Hard X-ray Nanoprobe Beamline Research Articles

The design of the front-end layout and first high-power-density masks for the hard X-ray nano-probe beamline at SSRF

The design of the front-end layout and first high-power-density masks for the hard X-ray nano-probe beamline at SSRF

Multilayer Kirkpatrick-Baez focusing mirrors with phase compensation for sub-20 nm focusing at the hard X-ray nanoprobe beamline of SSRF

The hard X-ray nanoprobe beamline is the first beamline to take advantage of the full coherent beam to attain the nanoscale focusing at the Shanghai Synchrotron Radiation Facility (SSRF). Here we introduce the beamline and specially go over the features of the multilayer Kirkpatrick-Baez focusing system and its supporting phase compensator system. The performance and stability of the phase compensator are also put to the test. By using the speckle scanning metrology, the wavefront of a focused beam was characterized and intensity distribution near the focus was reconstructed. The focusing performance was greatly enhanced by two phase compensations based on a global optimization technique, and a two-dimensional focal spot of 26 nm × 17 nm was achieved and maintained with good stability.

Orbit stabilization for the new insertion devices in SSRF

During the Shanghai Synchrotron Radiation Facility (SSRF) beamline project, fourteen new insertion devices (IDs) have been successfully installed and transitioned to operation. However, these new IDs led to considerable closed orbit distortions in the SSRF storage ring. In the canted beamlines, the theoretical current values of dipoles required for the closed dual-canted angle were established, however, errors in the actual machine make a significant effect on closed orbit. To address this, an adjustment configuration, based on the response matrix, was developed for the closed dual-canted angles. Additionally, an orbit feedforward compensation system equipped with corrector coils, was employed. As a result, the maximum horizontal and vertical orbit distortions induced by the IDs were successfully decreased to less than 5.0 μm and 3.5 μm, respectively. Furthermore, a specialized local fast feedback system was designed to maintain the precise orbit and angle stability for the Hard X-ray Nanoprobe beamline.

Research on the simulation environment of hard X-ray nanoprobe beamline station

In the hard X-ray nanoprobe beamline station, experiments need to be performed by adjusting the optical equipment in order to obtain good beamline performance. Due to many factors, only through the use of intelligent optimization, the beamline performance can be quickly improved. Therefore, an intelligent optimization method is proposed in this work to improve the performance of the beamline rapidly by using an adaptive algorithm to optimize the motor shaft of each device. Moreover, this paper introduces the simulation environment of the hard X-ray nanoprobe beamline equipment. In this environment, a multi-axis parallel optimization model of several optical devices is designed, and the ionization chamber feedback is replaced by Rastrigin function. Furthermore, the differential evolution algorithm is used to verify the model. The optimization tests of multiple devices in the beamline are carried out, and the automatic optimization of the devices is realized. As for the theoretical result, the designed intelligent beamline optimization program is capable of converging to the optimal value within 3-6 minutes on the simulation platform, this automated process could potentially enhance beamline adjusting efficiency by 10-20 times compared to manual beamline adjusting.

Dose-efficient multimodal microscopy of human tissue at a hard X-ray nanoprobe beamline.

X-ray fluorescence microscopy performed at nanofocusing synchrotron beamlines produces quantitative elemental distribution maps at unprecedented resolution (down to a few tens of nanometres), at the expense of relatively long measuring times and high absorbed doses. In this work, a method was implemented in which fast low-dose in-line holography was used to produce quantitative electron density maps at the mesoscale prior to nanoscale X-ray fluorescence acquisition. These maps ensure more efficient fluorescence scans and the reduction of the total absorbed dose, often relevant for radiation-sensitive (e.g. biological) samples. This multimodal microscopy approach was demonstrated on human sural nerve tissue. The two imaging modes provide complementary information at a comparable resolution, ultimately limited by the focal spot size. The experimental setup presented allows the user to swap between them in a flexible and reproducible fashion, as well as to easily adapt the scanning parameters during an experiment to fine-tune resolution and fieldof view.

Use of Multi-Modal Synchrotron Analytical Techniques Combined with Electrochemical Analysis to Understand Anomalous Localized and General Corrosion Behavior of Additively Manufactured 316L Stainless Steel

Additive manufacturing (AM) of alloys such as stainless steels has the potential to be a disruptive technology for design of complex structures which eliminates the potentially damaging effects of mechanical failure and localized corrosion associated with interfaces between separate parts (which can now be printed as part of a single assembly). In addition, increasingly complex geometries can be manufactured with nearly as much ease as simple ones, and new mechanisms for optimization and generative design can allow manufacturers to achieve significant material and weight savings. However, challenges remain, in particular due to the potential for material variability both between parts made with the same nominal build parameters and even within a single build, as the consistency in properties inherent in the commercial-scale forging of alloys to be machined into components is exchanged for the considerable advantages of on-site, distributed custom parts production. Our studies and related work by other groups indicates that this is clearly true in the case of corrosion susceptibility in AM alloys. By studying the relationship between build parameters and electrochemical properties, we propose that it will be possible to tailor alloys for enhanced corrosion properties.AM processes produce materials with hierarchical microstructures containing fusion boundaries at the macroscale, irregular grains and grain boundaries at the microscale, and subgrain dislocation structures at the nanoscale. In laser powder bed fusion (LPBF) formed 316L stainless steel structures, corrosion performance has been discussed in the context of chemical heterogeneities formed in the presence of these hierarchical microstructures. Furthermore, localized corrosion (pitting) is closely related to microstructural defects including dislocation structures, inclusions, and localized elemental segregation which has been found to occur during the very rapid heating and cooling which occurs during laser fusion AM processes.In this presentation, we explore multi-modal synchrotron X-ray techniques for quantifying hierarchical microstructures and their connection to the underlying chemical distribution in 316L stainless steel, as well as localized heterogeneities in the passive film structure. Our results show that the dislocation density depends on the printing conditions with implications for the chemical distribution at the nanoscale, which in turn may play a key role in inconsistent corrosion behavior. Furthermore, we discuss the correlation between this print-formed alloy surface microstructure (dislocation structures, Mn inclusions, and elemental segregation), and local heterogeneities in the passive film formed on LPDF 316L in Cl-containing media. These heterogeneities observed in the passive layer may in turn impact repassivation and other processes critical in localized cession phenomena.Samples formed at varying speeds using pulsed and continuous laser deposition are compared via cyclic polarization in 3.5% NaCl and 0.1M HCl solutions, as well as using Mott-Schottky analysis of passive layers formed in 0.1M HCl. Surface corrosion layers are characterized using laboratory-based X-ray photoelectron spectroscopy to determine the impact on passivity of the aforementioned microsegregation associated with process-induced microstructures. Corrosion rates and pit densities are then discussed to build a connection between printing conditions and corrosion performance vis-à-vis microstructural and chemical information from synchrotron measurements performed at Brookhaven National Laboratory (BNL), including high energy X-ray diffraction using the X-ray Powder Diffraction (XPD) beamline at the National Synchrotron Light Source-II (NSLS-II) which provided data on minor precipitate population(s), atomic structure and dislocation microstructures critical to corrosion behavior. In addition, heterogeneities in elemental composition data is provided by 2D X-ray fluorescence (XRF) and 2D X-ray Absorption Spectroscopy (XAS) nanometer resolution-mapping obtained at the Hard X-ray Nanoprobe (HXN) beamline at the NSLS-II and correlated with process-induced hierarchal structures via use of the microscopy facilities at the Center for Functional Nanomaterials (CFN). X-ray photoemission microspectroscopy/low energy electron microscopy (XPEEM/LEEM) conducted at the Electron Spectro-Microscopy beamline at the NSLS-II provides evidence that the passive layer itself contains inhomogeneities, including areas enriched in oxidized Cr and Mn, as well as microstructural boundaries, reflecting the inhomogeneities in the microstructure of the alloy surface beneath. Mott-Schottky analysis of the passive layer provides further evidence that these inhomogeneities, correlated with alloy microstructure, impact the semiconducting character (and hence protective properties) of the passive layer.By employing a combination of multi-modal synchrotron characterization techniques, electron microscopy, and baseline testing protocol combined with electrochemical polarization experiments, we are able to study the role of microstructure across multiple length scales on electrochemical properties and corrosion performance. Understanding the impact of microstructure and chemical heterogeneities on the susceptibility to pitting and intergranular attack will enable microstructurally-informed process optimization and materials design for enhancing the corrosion resistance of LPBF 316L stainless steel, with implications for AM and subsequent durability of alloys in general.

NanoMAX: the hard X-ray nanoprobe beamline at the MAX IV Laboratory.

NanoMAX is the first hard X-ray nanoprobe beamline at the MAX IV laboratory. It utilizes the unique properties of the world's first operational multi-bend achromat storage ring to provide an intense and coherent focused beam for experiments with several methods. In this paper we present the beamline optics design in detail, show the performance figures, and give an overview of the surrounding infrastructure and the operational diffraction endstation.

Beam and sample movement compensation for robust spectro-microscopy measurements on a hard X-ray nanoprobe.

Static and in situ nanoscale spectro-microscopy is now routinely performed on the Hard X-ray Nanoprobe beamline at Diamond and the solutions implemented to provide robust energy scanning and experimental operation are described. A software-based scheme for active feedback stabilization of X-ray beam position and monochromatic beam flux across the operating energy range of the beamline is reported, consisting of two linked feedback loops using extremum seeking and position control. Multimodal registration methods have been implemented for active compensation of drift during an experiment to compensate for sample movement during in situ experiments or from beam-induced effects.

The Hard X-ray Nanoprobe beamline at Diamond Light Source.

The Hard X-ray Nanoprobe beamline, I14, at Diamond Light Source is a new facility for nanoscale microscopy. The beamline was designed with an emphasis on multi-modal analysis, providing elemental mapping, speciation mapping by XANES, structural phase mapping using nano-XRD and imaging through differential phase contrast and ptychography. The 185 m-long beamline operates over a 5 keV to 23 keV energy range providing a ≤50 nm beam size for routine user experiments and a flexible scanning system allowing fast acquisition. The beamline achieves robust and stable operation by imaging the source in the vertical direction and implementing horizontally deflecting primary optics and an overfilled secondary source in the horizontal direction. This paper describes the design considerations, optical layout, aspects of the hardware engineering and scanning system in operation as well as some examples illustrating the beamline performance.

Magnetic Field Optimization of an In-Vacuum Undulator at NSLS-II Transactions on Applied Superconductivity

A 3.0 m long In-Vacuum Undulator (IVU) is employed at the National Synchrotron Light Source II (NSLS-II) for the Hard X-ray Nanoprobe (HXN) beamline providing structural and X-ray fluorescence imaging with world-leading spatial resolution. On July 1 st 2018 a gearbox shaft in the gap drive train assembly sheared due to corrosion fatigue caused by stress due to mechanical misalignment. The device was extracted from the storage ring and measured. The magnetic field measurements detected a degradation of the magnetic performance as well as a localized demagnetization of the magnetic modules of the first 3 upstream periods. This paper describes the mechanical repairs and the magnetic phase shimming optimization implemented to restore the spectral performance of the device.

Use of Multi-Modal Synchrotron Analytical Techniques to Understand Anomalous Localized and General Corrosion Behavior of Additively Manufactured 316L Stainless Steel

Additive manufacturing (AM) of alloys such as stainless steels has the potential to be a disruptive technology for design of complex structures which eliminates the potentially damaging effects of mechanical failure and localized corrosion associated with interfaces between separate parts (which can now be printed as part of a single assembly). In addition, increasingly complex geometries can be manufactured with nearly as much ease as simple ones, and new mechanisms for optimization and generative design can allow manufacturers to achieve significant material and weight savings. However, challenges remain, in particular due to the potential for material variabilities both between parts made with the same nominal build parameters and even within a single build, as the consistency in properties inherent in the commercial-scale forging of alloys to be machined into components is exchanged for the considerable advantages of on-site, distributed custom parts production. Our studies and related work by other groups indicates that this is clearly true in the case of corrosion susceptibility in AM alloys. By studying the relationship between build parameters and electrochemical properties, we propose that it will be possible to tailor alloys for enhanced corrosion properties.AM processes produce materials with hierarchical microstructures containing fusion boundaries at the macroscale, irregular grains and grain boundaries at the microscale, and subgrain dislocation structures at the nanoscale. In laser powder bed fusion (LPBF) formed 316L stainless steel structures, corrosion performance has been discussed in the context of chemical heterogeneities formed in the presence of these hierarchical microstructures. However, the large variability in reported measurements underscores the need for statistically significant microstructural data, which is often difficult to access via electron microscopy alone. In this presentation, we explore multi-modal synchrotron X-ray techniques for quantifying hierarchical microstructures and their connection to the underlying chemical distribution in 316L stainless steel. Our results show that the dislocation density depends on the printing conditions with implications for the chemical distribution at the nanoscale, which in turn may play a key role in inconsistent corrosion behavior.LPDF 316L samples formed at varying speeds using pulsed and continuous laser deposition are compared via cyclic polarization in 3.5% NaCl and 0.1M HCl solutions, as well as using standard methods for characterizing sensitization. Surface corrosion layers are characterized using laboratory-based X-ray photoelectron spectroscopy to determine the impact on passivity of the aforementioned microsegregation associated with process-induced microstructures. Corrosion rates and pit densities are then discussed to build a connection between printing conditions and corrosion performance vis-à-vis microstructural and chemical information from synchrotron measurements performed at Brookhaven National Laboratory (BNL), including high energy X-ray diffraction using the X-ray Powder Diffraction (XPD) beamline at the National Synchrotron Light Source-II (NSLS-II) which provided data on minor precipitate population(s), atomic structure and dislocation microstructures critical to corrosion behavior. In addition, heterogeneities in elemental composition data is provided by 2D X-ray fluorescence (XRF) and 2D X-ray Absorption Spectroscopy (XAS) nanometer resolution-mapping obtained at the Hard X-ray Nanoprobe (HXN) beamline at the NSLS-II and correlated with process-induced hierarchal structures via use of the microscopy facilities at the Center for Functional Nanomaterials (CFN).By employing a combination of multi-modal synchrotron characterization techniques, electron microscopy, and baseline testing protocol combined with electrochemical polarization experiments, we are able to study the the role of microstructure across multiple length scales on electrochemical properties and corrosion performance. Understanding the impact of microstructure and chemical heterogeneities on the susceptibility to pitting and intergranular attack will enable microstructurally-informed process optimization and materials design for enhancing the corrosion resistance of LPBF 316L stainless steel, with implications for AM and subsequent durability of alloys in general.

Metals Coprecipitation with Barite: Nano-XRF Observation of Enhanced Strontium Incorporation.

Coprecipitation can be an effective treatment method for the removal of environmentally relevant metals from industrial wastewaters such as produced waters from the oil and gas industry. The precipitation of barite, BaSO4, through the addition of sulfate removes barium while coprecipitating strontium and other alkaline earth metals even when these are present at concentrations below their solubility limit. Among other analytical methods, X-ray fluorescence (XRF) nanospectroscopy at the Hard X-ray Nanoprobe (HXN) beamline at the National Synchrotron Light Source II (NSLS-II) was used to quantify Sr incorporation into barite. Thermodynamic modeling of (Ba,Sr)SO4 solid solutions was done using solid solution—aqueous solution (SS-AS) theory. The quantitative, high-resolution nano-XRF data show clearly that the Sr content in (Ba,Sr)SO4 solid solutions varies widely among particles and even within a single particle. We observed substantial Sr incorporation that is far larger than thermodynamic models predict, likely indicating the formation of metastable solid solutions. We also observed that increasing barite supersaturation of the aqueous phase led to increased Sr incorporation, as predicted by available kinetic models. These results suggest that coprecipitation offers significant potential for designing treatment systems for aqueous metals' removal in desired metastable compositions. Solution conditions may be optimized to enhance the incorporation of Sr by increasing sulfate addition such that the barite saturation index remains above ∼3 or by increasing the aqueous Sr to Ba ratio.

Coherent Bragg imaging of 60 nm Au nanoparticles under electrochemical control at the NanoMAX beamline.

Nanoparticles are essential electrocatalysts in chemical production, water treatment and energy conversion, but engineering efficient and specific catalysts requires understanding complex structure-reactivity relations. Recent experiments have shown that Bragg coherent diffraction imaging might be a powerful tool in this regard. The technique provides three-dimensional lattice strain fields from which surface reactivity maps can be inferred. However, all experiments published so far have investigated particles an order of magnitude larger than those used in practical applications. Studying smaller particles quickly becomes demanding as the diffracted intensity falls. Here, in situ nanodiffraction data from 60 nm Au nanoparticles under electrochemical control collected at the hard X-ray nanoprobe beamline of MAX IV, NanoMAX, are presented. Two-dimensional image reconstructions of these particles are produced, and it is estimated that NanoMAX, which is now open for general users, has the requisites for three-dimensional imaging of particles of a size relevant for catalytic applications. This represents the first demonstration of coherent X-ray diffraction experiments performed at a diffraction-limited storage ring, and illustrates the importance of these new sources for experiments where coherence properties become crucial.

X-ray Fluorescence Nanotomography of Single Bacteria with a Sub-15\u2009nm Beam

X-ray Fluorescence (XRF) microscopy is a growing approach for imaging the trace element concentration, distribution, and speciation in biological cells at the nanoscale. Moreover, three-dimensional nanotomography provides the added advantage of imaging subcellular structure and chemical identity in three dimensions without the need for staining or sectioning of cells. To date, technical challenges in X-ray optics, sample preparation, and detection sensitivity have limited the use of XRF nanotomography in this area. Here, XRF nanotomography was used to image the elemental distribution in individual E. coli bacterial cells using a sub-15 nm beam at the Hard X-ray Nanoprobe beamline (HXN, 3-ID) at NSLS-II. These measurements were simultaneously combined with ptychography to image structural components of the cells. The cells were embedded in small (3–20 µm) sodium chloride crystals, which provided a non-aqueous matrix to retain the three-dimensional structure of the E. coli while collecting data at room temperature. Results showed a generally uniform distribution of calcium in the cells, but an inhomogeneous zinc distribution, most notably with concentrated regions of zinc at the polar ends of the cells. This work demonstrates that simultaneous two-dimensional ptychography and XRF nanotomography can be performed with a sub-15 nm beam size on unfrozen biological cells to co-localize elemental distribution and nanostructure simultaneously.

Nanospectroscopy Captures Nanoscale Compositional Zonation in Barite Solid Solutions

Scientists have long suspected that compositionally zoned particles can form under far-from equilibrium precipitation conditions, but their inferences have been based on bulk solid and solution measurements. We are the first to directly observe nanoscale trace element compositional zonation in <10 µm-sized particles using X-ray fluorescence nanospectroscopy at the Hard X-ray Nanoprobe (HXN) Beamline at National Synchrotron Light Source II (NSLS-II). Through high-resolution images, compositional zonation was observed in barite (BaSO4) particles precipitated from aqueous solution, in which Sr2+ cations as well as HAsO42− anions were co-precipitated into (Ba,Sr)SO4 or Ba(SO4,HAsO4) solid solutions. Under high salinity conditions (NaCl ≥ 1.0 M), bands contained ~3.5 to ~5 times more trace element compared to the center of the particle formed in early stages of particle growth. Quantitative analysis of Sr and As fractional substitution allowed us to determine that different crystallographic growth directions incorporated trace elements to different extents. These findings provide supporting evidence that barite solid solutions have great potential for trace element incorporation; this has significant implications for environmental and engineered systems that remove hazardous substances from water.

The Hard X-ray Nanoprobe Beamline at Diamond - Current Status

The Hard X-ray Nanoprobe Beamline at Diamond - Current Status

Imaging Capabilities, Performance and Applications of the Hard X-ray Nanoprobe Beamline at NSLS-II

Imaging Capabilities, Performance and Applications of the Hard X-ray Nanoprobe Beamline at NSLS-II

Design and performance of an X-ray scanning microscope at the Hard X-ray Nanoprobe beamline of NSLS-II.

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ∼15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature of a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.

Quantitative Nanostructure Analysis of Silver Vanadium Phosphorus Oxide (Ag2VO2PO4) Battery Material Using X-Ray and Electron Microscopy

With the state-of-art synchrotron-based X-ray and modern electron microscopy, the spatial resolution and measurement sensitivity have been significantly improved in analyzing materials’ nanostructure, by taking advantages of the high beam flux density or the source brightness. Associated with the ever brighter beam, it also brings the opportunity to investigate the beam effect to material structure modification, which is of significant interests in view of understanding the underlying physics, and it is also important to develop proper methodologies to use these state-of-the art probes to accurately characterize the intrinsic and extrinsic properties of materials. In our work, we performed x-ray imaging experiment on single crystalline Ag2VO2PO4 battery material sample with a 15 nm resolution using the recently commissioned x-ray imaging capability at the Hard X-ray Nanoprobe Beamline at the National Synchrotron Light Source II. Probe-induced electrochemical reaction was observed, which was revealed by the Ag reduction as well as diffusion and re-distribution of Ag. In order to better understand the probe-induced electrochemical reactions, we also performed imaging experiments with other imaging methods: white-beam microdiffraction, transmission x-ray microscopy (TXM), and transmission electron microscopy (TEM). These probes deliver different levels of radiation does and provides different pathways for probe-induced structural modification. This presentation will elaborate and quantify the probe-specific structural modifications.

(Invited) Multi-Modality X-Ray Imaging at a 10 Nanometer Resolution

The Hard X-ray Nanoprobe (HXN) beamline at the NSLS-II is constructed to explore new frontiers of the x-ray microscopy, by enabling an unprecedented spatial resolution of ~10 nm in the hard x-ray regime. The beamline offers simultaneous multi-modality imaging capabilities including x-ray fluorescence, x-ray diffraction, x-ray absorption, x-ray scattering, phase-contrast imaging, spectroscopy, and ptychography. These suite of imaging tools open up new scientific opportunities to visualize complex nanostructures with unprecedented sensitivity to material composition, morphology, crystalline phases/strain, and chemical state. Use of hard x-rays allows accurate quantification of buried nanostructure with straightforward analyses. Presentation will describe the present and near-future scientific capabilities of this new imaging facility with the recent results.