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DOE OSTI2021

Radiolysis of thermally dehydrated gibbsite

Aluminum hydroxide (gibbsite, Al (OH) 3 ) powders and their thermally dehydrated forms were rehydrated and irradiated with gamma rays to examine the effects of the collapse of the crystalline gibbsite structure as it is converted to alumina on the transport of precursors of molecular hydrogen to the surface. The amount of hydrogen gas, H 2 , production from irradiated gibbsite and its transition phases with adsorbed water increased substantially with increasing temperature for dehydration of the samples, up to a point. Furthermore, the production of H 2 for samples without water was considerably lower than the hydrated samples signifying the importance of surface water and the transport of precursors to the surface. EPR spectroscopy showed that the major radiolytic products are trapped electrons and related O – centers. Thermal gravimetric analysis (TGA) measurements of gibbsite dehydration established the temperatures of phase transitions from gibbsite to alumina. Changes to the surface and structure of gibbsite and its transition phases following irradiation were analyzed using nitrogen adsorption, powder X-ray diffraction (pXRD), Raman spectroscopy, electron paramagnetic resonance (EPR), and scanning electron microscopy (SEM). pXRD and Raman spectra showed amorphorization at about 300 °C, coupled to a substantial increase in specific surface area due to increasing porosity.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

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

The Explosive Hazards of Icosahedral Carboranes and Dodecaborate with Common Oxidizers and Salts

Carboranes find use in a wide variety of applications ranging from specialty catalysts to medicinal uses. Certain functionalized carboranes are described as explosive materials, although their nonfunctionalized precursors are regarded as inherently stable and not explosive. Herein, we report new findings on the sensitization of nonfunctionalized 12-vertex ortho-, meta-, and para-carboranes as well as dodecaborate in physical mixtures with several common inorganic salts. These mixtures were evaluated for explosive properties with drop hammer impact tests, friction tests, and differential scanning calorimetry thermal gravimetric analysis (DSC-TGA). Results indicate explosive sensitization to mechanical stimuli for the nonfunctionalized carboranes tested with a wide variety of inorganic salts, especially oxidizers. Sensitization of these compounds has not previously been reported, and raising awareness to the broader scientific community on this matter is warranted, especially as several of the mixtures evaluated are more sensitive to mechanical stimuli than primary explosives such as lead azide or pentaerythritol tetranitrate.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Kinetic Study of Polyvinyl Chloride Pyrolysis with Characterization of Dehydrochlorinated PVC

In this paper, we study the kinetics of polyvinyl chloride (PVC) decomposition using a combination of experimental and computational approaches. Here, we develop a simplified kinetic model that contains only two steps: dehydrochlorination of PVC and further decomposition of the PVC residue. The model is consistent with density functional theory (DFT) calculations and experimental data. Dehydrochlorination is an autocatalytic reaction that starts with a tertiary chloride (Cl) and generates hydrogen chloride (HCl) and benzene as the main products. Benzene and HCl formation rates showed similar trends, indicating that HCl likely catalyzes a homolytic carbon-carbon (C-C) bond cleavage, which gives rise to benzene and an aliphatic fragment. We characterized the structure of dehydrochlorinated PVC (PVC residue) by using thermal gravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FTIR), and nuclear magnetic resonance spectroscopy (NMR). FTIR and NMR results indicate that the PVC residue contains 20% quaternary carbon content, indicating a high concentration of cross-linked molecules. We predict that the most probable structure in the cross-linked centers of the PVC residue is cyclohexadiene, which is supported by DFT calculations, FTIR, and NMR.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Synthesis of a novel multifunctional organic–inorganic nanocomposite for metal ions and organic dye removals

In this study, we used solvent assisted mechano-synthesis strategies to form multifunctional organic–inorganic nanocomposites capable of removing both organic and inorganic contaminants. A zeolite X (Ze) and activated carbon (AC) composite was synthesized via state-of-the-art mechanical mixing in the presence of few drops of water to form Ze/AC. The second composite (Ze/L/AC) was synthesized in a similar fashion, however this composite had the addition of disodium terephthalate as a linker. Both materials, Ze/AC and Ze/L/AC, were characterized using scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), Powdered X-ray diffraction (P-XRD), Fourier-transform infrared spectrometry (FTIR), Accelerated Surface Area and Porosimetry System (ASAP), and thermal gravimetric analysis (TGA). The SEM–EDS displayed the surface structure and composition of each material. The sodium, oxygen and carbon contents increased after linker connected Ze and AC. The P-XRD confirmed the crystallinity of each material as well as the composites, while FTIR indicated the function groups (C=C, O–H) in Ze/L/AC. The contaminant adsorption experiments investigated the effects of pH, temperature, and ionic strength on the adsorption of methylene blue (MB) and Co(II) for each material. In MB adsorption, the first-order reaction rate of Ze/L/AC (0.02 h -1 ) was double that of Ze/AC (0.01 h -1 ). The reaction rate of Ze/L/AC (4.8 h -1 ) was also extraordinarily higher than that of Ze/AC (0.6 h -1 ) in the adsorption of Co(II). Ze/L/AC composite achieved a maximum adsorption capacity of 44.8 mg/g for MB and 66.6 mg/g for Co(II) ions. The MB adsorption of Ze/AC and Ze/L/AC was best fit in Freundlich model with R 2 of 0.96 and 0.97, respectively, which indicated the multilayer adsorption. In the Co(II) adsorption, the data was highly fit in Langmuir model with R 2 of 0.94 and 0.92 which indicated the monolayer adsorption. These results indicated both materials exhibited chemisorption. The activation energy of Ze/L/AC in MB adsorption (34.9 kJ mol -1 ) was higher than that of Ze/L/AC in Co (II) adsorption (26 kJ mol -1 ).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Iodine Capture Studies of Silver Mordenite and Novel Alternative Metal Sorbents

Radioiodine is one of the radionuclides of concern when considering reprocessing of used nuclear fuel (UNF). It is expected to be released primarily in the dissolver off-gas (DOG) stream. Sorbents that target I 2 removal from a UNF processing off gas must perform efficiently under elevated temperatures in the presence of water vapor and nitrogen oxide gasses (NOx). Many studies have been conducted that examine the adsorption of iodine species in the presence of NOx gases through reduced silver-exchanged mordenite (Ag 0 Z), a zeolite mineral. This study characterizes the effects of iodine, water vapor, and nitrogen dioxide on the adsorption of I 2 by Ag 0 Z at lower temperatures suitable for comparison with novel Cu- and Bi- bearing sorbents which offer a non-RCRA alternative. When exposed to ‘harsh’ conditions such as I 2 , H 2 O, and NO 2 vapors carried by air, Cu 2 S-polyacrylonitrile (PAN) is more efficient than Ag 0 Z and all other novel sorbents, providing with 11% I capture efficiency. However, under ‘ideal’ conditions in which I 2 is carried by dry air), Ag 0 Z is more efficient than Cu 2 S-PAN and other novel sorbents, providing 74% I capture efficiency. To investigate this result and the overall performance of all sorbents tested, several characterization techniques were employed, including thermal gravimetric analysis, scanning electron microscopy – electron dispersion X-Ray spectroscopy, powder X-ray diffraction, and X-ray photoelectron spectroscopy. These techniques are discussed within this report. This document also includes a design and test plan update from Idaho National Laboratory as the next step in testing the high performing sorbents from thin-bed tests carried out by Oak Ridge National Laboratory.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1979

Development of economical improved thick film solar cell contact

Materials were surveyed to provide candidates for an all metal electrode paste system. These consisted of a major constituent metal powder, a low melting metal powder suitable for a liquid phase sintering medium, and a powder material suitable as an etchant for silicon dioxide at sintering temperatures. By means of thermal gravimetric analysis a suitable binder was identified for low temperature fired inks. The all metal ink concept was first demonstrated with the silver system to avoid the problems of limited process windows encountered with base metal systems. A number of solid materials capable of selectively etching silicon dioxide at modest temperatures were identified. A paste with silver fluoride was screened onto N-type silicon with 5 ohm cm resistivity. The resulting contact pads had excellent adhesion but were not electrically ohmic. Metallurgically, these contacts have equal or better grain structure as commercial inks fired at the same temperatures.

Ross, B.↗

NASA NTRS1978

Ultrathin metallized PBI paper

A study to determine the feasibility of preparing ultrathin papers with a target weight of 3.5 g/m squared from polybenzimidazole (PBI) fibrids was undertaken. Small hand sheets of target weight were fabricated. They were light brown, low density materials with sufficient strength to be readily handleable. Characterization of these sheets included strength, fold endurance, thermal gravimetric analysis in air and nitrogen and photomicrographs. Two different batches of PBI fibrids were studied and differences in fabrication performance were noted. In neither case could target weight papers be prepared using conventional paper making techniques.

Chenevey, E. C.↗

NASA NTRS1979

Development of Economical Improved Thick Film Solar Cell Contact

Ross, B.↗

NASA NTRS1979

Release-rate calorimetry of multilayered materials for aircraft seats

Multilayered samples of contemporary and improved fire resistant aircraft seat materials (foam cushion, decorative fabric, slip sheet, fire blocking layer, and cushion reinforcement layer) were evaluated for their rates of heat release and smoke generation. Top layers (decorative fabric, slip sheet, fire blocking, and cushion reinforcement) with glass fiber block cushion were evaluated to determine which materials based on their minimum contributions to the total heat release of the multilayered assembly may be added or deleted. Top layers exhibiting desirable burning profiles were combined with foam cushion materials. The smoke and heat release rates of multilayered seat materials were then measured at heat fluxes of 1.5 and 3.5 W/sq cm. Choices of contact and silicone adhesives for bonding multilayered assemblies were based on flammability, burn and smoke generation, animal toxicity tests, and thermal gravimetric analysis. Abrasion tests were conducted on the decorative fabric covering and slip sheet to ascertain service life and compatibility of layers.

Fewell, L. L.↗

NASA NTRS1980

Release-rate calorimetry of multilayered materials for aircraft seats

Multilayered samples of contemporary and improved fire-resistant aircraft seat materials (foam cushion, decorative fabric, slip sheet, fire-blocking layer, and cushion-reinforcement layer) were evaluated for their rates of heat release and smoke generation. Top layers (decorative fabric, slip sheet, fire blocking, and cushion reinforcement) with glass-fiber block cushion were evaluated to determine which materials, based on their minimum contributions to the total heat release of the multilayered assembly, may be added or deleted. Top layers exhibiting desirable burning profiles were combined with foam cushion materials. The smoke and heat-release rate of multilayered seat materials were then measured at heat fluxes of 1.5 and 3.5 W/sq cm. Choices of contact and silicon adhesives for bonding multilayered assemblies were based on flammability, burn and smoke generation, animal toxicity tests, and thermal gravimetric analysis.

Fewell, L. L.↗

NASA NTRS1980

Water-deuterium oxide exchange in polymers used in spacecraft applications

The replacement of water (H2O) by deuterium oxide (D2O) and the exchange between atmospheric water and adsorbed or absorbed D2O were investigated for the polymeric materials Kapton and Mylar using thermal gravimetric analysis and infrared spectroscopy. Replacement of H2O by D2O is easily accomplished. However, exposure of D2O samples to the ambient atmosphere or gases containing H2O results in rapid proton and deuteron exchange between H2O vapor and adsorbed D2O. Replacement of H2O by D2O would not be a practical solution to alleviate spectral interferences that would result from water outgassing in spacecraft orbital environments. Maintaining the materials of interest in a dehydrated state is a more reasonable approach.

Carre, D. J.↗

NASA NTRS1983

Autothermal reforming of aliphatic and aromatic hydrocarbon liquids

Results are presented from a study of the autothermal reforming of paraffins and aromatics over nickel catalysts. The trials were performed to examine the carbon products that appear when steam is passed over hydrocarbon liquids to form H2-rich gases, i.e., the autothermal process (ATR). Attention was given to n-hexane, n-tetradecane, benzene, and benzene solutions of naphthalene with reactant preheat to 1000-1150 F. The carbon-formation limit was sought as a function of the steam-to-carbon and oxygen to carbon molar ratios at constant pressure and the preheat temperatures. The catalyst bed was examined after each trial to identify the locations and types of carbon formed using SEM, thermal gravimetric analysis, and X ray diffraction techniques. The hydrocarbon fuels each had a separate temperature and reaction profile, as well as carbon formation characteristics. No carbon formation was observed in the upper layer of the reactor bed, while both gas phase and surface-grown deposits were present in the lower part. The results are concluded of use in the study of No. 2 fuel oil for ATR feedstock.

Flytzani-Stephanopoulos, M.↗

NASA NTRS1983

Rubber-toughened polyfunctional epoxies - Brominated vs nonbrominated formulated for graphite composites

A new, commercially available, trifunctional epoxy resin (tris-(hydroxyphenyl)-methane triglycidyl ether) was modified with synthetic rubber to increase the impact resistance of epoxy/graphite composites. These composites were reinforced with commercially available satin-weave carbon cloth using two formulations of epoxies (brominated and nonbrominated) containing various amounts of carboxy-terminated butadience acrylonitrile (CTBN) rubber that had been prereacted with epoxy resin. The impact resistance was determined by measuring the interlaminar shear strength of the composites after impact. The mechanical properties, such as flexural strength and modulus at room temperature and at 93 C, were also determined. Measurements were taken of the flammability and glass transition temperature (Tg); and a thermal-gravimetric analysis was made.

Nir, Z.↗

NASA NTRS1985

Organosiloxane working fluids for the liquid droplet radiator

Siloxane-based working fluids for advanced space radiators requiring direct fluid exposure to the space environment are evaluated. Isolation of five candidate fluids by vacuum distillation from existing siloxane polymers is discussed. The five fluids recovered include a polydimethylsiloxane, three phenyl-containing siloxanes, and a methylhexylsiloxane. Vapor pressures and viscosities for the five fluids are reported over the temperature range of 250 to 400 K. Use of thermal-gravimetric analysis to reliably estimate vapor pressures of 10 to the -8 power Pascals is described. Polydimethylsiloxane (PDMS) and polymethylphenylsiloxane (PMPS) are selected from the five candidate fluids based on favorable vapor pressure and viscosity, as well as perceived stability in low-Earth orbit environments. Characterization of these fluids by infrared spectroscopy, Si-29 NMR, gel-permeation chromatography, and liquid chromatography is presented. Both fluids consist of narrow molecular weight distributions, with average molecular weights of about 2500 for PDMS and 1300 for PMPS.

Buch, R. R.↗

NASA NTRS1986

Evaluation of moisture barrier coatings on carbon-phenolic SRM nozzle materials

The carbon-phenolic composite ablative material used on the Solid Rocket Motor (SRM) nozzle is known to absorb moisture from the atmosphere. This could cause problems such as pocketing during firing. Several moisture barrier coatings were tested on the SRM nozzle material. Data are presented for six of the 12 coatings to be tested. The data were obtained from immersion of coated samples in an environmental chamber at 100 F and 100% relative humidity and by using a modified TGA (thermal gravimetric analysis) technique. The TGA technique involved allowing wet nitrogen (25 C, 80% relative humidity) to flow across a small sample at about 65 cu cm per minute while continually monitoring the weight increase. These preliminary results show Kel-F-800, a material supplied by 3M Corporation to be the better moisture barrier. A second task was to collect data on the relative absorption of water and kerosene into the carbon-phenolic SRM nozzle material. These data indicate that water absorbs into the nozzle material to a much greater extent than kerosene. Thus kerosene is the more likely solvent in which to make specific gravity measurements on the SRM nozzle material.

Mcnutt, Ronald C.↗

NASA NTRS1992

Determination of the oxidative stability of perfluoropolyalkyl ethers and correlation with chemical structure

The oxidative stabilities of several perfluoropolyalkyl ethers (PFPAE) with related chemical structures were determined by thermal gravimetric analysis and correlated with their chemical structures. These results show that oxidative stability increases as the number of difluoroformal groups decreases and as trifluoromethyl substituents are added. They are also consistent with a recently proposed intramolecular disproportionation reaction mechanism involving coordination of successive ether oxygens to a Lewis acid. Since polytetrafluoroethylene contains no oxygen, it provides an indication of the upper limit to oxidative stability of PFPAE fluids. These results also show that oxidative decomposition of PFPAE fluids requires the presence of an active metal as well as air. Consequently, it may be possible to minimize decomposition and thus improve oxidative stability by passivating reactive metal surfaces.

Helmick, Larry S.↗

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.↗