The structure of the Clostridium thermocellum RsgI9 ectodomain provides insight into the mechanism o
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Mahoney, Brendan J.↗
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Template‐Directed Growth of Palladium Nanoparticles in Holey Single‐Layer Graphene for High‐Performance Room‐Temperature Hydrogen Sensing
Holey graphene (HG), formed by introducing nanoscale perforations into graphene sheets, combines the structural advantages of continuous sp 2 conjugation with the beneficial effects of high surface area and enhanced chemical reactivity associated with nanoscopic holes. Conventional HG fabrication methods often rely on harsh oxidative treatments that compromise graphene's intrinsic electronic properties by disrupting its sp 2 conjugation. A new approach is introduced to fabricate HG directly from single-layer graphene (SLG), using two-dimensional covalent organic frameworks (COFs) as a template followed by controlled oxygen plasma etching. This method preserves the integrity of the SLG's sp 2 network while producing well-defined holes with an average diameter of 2.7 nm. These hole edges act as reactive sites that facilitate the confined, autoreductive growth of palladium nanoparticles (PdNPs) without external reducing agents. The confined hole geometry prevents NP agglomeration and ensures a uniform size distribution. The resulting Pd@HG hybrid exhibits exceptional chemiresistive hydrogen sensing characteristics, including ultrahigh sensitivity, low detection limits, rapid response and recovery, and long-term stability under both dry and humid conditions. Mechanistic investigations reveal a two-step sensing process involving surface redox interactions and hydrogen absorption into the PdNP lattices. This strategy presents a scalable platform for integrating metal NPs within conductive carbon frameworks for advanced sensing applications.
chemical vapor deposition↗
Assessment of wafer scale MoS 2 atomic layers grown by metal–organic chemical vapor deposition using organo-metal, organo-sulfide, and H 2 S precursors
Transition Metal Dichalcogenides (TMDs) are a unique class of materials that exhibit attractive electrical and optical properties which have generated significant interest for applications in microelectronics, optoelectronics, energy storage, and sensing. Considering the potential of these materials to impact such applications, it is crucial to develop a reliable and scalable synthesis process that is compatible with modern industrial manufacturing methods. Metal–organic chemical vapor deposition (MOCVD) offers an ideal solution to produce TMDs, due to its compatibility with large-scale production, precise layer control, and high material purity. Optimization of MOCVD protocols is necessary for effective TMD synthesis and integration into mainstream technologies. Additionally, improvements in metrology are necessary to measure the quality of the fabricated samples more accurately. In this work, we study MOCVD of wafer-scale molybdenum disulfide (MoS 2 ) utilizing two common chalcogen precursors, H 2 S and DTBS. We then develop a metrology platform for wafer scale samples quality assessment. For this, the coalesced films were characterized using Raman spectroscopy, atomic force microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and Kelvin probe force microscopy. We then correlate the structural analysis of these grown films with electrical performance by using aerosol jet printing to fabricate van der Pauw test structures and assess sheet resistance.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Exposure, health effects, sensing, and remediation of the emerging PFAS contaminants – Scientific challenges and potential research directions
Per- and polyfluoroalkyl substances (PFAS) make up a large group of persistent anthropogenic chemicals which are difficult to degrade and/or destroy. PFAS are an emerging class of contaminants, but little is known about the long-term health effects related to exposure. In addition, technologies to identify levels of contamination in the environment and to remediate contaminated sites are currently inadequate. In this opinion-type discussion paper, a team of researchers from the University of Connecticut and the University at Albany discuss the scientific challenges in their specific but intertwined PFAS research areas, including rapid and low-cost detection, energy-saving remediation, the role of T helper cells in immunotoxicity, and the biochemical and molecular effects of PFAS among community residents with measurable PFAS concentrations. Potential research directions that may be employed to address those challenges and improve the understanding of sensing, remediation, exposure to, and health effects of PFAS are then presented. Here, we hope our account of emerging problems related to PFAS contamination will encourage a broad range of scientific experts to bring these research initiatives addressing PFAS into play on a national scale.
Challenges and research directions↗
High field magnetometry with hyperpolarized nuclear spins
Abstract Quantum sensors have attracted broad interest in the quest towards sub-micronscale NMR spectroscopy. Such sensors predominantly operate at low magnetic fields. Instead, however, for high resolution spectroscopy, the high-field regime is naturally advantageous because it allows high absolute chemical shift discrimination. Here we demonstrate a high-field spin magnetometer constructed from an ensemble of hyperpolarized 13 C nuclear spins in diamond. They are initialized by Nitrogen Vacancy (NV) centers and protected along a transverse Bloch sphere axis for minute-long periods. When exposed to a time-varying (AC) magnetic field, they undergo secondary precessions that carry an imprint of its frequency and amplitude. For quantum sensing at 7T, we demonstrate detection bandwidth up to 7 kHz, a spectral resolution < 100mHz, and single-shot sensitivity of 410pT $$/\sqrt{{{{{{{{\rm{Hz}}}}}}}}}$$ / Hz . This work anticipates opportunities for microscale NMR chemical sensors constructed from hyperpolarized nanodiamonds and suggests applications of dynamic nuclear polarization (DNP) in quantum sensing.
73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
High spatial resolution charge sensing of quantum Hall states
Charge distribution offers a unique fingerprint of important properties of electronic systems, including dielectric response, charge ordering, and charge fractionalization. Here, we develop an architecture for charge sensing in two-dimensional electronic systems in a strong magnetic field. We probe local change of the chemical potential in a proximitized detector layer using scanning tunneling microscopy, allowing us to infer the chemical potential and the charge profile in the sample. Our technique has both high energy (<0.3 meV) and spatial (<10 nm) resolution exceeding that of previous studies by an order of magnitude. We apply our technique to study the chemical potential of quantum Hall liquids in monolayer graphene under high magnetic fields and their responses to charge impurities. The chemical potential measurement provides a local probe of the thermodynamic gap of quantum Hall ferromagnets and fractional quantum Hall states. The screening charge profile reveals spatially oscillatory response of the quantum Hall liquids to charge impurities and is consistent with the composite Fermi liquid picture close to the half-filling. Our technique also paves the way to map moiré potentials, probe Wigner crystals, and investigate fractional charges in quantum Hall and Chern insulators.
charge sensing↗
Dopant Segregation in Single-Crystal Optical Fiber Grown via the Laser-Heated Pedestal Growth Technique
Single crystal (SC) optical fiber has promising potential to be used for optical fiber sensing applications in harsh conditions due to its robustness to high temperature, high radioactivity, and resistance to chemical corrosion as compared to optical sensors using silica fiber. However, SC fiber grown via the laser-heated pedestal growth (LHPG) technique innately does not have a core-cladding structure found in standard optical fiber, resulting in optical losses. In this work we investigate optimization of the growth parameters of a two LHPG process used to grow SC fiber with a graded index via introduction of dopants to the feedstock material. Feedstock material is fabricated with the first LHPG device, then sol-gel dip-coated to create outer films of dopant material. The dip-coated feedstock is used to grow SC fiber in which segregation of the dopant constituents occurs, resulting in a graded index of refraction across the fiber, and an effective core-cladding structure. Hardware and software improvements to both LHPG systems are presented and the growth parameters for short pieces of ~320-330 μm diameter YAG fiber has been established. Characterization techniques/procedures have also been established for future grown SC fiber. These improvements and preparations are anticipated to result in a significant increase in grown fiber quality with a similar growth rate to that previously established.
Lander, Gary↗
Dopant Segregation in Single-Crystal Optical Fiber Grown via the Laser-Heated Pedestal Growth Technique
Single crystal (SC) optical fiber has promising potential to be used for optical fiber sensing applications in harsh conditions due to its robustness to high temperature, high radioactivity, and resistance to chemical corrosion as compared to optical sensors using silica fiber. However, SC fiber grown via the laser-heated pedestal growth (LHPG) technique innately does not have a core-cladding structure found in standard optical fiber, resulting in optical losses. In this work we investigate optimization of the growth parameters of a two LHPG process used to grow SC fiber with a graded index via introduction of dopants to the feedstock material. Feedstock material is fabricated with the first LHPG device, then sol-gel dip-coated to create outer films of dopant material. The dip-coated feedstock is used to grow SC fiber in which segregation of the dopant constituents occurs, resulting in a graded index of refraction across the fiber, and an effective core-cladding structure. Hardware and software improvements to both LHPG systems are presented and the growth parameters for short pieces of ~320-330 μm diameter YAG fiber has been established. Characterization techniques/procedures have also been established for future grown SC fiber. These improvements and preparations are anticipated to result in a significant increase in grown fiber quality with a similar growth rate to that previously established.
Lander, Gary↗
Universal Approach to Rapid Amplified Plasmonic Sensing Using Helix Defect Phase Transition Polymers
Abstract Permittivity sensing is a critically important analytical tool for bioscience, environmental, and industrial applications. The response time for commonly used plasmonic permittivity sensors is fundamentally set by the reaction kinetics of chemically adsorbed analytes. In this work, the proposal is to overcome this limit by combining plasmonic sensors with phase transition materials possessing a rapid amplified electrostatic response such as quadrupole moment induced molecular helix reversal. As a proof‐of‐concept, rapid sensing of CO 2 on a phase transition polytetrafluoroethylene substrate and amplification of permittivity response in plasmonic Fabry–Perot sensor is shown. The demonstrated universal approach holds promise for a wide range of applications in fast, real time sensing and monitoring of biological and environmental processes.
Shugayev, Roman↗
A Review: PFAS Adsorption, Sensing, and Remediation with Engineered Nanoporous Materials
Per- and polyfluoroalkyl substances (PFAS) are among the most abundant environmental contaminant species. They are widespread due to uncontrolled industrial and commercial use and have been linked to health risks such as cancer. With rising global concerns about the public health effects of PFAS, there is an incentive to develop strategies for reliable monitoring and effective PFAS removal, particularly in drinking water. Traditional PFAS sensing techniques are inefficient due to long measurement times, high labor input, high costs, and limitations to ex situ analysis. Current commercially available sorbents for PFAS removal generally lack the ability to capture PFAS components rapidly and quantitatively. Furthermore, existing sorbents are notably inefficient in removing the more toxic, smaller PFAS chemical chains. Large-scale applications of these methods tend to be costly and resource-intensive. Pacific Northwest National Laboratory has developed unique strategies for PFAS sensing and removal with capture probe technology that has an affinity for fluorocarbons, including PFAS. For both sensing and removal, the customizable capture probes can target specific PFAS compounds since they used a metal-organic framework (MOF)-based technology that can be fine-tuned and molecularly tailored. This tailoring of the materials enables high PFAS sensitivity, selectivity, and faster uptake. PNNL’s capture probe materials have been developed into a sensing technique based on the interactions of the capture probes with PFAS at the molecular level and further transduced that to a quantifiable electrochemical response. The materials have been integrated into a sensor platform developed by New Jersey Institute of Technology (NJIT). Tunable capture probes with a range of detection sensitivities allow for faster and more sensitive PFAS detection limits as low as what appears to be 0.5 ng/L (compared to the U.S. Environmental Protection Agency health advisory level of 70 ng/L). Customization of the capture probe results in improved sorption capacities (fast kinetics and high capacities) compared to commercial granular activated carbons. This research applied various experimental and modeling tools to improve understanding the molecular level interactions between the sorbents towards PFAS adsorption properties.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Compressed sensing methods with applications to advanced air sampling
Environmental sampling methods developed by the Savannah River National Laboratory (SRNL) employ collectors with sorbent media tubes set at various locations to collect airborne emissions. Laboratory analyses of these tubes results in one-dimensional signals regarding what chemicals are being released and transported within the atmosphere. The analysis process is time consuming especially when analyzing a full year’s worth of tubes (hourly sample collection results in nearly 9,000 tubes per year). Using a signal processing method such as compressed sensing allows for recreation of the full signal while greatly reducing the number of analyzed samples required. Due to the sparsity of data retrieved from the air tubes, it is possible to use measurements a fraction of the size of the original data to gain much of the same information. This would improve the overall time and cost of analysis when modeling one-dimensional sampling signals.
54 ENVIRONMENTAL SCIENCES↗
Scheimpflug LIDAR for Gas Sensing at Elevated Temperatures
Localized operating conditions inside boilers, heat recovery steam generators, or other large thermal systems have a huge impact on the efficiency, environmental performance, and lifetime of components. It is extremely difficult to measure species accurately within these systems due to the high temperatures and harsh environments, locally oxidizing or reducing atmospheres, ash, other particulates, and other damaging chemical species. Physical probes quickly suffer damage and are rendered nonfunctional. This work has attempted to adapt the measurement approach based on Scheimpflug light detection and ranging (S-LIDAR) for the remote sensing of gas species inside the high-temperature boiler environment. For a proof-of-concept, the detection of Raman signals of N 2 , O 2 , and CO 2 and their behavior with increasing temperature have been presented.
47 OTHER INSTRUMENTATION↗
Versatile & Intelligent Biodetection via Environmental Sensing (VIBES)
Reactive health monitoring strategies during events like the COVID-19 pandemic highlighted the need for predictive, threat-agnostic diagnostics that can detect both known diseases and novel chemical or biological threats. To address this, we investigated an optical biosensor as a breath volatile organic compound (VOC) analyzer, aiming to emulate biological olfaction. We assembled and validated the device with thin film metal coated substrate-based sensors. We immobilized small biological recognition elements on the substrates and delivered controlled concentrations of target VOCs. The sensor was irradiated with a visible laser and the sensor signal was recorded. We characterized the laser performance and tested 3 recognition elements for 2 VOCs with varying concentrations (1-100 ppm). We also evaluated enhancement of the signal using nanostructures on the metal film in comparison with planar film substrate. We demonstrated detecting ethanol reliably at concentrations as low as ~2 ppm along with preliminary detection of acetone (<100 ppm). We also found several unexpected factors that influence the sensor behavior that should be addressed to further refine the device’s performance. The nanostructures were, as expected, found to amplify the sensor signals. These findings demonstrate the feasibility of the optical bio-sensing modality for breath VOC monitoring at physiologically relevant levels. This positions LLNL to develop a low-cost, scalable, broad-spectrum health monitoring capability aligned with the Early Detection thrust of the Bioresilience Mission Focus Area and attract external funding.
47 OTHER INSTRUMENTATION↗
Compressed Sensing Methods with Applications to Advanced Air Sampling [Poster]
Environmental sampling methods developed by the Savannah River National Laboratory (SRNL) employ collectors with sorbent media tubes set at various locations to collect airborne emissions. Laboratory analyses of these tubes results in one-dimensional signals regarding what chemicals are being released and transported within the atmosphere. The analysis process is time consuming especially when analyzing a full year’s worth of tubes (hourly sample collection results in nearly 9,000 tubes per year). Using a signal processing method such as compressed sensing allows for recreation of the full signal while greatly reducing the number of analyzed samples required. Due to the sparsity of data retrieved from the air tubes, it is possible to use measurements a fraction of the size of the original data to gain much of the same information. This would improve the overall time and cost of analysis when modeling one-dimensional sampling signals.
Campbell, Cassidy [Savannah River National Laborat↗
Intercomparison of Planetary Boundary Layer Heights Using Remote Sensing Retrievals and ERA5 Reanalysis over Central Amazonia
The atmospheric boundary layer height (zi) is a key parameter in the vertical transport of mass, energy, moisture, and chemical species between the surface and the free atmosphere. There is a lack of long-term and continuous observations of zi, however, particularly for remote regions, such as the Amazon forest. Reanalysis products, such as ERA5, can fill this gap by providing temporally and spatially resolved information on zi. In this work, we evaluate the ERA5 estimates of zi (zi-ERA5) for two locations in the Amazon and corrected them by means of ceilometer, radiosondes, and SODAR measurements (zi-experimental). The experimental data were obtained at the remote Amazon Tall Tower Observatory (ATTO) with its pristine tropical forest cover and the T3 site downwind of the city of Manaus with a mixture of forest (63%), pasture (17%), and rivers (20%). We focus on the rather typical year 2014 and the El Niño year 2015. The comparison of the experimental vs. ERA5 zi data yielded the following results: (i) zi-ERA5 underestimates zi-experimental daytime at the T3 site for both years 2014 (30%, underestimate) and 2015 (15%, underestimate); (ii) zi-ERA5 overestimates zi-experimental daytime at ATTO site (12%, overestimate); (iii) during nighttime, no significant correlation between the zi-experimental and zi-ERA5 was observed. Based on these findings, we propose a correction for the daytime zi-ERA5, for both sites and for both years, which yields a better agreement between experimental and ERA5 data. These results and corrections are relevant for studies at ATTO and the T3 site and can likely also be applied at further locations in the Amazon.
54 ENVIRONMENTAL SCIENCES↗
Facile microwave synthesis of zirconium metal-organic framework thin films on gold and silicon and application to sensor functionalization
Zirconium-based metal-organic frameworks, including UiO-66 and related frameworks, have become the focus of considerable research in the area of chemical warfare agent (CWA) decontamination. However, little work has been reported exploring these metal-organic frameworks (MOFs) for CWA sensing applications. For many sensing approaches, the growth of high-quality thin films of the active material is required, and thin film growth methods must be compatible with complex device architectures. Several approaches to synthesize thin films of UiO-66 have been described but many of these existing methods are complex or time consuming. In this work, we describe the development of a simple and rapid microwave assisted synthesis of oriented UiO-66 thin films on unmodified silicon (Si) and gold (Au) substrates. Thin films of UiO-66 and UiO-66-NH 2 can be grown in as little as 2 min on gold substrates and 30 min on Si substrates. The film morphology and orientation are characterized and the effects of reaction time and temperature on thin film growth on Au are investigated. Both reaction time and temperature impact the overgrowth of protruding discrete crystallites in the thin film layer but, surprisingly, no strong correlation is observed between film thickness and reaction time or temperature. We also briefly describe the synthesis of Zr/Ce solid solution thin films of UiO-66 on Au and report the first synthesis of a solid solution thin film MOF. Finally, we demonstrate the utility of the microwave method for the facile functionalization of two sensor architectures, plasmonic nanohole arrays and microresonators, with UiO-66 thin films.
36 MATERIALS SCIENCE↗
3D Printed Chromophoric Sensors
Eight chromophoric indicators are incorporated into Sylgard 184 to develop sensors that are fabricated either by traditional methods such as casting or by more advanced manufacturing techniques such as 3D printing. The sensors exhibit specific color changes when exposed to acidic species, basic species, or elevated temperatures. Additionally, material properties are investigated to assess the chemical structure, Shore A Hardness, and thermal stability. Comparisons between the casted and 3D printed sensors show that the sensing devices fabricated with the advanced manufacturing technique are more efficient because the color changes are more easily detected.
3d printing↗
Molecular qubits based on photogenerated spin-correlated radical pairs for quantum sensing
Photogenerated spin-correlated radical pairs (SCRPs) in electron donor–bridge–acceptor (D–B–A) molecules can act as molecular qubits and inherently spin qubit pairs. SCRPs can take singlet and triplet spin states, comprising the quantum superposition state. Their synthetic accessibility and well-defined structures, together with their ability to be prepared in an initially pure, entangled spin state and optical addressability, make them one of the promising avenues for advancing quantum information science. Coherence between two spin states and spin selective electron transfer reactions form the foundation of using SCRPs as qubits for sensing. We can exploit the unique sensitivity of the spin dynamics of SCRPs to external magnetic fields for sensing applications including resolution-enhanced imaging, magnetometers, and magnetic switch. Molecular quantum sensors, if realized, can provide new technological developments beyond what is possible with classical counterparts. While the community of spin chemistry has actively investigated magnetic field effects on chemical reactions via SCRPs for several decades, we have not yet fully exploited the synthetic tunability of molecular systems to our advantage. This review offers an introduction to the photogenerated SCRPs-based molecular qubits for quantum sensing, aiming to lay the foundation for researchers new to the field and provide a basic reference for researchers active in the field. We focus on the basic principles necessary to construct molecular qubits based on SCRPs and the examples in quantum sensing explored to date from the perspective of the experimentalist.
Mani, Tomoyasu (ORCID:0000000241255195)↗