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At least 109 records · Page 6

Developing Fluorescence-Based Sensors to Support Rare Earth Element Separation

Rare earth elements (REEs) are essential to most renewable energy technologies. Unfortunately, as we transition to sustainable energy production, the demand for REEs is rapidly growing well beyond current rates of production. As a result, novel means of efficient, scalable, and easily adaptable methods for processing primary and recycle feedstocks are needed. Development and integration of sensors for highly selective in-line monitoring can support more efficient design and testing of such novel separation processes, as well as more cost-effective deployment of those separation flowsheets. Work here will explore the application of fluorescence spectroscopy, a highly sensitive and selective technique, to quantify multiple lanthanides in complex mixtures including known interferents or quenching agents. Results include identification of the optimal excitation wavelength and the limit of detection of various rare earth elements as well as the performance of data-science-based quantification approaches in streams where “unknowns” are present. Overall, the data science tools in conjunction with optical sensor data were able to quantify analytes in the presence of other lanthanides which can be anticipated in the actual industrial stream. Here we include characterization of lanthanides in a microfluidic device similar to those used in new process development. This study demonstrates the capability of utilizing fluorescence spectroscopy to quantify analytes in a complicated solution matrix, suggesting this is a successful approach for in-line monitoring to optimize the separation efficiency in an industrial stream.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Magnetic field sensors for detection of trapped flux in superconducting radio frequency cavities

Superconducting radio-frequency (SRF) cavities are fundamental building block of modern particle accelerators. They operate at liquid helium temperatures 2-4 K to achieve very high quality factors 1e10-1e11. Trapping of magnetic flux within the superconductor is a significant contribution to the residual RF losses which limit the achievable quality factor. Suitable diagnostic tools are in high demand to understand the mechanisms of flux trapping in technical superconductors and the fundamental components of such diagnostic tool are magnetic field sensors. We have studied the performance of commercially available Hall probes, anisotropic magnetoresistive sensors and flux-gate magnetometers with respect to their sensitivity and capability to detect localized, low magnetic flux amplitudes, of the order of few tens of magnetic flux quantum at liquid helium temperature. Although Hall probes have the lowest magnetic field sensitivity (~96$ nV$/microT at 2 K), their physical dimensions are such that they have the ability to detect the lowest number of trapped vortices among the three type of sensors. Hall probes and anisotropic magnetoresistive sensors have been selected to be used in a setup to map regions of trapped flux on the surface of a single-cell SRF cavity.

47 OTHER INSTRUMENTATION↗

Elevation distributed micro-climatology data in a coastal glaciated watershed

Air temperature, ground temperature and relative humidity data were collected in a longitudinal transect of the Nooksack watershed at varying elevations from 500 to 1800 m above sea level. Data were collected by anchoring sensors from trees above winter snow levels and shaded from direct solar radiation. Paired sensors were also buried 3 cm under ground near each air temperature sensor to determine snow absence or presence. Select sites included relative humidity sensors to indicate whether precipitation was occurring. Data were collected every 3-4 h from December 2015 to Sept 2018 (with ongoing collection). Code for analysis of daily mean, minimum, maximum, and temperature change with elevation (lapse rates) are available on Github (https://doi.org/10.5281/zenodo.3239539). The sensor download and intermediate data products are available on HydroShare at (http://www.hydroshare.org/resource/222e832d3df24dea9bae9bbeb6f4219d) with publicly accessible visualization available from the Nooksack Observatory at data.cuahsi.org. Hydrologic models are generally structured with a single annual average lapse rate parameter which assumes a linear temperature gradient with elevation. The daily data (2016-2018) is used as part of ongoing studies on the non-linear dynamics and temporal variability of temperature with elevation to improve assessments of watershed function and salmon habitat.

54 ENVIRONMENTAL SCIENCES↗

MARVEL Instrumentation, Control, and Software Considerations

This paper details the various I&C considerations and design decisions made throughout the MARVEL (Micro-reactor Applications Research Validation and Evaluation) project, including sensor and actuator selection, safety-related functionality, digital control hardware and software, and testing methodologies. Key challenges such as managing radiation, temperature, and space constraints are discussed, along with the trade-offs between using standard equipment and custom solutions. The successful integration of off-the-shelf components, the emphasis on minimizing safety-related instrumentation, and the lessons learned from prototyping and testing are highlighted. The authors aim to provide insights that can benefit future micro-reactor designs and emphasize the importance of real-world testing in advancing reactor technology.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

Exceptional Electrical Detection of Trace NO 2 via Mixed Metal MOF-on-MOF Film-Based Sensors

The tunability of metal–organic frameworks (MOFs) makes them exceptional materials for the development of highly selective, low-power sensors for toxic gas detection. Herein, we demonstrate enhanced detection of NO 2 gas by a MOF-based electrical impedance sensor made using a unique mixed metal MOF-on-MOF synthesis. For this work, a combined experimental and computational study was performed using the exemplar Ni x Mg 1–x -MOF-74 to understand the fundamental structure–property relationships behind metal mixing and MOF film synthesis methods on sensor performance. Density functional theory results indicated that the presence of Ni in Mg-MOF-74 increased framework stability and increased the electron density of states at lower energies near the HOMO, as well as enhanced the NO 2 –Mg adsorption interaction. Impedance data of the Ni x Mg 1–x -MOF-74 films with larger Ni contents showed greater impedance change after exposure to 1 ppm of NO 2 gas. Furthermore, when synthesized through either a drop-cast or direct solvothermal film growth approach, the monometallic Ni-based sensors had the best performance. However, the mixed metal Ni x Mg 1–x -MOF-74 sensors synthesized through a MOF-on-MOF approach resulted in the highest impedance change, outperforming all monometallic Ni-based sensors. In particular, the mixed metal Ni-on-Mg-MOF-74 film was the best-performing sensor with an impedance change of 309 upon trace NO 2 exposure. Change in impedance response after NO 2 exposure was improved by 52% compared to the best monometallic Ni-on-Ni-MOF-74 sensor. Structural analysis of the Ni-on-Mg film showed that the first Mg-MOF-74 layer acts as a structural template controlling the structural features of the final film after metal exchange with Ni. This led to improved film quality, evidenced by the greater crystallinity and larger MOF grain sizes, and resulted in enhanced sensor performance which was not achievable through other metal mixing methods. Altogether, this study identifies structure–property relationships and synthetic templating methods that inform MOF-based sensor design, allowing for improved detection of toxic compounds.

36 MATERIALS SCIENCE↗

Reversible parts-per-trillion-level detection of perfluorooctane sulfonic acid in tap water using field-effect transistor sensors

Widespread, persistent and toxic per- and polyfluoroalkyl substances (PFAS) pose a major threat to water systems and human health. Current detection methods are relatively expensive, slow and complex, underscoring the need for more accessible alternatives to meet increasingly stringent PFAS regulations. Here, in this study, we present an ultrasensitive sensing platform for perfluorooctane sulfonic acid detection in tap water with a reporting limit ( ~ 250 parts per quadrillion) lower than the US Environmental Protection Agency’s regulatory standard (4 parts per trillion), using a remote gate field-effect transistor featuring β-cyclodextrin (β-CD)-modified reduced graphene oxide as the sensing membrane. The sensor exhibits excellent selectivity against common inorganic ions, natural organic matter and select organic pollutants in tap water. The reversible and rapid response ( < 2 min) indicates the potential of remote gate field-effect transistor for continuous in-line monitoring. Mechanistic studies using quartz crystal microbalance and molecular dynamics simulations reveal key roles of analyte adsorption and charge properties in sensing performance and offer insights for designing more selective PFAS capture probes.

Wang, Yuqin [University of Chicago, IL (United Sta↗

Time-resolved detectors for quantum ghost imaging

Quantum ghost imaging is a method that utilizes the correlated detection of two photons to generate an image. One photon is detected by an imaging sensor and the other by a single-element bucket detector. The selection of the imaging sensor and its capabilities relative to the bucket detector impact the quality of the ghost images. This work examines a SPAD array and a photocathode detector as imaging sensors for quantum ghost imaging. We discuss how to achieve optimal images using these two technologies. We also demonstrate that these devices are able to generate ghost images at 1Hz frame rates, expanding the technique to biologically relevant time scales.

36 MATERIALS SCIENCE↗

Improved Hydrogen Sensitivity and Selectivity in PdO with Metal-Organic Framework Membrane

Metal-organic frameworks (MOFs) are highly designable porous materials and are recognized for their exceptional selectivity as chemical sensors. However, they are not always suitable for incorporation with existing sensing platforms, especially sensing modes that rely on electronic changes in the sensing material (e.g., work-function response or conductometric response). One way that MOFs can be utilized is by growing them as a porous membrane on a sensing layer and using the MOF to affect the electronic structure of the sensing layer. In this paper, a proof-of-concept for electronic modulation with MOFs is demonstrated. A PdO nanoparticle sensing layer on a chemical-sensitive field-effect-transistor is made more sensitive to a reducing gas, hydrogen, and less sensitive to oxidizng molecules, like H 2 S and NO 2 , by growing a layer of the MOF “ZIF-8” over the nanoparticles. The proposed mechanism is supported by X-ray photoelectron spectroscopy showing that the ZIF-8 membrane partially reduces the PdO sensing layer.

Gardner, David W. (ORCID:0000000193518391)↗

All-optical, Microwave-free NV-Diamond Magnetometer for Weak Magnetic Field Environments

Sensitive nitrogen-vacancy (NV) magnetometry typically requires a bias field to lift the spin level degeneracy and has commonly utilized microwave sources to selectively manipulate the sensor's spin state. However, this external bias field and microwave sources may perturb the sample of interest or be incompatible with operational conditions. Here, we demonstrate an all-optical, microwave-free NV-diamond magnetometer in the presence of weak or no bias magnetic field (<20 G). We experimentally measure photoluminescence spectra using diamonds with varying NV concentrations; and numerically simulate matching features due to cross-relaxation between NVs. Our results pave the way towards a sensitive probe to study magnetic systems that can be disrupted by microwave signals and can only tolerate weak bias magnetic field.

Ung, Kristine↗

Ocean surface radiation measurement best practices

Ocean surface radiation measurement best practices have been developed as a first step to support the interoperability of radiation measurements across multiple ocean platforms and between land and ocean networks. This document describes the consensus by a working group of radiation measurement experts from land, ocean, and aircraft communities. The scope was limited to broadband shortwave (solar) and longwave (terrestrial infrared) surface irradiance measurements for quantification of the surface radiation budget. Best practices for spectral measurements for biological purposes like photosynthetically active radiation and ocean color are only mentioned briefly to motivate future interactions between the physical surface flux and biological radiation measurement communities. Topics discussed in these best practices include instrument selection, handling of sensors and installation, data quality monitoring, data processing, and calibration. It is recognized that platform and resource limitations may prohibit incorporating all best practices into all measurements and that spatial coverage is also an important motivator for expanding current networks. Thus, one of the key recommendations is to perform interoperability experiments that can help quantify the uncertainty of different practices and lay the groundwork for a multi-tiered global network with a mix of high-accuracy reference stations and lower-cost platforms and practices that can fill in spatial gaps.

54 ENVIRONMENTAL SCIENCES↗

Embedding sensors in 3D-printed silicon carbide

An improved method for embedding one or more sensors in SiC is provided. The method includes depositing a binder onto successive layers of a SiC powder feedstock to produce a dimensionally stable green body have a true-sized cavity. A sensor component is then press-fit into the true-sized cavity. Alternatively, the green body is printed around the sensor component. The assembly (the green body and the sensor component) is heated within a chemical vapor infiltration (CVI) chamber for debinding, and a precursor gas is introduced for densifying the SiC matrix material. During infiltration, the sensor component becomes bonded to the densified SiC matrix, the sensor component being selected to be thermodynamically compatible with CVI byproducts at elevated temperatures, including temperatures in excess of 1000° C.

Petrie, Christian M.↗

Molecularly Imprinted Polymer Sensor Empowered by Bound States in the Continuum for Selective Trace-Detection of TGF-beta

The integration of advanced materials and photonic nanostructures can lead to enhanced biodetection capabilities, crucial in clinical scenarios and point-of-care diagnostics, where simplified strategies are essential. Herein, a molecularly imprinted polymer (MIP) photonic nanostructure is demonstrated, which selectively binding to transforming growth factor-beta (TGF-β), in which the sensing transduction is enhanced by bound states in the continuum (BICs). The MIP operating as a synthetic antibody matrix and coupled with BIC resonance, enhances the optical response to TGF-β at imprinted sites, leading to an augmented detection capability, thoroughly evaluated through spectral shift and optical lever analogue readout. The validation underscores the MIP-BIC sensor capability to detect TGF-β in spiked saliva, achieving a limit of detection of 10 fM and a resolution of 0.5 pM at physiological concentrations, with a precision of two orders of magnitude above discrimination threshold in patients. The MIP tailored selectivity is highlighted by an imprinting factor of 52, showcasing the sensor resistance to interference from other analytes. The MIP-BIC sensor architecture streamlines the detection process eliminating the need for complex sandwich immunoassays and demonstrates the potential for high-precision quantification. This positions the system as a robust tool for biomarker detection, especially in real-world diagnostic scenarios.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Postirradiation Examination of WIRE-21 Experiment Irradiated in the High Flux Isotope Reactor

Westinghouse Electric Company is developing wireless sensors to monitor the centerline temperature and internal pressure of commercial light-water reactor fuel rods during irradiation. Oak Ridge National Laboratory and Westinghouse Electric Company developed the Wireless Instrumented RB Experiment 2021 (WIRE-21) to test wireless temperature and pressure sensor technologies in a removable beryllium position in the High Flux Isotope Reactor. The experiment was irradiated for a total of 75 days, at temperatures ranging from approximately 150°C to 400°C, resulting in a peak fast (energy > 0.1 MeV) neutron fluence of about 3 × 10 21 n/cm 2 . The temperature was intentionally cycled multiple times to compare the response of the wireless temperature sensor to collocated thermocouples. Similarly, the pressure sensor was actuated in multiple steps to compare the response of the wireless measurement to excore pressure transducers (Petrie et al., 2023). After irradiation, the experiment was disassembled in the Irradiated Fuels Examination Laboratory (IFEL) hot cell at Oak Ridge National Laboratory with the intent to recover sensor and dosimetry components, document the as-irradiated condition of the hardware, and investigate possible causes of the sensor behavior observed during irradiation. The postirradiation examination successfully recovered and preserved key WIRE-21 components. After the housing was removed using a milling machine, the internal experiment sections were examined. All eight fiber-optic sensors were recovered, cut, and stored. The silicon carbide thermometry, temperature sensor, pressure sensor, lower spacer, and selected pressure and temperature cable sections were also removed and stored. The metal bellows of the pressure sensor was found to be plastically deformed, indicating that it had been properly pressurized during irradiation and generally behaved as expected. X-ray diffraction analysis of a section of one of the irradiated inductor cores within the pressure sensor was performed and confirmed the presence of phase-pure alpha ferrite (i.e., no unexpected phase transformations). Inductance testing was performed on the irradiated pressure sensor cores using an unirradiated test coil, and DC resistance measurements of the transceiver coils were also performed. The measurements with irradiated inductor cores assembled inside unirradiated coils showed slightly reduced inductance compared to measurements made with unirradiated cores, but the difference was not sufficient to explain the more significant reductions in inductance that were observed in-pile. Therefore, it is suspected that degradation of the inductor coils (specifically the wire wrapping) is responsible for the reduced inductance observed in-pile.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Development and Test of High Temperature Surface Acoustic Wave Gas Sensors

The demand for sensors in hostile environments, such as power plant environments, aerospace environments, oil and gas extraction, and high-temperature metallurgy environments, has risen over the past decades in a continuous attempt to increase process control, improve energy and process efficiency in production, reduce operational and maintenance costs, increase safety, and perform condition-based maintenance in equipment and structures operating in high-temperature harsh-environment conditions. The increased reliability, improved performance, and development of new sensors and networks with a multitude of components, especially wireless networks, are the target for operation in harsh environments. Gas sensors, in particular H2 sensors, operating above 200 C are required in the instrumentation, process control and general safety of a number of industries including coal, natural gas, and nuclear power generation facilities, the aerospace and automotive industries, metallurgical production and defense-related applications. The surface acoustic wave (SAW) platform is a particularly promising option for high-temperature, harsh-environment gas sensing applications since the platform exhibits advantages, such as battery-free and wireless operation, small size, possibility for scale production using well-developed technologies from the semiconductor industry, and low cost of installation and operation. In this work, one-port SAW resonators (SAWRs) operating along five different orientations on a commercially available langasite (LGS) wafer employing Pt-Al2O3 electrodes and reflectors were designed, fabricated, and used as high-temperature H2 sensors. Two of the selected orientations were predicted and confirmed to have temperature-compensated operation above 150 C. A gas sensor test setup was developed, capable of gas cycling between N2, O2 and N2/H2 mixtures under extended high-temperature periods (up to 650 C for over 20 hours). Thin film Pt-Al2O3 was used as the electrode material for the transducers and reflectors capable of high-temperature operation, and also as H2 sensing film. In addition, yttria-stabilized zirconia (YSZ) thin films with Pt decoration were tested as sensing films aimed to enhance the SAWR sensor response to H2. The SAW devices were monitored in excess of 1700 hours in real-time during gas cycling sequences up to 600 C, leading to the following findings: i) the Pt-Al2O3 electrodes performed better for H2 sensing than the Pt-decorated YSZ sensing film, showing as much as 50% higher frequency variation response in the 200 C to 400 C range; ii) different crystallographic orientations operating on the same LGS wafer experienced different responses to H2 exposures up to 500 C; iii) the surface oxidation state of the SAWR sensors was shown to have an important impact on subsequent H2 exposure responses. In addition, a sensor system employing two LGS SAWRs, aligned along two different orientations, has been developed to simultaneously determine H2 presence and temperature. Finally, wireless interrogation of a SAWR sensor was successful within the gas cycling test fixture, and successful wireless H2 detection was achieved above 400 C.

Ayes Moncada, Armando↗

In Situ Synthesis of Molybdenum Carbide Nanoparticles Incorporated into Laser‐Patterned Nitrogen‐Doped Carbon for Room Temperature VOC Sensing

Abstract Carbon laser‐patterning (CLaP) is emerging as a new tool for the precise and selective synthesis of functional carbon‐based materials for on‐chip applications. The aim of this work is to demonstrate the applicability of laser‐patterned nitrogen‐doped carbon (LP‐NC) for resistive gas‐sensing applications. Films of pre‐carbonized organic nanoparticles on polyethylenetherephthalate are carbonized with a CO 2 ‐laser. Upon laser‐irradiation a compositional and morphological gradient in the films is generated with a carbon content of 92% near the top surface. The specific surface areas of the LP‐NC are increased by introducing sodium iodide (NaI) as a porogen. Electronic conductivity and surface area measurements corroborate the deeper penetration of the laser‐energy into the film in the presence of NaI. Furthermore, impregnation of LP‐NC with MoC 1− x (<10 nm) nanoparticles is achieved by addition of ammonium heptamolybdate into the precursor film. The resulting doping‐sensitive nano‐grain boundaries between p‐type carbon and metallic MoC 1− x lead to an improvement of the volatile organic compounds sensing response of Δ R / R 0 = −3.7% or −0.8% for 1250 ppm acetone or 900 ppm toluene at room temperature, respectively, which is competitive with carbon‐based sensor materials. Further advances in sensitivity and in situ functionalization are expected to make CLaP a useful method for printing selective sensor arrays.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Virtual refrigerant charge sensor for variable-speed heat pumps based on feature selection

The refrigerant charge level in heat pump systems significantly impacts their energy efficiency. Virtual refrigerant charge (VRC) sensing technology has been comprehensively investigated and well-established due to its lower cost compared to physical sensors. However, the previous VRC research often relied on expert judgment and physical reasoning for their variable selection, which can potentially select redundant (or highly correlated) or insignificant features, and it is also primarily focused on single-speed systems. To address these challenges, this study proposes a VRC algorithm for variable-speed heat pumps that selects features through a rigorous feature selection method in combination with physical insights. We also propose a piecewise linear model structure segmented by subcooling temperature to accurately predict charge levels, particularly when subcooling temperatures are substantially low. The proposed algorithm was evaluated using experimental data of a residential R410A heat pump, and the performance was compared with two baseline VRC algorithms. The results are: (1) The proposed algorithm outperforms for the case with subcooling temperature less than 1 °C. (2) The proposed algorithm achieves a tested mean absolute percentage error (MAPE) of 4.23%, and improves the overall accuracy for cooling conditions by approximately 60%, compared with the two baseline algorithms. (3) The proposed algorithm uses two fewer features and improves the accuracy for undercharge cooling conditions by 68.0%, compared with baseline algorithm 2. These improvements enhance prediction accuracy and prevent overfitting, providing a more reliable refrigerant charge level prediction and helping improve the heat pump energy efficiency.

Liang, Chenjiyu↗

In-situ localized growth of porous metal oxide films on microheater platform for low temperature gas detection

A solid-state, low power microheater sensor platform that is configurable with selected metal oxide films for particular gas sensing applications is described. The sensor platform is configured by selecting a chemiresistive or catalytic material that is suitable for detecting a desired gas and then forming a porous nanostructured film on the designated surfaces of the microheater platform. Also described are methods for creating a highly porous, nanostructured metal oxide film in a controlled location from a liquid precursor using a localized heat source. By fast annealing deposited liquid precursors with the microheater, a highly porous, nanocrystalline metal oxide film can be generated in-situ and locally on the sensor platform.

Maboudian, Roya↗