Ultra-high-resolution Microcalorimeter X-ray Spectrometer for Nuclear Forensics Chemical and Elemental Analysis in the Scanning Electron Microscope
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Microcalorimeter pulse shape characteristics, such as pulse height, decay time and rise time, are dependent on the detector temperature and bias as well as the photon energy and flux. We examine the nature of the temperature dependency by illuminating the ASTRO-E2 X-ray Spectrometer (XRS) microcalorimeter array with X-rays generated by electron impact on a range of foil targets. The resulting pulses are collected for a range of detector temperatures. We observe and model the temperature dependence of the pulse shape characteristics by fitting the data with non-linear pulse models. Our aim is to determine a robust method for correcting the energy scale obtained in ground calibration for slight differences in the operating conditions while in orbit.
Nuclear forensics relies on the integration of complementary signatures to constrain the origins and history of materials. Outcomes benefit from the timeliness and precision of the disparate methods that form typical analysis chains. Sample forms are often either minute in quantity or contain signatures like morphology or composition heterogeneity encoded on a microscale, so many analysis techniques focus on resolving signatures on ever-smaller length scales. The new hyperspectral x-ray imaging (HXI) instrument developed at Los Alamos National Laboratory seeks to improve the information available from scanning electron microscopy (SEM) x-ray spectrum analysis through superior spectral energy resolution vs. typical energy dispersive spectroscopy (EDS) systems in common use in nuclear forensics and other microanalysis fields. Based on arrays of transition-edge sensor (TES) microcalorimeter detectors, this instrument achieves a typical energy resolution of 7 eV full-width at half-maximum (FWHM) at 2 keV, opening new possibilities in trace element detection/analysis and chemical state determination through spectral shape shifts. We present here some of the first applications of the HXI instrument to actinide samples and discuss potential maturation of this nascent technology for future analysis pipelines.
Microcalorimeter arrays used as imaging spectrometers will enable ground-breaking science in X-ray astrophysics. Their development has been one of the driving applications of the low temperature detector community since the early 1980s. While their application in space remains in relative infancy, we are on the verge of an era in which microcalorimeter spectrometers are likely to dominate instrumentation for high-energy astrophysics missions. NASA sounding rocket experiments such as the X-ray Quantum Calorimeter (XQC) and Micro-X have now paved the way for orbital observatories. JAXA’s Astro-H gave us a glimpse of this fantastic new capability before its unfortunate demise. The launch of XRISM later this year should finally demonstrate the sort of large suite of observations that X-ray microcalorimeter arrays will make major contributions to. In the mid-2030s, we will see the launch of ESA’s flagship Athena mission, that will further advance the imaging and spectroscopic capabilities for the high-energy X-ray community enormously. Numerous other potential new mission concepts using X-ray microcalorimeters have been studied in detail such as NASA’s Lynx and the Light Element Mapper (LEM), JAXA’s Super-DIOS, and China’s Hot Universe Baryon Surveyor (HUBS). In the first half of this presentation, I will review the development and desired requirements of the X-ray microcalorimeter missions and concepts, and describe the current progress and status missions being implemented and proposed. In the second half of this presentation, I will focus on The Line Emission Mapper (LEM) which is a probe-class mission concept under study by NASA that is designed to provide unprecedented insight into the physics of galaxy formation, including stellar and black-hole feedback and flows of baryonic matter into and out of galaxies. LEM incorporates a light-weight X-ray optic with 10” angular resolution and a large-format microcalorimeter array with a 15” pixel pitch over a 29’ field of view (FOV). The main microcalorimeter array and readout design takes advantage of mature technology that has been developed for Athena X-IFU. The central 7’ region of the array consists of ~ 800 transition-edge sensors (TESs), optimized for a bandpass of 0.3-2 keV and with an energy resolution of 1.2 eV at 1 keV. The rest of the FOV is covered by 4-pixel TES hydras with 2.5 eV energy resolution at 1 keV. Hydras are position-sensitive (‘thermally multiplexed’) detectors that enable extremely large numbers of effective pixels in an array, without a commensurate increase in the number of wires, bias circuit, and readout components. In total the array will have ~ 4k TESs with ~ 14k imaging elements on a 290 micron-pitch. The array will be read out with state-of-the-art time-division multiplexing (TDM), implement with 59 pixels (and 1 dark pixel) in each of the 69 TDM columns. Here we present a detailed overview of the baseline microcalorimeter detector design and present first results from both single pixel TESs and 4-pixel hydras. Our prototype LEM pixels utilize 15um x 50um Mo/Au TESs with a transition temperature of around 58 mK. These pixels incorporate high-fill-factor Au absorbers of thickness 0.54um. We have demonstrated an energy resolution of 0.90+/-0.02 eV and 1.90 +/-0.02 eV at 1.5 keV for single pixel and 4-pixel hydras, respectively, meeting the performance requirements of LEM. We show how the position discrimination in the hydra pixels can be achieved, down to energies of a few 100 eV, using the measured pulse rise-times. Finally, we will show that the properties of the LEM pixels are well optimized for the proposed TDM read out architecture.
The goal of this project is to develop specific aspects of ultra-high-resolution microcalorimeter technologies that support IAEA Nuclear Material Laboratory needs and the goals of SP-1 19/NML-003 "Microcalorimetry Analysis Technique for NML" but are outside the scope of the SP-1. The focus is on commissioning, assembly, and testing of the microcalorimeter decay energy spectrometer with superconducting transition-edge sensors (TESs) and magnetic microcalorimeters (MMCs) in preparation for transfer to the IAEA Nuclear Material Laboratory.
We are developing kilo-pixel arrays of TES microcalorimeters to enable high-resolution X-ray imaging spectrometers for future X-ray observatories and laboratory astrophysics experiments. Our current array design was targeted as a prototype for the X-ray Microcalorimeter Spectrometer proposed for the International X-ray Observatory, which calls for a 40x40-pixel core array of 300 micron devices with 2.5 e V energy resolution (at 6 keV). Here we present device characterization of our 32x32 arrays, including X-ray spectral performance of individual pixels within the array. We present our results in light of the understanding that our Mo/Au TESs act as weak superconducting links, causing the TES critical current (Ic) and transition shape to oscillate with applied magnetic field (B). We show Ic(B) measurements and discuss the uniformity of these measurements across the array, as well as implications regarding the uniformity of device noise and response. In addition, we are working to reduce pixel-to-pixel electrical and thermal crosstalk; we present recent test results from an array that has microstrip wiring and an angle-evaporated Cu backside heatsinking layer, which provides Cu coverage on the four sidewalls of the silicon wells beneath each pixel.
We are developing kilopixel arrays of TES microcalorimeters to enable high-resolution x-ray imaging spectrometers for future x-ray observatories and laboratory astrophysics experiments. Our current array design was targeted as a prototype for the X-ray Microcalorimeter Spectrometer proposed for the International X-ray Observatory, which calls for a 40×40-pixel core array of 300 micron devices with 2.5 eV energy resolution (at 6 keV). Here we present device characterization of our 32×32 arrays, including x-ray spectral performance of individual pixels within the array. We present our results in light of the understanding that our Mo/Au TESs act as weak superconducting links, causing the TES critical current (I(sub c)) and transition shape to oscillate with applied magnetic field (B). We show I(sub c)(B) measurements and discuss the uniformity of these measurements across the array, as well as implications regarding the uniformity of device noise and response. In addition, we are working to reduce pixel-to-pixel electrical and thermal crosstalk; we present recent test results from an array that has microstrip wiring and an angle-evaporated copper backside heatsinking layer, which provides copper coverage on the four sidewalls of the silicon wells beneath each pixel.
Absolute wavelength references are needed to derive the plasma velocities from the Doppler shift of a given line emitted by a moving plasma. We show that such reference standards exist for the strongest x-ray line in neonlike W64+, which has become the line of choice for the ITER (Latin the way) core imaging x-ray spectrometer. Close-by standards are the Hf L3 line and the Ir L2 line, which bracket the W64+ line by 30 eV; other standards are given by the Ir L1 and L2 lines and the Hf L1 and L2 lines, which bracket the W64+ line by 40 and 160 eV, respectively. The reference standards can be produced by an x-ray tube built into the ITER spectrometer. We present spectra of the reference lines obtained with an x-ray microcalorimeter and compare them to spectra of the W64+ line obtained both with an x-ray microcalorimeter and a crystal spectrometer
During the past 13 years high resolution X ray spectrometers have been developed that use cryogenically cooled microcalorimeters. These devices have inherently high signal-to-noise by operating at temperatures below 0.1 K and can achieve an energy resolution of < 10 eV over the 0.1-10 keV band. Existing devices use doped semiconductor thermometers and typically employ HgTe absorbers. The energy resolution depends on achieving a low heat capacity for the device. For soft X ray applications a relatively thin absorber (approximately 1 micrometer) may be used and an energy resolution of approximately 7 eV has been achieved. For applications up to approximately 10 keV an absorber thickness of approximately 10 micrometer is required and the energy resolution is typically approximately 12 eV. Improvements to the energy resolution in this energy band could be achieved if the problems of thermalizing X rays in low heat capacity superconductors can be overcome. The recent work on transition edge thermometers by Irwin et nl. looks particularly promising because of the higher sensitivity achievable from a sharp superconducting transition. The relatively low impedance of such a device permits the use of a low noise SQUID amplifier for readout. This would also significantly reduce the cryogen heat load compared with JFETs required by higher impedance semiconductor thermometers.
The X-Ray Imaging and Spectroscopy Mission satellite was launched on September 6, 2023 (UT). Its Resolve instrument is a high-resolution X-ray spectrometer enabled by a microcalorimeter array thermally anchored to a 50-mK heat sink. Many sensitive, critical sub-systems comprise Resolve, including a multistage cryogenic cooling system, thin-film aperture filters, low-noise electronics, on-board signal processing, and several sources of X-rays for calibration. We summarize the initial on-orbit power-on and checkout of Resolve that commenced immediately after launch. Soon after launch, the cryocoolers were activated, and their operation was successfully established. On October 9, 2023, the first cycle of the adiabatic demagnetization refrigerator was carried out, bringing the sensors to their steady-state operational temperatures. Following this, the energy resolution at 5.9 keV was successfully measured. The energy scale of the system is highly sensitive to the thermal environment surrounding both the sensors and their analog electronics. Gain correction was performed using reference X-ray lines from onboard calibration sources. To optimize cooler frequency settings, noise spectra were collected across a range of frequencies, and the most suitable frequency pair was selected based on the in-orbit environment. During the final phase of the checkout, an attempt was made to open the gate valve, which is designed to protect the Dewar’s interior from external pressure during ground operations and launch. Unfortunately, this attempt was unsuccessful. As a result, the checkout process was temporarily paused, and a stable operational strategy was subsequently developed to enable Resolve to function effectively with the gate valve remaining closed.
We report on our progress towards the development of arrays of X-ray microcalorimeters as candidates for the high resolution x-ray spectrometer on the Constellation-X mission. The microcalorimeter arrays (30 x 30) with appropriate pixel sizes (0.25 mm. x 0.25 mm) and high packing fractions (greater than 96%) are being developed. Each individual pixel has a 10 micron thick Bi X-ray absorber that is shaped like a mushroom to increase the packing fraction, and a Mo/Au proximity effect superconducting transition edge sensor (TES). These are deposited on a 0.25 or 0.5 micron thick silicon nitride membrane with slits to provide a controllable weak thermal link to the sink temperature. Studies are underway to model, test and optimize the TES pixel uniformity, critical current, heat capacity and the membrane thermal conductance in the array structure. Fabrication issues and procedures, and results of our efforts based on these optimizations will be provided.
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.
The Lynx x-ray microcalorimeter (LXM) is an imaging spectrometer for the Lynx satellite mission, an x-ray telescope being considered by NASA to be a new flagship mission. Lynx will enable unique astrophysical observations into the x-ray universe due to its high angular resolution and large field of view. The LXM consists of an array of over 100,000 pixels and poses a significant technological challenge to achieve the high degree of multiplexing required to read out these sensors. We discuss the details of microwave superconducting quantum interference device (SQUID) multiplexing and describe why it is ideally suited to the needs of the LXM. This case is made by summarizing the current and predicted performance of microwave SQUID multiplexing and describing the steps needed to optimize designs for all the LXM arrays. Finally, we describe our plan to advance the technology readiness level (TRL) of microwave SQUID multiplexing of the LXM microcalorimeters to TRL-5 by 2024.
Metallic magnetic calorimeter (MMC) technology is a leading contender for detectors for the Lynx X-ray Microcalorimeter, which is an imaging spectrometer consisting of an array of greater than 100,000 pixels. The fabrication of such large arrays presents a challenge when attempting to route the superconducting wiring from the pixels to the multiplexed readout. If the wiring is designed to be planar, then an aggressive, submicron scale wiring pitch has to be employed, which is technically challenging to design and fabricate on account of the requirements of low inductance, low cross-talk, high critical currents and high yield. An alternative way to achieve large scale, high density wiring is through the use of multiple buried metal layers, planarized by Chemical Mechanical Planarization. This approach is well-suited for connecting thousands of pixels on a large focal plane to readout chips, and also for fabricating sensor meander coils with narrow line widths, which helps in increasing the sensor inductance and thus alleviates stray inductance issues associated with the wiring in large size arrays. In this work we describe the fabrication of high sensor inductance MMC arrays implementing Lynx concepts and incorporating multiple layers of buried Nb wiring. The detector array is composed of three sub-arrays with pixels optimized to meet the different science driven performance requirements of Lynx. In two of the sub-arrays we adopt a thermal multiplexing scheme to read out pixels by coupling 25 absorbers to a single sensor through thermal links of varied thermal conductance. We demonstrate the successful fabrication of multi-absorber MMCs with fine pitch pixels in very large size arrays.
Lynx is an x-ray telescope, one of four large satellite mission concepts currently being studied by NASA to be a flagship mission. One of Lynx’s three instruments is an imaging spectrometer called the Lynx x-ray microcalorimeter (LXM), an x-ray microcalorimeter behind an x-ray optic with an angular resolution of 0.5 arc sec and ∼2 sq. m of area at 1 keV. The LXM will provide unparalleled diagnostics of distant extended structures and, in particular, will allow the detailed study of the role of cosmic feedback in the evolution of the Universe. We discuss the baseline design of LXM and some parallel approaches for some of the key technologies. The baseline sensor technology uses transition-edge sensors, but we also consider an alternative approach using metallic magnetic calorimeters. We discuss the requirements for the instrument, the pixel layout, and the baseline readout design, which uses microwave superconducting quantum interference devices and high-electron mobility transistor amplifiers and the cryogenic cooling requirements and strategy for meeting these requirements. For each of these technologies, we discuss the current technology readiness level and our strategy for advancing them to be ready for flight. We also describe the current system design, including the block diagram, and our estimate for the mass, power, and data rate of the instrument.
Lynx is an x-ray telescope, one of four large satellite mission concepts currently being studied by NASA to be the next astrophysics flagship mission after WFIRST. One of Lynx's three instruments is an imaging spectrometer consisting of an x-ray microcalorimeter behind an X-ray optic with an angular resolution of 0.5 arc-seconds and approximately 3 sq m of area at 1 keV. This instrument will provide unparalleled diagnostics of distant extended structures and in particular will allow the detailed study of the role of cosmic feedback in the evolution of the Universe. We discuss the design and read-out of the of the array configuration including a number of sub-array options for increasing the capabilities to maximize the scientific return of the Lynx observatory.
The measured instrumental background of the XRS calorimeter spectrometer of Suzaku had several sources, including primary cosmic rays and secondary particles interacting with the pixels and with the silicon structure of the array. Prior to the launch of Suzaku, several data sets were taken without x-ray illumination to study the characteristics and timing of background signals produced in the array and anti-coincidence detector. Even though the source of the background in the laboratory was different from that in low-earth orbit (muons and environmental gamma-rays on the ground versus Galactic cosmic-ray (GCR) protons and alpha particles in space), the study of correlations and properties of populations of rare events was useful for establishing the preliminary screening parameters needed for selection of good science data. Sea-level muons are singly charged minimum-ionizing particles, like the GCR protons, and thus were good probes of the effectiveness of screening via the signals from the anti-coincidence detector. Here we present the first analysis of the on-ground background of the SXS calorimeter of Astro-H. On XRS, the background prior to screening was completely dominated by coincident events on many pixels resulting from the temperature pulse arising from each large energy deposition (greater than 200 keV) into the silicon frame around the array. The improved heat-sinking of the SXS array compared with XRS eliminated these thermal disturbances, greatly reducing the measured count rate in the absence of illumination. The removal of these events has made it easier to study the nature of the residual background and to look for additional event populations. We compare the SXS residual background to that measured in equivalent ground data for XRS and discuss these preliminary results.
Reliable results when fitting X-ray data require proper consideration of the statistics involved. We probe the impact of Gaussian versus Poisson statistics at low count levels using both the standard χ^(2) method and maximum likelihood based on Poisson (C) statistics. The difference is studied and quantified through simulated spectra with known properties. We then test the results through analysis of Mn Kα calibration data taken with the flight spare microcalorimeter for the Hitomi soft X-ray spectrometer. Through comparison with simulations, our results show that the χ^(2) method tends to give overly optimistic estimates of the detector energy resolution, in particular when there are few counts. Given an energy resolution of ∼5 eV and a line with about 100 photons, the line width becomes ∼10% lower in the χ^(2) method than in Poisson statistics. This is a consequence of the uncertainties being dominated by counting statistics, and therefore highlights the need to choose the appropriate fit statistic.