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At least 1,063 records · Page 59

Interlaminar shear fracture toughness and fatigue thresholds for composite materials

Static and cyclic end notched flexure tests were conducted on a graphite epoxy, a glass epoxy, and graphite thermoplastic to determine their interlaminar shear fracture toughness and fatigue thresholds for delamination in terms of limiting values of the mode II strain energy release rate, G-II, for delamination growth. The influence of precracking and data reduction schemes are discussed. Finite element analysis indicated that the beam theory calculation for G-II with the transverse shear contribution included was reasonably accurate over the entire range of crack lengths. Cyclic loading significantly reduced the critical G-II for delamination. A threshold value of the maximum cyclic G-II below which no delamination occurred after one million cycles was identified for each material. Also, residual static toughness tests were conducted on glass epoxy specimens that had undergone one million cycles without delamination. A linear mixed-mode delamination criteria was used to characterize the static toughness of several composite materials; however, a total G threshold criterion appears to characterize the fatigue delamination durability of composite materials with a wide range of static toughness.

O'Brien, T. Kevin↗

Flexure fatigue testing of 90 deg graphite/epoxy composites

A great deal of research has been performed characterizing the in-plane fiber-dominated properties, under both static and fatigue loading, of advanced composite materials. To the author's knowledge, no study has been performed to date investigating fatigue characteristics in the transverse direction. This information is important in the design of bonded composite airframe structure where repeated, cyclic out-of-plane bending may occur. Recent tests characterizing skin/stringer debond failures in reinforced composite panels where the dominant loading in the skin is flexure along the edge of the frame indicate failure initiated either in the skin or else the flange, near the flange tip. When failure initiated in the skin, transverse matrix cracks formed in the surface skin ply closest to the flange and either initiated delaminations or created matrix cracks in the next lower ply, which in turn initiated delaminations. When failure initiated in the flanges, transverse cracks formed in the flange angle ply closest to the skin and initiated delamination. In no configuration did failure propagate through the adhesive bond layer. For the examined skin/flange configurations, the maximum transverse tension stress at failure correlates very well with the transverse tension strength of the composites. Transverse tension strength (static) data of graphite epoxy composites have been shown to vary with the volume of material stressed. As the volume of material stressed increased, the strength decreased. A volumetric scaling law based on Weibull statistics can be used to predict the transverse strength measurements. The volume dependence reflects the presence of inherent flaws in the microstructure of the lamina. A similar approach may be taken to determine a volume scale effect on the transverse tension fatigue behavior of graphite/epoxy composites. The objective of this work is to generate transverse tension strength and fatigue S-N characteristics for composite materials using 3-point flexure tests of 90 deg graphite/epoxy specimens. Investigations will include the volume scale effect as well as frequency and span-to-thickness ratio effects. Prior to the start of the experimental study, an analytical study using finite element modeling will be performed to investigate the span-to-thickness effect. The ratio of transverse flexure stress to shear stress will be monitored and its values predicted by the FEM analysis compared with the value obtained using a 'strength of materials' based approach.

Peck, Ann Nancy W.↗

High contrast imaging and thickness determination of graphene with in-column secondary electron microscopy

We report a new method for quantitative estimation of graphene layer thicknesses using high contrast imaging of graphene films on insulating substrates with a scanning electron microscope. By detecting the attenuation of secondary electrons emitted from the substrate with an in-column low-energy electron detector, we have achieved very high thickness-dependent contrast that allows quantitative estimation of thickness up to several graphene layers. The nanometer scale spatial resolution of the electron micrographs also allows a simple structural characterization scheme for graphene, which has been applied to identify faults, wrinkles, voids, and patches of multilayer growth in large-area chemical vapor deposited graphene. We have discussed the factors, such as differential surface charging and electron beam induced current, that affect the contrast of graphene images in detail.

36 MATERIALS SCIENCE↗

Surface analysis insight note: Differentiation methods applicable to noisy data for determination of sp2‐ versus sp3‐hybridization of carbon allotropes and AES signal strengths

The derivatives of the spectra are commonly used for quantification in Auger Electron Spectroscopy (AES) spectra, while the derivative of the KLL C Auger line has proven to be valuable in obtaining a measure of the relative proportions of sp 2 ‐ and sp 3 ‐hybridization using the D‐parameter in both AES and X‐ray Photoelectron Spectroscopy (XPS). Differentiation of X‐ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES) spectra by numerical means is presented and illustrated for polymeric, such as PEEK and Nylon, as well as for graphitic materials including highly ordered pyrolytic graphite and graphene oxide. The most commonly available Savitzky–Golay method is explained mathematically and developed through the case of constructing a 5‐point quadratic polynomial convolution kernel suitable for differentiating spectra of adequate signal to noise. The concept of differentiation of spectra where signal to noise is less than adequate is also developed. Two alternative strategies to Savitzky–Golay differentiation are presented, which fit curves to data that allow derivatives to be obtained where Savitzky–Golay would otherwise fail. These alternative methods involve constructing a parametric curve that fits data over the entire energy interval of interest. Derivatives of spectra are then obtained by differentiating these parametric curves directly. A comparison of results for different materials for which specific sp 2 ‐ vs sp 3 ‐hybridized carbon proportions are of interest is used to emphasize the importance of characterizing methods used to differentiate spectra and understanding the characteristics of instrumentation used to measure spectra. The case for using Principal Component Analysis noise reduction with C KLL spectra is made for spectra collected from a heterogeneous graphene oxide sample.

Fairley, Neal↗

Mechanical and thermophysical properties of graphite/polyimide composite materials

An on-going program to characterize advanced composites for up to 50,000 hours of exposure to simulated supersonic cruise environments is summarized. Results are presented for up to 25,000 hours of thermal exposure and 10,000 hours of flight simulation at temperatures up to 560K (550 F) with emphasis on HTS/710 graphite/polyimide composite material. Results to date indicate that the maximum use temperature for HTS/710 may be reduced to 505K (450 F) for long-time (1000 hours) application such as the supersonic transport. Preliminary thermophysical properties data for HTS/PMR15 graphite/polyimide were generated. These data include thermal conductivity, thermal expansion, and specific heat from 115K (-252 F) to 590K (600 F) and emittance at room temperature and 590K (600 F). The purpose in generating these data was to validate use of state-of-the-art property measurement methods for advanced graphite fiber reinforced resin matrix composites. Based on results to this point, thermal expansion measurements for composites are most difficult to perform. A high degree of caution in conducting thermal expansion tests and analyzing results is required to produce reliable data.

Rummler, D. R.↗

Hydrogen adsorption at the graphene surface: A vdW-DF perspective

We use the recently developed van der Waals density functional (vdW-DF) along with the C09x exchange functional to explore the interactions of molecular hydrogen with a single sheet of graphene. Our calculations demonstrate the importance of the inclusion of dispersion interactions for evaluating the adsorption capacity of graphitic, sparsely packed materials. In particular we show that, although the commonly used local density approximation (LDA) exchange-correlation functional gives reasonable H$_2$-graphene separation distances, these interactions are in fact too strong and decrease too rapidly as the H$_2$-graphene distance increases. On the other hand, calculations employing the generalized gradient approximation (GGA) for exchange and correlation exhibit very little binding. The vdW-DF$^{\rm C09x}$ functional, however, gives binding very similar to benchmark second-order M$\o$ller-Plesset (MP2) theory results for the H$_2$-coronene interaction and has an appropriate long range interaction with the graphene sheet. This shortcoming of the LDA and GGA functionals is shown to have significant consequences on the overall adsorption densities of H$_2$ near the graphene, thus emphasizing the fundamental importance of properly characterizing the interactions of adsorbed molecules in porous media.

08 HYDROGEN↗

Synthesis of Co-containing mesoporous carbon foams using a new cobalt-oxo cluster as a precursor

A novel trinuclear cobalt-oxo cluster 2[Co{sub 3}O(Ac){sub 6}(H{sub 2}O){sub 3}]{center_dot}H{sub 2}O (Co-OXO) has been obtained and characterized by X-ray single-crystal diffraction and elemental analysis. The structure of Co-OXO displays 3D supramolecular networks through hydrogen bonds and generates boron nitride (bnn) topology. Co-OXO was further used as a precursor to synthesize Co-containing mesoporous carbon foams (Co-MCFs), which exhibit highly ordered mesostructure with specific surface area of 614 m{sup 2} g{sup -1} and uniform pore size of 2.7 nm. Charge-discharge tests show that the specific discharge capacitance of Co-MCFs is 7% higher than that of the MCFs at the current density of 100 mA g{sup -1}, and 26% higher than that of MCFs at the current density of 3 A g{sup -1}. The electrochemical behaviors of Co-MCFs are obviously improved due to the improved wettability, increased graphitization degree and the pseudo-capacitance through additional faradic reactions arising from cobalt. - Graphical Abstract: A new trinuclear cobalt-oxo cluster, 2[Co{sub 3}O(Ac){sub 6}(H{sub 2}O){sub 3}]{center_dot}H{sub 2}O (1), was obtained and further used as a precursor to synthesize Co-containing mesoporous carbon foams (Co-MCFs) which exhibit improved electrochemical behaviors. Highlights: Black-Right-Pointing-Pointer A new trinuclear cobalt-oxo cluster (1) were obtained. Black-Right-Pointing-Pointer 1 is joined by hydrogen bonds to construct a 3D structure showing bnn topology. Black-Right-Pointing-Pointer 1 was further used to obtain Co-containing mesoporous carbon foams (Co-MCFs). Black-Right-Pointing-Pointer Co-MCFs exhibit highly ordered mesostructure and uniform pore sizes. Black-Right-Pointing-Pointer Electrochemical behaviors of Co-MCFs are obviously improved compared with pure MCFs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Evaluation of Vapor Pressure and Ultra-High Vacuum Tribological Properties of Ionic Liquids (2) Mixtures and Additives

Ionic liquids are salts, many of which are typically viscous fluids at room temperature. The fluids are characterized by negligible vapor pressures under ambient conditions. These properties have led us to study the effectiveness of ionic liquids containing both organic cations and anions for use as space lubricants. In the previous paper we have measured the vapor pressure and some tribological properties of two distinct ionic liquids under simulated space conditions. In this paper we will present vapor pressure measurements for two new ionic liquids and friction coefficient data for boundary lubrication conditions in a spiral orbit tribometer using stainless steel tribocouples. In addition we present the first tribological data on mixed ionic liquids and an ionic liquid additive. Post mortem infrared and Raman analysis of the balls and races indicates the major degradation pathway for these two organic ionic liquids is similar to those of other carbon based lubricants, i.e. deterioration of the organic structure into amorphous graphitic carbon. The coefficients of friction and lifetimes of these lubricants are comparable to or exceed these properties for several commonly used space oils.

Morales, Wilfredo↗

Using In Situ High-Energy X-ray Diffraction to Quantify Electrode Behavior of Li-Ion Batteries from Extreme Fast Charging

Extreme fast charging (XFC, =15 min charging time) of Li-ion batteries (LIBs) has been proposed as an immediate target to increase the commercial appeal of electric vehicles. However, XFC of LIBs is associated with the degradation of battery performance and safety concerns. Quantitative and simultaneous characterization of various components during cell degradation represents a major experimental challenge. In this work, we outline a methodology for the use of spatially resolved, high-energy X-ray diffraction as a quantitative, in situ method of mapping the degradation of LIBs. We use this approach to study the battery cell capacity loss, both locally (mm scale) and globally over the entire cell (cm scale). Specifically, our workflow allows us to quantify the total amount of plated Li on the anode, as well as its spatial correlation to the structural properties of the anode and cathode. The method complements existing optical methods to resolve the spatial heterogeneity of local degradation mechanisms such as Li plating and provides simultaneous insights into concomitant anode state-of-charge variability. We apply it to commercially relevant single-layer pouch cells with the graphite anode and the LiNi 0.5 Mn 0.3 Co 0.2 O 2 cathode. Our results show that Li plating occurs heterogeneously on the graphite anode and that it is spatially correlated to the extent of anode lithiation. In this work, we anticipate that the described workflow will allow for understanding multiscale degradation in energy-storage devices beyond LIBs, where quantitative analysis at a local and global length scale can be performed without the necessity to tear down the device, due to the applicability of high-energy X-rays to probe in situ degradation.

25 ENERGY STORAGE↗

Overview of diagnostic performance and results for the first operation phase in Wendelstein 7-X (invited)

Wendelstein 7-X, a superconducting optimized stellarator built in Greifswald/Germany, started its first plasmas with the last closed flux surface (LCFS) defined by 5 uncooled graphite limiters in December 2015. At the end of the 10 weeks long experimental campaign (OP1.1) more than 20 independent diagnostic systems were in operation, allowing detailed studies of many interesting plasma phenomena. For example, fast neutral gas manometers supported by video cameras (including one fast-frame camera with frame rates of tens of kHz) as well as visible cameras with different interference filters, with field of views covering all ten half-modules of the stellarator, discovered a MARFE-like radiation zone on the inboard side of machine module 4. This structure is presumably triggered by an inadvertent plasma-wall interaction in module 4 resulting in a high impurity influx that terminates some discharges by radiation cooling. The main plasma parameters achieved in OP1.1 exceeded predicted values in discharges of a length reaching 6 s. Although OP1.1 is characterized by short pulses, many of the diagnostics are already designed for quasi-steady state operation of 30 min discharges heated at 10 MW of ECRH. Finally, an overview of diagnostic performance for OP1.1 is given, including some highlights from the physics campaigns.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

High Temperature Mechanical Characterization of Ceramic Matrix Composites

A high temperature mechanical characterization laboratory has been assembled at NASA Lewis Research Center. One contribution of this work is to test ceramic matrix composite specimens in tension in environmental extremes. Two high temperature tensile testing systems were assembled. The systems were assembled based on the performance and experience of other laboratories and meeting projected service conditions for the materials in question. The systems use frames with an electric actuator and a center screw. A PC based data acquisition and analysis system is used to collect and analyze the data. Mechanical extensometers are used to measure specimen strain. Thermocouples, placed near the specimen, are used to measure the specimen gage section temperature. The system for testing in air has a resistance element furnace with molybdenum disilicide elements and pneumatic grips with water cooling attached to hydraulic alignment devices. The system for testing in an inert gas has a graphite resistance element furnace in a chamber with rigidly mounted, water cooled, hydraulically actuated grips. Unidirectional SiC fiber reinforced reaction bonded Si3N4 and triaxially woven, two dimensional, SiC fiber reinforced enhanced SiC composites were tested in unidirectional tension. Theories for predicting the Young's modulus, modulus near the ultimate strength, first matrix cracking stress, and ultimate strength were applied and evaluated for suitability in predicting the mechanical behavior of SiC/RBSN and enhanced SiC/SiC composites. The SiC/RBSN composite exhibited pseudo tough behavior (increased area under the stress/strain curve) from 22 C to 1500 C. The rule of mixtures provides a good estimate of the Young's modulus of the SiC/RBSN composite using the constituent properties from room temperature to 1440 C for short term static tensile tests in air or nitrogen. The rule of mixtures significantly overestimates the secondary modulus near the ultimate strength. The ACK theory provides the best approximation of the first matrix cracking stress when residual stresses are ignored. The theory of Cao and Thouless, based on Weibull statistics, gave the best prediction for the composite ultimate strength. The enhanced SiC/SiC composite exhibited nonlinear stress/strain behavior from 24 C to 1370 C in air with increased ultimate strain when compared to monolithic SiC. The theory of Yang and Chou with the assumption of a frictional fiber/matrix interface provided the best estimate of the Young's modulus. The theory of Cao and Thouless gave the best estimate for the ultimate strength.

Gyekenyesi, John Z.↗

Materials for Advanced Ultrasupercritical Steam Turbines Task 4: Cast Superalloy Development

The Steam Turbine critical stationary structural components are high integrity Large Shell and Valve Casing heavy section Castings, containing high temperature steam under high pressures. Hence to support the development of advanced materials technology for use in an AUSC steam turbine capable of operating with steam conditions of 760°C (1400°F) and 35 Mpa (5000 psia), Casting alloy selection and evaluation of mechanical, metallurgical properties and castability with robust manufacturing methods are mandated. Alloy down select from Phase 1 based on producability criteria and creep rupture properties tested by NETL-Albany and ORNL directed the consortium to investigate cast properties of Haynes 282 and Haynes 263. The goals of Task 4 in Phase 2 are to understand a broader range of mechanical properties, the impact of manufacturing variables on those properties. Scale up the size of heats to production levels to facilitate the understanding of the impact of heat and component weight, on metallurgical and mechanical behavior. GE Power & Water Materials and Processes Engineering for the Phase 2, Task 4.0 Castings work, systematically designed and executed casting material property evaluation, multiple test programs. Starting from 15 lbs. cylinder castings to world’s first 17,000 lbs. poured weight, heavy section large steam turbine partial valve Haynes 282 super alloy casting. This has demonstrated scalability of the material for steam Turbine applications. Activities under Task 4.0, Investigated and characterized various mechanical properties of Cast Haynes 282 and Cast Nimonic 263. The development stages involved were: 1) Small Cast Evaluation: 4 inch diam. Haynes 282 and Nimonic 263 Cylinders. This provided effects of liquidus super heat range and first baseline mechanical data on cast versions of conventional vacuum re-melted and forged Ni based super alloys. 2) Step block castings of 300 lbs. and 600 lbs. Haynes 282 from 2 foundry heats were evaluated which demonstrated the importance of proper heat treat cycles for Homogenization, and Solutionizing parameters selection and implementation. 3) Step blocks casting of Nimonic 263: Carried out casting solidification simulation analysis, NDT inspection methods evaluation, detailed test matrix for Chemical, Tensile, LCF, stress rupture, CVN impact, hardness and J1C Fracture toughness section sensitivity data and were reported. 4) Centrifugal Casting of Haynes 282, weighing 1400 lbs. with hybrid mold (half Graphite and half Chromite sand) mold assembly was cast using compressor casing production tooling. This test provided Mold cooling rates influence on centrifugally cast microstructure and mechanical properties. Graphite mold section out performs sand mold across all temperatures for 0.2% YS; %Elongation, %RA, UTS at 1400°F. Both Stress-LMP and conditional Fracture toughness plots data were in the scatter band of the wrought alloy. 5) Fundamental Studies on Cooling rates and SDAS test program. Evaluated the influence of 6 mold materials Silica, Chromite, Alumina, Silica with Indirect Chills, Zircon and Graphite on casting solidification cooling rates. Actual Casting cooling rates through Liquidus to Solidus phase transition were measured with 3 different locations based thermocouples placed in each mold. Compared with solidification simulation cooling rates and measurement of SDAS, microstructure features were reported. The test results provided engineered casting potential methods, applicable for heavy section Haynes 282 castings for optimal properties, with foundry process methods and tools. 6) Large casting of Haynes 282 Drawings and Engineering FEM models and supplemental requirements with applicable specifications were provided to suppliers for the steam turbine proto type feature valve casing casting. Molding, melting and casting pouring completed per approved Manufacturing Process Plan during 2014 Q4. The partial valve casing was successfully cast after casting methods were validated with solidification simulation analysis and the casting met NDT inspection and acceptance criteria. Heat treated and sectioned to extract trepan samples at different locations comparing with cast on coupons test data. Material properties requisite for design, such as tensile, creep/rupture, LCF, Fracture Toughness, Charpy V-notch chemical analysis testing were carried out. The test results will be presented in the final report. The typical Haynes 282 large size Steam Turbine production casting from Order to Delivery foundry schedule with the activity break up is shown in Figures 107 and 108. • From Purchase Order placement to Casting pouring ~ 26 weeks. 1. Sales and commercial review 3 2. Engineering Drawings/models review 4 3. Pattern and core box manufacturing 6 4. Casting process engineering review 4 5. FEM and solidification simulation analysis 4 6. Gating & Feeder Attachments, Ceramic tiling 2 7. Molding and coremaking production scheduling 6 8. Melting planning and schedule 3 9. Pouring, cooling and shake out 2 • From Pouring to casting Delivery ~ 29 weeks 10. Shot blast and riser cutting, gates removal 3 11. Homogenizing , solutionizing HT furnace prep 4 12. Grinding, Fettling 2 13. Aging HT Cycle, cooling 2 14. VT and LPT NDT inspections 2 15. Radiographic inspection 4 16. Mechanical testing, Chemical analysis test certs 4 17. Casting weld repair upgrades and Aging PWHT 4 18. NDT after weld repairs and casting upgrades 3 19. Casting Final Inspection and test certifications 3 20. Package and delivery 2 Hence the Total Lead time from P.O to Casting delivery is approximately 55 weeks. The Task 4.2 and Task 4.3 activities and reporting completed.

Thangirala, Mani↗

Imaging Local Electronic Corrugations and Doped Regions in Graphene

Electronic structure heterogeneities are ubiquitous in two-dimensional graphene and profoundly impact the transport properties of this material. Here we show the mapping of discrete electronic domains within a single graphene sheet using scanning transmission X-ray microscopy in conjunction with ab initio density functional theory calculations. Scanning transmission X-ray microscopy imaging provides a wealth of detail regarding the extent to which the unoccupied levels of graphene are modified by corrugation, doping and adventitious impurities, as a result of synthesis and processing. Local electronic corrugations, visualized as distortions of the {pi}*cloud, have been imaged alongside inhomogeneously doped regions characterized by distinctive spectral signatures of altered unoccupied density of states. The combination of density functional theory calculations, scanning transmission X-ray microscopy imaging, and in situ near-edge X-ray absorption fine structure spectroscopy experiments also provide resolution of a longstanding debate in the literature regarding the spectral assignments of pre-edge and interlayer states.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of purity, edge length, and growth area on field emission of multi-walled carbon nanotube emitter arrays

Present report aims to study the effect of purity, edge length, and growth area on field emission of patterned carbon nanotube (CNT) emitter arrays. For development of four CNT emitter arrays (CEAs), low resistively silicon substrates were coated with thin film of iron catalyst using photolithography, sputtering, and lift off process. Four CEAs were synthesized on these substrates using thermal chemical vapor deposition with minor changes in pretreatment duration. Out of these, two CEAs have 10 {mu}m Multiplication-Sign 10 {mu}m and 40 {mu}m Multiplication-Sign 40 {mu}m solid square dots of CNTs with constant 20 {mu}m inter-dot separation. Other two CEAs have ring square bundles of CNTs and these CEAs are envisioned as 10 {mu}m Multiplication-Sign 10 {mu}m square dots with 4 {mu}m Multiplication-Sign 4 {mu}m scooped out area and 15 {mu}m Multiplication-Sign 15 {mu}m square dots with 5 {mu}m Multiplication-Sign 5 {mu}m lift out area with constant 20 {mu}m inter-dot spacing. Solid square dot structures have exactly constant edge length per unit area with more than four-fold difference in CNT growth area however ring square dot patterns have minor difference in edge length per unit area with approximately two times difference in CNT growth area. Quality and morphology of synthesized CEAs were assessed by scanning electron microscope and Raman characterization which confirm major differences. Field emission of all CEAs was carried out under same vacuum condition and constant inter-electrode separation. Field emission of solid square dot CEAs show approximately identical current density-electric field curves and Fowler-Nordheim plots with little difference in emission current density at same electric field. Similar results were observed for ring square structure CEAs when compared separately. Maximum emission current density observed from these four CEAs reduces from 14.53, 12.23, 11.01, to 8.66 mA/cm{sup 2} at a constant electric field of 5 V/{mu}m, according to edge length of 1361.7, 1221.08, 872.20, to 872.16 mm rather than growth area and purity. Although, the 40 {mu}m Multiplication-Sign 40 {mu}m CEAs possessed highest CNT growth area of 8.7 mm{sup 2} and best purity defined in terms of lowest defect band to graphitic band ratio of 0.614, the current observed from this CEAs was least.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Highly concentrated nebular noble gases in porous nanocarbon separates from the Saratov (L4) meteorite

The majority of heavy noble gases (Ar, Kr, and Xe) in primitive meteorites are stored in a poorly understood phase called Q. Although Q is thought to be carbonaceous, the full identity of the phase has remained elusive for almost four decades. In order to better characterize phase Q and, in turn, the early solar nebula, we separated carbon-rich fractions from the Saratov (L4) meteorite. We chose this meteorite because Q is most resistant in thermal alteration among carbonaceous noble gas carriers in meteorites and we hoped that, in this highly metamorphosed meteorite, Q would be present but not diamond: these two phases are very difficult to separate from each other. One of the fractions, AJ, has the highest {sup 132}Xe concentration of 2.1 × 10{sup –6} cm{sup 3} STP g{sup –1}, exceeding any Q-rich fractions that have yet been analyzed. Transmission electron microscopy studies of the fraction AJ and a less Q-rich fraction AI indicate that they both are primarily porous carbon that consists of domains with short-range graphene orders, with variable packing in three dimensions, but no long-range graphitic order. The relative abundance of Xe and C atoms (6:10{sup 9}) in the separates indicates that individual noble gas atoms are associated with only a minor component of the porous carbon, possibly one or more specific arrangements of the nanoparticulate graphene.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The History of Presolar Grains

Below we summarize the results of our investigations into the history of presolar grains that were conducted in the last year. During this time we have expended much of our effort in the development of experimental techniques and sample preparation methods that are needed to laboratory in December, 2000. Specific information on this instrument is contained in the Full Proposal of PI Ernst Zinner and will not be repeated here. Our general strategy in the past year has been in large measure to explore novel sample handling methods for the very small (sub-micron), but more representative, presolar grains that can now be characterized isotopically in the NanoSIMS. We have developed experimental techniques that will permit NanoSIMS analyses of the very same ultramicrotome sections studied in the TEM, and we have developed grain dispersion, handling and mounting techniques that permit NanoSIMS isotopic analysis as well as field emission SEM, high energy TEM, and atomic force microscopy of pristine presolar grains. Although much of this has been slow and very difficult work that has no immediate payoff in terms of publishable results, we considered it absolutely necessary groundwork for future discoveries, especially in the realm of individual presolar grains that have been inaccessible to past studies due to size constraints. As discussed below, we have been largely successful in these endeavors, and expect to reap the benefits of this work in the next year. We also report on our continued morphologic studies of pristine presolar grains, on our investigations of presolar graphite grains from supernovae as well as on rarer types of presotar SIC, on the search for presolar silicates, and on our efforts to obtain direct size-distribution information on presolar SiC through X-ray mapping techniques.

Bernatowicz, Thomas J.↗

USING A NEW FINITE SLIT PORE MODEL FOR NLDFT ANALYSIS OF CARBON PORE STRUCTURE

In this work, we present a model for analyzing activated carbon micropore structures based on graphene sheet walls of finite thickness and extent. This is a two-dimensional modification of the widely used infinite slit pore model that assumes graphite-like infinitely extended pore walls. The proposed model has two versions: (1) a strip pore constructed with graphene strip walls that have finite length L in the x direction and are infinite in the y direction. Strip pores are open on both sides in the x direction. (2) A channel pore is a strip pore partially closed along one edge by a perpendicularly oriented graphene wall. This more realistic model allows pore termination via both physical pore entrances and pore blockage. The model consequently introduces heterogeneity of the adsorption potential that is reduced near pore entrances and enhanced near corners of pore walls. These energetically heterogeneous structures fill with adsorbate more gradually than homogeneous pores of the same width. As a result, the calculated adsorption isotherms are smoother and less steep for the finite versus the infinite pore model. In the application of this model for carbon characterization it is necessary to make an assumption about the pore length. In this work we made this assumption based on the high resolution scanning transmission electron microscopy (STEM) results. We find the agreement between the experiment and the model significantly better for the finite than for the infinite pore model.

54 ENVIRONMENTAL SCIENCES↗

Ultra-high modulus organic fiber hybrid composites

An experimental organic fiber, designated Fiber D, was characterized, and its performance as a reinforcement for composites was investigated. The fiber has a modulus of 172 GPa, tensile strength of 3.14 GPa, and density of 1.46 gm/cu cm. Unidirectional Fiber D/epoxy laminates containing 60 percent fiber by volume were evaluated in flexure, shear, and compression, at room temperature and 121 C in both the as fabricated condition and after humidity aging for 14 days at 95 percent RH and 82 C. A modulus of 94.1 GPa, flexure strength of 700 MPa, shear strength of 54 MPa, and compressive strength of 232 MPa were observed at room temperature. The as-fabricated composites at elevated temperature and humidity aged material at room temperature had properties 1 to 20 percent below these values. Combined humidity aging plus evaluated temperature testing resulted in even lower mechanical properties. Hybrid composite laminates of Fiber D with Fiber FP alumina or Thornel 300 graphite fiber were also evaluated and significant increases in modulus, flexure, and compressive strengths were observed.

Champion, A. R.↗