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At least 271 records · Page 15

Forward and reverse transfer function model synthesis

A process for synthesizing a mathematical model for a linear mechanical system using the forward and reverse Fourier transform functions is described. The differential equation for a system model is given. The Bode conversion of the differential equation, and the frequency and time-domain optimization matching of the model to the forward and reverse transform functions using the geometric simplex method of Nelder and Mead (1965) are examined. The effect of the window function on the linear mechanical system is analyzed. The model is applied to two examples; in one the signal damps down before the end of the time window and in the second the signal has significant energy at the end of the time window.

Houghton, J. R.↗

Lithium metal recovery and synthesis

A process and system for creating a lithium ion anolyte from lithium alloys. Metal and lithium alloys are processed to remove the metal with lithium from the alloy remaining. A lithium ion anolyte formed may be used in a process to form lithium metal. Alternatively, a process and system for recovering lithium from sources such as lithium alloys and lithium metal oxides and other feedstock such as recycled batteries into a thin lithium metal film via electrodeposition in an organic electrolyte contacting both anode (holder for lithium source) and cathode (substrate for lithium deposition) in a single-compartment electrolysis cell.

Ignacio de Leon, Patricia Anne↗

Synthesis and characterization of polylactic acid microspheres via emulsion-based processing

Polylactic acid (PLA) microspheres are primarily used in drug delivery applications and rarely manufactured commercially. In encapsulation, the drug encapsulation and microsphere synthesis process happen simultaneously. Simultaneous synthesis necessitates conditions that ensure the drugs to be encapsulated remain viable in the synthesis process. Here, in the present work, solid pure PLA microspheres are prepared using a repeatable centrifugal mixing method to create a single emulsion system. A planetary thinky mixer is used to achieve centrifugal mixing. PLA acts as the dispersed phase of the emulsion, whereas Polyvinyl alcohol (emulsifier) dissolved in deionized water serves as the bulk phase. The emulsions are stirred for about 4 min at 2000 rpm. Microspheres prepared by mechanical mixing are compared with microspheres prepared by centrifugal mixing. The microspheres prepared by centrifugal mixing proved to be narrower and closer to a normal distribution with a mean size (D x 50) of 30 microns. The size distribution of planetary mixed microspheres did not change from one batch to another.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Lignin Derived Ionic Liquids: Synthesis and Application for Biopolymer Processing (CRADA Final Report)

We have established a scalable and economically viable process to convert lignin into ionic liquids for use in biopolymer processing. We have studied the four main topics: 1) lignin depolymerization to produce vanillin through oxidation, 2) lignin reduction to produce guaiacols, 3) oxidation process scale up, and 4) ionic liquid synthesis and application for biopolymer processing. The main accomplishment is summarized below: A maximal vanillin yield of 4.9% (8.8% total product yield) was achieved under optimal oxidation conditions using design of experiments (DOE); Aminophenol with 94.5% purity was synthesized via reductive amination using vanillin isolated from ion-exchange chromatography; At a higher lignin loading (10%), the vanillin yield in the scale up reaction was lower than the bench scale reaction; The filtration-based downstream separation of the scale-up process was able to recover 76% of vanillin; A maximal lignin reduction product (guaiacols) yield of 6.5% was achieved in the presence of Ru/C, formic acid, and methanol; The lignin reduction product yield and composition were affected by the use of different solvent and catalytic reagents (methanol in combination of Ru/C and formic acid gives the highest product yield); Lignin oxidation and reduction products: vanillin, acetovanillone, guaiacols, and eugenol are successfully used for IL synthesis; XX based ILs showed cellulose solubility with up to xx%; Technoeconomic analysis results indicate the potential of producing affordable ILs from kraft lignin (MSP: $14/kg); Life-cycle assessment results show the potential to reduce GHG emissions by up to 85% relative to existing ILs ([Ch][Lys]) with GHG emission: 1.2 kg CO 2e /kg of IL produced.

09 BIOMASS FUELS↗

Polyphenylquinoxalines Via Aromatic Nucleophilic Displacement

Process for synthesis of polyphenylquinoxalines (PPQ's) involves nucleophilic displacement reactions of di(hydroxyphenyl) quinoxaline monomers with activated aromatic dihalides. New process costs less than other processes for synthesis of PPQ's. Facilitates synthesis of PPQ's of new and varied molecular structures. Useful as adhesives, coatings, films, membranes, and matrices for composites.

Hergenrother, Paul M.↗

Sol-Gel Synthesis Of Aluminoborosilicate Powders

Application of sol-gel process to synthesis of aluminoborosilicate powders shows potential for control of microstructures of materials. Development of materials having enhanced processing characteristics prove advantageous in extending high-temperature endurance of fibrous refractory composite insulation made from ceramic fibers.

Bull, Jeffrey↗

Irreversible Multielement Diffusion and the Resulting Compositional and Processing Flexibility in the Synthesis and Densification of Lithium Aluminum Lanthanum Zirconium Oxide

Despite the broad interest in Al-doped lithium lanthanum zirconium oxide (LLZO), the wide range of reported ionic conductivities suggests that the effect of processing parameters on the resulting phase purity and bulk conductivity is not well-understood. Here, in this work, we synthesized six separate series of LLZO with variations in Al concentration, Li excess, Li addition order, Li source, densification method, and mother powder to determine the effect on the composition, phase purity, density, and bulk conductivity. We found that a wider range of compositions (6.08–7.61 mol of Li and 0.06–0.23 mol of Al) than previously reported can result in cubic phase stability and that nearly all elements (Li, Al, Zr, and La) are lost to the MgO crucible during calcination and sintering. The manner in which different elements are lost is affected by the processing parameters. We observed that Al-doped LLZO shows great compositional flexibility in stabilizing the cubic phase, offering an explanation for the range of electrochemical performance metrics reported in the literature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A Case Study of Multimodal, Multi-institutional Data Management for the Combinatorial Materials Science Community

Although the convergence of high-performance computing, automation, and machine learning has significantly altered the materials design timeline, transformative advances in functional materials and acceleration of their design will require addressing the deficiencies that currently exist in materials informatics, particularly a lack of standardized experimental data management. The challenges associated with experimental data management are especially true for combinatorial materials science, where advancements in automation of experimental workflows have produced datasets that are often too large and too complex for human reasoning. The data management challenge is further compounded by the multimodal and multi-institutional nature of these datasets, as they tend to be distributed across multiple institutions and can vary substantially in format, size, and content. Furthermore, modern materials engineering requires the tuning of not only composition but also of phase and microstructure to elucidate processing–structure–property–performance relationships. To adequately map a materials design space from such datasets, an ideal materials data infrastructure would contain data and metadata describing (i) synthesis and processing conditions, (ii) characterization results, and (iii) property and performance measurements. In this work, we present a case study for the low-barrier development of such a dashboard that enables standardized organization, analysis, and visualization of a large data lake consisting of combinatorial datasets of synthesis and processing conditions, X-ray diffraction patterns, and materials property measurements generated at several different institutions. While this dashboard was developed specifically for data-driven thermoelectric materials discovery, we envision the adaptation of this prototype to other materials applications, and, more ambitiously, future integration into an all-encompassing materials data management infrastructure.

36 MATERIALS SCIENCE↗

Controllable Thin‐Film Approaches for Doping and Alloying Transition Metal Dichalcogenides Monolayers

Abstract Two‐dimensional (2D) transition metal dichalcogenides (TMDs) exhibit exciting properties and versatile material chemistry that are promising for device miniaturization, energy, quantum information science, and optoelectronics. Their outstanding structural stability permits the introduction of various foreign dopants that can modulate their optical and electronic properties and induce phase transitions, thereby adding new functionalities such as magnetism, ferroelectricity, and quantum states. To accelerate their technological readiness, it is essential to develop controllable synthesis and processing techniques to precisely engineer the compositions and phases of 2D TMDs. While most reviews emphasize properties and applications of doped TMDs, here, recent progress on thin‐film synthesis and processing techniques that show excellent controllability for substitutional doping of 2D TMDs are reported. These techniques are categorized into bottom–up methods that grow doped samples on substrates directly and top–down methods that use energetic sources to implant dopants into existing 2D crystals. The doped and alloyed variants from Group VI TMDs will be at the center of technical discussions, as they are expected to play essential roles in next‐generation optoelectronic applications. Theoretical backgrounds based on first principles calculations will precede the technical discussions to help the reader understand each element's likelihood of substitutional doping and the expected impact on the material properties.

36 MATERIALS SCIENCE↗

Halide sublattice dynamics drive Li-ion transport in antiperovskites

Here, in this work, we resolve how proton dynamics and halide mixing enhance or impede ionic conduction in protonated lithium antiperovskites (pLiAP) at compositions near the eutectic points of the halide salts. As a material class, pLiAPs of the form Li 3-x OH x X, (X = Cl, Br) show vast compositional design freedom; however, the resulting properties are susceptible to synthesis and processing methodologies. Proton incorporation and halide mixing stabilize the perovskite cubic phase at low temperatures (<50 °C) and using halide mixtures near the eutectic points (~250 to 300 °C) offer possibilities of lower temperature and faster synthesis and processing conditions (<1 h). Mixed-halide compositions such as Li 2 OHCl 0.37 Br 0.63 lead to a 30-fold improvement in room temperature ionic conductivity of a single halide structure, 1.5 × 10 -6 vs. 4.9 × 10 -8 S cm -1 (Li 2 OHCl). We combine infrared spectroscopy and nuclear magnetic resonance with first-principles density functional theory calculations to deconvolute halide mixing effects from local proton dynamics on Li-ion transport. In contrast to what has been supposed, our findings suggest that the halide sublattice dynamics, besides the OH rotation, correlate strongly with the fast-ion conduction at high temperatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In-situ synthesis of oxides by reactive process atmospheres during L-PBF of stainless steel

Traditionally, reactive gases such as oxygen (O 2 ) and carbon dioxide (CO 2 ) have been avoided during laser powder bed fusion (L-PBF) of metals and alloys based on the notion that it may lead to defect formation and poor properties. Here, in this work, we show that instead, these gases can be used to form sub-μm-sized oxide particles in-situ during the L-PBF process in an Fe-Cr-Al-Ti stainless steel and lead to improved room temperature and high-temperature mechanical properties. We manufactured cube samples using pure Ar and various reactive gas atmospheres, namely an O 2 /Argon (Ar) mixture containing 0.2 % O 2 and CO 2 /Ar mixtures containing up to 100 % CO 2 . Co-axial measurements of infrared radiation emitted from the melt pool showed correlation to the presence of O 2 or CO 2 in the gas mixture. Builds produced under CO 2 -containing atmosphere contained complex oxides with an average diameter of ~40 nm, an Al-rich core and a Ti-rich shell. Due to the high cooling rates typical to L-PBF, agglomeration of oxides and slag formation on the surface of the samples could almost be entirely avoided. Compression tests at temperatures up to 800 °C showed that the samples produced in 100 % CO 2 have about 20 % higher yield stress compared to samples produced in Ar. The paper concludes with a discussion of the formation mechanism of the observed oxides. Our results show that in-situ reactions during additive manufacturing processes are a promising pathway to the synthesis of particle-reinforced alloys.

36 MATERIALS SCIENCE↗

Synthesis and Post-Processing of Chemically Homogeneous Nanothreads from 2,5-Furandicarboxylic Acid

Compared with conventional, solution-phase approaches, solid-state reaction methods can provide unique access to novel synthetic targets. Nanothreads—one-dimensional diamondoid polymers formed through the compression of small molecules—represent a new class of materials produced via solid-state reactions, however, the formation of chemically homogeneous products with targeted functionalization represents a persistent challenge. Through careful consideration of molecular precursor stacking geometry and functionalization, we report here the scalable synthesis of chemically homogeneous, functionalized nanothreads through the solid-state polymerization of 2,5-furandicarboxylic acid. The resulting product possesses high-density, pendant carboxyl functionalization along both sides of the backbone, enabling new opportunities for the post-synthetic processing and chemical modification of nanothread materials applicable to a broad range of potential applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Atoms to fibers: Identifying novel processing methods in the synthesis of pitch-based carbon fibers

Understanding and optimizing the key mechanisms used in the synthesis of pitch-based carbon fibers (CFs) are challenging, because unlike polyacrylonitrile-based CFs, the feedstock for pitch-based CFs is chemically hetero- geneous, resulting in complex fabrication leading to inconsistency in the final properties. In this work, we use molecular dynamics simulations to explore the processing and chemical phase space through a framework of CF models to identify their effects on elastic performance. The results are in excellent agreement with experiments. We find that density, followed by alignment, and functionality of the molecular constituents dictate the CF mechanical properties more strongly than their size and shape. Last, we propose a previously unexplored fabrication route for high-modulus CFs. Unlike graphitization, this results in increased sp 3 fraction, achieved via generating high-density CFs. In addition, the high sp 3 fraction leads to the fabrication of CFs with isometric compressive and tensile moduli, enabling their potential applications for compressive loading.

01 COAL, LIGNITE, AND PEAT↗

Continuous Polymer Synthesis and Manufacturing of Polyurethane Elastomers Enabled by Automation

Connecting polymer synthesis and processing is an important challenge for streamlining the manufacturing of polymeric materials. In this work, the automated synthesis of acrylate-capped polyurethane oligomers is integrated with vat photopolymerization 3D printing. This strategy enabled the rapid manufacturing of a library of polyurethane-based elastomeric materials with differentiated thermal and mechanical properties. The automated semi-continuous batch synthesis approach proved enabling for resins with otherwise short shelf lives because the intimate connection between synthesis, formulation, and processing. Structure-property studies demonstrated the ability to tune properties through systematic alteration of crosslink density and chemical composition.

36 MATERIALS SCIENCE↗

Smart Material Demonstrators Based on Shape Memory Alloys and Electroceramics

This paper describes the development and characterization of two technology demonstrators that were produced under the auspices of an ARPA sponsored smart materials synthesis and processing effort. The ARPA Smart Materials and Synthesis (SMS) Program was a 2 year, $10M partnership led by Martin Marietta Laboratories - Baltimore and included Lockheed Missiles & Space Co., NRL, AVX Corp., Martin Marietta Astronautics Groups, BDM Federal, Inc., Virginia Tech, Clemson, University of Maryland, Denver University, and The Johns Hopkins University. In order to demonstrate the usefulness of magnetron sputtered shape memory foil and the manufacturability of reliable, reproducible electrostrictive actuators, the team designed a broadband active vibration cancellation device for suppressing the vibration load on delicate instruments and precision pointing devices mounted on orbiting satellites and spacecraft. The results of extensive device characterization and bench testing are discussed. Initial simulation results show excellent control authority and amplitude attenuation over the range of anticipated disturbance frequencies. The SMS Team has also developed an active 1-3 composite comprising micro-electrostrictive actuators embedded in a polymeric matrix suitable for underwater applications such as sonar quieting and listening arrays, and for medical imaging. Follow-on programs employing these technologies are also described.

Cooke, Arther V.↗

Cobalt-Free Cathodes for Next Generation Li-Ion Batteries

In this U.S. Department of Energy sponsored project Nexceris, in collaboration with project partners; The Ohio State University and Navitas Advanced Systems have advanced the technical maturity of a non-cobalt containing cathode for next-generation Li-ion batteries. The cathode is based on the lithium manganese nickel-titanium oxide, LiNi 0.5 Mn 1.5 TiO 4 (LNMTO) high voltage spinel. To address limitations with poor cycle and calendar life an microstucturally hierarchical LNMO/LNMTO core-shell cathode powder has been developed that enables the formation of a solid-electrolyte interface that effectively passivates the cathode surface. The microstructural enhancements of the cathode material focus on preferentially enriching the surface with titanium. In parallel, new, optimized binder and electrolyte chemistries have been incorporated to address degradation mechanisms associated with high-voltage systems. Single-layer pouch cell and large-format 2-Ah cell testing have shown that an optimized LNMO/LNMTO core-shell powder significantly improves initial cell capacity and cycle life compared to homogeneous LNMO powder. To support development and the fabrication of 2-Ah cells a novel Hybrid Alternative Wet-Chemical Synthesis (HAWCS) process have been developed. This low-cost, synthesis approach enables the excellent compositional and particle morphology control achieved with co-precipitation without the strict process controls and associated expensive process equipment.

25 ENERGY STORAGE↗

High Energy Systems for Transforming CO 2 to Valuable Products (Final Report)

The objective of this project is to develop the Direct E-Beam Synthesis (DEBS) process that uses high-energy electron beams (E-Beam) to break chemical bonds. This allows the production of valuable chemicals, such as acetic acid, methanol, and carbon monoxide, at relatively low severity (pressure near one atmosphere and temperatures <150°C) from near-pure CO 2 captured from a pulverized coal-fired power plant and methane, imported as natural gas. Creating such valuable products will offset the cost of carbon capture and storage. Through this project, we have designed, constructed, and operated an E-Beam reactor to examine the feasibility of performing dry reforming reaction without a catalyst using only DEBS. We have verified the production of syngas with 1:1 H2:CO ratio and calculated that the energy cost for conversion is about 5.2 eV/molecule of product for dry reforming reaction which is similar to the energy cost for conversion using conventional thermochemical conversion but under significantly milder conditions (room temperature and atmospheric pressure). We have performed a technoeconomic analysis (TEA) to estimate the total capital requirement and the cost of production for a 99.4 MMSCFD syngas production plant via non-catalytic Direct E-Beam Synthesis (DEBS) technology utilizing a high-energy electron beam (E-Beam) accelerator. No assumption is made for syngas utilization downstream, and the incoming reactants are pure CO 2 from carbon capture (assumed to be at zero cost) and natural gas. The Total As-Spent Cost (TASC) was calculated to be $\$242.5$ million, resulting in a levelized cost of syngas (LCOS) of $\$175.84$/tonne (metric) at a natural gas price of $\$6.24$/MMBTU1. The cost of syngas is primarily determined by the price of natural gas. If the cost of the CO 2 feedstock is assumed to be non-zero, then the price of the CO 2 feed also heavily influences the levelized cost of syngas. The potential impact on the cost of electricity from syngas revenue is significant. Following DOE NETL’s guidance, a lifecycle analysis (LCA) was conducted to compare the cradle-to-gate life cycle emissions of GTI Energy’s novel Direct E-Beam Synthesis (DEBS) process that produces syngas via the reaction of methane and carbon dioxide to the emissions of a state-of-the-art Steam Methane Reforming (SMR) process that also produces syngas via the reaction of methane and steam. The DEBS process results in less GHG emissions than SMR (with CO product as the basis of comparison). openLCA was used for the LCA and the results show that the total global warming potential (GWP) of DEBS is 0.981 kg CO 2 e per kg CO product, while the SMR process has a global warming potential of 2.573 kg CO 2 e per kg CO product. The ratio of the GWP of the proposed product system to the comparison product system is 0.381. This percent change is 61.9% lower GWP than SMR.

20 FOSSIL-FUELED POWER PLANTS↗