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The design and operational performance of beamline I14, the Hard X-ray Nanoprobe at Diamond Light Source, is presented., 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.

X-ray magnetic circular dichroism (XMCD) spectroscopy is a key technique for studying magnetic materials, providing element specificity and significantly high detection sensitivity to magnetic mome...

Time-resolved cathodoluminescence is a key tool with high temporal and spatial resolution. However, optical spectroscopic information can be also extracted using synchrotron pulses in a hard X-ray nanoprobe, exploiting a phenomenon called X-ray excited optical luminescence. Here, with 20 ps time resolution and 80 nm lateral resolution, we applied this time-resolved X-ray microscopy technique to individual core-shell InGaN/GaN multiple quantum well heterostructures deposited on GaN wires. Our findings suggest that the m-plane related multiple quantum well states govern the carrier dynamics. Likewise, our observations support not only the influence of In incorporation in the recombination rates, but also carrier localization phenomena at the hexagon wire apex. In addition, our experiment calls for further investigations of the spatiotemporal domain on the underlying mechanisms of optoelectronic nanodevices. Its great potential becomes more valuable when time-resolved X-ray excited optical luminescence microscopy is used in operando with other methods, such as X-ray absorption spectroscopy., G.M.-C. acknowledges the funding by the Spanish Ministry of Innovation, Science, and Technology and the Spanish Ministry of Economy through Research Project RTI2018-097195-B-I00. In addition, the MSCA-ITN-2020 Funding Scheme from the European Union’s Horizon 2020 programme under Grant agreement ID: 956548 is acknowledged.

This work is an overview of the multi-modal hard X-ray nanoprobe beamline at the MAX IV Laboratory. The beamline provides an intense and coherent beam, focused to 40–200 nm in the energy range 5–28 eV., 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 stability and sample drift compensation schemes are presented for use on I14, the Hard X-ray Nanoprobe at Diamond Light Source., 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.

International audience; Benefiting from the recent advances of synchrotron X-ray nanoprobes, we demonstrate three-dimensional (3D) correlative nano-imaging on malaria-infected human red blood cells. By combining X-ray fluorescence to-mography and phase contrast nanotomography on the same cell with sub-100 nm pixel size, we establish a routine workflow from the data acquisition, data processing to tomographic reconstruction. We quantitatively compare the elemental volumes obtained with different reconstruction methods, the total variation minimization giving the most satisfactory results. We reveal elemental correlations in different cell compartments more reliably on reconstructions as opposed to 2D projections. Finally, we determine for the first time the 3D mass fraction maps of multiple elements at sub-cellular level. The estimated total number of Fe atoms and the total mass of the red blood cell show very good agreement with previously reported values.

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.

A synchrotron source offers the advantage of continuous and tunable x rays. Therefore, not only an X-ray nanoprobe can provide the desired spatial resolution to measure the elemental distribution of CaAlSiN3:Eu2+ via X-ray fluorescence mapping but X-ray absorption spectroscopy can also be used to unambiguously analyze the valence states of europium ions (Eu2+ or Eu3+) in different local areas. X-ray excited optical luminescence spectra exhibit only one red emission peak (∼650 nm) corresponding to the 4f65d1 to 4f7 transition of Eu2+, which reveals the fact that Eu2+ ions substitute perfectly for Ca2+ ions at the same site. Through detailed analysis, we demonstrated that the main contribution to the luminescence intensity of CASIN:Eu2+ comes from the Eu2+ activator in the product. We anticipate that X-ray nanoprobes will open new avenues with great characterization ability for studying the emission properties of CASIN:Eu2+.

Scanning hard x-ray microscopy is a versatile imaging tool that offers a suite of analytic x-ray techniques for studying spatially-resolved elemental, structural and chemical variations. Recent advances in nano-focusing optics and instrumentation have pushed the frontier of the field into multi-modal imaging in 3D and with nanoscale resolution. Here we present current imaging capabilities provided by the hard x-ray nanoprobe of the National Synchrotron Light Source II at Brookhaven National Laboratory. A variety of imaging modalities (absorption, phase, fluorescence and diffraction) will be discussed, as well as the data analysis challenges associated with them. We show that x-ray imaging at about 10 nm resolution has become routine measurements at the beamline, and has been used for a wide spectrum of scientific applications.

CARNAUBA (Coherent X-Ray Nanoprobe Beamline) is an X-ray beamline under construction for the SIRIUS light source at LNLS (Brazilian Synchrotron Light Laboratory). The aim of the beamline is to provide multi-analytical and coherent X-ray imaging techniques based on achromatic optics in the energy range between 2 and 15 keV. Computed tomography will extend these techniques into three dimensions. Two end-stations are under development: an all-invacuum nanoprobe (SAPOTI) and a sub-microprobe (TARUMA), with a more flexible sample environment and much larger working distance. TARUMA will cover a large variety of scientific areas, from environmental, geophysical, agricultural and biological research to energy and more condensed matter related areas. Its design characteristics, with its mechanical design heavily based on precision engineering concepts and predictive modeling, are presented here, as well as some prospects on in situ, in operando and cryogenic sample environment experiments.

Time-resolved X-ray excited optical luminescence (TR-XEOL) was developed successfully for the 23A X-ray nanoprobe beamline located at the Taiwan Photon Source (TPS). The advantages of the TR-XEOL facility include (i) a nano-focused X-ray beam (

International audience; High Sn-content Ge1-xSnx alloys are excellent candidates for the fabrication of electronic and optoelectronic monolithically integrated devices on CMOS platforms. The fabrication of high performance devices requires high quality GeSn layers free of Sn precipitates. This work reports on the characterization of GeSn layers and micro-disk lasers with Sn concentrations ranging from 6 to 16% using synchrotron nano X-ray fluorescence mapping and nano X-ray absorption spectroscopy techniques. We demonstrate that the Sn precipitation observed in thick GeSn layers grown directly on Ge buffers can be fully suppressed, for Sn concentrations as high as 16%, with Ge1-xSnx step-graded buffers. The combination of optimal micro-disk fabrication parameters and full suppression of Sn precipitation can explain the superior lasing performance obtained in micro-disk lasers fabricated using such stacks.

Next-generation hard X-ray nanoprobe beamlines such as the In Situ Nanoprobe (ISN) beamline being planned at the Advanced Photon Source aim at providing very high spatial resolution while also enabling very high focused flux, to study complex materials and devices using fast, multidimensional imaging across many length scales. The ISN will use diffractive optics to focus X-rays with a bandpass of ∆E/E = 10−4 into a focal spot of 20 nm or below. Reflective optics in Kirkpatrick-Baez geometry will be used to focus X-rays with a bandpass as large as ∆E/E = 10−2 into a focal spot of 50 nm. Diffraction-limited focusing with reflective optics is achieved by spatial filtering and use of a very long, vertically focusing mirror. To quantify the performance of the ISN beamline, we have simulated the propagation of both partially and fully coherent wavefronts from the undulator source, through the ISN beamline and into the mirror-based focal spot. Simulations were carried out using the recently developed software “HYBRID.”

The multifunctional hard X-ray nanoprobe at Taiwan Photon Source (TPS) exhibits the excellent ability to simultaneously characterize the X-ray absorption, X-ray excited optical luminescence (XEOL) as well as the dynamics of XEOL of materials. Combining the scanning electron microscope (SEM) into the TPS 23A end-station, we can easily and quickly measure the optical properties to map out the morphology of a ZnO microrod. A special phenomenon has been observed that the oscillations in the XEOL associated with the confinement of the optical photons in the single ZnO microrod shows dramatical increase while the X-ray excitation energy is set across the Zn K-edge. Besides having the nano-scale spatial resolution, the synchrotron source also gives a good temporal domain measurement to investigate the luminescence dynamic process. The decay lifetimes of different emission wavelengths and can be simultaneously obtained from the streak image. Besides, SEM can provide the cathodoluminescence (CL) to be a complementary method to analyze the emission properties of materials, we anticipate that the X-ray nanoprobe will open new avenues with great characterization ability for developing nano/microsized optoelectronic devices.

Hard X-ray excited optical luminescence (XEOL) with a nanofocused beam provides both excellent spatial resolution and high enough peak power density, which makes XEOL mapping and luminescence dynamics study achievable. We present here the time and X-ray intensity dependence of the near-band-edge (NBE) luminescence from the nonpolar a-plane MgZnO/ZnO multiple quantum wells (MQWs): the emission intensity increases more than 10 times after high X-ray irradiation. Different from the well-known NBE emission lifetime of ZnO (less than 1 ns), the long decay time gradually decreases from 130 ns to 35 ns with the increasing X-ray irradiation time. We attribute the observed changes in NBE luminescence to the excitation of the Mg-related energy state by the high energy X-ray nanobeam. This suggestion was further confirmed in the XEOL spectra of the Mg-doped and Si-doped c-plane GaN epi-films.

This on-the-fly scanning control system is for the x-ray nanoprobe endstation at Taiwan Photon Source(TPS) and built base-on the high speed Hardware (H/W), high throughput data stream and multi-channel control interfaces. The main idea is to tag each data with information of time and position, which generates by circuit and laser interferometer. The data is then processed by a computer to be analyzed and visualized. By using high speed FPGA with embedded processer to process the input and output data which includes the DAC, ADC, Gigabit Ethernet (GbE), X-ray fluorescence (XRF) and laser interferometer control interfaces. Three DAC control the X,Y and Z axes of the flexure stage, four ADCs and sensor interfaces gather the data and packet it into data packet. GbE send data back to computer to do image processing then reconstruct the scanning image. The numerous data not only for rebuild the image but also good for information analysis. Including the vibration, time slide analysis. Our demo system is built by an e-beam source, flexure stage and laser interferometer. The current maximum scanning speed is up to 5 lines/sec which is limited by the mechanical, the sample rate can be as high as 20M samples/sec which limited by laser interferometer, and the maximum data rate is close to 100M bytes/sec which is limited by the GbE. Interferometer information combine with position data in data packet, makes easy for data analysis and also for image stitching. The system is going to commission on beamline at March, 2017. The commission result for this system will be presented.

The diffraction-limited Montel mirrors, equipped at the X-ray Nanoprobe (XNP) at Taiwan Photon Source (TPS), provide a 40 nm focal spot and working distance 55 mm under the total beamline length of 69 m. The underneath holder supporting for the Montel mirrors is a 12 axes flexure based manipulators in which 10 out of the 12 axes are motorized. To monitor the position and stability of individual holder motion, a monitoring system consisted of three optical encoders and three- axes laser interferometers for angle movement is implemented. The gap width between the two mirrors and their orthogonality can be adjusted by a tilting sensor and a high magnification optical microscope. The focusing properties, phase and amplitude, after the Montel mirrors will be investigated by means of coherent Ptychography, as well as by zone plate imaging. An SEM in close cooperation with laser interferometers is equipped to precisely position the samples and conduct the on-the-fly scan. A high speed FPGA based circuit is developed to address signal from XRF, XAS, XEOL and XRD. Data is in tag with position and time information and been processed by computers to allow 5nm precision stage scanning free from mechanical feedback. The XNP at TPS is under commissioning since February 2017. The commissioning result, particularly the performance of the Montel mirrors will be reported in this presentation.

Motivated by the Advanced Photon Source Upgrade (APS-U), a new hard X-ray microscope called “Velociprobe” has been recently designed and built for fast ptychographic imaging with high spatial resolution. We are addressing the challenges of high-resolution and fast scanning with novel hardware/stage designs, new positioner control designs, and new data acquisition strategies, including the use of high bandwidth interferometric measurements. The use of granite, air-bearing-supported stages provides the necessary long travel ranges for coarse motion to accommodate real samples and variable energy operation while remaining highly stable during fine scanning. Scanning the low-mass zone plate enables high-speed high-precision motion of the probe over the sample. Our primary goal is to use this instrument to demonstrate sub-10 nm spatial resolution ptychography over a 1-square-micron area in under 10 seconds. We have also designed the instrument to take advantage of the upgraded source when the APS-U is completed. This presentation will describe the unique designs and characteristics of this instrument, and some preliminary data obtained during the instrument commission.

NanoMAX is a hard x-ray nanoimaging beamline at the new Swedish synchrotron radiation source MAX IV that became operational in 2016. Being a beamline dedicated to x-ray nanoimaging in both 2D and 3D, NanoMAX is the first to take full advantage of MAX IVs exceptional low emittance and resulting coherent properties. We present results from the first experiments at NanoMAX that took place in December 2016. These did not use the final experimental stations that will become available to users, but a temporary arrangement including zone plate and order-sorting aperture stages and a piezo-driven sample scanner. We used zone plates with outermost zone widths of 100 nm and 30 nm and performed experiments at 8 keV photon energy for x-ray absorption and fluorescence imaging and ptychography. Moreover, we investigated stability and coherence with a Ronchi test method. Despite the rather simple setup, we could demonstrate spatial resolution below 50 nm after only a few hours of beamtime. The results showed that the beamline is working as expected and experiments approaching the 10 nm resolution level or below should be possible in the future.

The hard X-ray nanoprobe beamline (HXN) designed at the Shanghai Synchrotron Radiation facility (SSRF) will be of capability to realize a focal spot size of 10 nm for hard X-rays to satisfy requirements in biology, environmental, material sciences and etc.. The beamline includes two modes of operation, high energy resolution mode and high flux mode respectively. High flux mode utilizes the multilayer KB system to obtain high-flux diffraction-limited focusing of ~10nm. An ultra-high-precision figure fabrication for diffraction-limited focusing is required to meet the Rayleigh Criterion. An idea to overcome this problem is to introduce a phase compensator upstream of the KB system to compensate the wavefront errors in the beamline. At wavelength speckle-based method will be used to measure the wavefront error in the beamline and feedback to the phase compensator. Vibration measurements have been carried out at the secondary source and endstation hutch. The flexure hinge mechanisms and high-precision actuators ensure the KB system and sample manipulator working with high stability. The building of HXN has been designed and is under construction at present.

The CARNAUBA beamline is the tender-to-hard X-ray (2 – 15 keV) scanning nanoprobe planned for the 4th generation storage ring SIRIUS at the LNLS. CARNAUBA uses an undulator source with vertical linear polarization in a low-beta straight section and grazing incidence-focusing mirrors to create a nanoprobe at 143 m from the source. The beamline optic is based on KB mirrors and provides high brilliance at an achromatic focal spot down to the diffraction limit diameter of ~30 nm with a working distance of ~6 cm. These characteristics are crucial for studying nanometric samples in experiments involving complex stages and environments. The CARNAUBA beamline aims to perform raster scans using x-ray fluorescence, x-ray absorption spectroscopy, x-ray diffraction and coherent x-ray imaging techniques. Computed tomography will extend these methods to three dimensions.

We have performed near-field x-ray imaging with simultaneous object and probe reconstruction. By an advanced ptychographic algorithm based on longitudinal and lateral translations, full-field images of nanoscale objects are reconstructed with quantitative contrast values, along with the extended wavefronts used to illuminate the objects. The imaging scheme makes idealizing assumptions on the probe obsolete, and efficiently disentangles phase shifts related to the object from the imperfections in the illumination. We validate this approach by comparison to the conventional reconstruction scheme without simultaneous probe retrieval, based on the contrast transfer function algorithm. To this end, a set of semiconductor nanowires with controlled chemical composition (InP core, insulating SiO2 layer, and indium tin oxide cover) is imaged using the quasi-point source illumination realized by the hard x-ray nanofocus (26 nm×39 nm spot size) of the ID16A Nano-Imaging beamline at the European Synchrotron Radiation Facility.

Motivated by the advanced photon source upgrade, a new hard X-ray microscope called "Velociprobe" has been recently designed and built for fast ptychographic imaging with high spatial resolution. We are addressing the challenges of high-resolution and fast scanning with novel hardware designs, advanced motion controls, and new data acquisition strategies, including the use of high-bandwidth interferometric measurements. The use of granite, air-bearing-supported stages provides the necessary long travel ranges for coarse motion to accommodate real samples and variable energy operation while remaining highly stable during fine scanning. Scanning the low-mass zone plate enables high-speed and high-precision motion of the probe over the sample. With an advanced control algorithm implemented in a closed-loop feedback system, the setup achieves a position resolution (3σ) of 2 nm. The instrument performance is evaluated by 2D fly-scan ptychography with our developed data acquisition strategies. A spatial resolution of 8.8 nm has been demonstrated on a Au test sample with a detector continuous frame rate of 200 Hz. Using a higher flux X-ray source provided by double-multilayer monochromator, we achieve 10 nm resolution for an integrated circuit sample in an ultrafast scan with a detector's full continuous frame rate of 3000 Hz (0.33 ms per exposure), resulting in an outstanding imaging rate of 9 × 104 resolution elements per second.

The unique potential of nanoscale elemental imaging of major/minor and trace-level elemental distributions within thin biological tissue sections of the ecotoxicological model organism Daphnia magna is demonstrated by synchrotron radiation nano-X-ray fluorescence (nano-XRF). The applied highly specialized sample preparation method, coupled with the high spatial resolution (∼180 nm) and high X-ray photon flux (6 × 10(11) photons/s) available at the European Synchrotron Radiation Facility (ESRF) ID22NI beamline proved to be critical for the high-quality visualization of (trace-)metal distributions on the submicron level within the target structures of interest. These include the branchial sacs on the thoracic appendages (epipodites) of D. magna, which are osmoregulatory regions where ion exchange occurs. For the main element of interest (Zn), detection limits of 0.7 ppm (3 ag) was reached in fast-scanning mode using an acquisition time of 0.3 s/pixel. As demonstrated, synchrotron radiation nano-XRF revealed the elemental distributions of Ca, Fe, and Zn within this osmoregulatory region on the submicron scale, aiding the exploration of possible detoxification mechanisms of Zn within D. magna at the subtissue level.

Here for the first time we describe the use of high resolution nanoprobe X-ray fluorescence (XRF) mapping for the analysis of artists’ paints, hierarchically complex materials typically composed of binder, pigments, fillers, and other additives. The work undertaken at the nanoprobe sought to obtain highly spatially resolved, highly sensitive mapping of metal impurities (Pb, Cd, Fe, and other metals) in submicron particles of zinc oxide pigments used in early 20th century artists’ tube paints and enamel paints, with particular emphasis on Ripolin, a popular brand of French house paint used extensively by Pablo Picasso and some of his contemporaries. Analysis revealed that the Zn oxide particles only contain a little Fe, proving that the highest quality Zn oxide pigment, free of Pb and Cd, was used for Ripolin house paints as well as artists’ paints. Nanoprobe XRF mapping also demonstrated that artists’ tube paints generally have more abundant fillers and additional whites (based on Pb, Ti, Ca) than Ripolin paints, which contain mostly pure zinc oxide. The chemical characterization of paints at the nanoscale opens the path to a better understanding of their fabrication and chemical reactivity.

ID16B is a versatile hard X-ray nanoprobe devoted to X-ray nano-analysis. It combines X-ray fluorescence, X-ray diffraction, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques., Within the framework of the ESRF Phase I Upgrade Programme, a new state-of-the-art synchrotron beamline ID16B has been recently developed for hard X-ray nano-analysis. The construction of ID16B was driven by research areas with major scientific and societal impact such as nanotechnology, earth and environmental sciences, and bio-medical research. Based on a canted undulator source, this long beamline provides hard X-ray nanobeams optimized mainly for spectroscopic applications, including the combination of X-ray fluorescence, X-ray diffraction, X-ray excited optical luminescence, X-ray absorption spectroscopy and 2D/3D X-ray imaging techniques. Its end-station re-uses part of the apparatus of the earlier ID22 beamline, while improving and enlarging the spectroscopic capabilities: for example, the experimental arrangement offers improved lateral spatial resolution (∼50 nm), a larger and more flexible capability for in situ experiments, and monochromatic nanobeams tunable over a wider energy range which now includes the hard X-ray regime (5–70 keV). This paper describes the characteristics of this new facility, short-term technical developments and the first scientific results.

We describe the first use of a novel photoresist-free X-ray nanopatterning technique to fabricate an electronic device. We have produced a proof-of-concept device consisting of a few Josephson junctions by irradiating microcrystals of the Bi2Sr2CaCu2O8+δ (Bi-2212) superconducting oxide with a 17.6 keV synchrotron nanobeam. Fully functional devices have been obtained by locally turning the material into a nonsuperconducting state by means of hard X-ray exposure. Nano-XRD patterns reveal that the crystallinity is substantially preserved in the irradiated areas that there is no evidence of macroscopic crystal disruption. Indications are that O ions have been removed from the crystals, which could make this technique interesting also for other oxide materials. Direct-write X-ray nanopatterning represents a promising fabrication method exploiting material/material rather than vacuum/material interfaces, with the potential for nanometric resolution, improved mechanical stability, enhanced depth of patterning, and absence of chemical contamination with respect to traditional lithographic techniques.

The hard x-ray scanning microscope at beamline P06 of PETRA III at DESY in Hamburg serves a large user community, from physics, chemistry, and nanotechnology to the bio-medical, materials, environmental, and geosciences. It has been in user operation since 2012, and is mainly based on nanofocusing refractive x-ray lenses. Using refractive optics, nearly gaussian-limited nanobeams in the range from 50 to 100 nm can be generated in the hard x-ray energy range from 8 to 30 keV. The degree of coherence can be traded off against the flux in the nanobeam by a two-stage focusing scheme. We give a brief overview on published results from this instrument and describe its most important components and parameters.

The hard X-ray nanoprobe facility at Taiwan Photon Source (TPS) provides versatile X-ray analysis techniques, with tens of nanometer resolution, including XRF, XAS, XEOL, projection microscope, CDI, etc. Resulting from the large numerical aperture obtained by utilizing Montel KB mirrors, the beamline with a moderate length 75 meters can conduct similar performance with those beamlines longer than 100 meters. The two silica-made Montel mirrors are 45 degree cut and placed in a V-shape to eliminate the gap loss and the deformation caused by gravity. The slope error of the KB mirror pair is less than 0.04 µrad accomplished by elastic emission machining (EEM) method. For the beamline, a horizontal DCM and two-stage focusing in horizontal direction is applied. For the endstation, a combination of SEM for quickly positioning the sample, a fly scanning system with laser interferometers, a precise temperature control system, and a load lock transfer system will be implemented. In this presentation, the design and...