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At least 271 records · Page 15

Towards Automated and High-Throughput Quantitative Sizing and Isotopic Analysis of Nanoparticles via Single Particle-ICP-TOF-MS

The work described herein assesses the ability to characterize gold nanoparticles (Au NPs) of 50 and 100 nm, as well as 60 nm silver shelled gold core nanospheres (Au/Ag NPs), for their mass, respective size, and isotopic composition in an automated and unattended fashion. Here, an innovative autosampler was employed to mix and transport the blanks, standards, and samples into a high-efficiency single particle (SP) introduction system for subsequent analysis by inductively coupled plasma–time of flight–mass spectrometry (ICP-TOF-MS). Optimized NP transport efficiency into the ICP-TOF-MS was determined to be >80%. This combination, SP-ICP-TOF-MS, allowed for high-throughput sample analysis. Specifically, 50 total samples (including blanks/standards) were analyzed over 8 h, to provide an accurate characterization of the NPs. This methodology was implemented over the course of 5 days to assess its long-term reproducibility. Impressively, the in-run and day-to-day variation of sample transport is assessed to be 3.54 and 9.52% relative standard deviation (%RSD), respectively. The determination of Au NP size and concentration was of <5% relative difference from the certified values over these time periods. Isotopic characterization of the 107 Ag/ 109 Ag particles (n = 132,630) over the course of the measurements was determined to be 1.0788 ± 0.0030 with high accuracy (0.23% relative difference) when compared to the multi-collector–ICP-MS determination.

36 MATERIALS SCIENCE↗

High-Throughput Strategies that Encompass Experiments and Machine Learning to Predict the Mechanical Properties of Additive Manufactured Aerospace Alloys

Small Punch Test (SPT) uses a thin disk of material to predict mechanical properties. While SPT has existed for decades, it has been used largely as a qualitative evaluator of mechanical properties. Recent advances in computational modeling have enabled the extraction of uniaxial stress-strain response from the measured SPT load-displacement data. Due to small sample volumes and unidirectional testing, SPT is conducive to high-throughput automation and ideally suited to extract properties from high-cost materials. Aerospace alloys have been of recent interest to the Additive Manufacturing (AM) community due to AM’s unique ability to fabricate complex designs not possible, or extremely arduous, with conventional manufacturing. In this research, SPT, coupled with Materials Informatics and computational modeling, is used to develop relevant Process-Structure-Property relationships to decrease the cost and time of process optimization for AM aerospace alloys, namely Inconel 718, Inconel 625, and Niobium C103.

High-throughput Testing↗

High Throughput Laser Processing for Enhanced Battery Performance and Manufacturing

For widespread adoption of electric vehicles, lithium-ion batteries (LiBs) need to achieve energy densities of >275 Wh/kg, cell costs less than $100/kWh, and charge to more than 80% capacity within 15 minutes. Recently, it has been shown that introducing a secondary pore network in thick battery electrodes enables higher extracted capacity without a severe reduction in charge/discharge rate performance. Secondary pore networks consisting of ordered arrays of microstructures reduce tortuosity of Li+-ion transport deep into the thick electrodes, diminishing detrimental concentration gradients within the cell. Ultrafast (femtosecond)-pulsed laser ablation is a promising method to introduce such micro pores or channels in thick battery electrodes as it allows for precise control of pattern geometries, results in minimal damage to the electrode, and can be introduced into existing roll-to-roll electrode manufacturing lines. We have explored laser patterning to create secondary pore networks in a variety of battery electrode materials for both anode and cathode applications and characterized the laser-material interaction parameters. In addition, advanced materials characterization techniques (SEM-EDS, XRD) were used to explore whether ultrafast laser ablation affects the remaining electrode materials' morphology and structure. Furthermore, we have translated lab-scale laser ablation to high-throughput roll-to-roll processing at industrially relevant scales. Finally, we worked with Argonne National Laboratory, developers of the battery cost-analysis package BatPac, to estimate the additional manufacturing costs (CapEx and OpEx) for incorporation of laser-ablation processing to current battery electrode manufacturing. We estimate that ultrafast laser processing will add only -$1kWh, which for considerable improvements in cell performance, creates a compelling case for industry adoption.

battery↗

High-Throughput Electric-Field-Assisted Sintering and Characterization Techniques for Materials Discovery

Despite improvements in computing and modeling capabilities, the performance of new materials, particularly those which deviate greatly in composition from well-studied materials (e.g., high-entropy alloys), can be difficult to simulate given the lack of available experimental property data. While some modeling techniques may attempt to predict the properties of these exotic materials, most are forced to make extrapolations from more traditional materials. To fulfill the need for accelerated material synthesis and property measurement, a high-throughput methodology has been developed. Utilizing electric-field-assisted sintering (EFAS), also known as spark plasma sintering (SPS), equipped with custom tooling, samples of differing alloy compositions can be produced simultaneously as a single alloy array. Several arrays have been produced with compositions spanning the Co-Cr-Fe-Mn-Ni alloy family, including many high-entropy alloys, while the novel array geometry has enabled the samples to be polished and characterized in parallel, using X-ray diffraction, scanning-electron microscopy, and laser-based thermal diffusivity measurements.

36 MATERIALS SCIENCE↗

High-Throughput Ion Irradiation and Microstructural Characterization of Multi-Principal-Element Alloys

Multi-principal-element alloys (MPEAs) have garnered interest in the nuclear community for their apparent resistance to microstructural damage under irradiation. While both experimentation and simulation have demonstrated reduced hardening and void swelling in MPEAs, the relationship between composition and irradiation response is still poorly understood since a rich experimental database for MPEAs does not yet exist. In this work, to accelerate the generation of experimental irradiation-response data for MPEAs, high-throughput synthesis, irradiation, and characterization techniques have been employed. Specifically, additive manufacturing has been used to produce arrays of various MPEAs (1-cm2 coupons), which have been subsequently irradiated using 4-MeV Ni2+ ions to a peak damage of 200 dpa at 500 °C. Hardening and void swelling have been assessed using nanoindentation and trenching via plasma focused ion beam (PFIB), respectively. Trends in the experimental data relating hardening and void swelling behavior to composition have been analyzed using different machine learning approaches.

36 MATERIALS SCIENCE↗

Enhancing Post-Irradiation Examination (PIE) Efficiency with High-Throughput Experiments

Nuclear materials testing is essential for understanding changes in reactor environments, but traditional methods are costly and time-consuming. High-Throughput Experimentation (HTE) enables rapid screening and optimization of material properties by significantly increasing the number of specimens in the experiment. In this work, HTE methods were employed to irradiate novel materials at the Advanced Test Reactor (ATR) at Idaho National Laboratory. A total of 367 sub-sized tensile specimens were irradiated using the standard capsule design. To facilitate HTE, automated systems such as the Automated Mechanical Testing System were implemented for mechanical testing within hot cell environments, thereby reducing the need for manual interaction with hot cell manipulators and significantly lowering both the cost and duration of experiments. Digital image correlation (DIC) was used to measure displacement during mechanical testing, providing precise, non-contact measurement capabilities. The methodologies developed in this research will support the advancement of HTE techniques for future nuclear materials testing experiments at ATR. This approach allows for more efficient and cost-effective evaluation of new materials, ultimately leading to improved reactor performance, enhanced safety, and extended longevity within the nuclear industry.

22 - GENERAL STUDIES OF NUCLEAR REACTORS↗

Optimizing Piezoelectric Nanocomposites by High‐Throughput Phase‐Field Simulation and Machine Learning

Abstract Piezoelectric nanocomposites with oxide fillers in a polymer matrix combine the merit of high piezoelectric response of the oxides and flexibility as well as biocompatibility of the polymers. Understanding the role of the choice of materials and the filler‐matrix architecture is critical to achieving desired functionality of a composite towards applications in flexible electronics and energy harvest devices. Herein, a high‐throughput phase‐field simulation is conducted to systematically reveal the influence of morphology and spatial orientation of an oxide filler on the piezoelectric, mechanical, and dielectric properties of the piezoelectric nanocomposites. It is discovered that with a constant filler volume fraction, a composite composed of vertical pillars exhibits superior piezoelectric response and electromechanical coupling coefficient as compared to the other geometric configurations. An analytical regression is established from a linear regression‐based machine learning model, which can be employed to predict the performance of nanocomposites filled with oxides with a given set of piezoelectric coefficient, dielectric permittivity, and stiffness. This work not only sheds light on the fundamental mechanism of piezoelectric nanocomposites, but also offers a promising material design strategy for developing high‐performance polymer/inorganic oxide composite‐based wearable electronics.

42 ENGINEERING↗

Inverse Design of Photonic Surfaces via High throughput Femtosecond Laser Processing and Tandem Neural Networks

Abstract This work demonstrates a method to design photonic surfaces by combining femtosecond laser processing with the inverse design capabilities of tandem neural networks that directly link laser fabrication parameters to their resulting textured substrate optical properties. High throughput fabrication and characterization platforms are developed that generate a dataset comprising 35280 unique microtextured surfaces on stainless steel with corresponding measured spectral emissivities. The trained model utilizes the nonlinear one‐to‐many mapping between spectral emissivity and laser parameters. Consequently, it generates predominantly novel designs, which reproduce the full range of spectral emissivities (average root‐mean‐squared‐error < 2.5%) using only a compact region of laser parameter space 25 times smaller than what is represented in the training data. Finally, the inverse design model is experimentally validated on a thermophotovoltaic emitter design application. By synergizing laser‐matter interactions with neural network capabilities, the approach offers insights into accelerating the discovery of photonic surfaces, advancing energy harvesting technologies.

36 MATERIALS SCIENCE↗

Design of additively manufactured methanol conversion reactor for high throughput production

Additively manufactured methanol conversion reactor was designed and fabricated for high throughput fuel production while capturing carbon dioxide. Here, the reactor designed is part of large effort in integrating electrolyzer and catalytic reactor system. Processing in fabricating the steel, titanium, and nickel alloy reactors were optimized to improve the catalyst deposition process and reaction efficiency. Microstructure of the additively manufactured reactors were characterized. General design is utilized to improve the performance of the reactor while exploring the benefit of freeform in additive manufacturing.

08 HYDROGEN↗

Improved high-throughput screening technique to rapidly isolate Chlamydomonas transformants expressing recombinant proteins

Abstract The single-celled eukaryotic green alga Chlamydomonas reinhardtii has long been a model system for developing genetic tools for algae, and is also considered a potential platform for the production of high-value recombinant proteins. Identifying transformants with high levels of recombinant protein expression has been a challenge in this organism, as random integration of transgenes into the nuclear genome leads to low frequency of cell lines with high gene expression. Here, we describe the design of an optimized vector for the expression of recombinant proteins in Chlamydomonas , that when transformed and screened using a dual antibiotic selection, followed by screening using fluorescence activated cell sorting (FACS), permits rapid identification and isolation of microalgal transformants with high expression of a recombinant protein. This process greatly reduces the time required for the screening process, and can produce large populations of recombinant algae transformants with between 60 and 100% of cells producing the recombinant protein of interest, in as little as 3 weeks, that can then be used for whole population sequencing or individual clone analysis. Utilizing this new vector and high-throughput screening (HTS) process resulted in an order of magnitude improvement over existing methods, which normally produced under 1% of algae transformants expressing the protein of interest. This process can be applied to other algal strains and recombinant proteins to enhance screening efficiency, thereby speeding up the discovery and development of algal-derived recombinant protein products. Key points • A protein expression vector using double-antibiotic resistance genes was designed • Double antibiotic selection causes fewer colonies with more positive for phenotype • Coupling the new vector with FACS improves microalgal screening efficiency > 60%

59 BASIC BIOLOGICAL SCIENCES↗

Accelerated screening of functional atomic impurities in halide perovskites using high-throughput computations and machine learning

The pressing need for novel materials that can serve rising demands in solar cell and optoelectronic technologies makes the nexus of halide perovskites, high-throughput computations, and machine learning, very promising. Ever increasing amounts of data on the structure, fundamental properties, and device performance of halide perovskites provide opportunities for learning chemical rules and design principles that make these materials attractive, and applying them across wide chemical spaces. In this work, we show that impurity properties of halide perovskites computed using density functional theory (DFT) can be combined with machine learning (ML) to deliver predictive models and quick identification of optoelectronically active impurity atoms. Our computation lead to the largest reported dataset of the formation energies and charge transition levels of Pb-site impurities in methylammonium lead halide (MAPbX 3 ) perovskites. Descriptors are defined to uniquely represent any impurity atom in any MAPbX 3 compound and mapped to the computed impurity properties using regression techniques such as Gaussian process regression, neural networks, and random forests. We use the best optimized predictive models to make predictions for hundreds of impurities across 9 MAPbX 3 compounds and create lists of dominating impurities, that is, impurities that can shift the equilibrium Fermi level in the perovskite as determined by native point defects. Finally, this accelerated screening powered by computations and machine learning can guide the identification of problematic impurities that may cause undesired recombination of charge carriers, as well as impurities that can be deliberately introduced to tune the perovskite conductivity and resulting photovoltaic absorption.

36 MATERIALS SCIENCE↗

Combining Deep Learning and scatterControl for High-Throughput X-ray CT Based Non-Destructive Characterization of Large-Scale Casted Metallic Components

X-ray computed tomography (XCT) is essential for nondestructive evaluation and quality control of large-scale metal components. XCT imaging, however, faces significant challenges from metal artifacts, particularly those caused by Compton scattering, which degrade image quality and obscure critical details. Hardware-based solutions (e.g. scatterControl) offer advancements by intercepting scattered photons and reducing artifacts, but they can be time-consuming and require additional processing. Here, we propose modifying and leveraging a novel deep learning (DL) framework, Simurgh, to enhance and accelerate scatter correction in XCT. By combining scatterControl with DL-based artifact removal, we demonstrate significant reduction in scan time while producing high-quality reconstructions. Through extensive evaluation on industrial XCT data, we show that our methods reduce scan time by up to more than 10 x while preserving flaw detectability. Quantitative analysis across multiple segmentation techniques confirms that Simurgh-based reconstructions consistently outperform traditional Feldkamp-Davis-Kress, model-based iterative reconstruction, and commercial DL models in both pixel-level and task-specific evaluations, enabling scalable, high-throughput XCT workflows for characterization of large scale components in applications such as casting and metal additive manufacturing.

Complex metal parts↗

Plasma Bubble Column Reactor: A High Throughput Reactor Design for Water Treatment

Plasma-based water treatment (PWT) is a promising technology that can degrade various emerging contaminants. However, PWT application on an industrially viable scale is hindered by the lack of an efficient reactor design that combines enhanced plasma-liquid contact with high liquid throughput. This work investigates the applicability of a bubble column gas-liquid contactor to PWT. A pulsed plasma bubble column reactor (PBCR) with a concentric rod-cylinder electrode configuration was used to correlate contaminant removal performance with the gas-liquid contact parameters of the bubble column. A surfactant, rhodamine B dye, and a nonsurfactant, caffeine, were used as model contaminants at µM concentration levels. The bubble column characteristics, i.e., gas holdup, bubble size distribution, and gas-liquid area, were measured as a function of superficial gas velocity using image-based methods. Degradation rates of both contaminants increased with gas flowrate. For caffeine, the increase was attributed to intensified bulk liquid mixing, while dye degradation increased due to the increased gas-liquid area. Ultimately, we show that bubble column contactors significantly improve the utilization of plasma-generated reactive species toward contaminant degradation by distributing them over a large contact area. As a result, a better match between the plasma species interfacial flux and the interfacial contaminant concentration leads to improved treatment energy efficiency. Furthermore, typical degradation energy efficiencies were ~10 g/kWh for caffeine and ~60 g/kWh for rhodamine B.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High-Throughput Statistical Interrogation of Mechanical Properties with Build Plate Location and Powder Reuse in AlSi10Mg

Abstract Additive manufacturing (AM) allows agile, rapid manufacturing of geometrically complex components that would otherwise be impossible through traditional manufacturing methods. With this maturing manufacturing technology comes the need to adopt testing methods that are commensurate with the speed of additive manufacturing and take advantage of its geometric flexibility. High-throughput tensile testing (HTT) is a technique that allows a large number of tensile bars to be tested in a short amount of time. In the present study, HTT is used to evaluate AM AlSi10Mg produced using powder bed fusion with a Renishaw AM250 machine. Three parameters were varied in this study: (1) powder reuse history, (2) location on the build plate, and (3) size of the tensile specimen. For all parameter combinations, at least 22 specimens were tested; in several cases, over 40 were tested. This large dataset, consisting of over 500 tensile tests, permits Weibull statistical analysis and provides sufficient fidelity to isolate subtle trends that would have likely been missed in smaller, traditional datasets. The observed trends are rationalized in terms of the role of porosity and surface crust on mechanical response.

Carroll, Jay D. (ORCID:0000000258184709)↗

High-Throughput Nanoindentation Mapping of Additively Manufactured T91 Steel

Here, this work aims to adapt nanoindentation mapping combined with a k-means algorithm as a high-throughput technique to study the nano-scale spatial changes in mechanical properties for a heterogeneous material. This technique can also classify the individual data points based on their properties. Hundreds to thousands of indents were performed on additively manufactured T91 at room temperature, 300°C, 400°C, and 500°C across a square area with a side length of 120 μm to 400 μm. From this data, the hardness and reduced modulus at each point could be calculated and mapped. Using k-means clustering, we were able to arrange the data into three or four clusters corresponding roughly to the ferritic and martensitic phases as well as one or two intermediate clusters sampling both the phases. The hardness of these two phases appears to be quite stable as a function of temperature. Nanoindentation mapping and the k-means algorithm can therefore be used to rapidly assess the feasibility of heterogeneous materials under extreme conditions, such as nuclear reactor steels.

36 MATERIALS SCIENCE↗

L-PBF High-Throughput Data Pipeline Approach for Multi-modal Integration

Abstract Metal-based additive manufacturing requires active monitoring solutions for assessing part quality. Multiple sensors and data streams, however, generate large heterogeneous data sets that are impractical for manual assessment and characterization. In this work, an automated pipeline is developed that enables feature extraction from high-speed camera video and multi-modal data analysis. The framework removes the need for manual assessment through the utilization of deep learning techniques and training models in a weakly supervised paradigm. We demonstrate this pipeline’s capability over 700,000 high-speed camera frames. The pipeline successfully extracts melt pool and spatter geometries and links them to corresponding pyrometry, radiography, and processparameter information. 715 individual prints are examined to reveal melt pool areas that exceeds 0.07 mm 2 and pyrometry signal over a threshold (375 pyrometry units) were more likely to have defects. These automated processes enable massive throughput of characterization techniques.

36 MATERIALS SCIENCE↗

Electroslag additive manufacturing: A pathway for high throughput near net shape production

Electroslag Additive Manufacturing (ESAM), a new high-throughput additive manufacturing (AM) method that combines Electroslag Strip Cladding (ESC) and wire arc AM (WAAM) is introduced. This combination enables the high deposition rate of ESC (more than 20 kg/h with a 60 mm strip electrode) to benefit from the precise geometric control of WAAM. As a precursor to ESAM, the ESC process is investigated in an AM context independently by evaluating both direct and staggered bead-stacking strategies and analyzing the microstructural and mechanical properties of each. This is followed by an ESAM demonstration producing an annular geometry by pairing ESC with gas tungsten arc welding (GTAW), wherein GTAW is utilized to construct annular walls that are subsequently infilled via ESC. The microstructure and mechanical properties of ESC-only AM are compared with that of the ESAM method and it is shown that printed integral retaining walls do not impact the resulting mechanical properties of ESAM. Furthermore, results indicate that ESAM-produced Alloy 625 parts exhibit tensile properties on par with cast counterparts, supporting the method’s scalability to components exceeding one metric ton, and possibly making ESAM a viable future manufacturing approach for competitive production of large-scale components currently manufactured by casting and forging.

Additive manufacturing↗

Noise-aware optimization in nominally identical manufacturing and measuring systems for high-throughput parallel workflows

Device-to-device variability in experimental noise critically impacts reproducibility, especially in automated, high-throughput systems like additive manufacturing farms. While manageable in small labs, such variability can escalate into serious risks at larger scales, such as architectural 3D printing, where noise may cause structural or economic failures. This contribution presents a noise-aware decision-making algorithm that quantifies and models device-specific noise profiles to manage variability adaptively. It uses distributional analysis and pairwise divergence metrics with clustering to choose between single-device and robust multi-device Bayesian optimization strategies. Unlike conventional methods that assume homogeneous devices or enforce generic robustness, the proposed framework explicitly determines whether shared optimization across devices is appropriate based on the degree of inter-device noise heterogeneity. This enables improved performance, reproducibility, and efficiency. An experimental case study involving three nominally identical 3D printers (same brand, model, and close serial numbers) demonstrates reduced redundancy, lower resource usage, and improved reliability, along with improved convergence stability and solution quality through the selection of the appropriate optimization strategy based on the degree of inter-device noise heterogeneity. Overall, this framework establishes a general approach for precision- and resource-aware optimization in scalable, automated experimental platforms, demonstrated here on a representative multi-device 3D printing case study.

Schenk, Christina↗