The soft X-ray spectromicroscopy beamline BL08U1A upgrade at SSRF.

Beamline BL08U1A is a soft X-ray spectromicroscopy beamline at Shanghai Synchrotron Radiation Facility (SSRF) that exhibits the capabilities of high spatial resolution (30 nm) and high energy resolving power (over 104). As a first-generation beamline of SSRF, owing to its continuous operation over the last ten years, an urgent upgrade of the equipment including the monochromator was deemed necessary. The upgrade work included the overall construction of the monochromator and replacement of the mirrors upstream and downstream of the monochromator. Based on its original skeleton, two elliptically cylinder mirrors were designed to focus the beam horizontally, which can increase the flux density by about three times on the exit slits. Meanwhile, the application of variable-line-space gratings in the monochromator demonstrates the dual functions of dispersing and focusing on the exit slits which can decrease abberations dramatically. After the upgrade of the main components of the beamline, the energy range is 180-2000 eV, the energy resolving power reaches 16333 @ 244 eV and 12730 @ 401 eV, and the photon flux measured in the experimental station is over 2.45 × 109 photons s-1 (E/ΔE = 6440 @ 244 eV).

Development and commissioning of a broadband online X-ray spectrometer for the SXFEL Facility.

A broadband online X-ray spectrometer has been designed and commissioned at the SUD beamline of the Shanghai Soft X-ray Free-Electron Laser Facility, which can deliver both SASE and seeded FEL pulses to user experiments, spanning the photon energy range of 50-620 eV. The resolving powers of the spectrometer calibrated via online measurement at 92 eV and 249 eV are ∼20000 and ∼15000, respectively, and the absolute photon energy is characterized by an electron time-of-flight spectrometer. The high energy resolution provided by the spectrometer can differentiate the fine structure in the FEL spectrum, to determine its pulse length.

High-accuracy measurement, advanced theory and analysis of the evolution of satellite transitions in manganese Kα using XR-HERFD.

Here, the novel technique of extended-range high-energy-resolution fluorescence detection (XR-HERFD) has successfully observed the n = 2 satellite in manganese to a high accuracy. The significance of the satellite signature presented is many hundreds of standard errors and well beyond typical discovery levels of three to six standard errors. This satellite is a sensitive indicator for all manganese-containing materials in condensed matter. The uncertainty in the measurements has been defined, which clearly observes multiple peaks and structure indicative of complex physical quantum-mechanical processes. Theoretical calculations of energy eigenvalues, shake-off probability and Auger rates are also presented, which explain the origin of the satellite from physical n = 2 shake-off processes. The evolution in the intensity of this satellite is measured relative to the full Kα spectrum of manganese to investigate satellite structure, and therefore many-body processes, as a function of incident energy. Results demonstrate that the many-body reduction factor S02 should not be modelled with a constant value as is currently done. This work makes a significant contribution to the challenge of understanding many-body processes and interpreting HERFD or resonant inelastic X-ray scattering spectra in a quantitative manner.

Energy Resolution from a Silicon Detector's Interstrip Regions.

In this work, we present a novel approach for improving the energy resolution from particles impinging on the interstrip regions of silicon strip detectors. We employed three double-sided strip detectors from the GRIT array and a triple α-source under laboratory conditions. The results showed that the interstrip resolution depends not only on the impinging side but also on whether it is a P- or an N-interstrip. We obtained the interstrip energy resolution down to 0.4%, and, depending on the scenario, the resolution was enhanced by a factor of 2. We believe that this new rotation method allows for the possibility of applying particle identification methods on interstrip events, which in most cases are dismissed during data recording.

Synchrotron speciation of umbilical cord mercury and selenium after environmental exposure in Niigata.

The insidious and deadly nature of mercury's organometallic compounds is informed by two large scale poisonings due to industrial mercury pollution that occurred decades ago in Minamata and Niigata, Japan. The present study examined chemical speciation for both mercury and selenium in a historic umbilical cord sample from a child born to a mother who lived near the Agano River in Niigata. The mother had experienced mercury exposure leading to more than 50 ppm mercury measured in her hair and was symptomatic 9 years prior to the birth. We sought to determine the mercury and selenium speciation in the child's cord using Hg Lα1 and Se Kα1 high-energy resolution fluorescence detected X-ray absorption spectroscopy, the chemical speciation of mercury was found to be predominantly organometallic and coordinated to a thiolate. The selenium was found to be primarily in an organic form and at levels higher than those of mercury, with no evidence of mercury-selenium chemical species. Our results are consistent with mercury exposure at Niigata being due to exposure to organometallic mercury species.

Sub-nanotesla sensitivity at the nanoscale with a single spin.

High-sensitivity detection of the microscopic magnetic field is essential in many fields. Good sensitivity and high spatial resolution are mutually contradictory in measurement, which is quantified by the energy resolution limit. Here we report that a sensitivity of 0.5 nT/[Formula: see text] at the nanoscale is achieved experimentally by using nitrogen-vacancy defects in diamond with depths of tens of nanometers. The achieved sensitivity is substantially enhanced by integrating with multiple quantum techniques, including real-time-feedback initialization, dynamical decoupling with shaped pulses and repetitive readout via quantum logic. Our magnetic sensors will shed new light on searching new physics beyond the standard model, investigating microscopic magnetic phenomena in condensed matters, and detection of life activities at the sub-cellular scale.

Achieving a Record Scintillation Performance by Micro-Doping a Heterovalent Magnetic Ion in Cs3 Cu2 I5 Single-Crystal.

An ultrabright, ultrafast, and low-cost ideal scintillator has been critically absent and is sorely desired in scintillation detection, but has hitherto not been found. Here, a high-quality bulk Cs3 Cu2 I5 :Mn single-crystal scintillator with ultrahigh light yield (≈95 772 photons per MeV, 137 Cs γ-rays), excellent energy resolution (3.79%, 662 keV), and ultrafast scintillation decay time (3 ns, 81.5%) is reported. In mechanism, it is found that micro-doping of a heterovalent magnetic ion (at the ppm level) can effectively modulate the luminescence kinetics of self-trapped excitons in the scintillator. Compared with previous reports, the introduction of trace amounts of magnetic Mn2+ (≈18.6 ppm) in Cs3 Cu2 I5 single-crystal shortens the scintillation decay time by several hundred times, transforming the slow decay into an ultrafast decay. Simultaneously, the light yield is also increased about three times to the highest value so far. From the comprehensive performance of the micro-doped Cs3 Cu2 I5 :Mn single-crystal, these excellent scintillation properties, physical characteristics suitable for practical applications, and low-cost advantages render this single-crystal an ideal scintillator with great potential for commercialization.

Np(V) Retention at the Illite du Puy Surface.

In this study, Np(V) retention on Illite du Puy (IdP) was investigated since it is essential for understanding the migration behavior of Np in argillaceous environments. The presence of structural Fe(III) and Fe(II) in IdP was confirmed by Fe K-edge X-ray absorption near-edge structure (XANES) and 57Fe Mössbauer spectroscopy. In batch sorption experiments, a higher Np sorption affinity to IdP was found than to Wyoming smectite or iron-free synthetic montmorillonite. An increase of the relative Np(IV) ratio sorbed onto IdP with decreasing pH was observed by solvent extraction (up to (24 ± 2)% at pH 5, c0(Np) = 10-6 mol/L). Furthermore, up to (33 ± 5)% Np(IV) could be detected in IdP diffusion samples at pH 5. Respective Np M5-edge high-energy resolution (HR-) XANES spectra suggested the presence of Np(IV/V) mixtures and weakened axial bond covalency of the NpO2+ species sorbed onto IdP. Np L3-edge extended X-ray absorption fine structure (EXAFS) analysis showed that significant fractions of Np were coordinated to Fe─O entities at pH 9. This highlights the potential role of Fe(II/III) clay edge sites as a strong Np(V) surface complex partner and points to the partial reduction of sorbed Np(V) to Np(IV) via structural Fe(II).

Radiation Damage by Heavy Ions in Silicon and Silicon Carbide Detectors.

While silicon has been a steadfast semiconductor material for the past 50 years, it is now facing competition from other materials, especially for detector design. In that respect, due to its high resistance to radiation damage, silicon carbide is one of the most promising materials. In this work, we discuss the radiation damage studies of a new, large area, p-n junction silicon carbide device developed by the SiCILIA collaboration. We have studied the general performances of several devices, as a function of fluence, irradiated in different experimental conditions with different beams. A standard p-n junction silicon detector was also irradiated for comparison. The new detectors manifest excellent performance in terms of stability of the main parameters, linearity, defect distribution, charge collection efficiency, energy resolution, leakage current, etc. Experimental results evidence a radiation resistance of SiC devices more than two order of magnitude higher than Si devices. The new construction technology applied to silicon carbide material has made it possible to create very robust devices with excellent performance. These devices will soon be available for all those scientific projects where a high resistance to radiation damage is required.

Gun energy filter for a low energy electron microscope.

In a Low Energy Electron Microscope (LEEM) the sample is illuminated with an electron beam with typical electron landing energies from 0-100 eV. The energy spread of the electron beam is determined by the characteristics of the electron source. For the two most commonly used electron sources, LaB6 and cold field emission W, typical energy spreads ΔE are 0.75 and 0.25 eV at full width half maximum, respectively. Here we present a design for a LEEM gun energy filter, that reduces ΔE to ∼100 meV. Such a filter has been incorporated in the IBM/SPECS AC-LEEM system at IBM. Experimental results are presented and found to be in excellent agreement with expectations.

Development of a high energy resolution and wide dose rate range portable gamma-ray spectrometer.

In this paper, a portable gamma-ray spectrometer for real-time and in-situ gamma-ray detection applications is presented. By combining a quasi-hemispherical CdZnTe (CZT) semiconductor detector and a Geiger-Muller (GM) counter together, a wide dose rate range is achieved, ranging from 0.1 µSv/h to 100 mSv/h with a relative error of less than 10%. The GM counter is used to measure dose rate from 1 mSv/h to 100 mSv/h. With CZT, the spectrometer can provide a high energy resolution spectrum for nuclide identification and a high precision dose rate at low dose rates. The full width half maximum (FWHM) resolution is 2.2% at 662 keV below 70 µSv/h and is better than 3.3% at 3.8 mSv/h. The weight of the spectrometer is 3.2 kg for handheld and the runtime is up to 12 h without charging. For preliminary applications, the spectrometer was used to measure the gamma radiation around the Back-n white neutron beam line at China Spallation Neutron Source and around the steam generator in the nuclear power plant at Daya Bay Nuclear Power Station.

Impact of Flexible Circuit Bonding and System Integration on Energy Resolution of Cross-Strip CZT Detectors.

Cadmium zinc telluride (CZT) detectors enable high spatial resolution and high detection efficiency and are utilized for many gamma-ray and X-ray spectroscopy applications. In this article, we describe a stable bonding process and report on the characterization of cross-strip CZT detectors before and after bonding to flexible circuit. The bonding process utilizes gold stud bonding and polymer epoxy technique to bond the flexible circuits to two CZT crystals and form a detector module in an anode-cathode-cathode-anode (ACCA) configuration. The readout electronics is optimized in terms of shaper setting and steering electrode voltage. The average full-width half maximum (FWHM) energy resolution at 662 keV of 110 CZT crystals tested individually was 3.5% ± 0.59% and 4.75% ± 0.48% prebonded and post-bonded, respectively. No depth correction was performed in this study. The average FWHM energy resolution at 662 keV of the scaled-up system with 80 CZT crystals was 4.40% ± 0.53%, indicating the scaled-up readout electronics and stacking of the modules does not deteriorate performance. The proper shielding and grounding of the scaled-up system slightly improved the system-wide performance. The FWHM energy resolution at 511 keV of the scaled-up system was 5.85% ± 0.73%.

The Effects of Different Anode Positions on the Electrical Properties of Square-Silicon Drift Detector.

The Silicon Drift Detector (SDD) with square structure is often used in pixel-type SDD arrays to reduce the dead region considerably and to improve the detector performance significantly. Usually, the anode is located in the center of the active region of the SDD with square structure (square-SDD), but the different anode positions in the square-SDD active area are also allowed. In order to explore the effect on device performance when the anode is located at different positions in the square-SDD active region, we designed two different types of square-SDD in this work, where the anode is located either in the center (SDD-1) or at the edge (SDD-2) of its active region. The simulation results of current density and potential distribution show that SDD-1 and SDD-2 have both formed a good electron drift path to make the anode collect electrons. The experimental results of device performance at the temperature range from -60 °C to 60 °C show that the anode current of the two fabricated SDDs both decreased with the decrease of temperature, but their voltage divider characteristics exhibited high stability resistance value and low temperature coefficient, thereby indicating that they could both provide corresponding continuous and uniform electric field at different temperatures. Finally, SDD-1 and SDD-2 have energy resolutions of 248 and 257 eV corresponding to the 5.9 keV photon peak of the Fe-55 radioactive source, respectively. Our experimental results demonstrate that there is no significant impact on the device performance irrespective of the anode positions in the square-SDD devices.

Multicolor single-analyzer high-energy-resolution XES spectrometer for simultaneous examination of different elements.

The present work demonstrates the performance of a von Hámos high-energy-resolution X-ray spectrometer based on a non-conventional conical Si single-crystal analyzer. The analyzer is tested with different primary and secondary X-ray sources as well as a hard X-ray sensitive CCD camera. The spectrometer setup is also characterized with ray-tracing simulations. Both experimental and simulated results affirm that the conical spectrometer can efficiently detect and resolve the two pairs of two elements (Ni and Cu) Kα X-ray emission spectroscopy (XES) peaks simultaneously, requiring a less than 2 cm-wide array on a single position-sensitive detector. The possible applications of this simple yet broad-energy-spectrum crystal spectrometer range from quickly adapting it as another probe for complex experiments at synchrotron beamlines to analyzing X-ray emission from plasma generated by ultrashort laser pulses at modern laser facilities.

Advances in Detector Instrumentation for PET.

During the last 3 decades, PET has become a standard-of-care imaging technique used in the management of cancer and in the characterization of neurologic disorders and cardiovascular disease. It has also emerged as a prominent molecular imaging method to study the basic biologic pathways of disease in rodent models. This review describes the basics of PET detectors, including a detailed description of indirect and direct 511-keV photon detection methods. We will also cover key detector performance parameters and describe detector instrumentation advances during the last decade.

Design and characterization of third-order Sallen-Key digital filter in nuclear signal processing.

The Gaussian filter shaping circuit is widely used in the nuclear pulse signal processing due to its good performance in amplitude extraction and pulse counting. A third-order Sallen-Key (3rd S-K) filter shaping circuit is designed based on a RC integrator and a second-order Sallen-Key (2nd S-K) circuit. According to the digital 3rd S-K, the transfer functions is derived in the Laplacian domain, and the numerical recurrence model is analyzed and researched, the purpose is to obtain its transfer function and amplitude-frequency response curve in the z-domain. For the simulation and actual sampling of the nuclear signal, digital shaping processing is performed at different parameters, three parameters (d, SNR, δ) are defined to compare and analyze the amplitude extraction, noise suppression and symmetry of the digital shaping method, which shows that as the shaping parameters increases, the digital shaping output noise suppression performance is better, the SNR increased from 49.25 to 64.21, the waveform is more symmetrical, the δ reduced from 34.05 to 0.22. At the same parameters, it is compared and analyzed with CR-RC3 and 2nd S-K shaping methods, according to the digital Gaussian shaping results, the 3rd S-K digital shaping method has better pulse amplitude extraction(d = 36.06%), noise suppression performance (SNR = 64.21) and waveform symmetry (δ = 0.22). Under different shaping methods, the energy resolution and pulse counting rate of the Fe characteristic X-ray energy spectrum are compared based on a Si-PIN detector. The results show that the 3rd S-K digital shaping method has better energy resolution performance and comprehensive performance indicators, which can be further applied for digital shaping of nuclear pulse signals.

Paving the way for examination of coupled redox/solid-liquid interface reactions: 1 ppm Np adsorbed on clay studied by Np M5-edge HR-XANES spectroscopy.

The recently emerged actinide (An) M4,5-edge high-energy resolution X-ray absorption near-edge structure (HR-XANES) technique has proven to be very powerful for oxidation state studies of actinides. In this work, for the first time, Np M5-edge HR-XANES was applied to study Np sorption on illite. By improving the experimental conditions, notably by operation of the spectrometer under He atmosphere, it was possible to measure Np M5-edge HR-XANES spectra of a sample with ≈ 1 µg Np/g illite (1 ppm). This is 30-2000 times lower than Np loadings on mineral surfaces usually investigated by X-ray absorption spectroscopy. A newly designed cryogenic configuration enabled sample temperatures of 141.2 ± 1.5 K and successfully prevented beam-induced changes of the Np oxidation state. The described approach paves the way for the examination of coupled redox/solid-liquid interface reactions of actinide ions via An M4,5-edge HR-XANES spectroscopy at low metal ion concentrations, which are of specific relevance for contaminated sites and nuclear waste disposal studies.

The Performance of EDXS at Elevated Sample Temperatures Using a MEMS-Based In Situ TEM Heating System.

Since the development of MEMS heating holders, dynamic in-situ experiments at elevated temperatures may be complemented by X-ray spectrometry for chemical analysis. Although the amount of IR radiation is small when compared to furnace holders, the influence of IR radiation emitted from the heating device on the quality of the X-ray spectra is significant. In this work, we systematically examine the influence of infrared (IR) radiation generated by MEMS-based in situ heating systems (DENSsolutions single- and double-tilt holders) on the results and interpretation of energy-dispersive X-ray (EDX) spectra through simulation and measurement. Focal points of interest in this study are the influence of holder geometry, shadowing and orientation with respect to the different emission characteristics of IR and X-ray photons and their interaction with a side-entry and a multi-detector system. IR photons substantially contribute to count rates, dead time, electronic noise levels, energy resolution, and detection efficiency of semiconductor detectors. At higher sample temperatures, they ultimately limit the feasibility of EDXS for elemental characterization and especially the traceability of low-Z elements. This work provides a quantitative insight into the influence of all relevant parameters related to in situ heating experiments on the spectral quality. Bearing this in mind, we aim to provide a guide to optimizing in situ heating experiments with respect to chemical EDXS analysis.

Data and simulation studies on the influence of scintillation crystal dimensions on spectrometric parameters.

The study presented in this paper aims to explain the influence of scintillation detector size on spectrometric parameters. For this purpose, a setup composed of 1.5"×1.5", 2"×2" and 3"×3" NaI(Tl) detectors from the same manufacturer was performed. Furthermore, the linearity of detector response to gamma-ray energy was examined for all detectors. Our results show that the energy resolution presents a remarkable dependency to detector size, governed by a second order polynomial function. Thus, the energy resolution shows a significant decrease for almost all energies. As expected, full-energy peak efficiency and Peak-to-Total coefficients have a notable correlation with NaI(Tl) crystal size. In order to study a larger range of crystal sizes, we have developed a Monte Carlo (MC) simulation model using Geant4 (V 10.05). The obtained results were presented using ROOT (V 6.14/08) data analysis framework. The statistical uncertainties were below 4% for all obtained spectra. The comparison of simulated and measured results shows an excellent agreement. The accuracy of our model and the real detector responses has been quantified by applying statistical tests. In this context, a negligible deviation within 4.1% and 3.96% was found, for the obtained response functions and efficiency curves, respectively. An important improvement of intrinsic efficiency and photoelectric effect probability was observed for larger crystals. However, our study shows that CPU-time increases with increasing the active volume of the detector.

Development and Characterization of Modular Readout Design for Two-Panel Head-and-Neck Dedicated PET System Based on CZT Detectors.

Cadmium zinc telluride (CZT) detectors are suitable for various applications due to the good energy resolution and the simple pixilation to achieve high spatial resolution. Our group is developing a two-panel head and neck dedicated positron emission tomography system based on CZT detectors. Each panel will consist of 150 CZT crystals (4×4×0.5 cm3) covering an area of 20×15 cm2 in an edge-on configuration to achieve high detector efficiency at 511 keV. In this work, we present the design and development of a full data acquisition chain that enables a low noise and compact readout for each panel. The initial results of the readout circuit were quantified using a 1 kHz square wave test pulse. The pulse amplitude was chosen to generate approximately the same amount of charges as a 511 keV photon would provide in CZT. The best-case FWHM electronic noise at 511 keV was measured to be 0.69% ± 0.16% (3.52 ± 0.81 in keV units after conversion). The FWHM electronic noise at 511 keV for a complete DAQ chain was 4.33% ± 0.30% (22.13 ± 1.53 in keV units).