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At least 55 records · Page 3

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DOE OSTI2020

High-capacity rotary drum for atomic layer deposition onto powders and small mechanical parts in a hot-walled viscous flow reactor

Atomic layer deposition (ALD) is uniquely capable of providing uniform thin-film coatings on powder substrates, but powder processing has historically required an ALD reactor designed specifically for powders-e.g., a fluidized bed. Tubular hot-walled viscous-flow reactors commonly employed in laboratory-scale ALD research for coating planar substrates such as silicon have been employed previously to coat gram quantities of powder spread out in a thin layer on a tray, but larger quantities of powder introduce long diffusion pathways where reactants are unable to percolate to the bottom of the powder bed to provide uniform coating in reasonable time periods. In this work, we report a rotary drum with a capacity of 100s of grams that is compatible with conventional tubular hot-walled ALD reactors and provides uniform coatings on powders in viscous flow operation. We benchmark this system using Al 2 O 3 ALD with trimethylaluminum and water. We examine the effect of rotation speed and powder quantity on saturation time via in situ quadrupole mass spectroscopy measurements and gravimetric analysis. Finally, the rotary drum we report is able to provide homogenous coating of up to 75g of silica gel powder with a total surface area of similar to 1500m 2 in viscous flow operation with precursor utilization as high as 70%.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Synthesis of Zeolites LiX and LiAgX

In this work, we produced approximately 50 grams of zeolite LiX and 50 grams of zeolite LiAgX from commercially available zeolite X. The production of the two specialized zeolite phases was accomplished via a series of ion exchange steps followed by washing, drying, and calcining to produce the final materials. The ion exchange was confirmed by several methods including inductively-coupled plasma emission spectroscopy of exchange solution aliquots, gravimetric analysis, energy dispersive x-ray spectroscopy, and X-ray diffraction. We synthesized approximately 115 grams of zeolite LiX in a large-scale production step after completing a proof-of-concept experiment demonstrating the methodology. The production of zeolite LiX from zeolite X yielded an ion exchange (Li + →Na + ) of approximately 82%. The production of zeolite LiAgX from the previously synthesized zeolite LiX was targeted to exchange approximately 20% of the Li + ions with Ag + ions. We first performed a proof-of-concept experiment demonstrating the reaction pathway and selectivity of the Ag + ion, and then performed a large-scale synthesis of zeolite LiAgX using approximately 50 grams of the zeolite LiX. Our final exchange percentage of silver into the zeolite LiX matrix was approximately 20.8%.

36 MATERIALS SCIENCE↗

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 NTRS1971

Effects of thermal and environmental exposure on the mechanical properties of graphite/polyimide composites

Composites were exposed in circulating and static air environments up to 589 K for a maximum of 1000 hours. Composites of HT-S, HM-S, Thornel 50S, and Fortafil 5-Y fiber and a new addition type polyimide resin were laminated in a matched-die mold. Flexural strengths, flexural modulus, and interlaminar shear strengths were determined at 297, 533, and 598 K after various durations of exposure. Composite and fiber weight loss characteristics were determined by isothermal gravimetric analysis in air. Properties of composites exposed and tested at the environment temperatures were compared with those determined under short-term exposure. A new short beam interlaminar shear fixture is described. Environmental effects of long-term ambient temperature exposure on the elevated temperature mechanical properties of graphite/polyimide composites are presented.

Hanson, M. P.↗

NASA NTRS1971

Effects of thermal and environmental exposure on the mechanical properties of graphite/polyimide composites.

Composites were exposed in circulating and static air environments up to 600 F for a maximum of 1000 hours. Composites of HT-S, HM-S, Thornel 50S, and Fortafil 5-Y fiber and a new addition type polyimide resin were laminated in a matched-die mold. Flexural strength, flexural modulus, and interlaminar shear strengths were determined at 75, 500 and 600 F after various durations of exposure. Composite and fiber weight loss characteristics were determined by isothermal gravimetric analysis in air. Properties of composites exposed and tested at the environment temperatures are compared with those determined under short-term exposure. A new short beam interlaminar shear fixture is described. Environmental effects of long-term (up to one year) ambient temperature exposure on the elevated temperature mechanical properties of graphite/polyimide composites are presented.

Hanson, M. P.↗

NASA NTRS1973

Flame retardant polyphosphazenes

Six polyphosphazene compositions were prepared by reaction of three bis-tertiary phosphines with two phenyl-s-triazine derived diazides. All six polyphosphazenes produced were completely characterized, four of them were furthermore subjected to isothermal gravimetric analysis, smoke density measurements, flammability and oxidative thermal degradation testing. The results of the characterization studies indicate that only low molecular weight oligomers, possibly of a cyclic structure, were obtained in the polymerization reactions. Despite this, however, two of the materials showed no weight loss after 96 hr at 200 C, one did not autoignite at 500 C in air, and all four self extinguished when exposed to a flame as soon as contact between flame and resin was lost. The only toxic decomposition products to be concerned about were found to be hydrogen cyanide and benzene. Under the conditions employed it was proven, however, that the quantities of toxic products are greatly reduced if no ignition takes place, e.g., if thermal decomposition proceeds at a sufficiently low rate.

Paciorek, K. L.↗

NASA NTRS1974

Shuttle filter study. Volume 2: Contaminant generation and sensitivity studies

Contaminant generation studies were conducted at the component level using two different methods, radioactive tracer technique and gravimetric analysis test procedure. Both of these were reduced to practice during this program. In the first of these methods, radioactively tagged components typical of those used in spacecraft were studied to determine their contaminant generation characteristics under simulated operating conditions. Because the purpose of the work was: (1) to determine the types and quantities of contaminants generated; and (2) to evaluate improved monitoring and detection schemes, no attempt was made to evaluate or qualify specific components. The components used in this test program were therefore not flight hardware items. Some of them had been used in previous tests; some were obsolete; one was an experimental device. In addition to the component tests, various materials of interest to contaminant and filtration studies were irradiated and evaluated for use as autotracer materials. These included test dusts, plastics, valve seat materials, and bearing cage materials.

Source record↗

NASA NTRS1975

Soil moisture ground truth, Lafayette, Indiana, site; St. Charles Missouri, site; Centralia, Missouri, site

The soil moisture ground-truth measurements and ground-cover descriptions taken at three soil moisture survey sites located near Lafayette, Indiana; St. Charles, Missouri; and Centralia, Missouri are given. The data were taken on November 10, 1975, in connection with airborne remote sensing missions being flown by the Environmental Research Institute of Michigan under the auspices of the National Aeronautics and Space Administration. Emphasis was placed on the soil moisture in bare fields. Soil moisture was sampled in the top 0 to 1 in. and 0 to 6 in. by means of a soil sampling push tube. These samples were then placed in plastic bags and awaited gravimetric analysis.

Jones, E. B.↗

NASA NTRS1976

Soil-moisture ground truth, Hand County, South Dakota

Soil samples were taken in the field and carefully preserved in taped metal containers for later laboratory gravimetric analysis to determine soil-moisture content. The typical sampling pattern used in this mission is illustrated, and the soil types encountered on the soil-moisture lines are summarized. The actual soil-moisture data were tabulated by range, township and section. Soil-moisture data obtained in fields of winter wheat and spring wheat are briefly summarized.

Jones, E. B.↗

NASA NTRS1978

Fiber reinforced PMR polyimide composites

Commercially obtained PMR-15 polyimide prepregs with S-glass and graphite fiber reinforcements were evaluated along with in-house prepared glass and graphite cloth PMR 2 materials. A novel autoclave approach was conceived and used to demonstrate that both the PMR systems respond to 1.4 MPa (200 psi) autoclave pressures to produce void free composites equivalent to die molded laminates. Isothermal gravimetric analysis and subsequent mechanical property tests indicated that the PMR 2 system was significantly superior in thermo-oxidative stability, and that S-glass reinforcements may contribute to the accelerated degradation of composites at 316 C (600 F) when compared to graphite fiber reinforced composites. Fully reversed bending fatigue experiments were conducted with a type of fixture unused for organic matrix composites. These studies indicated that the graphite fiber composites were clearly superior in fatigue resistance to the glass fiber reinforced material and that PMR matrix composite systems yield performance of the same order as composite materials employing other families of matrices.

Cavano, P. J.↗

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.↗