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Provided are batteries and fuel cells incorporating a stripline detector for use in nuclear magnetic resonance (NMR). The stripline batteries and fuel cells can be used for in situ NMR measurement of battery or fuel cell chemistry. Also provided are methods for measuring in situ battery and fuel cell NMR using the stripline batteries and fuel cells of the invention.
Provided are batteries and fuel cells incorporating a stripline detector for use in nuclear magnetic resonance (NMR). The stripline batteries and fuel cells can be used for in situ NMR measurement of battery or fuel cell chemistry. Also provided are methods for measuring in situ battery and fuel cell NMR using the stripline batteries and fuel cells of the invention.
Fringe Projection Profilometry (FPP) is a cost-effective and non-invasive technology that has been shown to measure finer features. Here, in this work, we developed an in-situ FPP method to measure the dynamic topography of powder bed and printed layer during Laser Powder Bed Fusion (LPBF) additive manufacturing (AM) process. A systematic study towards developing a comprehensive framework of LPBF-specific FPP is demonstrated to enhance and evaluate the performance of applying FPP for in-situ LPBF monitoring, including 1) a modified sensor model with localized correction; 2) improved phase unwrapping with FFT filtering 3) quantitative uncertainty analysis; and 4) experimental validation with ex-situ characterization. The developed LPBF-specific FPP system and methods are implemented on a commercial LPBF-AM machine, achieving better accuracy, more robustness, and increased field of view while maintaining sufficient measurement range and decent resolution, in contrast to literature methods. The established FPP framework will facilitate the development of closed-loop control strategies for advancing LPBF based AM.
Student poster for HEART 2025. Abstract: Experimental data from multiple methods of measurement as compared to simulation and model data show that free-field antenna characterization methods can be appropriately applied to short, surface mount monopole antennas used in small cavities for shielding effectiveness testing.
Recently, a method to infer the polarization of modes with frequencies much less than the ion cyclotron frequency was published [X.D. Du et al., Phys. Rev. Lett. 132 (2024) 215101]. The method uses measurements of electron temperature and density fluctuations δTₑ and δnₑ at the same spatial position to infer the local ratio of “acoustic polarization,” |δϕ ∥ |/(|δϕ ∥ |+|δψ|), where δϕ ∥ is the effective parallel potential and δψ is related to the parallel magnetic vector potential A ∥ . This paper summarizes key formulas, with emphasis on their range of validity, and elaborates on the workflow required to infer the acoustic polarization from experimental data. The drift-acoustic polarization of ellipticity-induced, toroidicity-induced, and reversed shear Alfvén eigenmodes is nearly zero, as expected for modes with predominately shear-Alfvénic polarization. The polarization of beta-induced Alfvén eigenmodes contains an acoustic component that increases with poloidal wave number. “Low frequency modes,” (instabilities that appear transiently when the minimum of the safety factor qₘᵢₙ passes through rational values) have large and highly variable acoustic polarization. In both experiment and simulation, fishbones have non-zero acoustic polarization that increases as the mode chirps down in frequency.
Diamagnetic loops (DML) are used as a non-invasive method for measurements of beam size in electron beam accelerators that use solenoidal magnetic transport. The loop fundamentally measures the magnetic flux excluded by a diamagnetic object. One of the sources of background in these measurements is the flux produced by a straight filamentary current that is offset from the axis and tilted in the plane orthogonal to the offset. This was only a small effect in our experiments, because the beam was steered to be centered on average at the DML. However, we devoted some time to understanding and quantifying the effect, and we recount that effort in this report.
Here we present a method for measurement of the rate of solvent absorption by perfluorosulfonic acid (PFSA) membranes using a force tensiometer. The method presented here can be used as a tool to understand solvent absorption and should provide a rationale for designing catalyst inks for direct coating processes since it is necessary to understand how the absorption rate – on a time scale of seconds to minutes – compares to the time scales of the coating process in order to minimize membrane swelling. This method allows for rapid screening of the absorption and swelling behavior of different solvents and mixtures. Using this method, the absorption of water/1-propanol mixtures were measured for three thicknesses of Nafion PFSA membrane – Nafion 1135, Nafion 115, and Nafion 117. We find that the absorption rate is dependent on the ratio of the solvents as well as the thickness of the membrane. The analysis indicates that the highest absorption rate occurs when the mass percentage of 1-propanol in the mixture is 50%, whereas the lowest rates are for pure water and 1-propanol. In addition, membrane distortion also occurs most quickly for the 50% 1-propanol mixture. Our results suggest that catalyst inks that are highly rich (=90%) in water or 1-propanol are likely best for direct coating as such formulations will minimize absorption and swelling.
In this work, we report a method for measuring spot size and focusing conditions of the femtosecond (fs) excitation laser in situ at the specimen location in 4D ultrafast electron microscopy (UEM). The method makes use of threshold laser ablation behaviors of thin amorphous carbon membranes. For Gaussian beam profiles and for ablation threshold fluence values, we analytically derive expressions describing the relationship between ablated hole size and the actual laser spot size. Using these expressions, we developed experimental procedures for characterizing the shape and spot size of the pump beam at the specimen. We demonstrate the viability of the approach for incident excitation wavelengths of 343 nm and 515 nm, thus illustrating the applicability of the method to a range of optical wavelengths without modification. Further, we show that by measuring ablated hole size as a function of focusing condition, a full metrological characterization of the Gaussian beam propagation properties can be performed. Finally, we find good agreement for spot sizes determined with this method and with those determined by extrapolation from measurements taken outside the microscope column. Overall, this method is a simple, cost-effective means for accurate and precise determination of key pump-beam parameters in situ at the specimen location in UEM experiments.
Radiofrequency quadrupole (RFQ) linear accelerators with variable aperture cell parameters offer an effective means of accelerating high-intensity ion beams exceeding 100 mA and have been implemented in various RFQ designs. However, in a four-rod RFQ, the use of dielectric perturbation methods to measure the voltage distribution behind the rod electrodes is not applicable when implementing variable aperture geometries, because changes in the rod shape influence the electric field at the location of the perturbation element. Therefore, it was necessary to design the rod profile for each cell such that the electric field distribution behind the rods remains unaffected by changes in the aperture. In this study, we present a method to adjust the voltage distribution by modifying the geometry of the rod electrodes according to each cell's aperture parameters. This design approach enables the integration of variable aperture cells into a four-rod RFQ linac, significantly enhancing the achievable beam current. To ensure uniform capacitance and maintain a constant rod-electrode voltage despite variations in the average aperture radius, we developed a systematic method for shaping the rod electrodes. This method was refined using two-dimensional (2D) and three-dimensional (3D) electromagnetic field simulations to optimize the electrode cross-sectional profiles. The fabricated rod electrodes were then installed in a four-rod RFQ, and the electric field distribution was measured using the perturbation method and tuned by adjusting the base plates. As a result, the measured variation of ±1.1 % confirms that this design methodology can produce a sufficiently uniform voltage distribution for high-current beam acceleration. These results demonstrate the practical feasibility of a variable-aperture four-rod RFQ linac.
Knowledge of the crustal thickness history of southern Tibet during the India-Asia collision is key to understanding what deformation mechanisms accommodated northward propagating crustal shortening. Thermoisotopic models suggest that a relatively thin margin of southern Asia persisted from ca. 200 to 45 Ma whereas trace element paleodepth proxies are interpreted to indicate a thinning phase from ca. 100 to 65 Ma when the crust reached ∼30 km-thickness. As neither of these methods directly measures crustal thickness, resolution of this conflict awaits development of a method that can. Here, in this study, we place bounds on the thickening history of southern Tibet using coupled quartz-zircon thermobarometry and U-Pb geochronology of granitoid plutons in the Gangdese batholith. We find that crustal thicknesses were as high (or higher) as 60–75 km at 65 Ma, or 10–15 Ma prior to the onset of hard continental collision. Magmatic inflation in the lower crust likely contributed to crustal thickening and thermal weakening of the lower crust, suggesting that pure shear in the lower crust was likely the primary accommodation mechanism for N-S shortening during collision. These data are in partial agreement with results of thermoisotopic models of crustal thickness but contradict thickness histories derived from empirical trace element proxies.
Abstract To realize the full promise of high-throughput experimental workflows, the rate of sample synthesis must be matched by that of characterization. Of growing interest are contactless optical techniques that can rapidly measure material homogeneity and properties. Here, we present a hyperspectral imaging method to measure local optical bandgap distributions within samples, utilizing spatially-resolved reflectance spectra coupled with automated data analysis. We collect approximately one million optical bandgap data across the compositional space of Cs 3 (Bi x Sb 1-x ) 2 (Br y I 1-y ) 9 perovskite-inspired materials. Our results show non-monotonic bandgap variations (i.e., bandgap bowing) along six composition gradient sequences, in addition to identifying samples with multiple bandgaps in statistics. High-throughput transient absorption spectroscopy reveals that within these compositions, the depletion of the ground state carriers to excited states occurred at discrete energy levels with independent carrier dynamics, consistent with the bandgap observation and indicative of phase separation. This work demonstrates the potential for rapid optical measurements to assess material quality and homogeneity in a high-throughput experimental setting, supporting screening and recipe optimization of optoelectronic material candidates with desired carrier dynamics and optical properties.
Model improvement efforts involve an evaluation of changes in model skill in response to changes in model physics and parameterization. When using wind measurements from various remote sensors to determine model forecast accuracy, it is important to understand the effects of measurement-uncertainty differences among the sensors resulting from differences in the methods of measurement, the vertical and temporal resolution of the measurements, and the spatial variability of these differences. Here we quantify instrument measurement variability in 80-m wind speed during WFIP2 and its impact on the calculated errors and the change in error from one model version to another. Here the model versions tested involved updates in model physics from HRRRv1 to HRRRv4, and reductions in grid interval from 3 km to 750 m. Model errors were found to be 2–3 m s –1 . Differences in errors as determined by various instruments at each site amounted to about 10% of this value, or 0.2–0.3 m s –1 . Changes in model skill due to physics or grid-resolution updates also differed depending on the instrument used to determine the errors; most of the instrument-to-instrument differences were ~0.1 m s –1 , but some reached 0.3 m s –1 . All instruments at a given site mostly showed consistency in the sign of the change in error. In two examples, though, the sign changed, illustrating a consequence of differences in measurements: errors determined using one instrument may show improvement in model skill, whereas errors determined using another instrument may indicate degradation. This possibility underscores the importance of having accurate measurements to determine the model error.
This report documents the interim experimental status of small-scale drying tests currently being performed at Pacific Northwest National Laboratory. These small-scale drying tests are to develop the technical bases for sensors, techniques, and approaches that will be used to address the challenges faced when determining moisture content from gas samples taken at the North Anna Nuclear Generating Station for the High Burnup Demonstration Project. Specifically, the purpose of these tests is to support Sandia National Laboratories gas sample methods and analyses through a series of small-scale experiments. Key focus areas include performing tests to: • Correlate sample bottle measurements to in-cask conditions • Estimate the amount of trapped and absorbed water on cask features and surfaces that can contribute to water vapor • Assess the accuracy of the hygrometer used in the measurements under similar conditions • Identify additional methods for measuring humidity in casks easily and accurately using lessons-learned from Sandia National Laboratories, including direct gravimetric and isotopic tracer techniques. To address these topics this report outlines a series of five tests and any data collected to date that were planned for FY 2020 that include 1) humidity measurement method development, 2) gas bottle sampling tests, 3) surface drying tests on cladding, 4) small-scale drying of cladding, and 5) small-scale drying of guide-tube/dashpots. This interim report documents the experimental background, design and progress of these small-scale drying tests. Further data gathered will be summarized in the FY 2021 report.
Hydrogels are soft, water-absorbing polymer materials with diverse applications in biomedicine and agriculture. Recently, hydrogels have been proposed to encapsulate water-soluble phase change materials which store energy in their latent heat of solidification. In these applications, the thermal conductivity of these materials affects their performance. Few methods exist for measuring the thermal conductivity of small quantities of hydrogels. Here, we describe an implementation of the bidirectional 3w technique to measure the thermal conductivity of hydrogels with particular attention to their moisture content. Our implementation of the technique can probe sample volumes as little as ~20 mL and yields the thermal conductivity without requiring fitting of additional thermal parameters. We numerically simulate 3w sensor designs with frequency-domain 3-D models to quantify and reduce errors introduced by the choice of substrate and insulation layer thickness. Frequencies in the ~1−20 Hz range yield less error for the materials considered here. We verify our setup with measurements on water and report values for polyacrylamide and poly(2-acrylamido-2-methylpropane sulfonic acid) (PAMPS) hydrogels. Our swollen hydrogels exhibited thermal conductivities nearly equivalent to water, 0.6 W m-1 K-1, and we estimate thermal conductivities of 0.43 and 0.42 W m-1 K-1 for neat polyacrylamide and PAMPS, respectively. Finally, we estimate an error of ±7%, consistent with other 3ω methods, with the largest error coming from the sensor calibration. We find our implementation of the bidirectional 3w method gives reasonable results and can be employed for prototyping soft materials relevant for thermal storage.
The Netzsch LFA 447 Nanoflash Instrument uses the laser flash method to measure thermal diffusivity of a material. Thermal conductivity can be determined if specific heat and density are known for that material. The 238 Pu Supply Program is interested in re-establishing the capability to determine thermal diffusivity and thermal conductivity of various 237Np Al/cermet samples during heating. The bottom side of a plane parallel sample is heated by an energy pulse from a light source (in this case a xenon lamp). An infrared (IR) detector is on the top side of the sample which detects the time dependent temperature rise of the sample due to the energy input from the xenon lamp. The LFA 447 Nanoflash is user-friendly, simple to operate, and has minor sample preparation which will allow technicians to be trained easily on its use. When using the multi-property measurement option, the LFA 447 Nanoflash can determine both thermal diffusivity and specific heat which means only density is needed to identify the thermal conductivity of a sample. This equipment is recognized for being highly accurate and having fast test times, replacing steady-state methods which have proven to be difficult and much slower.
Most crystalline materials present a highly heterogeneous response at the microscale, which can be affected by both internal factors (such as microstructural parameters) and external factors (such as loading). Relating microscale inhomogeneities to the macroscale response of a material requires the use of homogenisation techniques, usually based on the concept of a representative volume element (RVE)—the smallest volume of material that represents the global average response. Here, in this work, we present a new and robust experimental method of measuring the size of a strain-based RVE from high-resolution grain-scale strain fields obtained using digital image correlation (DIC). The proposed method is based on the statistical (stereological) nature of the RVE, which has been widely adopted in numerical studies, and involves dividing a strain field into randomly selected regions of varying sizes and statistically analysing the distributions of average strains within them. To validate the new method, we generate a large number of synthetic strain fields from a fractional Gaussian noise algorithm. The proposed stereological method is shown to be capable of producing reliable RVE measurements from a very large range of possible microscale strain fields while at the same time being robust in that it can produce RVE measurement results even in cases where other existing methods may be unable to do so. The proposed method has a low field-of-view requirement, only needing a field-of-view about 1.2 times as large as the RVE to produce reliable measurements. In addition, the stereological method offers significant flexibility since its statistical nature allows for control over how strict the RVE measurement should be in each case.
Osmometry is the analytical method of measuring osmotic pressure ($π$) and related colligative properties. Accurately measuring $π$ is essential for applications that use osmosis, including drug delivery systems and water filtration methods such as forward osmosis. The three most common forms of directly or indirectly measuring $π$ are vapour pressure osmometry (VPO), freezing point osmometry (FPO), and direct membrane osmometry (DMO). In this report, the performance of VPO, FPO, and DMO are compared for various aqueous solutions, including small molecule and polymer solutes, and potentially more difficult samples such as concentrated, carbonated, or viscous solutions. Furthermore, potential problems with each of the three methods are examined. Good practices can avoid inaccuracies in DMO due to external concentration polarization and solute diffusion through the membrane. Similarly, it is important to be aware of and avoid weaknesses in VPO and FPO in order to obtain reliable results. Even with care, however, the three methods still give different values of $π$ for concentrated aqueous solutions.
Quick, reliable methods to measure the rare earth elements (REEs) in process streams are needed to support real-time parameterization and monitoring for a burgeoning number of REE extraction schemes. Such methods would ideally be fast, reproducible, and field-deployable. This study evaluates the feasibility of using a chromogenic indicator, arsenazo(III) (hereafter abbreviated as Arsz(III)) to detect the concentration of REEs in complex citrate leaching solutions using a spectrophotometer. Arsz(III) forms a chromogenic complex with the lanthanide elements that produces a blue/purple color detectable in the visible light range. Matrices of solutions containing varied concentrations of calcium, iron, and lanthanum were scanned in the presence of an Arsz(III) indicator to generate a modeled relationship that could be used to back calculate REE concentrations. While relatively quick (scan times on the order of seconds), the results indicated that the calcium and iron concentrations of typical mining solutions overwhelm the signal of the REEs, to the extent that sensitivity of the method is no less than 50 µM REEs. These results demonstrate the difficulties of accurately measuring trace metals in complex solutions, although the method may still hold utility for processes with significantly lower calcium and iron concentrations or REE concentrations much greater than 50 µM.