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Modern steels at atomic and nanometre scales

Processing bulk nanocrystalline materials for structural applications still poses a difficult challenge, particularly in achieving an industrially viable process. Recent work in ferritic steels has proved that it is possible to move from ultrafine to nanoscale by exploiting the bainite reaction without the use of severe deformation, rapid heat treatment or mechanical processing. This new generation of steels has been designed in which transformation at low temperature leads to a nanoscale structure consisting of extremely fine, 20–40 nm thick plates of bainitic ferrite and films of retained austenite. Finally, a description of the characteristics and significance of this remarkable microstructure is provided here.

59 BASIC BIOLOGICAL SCIENCES↗

Structural Evaluation of Complex Subcomponents Manufactured by Large Scale Extrusion Deposition of Carbon Fiber Reinforced ABS

The large scale extrusion deposition process has recently been commercialized in the form of additive manufacturing machines such as the BAAM from Cincinnati Inc., which enables layered production of chopped fiber reinforced thermoplastic polymer systems. The application of this process to the automotive market is being pursued by Local Motors to enable rapid design to market cycles and build on-demand capability for a wide range of vehicle styles from a distributed network of micro-factories. This endeavor will require an understanding of the structural performance of components with complex geometries, where the properties are known to vary as a function of printing conditions, as well as orientation and shape. In order to rapidly build a database of structural performance, a beam specimen with outer dimensions of 914 x 305 x 64 mm3 was selected to be subjected to bending, torsion, and shear loading with full field displacement measurement by digital image correlation (DIC). A total of 25 different specimen configurations were designed including variation of print geometry, reinforcement by foam filling, and overwrapping with advanced composites. This work documents the results of the study and presents the relative performance of the structures in addition to the approach to simulation that is being initiated to serve as a framework for efficient design of structures manufactured in this way. The results are presented as a table of structural efficiency including stiffness and strength as functions of mass for each design. Additional results will also be provided in the form of surface displacements from DIC; future work will utilize this data to better optimize simulations for predicting structural performance of articles manufactured by this process.

Bedsole, Robert↗

wa-hls4ml and lui-gnn: A benchmark and GNN-based surrogate model for hls4ml resource and latency estimation

As machine learning (ML) increasingly serves as a tool for addressing real-time challenges in scientific applications, the development of advanced tooling has significantly reduced the time required to iterate on various designs. These advancements have solved major obstacles, but also exposed new challenges. For example, processes that were not previously considered bottlenecks, such as model synthesis, are now becoming limiting factors in the rapid iteration of designs. To reduce these emerging constraints, multiple efforts are being launched toward designing an ML-based surrogate model that estimates resource usage of synthesized accelerator architectures. This model would reduce the design iteration time, especially when designing within a set of given hardware constraints. This approach shows considerable potential, but as it stands, the effort is early and would benefit from coordination and standardization to assist future work as it emerges. We introduce wa-hls4ml, a benchmark for ML accelerator resource and latency estimation, and its corresponding initial dataset of more than 100,000 fully connected neural networks, all synthesized using hls4ml and targeting Xilinx FPGAs. In addition to the resource utilization and latency data provided, the dataset includes generated artifacts and log files for many of the synthesized neural networks, in order to support future research in ML-based code generation. The benchmark evaluates the performance of resource and latency predictors against several common ML model architectures, primarily originating from scientific domains, as exemplar models, as well as the average performance across a subset of the dataset. We measure the performance of a given predictor model through multiple metrics, including $R^2$ score and SMAPE on regression tasks, as well as inference time to further characterize the estimator under test. Additionally, we introduce the latency/utilization inference graph neural network (lui-gnn), a surrogate model that uses a graph neural network to represent input architectures in the form of a directed graph. This graph representation allows for a diverse set of model architectures to all be effectively handled by a surrogate model. We present the architecture and performance of the model, as evaluated by the new proposed benchmark, including SMAPE, $R^2$ score, and inference times, and find that lui-gnn generally predicts latency and utilization for the 75\% quantile within several percent of the synthesized resources on the synthetic test dataset, indicating that this approach of estimating resource and latency via a surrogate models has promise and warrants further research.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

RapidClave® Technology Demonstrations – II Hat Stiffener

This project sought to evaluate the cost and performance of both polymeric and metallic tooling for use with the RapidClave® composite process. Teijin’s rapid cure carbon/epoxy prepreg, Q183, was selected to fabricate demonstration components, of aerospace design, which currently are fabricated via compression molding using matched steel tooling. The ability to fabricate components using this prepreg in the RapidClave®, and using low cost single sided tooling, could significantly reduce the cost of part manufacture and shorten production lead times for tooling fabrication. The component demonstration article was a “hat stiffener” geometry typically used to reinforce fuselage or wing skins of an aircraft. A rapid preforming process was demonstrated and rapid process cycle times similar to compression molding were achieved by placing the preform on hot tooling, thus avoiding the time and energy associated with typical thermal cycling. A 90% reduction in tooling cost was achieved through the use of single sided aluminum or polymeric additive tooling when compared to compression molding matched steel tooling. In addition to rapid cycle times, RapidClave® offers the ability to change out tooling in minutes such that multiple part geometries can be fabricated in one shift.

36 MATERIALS SCIENCE↗

Laser 3D printing of highly compacted protonic ceramic electrolyzer stack

Solid oxide electrolysis cells (SOECs) for H 2 production is a core technology for H2@scale. However, its conventional manufacturing methods adapted from the manufacture of solid oxide fuel cells (SOFC) need high cost, especially for small-volume production. The emerging laser 3D printing (L3DP) technology with computer-aided 3D printing and computer-controlled laser processing can fulfill layer-by-layer digital shaping and rapid in-situ consolidating feedstock into complicated geometries. L3DP, a promising additive manufacturing (AM) technology, has achieved significant success in manufacturing plastic and metal parts, which is currently attracting considerable attention for the cost-effective, rapid, and flexible manufacturing of heterogeneous multilayered ceramic devices (e.g., SOECs, SOFCs, and solid-state batteries). It is believed that the L3DP can integrate the advantages of selective consolidation of heterogeneous layers, accurate control of layer microstructures, high processing heat efficiency, high processing speed, high stack compactness, high stack design flexibility, and low stack sealing area for cost-effective, rapid, and flexible manufacturing of SOECs to meet DOE’s electrolyzer target.

08 HYDROGEN↗

Additive Manufacturing in the Nuclear Reactor Industry

This article discusses the application of additive manufacturing in the nuclear reactor industry.Additive manufacturing for nuclear applications increased significantly in the late 2010s due to rapid progress in technology, particularly with methods using metals and ceramics.Because these manufacturing technologies are uniquely data-rich, they allow for an advanced understanding of materials, and they offer the potential to predict part performance based on build data. The inherent characteristics of additive manufacturing technologies allow for rapid prototyping and geometric freedom, making it possible to implement an accelerated agile design process for advanced nuclear reactor applications. Predictive high-fidelity multiphysics simulations are crucial to fully leverage this geometric flexibility. Qualification and regulator acceptance ultimately determine the breadth and scope of applications for these technologies. The US Department of Energy Office of Nuclear Energy Transformational Challenge Reactor program integrates many of these elements to accelerate the deployment of additive manufacturing technologies to industry.

Betzler, Benjamin↗

A Statistical Perspective on Highly Accelerated Testing

Highly accelerated life testing has been heavily promoted at Sandia (and elsewhere) as a means to rapidly identify product weaknesses caused by flaws in the product's design or manufacturing process. During product development, a small number of units are forced to fail at high stress. The failed units are then examined to determine the root causes of failure. The identification of the root causes of product failures exposed by highly accelerated life testing can instigate changes to the product's design and/or manufacturing process that result in a product with increased reliability. It is widely viewed that this qualitative use of highly accelerated life testing (often associated with the acronym HALT) can be useful. However, highly accelerated life testing has also been proposed as a quantitative means for "demonstrating" the reliability of a product where unreliability is associated with loss of margin via an identified and dominating failure mechanism. It is assumed that the dominant failure mechanism can be accelerated by changing the level of a stress factor that is assumed to be related to the dominant failure mode. In extreme cases, a minimal number of units (often from a pre-production lot) are subjected to a single highly accelerated stress relative to normal use. If no (or, sufficiently few) units fail at this high stress level, some might claim that a certain level of reliability has been demonstrated (relative to normal use conditions). Underlying this claim are assumptions regarding the level of knowledge associated with the relationship between the stress level and the probability of failure. The primary purpose of this document is to discuss (from a statistical perspective) the efficacy of using accelerated life testing protocols (and, in particular, "highly accelerated" protocols) to make quantitative inferences concerning the performance of a product (e.g., reliability) when in fact there is lack-of-knowledge and uncertainty concerning the assumed relationship between the stress level and performance. In addition, this document contains recommendations for conducting more informative accelerated tests.

42 ENGINEERING↗

Autonomous Flow Electrochemistry for Accelerated Catalyst Discovery

Our objective is to develop an Autonomous Chemical Experimentation (ACE) platform that accelerates discovery of new catalytic transformations and other energy-relevant chemical reactions and processes. We intentionally designed ACE to be highly modular, both with respect to its rapid deployment to different chemistries and experimental workflows as well as incorporation of a wide range of different AI algorithms. In addition to the development of the core software architecture, initial efforts were made to incorporate Large Language Models to provide human-interpretable reasoning of the optimizer’s actions, and to develop a user-friendly graphical interface for experimental researchers. ACE was demonstrated using a flow electrocatalysis platform containing an inline FTIR spectrometer for real-time analysis and quantification of the reaction outcome. Human-in-the-loop experiments were performed in which a human researcher conducted an experiment using electrode potentials suggested by ACE, then fed the spectral data back to ACE for decision making. After confirming the successful function of the optimizer, efforts were next directed to automation of the hardware and performed full autonomy tests using three reactions: catalytic oxidation of formate, catalytic oxidation of cyclohexanol, and oxidation of hydroquinone. These studies confirm that ACE can close the loop between reaction execution, analysis, and optimization. They also reveal that more improved product detection methods will be essential for ACE to make well-informed decisions for reactions with low conversions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Transforming BIM to BEM: Generation of Building Geometry for the NASA Ames Sustainability Base BIM

Typical processes of whole Building Energy simulation Model (BEM) generation are subjective, labor intensive, time intensive and error prone. Essentially, these typical processes reproduce already existing data, i.e. building models already created by the architect. Accordingly, Lawrence Berkeley National Laboratory (LBNL) developed a semi-automated process that enables reproducible conversions of Building Information Model (BIM) representations of building geometry into a format required by building energy modeling (BEM) tools. This is a generic process that may be applied to all building energy modeling tools but to date has only been used for EnergyPlus. This report describes and demonstrates each stage in the semi-automated process for building geometry using the recently constructed NASA Ames Sustainability Base throughout. This example uses ArchiCAD (Graphisoft, 2012) as the originating CAD tool and EnergyPlus as the concluding whole building energy simulation tool. It is important to note that the process is also applicable for professionals that use other CAD tools such as Revit (“Revit Architecture,” 2012) and DProfiler (Beck Technology, 2012) and can be extended to provide geometry definitions for BEM tools other than EnergyPlus. Geometry Simplification Tool (GST) was used during the NASA Ames project and was the enabling software that facilitated semi-automated data transformations. GST has now been superseded by Space Boundary Tool (SBT-1) and will be referred to as SBT-1 throughout this report. The benefits of this semi-automated process are fourfold: 1) reduce the amount of time and cost required to develop a whole building energy simulation model, 2) enable rapid generation of design alternatives, 3) improve the accuracy of BEMs and 4) result in significantly better performing buildings with significantly lower energy consumption than those created using the traditional design process, especially if the simulation model was used as a predictive benchmark during operation. Developing BIM based criteria to support the semi-automated process should result in significant reliable improvements and time savings in the development of BEMs. In order to define successful BIMS, CAD export of IFC based BIMs for BEM must adhere to a standard Model View Definition (MVD) for simulation as provided by the concept design BIM MVD (buildingSMART, 2011). In order to ensure wide scale adoption, companies would also need to develop their own material libraries to support automated activities and undertake a pilot project to improve understanding of modeling conventions and design tool features and limitations.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Opportunities for Process Intensification with Membranes to Promote Circular Economy Development for Critical Minerals

Critical minerals are essential to the future of clean energy, especially energy storage, electric vehicles, and advanced electronics. In this paper, we argue that process systems engineering (PSE) paradigms provide essential frameworks for enhancing the sustainability and efficiency of critical mineral processing pathways. As a concrete example, we review challenges and opportu-nities across material-to-infrastructure scales for process intensification (PI) with membranes. Within critical mineral processing, there is a need to reduce environmental impact, especially con-cerning chemical reagent usage. Feed concentrations and product demand variability require flex-ible, intensified processes. Further, unique feedstocks require unique processes (i.e., no one-size-fits-all recycling or refining system exists). Membrane materials span a vast design space that allows significant optimization. Therefore, there is a need to rapidly identify the best opportunities for membrane implementation, thus informing materials optimization with process and infrastructure scale performance targets. Finally, scale-up must be accelerated and de-risked across the materials-to-process levels to fully realize the opportunity presented by membranes, thereby fostering the development of a circular economy for critical minerals. Tackling these challenges requires integrating efforts across diverse disciplines. We advocate for a holistic molecular-to-systems perspective for fully realizing PI with membranes to address sustainability challenges in critical mineral processing. The opportunities for PI with membranes are excellent applications for emerging research in machine learning, data science, automation, and optimization.

Dougher, Molly↗

Understanding Fundamental Material Degradation Processes in High Temperature Aggressive Chemomechanical Environments

The objective of this project is to develop a fundamental understanding of the mechanisms that limit materials durability for very high-temperature applications. Current design limitations are based on material strength and corrosion resistance. This project will characterize the interactions of high-temperature creep, fatigue, and environmental attack in structural metallic alloys of interest for the very high-temperature gas-cooled reactor (VHTR) or Next–Generation Nuclear Plant (NGNP) and for the associated thermo-chemical processing systems for hydrogen generation. Each of these degradation processes presents a major materials design challenge on its own, but in combination, they can act synergistically to rapidly degrade materials and limit component lives. This research and development effort will provide experimental results to characterize creep-fatigue-environment interactions and develop predictive models to define operation limits for high-temperature structural material applications. Researchers will study individually and in combination creep-fatigue-environmental attack processes in Alloys 617, 230, and 800H, as well as in an advanced Ni-Cr oxide dispersion strengthened steel (ODS) system. For comparison, the study will also examine basic degradation processes in nichrome (Ni-20Cr), which is a basis for most high-temperature structural materials, as well as many of the superalloys. These materials are selected to represent primary candidate alloys, one advanced developmental alloy that may have superior high-temperature durability, and one model system on which basic performance and modeling efforts can be based. The research program is presented in four parts, which all complement each other. The first three are primarily experimental in nature, and the last will tie the work together in a coordinated modeling effort. The sections are (1) dynamic creep-fatigue-environment process, (2) subcritical crack processes, (3) dynamic corrosion – crack initiation processes, and (4) modeling.

36 MATERIALS SCIENCE↗

Additive manufacturing of carbon fiber-reinforced thermoset composites via in-situ thermal curing

Fiber-reinforced polymer composites are lightweight structural materials widely used in the transportation and energy industries. Current approaches for the manufacture of composites require expensive tooling and long, energy-intensive processing, resulting in a high cost of manufacturing, limited design complexity, and low fabrication rates. Here, we report rapid, scalable, and energy-efficient additive manufacturing of fiber-reinforced thermoset composites, while eliminating the need for tooling or molds. Use of a thermoresponsive thermoset resin as the matrix of composites and localized, remote heating of carbon fiber reinforcements via photothermal conversion enables rapid, in-situ curing of composites without further post-processing. Rapid curing and phase transformation of the matrix thermoset, from a liquid or viscous resin to a rigid polymer, immediately upon deposition by a robotic platform, allows for the high-fidelity, freeform manufacturing of discontinuous and continuous fiber-reinforced composites without using sacrificial support materials. This method is applicable to a variety of industries and will enable rapid and scalable manufacture of composite parts and tooling as well as on-demand repair of composite structures.

36 MATERIALS SCIENCE↗

A Structural Design Approach Tailored for the Rapid Preliminary Design of Microreactor Components

High-temperature microreactors can play a role in developing reliable, portable energy sources for off-grid remote locations, microgrid concepts, and industrial process heat. Portability and passive safety criteria tend to skew microreactor structural component designs toward complex geometries, high thermal stresses, and design bases with large numbers of startup/shutdown cycles. Current design rules, as typified by Section III of the American Society of Mechanical Engineers (ASME) Boiler & Pressure Vessel Code, are less than optimal for these conditions, particularly for preliminary component designs where developers need to rapidly consider a large number of potential component configurations. This paper presents a design method targeted toward rapid, efficient evaluation of preliminary component designs using modern finite element analysis. The new method retains key connections with the ASME Code rules and design data while streamlining the design approach. This paper presents the design method, several verification examples illustrating the similarities and differences between the new method and the current ASME rules, and the application of the new approach to the evaluation of a test article mimicking key features of a heat pipe–cooled microreactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A Limit to Accelerated Free-Sintering: Nano-Phase Separation Interferes With Organic Debinding

Nano-phase separating Ni–12 at. pct Ag powders are processed via high-energy ball milling and brought into a supersaturated state with a reduction of the grain size to the nanocrystalline scale, a combination that is designed to encourage rapid densification by phase separation upon heating. This unstable powder is then characterized by dilatometry, in-situ x-ray diffraction, thermogravimetry and microstructure analysis for sintering cycles up to 940 °C. However, these powder compacts exhibit excessive pore evolution and significant macroscopic swelling caused by removal of the organic process additives. This competition of organic removal with densification is known in nanocrystalline metals, but the present study adds an additional dimension of phase separation, which shifts the dominant swelling mechanism as the formation of the second phase traps the volatilizing organics and hinders the debinding process. The creep swelling and overall loss in relative density is then dominated by the creep deformation of the second Ag phase. The interference between organic removal and low-temperature onset of consolidation represents a new challenge to efforts aimed at rapid free sintering and should guide the design of rapidly sintering alloys; specifically, the present work emphasizes the need to select alloys that have their sintering-accelerating phase separation temperature above the range where gases are evolved.

36 MATERIALS SCIENCE↗

Design and Validation Testing of TruckScan to Assay Large Sacks of Fukushima Radioactive Debris on a Truck

As a result of the March 2011 earthquake and resulting tsunami in Japan, there was a serious accident at the Fukushima Dai-ichi Nuclear Power Plant. This accident has contaminated soil and vegetation in a wide area around the plant. Decontamination projects over the last 4 years have resulted in large numbers of 1 cubic meter canvas bags of debris, commonly called Super Sacks [SS]. These are currently stored nearby where they were generated, but starting in 2015, they will be moved to various Interim Storage Facilities [ISF]. Trucks will typically carry 8-20 of these SSs. When the trucks arrive at the ISF they need to be rapidly sorted into groups according to radioactivity level, for efficient subsequent processing. Canberra Industries, Inc. [CI] has designed a new truck monitoring system 'TruckScan' for use at these ISFs. The TruckScan system must measure the entire truck loaded with multiple closely packed SSs, and generate a nuclide specific assay report showing the radioactivity in each individual SS. The Canberra-Japan office, along with Obayashi Corporation have performed validation testing to demonstrate to the regulatory authorities that the proposed technique was sufficiently accurate. These validation tests were conducted at a temporary storage area in Fukushima prefecture. Decontaminated waste of various representative types and of various levels of radioactivity was gathered and mixed to create homogeneous volumes. These volumes were sampled multiple times and assayed with laboratory HPGe detectors to determine the reference concentration of each pile. Multiple SSs were loaded from each pile. Some of the SSs were filled 50% full, others 75% full, and others 100% full, to represent the typical loading configuration of the existing SSs in the field. The content of the SSs are either sand, soil, or vegetation with densities ranging from 0.3 g/cc - 1.6 g/cc. These SSs with known concentrations of Cs-134 and Cs-137 were then loaded onto trucks in a variety of configurations, typical of how they might be on the real trucks. A partial system was installed at the site and used to assay these trucks with the various loading configurations. Whereas the full system will have 8 collimated 3 x 3'' NaI detectors, the test system only had two detectors; therefore the truck was moved and counted 4 times. The data were acquired and analyzed with the Canberra Genie software to determine the peak counts for both Cesium nuclides. That data was then analyzed with a prototype version of a Maximum Entropy algorithm, to determine the individual SS activity. The goal of the validation tests was to demonstrate that the system could detect 1000 Bq/kg in 15 seconds, and to determine how accurately it could quantify individual SSs. The validation tests demonstrated that the product would perform as predicted. The TruckScan results were consistent with the sample assay results [y = 1.0029 x, R{sup 2} = 0.914]. The Total Propagated Uncertainty, including both uncertainties from these tests and others that were estimated but not tested was 16.6% percent. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Ultrafast (1‐5 sec) Lamination of Perovskite Solar Cells With Self‐Encapsulation Using Rapid Joule Heating

Perovskite solar cells (PSCs) are traditionally fabricated using sequential layer‐by‐layer deposition, in which each layer of the device is processed on top of the preceding layer. This constrains the processing techniques and selection of transport layer materials that can be used in the solar cell. To overcome these challenges, two half‐cells can be processed independently and then diffusion‐bonded through a lamination process. However, current lamination processes for perovskite solar cells suffer from relatively long process times, which can limit throughput when moving toward high‐volume manufacturing. In this study, a custom platform was designed for rapid‐joule heating of perovskite materials and devices. This enabled more than a 99% reduction in lamination time from 26 min to 1 s. Perovskite samples that were laminated in 1 s exhibited comparable values of percent bonded area, interfacial toughness, grain domain size, and X‐ray diffraction spectra to those laminated in greater than 10 min. As a proof‐of‐concept, 18.3% efficient devices were successfully laminated in 5 s. A transient heat transfer model was developed to describe the relationship between the perovskite temperature and the electrical power supplied to the heaters, establishing a baseline for predicting processing conditions in large‐scale manufacturing systems. Ultra‐fast lamination provides a pathway toward scalable roll‐to‐roll or sheet‐to‐sheet manufacturing of PSCs.

heat transfer↗

AOI [1] Advanced Manufacturing of Ceramic Anchors with Embedded Sensors for Process and Health Monitoring of Coal Boilers

Researchers at West Virginia University (WVU) developed methods to fabricate and test ceramic anchors with an embedded sensor technology for monitoring the health and processing conditions within pulverized coal (PC) and fluidized-bed combustion (FBC) boiler systems. The technology included the development of advanced manufacturing processes for 2D/3D printing electroceramic (conductive ceramic) sensor designs within the ceramic anchor microstructure during the manufacturing process. This advanced manufacturing process would allow for the precise control of local microstructure and composition in order to engineer layer-by-layer any protective and electrically active materials within the refractory anchor. This 3D printing technology would permit the rapid and controlled design of the refractory microstructure and embedded sensor design throughout the volume of the ceramic anchor. The work also included a method to interconnect the sensors to boiler shell through the anchor clamp, where the sensor signals will be processed by low-power electronics and transmitted wirelessly to a central processing hub. The end-goal of the program was to produce a ceramic anchor sensor system which would be ready for implementation within a coal boiler, and/or other similar refractory liner systems (such as that in the glass and metal manufacturing areas). The project objectives were to: 1) Define the chemical and microstructural stability, in addition to the electrical properties, of oxide and non-oxide ceramic composites to be embedded within the ceramic anchor compositions that may operate up to 1400ºC; 2) Develop and implement the 2D/3D printing technology to pattern and control the microstructure of the ceramic anchor and embedded sensor circuits; 3) Develop an interconnect technology which will permit easy installation of the ceramic anchors and signal collection at the boiler shell; 4) Develop low power analog electronics and wireless communication hardware to efficiently collect the sensor signal at each processing unit and transmit data to a central hub for data analysis; 5) Demonstrate the smart ceramic anchor system for temperature and liner fracture within a high-temperature processing unit, such as a boiler furnace or glass melting furnace floor/wall liner.

20 FOSSIL-FUELED POWER PLANTS↗