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At least 145 records · Page 8

Boride-based Ceramic Super-high Temperature Thermocouples in Harsh Environments (Final Scientific/Technical Report)

An electromotive force (emf) can be generated along a temperature gradient between the cold end and hot end of a thermoelectric material, termed the Seebeck effect. Based on the Seebeck effect, metallic alloys have been extensively employed to detect temperatures for centuries, named thermocouples. However, commercially available thermocouple alloys suffer from limitations, such as oxidation, chemical degradation, and poor long-term stability under high-temperature harsh environments. This DOE-funded project aimed to develop high-temperature, chemically tolerant thermocouples suitable for operation in extreme environments relevant to semiconducting thermoelectric materials. The research focused on boride-based semiconducting thermoelectric compounds as candidates for next-generation thermocouples with enhanced oxidation resistance, chemical stability, and thermal robustness under conditions representative of charcoal-fired electricity facilities. During the funded years, boride materials were synthesized using an arc-plasma technique under ambient air and argon atmospheres, enabling scalable and cost-effective production compared with conventional boride fabrication methods. The synthesized borides were processed into nanostructured powders, followed by consolidation into dense bulk materials using a spark plasma sintering (SPS) bottom-up approach. Comprehensive characterization was performed, including microstructural analysis, electrical transport measurements, and optical and thermal property evaluation. Both p-type and n-type boride electric legs were fabricated and integrated into boride-based thermocouples. The thermal and irradiation stabilities of the boride nanomaterials and bulk thermoelectric materials were systematically evaluated to assess suitability for long-term operation in harsh environments. Additionally, 12 students were broadly hands-on trained spanning the full research workflow, including word processing and technical editing (e.g., LATEX for manuscript and poster preparation), data collection and analysis (using Python and related libraries and hardware interfaces), sample preparation (including arc-plasma synthesis and spark plasma sintering), and advanced characterization techniques (such as X-ray diffraction, UV–vis spectroscopy, electron microscopy, differential thermal analysis (DTA), and Seebeck coefficient measurements, etc). Overall, this project demonstrated the feasibility of boride-based thermoelectric materials as durable high-temperature thermocouples, providing a promising pathway toward robust temperature sensing technologies aligned with DOE energy infrastructure and extreme-environment monitoring needs.

20 FOSSIL-FUELED POWER PLANTS↗

Rapid Prototyping for Nanoparticle-Based Photonic Crystal Fiber Sensors

The advent of nanotechnology has motivated a revolution in the development of miniaturized sensors. Such sensors can be used for radiation detection, temperature sensing, radio-frequency sensing, strain sensing, and more. At the nanoscale, integrating the materials of interest into sensing platforms can be a common issue. One promising platform is photonic crystal fibers, which can draw in optically sensitive nanoparticles or have its optical properties changed by specialized nanomaterials. However, testing these sensors at scale is limited by the the need for specialized equipment to integrate these photonic crystal fibers into optical fiber systems. Having a method to enable rapid prototyping of new nanoparticle-based sensors in photonic crystal fibers would open up the field to a wider range of laboratories that could not have initially studied these materials in such a way before. This manuscript discusses the improved processes for cleaving, drawing, and rapidly integrating nanoparticle-based photonic crystal fibers into optical system setups. The method proposed in this manuscript achieved the following innovations: cleaving at a quality needed for nanoparticle integration could be done more reliably (≈100% acceptable cleaving yield versus ≈50% conventionally), nanoparticles could be drawn at scale through photonic crystal fibers in a safe manner (a method to draw multiple photonic crystal fibers at scale versus one fiber at a time), and the new photonic crystal fiber mount was able to be finely adjusted when increasing the optical coupling before inserting it into an optical system (before, expensive fusion splicing was the only other method).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Surface Acoustic Wave H2 and O2 Sensors Based on Conducting Metal Oxides/Langasite for Elevated Temperature Applications - presentation

<p style="text-align: justify;"><span style="font-family: Arial; font-size: 10pt;">• </span><span style="color: black; font-family: Arial; font-size: 10pt;">SAW reflective delay line devices were designed and successfully fabricated on Langasite by patterning platinum electrodes.</span><p style="text-align: justify;"><span style="font-family: Arial; font-size: 10pt;">• </span><span style="color: black; font-family: Arial; font-size: 10pt;">Fabricated devices successfully tested up to 500°C for temperature sensing applications.</span><p style="text-align: justify;"><span style="font-family: Arial; font-size: 10pt;">• </span><span style="color: black; font-family: Arial; font-size: 10pt;">Indium oxide (IO) and indium tin oxide (ITO) sensing layers were developed on the SAW devices using sputtering and sol-gel method.</span><p style="text-align: justify;"><span style="font-family: Arial; font-size: 10pt;">• </span><span style="color: black; font-family: Arial; font-size: 10pt;">IO- and ITO-functionalized langasite SAW reflective delay line devices were used for sensing H2 and O2 at 350°C. </span><br>

Mao, Elizabeth↗

Characterization of Advanced Manufactured Surface Acoustic Wave Sensor for Temperature Measurement in Nuclear Applications

As part of a collaborative effort between Idaho National Laboratory and the Boise State University, printed SAW transducers were developed. The transducers were first modelled and evaluated for optimum performance, then fabricated using several piezoelectric substrates. These printed SAW-sensors were tested for temperature sensing ability and found to be highly sensitive and with a very linear response over the tested range.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Room-Temperature Quantitative Quantum Sensing of Lithium Ions with a Radical-Embedded Metal–Organic Framework

Recent advancements in quantum sensing have sparked transformative detection technologies with high sensitivity, precision, and spatial resolution. Owing to their atomic-level tunability, molecular qubits and ensembles thereof are promising candidates for sensing chemical analytes. Here, in this study, we show quantum sensing of lithium ions in solution at room temperature with an ensemble of organic radicals integrated in a microporous metal–organic framework (MOF). The organic radicals exhibit electron spin coherence and microwave addressability at room temperature, thus behaving as qubits. The high surface area of the MOF promotes accessibility of the guest analytes to the organic qubits, enabling unambiguous identification of lithium ions and quantitative measurement of their concentration through relaxometric and hyperfine spectroscopic methods based on electron paramagnetic resonance (EPR) spectroscopy. The sensing principle presented in this work is applicable to other metal ions with nonzero nuclear spin.

36 MATERIALS SCIENCE↗

Electrical, structural and thermomechanical properties of doped-LaCrO3 ceramics for high temperature electronics and sensing applications.

Many important electrical and sensor applications require stable conductors under working temperatures up to 1500oC various redox environments. Common high temperature conductors such as nitrides and carbides are not stable under oxidizing atmospheres, for this reason low redox behavior materials would be more attractive. In this work, further dopant studies of the LaCrO3 system were completed in order to control the electronic and ionic conductivity, as well as the relative chemical and microstructural stability. Neodymium and Niobium dopants were initially studied to control the p-type, and potentially n-type conductive mechanisms, respectively, but other dopants strategies were also investigated. The electrical conductivity and Seebeck coefficient were characterized up to 1500oC under varying oxygen partial pressures. The phase and microstructural evolution of each material was also investigated for these compositions by XRD and SEM. The materials showing the best electrical and thermomechanical performance were included within thick films sensors and were tested.

20 FOSSIL-FUELED POWER PLANTS↗

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↗

Wireless sensing and control of temperature using magnetic fields

A method and system for sensing and controlling temperature with magnetic fields are provided. The method comprises placing a compound in thermal communication with a number of temperature or heat sources and placing a number of magnets in thermal communication with the compound. A number of magnetic sensors are placed in electromagnetic communication with the number of magnets. Changes in the magnetic field of the magnets are detected by the sensors and used to determine the temperature of the compound according to a model that maps magnetic field characteristics to temperature. The amount of cure of the compound can then be estimated from the temperature. The temperature or heat sources are controlled in response to the temperature measurement and the estimated amount of cure of the compound.

Chen Mazumdar, Yi↗

Soil Carbonyl Sulfide (OCS) Fluxes in Terrestrial Ecosystems: An Empirical Model

Measurements of carbonyl sulfide (OCS) enable independent estimates of regional stomatal conductance provided that non-stomatal OCS fluxes are well constrained. OCS is taken up through plant leaves, following the same pathway as CO 2 ; in contrast to CO 2 , OCS is irreversibly destroyed in plant leaves and plants do not typically exhibit OCS emissions. Ecosystem uptake of OCS can indicate changes in stomatal opening. Here we present an empirical model to assess the potential impact of soil OCS exchange, the non-Stomatal OCS exchange Empirical Model (SOCSEM, version 0). We created biome-specific response curves characterizing soil OCS exchange and restricted the model design to require only knowledge of soil moisture and surface temperature because remote sensing observations are available for these two features. Comparing the model to field-based chamber observations reveal deviations that can be attributed to missing complexity of the ground surface (having excluded litter and plants without regulated stomata), shortwave radiation, or the soil environment. For agricultural regions with known net emissions, we use remotely-sensed surface temperature data and demonstrate that data resolution can affect anticipated fluxes. We further investigate the influence of regions with unknown soil OCS responses, for example, Arctic tundra. We compare our model to a process-based and respiration-based soil OCS exchange model that has been implemented in a land surface model. Further field study of tropical and arctic ecosystems in conjunction with studies of non-stomatal surfaces in addition to soil (e.g., bryophytes) will increase confidence in applying OCS as a regional tracer for stomatal conductance.

54 ENVIRONMENTAL SCIENCES↗

Integrated Monitoring Volume: A Summary of Monitoring Studies Conducted in Niagaran Carbonate Pinnacle Reefs During Enhanced Oil Recovery with CO 2

The Midwest Regional Carbon Sequestration Partnership (MRCSP) was founded in 2003 as part of the U.S. Department of Energy’s (DOE’s) Regional Carbon Sequestration Partnership initiative. Since its founding, MRCSP has made significant strides toward making CCUS a viable option for states in the region. The public/private consortium, funded through the DOE Regional Carbon Sequestration Initiative, brings together nearly 40 industry partners and 10 states. Battelle, as the project lead, oversees research, development and operations and coordinates activities among the partners. The incremental, phased approach has built a valuable knowledge base for the industry and paved the way for commercial-scale adoption of CCUS technologies. From 2008 to 2020, MRCSP Phase III focused on the development of large-scale injection projects. This report is part of a series of reports prepared under the Midwestern Regional Carbon Sequestration Partnership (MRCSP) Phase III (Development Phase). These reports summarize and detail the findings of the work conducted under the Phase III project. During the MRCSP Phase III monitoring period, over 1 million metric tons of CO 2 was injected into ten Silurian-age (Niagaran) pinnacle reef reservoirs in Otsego County, Michigan that are operated by Core Energy, LLC. There are over 800 pinnacle reefs in northern Michigan, and collectively, these geologic features have sufficient capacity to store several hundred million metric tons of CO 2 . Moreover, most of the reefs are oil-bearing and went through primary production in the 1970s and 1980s; therefore, by injecting CO 2 into the reefs, there is a real opportunity to realize additional (enhanced) oil recovery (EOR) and to permanently store CO 2 after EOR. A key objective of the MRCSP Phase III project is to evaluate the effectiveness of various technologies for monitoring CO 2 that has been injected into deep geologic formations. Monitoring may be required at CO 2 storage sites for a variety of reasons, including to meet UIC Class II (EOR sites) or Class VI (storage only sites) permit requirements or EPA greenhouse gas reporting rule requirements or to qualify for tax credits under the 45Q tax credit rule. The results of this monitoring study should prove useful to operators considering using carbonate pinnacle reefs of Northern Michigan for CO 2 storage.

01 COAL, LIGNITE, AND PEAT↗

High temperature thick film sensor development based on doped lanthanum chromites refractory semiconductors materials

High temperature advanced sensing materials have generated high demand due the high accuracy temperature measurements requirements for process optimization, controlling and sensing. Some technological applications of harsh conditions sensing include monitoring tiles of space shuttles, rotating bearings in aircraft engines, turbines, jet engines dynamics and chemical reactors. High temperature conditions limit the sensing strategies, where typically traditional metal thermocouples are unstable, and the sensing options are limited to optical spectroscopy methods. Recently, refractory semiconductors thick- and thin-film thermocouples have been developed and, in many cases, preferred over conventional metallic thermocouples due their spatial resolution, and capability of direct deposition on any surface. Rare earth chromites ceramics materials, exhibit some properties of interest for high temperature sensing technologies development, such as: high microstructure and sintering stability, excellent conductive behavior at high temperatures, and matching thermal expansion coefficients relative to other conductors and refractory ceramics. In this work, high performance ultra-high temperature thermocouples using p-type and n-type doped lanthanum chromites materials were fabricated and tested at temperatures up to 1500 o C. Thermoelectric voltage, Seebeck Coefficients were established for all devices, evidencing high stability and performance in prolongated operational time and harsh conditions.

20 FOSSIL-FUELED POWER PLANTS↗

High-temperature all-fiber non-destructive multi-parameter sensing system with consistent performance

A high-temperature all-fiber non-destructive multi-parameter sensing system is developed. The system can operate consistently in a wide range of temperature changes by specially designed active signal generation and detection units. It is capable of monitoring temperature up to 600°C and cracks on metal pipes with an acoustic wave generation unit and an acoustic detection unit. A gold-coated multi-mode fiber is used to deliver a laser pulse for acoustic excitation while minimizing parasitic acoustic signals at high temperature. An in-fiber Fabry–Perot fiber Bragg grating (FP-FBG) is fabricated in another single-mode fiber and bonded to the test object for acoustic detection. The FP-FBG avoids strain redistribution inside the bonder at high temperature to ensure consistent operation. The feasibility of the system for temperature monitoring and crack detection in real-world applications is also demonstrated on an industry-standard P91 pipe.

He, Jiaji (ORCID:0000000165661887)↗

CEM MARS 6 Microwave Incident

A fire occurred in a CEM MARS 6 analytical microwave during microwave-assisted, acid digestion of a soil sample in a Research and Development (R&D) laboratory. The soil sample had been pretreated at 550°C for approximately 4 hours in a furnace prior to digesting in the microwave. Less than 1-gram aliquots of the pretreated soil sample were placed into separate microwave reaction vessels along with an acid mixture used for digestion. The microwave was used to facilitate digestion of the samples. Microwave reaction vessels were loaded with acid and soil samples, sealed in cassettes, and the cassettes placed onto a microwave carousel. A temperature probe that senses the reaction temperature during the run was inserted into the Reference Cell thermowell. The contents of the Reference Cell were identical to the contents of the other reaction cells. The researcher initiated the run and then left the laboratory to perform other work. Upon returning to check the digestion run, flames and smoke were observed originating from the microwave. The researcher exited the lab, immediate emergency actions were taken, and the local fire department responded and extinguished the fire. No personnel were injured, and no facility structural damage occurred. The affected microwave is a total loss. The fire investigation revealed the most credible cause of the fire is an incompatible temperature probe that did not accurately measure temperature of the liquid phase of the Reference sample.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Projecting spatiotemporally explicit effects of climate change on stream temperature: A model comparison and implications for coldwater fishes

Conservation planners and resource managers seek information about how the availability and locations of cold-water habitats will change in the future and how these predictions vary among models. In this work, we used a physical process-based model to demonstrate the implications of climate change for streamflow and water temperature in two watersheds with distinctive flow regimes: the Snoqualmie watershed (WA) and Siletz watershed (OR), USA. Our model incorporated a downscaled ensemble of global climate model outputs and was calibrated with in situ and remotely sensed water temperatures. Furthermore, we compared predictions from our processed-based model to those from a publicly available and widely used statistical model. The process-based model projected greater changes in summer maximum water temperatures for the mixed-rain-snow Snoqualmie watershed than for the rain-dominated Siletz watershed as a result of the near-complete loss of winter snowpack and significant reduction in summer flow in the Snoqualmie watershed expected by the 2080s. Both models projected generally similar future spatial patterns of maximum water temperature in the two rivers, with cool reaches distributed farther upstream and fewer in number. However, the process-based model projected higher spatial heterogeneity in water temperature due to our spatially explicit simulation of streamflow and because we calibrated the model with spatially continuous remotely sensed water temperature data. We used stream temperature projections to assess the vulnerability of Pacific salmon and trout to changes in the spatial distribution of cold-water habitats during August by the 2080s. Results suggest that salmonids may have fewer summertime cold-water habitats in both watersheds. Projected stream warming may further limit particular species and life stages, especially in the Snoqualmie watershed. Our comparison of models highlights the importance of considering what might be gained by using a process-based model for evaluating and prioritizing management actions that mitigate climate impacts on cold-water habitats for stream fishes.

54 ENVIRONMENTAL SCIENCES↗

Distributed fiber sensing systems for 3D combustion temperature field monitoring in coal-fired boilers using optically generated acoustic waves (Final Report)

In this project, we have developed and tested three kinds of fiber optic sensing systems for real time monitoring of temperature variations within an industrial scale boiler furnace. The fiber optic sensing systems target spatial and temporal distributions of high temperature profiles in a boiler furnace in fossil power plants. The reconstructed temperature profile will provide critical input for the control mechanisms to optimize the combustion process. This temperature profile will address the essential problem for fossil power plants in achieving higher efficiency and fewer pollutant emissions. Acoustic pyrometer systems have been used to reconstruct temperature field of power plant boilers based on measuring TOF (times-of-flight) of sound waves along some straight paths in a 2D cross-section of the boiler. In this project, optically generated acoustic signals from a fiber optic sensing system have replaced the acoustic signals generated from an electrical transducer. A 3D reconstruction algorithm replaced the previous 2D model. In this project, three kinds of fiber optic sensing systems have been developed and tested. They are fiber optic sensing system I, fiber optic sensing system II (Distributed Sensing System I) and fiber optic sensing system III (Distributed Sensing System II). For fiber optic sensing system I, the fiber optic ultrasound generator acts as a signal generator. A microphone, hydrophone or other electronic devices serve as a signal receiver. In this system, there are one generator and one receiver. Distance test, water temperature test, air temperature test, air temperature reconstruction, and GE ISBF pilot test were performed by Fiber optic sensing system I. The fiber optic sensing system I successfully detected temperature in all these tests. We got 2D temperature reconstruction results by using the fiber optic sensing system I and it matched the reference data. The fiber optic sensing system I successfully survived in GE ISBF boiler environment (480 °F). For fiber optic sensing system II (Distributed Sensing System I), it is an all optical ultrasound system. The fiber optic ultrasound generator acts as a signal generator. Fiber Bragg Grating (FBG) and Fabry-Perot (FP) sensor act as a signal receiver. In this system, there is one generator and one receiver. Aluminum plate temperature test, furnace high temperature test, and GE ISBF pilot test were performed by the fiber optic sensing system II. Fiber optic sensing system II successfully detected the temperature in all these tests. The fiber optic sensing system II successfully survived at up to 700 °C furnace environment and 320 °C GE ISBF boiler environment. For fiber optic sensing system III (Distributed Sensing System II), it is also an all optical ultrasound system. The fiber optic ultrasound generator acts as a signal generator. Multiple FP fiber sensors act as signal receivers. In this system, there is one generator and three receivers. Three GE ISBF pilot tests were performed by fiber optic sensing system III. The fiber optic sensing system III survived in the cold flow tests in GE’s ISBF pilot test facility. However, we didn’t get high temperature data by using this system since the nanosecond laser issues. During the period of the project, test trials, data simulation and algorithm optimization was performed successfully. For real time temperature field construction, the sampling rate must be fast enough to capture the field variations. The technology of Code-division multiple access (CDMA) is well studied which could allow parallel multiplexing, even if signals overlap in time or frequencies. Moreover, it has been known that extending the length of signal significantly improves SNR. For acoustic signals, these multiplexing techniques have also been widely used, mainly for sonar and acoustic communications. The CDMA modulation technique has been proposed and studied to guarantee high network throughput, low channel access delay and low energy consumption. We have studied the temperature field reconstruction using Gaussian Radial Basis Functions (GRBF)-based approximation approach. Reconstruction of 3D temperature field using Neural Networks with measured TOF and known propagation paths is feasible. 2D and 3D temperature field reconstruction simulation results are achieved. The milestone status is shown in Table 1. We finished milestone 1-8 and milestone 10. For milestone 9, we did three pilot tests by using the fiber optic sensing system III (Distributed Sensing System II) at GE Power. However, due to the failure of the ns laser, we did not get the temperature results. We conducted some additional tasks that were not originally proposed: 1) We fabricated a fiber optic sensing system I and did a pilot test based on this system. 2) In the proposal, we proposed two pilot tests at GE Power. In reality, we finished at least seven pilot tests at GE Power. GE Power has made a lot of efforts for supporting the pilot tests. 3) We got a simulation results based on CDMA. In summary, most of the tasks have been accomplished. The outcome of this project removed a few barriers that hinder the achievement of the final product of the distributed sensing systems. With the successful accomplishment of this project, a prototype of the fiber optic sensing system can be fabricated to attract more interests from companies and other funding agencies.

47 OTHER INSTRUMENTATION↗