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DOE OSTI2022

Salt Sampling FY21 Technical Report

The goal of the salt sampling program at Argonne is to develop and deploy automated molten salt sampling approaches to enable high-precision in-process salt sample analysis to improve the timeliness of sampling-based accountancy measurements. Tools currently under development in support of this goal include (1) a modular vacuum sampler with an accompanying sample handling method for coupling vacuum sampling with high-precision at-line sample analysis, (2) a pneumatic sample generator that enables high-throughput sample analysis to improve the precision of existing analytical techniques, and (3) a windowless flow cell to enable on-line optical analysis of molten salt in a sampling loop. Compared to point sampling approaches (i.e., dip probes), vacuum sampling systems and on-line sampling loops facilitate access to a larger cross-section of a process fluid. This is known to improve the characterization of the process fluid by producing more representative samples and by enabling the analysis of a larger cross section of the fluid. A vacuum sampling approach for molten salts eliminates the risk of dross contamination of samples and avoids the use of moving parts in the salt. In FY21, two methods for integrating a vacuum sampler with a pneumatic sample generator were tested. These included direct fluidic coupling and coupling using a solid salt transfer mechanism. Solid salt transfer was ultimately selected over fluidic coupling, primarily to enable the transport of samples over longer distances to support automated at-line integration with high-precision techniques (such as microcalorimetry) that cannot withstand the extreme conditions near an electrorefining process. To facilitate rapid solid salt coupling, new mechanisms were developed for rapidly charging and discharging salt sample tubes at the vacuum sampler and pneumatic sample generator, respectively. While the charging mechanism will be deployed in FY22, the tube transfer method and discharge mechanism were tested in FY21. These were deployed at one of Argonne’s engineering-scale electrorefiners to implement at-line high-throughput pneumatic micro-sample generation capabilities. The method was used to generate precise uranium- and lanthanide-bearing electrorefiner micro-samples with the specific dimensions requested by researchers at Los Alamos National Laboratory for use in testing their novel microcalorimeter x-ray techniques. The solid salt transfer mechanism proved not only to be an effective means of integrating the precision sample generator with vacuum sampling, but also improved the performance of the sampler generator. Because the modular sampling approach described here eliminates the need for new high-radiation sample handling capabilities, salt-wetted seals, salt-wetted moving parts, and heated transfer lines outside the electrorefiner, it will address most of the remaining technical challenges for the at-line deployment of high-precision analytical techniques. This will enable significant reductions in the time delay for sampling-based accountancy measurements by eliminating the need for manual off-line sample processing and analysis. On-line optical analysis of molten salt in a sampling loop would provide complementary information to at-line and in-situ techniques. In FY21, an open-aperture molten salt gravity flow cell with windowless optical access to flowing salt was successfully demonstrated. Future work should include the refinement and performance testing of the on-line and at-line sampling tools, integration of additional analysis techniques, stakeholder outreach and collaboration, evaluation of the integrated methods, and analyses to determine how the various tools might fit into an integrated safeguards monitoring system of unattended near real time monitoring tools.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

Deployment of salt sample extraction system at an engineering-scale electrorefiner

The goal of the salt sampling program at Argonne is to develop and deploy automated molten salt sampling approaches for interfacing relevant unit operations with salt analysis to improve the timeliness of sampling-based accountancy measurements. Two technologies under development in support of this goal are a vacuum sampling loop module and a high-throughput pneumatic sample generator module. Compared to traditional point sampling approaches (i.e., dip probes), the vacuum sampling loop facilitates the collection of a larger cross-section of the bulk salt in order to collect more representative samples. The vacuum sampling approach also eliminates the risk of dross contamination of samples and avoids the use of moving parts in the salt. The pneumatic sample generator module is used to facilitate high-throughput sample analysis to improve the measurement precision of any given analytical technique by averaging out random sampling and measurement errors. In FY21, two methods for integrating these two modules were tested including direct fluidic coupling and coupling using a solid salt transfer mechanism. Solid salt transfer was ultimately selected over fluidic coupling, primarily to enable the transport of samples over longer distances to support automated at-line integration with high-precision techniques (such as microcalorimetry) that cannot withstand the conditions near an electrorefining process. To facilitate rapid solid salt coupling, new mechanisms were developed for rapidly charging and discharging salt sample tubes at the vacuum sampling loop and pneumatic sample generator modules, respectively. While the charging mechanism will be deployed in FY22, the discharge mechanism was tested in FY21 and is described here. The solid salt tube transfer method was deployed at one of Argonne’s engineering-scale electrorefiners to implement at-line high-throughput pneumatic micro-sample generation capabilities. The approach was used to generate precise uranium- and lanthanide-bearing electrorefiner micro-samples with the specific dimensions requested by researchers at Los Alamos National Laboratory for use in testing their novel microcalorimeter x-ray techniques. The solid salt transfer mechanism proved not only to be an effective means of integrating the precision sample generator with vacuum sampling, but also improved the performance of the sampler generator. To discharge salt from the sample tubes at the sampler generator, tube segments were inserted directly into the sample generator’s Helmholtz chamber and pressure pulse actuations were used to generate precision molten salt samples directly from the tube segments. The direct insertion of sample tubes into the sample generator enabled rapid loading of the salt and prevented salt from contacting most of the interior surfaces of the sample generator, which eliminated cross-contamination between runs. The vacuum sampling-loop tube charging mechanism will support high-throughput tube sampling operations by employing a dynamic vacuum filling process to fill short charge tubes that are configured to be rapidly connected and disconnected from the loop. The dynamic vacuum sampling operation will be automated, and sample tube handling can be executed with simple overhead actuation. Because the modular sampling approach described here eliminates the need for new high-radiation sample handling capabilities, salt-wetted seals, salt-wetted moving parts, and heated transfer lines outside the electrorefiner, it will address most of the remaining technical challenges for the at-line deployment of high-precision analytical techniques which will enable significant reductions in the time delay for sampling-based high-precision accountancy measurements.

42 ENGINEERING↗

DOE OSTI2024

Nanoscale Three-Dimensional Imaging of Integrated Circuits Using a Scanning Electron Microscope and Transition-Edge Sensor Spectrometer

X-ray nanotomography is a powerful tool for the characterization of nanoscale materials and structures, but it is difficult to implement due to the competing requirements of X-ray flux and spot size. Due to this constraint, state-of-the-art nanotomography is predominantly performed at large synchrotron facilities. We present a laboratory-scale nanotomography instrument that achieves nanoscale spatial resolution while addressing the limitations of conventional tomography tools. The instrument combines the electron beam of a scanning electron microscope (SEM) with the precise, broadband X-ray detection of a superconducting transition-edge sensor (TES) microcalorimeter. The electron beam generates a highly focused X-ray spot on a metal target held micrometers away from the sample of interest, while the TES spectrometer isolates target photons with a high signal-to-noise ratio. This combination of a focused X-ray spot, energy-resolved X-ray detection, and unique system geometry enables nanoscale, element-specific X-ray imaging in a compact footprint. The proof of concept for this approach to X-ray nanotomography is demonstrated by imaging 160 nm features in three dimensions in six layers of a Cu-SiO 2 integrated circuit, and a path toward finer resolution and enhanced imaging capabilities is discussed.

47 OTHER INSTRUMENTATION↗

DOE OSTI2026

High-spectral-resolution X-Ray Observations of the Evolved Supermassive Stellar Binary System η Carinae: Fe K α Band Profile Revealed with XRISM

The supermassive binary system, η Carinae, is experiencing enormous wind-driven mass loss at a rate unparalleled in the rest of the Galaxy. Their wind–wind collision (WWC) continuously produces shock heated, X-ray-emitting plasmas. The XRISM X-ray observatory observed the system in 2023 and 2024 when the X-ray emission began to increase toward periastron passage in 2025. This paper reports unprecedentedly high-resolution X-ray spectra in the Fe Kα band between 6.2 and 7.1 keV, obtained with the Resolve X-ray microcalorimeter. The hydrogen-like (Lyα) and helium-like (Heα) lines reveal three velocity components. Two of them are broadened with maximum velocities of 2000–3000 km s −1 , likely originating from the postshock companion wind. The other is relatively narrow, with a Gaussian broadening of only ∼290 km s −1 in 1σ, which may originate from the postshock companion wind at the WWC stagnation point or penetrating the primary wind. The Fe fluorescent lines exhibit a moderate blueshift and broadening with velocities at 100–200 km s −1 , consistent with the primary wind’s velocity field. The spectra also confirm a Compton shoulder of the Heα line complex for the first time. Both fluorescing and scattering spectral profiles indicate that the binary system is seen from the companion side during these observations. The flux ratio of the Compton-scattering emission to the fluorescent line suggests substantial hydrogen depletion of the primary wind, expected from CNO-cycled hydrogen nuclear fusion gas.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2024

Detection of the Orbital Modulation of Fe Kα Fluorescence Emission in Centaurus X-3 Using the High-resolution Spectrometer Resolve on board XRISM

Abstract The Fe K α fluorescence line emission in X-ray spectra is a powerful diagnostic tool for various astrophysical objects to reveal the distribution of cold matter around photoionizing sources. The advent of the X-ray microcalorimeter on board the XRISM satellite will bring new constraints on the emission line. We present one of the first such results for the high-mass X-ray binary Centaurus X-3, which is composed of an O-type star and a neutron star (NS). We conducted a 155 ks observation covering an entire binary orbit. A weak Fe K α line was detected in all orbital phases at an equivalent width (EW) of 10–20 eV. We found for the first time that its radial velocity (RV) is sinusoidally modulated by the orbital phase. The RV amplitude is 248 ± 13 km s −1 , which is significantly smaller than the value (391 km s −1 ) expected if the emission is from the NS surface, but is consistent if the emission takes place at the O star surface. We discuss several possibilities of the line production site, including the NS surface, O star surface, O star wind, and accretion stream from the O star to the NS. We ran radiative transfer calculation for some of them assuming spherically symmetric density and velocity profiles and an isotropic distribution of X-ray emission from the NS. None of them explains the observed EW and velocity dispersion dependence on the orbital phase, suggesting that more elaborated modeling is needed. In other words, the present observational results have the capability to constrain deviations from these assumptions.

High energy astrophysics↗

DOE OSTI2025

XRISM Forecast for the Coma Cluster: Stormy, with a Steep Power Spectrum

The XRISM Resolve microcalorimeter array measured the velocities of hot intracluster gas at two positions in the Coma galaxy cluster: ${3}^{{\prime} }\times {3}^{{\prime} }$ squares at the center and at 6$^{\prime} $ (170 kpc) to the south. We find the line-of-sight velocity dispersions in those regions to be σ z = 208 ± 12 km s −1 and 202 ± 24 km s −1 , respectively. The central value corresponds to a 3D Mach number of M = 0.24 ± 0.015 and a ratio of the kinetic pressure of small-scale motions to thermal pressure in the intracluster plasma of only 3.1% ± 0.4%, at the lower end of predictions from cosmological simulations for merging clusters like Coma, and similar to that observed in the cool core of the relaxed cluster A2029. Meanwhile, the gas in both regions exhibits high line-of-sight velocity differences from the mean velocity of the cluster galaxies, Δv z = 450 ± 15 km s −1 and 730 ± 30 km s −1 , respectively. A small contribution from an additional gas velocity component, consistent with the cluster optical mean, is detected along a sight line near the cluster center. The combination of the observed velocity dispersions and bulk velocities is not described by a Kolmogorov velocity power spectrum of steady-state turbulence; instead, the data imply a much steeper effective slope (i.e., relatively more power at larger linear scales). This may indicate either a very large dissipation scale, resulting in the suppression of small-scale motions, or a transient dynamic state of the cluster, where large-scale gas flows generated by an ongoing merger have not yet cascaded down to small scales.

coma cluster↗

DOE OSTI2025

Kinematic Evidence for Bipolar Ejecta Flows in the Galactic Supernova Remnant W49B

W49B is a unique Galactic supernova remnant with centrally peaked, “bar”-like ejecta distribution, which was once considered evidence for a hypernova origin that resulted in a bipolar ejection of the stellar core. However, chemical abundance measurements contradict this interpretation. Closely connected to the morphology of the ejecta is its velocity distribution, which provides critical details for understanding the explosion mechanism. We report the first ever observational constraint on the kinematics of the ejecta in W49B using the Resolve microcalorimeter spectrometer on the X-ray Imaging and Spectroscopy Mission (XRISM). Using XRISM/Resolve, we measured the line-of-sight velocity traced by the Fe Heα emission, which is the brightest feature in the Resolve spectrum, to vary by ±300 km s −1 with a smooth east-to-west gradient of a few tens of kilometers per second per parsec along the major axis. Similar trends in the line-of-sight velocity structure were found for other Fe-group elements Cr and Mn, traced by the Heα emission, and also for intermediate-mass elements Si, S, Ar, and Ca, traced by the Lyα emission. The discovery of the east–west gradient in the line-of-sight velocity, together with the absence of a twin-peaked line profile or enhanced broadening in the central region, clearly rejects the equatorially expanding disk model. In contrast, the observed velocity structure suggests bipolar flows reminiscent of a bipolar explosion scenario. An alternative scenario would be a collimation of the ejecta by an elongated cavity sculpted by bipolar stellar winds.

High resolution spectroscopy↗

DOE OSTI2025

Discovery of Powerful Multivelocity Ultrafast Outflows in the Starburst Merger Galaxy IRAS 05189–2524 with XRISM

We observed the X-ray-bright ultraluminous infrared galaxy IRAS 05189−2524 with XRISM during its performance verification phase. The unprecedented energy resolution of the onboard X-ray microcalorimeter revealed complex spectral features at ∼7–9 keV, which can be interpreted as blueshifted Fe XXV/XXVI absorption lines with various velocity dispersions, originating from ultrafast outflow (UFO) components with multiple bulk velocities of ∼0.076c, ∼0.101c, and ∼0.143c. In addition, a broad Fe–K emission line was detected around ∼7 keV, forming a P Cygni profile together with the absorption lines. The onboard X-ray CCD camera revealed a 0.4–12 keV broadband spectrum characterized by a neutrally absorbed power-law continuum with a photon index of ∼2.3 and intrinsic flare-like variability on timescales of ∼10 ks, both of which are likely associated with near-Eddington accretion. We also found potential variability of the UFO parameters on a timescale of ∼140 ks. Using these properties, we propose new constraints on the outflow structure and suggest the presence of multiple outflowing regions on scales of about tens to 100 Schwarzschild radii, located within roughly 2000 Schwarzschild radii. Since both the estimated momentum and energy outflow rates of the UFOs exceed those of galactic molecular outflows, our results indicate that powerful, multivelocity UFOs are already well developed during a short-lived evolutionary phase following a major galaxy merger, characterized by intense starburst activity and likely preceding the quasar phase. This system is expected to evolve into a quasar, sustaining strong UFO activity and suppressing star formation in the host galaxy.

Astronomy and AstroPhysics↗

NASA NTRS1985

Thermal detectors as single photon X-ray spectrometers

In a thermal detector employed for X-ray spectroscopy applications, the energy of an X-ray is converted to heat in a small mass, and the energy of that X-ray inferred from the size of the temperature rise. The present investigation is concerned with the possibility to make an extremely low heat capacity calorimeter which can be employed as a thermal detector. Several types of calorimeters were fabricated and tested at temperatures as low as approximately 0.05 K. The obtained devices make use of thermistors constructed of melt-doped silicon, nuclear transmutation doped (NTD) germanium, and ion-implanted silicon with a variety of materials for the support and electrical leads. The utility of these microcalorimeters as X-ray spectrometers could be verified.

Moseley, S. H.↗

NASA NTRS1986

Thermal detectors for high resolution spectroscopy

Cryogenic microcalorimeters can be made sensitive enough to measure the energy deposited by a single particle or X-ray photon with an accuracy of about one electron volt. It may also be possible to construct detectors of several-kilograms mass whose resolution is only a few times worse than this. Data from relatively crude test devices are in good agreement with thermal performance calculations, and a total system noise of 11 eV FWHM has been obtained for a silicon detector operating at 98 mK. Observations of 35 eV FWHM for 6-keV X-rays with a different device have been made.

Mccammon, D.↗

NASA NTRS1987

X-ray astronomical spectroscopy

The contributions of the Goddard group to the history of X-ray astronomy are numerous and varied. One role that the group has continued to play involves the pursuit of techniques for the measurement and interpretation of the X-ray spectra of cosmic sources. The latest development is the selection of the X-ray microcalorimeter for the Advanced X-ray Astrophysics Facility (AXAF) study payload. This technology is likely to revolutionize the study of cosmic X-ray spectra.

Holt, Stephen S.↗

NASA NTRS1988

Advances toward high spectral resolution quantum X-ray calorimetry

Thermal detectors for X-ray spectroscopy combining high spectral resolution and quantum efficiency have been developed. These microcalorimeters measure the energy released in the absorption of a single photon by sensing the rise in temperature of a small absorbing structure. The ultimate energy resolution of such a device is limited by the thermodynamic power fluctuations in the thermal link between the calorimeter and isothermal bath and can in principle be made as low as 1 eV. The performance of a real device is degraded due to noise contributions such as excess 1/f noise in the thermistor and incomplete conversion of energy into phonons. The authors report some recent advances in thermometry, X-ray absorption and thermalization, fabrication techniques, and detector optimization in the presence of noise. These improvements have resulted in a device with a spectral resolution of 17 eV FWHM, measured at 6 keV.

Moseley, S. H.↗

NASA NTRS1988

Measuring H0 and q0 with X-ray lines from galaxy clusters

A new method of measuring angular diameter distances, and hence H0 and q0, by means of X-ray observations of galaxy clusters is proposed. It resembles the method which combines maps of X-ray continuum emission with maps of the Suniaev-Zel'dovich effect, but substitutes measurements of X-ray absorption lines in the spectra of background quasars for the Suniaev-Zel'dovich effect. When the high resolution permitted by the AXAF microcalorimeter becomes available, this method should yield results with significantly smaller uncertainty.

Krolik, Julian H.↗

NASA NTRS1990

X-ray spectroscopic instrumentation for the 21st century

Several technologies being developed for high resolution X-ray spectroscopy are compared to determine the most suitable applications for each. Nondispersive cryogenic technology is considered by means of devices such as microcalorimeters and superconducting tunnel-junction detectors, and dispersive technologies are represented by crystal diffractors, transmission gratings and reflection gratings. Calorimeters and superconducting tunnel-junction conductors are found to be suitable for high energies while reflection gratings are more effective at lower energies. In general, however, the selected technology depends primarily on the particular implementation. Parameters such as launch capability, constraints, and scientific drivers are the guiding forces for selecting a particular device.

Kahn, Steven M.↗

NASA NTRS1992

Nickel-hydrogen battery self-discharge mechanism and methods for its inhibition

A review of our studies on the elucidation of the self-discharge mechanism of the Ni/H2 battery and methods to inhibit this phenomena is presented. The results show that (1) the rate of heat generation from nickel hydroxide powders and from electrodes increases with increase of hydrogen pressure, simultaneously, the open-circuit potential of the nickel hydroxide electrode is shifted in a negative direction more rapidly, indicating the transformation of NiOOH to Ni(OH)2; (2) heat generation rates measured in the microcalorimeter are considerably faster for electrolyte starved electrodes than for electrolyte-flooded electrodes; (3) there is a good correlation between the extent of self-discharge, as determined by heat generation in microcalorimetric measurement and capacity change; and (4) the self-discharge in Ni/H2 battery occurs via direct reduction of the active material by pressurized hydrogen. The addition of cadmium to the electrode reduces the self-discharge.

Visintin, Arnaldo↗

NASA NTRS1991

The AXAF/XRS ADR - Engineering model

A spaceworthy Adiabatic Demagnetization Refrigerator is under development at Goddard Space Flight Center as part of the X-Ray Spectrometer (XRS), an instrument on the Advanced X-ray Astrophysics Facility (AXAF). XRS will employ an array of 32 microcalorimeters capable of detecting X-rays in the energy range of 0.3 - 10 keV. In order to achieve a desired resolution of 12 eV, these detectors must be operated at a temperature of 0.065 - 0.100 K. An ADR must be used to cool these detectors in space. A breadboard model was designed and built less than two years ago, and provided excellent results. We are presently at the development stage of the engineering model. Several changes have been made to the original design in order to improve the efficiency of the ADR, to reduce its weight, and to strengthen the salt pill suspension system so that the ADR can survive launch loads and have low sensitivity to microphonic inputs. We shall report on the results of these changes; what worked and what did not.

Serlemitsos, Aristides T.↗

NASA NTRS1991

The AXAF/XRS test dewar - A versatile design

The X-Ray Spectrometer (XRS) to be flown on the Advanced X-ray Astrophysics Facility (AXAF) consists of an array of microcalorimeters and an Adiabatic Demagnetization Refrigerator (ADR). The ADR provides an operating temperature of 0.065 to 0.100 K. To support extensive development testing of the ADR and the detector array, a test dewar has been designed and built that surpasses specification requirements. Pumping on the liquid helium bath with a 47 l/s pump, we have achieved temperatures lower than 1.5 K with a hold time in excess of 72 hrs. The dewar can be operated without liquid nitrogen with a hold time of 36 hrs. This feature was incorporated in the design because boiling nitrogen may introduce microphonic noise to the detectors. To further reduce the susceptibility to microphonic vibration a unique suspension system utilizing Kevlar fibers was devised which provides both translational and rotational rigidity to the detector mount. Finally, the dewar is very manageable and may be rotated by only one person.

Weintz, Karl F.↗

NASA NTRS1999

The Astro-E/XRS Calibration Program and Results

XRS is the microcalorimeter X-ray detector aboard the US-Japanese ASTRO-E observatory, which is scheduled to be launched in early 2000. XRS is a high resolution spectrometer- with less than 9 eV resolution at 3 keV and better than 14 eV resolution over its bandpass ranging from about 0.3 keV to 15 keV. Here we present the results of our first calibration of the XRS instrument. We describe the methods used to extract detailed information about the detection efficiency and spectral redistribution of the instrument. We also present comparisons of simulations and real data to test our detector models.

Gendreau, Keith C.↗