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Embedding Sensors in 3D Printed Metal Structures

The Transformational Challenge Reactor (TCR) program is leveraging recent advances in modeling and simulation, materials, and additive manufacturing (AM) technologies to design a modern nuclear reactor. Some of the main TCR technologies include in situ monitoring and the integration of sensors during the manufacturing of quality-significant nuclear reactor components. This report describes the general procedure and process optimization for embedding sensors within generic stainless steel 316 (SS316) components using laser powder bed fusion (LPBF). A more detailed, quality-significant test plan and supporting procedures are available upon request (ORNL/TM-2021/2127). LPBF involves the use of a scanning laser to selectively melt regions of a powder bed, additively building a part layer by layer. This report describes the LPBF processing technique and discusses the effects of LPBF processing parameters on the success of the sensor embedding process. Experiments used machined cavities in the form of channels in an SS316 base for the sensors to lay in while material is additively built over the top, thereby embedding them in an SS316 matrix. A preliminary investigation involved using empty SS316 sheaths as surrogates to explore the effects of various LPBF processing parameters and the dimensional requirements of the machined channels. Microstructural investigations showed that a smaller channel width/depth combination closer to the sensor’s diameter was best for the embedding process. After the desired parameters were selected, Type-K thermocouples were embedded and evaluated post-embedding using nondestructive thermal testing, as well as destructive sectioning and microscopy. Post-build characterization showed that the thermocouples were well-bonded to the SS316 matrix and were fully functional after embedding. During thermal testing to temperatures up to 500 °C, the embedded thermocouples read consistently with one another and deviated only slightly from the readings of a nonembedded thermocouple located within the furnace. This slight discrepancy was most likely due to differences in the thermal time constants for a nonembedded thermocouple vs. a thermocouple embedded in a solid SS316 block. The results presented in this report will serve as the foundation for future work that will focus on embedding sensors in relevant TCR reactor components and eventually testing those components under neutron irradiation.

36 MATERIALS SCIENCE↗

Highlights of NASA’s Orbital Debris Program Office In Situ and Laboratory Measurements

NASA’s Orbital Debris Program Office (ODPO) maintains various returned spacecraft materials, capabilities, and facilities used for in situ and laboratory measurements that directly support orbital debris environmental models. In situ measurements include the analysis of exposed and returned hardware surfaces. These surfaces serve as passive sensors for the small-sized micrometeoroid and orbital debris (MMOD) flux below the sensitivity of ground-based radar and optical sensors. Various instruments and techniques are used to determine the size and depth of selected impact features, and – if feasible – the composition of the projectile material. Analysis of the impactor residues enables the differentiation of MM and OD for debris below 1 mm to support modeling the OD environment. In addition, projectiles identified as OD can be further differentiated in low-, medium-, and high- density impactors based on chemical analyses. In addition to in situ measurements, the ODPO has also worked in collaboration with the U.S. Space Force Space Systems Command (formerly the U.S. Air Force Space and Missile Systems Center), the Aerospace Corporation, and the University of Florida on a laboratory-based hypervelocity impact test, DebriSat, conducted at the Air Force Arnold Engineering Development Complex in 2014. The resulting data from this impact test series are being analyzed to assess the fragments’ sizes/masses, materials/densities, shapes, and other parameters of interest. The DebriSat project provides the data needed to update NASA’s breakup models and size estimation models using the simulated orbital breakup of a modern, low Earth orbit spacecraft. Ultimately, over 200,000 fragments from this impact test will be stored at NASA Johnson Space Center (JSC) and further analyzed by the ODPO. This project will also use machine learning techniques to infer physical parameters of fragments embedded in the soft-catch foam used in the impact experiment. Applied to X-ray imagery of the foam panels, these techniques promise to minimize human-in-the-loop processes for fragment extraction and physical characterization. A brief overview of this project and data collected will be presented. Lastly, the ODPO provides various capabilities hosted at NASA JSC for optical inspections and measurements using a variety of techniques and scientific instrumentation to support both in situ and laboratory measurements. The ODPO’s Optical Measurement Center (OMC) is an advanced facility for photometric and spectroscopic laboratory measurements of targets, including fragments from the DebriSat project. The OMC simulates telescopic observations by using space-like illumination conditions and source-target-sensor orientation techniques. Additionally, the OMC is uniquely equipped to acquire pseudo-bidirectional reflectance distribution data for broadband photometric measurements, thus removing aspect angle dependencies that can affect target size estimates using the optical size estimation model. Narrow-band surface material characterization using spectroscopic instrumentation gives insight into how the albedo parameter – also important in the optical size estimation model – may vary depending on the state of the material. The OMC also performs simulations of photometric measurements using optical ray-tracing software to model the OMC optical throughput. In addition to the OMC, the ODPO houses a start-of-the-art Fragment Analysis Facility that uses multiple microscopic inspection instruments to support in situ measurements and material characterization. An overview of both facilities will be highlighted in this paper.

Orbital Debris↗

Highlights of NASA’s Orbital Debris Program Office In Situ and Laboratory Measurements

NASA’s Orbital Debris Program Office (ODPO) maintains various returned spacecraft materials, capabilities, and facilities used for in situ and laboratory measurements that directly support orbital debris environmental models. In situ measurements include the analysis of exposed and returned hardware surfaces. These surfaces serve as passive sensors for the small-sized micrometeoroid and orbital debris (MMOD) flux below the sensitivity of ground-based radar and optical sensors. Various instruments and techniques are used to determine the size and depth of selected impact features, and – if feasible – the composition of the projectile material. Analysis of the impactor residues enables the differentiation of MM and OD for debris below 1 mm to support modeling the OD environment. In addition, projectiles identified as OD can be further differentiated in low-, medium-, and high- density impactors based on chemical analyses. In addition to in situ measurements, the ODPO has also worked in collaboration with the U.S. Space Force Space Systems Command (formerly the U.S. Air Force Space and Missile Systems Center), the Aerospace Corporation, and the University of Florida on a laboratory-based hypervelocity impact test, DebriSat, conducted at the Air Force Arnold Engineering Development Complex in 2014. The resulting data from this impact test series are being analyzed to assess the fragments’ sizes/masses, materials/densities, shapes, and other parameters of interest. The DebriSat project provides the data needed to update NASA’s breakup models and size estimation models using the simulated orbital breakup of a modern, low Earth orbit spacecraft. Ultimately, over 200,000 fragments from this impact test will be stored at NASA Johnson Space Center (JSC) and further analyzed by the ODPO. This project will also use machine learning techniques to infer physical parameters of fragments embedded in the soft-catch foam used in the impact experiment. Applied to X-ray imagery of the foam panels, these techniques promise to minimize human-in-the-loop processes for fragment extraction and physical characterization. A brief overview of this project and data collected will be presented. Lastly, the ODPO provides various capabilities hosted at NASA JSC for optical inspections and measurements using a variety of techniques and scientific instrumentation to support both in situ and laboratory measurements. The ODPO’s Optical Measurement Center (OMC) is an advanced facility for photometric and spectroscopic laboratory measurements of targets, including fragments from the DebriSat project. The OMC simulates telescopic observations by using space-like illumination conditions and source-target-sensor orientation techniques. Additionally, the OMC is uniquely equipped to acquire pseudo-bidirectional reflectance distribution data for broadband photometric measurements, thus removing aspect angle dependencies that can affect target size estimates using the optical size estimation model. Narrow-band surface material characterization using spectroscopic instrumentation gives insight into how the albedo parameter – also important in the optical size estimation model – may vary depending on the state of the material. The OMC also performs simulations of photometric measurements using optical ray-tracing software to model the OMC optical throughput. In addition to the OMC, the ODPO houses a start-of-the-art Fragment Analysis Facility that uses multiple microscopic inspection instruments to support in situ measurements and material characterization. An overview of both facilities will be highlighted in this paper.

Orbital Debris↗

Collaborative Research On Ecophysiological Controls on Amazonian Precipitation Seasonality And Variability

We developed and deployed a robust and accurate instrumentation package for measurement of solar induced chlorophyll fluorescence (SIF) from above a plant canopy. The sensor collects light from identical up and down facing hemispheric collectors. A fiber optic transmits the collected light (selected by a rotatable prism) to spectrometers located at the base of the tower. Spectra of the down welling and upwelling light were collected alternatively and stored for later analysis. SIF was retrieved by a spectral unmixing approach using high resolution spectra in the 730-760 nm band. Most other ground-based sensors base their analysis on O 2 -alpha band (760-780 nm) for SIF retrieval. We found that the former gave identical results when the atmosphere was clear, but the former was more stable in the cloudy conditions that often prevailed in the Amazon. The mechanical design and software developed for the system are available on request. The sensor was mounted near the top of an 80 m tower at K34 near Manaus in the Brazilian Amazon Forest. The sensor system proved weather-tight and functioned flawlessly over the time of deployment. Our experiment was cut short at 6 months by failure of air conditioning infrastructure at the tower. We found that SIF emitted by canopy was remarkably stable when scaled by the downwelling photosynthetically active radiation or the upwelling near infrared light. We detected a 3.4% increase in SIF over the course of the dry season. This finding is consistent with the observation that several trees in the field of view flushed new leaves in the dry season. We saw no evidence of drought stress or photo damage of the forest canopy during our study.

54 ENVIRONMENTAL SCIENCES↗

High Speed PC Based Data Acquisition and Instrumentation for Measurement of Simulated Low Earth Orbit Thermally Induced Disturbances

The Hubble Space Telescope (HST) Disturbance Verification Test (DVT) was conducted to characterize responses of the Observatory's new set of rigid solar array's (SA3) to thermally induced 'creak' or stiction releases. The data acquired in the DVT were used in verification of the HST Pointing Control System on-orbit performance, post-Servicing Mission 3B (SM3B). The test simulated the on-orbit environment on a deployed SA3 flight wing. Instrumentation for this test required pretest simulations in order to select the correct sensitivities. Vacuum compatible, highly accurate accelerometers and force gages were used for this test. The complexity of the test, as well as a short planning schedule, required a data acquisition system that was easy to configure, highly flexible, and extremely robust. A PC Windows oriented data acquisition system meets these requirements, allowing the test engineers to minimize the time required to plan and perform complex environmental test. The SA3 DVT provided a direct practical and complex demonstration of the versatility that PC based data acquisition systems provide. Two PC based data acquisition systems were assembled to acquire, process, distribute, and provide real time processing for several types of transducers used in the SA3 DVT. A high sample rate digital tape recorder was used to archive the sensor signals. The two systems provided multi-channel hardware and software architecture and were selected based on the test requirements. How these systems acquire and processes multiple data rates from different transducer types is discussed, along with the system hardware and software architecture.

Sills, Joel W., Jr.↗

Enzymatic Laser-Induced Graphene Biosensor for Electrochemical Sensing of the Herbicide Glyphosate

Glyphosate is a globally applied herbicide yet it has been relatively undetectable in-field samples outside of gold-standard techniques. Its presumed nontoxicity toward humans has been contested by the International Agency for Research on Cancer, while it has been detected in farmers’ urine, surface waters and crop residues. Rapid, on-site detection of glyphosate is hindered by lack of field-deployable and easy-to-use sensors that circumvent sample transportation to limited laboratories that possess the equipment needed for detection. Herein, the flavoenzyme, glycine oxidase, immobilized on platinum-decorated laser-induced graphene (LIG) is used for selective detection of glyphosate as it is a substrate for GlyOx. The LIG platform provides a scaffold for enzyme attachment while maintaining the electronic and surface properties of graphene. The sensor exhibits a linear range of 10–260 µm, detection limit of 3.03 µm, and sensitivity of 0.991 nA µm -1 . The sensor shows minimal interference from the commonly used herbicides and insecticides: atrazine, 2,4-dichlorophenoxyacetic acid, dicamba, parathion-methyl, paraoxon-methyl, malathion, chlorpyrifos, thiamethoxam, clothianidin, and imidacloprid. Sensor function is further tested in complex river water and crop residue fluids, which validate this platform as a scalable, direct-write, and selective method of glyphosate detection for herbicide mapping and food analysis.

47 OTHER INSTRUMENTATION↗

Active vibration damping using smart material

We consider the modeling and active damping of an elastic beam using distributed actuators and sensors. The piezoelectric ceramic material (PZT) is used to build the actuator. The sensor is made of the piezoelectric polymer polyvinylidene fluoride (PVDF). These materials are glued on both sides of the beam. For the simple clamped beam, the closed loop controller has been shown to be able to extract energy from the beam. The shape of the actuator and its influence on the closed loop system performance are discussed. It is shown that it is possible to suppress the selected mode by choosing the appropriate actuator layout. It is also shown that by properly installing the sensor and determining the sensor shape we can further extract and manipulate the sensor signal for our control need.

Baras, John S.↗

The Impact of Crosstalk in the X-IFU Instrument on Athena Science Cases

In this paper we present a first assessment of the impact of various forms of instrumental crosstalk on the science performance of the X-ray Integral Field Unit (X-IFU) on the Athena X-ray mission. This assessment is made using the SIXTE end-to-end simulator in the context of one of the more technically challenging science cases for the XIFU instrument. Crosstalk considerations may influence or drive various aspects of the design of the array of high-count-rate Transition Edge Sensor (TES) detectors and its Frequency Domain Multiplexed (FDM) readout architecture. The Athena X-ray mission was selected as the second L-class mission in ESA's Cosmic Vision 2015–25 plan, with alaunch foreseen in 2028, to address the theme ''Hot and Energetic Universe"1. One of the two instruments on boardAthena is the X-ray Integral Field Unit2 (X-IFU) which is based on an array of ~3800 Transition Edge Sensors (TES's)operated at a temperature of ~90 mK. The science cases pose an interesting challenge for this instrument, as they requirea combination of high energy resolution (2.5 eV FWHM or better), high spatial resolution (5 arcsec or better) and highcount rate capability (several tens of counts per second per detector for point sources as bright as 10 mCrab).The performance at the single sensor level has been demonstrated3, but the operation of such detectors in an array, usingmultiplexed readout, brings additional challenges, both for the design of the array in which the sensors are placed and forthe readout of the sensors. The readout of the detector array will be based on Frequency Domain Multiplexing (FDM)4.In this system of detectors and readout, crosstalk can arise through various mechanisms: on the TES array, neighboringsensors can couple through thermal crosstalk. Detectors adjacent in carrier frequency may suffer from electrical crosstalkdue to the finite width of the bandpass filters, and shared sources of impedance in their signal lines. The signals from theindividual detectors are summed and then amplified by a pair of SQUID amplifiers before being sent to warm front-endelectronics. The transfer function of the SQUID amplifiers is non-linear, which will give rise to higher harmonics ofcarriers and intermodulation products when multiple signal pulses are simultaneously present in the SQUID. Under highcount rate conditions this is another source of crosstalk. The effect of all these crosstalk sources is that parasitic pulseswill appear in the record of a signal pulse which will create a stochastic offset of the measured energy and thus adegradation of the energy resolution.

SIXTE↗

Extraction of Qualitative Features from Sensor Data Using Windowed Fourier Transform

In this paper, we use Matlab to model the health monitoring of a system through the information gathered from sensors. This implies assessment of the condition of the system components. Once a normal mode of operation is established any deviation from the normal behavior indicates a change. This change may be due to a malfunction of an element, a qualitative change, or a change due to a problem with another element in the network. For example, if one sensor indicates that the temperature in the tank has experienced a step change then a pressure sensor associated with the process in the tank should also experience a step change. The step up and step down as well as sensor disturbances are assumed to be exponential. An RC network is used to model the main process, which is step-up (charging), drift, and step-down (discharging). The sensor disturbances and spike are added while the system is in drift. The system is allowed to run for a period equal to three time constant of the main process before changes occur. Then each point of the signal is selected with a trailing data collected previously. Two trailing lengths of data are selected, one equal to two time constants of the main process and the other equal to two time constants of the sensor disturbance. Next, the DC is removed from each set of data and then the data are passed through a window followed by calculation of spectra for each set. In order to extract features the signal power, peak, and spectrum are plotted vs time. The results indicate distinct shapes corresponding to each process. The study is also carried out for a number of Gaussian distributed noisy cases.

Amini, Abolfazl M.↗

Tunable Fiber Bragg Grating Ring Lasers using Macro Fiber Composite Actuators

The research reported herein includes the fabrication of a tunable optical fiber Bragg grating (FBG) fiber ring laser (FRL)1 from commercially available components as a high-speed alternative tunable laser source for NASA Langley s optical frequency domain reflectometer (OFDR) interrogator, which reads low reflectivity FBG sensors. A Macro-Fiber Composite (MFC) actuator invented at NASA Langley Research Center (LaRC) was selected to tune the laser. MFC actuators use a piezoelectric sheet cut into uniaxially aligned rectangular piezo-fibers surrounded by a polymer matrix and incorporate interdigitated electrodes to deliver electric fields along the length of the piezo-fibers. This configuration enables MFC actuators to produce displacements larger than the original uncut piezoelectric sheet. The FBG filter was sandwiched between two MFC actuators, and when strained, produced approximately 3.62 nm of wavelength shift in the FRL when biasing the MFC actuators from 500 V to 2000 V. This tunability range is comparable to that of other tunable lasers and is adequate for interrogating FBG sensors using OFDR technology. Three different FRL configurations were studied. Configuration A examined the importance of erbium-doped fiber length and output coupling. Configuration B demonstrated the importance of the FBG filter. Configuration C added an output coupler to increase the output power and to isolate the filter. Only configuration C was tuned because it offered the best optical power output of the three configurations. Use of Plastic Optical Fiber (POF) FBG s holds promise for enhanced tunability in future research.

Geddis, Demetris L.↗

Synthesis and gas sensing properties of NiO/SnO2 hierarchical structures toward ppb-level acetone detection

Highlights: • The NiO/SnO{sub 2} hierarchical structures with different Ni contents have been prepared by facile hydrothermal method. • The NiO/SnO{sub 2} sensors exhibit the enhanced gas sensing performances comparing with pure SnO{sub 2}. • The Ni{sub 1}Sn{sub 3} sensor exhibits higher response, fast response/recovery time for acetone detection. - Abstract: We have synthesized pristine SnO{sub 2} and NiO/SnO{sub 2} hierarchical structures by a facile hydrothermal method. Structural and morphological characterizations of the obtained NiO/SnO{sub 2} samples were systematically studied using XRD, SEM, TEM and XPS. Meanwhile, gas-sensing properties of the as-fabricated pristine SnO{sub 2} and NiO/SnO{sub 2} sensor devices were investigated toward ppb-level acetone detection. The measured results show that the Ni{sub 1}Sn{sub 3} gas sensor can reach a response of 20.18 toward 50 ppm acetone under optimum operating temperature (300 °C), which is about 3.3 times higher than that of pristine sensor. Moreover, the Ni{sub 1}Sn{sub 3} gas sensor also exhibits fast response/recovery time (2 s/9 s), low detection limit (10 ppb) and good selectivity. We attribute the enhanced gas-sensing properties of NiO/SnO{sub 2} hierarchical structures to the synergetic effect as well as p-n heterojunction between the NiO and SnO{sub 2} structures.

36 MATERIALS SCIENCE↗

Atmospheric Boundary Layer Sensors for Application in a Wake Vortex Advisory System

Remote sensing of the atmospheric boundary layer has advanced in recent years with the development of commercial off-the-shelf (COTS) radar, sodar, and lidar wind profiling technology. Radio acoustic sounding systems for vertical temperature profiles of high temporal scales (when compared to routine balloon soundings- (radiosondes) have also become increasingly available as COTS capabilities. Aircraft observations during landing and departures are another source of available boundary layer data. This report provides an updated assessment of available sensors, their performance specifications and rough order of magnitude costs for a potential future aircraft Wake Vortex Avoidance System (WakeVAS). Future capabilities are also discussed. Vertical profiles of wind, temperature, and turbulence are anticipated to be needed at airports in any dynamic wake avoidance system. Temporal and spatial resolution are dependent on the selection of approach and departure corridors to be protected. Recommendations are made for potential configurations of near-term sensor technologies and for testing some of the sensor systems in order to validate performance in field environments with adequate groundtruth.

Zak, J. Allen↗

Software Testbed for Developing and Evaluating Integrated Autonomous Subsystems

To implement fault tolerant autonomy in future space systems, it will be necessary to integrate planning, adaptive control, and state estimation subsystems. However, integrating these subsystems is difficult, time-consuming, and error-prone. This paper describes Intelliface/ADAPT, a software testbed that helps researchers develop and test alternative strategies for integrating planning, execution, and diagnosis subsystems more quickly and easily. The testbed's architecture, graphical data displays, and implementations of the integrated subsystems support easy plug and play of alternate components to support research and development in fault-tolerant control of autonomous vehicles and operations support systems. Intelliface/ADAPT controls NASA's Advanced Diagnostics and Prognostics Testbed (ADAPT), which comprises batteries, electrical loads (fans, pumps, and lights), relays, circuit breakers, invertors, and sensors. During plan execution, an experimentor can inject faults into the ADAPT testbed by tripping circuit breakers, changing fan speed settings, and closing valves to restrict fluid flow. The diagnostic subsystem, based on NASA's Hybrid Diagnosis Engine (HyDE), detects and isolates these faults to determine the new state of the plant, ADAPT. Intelliface/ADAPT then updates its model of the ADAPT system's resources and determines whether the current plan can be executed using the reduced resources. If not, the planning subsystem generates a new plan that reschedules tasks, reconfigures ADAPT, and reassigns the use of ADAPT resources as needed to work around the fault. The resource model, planning domain model, and planning goals are expressed using NASA's Action Notation Modeling Language (ANML). Parts of the ANML model are generated automatically, and other parts are constructed by hand using the Planning Model Integrated Development Environment, a visual Eclipse-based IDE that accelerates ANML model development. Because native ANML planners are currently under development and not yet sufficiently capable, the ANML model is translated into the New Domain Definition Language (NDDL) and sent to NASA's EUROPA planning system for plan generation. The adaptive controller executes the new plan, using augmented, hierarchical finite state machines to select and sequence actions based on the state of the ADAPT system. Real-time sensor data, commands, and plans are displayed in information-dense arrays of timelines and graphs that zoom and scroll in unison. A dynamic schematic display uses color to show the real-time fault state and utilization of the system components and resources. An execution manager coordinates the activities of the other subsystems. The subsystems are integrated using the Internet Communications Engine (ICE). an object-oriented toolkit for building distributed applications.

Testbed↗

Improved Bayesian regularization of inverse problems in vibrations and acoustics using noise-only measurements

Here, this paper studies Tikhonov regularization (ridge regression) parameter selection for problems in vibrations and acoustics. The selection method is based on a popular Bayesian method, but it incorporates measurements of sensor noise. The regularization parameter is closely related to the ratio of system input energy to noise energy, so noise measurements inform the inference procedure and improve parameter identification. In cases where standard Bayesian regularization identifies zero as the optimal regularization parameter, noise measurements guarantee a unique nonzero optimum. Sufficient theoretical criteria are developed for this guarantee. The method is verified in even-determined and under-determined configurations in an acoustic source localization simulation and a vibration load identification experiment. It is shown to yield significant improvements over existing empirical Bayesian regularization. Improvements are larger in the even-determined case and smaller in the under-determined case, wherein the inverse solution is less sensitive to the regularization parameter.

42 ENGINEERING↗

Understanding the Influence of Urban Form on the Spatial Pattern of Precipitation

Urban areas are known to modify the spatial pattern of precipitation climatology. Existing observational evidence suggests that precipitation can be enhanced downwind of a city. Among the proposed mechanisms, the thermodynamic and aerodynamic processes in the urban lower atmosphere interact with the meteorological conditions and can play a key role in determining the resulting precipitation patterns. In addition, these processes are influenced by urban form, such as the impervious surface extent. This study aims to unravel how different urban forms impact the spatial patterns of precipitation climatology under different meteorological conditions. We use the Multi-Radar Multi-Sensor quantitative precipitation estimation data products and analyze the hourly precipitation maps for 27 selected cities across the continental United States from the years 2015–2021 summer months. Results show that about 80% of the studied cities exhibit a statistically significant downwind enhancement of precipitation. Additionally, we find that the precipitation pattern tends to be more spatially clustered in intensity under higher wind speed; the location of radial precipitation maxima is located closer to the city center under low background winds but shifts downwind under high wind conditions. The magnitude of downwind precipitation enhancement is highly dependent on wind directions and is positively correlated with the city size for the south, southwest, and west directions. This study presents observational evidence through a cross-city analysis that the urban precipitation pattern can be influenced by the urban modification of atmospheric processes, providing insight into the mechanistic link between future urban land-use change and hydroclimates.

54 ENVIRONMENTAL SCIENCES↗

Tri-molybdenum phosphide (Mo 3 P) and multi-walled carbon nanotube junctions for volatile organic compounds (VOCs) detection

Detection and analysis of volatile organic compounds' (VOCs) biomarkers lead to improvement in healthcare diagnosis and other applications such as chemical threat detection and food quality control. Here, we report on tri-molybdenum phosphide (Mo3P) and multiwalled carbon nanotube (MWCNT) junction-based vapor quantum resistive sensors (vQRSs), which exhibit more than one order of magnitude higher sensitivity and superior selectivity for biomarkers in comparison to pristine MWCNT junctions based vQRSs. Transmission electron microscope/scanning tunneling electron microscope with energy dispersive x-ray spectroscopy, x-ray diffraction, and x-ray photoelectron spectroscopy studies reveal the crystallinity and the presence of Mo and P elements in the network. The presence of Mo3P clearly enhanced the performance of vQRS as evidenced in sensitivity and selectivity studies. The vQRSs are stable over extended periods of time and are reproducible, making them a potential candidate for sensing related applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An Adaptive Reference Scheme to Extend the Functional Range of Optical Backscatter Reflectometry in Extreme Environments

Optical frequency domain reflectometry (OFDR) measurements are performed by recording the interference pattern of light backscattered by density fluctuations or Bragg gratings along the length of an optical fiber. Changes in local temperature or strain in the fiber cause shifts in the backscattered light spectrum, which can be calibrated to the applied temperature or strain. Comparing the backscattered optical spectra from each reflection site with a reference (unstrained) spectrum allows for quantification of local spectral shifts. While mature OFDR-based technologies can provide high-precision spatially distributed measurements over kilometer lengths, the post-processing approaches used to recover spectral shifts from raw optical intensity data can limit the use of OFDR in harsh environments. This paper presents a novel approach to post-processing OFDR data which extends the usability of optical fibers exposed to harsh environments. This approach is the first to use the spectral shift quality, calculated for two OFDR measurements, to identify an appropriate reference scan from which the spectral shift can be determined. Here, three experimental data sets are used to test the algorithm: (1) an optical fiber heated to >950°C, (2) an aluminum-embedded optical fiber under strain from differential thermal expansion, and (3) an optical fiber exposed to a total neutron flux of 2×10 13 n/cm 2 /s over 40 hours in a nuclear test reactor. Results show that using a metric of quality to select an appropriate reference measurement extends the functional range of OFDR strain and temperature sensors. Furthermore, this algorithm can be applied to existing OFDR data.

47 OTHER INSTRUMENTATION↗

Advanced SOFC quality control and the role of manufacturing defects on stack reliability

Atrex Energy rolled out first commercial SOFC generator products in 2013. Following that we embarked on implementation of mass production in order to ramp up productivity and lower the costs in the meantime. To ensure the goal of mass production, an accurate, cost effective and consistent quality control methodology needs to be in place. The aim of this DOE funded project is to devise a machine and methodology for cell quality control using modern non-destructive testing methods and cell rejection criterion based on the empirical determination of the role of manufacturing flaws on stack degradation and reliability. The work scope encompasses two goals aimed at 1) developing automatable techniques for objective flaw detection and 2) developing an understanding of the ramifications of flaws on stack and cell reliability. By accomplishing these two goals it is likely that an advanced stage Quality Control (QC) device can be developed. This project scope encompasses: 1) Invention of a high speed automated instrument for spatial mapping of surface and sub-surface imperfections in production cells (ex situ) using modern imaging techniques. 2) Identification of rejection criteria upon which to screen cells from production by: a. Magnification of the effect of production defects on cell degradation through fabrication and testing of micro-cells which encompass these imperfections. b. The long term testing of full size production cells both as single cells and in small stacks, in order to correlate the (in situ) performance and degradation with the imperfection type (identified ex-situ) and hence be able to classify imperfections as actual defects. We first built a defect library with the cells containing imperfections classified and documented. The cells with various imperfections were tested to evaluate the imperfection potential impact on cell electrochemical performance. Evaluations were conducted on minicell, single cell and stack levels. On minicell level, pinhole, scratch, crack, contamination, and pop-out were investigated. We found: (1) none of the imperfections causes calamity type failure, (2) pinholes do not show measurable effect on minicell performance, (3) imperfection such as electrolyte abrasion, scratch, and pop out cause minicell potential to fluctuate by different degrees; the cells with such imperfections exhibit sensitivity of potential to high fuel utilization and “self healing” behavior. On single cell level we evaluated the effect of long crack and high population pinholes. The cell with a long crack does not show performance compromise at start. There is no potential fluctuation or sensitivity to high fuel utilization or catastrophic failure. The voltage degradation due to thermal cycle is slightly higher than normal cells. The cells with high population pinholes perform surprisingly as well as normal cells over a period of 3,500h. Even when subjected to cyclic load condition, the cells 4 show negligible degradation. Our cells appear to have “self immunization” feature which fends off the adversary effects of certain imperfections. Defects were also evaluated on stack level. Two stacks were made each with ten defect cells. The first stack was tested for 13,2000h under steady load condition while the second was tested for 9,000h under transient load conditions. We found: (1) voltage fluctuation and sensitivity to thermal cycle were not observed in contrast to minicell test, (2) of the various cracks examined, including longitudinal cracks, circumferential crack, crack near closed and open ends, none exhibited distinguishable impact on performance, (3) defect cells exhibited higher degradation rates on average under steady load condition; Individually some defect cells performed similarly or better than reference cells, (4) under steady load condition all the cells degrade monotonically with degradation rate increasing with time, (5) under cyclic (transient) load condition, both defect and reference cells exhibit complex dynamic behaviors, (6) fuel loss (leak) was measured occasionally for stack 1, the cells with crack showed the highest fuel loss increase, nevertheless, no correlation with performance degradation could be established with certainty, and (7) no catastrophic failure ever happened other than incremental degradation. Posttest inspection and microanalysis were carried out; the observations are summarized in what follows: (1) Electrolyte pinholes, some scratches and IC porosity became undetectable after testing. (2) The cathode covering the popout defects is intact without any cracking or delamination. (3) The scratch was covered by cathode in pristine state; Ni oxide or NiO-YSZ filled the space where electrolyte was missing. After >10,000h operation, the cathode that used to cover the scratch was missing but the size of the scratch remains unchanged; there is a fairly dense Ni oxide layer on top of the scratch. (4) All of the cracks remain their original dimensions. Current collector kept longitudinal cracks closed which mitigated the adversary effect of crack on cell performance/durability. (5) The crack at open end showed some deterioration manifested by a small oxidation zone in the vicinity of the crack. Wide spectrum of imaging techniques were surveyed and evaluated to detect tubular SOFC defects. Optical methods, with and without assistance of expression technique, were applied to detect all kinds of defects. Thermograph method in combination of CO2 leak, ultra-sound and electric potential was also extensively evaluated to detect surface and under-surface defects such as short circuit. Based on these works, laser camera has been selected to build the final QC machine vision inspection system. The Gocator laser profile sensor was setup to generate 2D surface intensity images of tubular SOFC surface which were analyzed with Sherlock machine vision software supplied by Teledyne Dalsa. The Gocator output was integrated with the Sherlock software and enabled live images to be imported by a Common Vision Blox driver. The Sherlock software was programmed to detect various surface defects from the surface intensity images generated by the Gocator. These measurements are subsequently used to make pass or fail decisions.

01 COAL, LIGNITE, AND PEAT↗