Search NASA⌕ Search

SEARCH · Search NASA

Results for “Materials synthesis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Optimal thermodynamic conditions to minimize kinetic by-products in aqueous materials synthesis

Abstract Phase diagrams offer substantial predictive power for materials synthesis by identifying the stability regions of target phases. However, thermodynamic phase diagrams do not offer explicit information regarding the kinetic competitiveness of undesired by-product phases. Here we propose a quantitative and computable thermodynamic metric to identify synthesis conditions under which the propensity to form kinetically competing by-products is minimized. We hypothesize that thermodynamic competition is minimized when the difference in free energy between a target phase and the minimal energy of all other competing phases is maximized. We validate this hypothesis for aqueous materials synthesis through two empirical approaches: first, by analysing 331 aqueous synthesis recipes text-mined from the literature; and second, by systematic experimental synthesis of LiIn(IO 3 ) 4 and LiFePO 4 across a wide range of aqueous electrochemical conditions. Our results show that even for synthesis conditions that are within the stability region of a thermodynamic Pourbaix diagram, phase-pure synthesis occurs only when thermodynamic competition with undesired phases is minimized.

Wang, Zheren (ORCID:0000000227429451)↗
DOE OSTI2023

Autonomous and dynamic precursor selection for solid-state materials synthesis

Abstract Solid-state synthesis plays an important role in the development of new materials and technologies. While in situ characterization and ab-initio computations have advanced our understanding of materials synthesis, experiments targeting new compounds often still require many different precursors and conditions to be tested. Here we introduce an algorithm (ARROWS 3 ) designed to automate the selection of optimal precursors for solid-state materials synthesis. This algorithm actively learns from experimental outcomes to determine which precursors lead to unfavorable reactions that form highly stable intermediates, preventing the target material’s formation. Based on this information, ARROWS 3 proposes new experiments using precursors it predicts to avoid such intermediates, thereby retaining a larger thermodynamic driving force to form the target. We validate this approach on three experimental datasets, containing results from over 200 synthesis procedures. In comparison to black-box optimization, ARROWS 3 identifies effective precursor sets for each target while requiring substantially fewer experimental iterations. These findings highlight the importance of domain knowledge in optimization algorithms for materials synthesis, which are critical for the development of fully autonomous research platforms.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Benchmarking large language models for materials synthesis: The case of atomic layer deposition

In this work, we introduce an open-ended question benchmark, ALDbench, to evaluate the performance of large language models (LLMs) in materials synthesis, and, in particular, in the field of atomic layer deposition, a thin film growth technique used in energy applications and microelectronics. Our benchmark comprises questions with a level of difficulty ranging from the graduate level to domain expert current with the state of the art in the field. Human experts reviewed the questions along the criteria of difficulty and specificity, and the model responses along four different criteria: overall quality, specificity, relevance, and accuracy. We ran this benchmark on an instance of OpenAI’s GPT-4o. The responses from the model received a composite quality score of 3.7 on a 1–5 scale, consistent with a passing grade. However, 36% of the questions received at least one below average score. An in-depth analysis of the responses identified at least five instances of suspected hallucination. Finally, we observed statistically significant correlations between the difficulty of the question and the quality of the response, the difficulty of the question and the relevance of the response, the specificity of the question, and the accuracy of the response as graded by the human experts. Furthermore, this emphasizes the need to evaluate LLMs across multiple criteria beyond difficulty or accuracy.

Artificial intelligence↗
DOE OSTI2024

Navigating phase diagram complexity to guide robotic inorganic materials synthesis

Abstract Efficient synthesis recipes are needed to streamline the manufacturing of complex materials and to accelerate the realization of theoretically predicted materials. Often, the solid-state synthesis of multicomponent oxides is impeded by undesired by-product phases, which can kinetically trap reactions in an incomplete non-equilibrium state. Here we report a thermodynamic strategy to navigate high-dimensional phase diagrams in search of precursors that circumvent low-energy, competing by-products, while maximizing the reaction energy to drive fast phase transformation kinetics. Using a robotic inorganic materials synthesis laboratory, we perform a large-scale experimental validation of our precursor selection principles. For a set of 35 target quaternary oxides, with chemistries representative of intercalation battery cathodes and solid-state electrolytes, our robot performs 224 reactions spanning 27 elements with 28 unique precursors, operated by 1 human experimentalist. Our predicted precursors frequently yield target materials with higher phase purity than traditional precursors. Robotic laboratories offer an exciting platform for data-driven experimental synthesis science, from which we can develop fundamental insights to guide both human and robotic chemists.

Chen, Jiadong (ORCID:0009000476038838)↗
DOE OSTI2025

Data‐Driven Insights into Rare Earth Mineralization: Machine Learning Applications Using Functional Material Synthesis Data

Understanding rare‐earth element (REE) mineralization mechanisms is essential for developing efficient separation strategies. Although the geochemical pathways that generate REE deposits are qualitatively known, quantitative links between specific conditions and mineralization outcomes remain limited. Herein, the repurpose laboratory REE hydrothermal synthesis data—originally collected for functional‐materials fabrication—as a surrogate for studying mineralization with data‐driven methods. The compiled 1,200+ hydrothermal reaction records and trained three machine‐learning models—K‐nearest neighbors (KNN), random forest (RF), and extreme gradient boosting (XGB)—to predict product elements and phases from precursors, additives, reaction conditions, and engineered features. Validation shows XGB achieves the highest accuracy. Feature importance indicates thermodynamic properties of cations and anions dominate model decisions. Correlations reveal positive relationships among precursor concentration, reaction time, pH, and temperature, consistent with classical crystallization behavior. XGB‐based regressors are built to predict crystallization temperature and pH from precursor/product attributes. Performance is strongest when similar training examples exist, while accuracy declines for underrepresented reactions, notably REE carbonates and heavy‐REE systems. Overall, the study shows that functional‐materials datasets can illuminate REE mineralization and provide priors for exploration and processing. Expanding datasets with less‐studied chemistries and conditions will improve generality and support deposit discovery and more efficient REE recovery.

feature importance analysis↗
DOE OSTI2026

Battery Material Synthesis and Scalability using a 50L Taylor Vortex Reactor (Final CRADA Report)

Under this agreement, Laminar will loan Argonne a 50L Taylor Vortex Reactor (TVR) and provide mechanical troubleshooting guidance and consulting to ensure the successful setup of the pilot-scale synthesis process. The U.S. Department of Energy (DOE) will allocate funding for the labor and materials required for the study. To evaluate the physical and electrochemical properties of the materials produced by the 50L TVR, Argonne will perform comprehensive characterizations, including XRD, SEM, PSA, ICP, tap density, and coin half-cell testing. Throughout the collaboration, Argonne will provide feedback and recommendations for mechanical improvements to the reactor system. Furthermore, Argonne will credit Laminar as a collaborator in any presentations or publications resulting from data generated by the system. Laminar will retain no rights to experimental results or intellectual property generated through the experiments conducted with the 50L TVR at Argonne.

25 ENERGY STORAGE↗
DOE OSTI2026

A technoeconomic analysis of poly- and single-crystalline NMCxyz from material synthesis to battery pack design

A process model was developed for estimating the cost of manufacturing lithium nickel manganese cobalt oxide (LiNi x Mn y Co z O 2 , NMCxyz), the main cathode active material in lithium-ion batteries used for electric vehicles in the United States. The model was used to estimate the prices of NMC622, NMC811, and NMC955 with poly- and single-crystalline morphologies. The Battery Performance and Cost Model (BatPaC) was used to translate the NMC prices into battery pack prices. A decrease in cobalt content from NMC622 (20% Co) to NMC955 (5% Ni) decreases the material price by $\$$0.85/kg (−3%) due to a decrease in the cost of battery materials, which account for >60% of the total price. NMC622 only produce cheaper packs if the nickel sulfate cost is > 4 × its baseline, indicating higher nickel materials will lower pack cost under normal market conditions. Single-crystalline materials are $\$$2/kg (+8%) more expensive than their polycrystalline counterparts due to higher manufacturing costs from longer, hotter calcinations in less densely packed saggars. This increases the pack price by ∼$\$$3/kWh, assuming identical electrochemical properties. In conclusion, the single-crystalline materials could yield cheaper packs if cycled to higher upper cutoff voltages (i.e., 4.35 to 4.43 V for the single-crystalline material vs. 4.25 V for their polycrystalline counterparts).

Cost modeling↗
DOE OSTI2025

Autonomous Synthesis of Metastable Materials Using a Modular Mixed-Flow Reactor

Understanding and controlling atomic-level processes at solid-liquid interfaces is key to advancing technologies in energy storage, carbon capture, critical element recovery, and materials synthesis. Many of these processes are dominated by the formation of short-lived intermediate precipitates that determine the final properties of synthesized materials. However, studying these intermediates is challenging due to their sensitivity and the reliance on trial-and-error methods. To address this, we developed an automated variable-volume mixed-flow reactor (MFR) to optimize metastable material synthesis and investigate rapid kinetic processes. This state-of-the-art MFR system, paired with an automated modeling framework, enables efficient synthesis and real-time analysis of transient phases. Benchmarking with advanced capabilities, such as wide-/small-angle X-ray scattering, allows us to resolve fast nucleation and growth dynamics that were previously inaccessible. By combining automation, ML-guided optimization, and tailored kinetic modeling, this approach provides a robust platform for improving material design and achieving precise control over solid-liquid reactions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Advancing microelectronics through nanoscale science: A perspective on needs and opportunities from the nanoscale science research centers

Microelectronics are the cornerstone of the modern world, enhancing our daily lives by providing services such as communications and datacenters. These resources are accessible thanks to the continual pursuit of a deeper understanding of the chemical and physical phenomena underlying the materials synthesis approaches and fabrication processes used to create microelectronic components and subsequently the components' responses to electrical, optical, and other stimuli that are utilized within microelectronic systems. Today, further development of microelectronics requires multidisciplinary expertise across scientific disciplines and fields of study—synthesis, materials characterization, nanoscale fabrication, and performance characterization—with focus placed on comprehending the nanoscale forms and features of microelectronic components. The Nanoscale Science Research Centers (NSRCs) are Department of Energy, Office of Science user facilities that support the international scientific community in advancing nanoscale science and technology. As a key component of the U.S. Government's National Nanotechnology Initiative, the NSRCs enable transformative discoveries by providing world-class facilities, expertise, and collaborative opportunities. Here, in this perspective, we showcase a non-exhaustive cross-section of the capabilities housed at and developed by the NSRCs and their user communities to address fundamental synthesis, metrology, fabrication, and performance considerations toward advancing the development of new microelectronics. Finally, we provide a timely outlook on the next major areas of necessary development in nanoscale sciences to continue the innovation of microelectronics into the next generation.

2D materials↗
DOE OSTI2024

Elucidating the mechanical and thermal response of nanotwinned Ni alloys

Transformative advances in nanoscale materials synthesis, characterization and modeling are enabling the synthesis of materials with unprecedent properties and greater understanding of the nanoscale mechanisms that underpin these properties. Nanotwinned Cu alloys have received considerable attention due to their impressive balance of strength and ductility, but they have limited microstructural stability. Recent instantiation of nanotwins in sputter deposited Ni-Mo-W, and several commercial Ni-based superalloys, point to the potential development of a new class of high temperature materials with a very beneficial suite of mechanical and physical properties. The experimental study described in this report was undertaken to elucidate the nanoscale origins of the thermal and mechanical behavior of nanotwinned Ni alloys. Micropillar compression experiments have shown nanotwinned Ni 85 Mo 15-x W x alloys to possess unusually high strengths above 3.5GPa and enhanced microstructural stability. The strength of these nanotwinned alloys is determined by the abrupt formation of shear bands. This study focused on identifying the nanoscale trigger, or triggers, for shear banding in nanotwinned materials using in situ experiments and atomic-scale postmortem analysis. Contrasting and comparing the mechanical response and postmortem nanostructures of “Mo-rich” and “W-rich” nanotwinned specimens elucidated the importance of the lateral motion of easy glide defects that results in erasure of twins and local coarsening of the nanotwinned microstructure. This twin coarsening was then associated with very localized plasticity, strain softening, and shear band formation. The difference between alloys was further studied by considering the role of various material factors: stacking fault energy, coherent twin boundary spacing and flatness, grain size, and the interactions of solute atoms with twin and grain boundaries. The effect of alloy composition and sputtering power and temperature were also investigated and used to control twin spacing and geometry. Combined with atomic-scale simulations, these experiments insights should allow us to identify strategies for achieving concomitant ultrahigh strength and ductility in nanotwinned Ni alloys. In parallel but synergistic studies, our work was buoyed by collaborative state-of-the-art nanoscale orientation and strain mapping at the DOE National Center for Electron Microscopy (NCEM). For example, novel 4D-STEM techniques were used to acquire nanoscale strain maps. The extremely fine twin spacing limited our measurements of atomic-scale thermal expansion within twins, but recent results from NCEM suggest that it will soon be possible to conduct such measurements and to unravel the origins of the novel thermal expansion characteristics of nanotwinned Ni alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2024

High-temperature thermal imaging to inform the arc-melt synthesis of nuclear materials

The advancement of nuclear energy technology necessitates the development of novel materials and synthesis methods to produce materials which enable new fuel cycles. Alongside the maturation of R&D scale technologies to produce these materials, there is an ongoing effort to develop in situ monitoring capabilities to reduce the time to the discovery and development of these fuels. Monitoring data can be leveraged in artificial intelligence platforms to detect phenomena which lead to varied macro- and microstructural features which impact the application and performance of samples synthesized. The present study presents early-stage findings of the implementation of high-temperature, high-frame-rate infrared thermal imaging to monitor the arc-melt synthesis of novel fuels and compounds relevant to advanced nuclear reactors. The study illustrates both the challenges and opportunities of this methodology, highlighting the importance of internal standards while determining emissivity and transmission values as well as visualizing volatilization during melt synthesis.

Stone, Jordan↗
NASA NTRS1996

The VTLA System of Course Delivery and Faculty Development in Materials Education

There is a national need for high-quality, upper division courses that address critical topics in materials synthesis, particularly those beyond the present expertise of the typical university department's faculty. A new project has been started to test a novel distance education and faculty development system, called Video Tape Live Audio (VTLA). This, if successful, would at once enlarge the national Materials Science and Engineering (MSE) student cohort studying material synthesis and develop faculty expertise at the receiving sites. The mechanics for the VTLA scheme are as follows: A course is designed in the field selected for emphasis and for which there is likely to be considerable demand, in this example 'Ceramic Materials Synthesis: Theory and Case Studies'. One of the very best researcher/teachers records lectures of TV studio quality with appropriate visuals. Universities and colleges which wish to offer the course agree to offer it at the same hour at least once a week. The videotaped lectures and accompanying text, readings and visuals are shipped to the professor in charge, who has an appropriate background. The professor arranges the classroom TV presentation equipment and supervises the course. Video lectures are played during regular course hours twice a week with time for discussion by the supervising professor. Typically the third weekly classroom period is scheduled by all sites at a common designated hour, during which the course author/presenter answers questions, provides greater depth, etc. on a live audio link to all course sites. Questions are submitted by fax and e-mail prior to the audio tutorial. coordinating professors at various sites have separate audio teleconferences at the beginning and end of the course, dealing with the philosophical and pedagogical approach to the course, content and mechanics. Following service once or twice as an 'apprentice' to the course, the coordinating professors may then offer it without the necessity of the live audio tutorial.

Berrettini, Robert↗
NASA NTRS2000

Gravitational Effects on Combustion Synthesis of Advanced Porous Materials

Combustion Synthesis (self-Propagating high-temperature synthesis-(SHS)) of porous Ti-TiB(x), composite materials has been studied with respect to the sensitivity to the SHS reaction parameters of stoichiometry, green density, gasifying agents, ambient pressure, diluents and gravity. The main objective of this research program is to engineer the required porosity and mechanical properties into the composite materials to meet the requirements of a consumer, such as for the application of bone replacement materials. Gravity serves to restrict the gas expansion and the liquid movement during SHS reaction. As a result, gravitational forces affect the microstructure and properties of the SHS products. Reacting these SHS systems in low gravity in the KC-135 aircraft has extended the ability to form porous products. This paper will emphasize the effects of gravity (low g, 1g and 2g) on the SHS reaction process, and the microstructure and properties of the porous composite. Some of biomedical results are also discussed.

Zhang, X.↗