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At least 487 records · Page 27
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Pilot Testing of a Highly Efficient Pre-combustion Sorbent-based Carbon Capture System

TDA developed and demonstrated a highly efficient pre-combustion carbon capture system. The overall objective of this work was to develop a new sorbent-based pre-combustion carbon capture technology for Integrated Gasification Combined Cycle (IGCC) power plants. In this project our goal was to demonstrate the techno-economic viability of the new technology by 1) demonstrating it in large-scale slipstream tests, and 2) carrying out a high fidelity engineering and cost analysis. TDA’s process used an advanced physical adsorbent that selectively removes CO 2 from coal-derived synthesis gas above the dew point of the gas at temperatures as high as 300°C. The sorbent consists of a mesoporous carbon whose surface was grafted with functional groups that remove CO 2 via a well-known acid-base interaction. As documented in bench-scale experiments and field tests with actual coal gas, the sorbent achieved a very high capacity for CO 2 at temperatures as high as 300°C. The sorbent bound CO 2 more strongly than common physical adsorbents, providing the chemical potential needed for the high temperature operation. However, because CO 2 does not form a true covalent bond with the surface sites (as is the case with chemical absorbents), the sorbent regeneration could be carried out with only a very small energy input. The heat input to regenerate our sorbent was only 4.9 kcal per mol of CO 2 , which is much lower than that for chemical absorbents (e.g., 29.9 kcal/mol CO 2 for sodium carbonate) and was similar to the requirements of physical solvents (e.g., 4 kcal/mol CO 2 for Selexol TM ). Because the sorbent operates above the dew point of the synthesis gas (unlike the Selexol TM process), a higher power cycle efficiency can be achieved. With previous DOE/NETL funding (Contract No. DE-FE-0000469), we demonstrated the techno-economic viability of the technology in bench-scale tests and slipstream demonstrations at the National Carbon Capture Center (NCCC), Wilsonville, Alabama and Wabash River IGCC plant in Terra Haute, Indiana. We demonstrated a stable working CO 2 capacity for over 11,650 cycles with simulated synthesis gas. We also evaluated its performance with actual synthesis gas in two test campaigns at the Wabash River IGCC Plant, Terre Haute, IN and the National Carbon Capture Center (NCCC), Wilsonville, AL. The slipstream tests clearly showed that the actual coal gas constituents and potential contaminants (e.g. trace metals, halides, tars) had no effect on the sorbent’s ability to remove CO 2 (the same sorbent beds were used in both field tests with no sign of deactivation for 2,000 cycles with over 26,750 SCF of gas treated). As expected, due to the high temperature CO 2 removal capability and low energy needed to regenerate the sorbent, the power cycle efficiency with our process was greater than 34% on a higher heating value (HHV) basis; in comparison, the same IGCC plant equipped with the Selexol TM solvent for carbon capture can only achieve 31.4% HHV efficiency. The capital cost for an IGCC system with TDA’s process is estimated as $2,417/kW e , which is 12% lower than that of the IGCC/ Selexol TM process. The levelized cost for electricity including the transport, storage and monitoring (TS&M) cost for CO 2 was calculated as $\$ $92.9/MWh (lowest reported to our knowledge), which is much better than the $105.2/MWh estimated for the IGCC/ Selexol TM process. In this project (DE-FE0013105), TDA Research, in collaboration with our partners Gas Technology Institute (GTI), Illinois Clean Coal Institute (ICCI), University of California, Irvine (UCI), University of Alberta (UOA), Siemens, NCCC and Sinopec advanced the technical maturity of the technology; scaling it up by a factor of 100. We optimized the reactor design using computational fluid dynamics (CFD); using adsorption modeling we improved the pressure swing adsorption (PSA) cycle sequence. We carried out two field test campaigns with a fully-equipped 0.1 MW e prototype unit (for a total of 844 hours) using actual synthesis gas to prove the viability of the new technology. A successful 30 day (707 hrs) evaluation was completed at NCCC under air blown gasification conditions. We demonstrated 97.3% carbon capture at 1,500 SLPM, 93% carbon capture at 1,800 SLPM, and 90% carbon capture at 2,100 SLPM in the NCCC tests. We also demonstrated the system for 137 hours at a Sinopec petrochemical plant under oxygen blown gasification, demonstrating 86% carbon capture at 2,660 SLPM. In collaboration with University of California, Irvine (UCI), we completed a techno-economic analysis (TEA) for TDA’s warm gas cleanup technology integrated to IGCC power plant. The net plant efficiencies (on a coal HHV basis) for the warm gas cleanup cases were estimated to be 34.0% for E-GasTM gasifier, 34.4% for GE gasifier, 33.4 for the Shell gasifier and 34.2 for the TRIG TM gasifier (Cases 2, 4, 6 and 8 in this study) with a catalytic combustor for CO 2 purification, which are significantly higher than those for the Cold Gas Case, or an increase of as much as 12% in the heat rate for Case 2, 6% for Case 4, 9% for Case 6, and 9% for Case 8. The 1st year cost of electricity with the transport, storage and monitoring (TS&M) costs for the CO 2 included was $\$ $129.2/MWh for the E-GasTM gasifier Warm Gas Cleanup Case, $\$ $131.9/MWh for the GE gasifier Warm Gas Cleanup Case, $\$ $146.8/MWh for the Shell Gasifier Warm Gas Cleanup Case, and $\$ $129.9/MWh for the TRIG TM gasifier Warm Gas Cleanup Case. For comparison, the costs for the baseline Cold Gas CO 2 removal with Selexol for the different gasifiers were: $\$ $146.6/MWh for the E-Gas TM gasifier, $\$ $142.2/MWh for the GE gasifier, $\$ $159.0/MWh for the Shell gasifier and $\$ $144.3/MWh for the TRIG TM gasifier. In summary, the costs for our system were 7 to 12% lower than the corresponding Cold Gas Cleanup cases. The results of this techno-economic analysis suggested that TDA’s high temperature PSA-based Warm Gas Clean-up Technology can make a substantial improvement in the IGCC plant thermal performance for achieving near zero CO 2 emissions for E-Gas TM , GE, Shell and TRIG TM gasifier based IGCC power plants. The capital expenses were estimated to be lower than that of Selexol’s™. Taken together, the higher net plant efficiency and lower capital and operating costs resulted in substantial reduction in the cost of carbon capture for the IGCC plant equipped with TDA’s high temperature PSA-based carbon capture system. Finally, in collaboration with Gas Technology Institute (GTI) we completed the environmental health and safety assessment for TDA’s warm gas carbon capture technology.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2025

Sieving Hydrogen Isotopes via Machine Learning Assisted Chemical Vapor Deposition (CVD) of High‐Quality Monolayer Hexagonal Boron Nitride (h‐BN) on Iron Foils

Atomically thin two-dimensional (2D) ceramics, such as monolayer hexagonal boron nitride (h-BN), present potential for disruptive advances in separations. However, sub-atomic scale separation of hydrogen isotopes (H + /D + ) require near pristine 2D material membranes, and scalable synthesis of such high-quality h-BN comparable to mechanically exfoliated crystals remains a significant challenge. Here, we report a scalable Fe-catalyzed chemical vapor deposition (CVD) process for bottom-up synthesis of large-area, high-quality monolayer h-BN films, overcoming key limitations of conventional ammonia-based routes. By leveraging mechanistic insights and higher CVD temperatures, we suppress multilayer formation and achieve uniform monolayer h-BN coverage on commercially available Fe foils. Machine learning enables systematic exploration of the complex, multi-dimensional CVD parameter space (growth time, temperature, precursor temperature, multilayer faction, coverage), providing data-driven approaches to visualize and identify process regimes facilitating predominantly monolayer h-BN growth with minimal secondary nuclei/ad-layers. The optimized Fe-catalyzed CVD h-BN membranes show high-quality as observed by proton/deuteron (H + /D + ) selectivity ≈8.45, approaching the highest quality benchmark of mechanically exfoliated h-BN (H + /D + selectivity ≈10) as well as significantly outperforming Cu-catalyzed CVD h-BN membranes (H + /D + selectivity ≈3.62, control selectivity ≈1.7). Our work provides a scalable cost-effective route for high-quality monolayer h-BN synthesis for sub-atomic scale separations (H + /D + ) and demonstrates the broader potential of machine learning-guided optimization of CVD for advancing synthesis of 2D materials.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Simultaneously upgrading CO 2 and light alkanes into value-added products

We will discuss recent results from our group in reacting CO 2 and light alkanes to produce syngas, olefins, aromatics, and oxygenates. We will mainly use the simultaneous upgrading of CO 2 and ethane (SU-CO 2 Et) as examples to demonstrate the feasibility and reaction pathways of these processes. We will briefly discuss synthesis methods and essential structural characterization techniques that can be applied to SU-CO 2 Et catalysts. We will then illustrate how to identify and apply distinct active sites for different upgrading processes, using a combination of kinetic studies, in situ characterization, and density functional theory (DFT) calculations. We will conclude the Perspective by pointing out challenges and potential directions in catalyst design and synthesis, as well as structural characterization and mechanistic investigations, to further advance the simultaneous upgrading of CO 2 and light alkanes.

03 NATURAL GAS↗
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 OSTI2021

Recent advances in CO 2 hydrogenation to value-added products — Current challenges and future directions

Climate change, global warming, fossil fuel depletion and rising fuel prices have created great incentives to seek alternative fuel production technologies. CO 2 transformation to value-added products using renewable H 2 has proven to be an emerging solution to enable this goal. In this regard, three different promising processes, namely methane, methanol and hydrocarbon synthesis via CO 2 hydrogenation are thoroughly discussed. In addition, the influential factors affecting process efficiencies such as catalyst design and mechanistic insight, operating conditions as well as reactor types are investigated, with key pathways that dictate catalyst activity and selectivity of the most promising materials described. Furthermore, a brief overview of the reactor configuration and its crucial role in the improving process viability is analyzed. Accordingly, fixed-bed, fluidized-bed, annular and spherical reactors along with H 2 O/H 2 perm-selective membrane reactors are disscussed for hydrocarbon production. In addition, different reactor configurations are compared to assess the best one that is adjustable depending on the reaction mechanism. In conclusion, a corrugated-wall dual-type membrane reactor is proposed as an emerging alternative for CO 2 hydrogenation to value-added products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Wafer-Scale Synthesis of 2D Materials by an Amorphous Phase-Mediated Crystallization Approach

The interest in the wafer-scale growth of two-dimensional (2D) materials, including transition metal dichalcogenides (TMDCs), has been rising for transitioning from lab-scale devices to commercial-scale systems. Among various synthesis techniques, physical vapor deposition, such as pulsed laser deposition (PLD), has shown promise for the wafer-scale growth of 2D materials. However, due to the high volatility of chalcogen atoms (e.g., S and Se), films deposited by PLD usually suffer from a lack of stoichiometry and chalcogen deficiency. To mitigate this issue, excess chalcogen is necessary during the deposition, which results in problems like uniformity or not being repeatable. This study demonstrates a condensed-phase or amorphous phase-mediated crystallization (APMC) approach for the wafer-scale synthesis of 2D materials. This method uses a room-temperature PLD process for the deposition and formation of amorphous precursors with controlled thicknesses, followed by a post-deposition crystallization process to convert the amorphous materials to crystalline structures. This approach maintains the stoichiometry of the deposited materials throughout the deposition and crystallization process and enables the large-scale synthesis of crystalline 2D materials (e.g., MoS 2 and WSe 2 ) on Si/SiO 2 substrates, which is critical for future wafer-scale electronics. We show that the thickness of the layers can be digitally controlled by the number of laser pulses during the PLD phase. Optical spectroscopy is used to monitor the crystallization dynamics of amorphous layers as a function of annealing temperature. The crystalline quality, domain sizes, and the number of layers were explored using nanoscale and atomistic characterization (e.g., AFM, STEM, and EDS) along with electrical characterization to explore process–structure–performance relationships. Finally, this growth technique is a promising method that could potentially be adopted in conventional semiconductor industries for wafer-scale manufacturing of next-generation electronic and optoelectronic devices.

2D electronics↗
DOE OSTI2022

Phase controlled synthesis of transition metal carbide nanocrystals by ultrafast flash Joule heating

Nanoscale carbides enhance ultra-strong ceramics and show activity as high-performance catalysts. Traditional lengthy carburization methods for carbide syntheses usually result in coked surface, large particle size, and uncontrolled phase. Here, a flash Joule heating process is developed for ultrafast synthesis of carbide nanocrystals within 1 s. Various interstitial transition metal carbides (TiC, ZrC, HfC, VC, NbC, TaC, Cr 2 C 3 , MoC, and W 2 C) and covalent carbides (B 4 C and SiC) are produced using low-cost precursors. By controlling pulse voltages, phase-pure molybdenum carbides including β-Mo 2 C and metastable α-MoC 1-x and η-MoC 1-x are selectively synthesized, demonstrating the excellent phase engineering ability of the flash Joule heating by broadly tunable energy input that can exceed 3000 K coupled with kinetically controlled ultrafast cooling (>10 4 K s –1 ). Theoretical calculation reveals carbon vacancies as the driving factor for topotactic transition of carbide phases. The phase-dependent hydrogen evolution capability of molybdenum carbides is investigated with β-Mo 2 C showing the best performance.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2021

Solution-processable and functionalizable ultra-high molecular weight polymers via topochemical synthesis

Abstract Topochemical polymerization reactions hold the promise of producing ultra-high molecular weight crystalline polymers. However, the totality of topochemical polymerization reactions has failed to produce ultra-high molecular weight polymers that are both soluble and display variable functionality, which are restrained by the crystal-packing and reactivity requirements on their respective monomers in the solid state. Herein, we demonstrate the topochemical polymerization reaction of a family of para -azaquinodimethane compounds that undergo facile visible light and thermally initiated polymerization in the solid state, allowing for the first determination of a topochemical polymer crystal structure resolved via the cryoelectron microscopy technique of microcrystal electron diffraction. The topochemical polymerization reaction also displays excellent functional group tolerance, accommodating both solubilizing side chains and reactive groups that allow for post-polymerization functionalization. The thus-produced soluble ultra-high molecular weight polymers display superior capacitive energy storage properties. This study overcomes several synthetic and characterization challenges amongst topochemical polymerization reactions, representing a critical step toward their broader application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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 OSTI2021

Microwave-enhanced catalytic ammonia synthesis under moderate pressure and temperature

In this study, an alternative approach based on microwave-enhanced ammonia synthesis for Haber-Bosch process was carried out under moderate pressure of 0.1–0.65 MPa and temperature range of 280–400 °C over a stable CsRu/CeO 2 catalyst. The ammonia production rate is significantly improved under microwave conditions. At 0.65 MPa and 320 °C, maximum ammonia production rate was achieved at H 2 /N 2 ratio of 1/1. Stable performance was obtained in a 6-cycles of startup-shutdown operation for cumulative on-line time of 80 h. The work demonstrates the potential of microwave catalytic technology for the distributed ammonia synthesis using renewable power having intermittent nature of energy supply.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Methods and algorithms for computer synthesis of holographic elements to obtain a complex impulse response of optical information processing systems based on modern spatial light modulators

The possibilities of designing optical devices for data processing and imaging based on the manipulation of coherent light beams by means of spatial light modulators (SLMs) are investigated. A review of commercially available SLMs is presented and the limitations of their complex modulation characteristics are analysed. The main problem of using present-day SLMs is the lack of the ability to modulate directly all states within a unit circle in the complex plane. In this regard, the characteristics of current methods for the synthesis of holographic elements are described that implement a given complex impulse response of the optical system and are optimal for using SLMs with purely amplitude, purely phase, and hybrid amplitude – phase modulation. (paper)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

Flame aerosol synthesis of hollow alumina nanoshells for application in thermal insulation

Commercial implementation of hollow nanoshell materials is often limited by difficult scale-up and high cost. Here we present a scalable, continuous, and potentially low-cost route to hollow nanostructured materials using a High Temperature Reducing Jet flame aerosol reactor. The key advantage of this process over traditional flame aerosol synthesis methods is separation of flame chemistry and particle formation, which allows production of hollow nanoshells from an aqueous salt solution without any template or surfactant. We produced amorphous hollow alumina with an average diameter of 181 nm and shell thickness below 10 nm, and demonstrated the generality of the method by also producing hollow SiO 2 , ZrO 2 , Ga 2 O 3 , and Co 2 O 3 . We characterized the morphology, phase transition, thermal stability, and thermal conductivity of the flame-made hollow alumina by electron microscopy, x-ray diffraction, and thermal analysis methods. As a prototypical application, we incorporated hollow alumina into thermal insulation, combining it with common fiberglass insulation to reduce the thermal conductivity by 30% relative to pure fiberglass, to 0.028 W m -1 K -1 while maintaining robust fire-resistance and elasticity.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Ligand-Guided Growth of Alloyed Shells on Intermetallic Seeds as a Route toward Multimetallic Nanocatalysts with Shape-Control

In this work, shape-controlled core@shell PdCu@PtCu nanoparticles (NPs) were synthesized by seed-mediated co-reduction. Specifically, cubic-shaped NPs were achieved by selecting tetraoctylammonium bromide (TOAB) and triphenylphosphine (TPP) as capping ligands. Their roles were investigated by incorporating independently each ligand into the reaction and analyzing the products by transmission electron microscopy (TEM). This analysis revealed that the quasi-spherical PdCu seeds acquired cubic shapes during the synthesis and directed shell deposition. This process was mediated by TPP, which was central to achieving monodisperse NPs with shape-control. The synthesis conditions were modified to tune both the thickness and composition of the shells. Evaluation of the NPs as catalysts for the electrooxidation of formic acid found that the NPs with the thinnest Pt-rich shells gave the highest specific activity, with the nanocubic shape also enhancing performance with respect to the spherical counterpart. These results highlight the benefits of integrating compositional, architectural, and shape-control all in one NP construct.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Scaling-Up and Roll-to-Roll Processing if Highly Conductive Sulfide Solid-State Electrolytes (CRADA 510)

This project aims to identify and address key technical barriers in scale-up synthesis and roll-to-roll processing of highly conductive solid-state electrolytes (SSEs) by leveraging PNNL’s patent pending SSEs, Ampcera Inc.’s environmentally friendly manufacturing capability, and UW’s rollto-roll processing. The ultimate goals are 1) development of novel sulfide SSEs with room temperature Li+ conductivity > 5 mS/cm and Li/SSE interfacial resistance <5 Ωcm2, 2) scalable production of sulfide SSEs at 1 metric ton/year, and 3) a high throughput roll-to-roll processing of highly conductive (>1 mS/cm) and ultra-thin solid film (10-100 μm). The materials and the solid film achieved in the project will be tested at practical conditions and validated in a realistic pouch cell format with achievable energy > 300 Wh/Kg.

36 MATERIALS SCIENCE↗
DOE OSTI2025

ARCS: Agentic Retrieval-Augmented Code Synthesis with Iterative Refinement

Agentic Retrieval-Augmented Code Synthesis with Iterative RefinementIn supercomputing, efficient and optimized code generation is essential to leverage high-performance systems effectively. We have developed Agentic Retrieval-Augmented Code Synthesis (ARCS), an advanced framework for accurate, robust, and efficient code generation, completion, and translation. ARCS integrates Retrieval-Augmented Generation (RAG) with Chain-of-Thought (CoT) reasoning to systematically break down and iteratively refine complex programming tasks. An agent-based RAG mechanism retrieves relevant code snippets, while real-time execution feedback drives the synthesis of candidate solutions. This process is formalized as a state-action search tree optimization, balancing code correctness with editing efficiency. Evaluations on the Geeks4Geeks and HumanEval benchmarks demonstrate that ARCS significantly outperforms traditional prompting methods in translation and generation quality. By enabling scalable and precise code synthesis, ARCS offers transformative potential for automating and optimizing code development in supercomputing applications, enhancing computational resource utilization

Bhattarai, Manish [Los Alamos National Labs]↗
DOE OSTI2022

Dataset of solution-based inorganic materials synthesis procedures extracted from the scientific literature

The development of a materials synthesis route is usually based on heuristics and experience. A possible new approach would be to apply data-driven approaches to learn the patterns of synthesis from past experience and use them to predict the syntheses of novel materials. However, this route is impeded by the lack of a large-scale database of synthesis formulations. In this work, we applied advanced machine learning and natural language processing techniques to construct a dataset of 35,675 solution-based synthesis procedures extracted from the scientific literature. Each procedure contains essential synthesis information including the precursors and target materials, their quantities, and the synthesis actions and corresponding attributes. Every procedure is also augmented with the reaction formula. Through this work, we are making freely available the first large dataset of solution-based inorganic materials synthesis procedures.

36 MATERIALS SCIENCE↗