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At least 343 records · Page 19
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NASA NTRS2000

Structure, Hydrodynamics, and Phase Transition of Freely Suspended Liquid Crystals

Smectic liquid crystals are phases of rod shaped molecules organized into one dimensionally (1D) periodic arrays of layers, each layer being between one and two molecular lengths thick. In the least ordered smectic phases, the smectics A and C, each layer is a two dimensional (2D) liquid. Additionally there are a variety of more ordered smectic phases having hexatic short range translational order or 2D crystalline quasi long range translational order within the layers. The inherent fluid-layer structure and low vapor pressure of smectic liquid crystals enable the long term stabilization of freely suspended, single component, layered fluid films as thin as 30A, a single molecular layer. The layering forces the films to be an integral number of smectic layers thick, quantizing their thickness in layer units and forcing a film of a particular number of layers to be physically homogeneous with respect to its layer structure over its entire area. Optical reflectivity enables the precise determination of the number of layers. These ultrathin freely suspended liquid crystal films are structures of fundamental interest in condensed matter and fluid physics. They are the thinnest known stable condensed phase fluid structures and have the largest surface-to-volume ratio of any stable fluid preparation, making them ideal for the study of the effects of reduced dimensionality on phase behavior and on fluctuation and interface phenomena. Their low vapor pressure and quantized thickness enable the effective use of microgravity to extend the study of basic capillary phenomena to ultrathin fluid films. Freely suspended films have been a wellspring of new liquid crystal physics. They have been used to provide unique experimental conditions for the study of condensed phase transitions in two dimensions. They are the only system in which the hexatic has been unambiguously identified as a phase of matter, and the only physical system in which fluctuations of a 2D XY system and Kosterlitz Thouless phase transition has been observed and 2D XY quasi long range order verified. Smectic films have enabled the precise determination of smectic layer electron density and positional fluctuation profile and have been used to show that the interlayer interactions in anti-ferroelectric tilted smectics do not extend significantly beyond nearest neighbors. The interactions which are operative in liquid crystals are generally weak in comparison to those in crystalline phases, leading to the facile manipulation of the order in liquid crystals by external agents such as applied fields and surfaces. Effects arising from weak ordering are significantly enhanced in ultrathin free films and filaments wherein the intermolecular coupling is effectively reduced by loss of neighbors. Over the past four years this research, which we now detail, has produced a host of exciting new discoveries and unexpected results, maintaining the position of the study of freely suspended liquid crystal structures as one of most exciting and fruitful areas of complex fluid physics. In addition, several potentially interesting microgravity free film experiments have been identified.

Clark, Noel A.↗
NASA NTRS2000

Phase-Shifting Liquid Crystal Point-Diffraction Interferometry

Microgravity fluid physics experiments frequently measure concentration and temperature. Interferometers such as the Twyman Green illustrated have performed full-field measurement of these quantities. As with most such devices, this interferometer uses a reference path that is not common with the path through the test section. Recombination of the test and reference wavefronts produces interference fringes. Unfortunately, in order to obtain stable fringes, the alignment of both the test and reference paths must be maintained to within a fraction of the wavelength of the light being used for the measurement. Otherwise, the fringes will shift and may disappear. Because these interferometers are extremely sensitive to bumping, jarring and transmitted vibration, they are typically mounted on optical isolation tables. Schlieren deflectometers or the more recent Shack-Hartmann wavefront sensors also measure concentration and temperature in laboratory fluid flows. Ray optics describe the operation of both devices. In a schlieren system, an expanded, collimated beam passes through a test section where refractive index gradients deflect rays. A lens focuses the beam to a filter placed in the rear focal plane of the decollimating lens. In a quantitative color schlieren system, gradients in the index of refraction appear as colors in the field of view due to the action of the color filter. Since sensitivity is a function of the focal length of the decollimating lens, these systems are rather long and filter fabrication and calibration is rather difficult. A Shack-Hartmann wavefront sensor is an array of small lenslets. Typical diameters are on the order of a few hundred microns. Since these lenslets divide the test section into resolution elements, the spatial resolution can be no smaller than an individual lenslet. Such a device was recently used to perform high-speed tomography of heated air exiting a 1.27 cm diameter nozzle. While these wavefront sensors are very compact, the limited spatial resolution and the methods required for data reduction suggest that a more useful instrument needs to be developed. The category of interferometers known as common path interferometers can eliminate much of the vibration sensitivity associated with traditional interferometry as described above. In these devices, division of the amplitude of the wavefront following the test section produces the reference beam. Examples of these instruments include shearing and point diffraction interferometers. In the latter case, shown schematically, a lens focuses light passing through the test section onto a small diffracting object. Such objects are typically either a circle of material on a high quality glass plate or a small sphere in a glass cell. The size of the focused spot is several times larger than the object so that the light not intercepted by the diffracting object forms the test beam while the diffracted light generates a spherical reference beam. While this configuration is mechanically stable, phase shifting one beam with respect to the other is difficult due to the common path. Phase shifting enables extremely accurate measurements of the phase of the interferogram using only gray scale intensity measurements and is the de facto standard of industry. Mercer and Creath 2 demonstrated phase shifting in a point diffraction interferometer using a spherical spacer in a liquid crystal cell as the diffracting object. By changing the voltage across the cell, they were able to shift the phase of the undiffracted beam relative to the reference beam generated by diffraction from the sphere. While they applied this technology to fluid measurements, the device shifted phase so slowly that it was not useful for studying transient phenomena. We have identified several technical problems that precluded operation of the device at video frame rates and intend to solve them to produce a phase-shifting liquid crystal point-diffraction interferometer operating at video frame rates. The first task is to produce high contrast fringes. Since the diffracted beam is much weaker than the transmitted beam, interferograms have poor contrast unless a dye is added to the liquid crystal to reduce the intensity of the undiffracted light. Dyes previously used were not rigorously characterized and suffered from hysteresis in both the initial alignment state of the device and the electro-optic switching characteristics. Hence, our initial effort will identify and characterize dyes that do not suffer from these difficulties and are readily soluble in the liquid crystal host. Since the ultimate goal of this research is to produce interferometers capable of phase shifting at video frame rates, we will quantify the difference in switching times between ferroelectric and nematic liquid crystals. While we have more experience with nematic crystals, they typically switch more slowly than ferroelectric cells. As part of that effort, we will investigate the difference in the modulation of the interferograms as a function of the type of liquid crystal in the cell. Because the temporal switching response of a liquid crystal cell is directly related its thickness, we intend to explore techniques required to produce cells that are as thin as possible. However, the cells must still produce a total phase shift of two pi radians.

Griffin, DeVon W.↗
NASA NTRS1999

Effects of menstrual cycle phase and oral contraceptives on alertness, cognitive performance, and circadian rhythms during sleep deprivation

The influence of menstrual cycle phase and oral contraceptive use on neurobehavioral function and circadian rhythms were studied in healthy young women (n = 25) using a modified constant routine procedure during 24 h of sleep deprivation. Alertness and performance worsened across sleep deprivation and also varied with circadian phase. Entrained circadian rhythms of melatonin and body temperature were evident in women regardless of menstrual phase or oral contraceptive use. No significant difference in melatonin levels, duration, or phase was observed between women in the luteal and follicular phases, whereas oral contraceptives appeared to increase melatonin levels. Temperature levels were higher in the luteal phase and in oral contraceptive users compared to women in the follicular phase. Alertness on the maintenance of wakefulness test and some tests of cognitive performance were poorest for women in the follicular phase especially near the circadian trough of body temperature. These observations suggest that hormonal changes associated with the menstrual cycle and the use of oral contraceptives contribute to changes in nighttime waking neurobehavioral function and temperature level whereas these factors do not appear to affect circadian phase.

NASA Discipline Regulatory Physiology↗
NASA NTRS1996

Adaptation of primate vestibuloocular reflex to altered peripheral vestibular inputs. II Spatiotemporal properties of the adapted slow-phase eye velocity

1. The ability of the vestibuloocular reflex (VOR) to undergo adaptive modification after selective changes in the peripheral vestibular system was investigated in rhesus monkeys by recording three-dimensional eye movements before and after inactivation of selective semicircular canals. In the preceding paper we showed that the horizontal VOR gain evoked by passive yaw oscillations after lateral semicircular canal inactivation recovers gradually over time in a frequency-specific manner. Here we present the spatial tuning of the adapted slow-phase eye velocity and describe its spatiotemporal properties as a function of time after canal inactivation. 2. The spatial organization of the VOR was investigated during oscillations at different head positions in the pitch, roll, and yaw planes, as well as in the right anterior/left posterior and left anterior/right posterior canal planes. Acutely after bilateral inactivation of the lateral semicircular canals, a small horizontal response could still be elicited that peaked during rotations in pitched head positions that would maximally stimulate vertical semicircular canals. In addition, the phase of horizontal slow-phase velocity abruptly reversed through 180 degrees at positions close to upright, similarly to torsional slow-phase velocity. These spatial response properties suggest that the small, residual horizontal response components that are present acutely after plugging of both lateral canals originate from vertical semicircular canal signals. 3. As the horizontal response amplitude increased over time, consistent changes were also observed in the spatiotemporal tuning of horizontal slow-phase velocity. 1) The spatiotemporal response properties of horizontal slow-phase velocity acquired noncosine tuning characteristics, primarily in the pitch plane, in the right anterior/left posterior and left anterior/right posterior canal planes. Accordingly, horizontal response amplitude was nonzero during rotation in any head position in these planes and response phase varied significantly as a function of head orientation. 2) The peak horizontal response amplitude shifted spatially over time, such that 5-10 mo after plugging it was maximal during rotations at head positions close to upright. 4. In parallel to these unique spatiotemporal response properties characterizing the adapted horizontal VOR, torsional slow-phase velocity also exhibited small spatiotemporal changes after lateral canal inactivation that tended to precede in time the changes associated with the horizontal response components. In contrast, vertical slow-phase velocity in the plugged animals was unaltered and continued to be characterized by cosine-tuned spatial properties in three dimensions. 5. Recovery of the horizontal response gain during yaw oscillations in upright position, as well as the unique, noncosine spatiotemporal characteristics of the adapted horizontal VOR, were also observed in an animal with all but one vertical semicircular canals inactivated. There was, however, no sign of VOR gain recovery up to 2 mo after all semicircular canals were inactivated. These results suggest that the observed recovery of horizontal VOR is at least partly due to signals originating from the remaining intact vertical canal(s). Even in the presence of a single intact vertical canal, the improvement in horizontal gaze stability is at least partly restored through spatiotemporal changes in the processing of vestibuloocular signals that improve the gain and spatial tuning of horizontal VOR at the expense of temporal response properties.

NASA Discipline Number 16-10↗
NASA NTRS2005

Phase-Imaging with a Sharpened Multi-Walled Carbon Nanotube AFM Tip: Investigation of Low-k Dielectric Polymer Hybrids

Phase shift tapping mode scanning force microscopy (TMSFM) has evolved into a very powerful technique for the nanoscale surface characterization of compositional variations in heterogeneous samples. Phase shift signal measures the difference between the phase angle of the excitation signal and the phase angle of the cantilever response. The signal correlates to the tip-sample inelastic interactions, identifying the different chemical and/or physical property of surfaces. In general, the resolution and quality of scanning probe microscopic images are highly dependent on the size of the scanning probe tip. In improving AFM tip technology, we recently developed a technique for sharpening the tip of a multi-walled carbon nanotube (CNT) AFM tip, reducing the radius of curvature of the CNT tip to less than 5 nm while still maintaining the inherent stability of multi-walled CNT tips. Herein we report the use of sharpened (CNT) AFM tips for phase-imaging of polymer hybrids, a precursor for generating nanoporous low-k dielectrics for on-chip interconnect applications. Using sharpened CNT tips, we obtained phase-contrast images having domains less than 10 nm. In contrast, conventional Si tips and unsharpened CNT tips (radius greater than 15 nm) were not able to resolve the nanoscale domains in the polymer hybrid films. C1early, the size of the CNT tip contributes significantly to the resolution of phase-contrast imaging. In addition, a study on the nonlinear tapping dynamics of the multi-walled CNT tip indicates that the multi-walled CNT tip is immune to conventional imaging instabilities related to the coexistence of attractive and repulsive tapping regimes. This factor may also contribute to the phase-contrast image quality of multi-walled CNT AFM tips. This presentation will also offer data in support of the stability of the CNT tip for phase shift TMSFM.

Nguyen, Cattien V.↗
NASA NTRS2004

Ka-Band Multibeam Aperture Phased Array Being Developed

Phased-array antenna systems offer many advantages to low-Earth-orbiting satellite systems. Their large scan angles and multibeam capabilities allow for vibration-free, rapid beam scanning and graceful degradation operation for high rate downlink of data to users on the ground. Technology advancements continue to reduce the power, weight, and cost of these systems to make phased arrays a competitive alternative in comparison to the gimbled reflector system commonly used in science missions. One effort to reduce the cost of phased arrays is the development of a Ka-band multibeam aperture (MBA) phased array by Boeing Corporation under a contract jointly by the NASA Glenn Research Center and the Office of Naval Research. The objective is to develop and demonstrate a space-qualifiable dual-beam Ka-band (26.5-GHz) phased-array antenna. The goals are to advance the state of the art in Ka-band active phased-array antennas and to develop and demonstrate multibeam transmission technology compatible with spacecraft in low Earth orbit to reduce the cost of future missions by retiring certain development risks. The frequency chosen is suitable for space-to-space and space-to-ground communication links. The phased-array antenna has a radiation pattern designed by combining a set of individual radiating elements, optimized with the type of radiating elements used, their positions in space, and the amplitude and phase of the currents feeding the elements. This arrangement produces a directional radiation pattern that is proportional to the number of individual radiating elements. The arrays of interest here can scan the main beam electronically with a computerized algorithm. The antenna is constructed using electronic components with no mechanical parts, and the steering is performed electronically, without any resulting vibration. The speed of the scanning is limited primarily by the control electronics. The radiation performance degrades gracefully if a portion of the elements fail. The arrays can be constructed to conform to a mounting surface, and multibeam capability is integral to the design. However, there are challenges for mission designers using monolithic-microwave-integrated-circuit- (MMIC-) based arrays because of reduced power efficiency, higher costs, and certain system effects that result in link degradations. The multibeam aperture phased-array antenna development is attempting to address some of these issues, particularly manufacturing, costs, and system performance.

Reinhart, Richard C.↗
NASA NTRS2007

Advances in Scanning Reflectarray Antennas Based on Ferroelectric Thin Film Phase Shifters for Deep Space Communications

Though there are a few examples of scanning phased array antennas that have flown successfully in space, the quest for low-cost, high-efficiency, large aperture microwave phased arrays continues. Fixed and mobile applications that may be part of a heterogeneous exploration communication architecture will benefit from the agile (rapid) beam steering and graceful degradation afforded by phased array antennas. The reflectarray promises greater efficiency and economy compared to directly-radiating varieties. Implementing a practical scanning version has proven elusive. The ferroelectric reflectarray, under development and described herein, involves phase shifters based on coupled microstrip patterned on Ba(x)Sr(1-x)TiO3 films, that were laser ablated onto LaAlO3 substrates. These devices outperform their semiconductor counterparts from X- through and K-band frequencies. There are special issues associated with the implementation of a scanning reflectarray antenna, especially one realized with thin film ferroelectric phase shifters. This paper will discuss these issues which include: relevance of phase shifter loss; modulo 2(pi) effects and phase shifter transient effects on bit error rate; scattering from the ground plane; presentation of a novel hybrid ferroelectric-semiconductor phase shifter; and the effect of mild radiation exposure on phase shifter performance.

Romanofsky, Robert R.↗
NASA NTRS2004

Improved Phase-Mask Fabrication of Fiber Bragg Gratings

An improved method of fabrication of Bragg gratings in optical fibers combines the best features of two prior methods: one that involves the use of a phase mask and one that involves interference between the two coherent laser beams. The improved method affords flexibility for tailoring Bragg wavelengths and bandwidths over wide ranges. A Bragg grating in an optical fiber is a periodic longitudinal variation in the index of refraction of the fiber core. The spatial period (Bragg wavelength) is chosen to obtain enhanced reflection of light of a given wavelength that would otherwise propagate relatively unimpeded along the core. Optionally, the spatial period of the index modulation can be made to vary gradually along the grating (such a grating is said to be chirped ) in order to obtain enhanced reflection across a wavelength band, the width of which is determined by the difference between the maximum and minimum Bragg wavelengths. In the present method as in both prior methods, a Bragg grating is formed by exposing an optical fiber to an ultraviolet-light interference field. The Bragg grating coincides with the pattern of exposure of the fiber core to ultraviolet light; in other words, the Bragg grating coincides with the interference fringes. Hence, the problem of tailoring the Bragg wavelength and bandwidth is largely one of tailoring the interference pattern and the placement of the fiber in the interference pattern. In the prior two-beam interferometric method, a single laser beam is split into two beams, which are subsequently recombined to produce an interference pattern at the location of an optical fiber. In the prior phase-mask method, a phase mask is used to diffract a laser beam mainly into two first orders, the interference between which creates the pattern to which an optical fiber is exposed. The prior two-beam interferometric method offers the advantage that the period of the interference pattern can be adjusted to produce gratings over a wide range of Bragg wavelengths, but offers the disadvantage that success depends on precise alignment and high mechanical stability. The prior phase-mask method affords the advantages of compactness of equipment and relative insensitivity to both misalignment and vibration, but does not afford adjustability of the Bragg wavelength. The present method affords both the flexibility of the prior two-beam interferometric method and the compactness and stability of the prior phase-mask method. In this method (see figure), a laser beam propagating along the x axis is normally incident on a phase mask that lies in the (y,z) plane. The phase of light propagating through the mask is modulated with a spatial periodicity, p, along the y axis chosen to diffract the laser light primarily to first order at the angle . (The zero-order laser light propagating along the x axis can be used for alignment and thereafter suppressed during exposure of the fiber.) The diffracted light passes through a concave cylindrical lens, which converts the flat diffracted wave fronts to cylindrical ones, as though the light emanated from a line source. Then two parallel flat mirrors recombine the diffracted beams to form an interference field equivalent to that of two coherent line sources at positions A and B (virtual sources). The interference pattern is a known function of the parameters of the apparatus and of position (x,y) in the interference field. Hence, the tilt, wavelength, and chirp of the Bragg grating can be chosen through suitable adjustments of the apparatus and/or of the position and orientation of the optical fiber. In particular, the Bragg wavelength can be adjusted by moving the fiber along the x axis, and the bandwidth can be modified over a wide range by changing the fiber tilt angle or by moving the phase mask and/or the fiber. Alignment is easy because the zero-order beam defines the x axis. The interference is relatively stable and insensitive to the mechanical vibration because of the gh symmetry and compactness of the apparatus, the fixed positions of the mirrors and lens, and the consequent fixed positions of the two virtual line sources, which are independent of the translations of the phase mask and the laser relative to the lens.

Grant, Joseph↗
NASA NTRS2011

Digital Interface Board to Control Phase and Amplitude of Four Channels

An increasing number of parts are designed with digital control interfaces, including phase shifters and variable attenuators. When designing an antenna array in which each antenna has independent amplitude and phase control, the number of digital control lines that must be set simultaneously can grow very large. Use of a parallel interface would require separate line drivers, more parts, and thus additional failure points. A convenient form of control where single-phase shifters or attenuators could be set or the whole set could be programmed with an update rate of 100 Hz is needed to solve this problem. A digital interface board with a field-programmable gate array (FPGA) can simultaneously control an essentially arbitrary number of digital control lines with a serial command interface requiring only three wires. A small set of short, high-level commands provides a simple programming interface for an external controller. Parity bits are used to validate the control commands. Output timing is controlled within the FPGA to allow for rapid update rates of the phase shifters and attenuators. This technology has been used to set and monitor eight 5-bit control signals via a serial UART (universal asynchronous receiver/transmitter) interface. The digital interface board controls the phase and amplitude of the signals for each element in the array. A host computer running Agilent VEE sends commands via serial UART connection to a Xilinx VirtexII FPGA. The commands are decoded, and either outputs are set or telemetry data is sent back to the host computer describing the status and the current phase and amplitude settings. This technology is an integral part of a closed-loop system in which the angle of arrival of an X-band uplink signal is detected and the appropriate phase shifts are applied to the Ka-band downlink signal to electronically steer the array back in the direction of the uplink signal. It will also be used in the non-beam-steering case to compensate for phase shift variations through power amplifiers. The digital interface board can be used to set four 5-bit phase shifters and four 5-bit attenuators and monitor their current settings. Additionally, it is useful outside of the closed-loop system for beamsteering alone. When the VEE program is started, it prompts the user to initialize variables (to zero) or skip initialization. After that, the program enters into a continuous loop waiting for the telemetry period to elapse or a button to be pushed. A telemetry request is sent when the telemetry period is elapsed (every five seconds). Pushing one of the set or reset buttons will send the appropriate command. When a command is sent, the interface status is returned, and the user will be notified by a pop-up window if any error has occurred. The program runs until the End Program button is depressed.

Smith, Amy E.↗
NASA NTRS2012

Optical Phase Recovery and Locking in a PPM Laser Communication Link

Free-space optical communication holds great promise for future space missions requiring high data rates. For data communication in deep space, the current architecture employs pulse position modulation (PPM). In this scheme, the light is transmitted and detected as pulses within an array of time slots. While the PPM method is efficient for data transmission, the phase of the laser light is not utilized. The phase coherence of a PPM optical signal has been investigated with the goal of developing a new laser communication and ranging scheme that utilizes optical coherence within the established PPM architecture and photon-counting detection (PCD). Experimental measurements of a PPM modulated optical signal were conducted, and modeling code was developed to generate random PPM signals and simulate spectra via FFT (Fast Fourier Transform) analysis. The experimental results show very good agreement with the simulations and confirm that coherence is preserved despite modulation with high extinction ratios and very low duty cycles. A real-time technique has been developed to recover the phase information through the mixing of a PPM signal with a frequency-shifted local oscillator (LO). This mixed signal is amplified, filtered, and integrated to generate a voltage proportional to the phase of the modulated signal. By choosing an appropriate time constant for integration, one can maintain a phase lock despite long dark times between consecutive pulses with low duty cycle. A proof-of-principle demonstration was first achieved with an RF-based PPM signal and test setup. With the same principle method, an optical carrier within a PPM modulated laser beam could also be tracked and recovered. A reference laser was phase-locked to an independent pulsed laser signal with low-duty-cycle pseudo-random PPM codes. In this way, the drifting carrier frequency in the primary laser source is tracked via its phase change in the mixed beat note, while the corresponding voltage feedback maintains the phase lock between the two laser sources. The novelty and key significance of this work is that the carrier phase information can be harnessed within an optical communication link based on PPM-PCD architecture. This technology development could lead to quantum-limited efficient performance within the communication link itself, as well as enable high-resolution optical tracking capabilities for planetary science and spacecraft navigation.

Aveline, David C.↗
NASA NTRS2018

Explaining the Asymmetric Line Profile in Cepheus X-4 with Spectral Variation Across Pulse Phase

The high mass X-ray binary Cepheus X-4, during its 2014 outburst, showed evidence for an asymmetric cyclotron line in its hard X-ray spectrum. The 2014 spectrum provides one of the clearest cases of an asymmetric line profile among all studied sources with Cyclotron Resonance Scattering Features (CRSF). We present a phase-resolved analysis of NuSTAR and Suzaku data taken at the peak and during the decline phases of this outburst. We find that the pulse-phased resolved spectra are well-fit by a single, symmetric cyclotron feature. The fit parameters vary strongly with pulse phase: most notably the central energy and depth of the cyclotron feature, the slope of the power-law component, and the absorbing column density. We synthesise a ‘phase averaged’ spectrum using the best-fitting parameters for these individual pulse phases, and find that this combined model spectrum has a similar asymmetry in the cyclotron features as discovered in phase-averaged data. We conclude that the pulse phase resolved analysis with simple symmetric line profiles when combined can explain the asymmetry detected in the phase-averaged data.

Bhargave, Yash↗
NASA NTRSDate not supplied

Deciphering Extreme Mineral Records; Microstructural Phase Heritage of Shocked Materials

High-pressure minerals such as coesite, stishovite, and reidite are often used as indicators of shock metamorphism. However, high-pressure and high-temperature phases are metastable at ambient conditions and, therefore, often revert to a more energetically favorable phase. During solid-state transformations, the crystallographic orientations of the stable polymorph are controlled by the transformation pathway from the parent. Microstructural orientation analysis using electron backscatter diffraction (EBSD) of the stable phase can reveal systematic intercrystalline orientation relationships (OR) diagnostic of solid-state transformations from these high-pressure or high-temperature polymorph phases (Cayron et al., 2006). Knowledge of polymorph stability fields for a given system can thus be used to infer minimum shock P and/or T conditions that rocks have experienced, which are otherwise unavailable using traditional thermobarometers such as element partition coefficients. Using orientation relationships to infer the former presence of mineral phases has been termed microstructural “phase heritage”, and has successfully been used to probe for evidence of extreme pressures and temperatures resulting from hypervelocity impacts. The reconstruction of polymorphs of ZrSiO4 (zircon, reidite) and ZrO2 (baddeleyite) have further elucidated the behavior of these phases under hypervelocity impact conditions (Timms et al., 2017a; White et al., 2018), and OR analysis of shocked monazite has identified a previously unrecognized tetragonal high-P polymorph (Erickson et al., 2019). Zircon will convert to the low tetragonal polymorph reidite at shock stresses above ~21 GPa. However, upon decompression at temperatures above 1200 °C reidite will revert to zircon (Kusaba et al., 1985). Recrystallized zircon neoblasts encased in impact melt often show systematic misorientation relationships of 90° about <110> indicative of reversion from the reidite (Fig. 1), and preserving cryptic evidence of the high-P history that is often erased by the post shock thermal spike (Cavosie et al., 2016). Microstructural OR analysis of a dissociated zircon corona composed of baddeleyite (monoclinic-ZrO2) has identified the former presence of cubic zirconia within impact melt glass from the Mistastin Lake impact structure, Labrador, CA. Based on stability fields in the ZrO2-SiO2 binary phase diagram, cubic zirconia records thermal conditions in excess of 2370 °C at ambient P, indicating that the Mistastin impact melt is the hottest rock identified on Earth’s surface (Timms et al., 2017b). Shock-deformed monazite (monoclinic La,Ce,ThPO4) containing lamellae comprised of interlocking laths has been identified from the Haughton Dome impact structure, Nunavut, Canada and Nördlinger-Ries Crater, southern Germany. The lath-structured lamellae are composed of four systematic orientation variants, which OR analyses indicate originate from a tetragonal parent whereby the [010]monoclinic aligns with either [100] or [010]tetragonal (Erickson et al., 2019). These results highlight utility of microstructural phase heritage analyses for the identification of unstable high-P or high-T polymorphs that uniquely record the extremely transient shock conditions produced by hypervelocity impacts.

Timmons Erickson↗
NASA NTRS2022

Phase II and III Solid Waste Management Unit Assessment and Confirmatory Sampling Report for Per- and Polyfluorinated Alkyl Substances, Potential Release Location 237, Kennedy Space Center, Florida

Per- and polyfluoroalkyl substances (PFAS) Phase II and III Solid Waste Management Unit (SWMU) Assessment (SA) and Confirmatory Sampling (CS) were conducted at the John F. Kennedy Space Center (KSC), Potential Release Location (PRL) 237, located in Merritt Island, Brevard County, Florida for the National Aeronautics and Space Administration (NASA) under Contract 80KSC019D0010/80KSC019F0289. A Phase I SA and CS Report was previously submitted that identified 33 locations of concern (LOCs) at KSC associated with the storage, use, or release of materials containing PFAS. The objectives of the Phase II and III SA and CS were to: - Complete site and source characterization of identified LOCs; - Identify areas of potential concern (AOPCs) where past or present activities may have resulted in a release of PFAS to the environment; - Qualitatively characterize migration potential of released PFAS to environmental media (primarily soil, groundwater, surface water, and sediment); and - Identify potential receptors for exposure to PFAS-impacted environmental media. Surface water samples were collected from LOCs/AOPCs and locations on the KSC periphery during PFAS CS Phases I, II and III. Including duplicate samples, 143 environmental samples were analyzed for 14 PFAS compounds and 104 environmental samples were analyzed for 18 PFAS compounds. Ten of the analytes on the 14 compound list were detected at least once in surface water at KSC, with a wide range in magnitude of detections. The State of Florida has surface water screening levels (SWSLs) for perfluorooctanoic acid (PFOA) and perfluorooctanesulfonic acid (PFOS) in surface water, both for human and ecological receptors. The human health screening levels are lower than the ecological ones and are used in this report. PFOA was not detected in surface water at concentrations exceeding the SWSL at any LOC or Area of Potential Concern (AOPC). PFOS was detected in surface water at concentrations exceeding the SWSL at 28 LOCs/AOPCs, plus 42 locations on the KSC periphery. The data suggest a wide distribution of PFAS, particularly PFOS, in surface water but the sources of surface water contamination are not yet adequately understood. Sediment samples were collected during Phases II and III but not Phase I. Including duplicate samples, 104 environmental samples were analyzed for 14 PFAS compounds and 10 environmental samples were analyzed for 18 PFAS compounds. Twelve compounds were detected in sediment at KSC, with a wide range in magnitude of detections. There are currently no screening levels or cleanup target levels (CTLs) for sediment. The need to delineate and further characterize PFAS in sediment will be evaluated for those sites that move forward into Site Assessment. Groundwater samples were collected via DPT from LOCs/AOPCs and locations on the KSC periphery during PFAS CS Phases I, II and III. Including duplicate samples, 812 environmental DPT groundwater samples were analyzed for 14 PFAS compounds and 247 environmental samples were analyzed for 18 PFAS compounds. Twelve of the 14 compounds were detected in groundwater at KSC, with a wide range in magnitude of detections. The State of Florida has provisional groundwater cleanup target levels (GCTLs) for PFOA, PFOS and the additive concentration of PFOA+PFOS. PFOA was detected in groundwater at concentrations exceeding its provisional GCTL at 16 LOCs/AOPCs, with no exceedances on the KSC periphery. PFOS was detected in groundwater at concentrations exceeding its provisional GCTL at 30 LOCs/AOPCs, plus two locations on the KSC periphery. PFOA+PFOS was detected in groundwater at concentrations exceeding the provisional GCTL at 31 LOCs/AOPCs, plus two locations on the KSC periphery. Soil samples were collected during Phases II and III but not Phase I. Including duplicate samples, 292 environmental samples were analyzed for 14 PFAS compounds and 80 environmental samples were analyzed for 18 PFAS compounds. Fourteen compounds were detected in soil at KSC, with a wide range in magnitude of detections. The State of Florida has provisional soil cleanup target levels (SCTLs) for PFOA and PFOS. There were no PFOA results above its provisional SCTL. There was one LOC with a result above the provisional SCTL for residential settings. Recommendations are presented for each LOC and AOPC.

PFAS↗
NASA NTRSDate not supplied

X-Ray Diffraction Based Phase Identification in NiTiHf Shape Memory Alloys with Variable Hf Content

NiTiHf type shape memory alloys have been studied for use in high temperature actuator applications, the most studied of which is the NiTi-20Hf atomic % composition. In this study, six samples of NiTi-Hf including 20Hf, 30Hf, 35Hf, 40Hf, 45Hf, and 50Hf were evaluated by both 1D and 2D X-ray diffraction (XRD) to elucidate what phases and crystal structures were present at room temperature. Given small sample sizes and relatively large grains, multiple cross-sections were measured to increase the sampling statistics, and 2D XRD frames were collected to corroborate the 1D XRD data. Rietveld and structureless refinements were both performed, allowing for adjustments in orientation lattice constant, and structure factor. At room temperature, the primary martensitic phase in the NiTiHf alloys with 20 at% and lower Hf is a monoclinic B19’ phase (P1121/m space group). This phase was identifiable, even in small amounts, in the higher Hf samples. The primary phase in the 30 -50 at% Hf samples is an orthorhombic B33 (Cmcm space group) phase. This work supported thermal analyses indicating the phase transition paths from the two different room temperature martensitic phases to the B2 austenitic phase.

Laura Wilson↗
DOE OSTI2024

Theory of strain phase equilibria and diagrams

Chemical phase equilibria and phase diagrams are well established and have served as indispensable guides for designing materials through chemical tuning. However, a general thermodynamic theory for strain phase equilibria remains elusive despite extensive studies which have revealed dramatic impacts of mechanical strain on the stability of phases and domain states in solid-state materials. Here, we establish the thermodynamic theory of strain equilibria and a general framework for efficiently constructing multidomain and multiphase diagrams of arbitrarily strained solids under incoherent conditions. As examples, we obtain temperature-strain phase diagrams of ferroelectric PbTiO 3 , strongly correlated VO 2 , and unconventional ferroelectric Hf 0.5 Zr 0.5 O 2 . We reveal the analogs of the Gibbs phase rules, multiple- and multi-critical points, common-tangent construction, and level rule in strain equilibria to those in the familiar chemical phase equilibria. Finally, our strain equilibria theory offers a powerful framework for predicting the thermodynamic stability of structural phases and domains in strained solids and for guiding the strain engineering of their functional properties.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Multi-modal characterization of the B2 phase in the Ta-Re binary system

The energy and transportation industries demand materials that retain their mechanical property at high temperatures. Refractory complex concentrated alloys (RCCAs) with a BCC + B2 microstructure offer a potential solution, where maintaining the high temperature mechanical properties can be achieved by precipitation strengthening. This depends on the B2 phase in RCCAs being thermodynamically stable with a high solvus temperature. Recently, we predicted the high temperature stability of the B2 structure in the Ta-Re binary system, using density functional theory. Here, in this study, we provide experimental evidence for the existence of this phase for the first time, using a Ta 65 Re 35 alloy. Despite Ta-Re binary phase diagrams predicting a single-phase BCC microstructure for Ta 65 Re 35 , we show that a high Z nanoscale secondary phase appears after heat treatment at 1550 °C and 1100 °C. Scanning transmission electron microscopy (STEM) revealed that this phase has a cubic structure and is equiatomic TaRe though B2 superlattice reflections were absent in fast Fourier transforms (FFT) and diffraction patterns (DPs). DP simulations indicate that the B2 TaRe superlattice reflections are up to two orders of magnitude weaker than their fundamental reflections, making their detection challenging via electron microscopy. Neutron diffraction confirmed the second phase had a B2 structure. This study identified a previously unobserved high temperature stable B2 phase in the Ta-Re system, enabling the development of new high temperature BCC + B2 RCCAs.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Specifying angular reference for robust three-phase state estimation

While the phase angle of any of the bus voltages can be chosen as the angular reference in the state estimation formulation of positive sequence networks, the same approach does not readily extend to three-phase network state estimation problem. It is commonly assumed that there is at least one bus where the bus voltages are perfectly balanced with phase angles displaced ±120° and these balanced three phase voltages are used as the three-phase reference in solving the three-phase state estimation problem. This assumption may be quite realistic in transmission networks, and for distribution networks with a strong transmission system connection. However, it might not be realistic to assume existence of a perfectly balanced reference bus in today’s distribution systems with ever increasing penetration of renewable sources or for isolated operation of microgrids. In this paper, a novel state estimation formulation will be presented which facilitates correct solution irrespective of the existence of buses with perfectly balanced voltages. The new formulation is general, and lends itself to bad data processing. It yields accurate results in any three-phase power system irrespective of its operating conditions (balanced or highly unbalanced), configuration (isolated microgrid, connected to transmission system, etc.) and whether or not it contains any synchronous generators. The performance of the method is validated using the IEEE 123 bus three-phase system.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2024

Investigations on the Origin of Topotactic Phase Transition of LaCoO 3 Thin Films with In Situ XRD and Ambient Pressure Hard X-ray Photoelectron Spectroscopy

With the applications of in situ X-ray diffraction (XRD), electrical I–V measurement, and ambient pressure hard X-ray photoelectron spectroscopy (AP-HAXPES), the characteristics of the topotactic phase transition of LaCoO 3 (LCO) thin films are examined. XRD measurements show clear evidence of structural phase transition (SPT) of the LCO thin films from the perovskite (PV) LaCoO 3 to the brownmillerite (BM) La 2 Co 2 O 5 phases through the intermediate La 3 Co 3 O 8 phase at a temperature of 350 °C under high-vacuum conditions, ~10 –5 mbar. The reverse SPT from BM to PV phases is also found under ambient pressure (>100 mbar) of air near 100 °C. Both observed SPTs in XRD are also identified in the electrical I–V measurements, i.e., the metallic PV phase to the insulating BM phase and vice versa. During the onset of SPTs, the bulk chemical and electronic states of LCO thin films are monitored with AP-HAXPES. The oxidation states in Co 2p spectra indicate that the oxygen vacancies are closely related to the SPT of LCO thin films. Also, the presence of enlarged band gap is observed as the SPT from PV to BM phases takes place, revealing the modified electronic properties of LCO due to the creation of oxygen vacancies. In conclusion, the analysis of valence band structures is further compared to the I–V measurements.

36 MATERIALS SCIENCE↗