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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Gas-phase surface modification to control catalyst structure and yields in methane dehydroaromatization

Methane dehydroaromatization (MDA) is a promising approach for direct methane transformation to aromatics and hydrogen. The benchmark catalyst Mo/H-ZSM-5 struggles to find commercial adoption because of thermodynamically-limited yields and rapid coking on Brønsted acid and molybdenum carbide species, especially on zeolite external surfaces. Here, gas-phase atomic layer deposition (ALD) overcoats H-ZSM-5 external surfaces with SiO 2 or Al 2 O 3 . NH 3 -TPD, HRTEM, and textural properties show that these overcoats exclusively passivate zeolite external surfaces. Under MDA conditions, SiO 2 gives softer coke and increases cumulative benzene yields by 25%, while Al 2 O 3 strongly decreases yields. H 2 -TPR and UV-visible and Raman spectroscopy show how the overcoats redisperse the MoO x precatalysts, especially over multiple deactivation and isothermal oxidative regeneration cycles. Combined with 27 Al-MAS NMR, MoO x redistribution and dealumination are seen as the causes of long-term deactivation over multiple regeneration cycles, and this process continues to occur regardless of the overcoat. Altogether, the deposition of a small amount of silica on the outer surface of Mo/H-ZSM-5 reduces the formation of hard coke, which could be regenerated by milder methods such as hydrogen treatment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Deactivation of Mo/H-ZSM-5 in Microwave-Assisted and Thermal-Driven Methane Dehydroaromatization

A better understanding of catalyst deactivation is needed to improve catalyst design and performance in microwave-enhanced methane dehydroaromatization (MDA). Here, this study investigates the deactivation of a molybdenum supported H-ZSM-5 zeolite (Mo/H-ZSM-5) catalyst in MDA under microwave-heated conditions, comparing its performance to that of the same catalyst under conventional heating. While the microwave-assisted (MW) process achieved higher benzene yields, the catalyst experienced faster deactivation due to the selective and rapid deposition of coke within the pores of the zeolite, as confirmed through Brunauer–Emmett–Teller (BET), X-ray diffraction (XRD), ammonia-temperature programmed desorption (NH 3 -TPD), thermal gravimetric analysis (TGA), temperature programmed oxidation (TPO), and X-ray photoelectron spectroscopy (XPS) analyses. The quantification of total coke content via TGA/TPO and surface carbon (XPS) revealed that nearly twice as much coke was deposited on the catalyst under MW conditions compared to that on the conventionally heated material, and the coke exhibited a more conductive and graphitic nature. The accelerated deactivation rates were attributed to the formation of hot spots in the MW system, leading to enhanced coupling with coke formed in situ during the reaction and resulting in increased Mo reduction. Observations indicated that the CO activation used to carburize the catalyst prior to the reaction is not advantageous in the MW heating environment. The presence of large amounts of Mo oxides at elevated temperatures (through hot spots) exposed to methane leads to instability under the reaction conditions. Optimizing the activation environment and improvement of the Mo dispersion within the pores are potential strategies to improve catalyst stability.

Mo/H-ZSM-5 zeolite↗
DOE OSTI2026

Quantifying the Impact of Metal Population Distribution in MFI-Supported Mo Catalysts for Methane Dehydroaromatization

Precise evaluation of intrinsic kinetic behavior in Mo/MFI catalysts for methane dehydroaromatization (MDA) is confounded by variations in Mo dispersion and speciation, which are influenced by metal loading and zeolite acidity. This work advances the utility of H 2 -temperature programmed reduction (H 2 -TPR) for characterizing Mo/MFI catalysts by enabling quantitative comparison of MoO x populations distinguished by reduction behavior and linked to initial catalytic performance. A comprehensive H 2 reduction pathway is established through systematic H 2 - TPR studies varying catalyst composition (1–10 wt % Mo, Si/Al = 15, 40, ∞), supplemented by UV-Raman spectroscopy, X-ray powder diffraction, N 2 physisorption, NH 3 -TPD, and advanced spectroscopic analysis (in situ XAS with principal component analysis/multivariate curve resolution—alternating least squares). Two low-temperature H 2 -TPR regions capture distinct Mo populations undergoing initial Mo(VI)→Mo(IV) reduction: a lower-temperature population (Mo-RI) associated primarily with highly dispersed, anchored MoO x species expected to predominantly reside within MFI channels, and a higher-temperature population (Mo-RII) corresponding to a broader set of MoO x species that becomes increasingly bulk-like/extrazeolitic at higher Mo loading. Quantification of these populations provides practical, kinetically relevant descriptors for comparing initial MDA rates across catalysts with varying Mo loading, Si/Al ratio, and MoO x heterogeneity. Application of lower-temperature Mo-RI estimates to kinetic measurements reveals a minimum threshold of ∼0.12 × 10 –3 mol Mo-RI/g cat , above which initial forward benzene rates normalized to this population converge despite differences in metal loading and zeolite Brønsted acidity. This threshold coincides with a transition toward a common C 2 -mediated benzene-forming regime, as indicated by approach-to-equilibrium analysis of methane-to-ethane, ethane-to-ethylene, and ethylene-to-benzene reaction steps. Above this threshold, normalized initial benzene rates are nearly invariant with increasing Mo-RII/Mo-RI population ratio, indicating that excess Mo-RII populations, including bulk-like/extrazeolitic MoO x domains present at higher loading, do not measurably suppress benzene formation associated with anchored and mostly channel-confined Mo population under the initial-rate conditions examined.

Mo/MFI↗
DOE OSTI2025

A Near-Real-Time Model for Predicting Electricity Disruptions in Texas During Winter Storms

There has been an increase in extreme weather events, posing a threat to power grid systems, potentially influenced by factors such as population growth, changes in ecosystems, land cover, and land use in the service area, as well as the growth of certain vegetation types. This research seeks to develop a predictive model to mitigate potential damages caused by future winter storms. This research utilizes the Light Gradient Boosting Machine (LightGBM), incorporating the number of power outages experienced at the county level, geographic details, weather information, and lagged outage and lagged weather data. The developed models were broadly divided into two groups, with six models in each group - one group without optimization and another with optimization, totaling 12 trained models. For model optimization, Bayesian optimization was employed using Root Mean Squared Error (RMSE) as the objective function. In results, when comparing Group 2 (the optimized group) with Group 1 (the non-optimized group), it was found that optimization did not always lead to a reduction in RMSE and Mean Absolute Error (MAE). However, in terms of Mean Directional Accuracy (MDA), while all results in Group 1 were below the baseline accuracy of 0.33, all results in Group 2 exceeded 0.33, with some cases showing an increase of more than three times the baseline. The results indicated that, in the optimized model group, Population and Pressure were the most influential factors when using current weather data and geographical information. When using lagged data, lagged recorded outages and lagged Pressure emerged as the most significant factors. Among the 12 developed models, the L-1-2-O model showed the lowest RMSE and MAE, as well as the highest accuracy, with values of 390.62 households and 168.13 households, respectively. To normalize the RMSE and MAE values, each metric was divided by the average number of households among the counties in Texas. For the L-1-2-O model, the scaled RMSE was 0.88% and the scaled MAE was 0.38%. In terms of MDA, which indicates the accuracy of the prediction direction, the L-1-O model achieved the highest score of 0.41. Although this study focused on Texas, which suffered the greatest impact from the winter storms in 2021, with additional validation, the methodology used in this research could be applied to other regions.

Lee, Jangjae [Texas A & M Univ., College Station, ↗
NASA NTRS1974

Isomer effects on polyimide properties

The polymerization of 2,4'-methylene-dianiline with benzophenone tetracarboxylic acid dianhydride yields high molecular weight polyamic acid. Polyimide is formed when films of the polyamic acid are cured between 200 - 300 C. A lower molecular weight polyamic acid is obtained from 2,2'-MDA with BTDA, but it appears that a lowering of the reaction temperature will yield high molecular weight polymer. Evaluation of these polymers is underway. Continued efforts to synthesize 2,3'- MDA and 2,3'-diaminobenzophenone have met with little success.

Stump, B. L.↗
NASA NTRS1975

Molecular weight: Property relationships of high performance polymers used for adhesives and composites

Degradation of high performance polyimide precursor resins was investigated by measuring the molecular weight of the polymers in solution, using a membrane osmometer. It was found that polyimide precursor resins composed of BTDA and ODPA combined with DABP and MDA were unstable in DMAC. The degradation rate was found to depend upon the chemical nature of the isomeric diamine and the geometric structure about the amide linkage. The polymers of DABP were less susceptible to degradation than those of MDA and p,p'-compounds were more stable than m,m'-compounds. These results suggest that degradation is correlated with the basicity of the diamine. That is, the rate of the degradation reaction increases with the basicity of the diamine group in the polyimide precursor resin. The presence of water and a higher temperature increased the degradation rate of the polymers.

Kranbuehl, D.↗
NASA NTRS1980

Influence of excess diamine on properties of PMR polyimide resins and composites

By varying the stoichiometry of the reactants in the preparation of PMR polyimide resin, changes occur in molecular weight distribution which influence the rheological properties and thus the processability of the resin, as well as the mechanical properties of the composite. The influence of 1-10 percent molar excess MDA on the molecular weight distribution and rheological properties of an imidized PMR system were exposed. Molecular weight distribution is characterized by gel permeation chromatography of the imidized molding compound; shear viscosity is related to changes in average molecular weight. The thermo-oxidative stability at 600 F, glass transition temperature, flexural and interlaminar shear properties of PMR polyimide/Celion 6000 graphite fiber composites are compared as a function of the percent excess MDA in the monomer reactant mixture.

Hurwitz, F. I.↗
NASA NTRS1980

Influence of excess diamine on properties of PMR polyimide resins and composites

This preliminary study explores the influence of 1-10 percent molar excess MDA on the molecular weight distribution and rheological properties of an imidized PMR system. Molecular weight distribution is characterized by gel permeation chromatography of the imidized molding compound; shear viscosity is related to changes in average molecular weight. The thermo-oxidative stability at 600 F glass transition temperature, flexural and interlaminar shear properties of PMR polyimide/Celion 6000 graphite fiber composites are compared as a function of the percent excess MDA in the monomer reactant mixture.

Hurwitz, F. I.↗
NASA NTRS1983

A modular approach to developing a large deployable reflector

NASA is currently exploring the feasibility of developing a large deployable reflector (LDR) astronomical facility to perform astrophysical studies in the mid 1990's in the IR and submillimeter portion of the spectrum. This paper examines a combination of automatic deployment and on-orbit assembly that may reduce the technological complexity and cost of the LDR system. Two Shuttle volume budget scenarios are examined to assess the potential of various technological tools to reduce the LDR system complexity. It is noted that the LDR design must be flexible and allow one subsystem to be modified without adversely affecting the entire system. One way to achieve this flexibility is a modular design approach (MDA) in which the major subsystems are physically separated during launch and assembled on orbit. NASA is defining a technology development plan for LDR that will identify the technology advances that are required. It is concluded that the MDA offers the flexibility to easily incorporate these advances into the design.

Pittman, R.↗
NASA NTRS1986

Effect of solution concentration and aging conditions on PMR-15 resin

High performance liquid chromatography is utilized to evaluate the effect of temperature, solution concentration, and aging time on PMR-15 resin solutions. Fifty- and 70-wt percent PMR-15 resin solutions were prepared from the mixture of 5-norbornene-2,3-dicarboxylic ester (NE) acid, 4.4'-methylenedianiline (MDA), methanol, and 3,3',4.4.-benzophenonetetracarboxylic dimethyl ester (BTDE) acid solution. It is observed that in PMR-15 resin solution aged for 35 days at room temperature NE and MDA react to form amide and imide intermediates. The precipitation data reveal that in the 70-wt percent solution precipitation occurs after 12 days and in the 50-wt percent solution after 20 days; however, at lower temperatures (-11 C, and 2 C) no precipitation is detected. It is concluded that storage of resin solutions and powders at reduced temperatures extends shelf life by reducing the rate of imide formation.

Roberts, G. D.↗
NASA NTRS1988

Progress of research to identify rotating thunderstorms using satellite imagery

The possibility of detecting potentially tornadic thunderstorm cells from geosynchronous satelite imagery is determined. During the life of the contract, we examined eight tornado outbreak cases which had a total of 124 individual thunderstorm cells, 37 of which were tornadic.These 37 cells produced a total of 119 tornadoes. The outflow characteristics of all the cells were measured. Through the use of a 2-D flow field model, we were able to simulate the downstream developmemt of an anvil cloud plume which was emitted by the storm updraft at or near the tropopause. We used two parameters to characterize the anvil plume behavior: its speed of downstream propagation (U max) and the clockwise deviation of the centerline of the anvil plume from the storm relative ambient wind at the anvil plume outflow level (MDA). U max was the maximum U-component of the anvil wind parameter required to successfully maintain an envelope of translating particles at the tip of the expanding anvil cloud. MDA was the measured deviation angle acquired from McIDAS, between the storm relative ambient wind direction and the storm relative anvil plume outflow direction; tha latter being manipulated by controlling a tangential wind component to force the envelope of particles to maintain their position of surrounding the expanding outflow cloud.

Anderson, Charles E.↗
NASA NTRS1989

Mechanical properties of several neat polymer matrix materials and unidirectional carbon fiber-reinforced composites

The mechanical and physical properties of three neat matrix materials, i.e., PEEK (polyetheretherketone) thermoplastic, Hexcel F155 rubber-toughened epoxy and Hercules 8551-7 rubber-toughened epoxy, were experimentally determined. Twelve unidirectional carbon fiber composites, incorporating matrix materials characterized in this or earlier studies (with one exception; the PISO(sub 2)-TPI matrix itself was not characterized), were also tested. These composite systems included AS4/2220-1, AS4/2220-3, T500/R914, IM6/HX1504, T300/4901A (MDA), T700/4901A (MDA), T300/4901B (MPDA), T700/4901B (MPDA), APC2 (AS4/PEEK, ICI), APC2 (AS4/PEEK, Langley Research Center), AS4/8551-7, and AS4/PISO(sub 2)-TPI. For the neat matrix materials, the tensile, shear, fracture toughness, coefficient of thermal expansion, and coefficient of moisture expansion properties were measured as a function of both temperature and moisture content. For the unidirectional composites, axial and transverse tensile, longitudinal shear, coefficient of thermal expansion, and coefficient of moisture expansion properties were determined, at room temperature and 100 C.

Coguill, Scott L.↗
NASA NTRS1992

Materials dispersion and biodynamics project research

The Materials Dispersion and Biodynamics Project (MDBP) focuses on dispersion and mixing of various biological materials and the dynamics of cell-to-cell communication and intracellular molecular trafficking in microgravity. Research activities encompass biomedical applications, basic cell biology, biotechnology (products from cells), protein crystal development, ecological life support systems (involving algae and bacteria), drug delivery (microencapsulation), biofilm deposition by living organisms, and hardware development to support living cells on Space Station Freedom (SSF). Project goals are to expand the existing microgravity science database through experiments on sounding rockets, the Shuttle, and COMET program orbiters and to evolve,through current database acquisition and feasibility testing, to more mature and larger-scale commercial operations on SSF. Maximized utilization of SSF for these science applications will mean that service companies will have a role in providing equipment for use by a number of different customers. An example of a potential forerunner of such a service for SSF is the Materials Dispersion Apparatus (MDA) 'mini lab' of Instrumentation Technology Associates, Inc. (ITA) in use on the Shuttle for the Commercial MDAITA Experiments (CMIX) Project. The MDA wells provide the capability for a number of investigators to perform mixing and bioprocessing experiments in space. In the area of human adaptation to microgravity, a significant database has been obtained over the past three decades. Some low-g effects are similar to Earth-based disorders (anemia, osteoporosis, neuromuscular diseases, and immune system disorders). As new information targets potential profit-making processes, services and products from microgravity, commercial space ventures are expected to expand accordingly. Cooperative CCDS research in the above mentioned areas is essential for maturing SSF biotechnology and to ensure U.S. leadership in space technology. Currently, the MDBP conducts collaborative research with investigators at the Rockefeller University, National Cancer Institute, and the Universities of California, Arizona, and Alabama in Birmingham. The growing database from these collaborations provides fundamental information applicable to development of cell products, manipulation of immune cell response, bone cell growth and mineralization, and other processes altered by low-gravity. Contacts with biotechnology and biopharmaceutical companies are being increased to reach uninformed potential SSF users, provide access through the CMDS to interested users for feasibility studies, and to continue active involvement of current participants. We encourage and actively seek participation of private sector companies, and university and government researchers interested in biopharmaceuticals, hardware development and fundamental research in microgravity.

Lewis, Marian L.↗
NASA NTRS1992

Techniques used to identify tornado producing thunderstorms using geosynchronous satellite data

Satellite imagery in the outbreak region in the time prior to and during tornado occurrence was examined in detail to obtain descriptive characteristics of the anvil plume. These characteristics include outflow strength (UMAX), departure of anvil centerline from the storm relative ambient wind (MDA), storm relative ambient wind (SRAW), and maximum surface vorticity (SFCVOR). It is shown that by using satellite derived parameters which characterize the flow field in the anvil region, the occurrence and intensity of tornadoes, which the parent thunderstorm produces, can be identified. Analysis of the censored regression models revealed that the five explanatory variables (UMAX, MDA, SRAW, UMAX-2, and SFCVOR) were all significant predictors in the identification of tornadic intensity of a particular thunderstorm.

Schrab, Kevin J.↗
NASA NTRS1994

Design and flight test of the Propulsion Controlled Aircraft (PCA) flight control system on the NASA F-15 test aircraft

This report describes the design, development and flight testing of the Propulsion Controlled Aircraft (PCA) flight control system performed at McDonnell Douglas Aerospace (MDA), St. Louis, Missouri and at the NASA Dryden Flight Research Facility, Edwards Air Force Base, California. This research and development program was conducted by MDA and directed by NASA through the Dryden Flight Research Facility for the period beginning January 1991 and ending December 1993. A propulsion steering backup to the aircraft conventional flight control system has been developed and flight demonstrated on a NASA F-15 test aircraft. The Propulsion Controlled Aircraft (PCA) flight system utilizes collective and differential thrust changes to steer an aircraft that experiences partial or complete failure of the hydraulically actuated control surfaces. The PCA flight control research has shown that propulsion steering is a viable backup flight control mode and can assist the pilot in safe landing recovery of a fighter aircraft that has damage to or loss of the flight control surfaces. NASA, USAF and Navy evaluation test pilots stated that the F-15 PCA design provided the control necessary to land the aircraft. Moreover, the feasibility study showed that PCA technology can be directly applied to transport aircraft and provide a major improvement in the survivability of passengers and crew of controls damaged aircraft.

Wells, Edward A.↗
NASA NTRS1997

Structure-Property Relationships of Bismaleimides

The purpose of this research was to control and systematically vary the network topology of bismaleimides through cure temperature and chemistry (addition of various coreactants) and subsequently attempt to determine structure-mechanical property relationships. Characterization of the bismaleimide structures by dielectric, rheological, and thermal analyses, and density measurements was subsequently correlated with mechanical properties such as modulus, yield strength, fracture energy, and stress relaxation. The model material used in this investigation was 4,4'-BismaleiMidodIphenyl methane (BMI). BMI was coreacted with either 4,4'-Methylene Dianiline (MDA), o,o'-diallyl bisphenol A (DABA) from Ciba Geigy, or Diamino Diphenyl Sulfone (DDS). Three cure paths were employed: a low- temperature cure of 140 C where chain extension should predominate, a high-temperature cure of 220 C where both chain extension and crosslinking should occur simultaneously, and a low-temperature (140 C) cure followed immediately by a high-temperature (220 C) cure where the chain extension reaction or amine addition precedes BMI homopolymerization or crosslinking. Samples of cured and postcured PMR-15 were also tested to determine the effects of postcuring on the mechanical properties. The low-temperature cure condition of BMI/MDA exhibited the highest modulus values for a given mole fraction of BMI with the modulus decreasing with decreasing concentration of BMI. The higher elastic modulus is the result of steric hindrance by unreacted BMI molecules in the glassy state. The moduli values for the high- and low/high-temperature cure conditions of BMI/MDA decreased as the amount of diamine increased. All the moduli values mimic the yield strength and density trends. For the high-temperature cure condition, the room- temperature modulus remained constant with decreasing mole fraction of BMT for the BMI/DABA and BMI/DDS systems. Postcuring PMR-15 increases the modulus over that of the cured material even though density values of cured and postcured PMR were essentially the same. Preliminary results of a continuous and intermittent stress relaxation experiment for BMI:MDA in a 2:1 molar ratio indicate that crosslinking is occurring when the sample is in the undeformed state. Computer simulation of properties such as density, glass transition temperature, and modulus for the low- temperature cure conditions of BMI/MDA and BMI/DABA were completed. The computer modeling was used to help further understand and confirm the structure characterization results. The simulations correctly predicted the trends of these properties versus mole fraction BMI and were extended to other BMI/diamine systems.

Tenteris-Noebe, Anita D.↗
NASA NTRS1998

Low-Cost Production of Composite Bushings for Jet Engine Applications

The objectives of this research program were to reduce the manufacturing costs of variable stator vane bushings by 1) eliminating the expensive carbon fiber braiding operation, 2) replacing the batch mode impregnation, B-stage, and cutting operations with a continuous process, and 3) reducing the molding cycle and machining operations with injection molding to achieve near-net shapes. Braided bushings were successfully fabricated with both AMB-17XLD and AMB-TPD resin systems. The composite bushings achieved high glass transition temperature after post-cure (+300 C) and comparable weight loss to the PNM-15 bushings. ANM-17XLD bushings made with "batch-mode" molding compound (at 0.5 in. fiber length) achieved a +300 lb-force flange break strength which was superior to the continuous braided-fiber reinforced bushing. The non-MDA resin technology developed in this contract appears attractive for bushing applications that do not exceed a 300 C use temperature. Two thermoplastic polyimide resins were synthesized in order to generate injection molding compound powders. Excellent processing results were obtained at injection temperatures in excess of 300 C. Micro-tensile specimens were produced from each resin type and the Tg measurements (by TMA) for these samples were equivalent to AURUM(R). Thermal Gravimetric Analysis (TGA) conducted at 10 C/min showed that the non-MDA AMB-type polyimide thermoplastics had comparable weight loss to PMR-15 up to 500 C.

Gray, Robert A.↗
NASA NTRS1999

Analysis and Inverse Design of the HSR Arrow Wing Configuration with Fuselage, Wing, and Flow Through Nacelles

The design process for developing the natural flow wing design on the HSR arrow wing configuration utilized several design tools and analysis methods. Initial fuselage/wing designs were generated with inviscid analysis and optimization methods in conjunction with the natural flow wing design philosophy. A number of designs were generated, satisfying different system constraints. Of the three natural flow wing designs developed, the NFWAc2 configuration is the design which satisfies the constraints utilized by McDonnell Douglas Aerospace (MDA) in developing a series of optimized configurations; a wind tunnel model of the MDA designed OPT5 configuration was constructed and tested. The present paper is concerned with the viscous analysis and inverse design of the arrow wing configurations, including the effects of the installed diverters/nacelles. Analyses were conducted with OVERFLOW, a Navier-Stokes flow solver for overset grids. Inverse designs were conducted with OVERDISC, which couples OVERFLOW with the CDISC inverse design method. An initial system of overset grids was generated for the OPT5 configuration with installed diverters/nacelles. An automated regridding process was then developed to use the OPT5 component grids to create grids for the natural flow wing designs. The inverse design process was initiated using the NFWAc2 configuration as a starting point, eventually culminating in the NFWAc4 design-for which a wind tunnel model was constructed. Due to the time constraints on the design effort, initial analyses and designs were conducted with a fairly coarse grid; subsequent analyses have been conducted on a refined system of grids. Comparisons of the computational results to experiment are provided at the end of this paper.

Krist, Steven E.↗