimens yielded moduli between 7.5 and 11.3 and characteristics strengths between 333 and 339 MPa. A Weibull fit to data from LCM specimens subjected to the wet hydrogen fire yielded 14.2 and 376 MPa for the modulus and characteristic strength, respectively. The 95% confidence intervals for all Weibull parameters are reported. Average Archimedes bulk densities of LCM and conventional specimens were 3.732 and 3.730 g/cm3, respectively. Process dependent differences in surface morphology were observed in scanning electron microscope (SEM) images of specimen surfaces. SEM images of LCM specimen cross-sections showed alumina grain texture dependent on build direction, but no evidence of porosity concentrated in planes between printed layers. Fracture surfaces of LCM and conventionally processed specimens revealed hackle lines and mirror regions indicative of fracture initiation at the sample surface rather than the interior.
Ceramic to metal brazing is a common bonding process usedin many advanced systems such as automotive engines, aircraftengines, and electronics. In this study, we use optimizationtechniques and finite element analysis utilizing viscoplastic andthermo-elastic material models to find an optimum thermalprofile for a Kovar® washer bonded to an alumina button that istypical of a tension pull test. Several active braze filler materialsare included in this work. Cooling rates, annealing times, aging,and thermal profile shapes are related to specific materialbehaviors. Viscoplastic material models are used to represent thecreep and plasticity behavior in the Kovar® and braze materialswhile a thermo-elastic material model is used on the alumina.The Kovar® is particularly interesting because it has a Curiepoint at 435°C that creates a nonlinearity in its thermal strain andstiffness profiles. This complex behavior incentivizes theoptimizer to maximize the stress above the Curie point with afast cooling rate and then favors slow cooling rates below theCurie point to anneal the material. It is assumed that if failureoccurs in these joints, it will occur in the ceramic material.Consequently, the maximum principle stress of the ceramic isminimized in the objective function. Specific details of the stressstate are considered and discussed.
Additive Manufacturing (AM) offers the opportunity to transform design, manufacturing, and qualification with its unique capabilities. AM is a disruptive technology, allowing the capability to simultaneously create part and material while tightly controlling and monitoring the manufacturing process at the voxel level, with the inherent flexibility and agility in printing layer-by-layer. AM enables the possibility of measuring critical material and part parameters during manufacturing, thus changing the way we collect data, assess performance, and accept or qualify parts. It provides an opportunity to shift from the current iterative design-build-test qualification paradigm using traditional manufacturing processes to design-by-predictivity where requirements are addressed concurrently and rapidly. The new qualification paradigm driven by AM provides the opportunity to predict performance probabilistically, to optimally control the manufacturing process, and to implement accelerated cycles of learning. Exploiting these capabilities to realize a new uncertainty quantification-driven qualification that is rapid, flexible, and practical is the focus of this paper.
This SAND report fulfills the final report requirement for the Born Qualified Grand Challenge LDRD. Born Qualified was funded from FY16-FY18 with a total budget of ~$13M over the 3 years of funding. Overall 70+ staff, Post Docs, and students supported this project over its lifetime. The driver for Born Qualified was using Additive Manufacturing (AM) to change the qualification paradigm for low volume, high value, high consequence, complex parts that are common in high-risk industries such as ND, defense, energy, aerospace, and medical. AM offers the opportunity to transform design, manufacturing, and qualification with its unique capabilities. AM is a disruptive technology, allowing the capability to simultaneously create part and material while tightly controlling and monitoring the manufacturing process at the voxel level, with the inherent flexibility and agility in printing layer-by-layer. AM enables the possibility of measuring critical material and part parameters during manufacturing, thus changing the way we collect data, assess performance, and accept or qualify parts. It provides an opportunity to shift from the current iterative design-build-test qualification paradigm using traditional manufacturing processes to design-by-predictivity where requirements are addressed concurrently and rapidly. The new qualification paradigm driven by AM provides the opportunity to predict performance probabilistically, to optimally control the manufacturing process, and to implement accelerated cycles of learning. Exploiting these capabilities to realize a new uncertainty quantification-driven qualification that is rapid, flexible, and practical is the focus of this effort.
This report summarizes the data analysis activities that were performed under the Born Qualified Grand Challenge Project from 2016 - 2018. It is meant to document the characterization of additively manufactured parts and processe s for this project as well as demonstrate and identify further analyses and data science that could be done relating material processes to microstructure to properties to performance.
Erbium metal thin-films have been deposited on molybdenum-on-silicon substrates and then converted to erbium dideuteride (ErD{sub 2}). Here, we study the effects of deposition temperature ({approx}300 or 723 K) and deposition rate (1 or 20 nm/s) upon the initial Er metal microstructure and subsequent ErD{sub 2} microstructure. We find that low deposition temperature and low deposition rate lead to small Er metal grain sizes, and high deposition temperature and deposition rate led to larger Er metal grain sizes, consistent with published models of metal thin-film growth. ErD{sub 2} grain sizes are strongly influenced by the prior-metal grain size, with small metal grains leading to large ErD{sub 2} grains. A novel sample preparation technique for electron backscatter diffraction of air-sensitive ErD{sub 2} was developed, and allowed the quantitative measurement of ErD{sub 2} grain size and crystallographic texture. Finer-grained ErD{sub 2} showed a strong (1 1 1) fiber texture, whereas larger grained ErD{sub 2} had only weak texture. We hypothesize that this inverse correlation may arise from improved hydrogen diffusion kinetics in the more defective fine-grained metal structure or due to improved nucleation in the textured large-grain Er.
{sm_bullet}Mixing from some thermal process steps thought to drive H,D,T loss - This does not appear to be a problem with the Mo/Er occluder stacks {sm_bullet}Diffusion barriers investigated to prevent mixing
Sandia National Laboratories has cradle to grave responsibility for all neutron generators in the US nuclear weapons stockpile. As such, much research effort is exerted to develop a comprehensive understanding of all the major components of a neutron generator. One of the key components is the tritium containing target. The target is a thin metal tritide film. Sandia's research into metal tritides began in the early 1960's with a collaboration with the Denver Research Institute (DRI) and continues to this day with a major in house research effort. This document is an attempt to briefly summarize what is known about the aging of erbium tritide and to review the major publications conducted at Sandia in FY 07. First, a review of our knowledge of helium in erbium tritide will be presented. Second, executive summaries of the six major SAND reports regarding neutron tube targets published in FY07 by Department 2735, the Applied Science and Technology Maturation Department, and research partners are presented.
The potential for electrochromic (EC) materials to be incorporated into a Fabry-Perot (FP) filter to allow modest amounts of tuning was evaluated by both experimental methods and modeling. A combination of chemical vapor deposition (CVD), physical vapor deposition (PVD), and electrochemical methods was used to produce an ECFP film stack consisting of an EC WO{sub 3}/Ta{sub 2}O{sub 5}/NiO{sub x}H{sub y} film stack (with indium-tin-oxide electrodes) sandwiched between two Si{sub 3}N{sub 4}/SiO{sub 2} dielectric reflector stacks. A process to produce a NiO{sub x}H{sub y} charge storage layer that freed the EC stack from dependence on atmospheric humidity and allowed construction of this complex EC-FP stack was developed. The refractive index (n) and extinction coefficient (k) for each layer in the EC-FP film stack was measured between 300 and 1700 nm. A prototype EC-FP filter was produced that had a transmission at 500 nm of 36%, and a FWHM of 10 nm. A general modeling approach that takes into account the desired pass band location, pass band width, required transmission and EC optical constants in order to estimate the maximum tuning from an EC-FP filter was developed. Modeling shows that minor thickness changes in the prototype stack developed in this project should yield a filter with a transmission at 600 nm of 33% and a FWHM of 9.6 nm, which could be tuned to 598 nm with a FWHM of 12.1 nm and a transmission of 16%. Additional modeling shows that if the EC WO{sub 3} absorption centers were optimized, then a shift from 600 nm to 598 nm could be made with a FWHM of 11.3 nm and a transmission of 20%. If (at 600 nm) the FWHM is decreased to 1 nm and transmission maintained at a reasonable level (e.g. 30%), only fractions of a nm of tuning would be possible with the film stack considered in this study. These tradeoffs may improve at other wavelengths or with EC materials different than those considered here. Finally, based on our limited investigation and material set, the severe absorption associated with the refractive index change suggests that incorporating EC materials into phase correcting spatial light modulators (SLMS) would allow for only negligible phase correction before transmission losses became too severe. However, we would like to emphasize that other EC materials may allow sufficient phase correction with limited absorption, which could make this approach attractive.
Electrochromic (EC) materials are used in 'smart' windows that can be darkened by applying a voltage across an EC stack on the window. The associated change in refractive index (n) in the EC materials might allow their use in tunable or temperature-insensitive Fabry-Perot filters and transmissive-spatial-light-modulators (SLMs). The authors are conducting a preliminary evaluation of these materials in many applications, including target-in-the-loop systems. Data on tungsten oxide, WO{sub 3}, the workhorse EC material, indicate that it's possible to achieve modest changes in n with only slight increases in absorption between the visible and {approx}10 {micro}m. This might enable construction of a tunable Fabry-Perot filter consisting of an active EC layer (e.g. WO{sub 3}) and a proton conductor (e.g.Ta{sub 2}O{sub 5}) sandwiched between two gold electrodes. A SLM might be produced by replacing the gold with a transparent conductor (e.g. ITO). This SLM would allow broad-band operation like a micromirror array. Since it's a transmission element, simple optical designs like those in liquid-crystal systems would be possible. Our team has fabricated EC stacks and characterized their switching speed and optical properties (n, k). We plan to study the interplay between process parameters, film properties, and performance characteristics associated with the FP-filter and then extend what we learn to SLMs. Our goals are to understand whether the changes in absorption associated with changes in n are acceptable, and whether it's possible to design an EC-stack that's fast enough to be interesting. We'll present our preliminary findings regarding the potential viability of EC materials for target-in-the-loop applications.