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DOE OSTI2021

Embedding Sensors in 3D Printed Metal Structures

The Transformational Challenge Reactor (TCR) program is leveraging recent advances in modeling and simulation, materials, and additive manufacturing (AM) technologies to design a modern nuclear reactor. Some of the main TCR technologies include in situ monitoring and the integration of sensors during the manufacturing of quality-significant nuclear reactor components. This report describes the general procedure and process optimization for embedding sensors within generic stainless steel 316 (SS316) components using laser powder bed fusion (LPBF). A more detailed, quality-significant test plan and supporting procedures are available upon request (ORNL/TM-2021/2127). LPBF involves the use of a scanning laser to selectively melt regions of a powder bed, additively building a part layer by layer. This report describes the LPBF processing technique and discusses the effects of LPBF processing parameters on the success of the sensor embedding process. Experiments used machined cavities in the form of channels in an SS316 base for the sensors to lay in while material is additively built over the top, thereby embedding them in an SS316 matrix. A preliminary investigation involved using empty SS316 sheaths as surrogates to explore the effects of various LPBF processing parameters and the dimensional requirements of the machined channels. Microstructural investigations showed that a smaller channel width/depth combination closer to the sensor’s diameter was best for the embedding process. After the desired parameters were selected, Type-K thermocouples were embedded and evaluated post-embedding using nondestructive thermal testing, as well as destructive sectioning and microscopy. Post-build characterization showed that the thermocouples were well-bonded to the SS316 matrix and were fully functional after embedding. During thermal testing to temperatures up to 500 °C, the embedded thermocouples read consistently with one another and deviated only slightly from the readings of a nonembedded thermocouple located within the furnace. This slight discrepancy was most likely due to differences in the thermal time constants for a nonembedded thermocouple vs. a thermocouple embedded in a solid SS316 block. The results presented in this report will serve as the foundation for future work that will focus on embedding sensors in relevant TCR reactor components and eventually testing those components under neutron irradiation.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Factors Governing Oxygen Vacancy Formation in Oxide Perovskites

The control of oxygen vacancy (V O ) formation is critical to advancing multiple metal-oxide-perovskite-based technologies. In this work, we report the construction of a compact linear model for the neutral V O formation energy in ABO 3 perovskites that reproduces, with reasonable fidelity, Hubbard-U-corrected density functional theory calculations based on the state-of-the-art, strongly constrained and appropriately normed exchange-correlation functional. We obtain a mean absolute error of 0.45 eV for perovskites stable at 298 K, an accuracy that holds across a large, electronically diverse set of ABO 3 perovskites. Our model considers perovskites containing alkaline-earth metals (Ca, Sr, and Ba) and lanthanides (La and Ce) on the A-site and 3d transition metals (Ti, V, Cr, Mn, Fe, Co, and Ni) on the B-site in six different crystal systems (cubic, tetragonal, orthorhombic, hexagonal, rhombohedral, and monoclinic) common to perovskites. Physically intuitive metrics easily extracted from existing experimental thermochemical data or via inexpensive quantum mechanical calculations, including crystal bond dissociation energies and (solid phase) reduction potentials, are key components of the model. Beyond validation of the model against known experimental trends in materials used in solid oxide fuel cells, the model yields new candidate perovskites not contained in our training data set, such as (Bi,Y)(Fe,Co)O 3 , which we predict may have favorable thermochemical water-splitting properties. The confluence of sufficient accuracy, efficiency, and interpretability afforded by our model not only facilitates high-throughput computational screening for any application that requires the precise control of V O concentrations but also provides a clear picture of the dominant physics governing V O formation in metal-oxide perovskites.

08 HYDROGEN↗

DOE OSTI2024

Accelerating the Scalability of PrintCast structures using High Pressure Die Casting

PrintCast composites are fabricated by infiltrating a metal mesh or preform (e.g., an additively-manufactured 316L lattices) with molten metal of a lower melting temperature (e.g., A380 aluminum). The resulting PrintCast composite has been shown in the literature to produce diverse and unique mechanical properties that are controllable at the local or global level by adjusting volume-fraction and/or topology of the preforms geometry and overall volume fraction. Although promising mechanical and thermal properties have been achieved at the laboratory scale level, the scalability from laboratory to full scale components has been limited using conventional casting infiltration. This work highlights how using high pressure die casting can significantly advance the development and eventual deployment of PrintCast approaches at large scales. We have successfully produced 9-inch by 6-inch by 1-inch thick PrintCast 316L stainless steel/A380 aluminum “bricks” via high pressure die casting. Initial findings show excellent infiltration and production capability. The resulting approach demonstrates the scalability and manufacturability of hybrid cost effective metal-metal matrix composites at larger length scales with high quality infiltration results.

Splitter, Derek↗

DOE OSTI2023

Efficient Solar Spectrum-Like White-Light Emission in Zinc-Based Zero-Dimensional Hybrid Metal Halides

Organic–inorganic metal halides (OIMHs) with high-efficiency solar spectrum-like emission are attracting broad and current interest. Here, in this work, five 0D Zn-based hybrid halides are synthesized based on aromatic organic cations with different carbon-chain lengths: C 6 H 5 CH 2 NH 3 + (PMA + ) and C 6 H 5 (CH 2 ) 4 NH 3 + (PBA + ). (PMA) 2 ZnCl 4 exhibits the highest photoluminescence quantum yield of 37.2% of reported Zn-based white-emission OIMHs. The emission spectrum of (PBA) 2 ZnI 4 indicates a color rendering index of 98, which is the highest among single-component white-light-emitting phosphors. Spectral characterizations and density functional theory calculations demonstrate that the extremely broad emission of (PBA) 2 ZnI 4 originates from the synergistic emission of organic cations and self-trapped excitons. The optical properties of the obtained (PMA) 2 ZnBr 4 , (PMA) 2 ZnI 4 ·H 2 O, and (PBA) 2 ZnCl 4 are also characterized for comparison, and with the same organic cations, the PLQY decreases from chloride to bromide to iodide. This work demonstrates that the selection of appropriate organics and halogens can enable fine tuning of single-component white-light emission, satisfying varying needs for solid-state lighting.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Establishing a Design Strategy for Corrosion Resistant Structural Materials in Molten Salt Technologies

To address the gap in material design strategies for structural components in molten salt-powered technologies, the current work aimed to identify key parameters governing corrosion induced degradation of materials during exposures in molten halide salts. The applicability of the data on dissolution rates of pure metals (e.g., Cr) in a given molten salt to enable predictions of corrosion behavior of multicomponent binary and ternary Fe-based model and Ni-based commercial alloys isothermally exposed in the purified KCl-MgCl 2 in quartz capsules at 700 and 800°C was evaluated. The influence of alloy chemistry on initial dissolution rates and the consequent impact on the time-dependent corrosion induced microstructural evolution in the alloy subsurface was predicted with a coupled thermodynamic-kinetic model. Finally, the model was well able to predict the Cr depletion in all investigated alloys demonstrating the ability of the proposed approach to enable a unique design strategy for structural materials in molten salts.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Integrated process-structure–property–performance optimization of cold-sprayed zinc coatings on AZ91 magnesium alloy

High-pressure die cast (HPDC) AZ91 magnesium alloy is widely used in automotive components such as transmission housings and brackets for its excellent strength-to-weight ratio. Zinc-based cold spray coatings can be applied selectively to vulnerable areas to enhance corrosion resistance, minimize galvanic coupling with dissimilar metals, and eliminate the need for full-surface oxide coatings, making the process more efficient and targeted. A comprehensive evaluation of 16 combinations of nitrogen carrier gas temperatures and pressures led to the identification of an optimal range of process parameters, yielding Zn coatings with porosity <0.5 % by area, wear rates reduced by a factor of two compared to uncoated AZ91, and adhesion strengths up to 35 MPa. The enhanced mechanical performance of the coating is attributed to the low porosity and the formation of a metallurgical bond at the coating-substrate interface. Corrosion studies using macroscale potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS) revealed a significant decrease in corrosion rate and a shift to more noble corrosion potentials (ZCP) for coated substrates. Furthermore, the Zn cold-sprayed samples exhibited significantly lower corrosion-induced evolved hydrogen content compared to the base AZ91 substrate and AZ91 coated with industrial coatings, demonstrating that the Zn layer effectively protects the substrate from the corrosive environment. Overall, cold spray Zn coatings significantly improve the mechanical and corrosion performance of AZ91 Mg alloys, addressing key material challenges and enabling their broader use in automotive applications.

Corrosion performance↗

DOE OSTI2025

Aqueous-based recycling of perovskite photovoltaics

Abstract Cumulative silicon photovoltaic (PV) waste highlights the importance of considering waste recycling before the commercialization of emerging PV technologies 1,2 . Perovskite PVs are a promising next-generation technology 3 , in which recycling their end-of-life waste can reduce the toxic waste and retain resources 4,5 . Here we report a low-cost, green-solvent-based holistic recycling strategy to restore all valuable components from perovskite PV waste. We develop an efficient aqueous-based perovskite recycling approach that can also rejuvenate degraded perovskites. We further extend the scope of recycling to charge-transport layers, substrates, cover glasses and metal electrodes. After repeated degradation–recycling processes, the recycled devices show similar efficiency and stability compared with the fresh devices. Our holistic recycling strategy reduces by 96.6% resource depletion and by 68.8% human toxicity (cancer effects) impacts associated with perovskite PVs compared with the landfill treatment. With recycling, the levelized cost of electricity also decreases for both utility-scale and residential systems. This study highlights unique opportunities of perovskite PVs for holistic recycling and paves the way for a sustainable perovskite solar economy.

Science & Technology - Other Topics↗

DOE OSTI2023

Channeling Engineering of Hydroxide Ion Exchange Polymers and Reinforced Membranes

In this project, a team of researchers from Rensselaer Polytechnic Institute developed high performance alkaline conductors which can improve efficiency and lower cost of energy storage and conversion technology. The Rensselaer Polytechnic Institute team has developed a highly ion conductive, chemically stable, and mechanically durable alkaline membrane materials. Such membranes will serve as a critical component in electrochemical devices when energy was generated from renewable sources (e.g., sun and wind) or hydrogen fuel. The use of alkaline membrane in electrochemical reactions allows to replace expensive platinum catalyst to less expensive, earth abundant metals as catalysts, offering huge economic advantages in renewable energy technology.

08 HYDROGEN↗

DOE OSTI2021

Carbon material supported hollow metal oxide nanoparticles, methods and applications

A method for preparing a material composition comprising a hollow transition metal oxide nanoparticle supported upon a carbon material support includes a solution impregnation process step, followed by a thermal reduction process step and finally a thermal oxidation process step. The material composition, an electrode and an electrical component such as but not limited to a battery are all predicated at least in-part upon the material composition prepared in accord with the foregoing method. The foregoing material composition, electrode, battery and method may ultimately provide a LIB with enhanced performance.

Yu, Yingchao↗

DOE OSTI2023

Molten Salt Tritium Transport Experiment: A Versatile Fluoride Salt Loop for Validation of Tritium Transport Phenomena

Tritium is generated in Molten Salt Reactors (MSRs) from neutron capture by lithium and other constituents of the molten salt FLiBe. Tritium is a unique radionuclide as it readily permeates through hot structural materials. Thus, any material in contact with tritium laden molten salt is a potential pathway for release. Understanding tritium transport and devising adequate control strategies is necessary for the safe operation of MSRs. The Molten Salt Tritium Transport Experiment (MSTTE) is a forced-convection fluoride salt loop with the capability to inject hydrogen isotopes into flowing molten salt and to measure transport phenomena such as permeation through metals and evolution from free-surfaces. MSTTE is designed to be versatile to test potential control technology in future campaigns. This report focuses on the current design and analysis of MSTTE. Custom designed and fabricated experiment components such as the hydrogen injection system, permeation test section, diagnostics, and gas distribution system are discussed in detail. System-level tritium transport modeling using the System Analysis Module investigates experiment parameters such as hydrogen source terms, salt flow rate, and salt temperature. Computational fluid dynamics of the salt flow in the permeation test section informs design choices to establish fully developed flow in the measured permeation zone.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Unsupervised learning-enabled pulsed infrared thermographic microscopy of subsurface defects in stainless steel

Metallic structures produced with laser powder bed fusion (LPBF) additive manufacturing method (AM) frequently contain microscopic porosity defects, with typical approximate size distribution from one to 100 microns. Presence of such defects could lead to premature failure of the structure. In principle, structural integrity assessment of LPBF metals can be accomplished with nondestructive evaluation (NDE). Pulsed infrared thermography (PIT) is a non-contact, one-sided NDE method that allows for imaging of internal defects in arbitrary size and shape metallic structures using heat transfer. PIT imaging is performed using compact instrumentation consisting of a flash lamp for deposition of a heat pulse, and a fast frame infrared (IR) camera for measuring surface temperature transients. However, limitations of imaging resolution with PIT include blurring due to heat diffusion, sensitivity limit of the IR camera. We demonstrate enhancement of PIT imaging capability with unsupervised learning (UL), which enables PIT microscopy of subsurface defects in high strength corrosion resistant stainless steel 316 alloy. PIT images were processed with UL spatial–temporal separation-based clustering segmentation (STSCS) algorithm, refined by morphology image processing methods to enhance visibility of defects. The STSCS algorithm starts with wavelet decomposition to spatially de-noise thermograms, followed by UL principal component analysis (PCA), fine-tuning optimization, and neural learning-based independent component analysis (ICA) algorithms to temporally compress de-noised thermograms. The compressed thermograms were further processed with UL-based graph thresholding K-means clustering algorithm for defects segmentation. The STSCS algorithm also includes online learning feature for efficient re-training of the model with new data. For this study, metallic specimens with calibrated microscopic flat bottom hole defects, with diameters in the range from 203 to 76 µm, were produced using electro discharge machining (EDM) drilling. While the raw thermograms do not show any material defects, using STSCS algorithm to process PIT images reveals defects as small as 101 µm in diameter. To the best of our knowledge, this is the smallest reported size of a sub-surface defect in a metal imaged with PIT, which demonstrates the PIT capability of detecting defects in the size range relevant to quality control requirements of LPBF-printed high-strength metals.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Approaching the Practical Conductivity Limits of Aerosol Jet Printed Silver

Previous efforts to directly write conductive metals have been narrowly focused on nanoparticle ink suspensions that require aggressive sintering (>200°C) and result in low-density, small-grained agglomerates with electrical conductivities <25% of bulk metal. Here, we demonstrate aerosol jet printing of a reactive ink solution and characterize high-density (93%) printed silver traces having near-bulk conductivity and grain sizes greater than the electron mean free path, while only requiring low temperature (80°C) treatment. We have developed a predictive electronic transport model which correlates the microstructure to the measured conductivity and identifies a strategy to approach the practical conductivity limit for printed metals. Our analysis of how grain boundaries and tortuosity contribute to electrical resistivity provides insight into the basic materials science that governs how an ink formulator or process developer might approach improving the conductivity. Transmission line measurements validate that electrical properties are preserved up to 20GHz, which demonstrates the utility of this technique for printed RF components. Finally, this work reveals a new method of producing robust printed electronics that retain the advantages of rapid prototyping and three-dimensional fabrication while achieving the performance necessary for success within the aerospace and communications industries.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2025

Multi-Analytical Investigation of Arsenical Transfer and Remediation on Nineteenth-Century Green Books

Books containing heavy metals, specifically nineteenth-century green arsenical books, have been identified at Northwestern University Libraries, raising health and safety concerns related to handling. Copper acetoarsenite pigments, such as emerald green, were detected on book covers, decorative page edges, labels, and other components using noninvasive analytical techniques including X-ray fluorescence (XRF), Raman spectroscopy, and Fourier-transform infrared (FTIR) spectroscopy. Further examination of selected volumes using synchrotron radiation (SR) techniques revealed pigment migration, degradation, and arsenic transfer to adjacent books. This paper expands on initial findings through two related experiments. The first explored the transfer of arsenic using mechanical friction; Staedtler Mars® white vinyl erasers rubbed on arsenical books generated crumbs which were analyzed via scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM-EDX). Results confirmed the transfer of arsenic, copper, and lead, with decorative page edges being particularly prone to shedding arsenic onto other materials. The second experiment tested remediation methods on a book contaminated by prolonged exposure to an arsenical neighbor. Surface cleaning using erasers and a vacuum removed flecks of pigment but did not eliminate non-chromophoric arsenic as confirmed by SR analyses, which highlights its presence either as a degradation product embedded within the paper or present in the paper as part of its production process. Findings demonstrate the acute toxicity risk posed by arsenical books and support the need for safe handling protocols. However, materials with only trace levels of arsenic embedded during production may pose a lower risk of transfer. Cross contamination beyond prolonged direct contact appears limited. These results highlight critical considerations for library preservation practices and future research on arsenic in historical materials.

arsenic↗

DOE OSTI2024

Near-Field Nanoimaging of Colloidal Transition Metal Dichalcogenide Waveguides

Bulk transition metal dichalcogenide (TMDC) nanostructures are regarded as promising material candidates for integrated photonics due to their high refractive index at the near-infrared wavelengths. Here in this work, colloidal TMDC waveguides with tailorable dimensions are prepared by a scalable synthetic approach. The optical waveguiding properties of colloidal nanowires are studied by the near-field nanoimaging technique. In addition to dependence on thickness and wavelength, the excitonic responses and resultant waveguide modes in TMDC nanowires can be modulated by the environmental temperature. With the high-throughput production and tunable optical properties, colloidal TMDC nanowires highlight the potential for active optical components and integrated photonic devices.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Scoping Studies to ascertain the change in the phase transition temperature of metallic fuels

Microstructure evolution due to irradiation in a nuclear reactor can have a dramatic effect on material properties. A better understanding of this evolution is necessary for developing improved nuclear fuels and materials. In the current scoping study we evaluate the influence of irradiation induced defects on the recrystallization temperature of a single component fuel surrogate.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Expanding Linker Dimensionality in Metal‐organic Frameworks for sub‐Ångstrom Pore Control for Separation Applications

Abstract Metal‐organic frameworks (MOFs) are a class of porous materials with high surface areas, which are acquiring rapid attention on an exponential basis. A significant characteristic of MOFs is their ability to act as adsorbents to selectively separate component mixtures of similar size, thereby addressing the technological need for an alternative approach to conventional distillation methods. Recently, MOFs comprising a 3‐Dimensional (3D) linker have shown outstanding capabilities for difficult separations compared to the parent 2‐Dimensional (2D) analogue. 3D‐linkers with a polycyclic core are underrepresented in the MOF database due to the widespread preferred use of 2D‐linkers and the misconceived high‐cost of 3D linkers. We summarize the recent research of 3D‐linker MOFs and highlight their beneficial employment for selective gas and hydrocarbon adsorption and separation. Furthermore, we outline forecasts in this area to create a platform for widespread adoption of 3D‐linkers in MOF synthesis.

Macreadie, Lauren K.↗

DOE OSTI2023

Expanding Linker Dimensionality in Metal‐organic Frameworks for sub‐Ångstrom Pore Control for Separation Applications

Macreadie, Lauren K.↗

DOE OSTI2025

Mixed-Flux Techniques for Rational Synthesis and Structural Control in Silver Chalcogenides

The functionality of materials is intrinsically linked to their structures, an axiom encapsulated in the principle of structure-property relationships. The pinnacle of materials design is the tailoring of its structure for a specific function, which requires the ability of rational synthesis and the development of synthesis science. This idea, however, remains elusive for the synthesis of complex extended solids. A major obstacle is the difficulty in using established chemical principles selectively to control reaction paths and favor certain structural patterns over numerous other possible results. In this context, we are developing a synthesis science approach that facilitates the control of the structure and bonding to create new structures. This is achieved by employing a two-component flux consisting of mixed hydroxides and halides as the reaction medium. This enables reaction conditions that allow better control of the structure dimensionality and composition by manipulating the temperature and solvent basicity (via the flux component ratio). Here, we demonstrate the efficacy of this method in controlling their structural motifs to arrive at 23 unreported compositions and 6 unique structure types. These materials are expected to exhibit a broad range of properties, from metallic to semiconducting, with calculations suggesting the potential for emergent phenomena such as Dirac semimetals. The reaction paths afforded by these mixed fluxes establish a direct correlation between the synthetic variables and properties, providing significant insight into a broadly applicable approach for new materials.

Zhou, Xiuquan [Argonne National Laboratory (ANL), ↗