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At least 343 records · Page 19

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.↗

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↗

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.↗

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.↗

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↗

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↗

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↗

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↗

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↗

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↗

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↗

What Is the Limit of Quantification for the Minor Phase in Time-of-Flight Neutron Diffraction? A Case Study on Fe and Ni Powder Mixtures at VULCAN

A phase present in small quantities within materials may not simply serve as a secondary component; it can play a crucial role in determining the integrity, properties, and performance of the material. These minor but important phases usually draw attention in material design and processing for fundamental understanding as well as material quality control. Accurately quantifying a minor phase amid a majority phase, especially at extremely low fractions, remains a challenging task. Time-of-flight neutron diffraction, coupled with advanced pattern analysis techniques like Rietveld refinement, is a powerful tool for crystal structure identification and phase quantification. The deep penetrating capability of neutrons enables the detection and quantification of trace phases within materials. In this study, the quantification limits of time-of-flight neutron diffraction were explored using the VULCAN diffractometer at the Spallation Neutron Source, using Fe–Ni powder mixtures as a sample system. By comparing the refinement results to the known weighed values, it was determined that the reliable quantification of a minor Ni phase is achievable down to about 0.1 wt% while a Ni fraction as low as 0.02 wt% is difficult to trace. Effective control of the refinement parameters, especially the profile function parameters, are found to significantly influence the convergence of fittings and the accuracy of phase quantification.

Rietveld refinement↗

Self‐Strain Suppression of the Metal‐to‐Insulator Transition in Phase‐Change Oxide Devices

Strongly correlated materials exhibiting phase transitions which can be controlled through external stimuli, such as electric fields, are promising for future computing technologies beyond conventional semiconductor transistors. Devices that take advantage of structural phase transitions have inherent built‐in memory, reminiscent of synapses and neurons, and are thus natural candidates for neuromorphic computing. Of particular interest are phase‐change oxides, which allow for control over the metal‐to‐insulator transition. Here, X‐ray nano‐diffraction structural imaging of micro‐devices fabricated with the archetypal phase‐change material vanadium sesquioxide (V 2 O 3 ) is reported. The devices contain a Ga ion‐irradiated region where the metal‐to‐insulator transition critical temperature is lowered, a useful feature for controlling neuron‐like spiking behavior. Results show that strain, induced by crystal lattice mismatch between the pristine and irradiated material, leads to a suppression of the metal‐to‐insulator‐transition. Suppression occurs within the irradiated region or along its edges, depending on the defect‐distribution and the size of the region. The observed self‐straining effect can extend to other phase‐change oxides and dominate as device dimensions are reduced and become too small to dissipate strain within the irradiated region. The findings are important for phase engineering in phase‐change devices and highlight the necessity to study phase transitions at the nanoscale.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Understanding the Phase of Responsivity and Noise Sources in Frequency-Domain Multiplexed Readout of Transition Edge Sensor Bolometers

Abstract Cosmic microwave background (CMB) experiments have deployed focal planes with $$\mathcal {O}(10^{4})$$ O ( 10 4 ) transition edge sensor (TES) bolometers cooled to sub-Kelvin temperatures by multiplexing the readout of many TES channels onto a single pair of wires. Digital Frequency-domain Multiplexing (DfMux) is a multiplexing technique used in many CMB polarization experiments, such as the Simons Array, SPT-3 G, and EBEX. The DfMux system studied here uses LC filters with resonant frequencies ranging from 1.5 to 4.5 MHz connected to an array of TESs. Each detector has an amplitude-modulated carrier tone at the resonant frequency of its accompanying LC resonator. The signal is recovered via quadrature demodulation where the in-phase (I) component of the demodulated current is in phase with the complex admittance of the circuit and the quadrature (Q) component is orthogonal to I. Observed excess current noise in the Q component is consistent with fluctuations in the resonant frequency. This noise has been shown to be non-orthogonal to the phase of the detector’s responsivity. We present a detailed analysis of the phase of responsivity of the TES and noise sources in our DfMux readout system. Further, we investigate how modifications to the TES operating resistance and bias frequency can affect the phase of noise relative to the phase of the detector responsivity, using data from Simons Array to evaluate our predictions. We find that both the phase of responsivity and phase of noise are functions of the two tuning parameters, which can be purposefully selected to maximize signal-to-noise (SNR) ratio.

47 OTHER INSTRUMENTATION↗

Effect of stress on Laves phase precipitation in creep ruptured Grade 92 ferritic martensitic steel characterized by a novel accessible method

At high temperature conditions relevant to fossil and nuclear energy plants, Laves phase (Fe 2 X, X=Mo, W) precipitation is observed in common ferritic martensitic (FM) structural steels, with various reported effects on creep behavior. Despite being valuable metrics to correlate with mechanical properties and other precipitate phases, the volume fraction and number density of Laves phase precipitates has been difficult to quantify accurately using common techniques such as transmission electron microscopy (TEM) due to the relatively large size (∼0.25 μm) and low number density (∼10 11 cm −3 ) of Laves precipitates. Here, to address this characterization challenge, we developed and demonstrated a high-throughput and widely accessible method to quantify the volume fraction and number density of the Laves phase based on scanning electron microscope (SEM) images with a backscattered electron signal and the information depth (ID) of backscattered electrons. We applied this new technique in creep ruptured Grade 92 FM steel to study the effect of Laves phase on creep properties and determine the influence of stress on Laves phase precipitation. The quantitative accuracy of the SEM-based volume fraction and number density values was verified using synchrotron high energy X-ray diffraction and serial sectioning tomography. Stress did not significantly affect the Laves phase size or volume fraction during creep testing at 550 – 650°C and stress levels of 90 – 260 MPa (vs. unstressed conditions). Conversely, a moderate but statistically significant stress-enhanced increase in Laves phase number density, corresponding to an increase in nucleation rate, occurred during creep exposure above 110 MPa.

Creep↗

Formation mechanisms of Sn-rich δ phase and its role in strengthening Cu-10Sn manufactured by laser powder bed fusion

Cu-Sn alloys produced via laser powder bed fusion (L-PBF) additive manufacturing (AM) have gained significant attention because they combine the advantages of AM relevant to intricate component design with outstanding combinations of strength, ductility, and resistance to wear and corrosion. However, a detailed understanding of the microstructure that contributes to the enhancement of the mechanical properties of L-PBF Cu-10Sn alloys remains unclear. In particular, there is a lack of understanding of the formation mechanisms of the Sn-rich δ phase commonly observed in Cu-10Sn. This study reveals two distinct variants of the δ phase possessing unique morphological characteristics. These characteristics are attributed to the local solidification conditions inherent to the melt pool boundaries versus those at the interiors of melt pools. A phase transformation pathway that elucidates the origin of the morphological variants of the δ phase from the Sn-rich metastable phases during the cyclic heating of the AM process is proposed. We report superior mechanical properties in L-PBF Cu-10Sn compared to those of conventionally manufactured counterparts due to the synergistic contributions from grain boundaries, dislocations, and the δ phase. Notably, the δ phase alone contributes approximately 22 % to the overall strength observed in the L-PBF Cu-10Sn alloy. The discovery of two types of distinct Sn-rich δ phase offers key insights into precise microstructural control in AM Cu-Sn alloys to enhance mechanical properties, providing practical strategies for improving material performance for diverse applications in automotive, aerospace, and machinery industries.

36 MATERIALS SCIENCE↗

Effect of vanadium on phase composition and hard magnetic properties of as-solidified and heat-treated Sm–Fe–(Ti,V) alloys

Although the intrinsic magnetic properties of Ti-stabilized Sm(Fe,Co,Ti) 12 compounds exhibit potential of excellent rare-earth-lean permanent magnets, it has been much easier to realize large coercivities with the isostructural compounds stabilized by either V or by certain combinations of Ti and V. To elucidate the influence of V on the microstructure and magnetic properties, a series of Sm 8.1 Fe 78.4 (Ti 1-x V x ) 13.5 alloys was studied after arc-melting and annealing at 850–1000 °C. The alloys were found to fall into three groups. For x ≤ 0.2, solidification generates mostly the Sm(Fe,Ti,V) 12 phase, but annealing converts at least part of it into the non-magnetic Sm(Fe,Ti,V) 11 and the magnetically soft Sm 2 (Fe,Ti,V) 17 phases. For 0.2 < x < 0.6, the alloys solidify into a near-equilibrium mixture of the Sm(Fe,Ti,V) 12 , TiFe 2 and Sm-rich phases. For x ≥ 0.6, solidification generates large fractions of α-Fe solid solution and Sm-rich phases; an annealing step is necessary to complete the formation of Sm(Fe,Ti,V) 12 phase. Also, for x ≥ 0.6 the temperature below which the Sm(Fe,Ti,V) 12 phase is stable decreases with x, as does the fraction of this phase formed during solidification. Here, the differences between these three groups of alloys suggest different strategies for developing hard magnetic properties, with the likelihood of a success increasing with increasing x. For x ≥ 0.6, heat treatment alone is demonstrated to generate a microstructure of micron and submicron Sm(Fe,Ti 1-x V x ) 12 crystallites separated by a Sm-rich phase and exhibiting a coercivity with values up to 3.5 and 5.7 kOe for x = 0.8 and 1.0, respectively.

36 MATERIALS SCIENCE↗

Dynamic Bubbling Balanced Proactive CO 2 Capture and Reduction on a Triple-Phase Interface Nanoporous Electrocatalyst

The formation and preservation of the active phase of the catalysts at the triple-phase interface during CO 2 capture and reduction is essential for improving the conversion efficiency of CO 2 electroreduction toward value-added chemicals and fuels under operational conditions. Designing such ideal catalysts that can mitigate parasitic hydrogen generation and prevent active phase degradation during the CO 2 reduction reaction (CO 2 RR), however, remains a significant challenge. Herein, we developed an interfacial engineering strategy to build a new SnO x catalyst by invoking multiscale approaches. This catalyst features a hierarchically nanoporous structure coated with an organic F-monolayer that modifies the triple-phase interface in aqueous electrolytes, substantially reducing competing hydrogen generation (less than 5%) and enhancing CO 2 RR selectivity (~90%). This rationally designed triple-phase interface overcomes the issue of limited CO 2 solubility in aqueous electrolytes via proactive CO 2 capture and reduction. Concurrently, we utilized pulsed square-wave potentials to dynamically recover the active phase for the CO 2 RR to regulate the production of C1 products such as formate and carbon monoxide (CO). This protocol ensures profoundly enhanced CO 2 RR selectivity (~90%) compared with constant potential (~70%) applied at -0.8 V (V vs RHE). We further achieved a mechanistic understanding of the CO 2 capture and reduction processes under pulsed square-wave potentials via in situ Raman spectroscopy, thereby observing the potential-dependent intensity of Raman vibrational modes of the active phase and CO 2 RR intermediates. Finally, this work will inspire material design strategies by leveraging triple-phase interface engineering for emerging electrochemical processes, as technology moves toward electrification and decarbonization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗