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DOE OSTI2014

Further developments of capillary absorption spectrometers using small hollow-waveguide fibers

Our objective is to enhance quantification of stable carbon and oxygen isotope ratios to better than 1‰ relative isotope precision for sample sizes < 1 pico-mole. A newer variant Capillary Absorption Spectrometer (CAS) is described using a proprietary linear-taper hollow waveguide in conjunction with wavelength and frequency modulation techniques of tunable laser absorption spectrometry. Previous work used circular capillaries with uniform 1 mm ID to measure 13C/12C ratios with ≥ 20 pico-mole samples to ≤ 10 ppm (1‰ precision against standards) [1]. While performing fairly well, it generated residual modal noise due to multipath propagation in the hollow-waveguides (HWGs). This system has been utilized with laser ablation-catalytic combustion techniques to analyze small resolution (~ 25 μm spot diameter) laser ablation events on solids. Using smaller ID capillary waveguides could improve detection limits and spatial resolutions. Reducing an IR compatible hollow waveguide’s inner diameter (ID) to < 300 μm, reduces modal noise significantly for mid-IR operation, but feedback noise with high gain semiconductor lasers can become problematic. A proprietary linear-taper small waveguide (mean ID = 0.35 mm, L = 1 m) was tested to understand whether modal noise and optical feedback effects could be simultaneously reduced. We see better mode filtering and, significant reductions of feedback noise under favorable coupling of a multi-spatial mode QC laser to the smaller ID of the linear-tapered HWG. We demonstrate that better modal coupling operation is consistent with Liouville’s theorem, where greater suppression of feedback from spurious scatter within the HWG occurs by injecting the laser into the smaller ID port. Our progress on developing lighter weight, potentially fieldable alternatives to Isotope Ratio Mass Spectrometers (IRMS) with a small volume (≤ 0.1 cm3) CAS system will be discussed and compared to other competitive systems.

Kelly, James F.↗

NASA NTRS1981

Radiance profile enhancement for solar occultation measurements

It is pointed out that distortions in received signals in solar occultation measurements made from space derive from the systematic motion of the electrooptical sensor. In a wide range of cases, the motion-related signal distortions brought about by the instrument's full modulation transfer function are as important as those from the optics. It is shown through simulation that existing techniques in the field of digital-image processing can be applied directly to solar occultation experiments to correct for these distortions. The resulting enhanced radiation profile is found to be much closer to the true radiance profile than is the sampled output of the instrument.

Gomberg, R. I.↗

NASA NTRS1990

A fiber optic sensor for noncontact measurement of shaft speed, torque, and power

A fiber optic sensor which enables noncontact measurement of the speed, torque and power of a rotating shaft was fabricated and tested. The sensor provides a direct measurement of shaft rotational speed and shaft angular twist, from which torque and power can be determined. Angles of twist between 0.005 and 10 degrees were measured. Sensor resolution is limited by the sampling rate of the analog to digital converter, while accuracy is dependent on the spot size of the focused beam on the shaft. Increasing the sampling rate improves measurement resolution, and decreasing the focused spot size increases accuracy. Digital processing allows for enhancement of an electronically or optically degraded signal.

Madzsar, George C.↗

NASA NTRS1990

A fiber optic sensor for noncontact measurement of shaft speed, torque and power

Madzsar, George C.↗

NASA NTRS1992

Free-volume characteristics of epoxies

Positron annihilation spectroscopy was used to measure free-volume characteristics of selected epoxies. Fluorene resins, a new family of high-temperature thermosetting resins, were selected as the test medium. Experimental results indicate that the free-volume cell size V sub f varies with the molecular weight between the cross-links M sub c according to an equation of the form V sub f = AM sub c sup B, where A and B are structural constants. In two of the samples, the concentration of bulky fluorene groups was increased in the network backbone by replacement of some of the conventional bisphenol A epoxy resin with fluorene-derived epoxy resin. This resulted in an increase in their glass transition temperature for a given level of cross-linking. It was found that in these samples, the Doppler broadening of the annihilation peak decreases with the increasing fluorene content, presumably due to enhanced damping of the chain motions.

Singh, Jag J.↗

NASA NTRS1993

Real-time qualitative reasoning for telerobotic systems

This paper discusses the sensor-based telerobotic driving of a car in a-priori unknown environments using 'human-like' reasoning schemes implemented on custom-designed VLSI fuzzy inferencing boards. These boards use the Fuzzy Set theoretic framework to allow very vast (30 kHz) processing of full sets of information that are expressed in qualitative form using membership functions. The sensor-based and fuzzy inferencing system was incorporated on an outdoor test-bed platform to investigate two control modes for driving a car on the basis of very sparse and imprecise range data. In the first mode, the car navigates fully autonomously to a goal specified by the operator, while in the second mode, the system acts as a telerobotic driver's aid providing the driver with linguistic (fuzzy) commands to turn left or right, speed up, slow down, stop, or back up depending on the obstacles perceived by the sensors. Indoor and outdoor experiments with both modes of control are described in which the system uses only three acoustic range (sonar) sensor channels to perceive the environment. Sample results are presented that illustrate the feasibility of developing autonomous navigation modules and robust, safety-enhancing driver's aids for telerobotic systems using the new fuzzy inferencing VLSI hardware and 'human-like' reasoning schemes.

Pin, Eancois G.↗

NASA NTRS1993

Flame trench analysis of NLS vehicles

The present study takes the initial steps of establishing a better flame trench design criteria for future National Launch System vehicles. A three-dimensional finite element computer model for predicting the transient thermal and structural behavior of the flame trench walls was developed using both I-DEAS and MSC/NASTRAN software packages. The results of JANNAF Standardized Plume flowfield calculations of sea-level exhaust plume of the Space Shuttle Main Engine (SSME), Space Transportation Main Engine (STME), and Advanced Solid Rocket Motors (ASRM) were analyzed for different axial distances. The results of sample calculations, using the developed finite element model, are included. The further suggestions are also reported for enhancing the overall analysis of the flame trench model.

Zeytinoglu, Nuri↗

NASA NTRS2001

Microbial detection with low molecular weight RNA

The need to monitor microorganisms in the environment has increased interest in assays based on hybridization probes that target nucleic acids (e.g., rRNA). We report the development of liquid-phase assays for specific bacterial 5S rRNA sequences or similarly sized artificial RNAs (aRNAs) using molecular beacon technology. These beacons fluoresce only in the presence of specific target sequences, rendering as much as a 27-fold fluorescence enhancement. The assays can be used with both crude cell lysates and purified total RNA preparations. Minimal sample preparation (e.g., heating to promote leakage from cells) is sufficient to detect many Gram-negative bacteria. Using this approach it was possible to detect an aRNA-labeled Escherichia coli strain in the presence of a large background of an otherwise identical E. coli strain. Finally, by using a longer wavelength carboxytetramethylrhodamine beacon it was possible to reduce the fraction of the signal due to cellular autofluorescence to below 0.5%.

NASA Discipline Life Sciences Technologies↗

NASA NTRS2004

OVOC (Oxygenated Volatile Organic Chemicals) in the Global Atmosphere: Atmospheric Budgets, Oceanic Concentrations, and Uncertainties

Airborne measurements of oxygenated volatile organic chemicals (OVOC), OH free radicals, and tracers of pollution were performed over the Pacific during Winter/Spring of 2001. Large concentrations of OVOC are present in the global troposphere and are expected to play an important role in atmospheric chemistry. Their total abundance (SIGMAOVOC) was nearly twice that of non-methane hydrocarbons (SIGMAC2-C8 NMHC). Throughout the troposphere, the OH reactivity of OVOC is comparable to that of methane and far exceeds that of NHMC. A comparison of these data with western Pacific observations collected some seven years earlier (Feb.-March, 1994) did not reveal significant differences. Analysis of the relative enhancement of selected OVOC with respect to CH3Cl and CO in twelve plumes originating from fires and sampled in the free troposphere (3-11 km) is used to assess their primary and secondary emissions from biomass combustion. The composition of these plumes also indicates a large shift of reactive nitrogen into the PAN reservoir thereby limiting ozone formation. These data are combined with other observations and interpreted with the help of a global 3-D model to assess OVOC global sources and sinks. We further interpret atmospheric observations with the help of an air-sea exchange model io show that oceans can be both net so~rces and sinks. An extremely large oceanic reservoir of OVOC, that exceeds the atmospheric reservoir by more than an order of magnitude, can be inferred to be present. We conclude that OVOC sources are extremely large (150-500 TgC y-1) but remain poorly quantified. In many cases, measured concentrations are uncertain and incompatible with our present knowledge of atmospheric chemistry. Results based on observations from several field studies and critical gaps will be discussed.

Singh, Hanwant B.↗

NASA NTRS2005

Extracting trends from two decades of microgravity macromolecular crystallization history

Since the 1980s hundreds of macromolecular crystal growth experiments have been performed in the reduced acceleration environment of an orbiting spacecraft. Significant enhancements in structural knowledge have resulted from X-ray diffraction of the crystals grown. Similarly, many samples have shown no improvement or degradation in comparison to those grown on the ground. A complex series of interrelated factors affect these experiments and by building a comprehensive archive of the results it was aimed to identify factors that result in success and those that result in failure. Specifically, it was found that dedicated microgravity missions increase the chance of success when compared with those where crystallization took place as a parasitic aspect of the mission. It was also found that the chance of success could not be predicted based on any discernible property of the macromolecule available to us.

Review↗

NASA NTRS2004

Analysis of the Atmospheric Distribution, Sources, and Sinks of Oxygenated Volatile Organic Chemicals Based on Measurements over the Pacific during TRACE-P

Airborne measurements of a large number of oxygenated volatile organic chemicals (OVOC) were carried out in the Pacific troposphere (0.1-12 km) in winter/spring of 2001 (24 February to 10 April). Specifically, these measurements included acetone (CH3COCH3), methylethyl ketone (CH3COC2H5, MEK), methanol (CH3OH), ethanol (C2H5OH), acetaldehyde (CH3CHO), propionaldehyde (C2H5CHO), peroxyacylnitrates (PANs) (C(sub n)H(sub 2n+1)COO2NO2), and organic nitrates (C(sub n)H(sub 2n+1)ONO2). Complementary measurements of formaldehyde (HCHO), methyl hydroperoxide (CH3OOH), and selected tracers were also available. OVOC were abundant in the clean troposphere and were greatly enhanced in the outflow regions from Asia. Background mixing ratios were typically highest in the lower troposphere and declined toward the upper troposphere and the lowermost stratosphere. Their total abundance (Summation of OVOC) was nearly twice that of nonmethane hydrocarbons (Summation of C2-C8 NMHC). Throughout the troposphere, the OH reactivity of OVOC is comparable to that of methane and far exceeds that of NMHC. A comparison of these data with western Pacific observations collected some 7 years earlier (February-March 1994) did not reveal significant differences. Mixing ratios of OVOC were strongly correlated with each other as well as with tracers of fossil and biomass/biofuel combustion. Analysis of the relative enhancement of selected OVOC with respect to CH3Cl and CO in 12 plumes originating from fires and sampled in the free troposphere (3-11 km) is used to assess their primary and secondary emissions from biomass combustion. The composition of these plumes also indicates a large shift of reactive nitrogen into the PAN reservoir thereby limiting ozone formation. A three-dimensional global model that uses state of the art chemistry and source information is used to compare measured and simulated mixing ratios of selected OVOC. While there is reasonable agreement in many cases, measured aldehyde concentrations are significantly larger than predicted. At their observed levels, acetaldehyde mixing ratios are shown to be an important source of HCHO (and HO x ) and PAN in the troposphere. On the basis of presently known chemistry, measured mixing ratios of aldehydes and PANs are mutually incompatible. We provide rough estimates of the global sources of several OVOC and conclude that collectively these are extremely large (150-500 Tg C / yr) but remain poorly quantified.

Singh, H. B.↗

NASA NTRS2007

Nanoscale Subsurface Imaging via Resonant Difference-Frequency Atomic Force Ultrasonic Microscopy

A novel scanning probe microscope methodology has been developed that employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope, driven at a frequency differing from the ultrasonic frequency by the fundamental resonance frequency of the cantilever, engages the sample top surface. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave in the region defined by the cantilever tip-sample surface interaction force generates difference-frequency oscillations at the cantilever fundamental resonance. The resonance-enhanced difference-frequency signals are used to create images of embedded nanoscale features.

Cantrell, Sean A.↗

NASA NTRS2010

Process to Selectively Distinguish Viable from Non-Viable Bacterial Cells

The combination of ethidium monoazide (EMA) and post-fragmentation, randomly primed DNA amplification technologies will enhance the analytical capability to discern viable from non-viable bacterial cells in spacecraft-related samples. Intercalating agents have been widely used since the inception of molecular biology to stain and visualize nucleic acids. Only recently, intercalating agents such as EMA have been exploited to selectively distinguish viable from dead bacterial cells. Intercalating dyes can only penetrate the membranes of dead cells. Once through the membrane and actually inside the cell, they intercalate DNA and, upon photolysis with visible light, produce stable DNA monoadducts. Once the DNA is crosslinked, it becomes insoluble and unable to be fragmented for post-fragmentation, randomly primed DNA library formation. Viable organisms DNA remains unaffected by the intercalating agents, allowing for amplification via post-fragmentation, randomly primed technologies. This results in the ability to carry out downstream nucleic acid-based analyses on viable microbes to the exclusion of all non-viable cells.

LaDuc, Myron T.↗

NASA NTRS2010

Resonant difference-frequency atomic force ultrasonic microscope

A scanning probe microscope and methodology called resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope, driven at a frequency differing from the ultrasonic frequency by one of the contact resonance frequencies of the cantilever, engages the sample top surface. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave in the region defined by the cantilever tip-sample surface interaction force generates difference-frequency oscillations at the cantilever contact resonance. The resonance-enhanced difference-frequency signals are used to create images of nanoscale near-surface and subsurface features.

Cantrell, John H.↗

DOE OSTI2013

System and method for high precision isotope ratio destructive analysis

A system and process are disclosed that provide high accuracy and high precision destructive analysis measurements for isotope ratio determination of relative isotope abundance distributions in liquids, solids, and particulate samples. The invention utilizes a collinear probe beam to interrogate a laser ablated plume. This invention provides enhanced single-shot detection sensitivity approaching the femtogram range, and isotope ratios that can be determined at approximately 1% or better precision and accuracy (relative standard deviation).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Understanding the Role of Extrinsic Impurities in Bulk Nb SRF Cavities

High gradient and high quality factor superconducting radiofrequency (SRF) cavities are essential for efficient particle acceleration in next-generation accelerators. This work demonstrates that the superconducting performance of bulk niobium can be enhanced through a controlled introduction of interstitial oxygen and nitrogen. Thermal and chemical surface treatments modify the concentration and distribution of these impurities, enabling systematic tuning of SRF cavity performance. By combining cavity RF measurements with quantitative materials characterizations, we isolate the impact of impurity concentration on BCS surface resistance and identify the mechanisms by which interstitial impurities alter the superconducting properties of niobium. We find that nitrogen is an order of magnitude more effective than oxygen in reducing BCS resistance at 16 MV/m and that the reduction arises from a combination of mean free path optimization and superconducting gap enhancement. Using these insights, we develop a predictive model that estimates cavity performance directly from room temperature sample material studies, reducing the reliance on full-scale cryogenic tests for surface treatment development. We then apply this model to explore co-doping strategies, demonstrating that combining interstitial oxygen and nitrogen achieves a synergistic reduction in BCS resistance. These results establish co-doping as a viable path for the development of surface-engineered niobium for future high quality factor SRF applications.

Hu, Hannah [Chicago U.]↗

DOE OSTI2014

Variations of thermoelectric properties of Mg{sub 2.2}Si{sub 1−y}Sn{sub y−0.013}Sb{sub 0.013} materials with different Si/Sn ratios

Mg{sub 2}Si–Mg{sub 2}Sn solid solutions are a promising class of thermoelectric materials. Mg{sub 2.2}Si{sub 1−y}Sn{sub y−0.013}Sb{sub 0.013} compounds with different Si/Sn ratios were prepared by B{sub 2}O{sub 3} “flux” method followed by hot-pressing. The effect of Si/Sn ratio on the thermoelectric properties of the Mg{sub 2}Si–Mg{sub 2}Sn solid solutions at a fixed Sb doping level were measured in the temperature range 300–760 K. With the increase of Sn content (0.3≤y≤0.7), power factors are improved and lattice thermal conductivity decreased. Band convergence induced by Si/Sn ratio leads to enhanced effective mass and the materials parameter β which qualifies a kind of thermoelectric material is improved evidently. A maximum ZT of ∼1.1 at ∼760 K was achieved for the Mg{sub 2.2}Si{sub 0.3}Sn{sub 0.7–0.013}Sb{sub 0.013} sample arising from a high power factor of ∼4×10{sup -3} W m{sup −1} K{sup −2} and a low lattice thermal conductivity of ∼1.6 W m{sup −1} K{sup −1} at ∼760 K. - Graphical abstract: (a)Temperature dependence of power factor of Mg{sub 2.2}Si{sub 1−y}Sn{sub y−0.13}Sb{sub 0.013} samples. (b)Temperature dependence of lattice thermal conductivity of Mg{sub 2.2}Si{sub 1−y}Sn{sub y−0.13}Sb{sub 0.013} samples. (c)Temperature dependence of dimensionless figure of merit ZT of Mg{sub 2.2}Si{sub 1−y}Sn{sub y−0.13}Sb{sub 0.013} samples. - Highlights: • Mg{sub 2.2}Si{sub 1−y}Sn{sub y−0.013}Sb{sub 0.013} was prepared by B{sub 2}O{sub 3} ''flux'' method followed by hot-pressing. • Band convergence leads to enhanced m{sup ⁎} and improved materials parameter β. • ZT{sub max} of ∼1.1 at ∼760 K was achieved for the Mg{sub 2.2}Si{sub 0.3}Sn{sub 0.7−0.013}Sb{sub 0.013} sample.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Transient Spectroscopy of Glass-Embedded Perovskite Quantum Dots: Novel Structures in an Old Wrapping

Semiconductor doped glasses had been used by the research and engineering communities as color filters or saturable absorbers well before it was realized that their optical properties were defined by tiny specs of semiconductor matter known presently as quantum dots (QDs). Nowadays, the preferred type of QD samples are colloidal particles typically fabricated via organometallic chemical routines that allow for exquisite control of QD morphology, composition and surface properties. However, there is still a number of applications that would benefit from the availability of high-quality glass-based QD samples. These prospective applications include fiber optics, optically pumped lasers and amplifiers and luminescent solar concentrators (LSCs). In addition to being perfect optical materials, glass matrices could help enhance stability of QDs by isolating them from the environment and improving heat exchange with the outside medium. We conduct optical studies of a new type of all-inorganic CsPbBr 3 perovskite QDs fabricated directly in glasses by high-temperature precipitation. These samples are virtually scattering free and exhibit excellent waveguiding properties which makes them well suited for applications in, for example, fiber optics and LSCs. However, the presently existing problem is their fairly low room-temperature emission quantum yields of only ca. 1%–2%. Here we investigate the reasons underlying the limited emissivity of these samples by conducting transient photoluminescence (PL) and absorption measurements across a range of temperatures from 20 to 300K. We observe that the low-temperature PL quantum yield of these samples can be as high as ~25%. However, it quickly drops (in a nearly linear fashion) with increasing temperature. Interestingly, contrary to traditional thermal quenching models, experimental observations cannot be explained in terms of a thermally activated nonradiative rate but rather suggest the existence of two distinct QD sub-ensembles of “emissive” and completely “nonemissive” particles. The temperature-induced variation in the PL efficiency is likely due to a structural transformation of the QD surfaces or interior leading to formation of extremely fast trapping sites or nonemissive phases resulting in conversion of emissive QDs into nonemissive. Thus, future efforts on improving emissivity of glass-based perovskite QD samples might focus on approaches for extending the range of stability of the low-temperature highly emissive structure/phase of the QDs up to room temperature.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗