This PDF file contains the front matter associated with SPIE Proceedings Volume 10389, including the Title Page, Copyright information, Table of Contents, and Conference Committee listing.

We have explored two ways to improve the spatial resolution and/or visibility of cellular ultrastructure in full field soft X-ray nanotomography at the Mistral beamline (ALBA light source). The first one consists on a new data collection method and processing framework to computationally extend the depth of field (XTEND) of a Fresnel zone plate objective lens based on focal series projections and deconvolution. Visual details of a 3D-reconstructed eukaryotic cell that is affected by depth of field artifacts in standard tomographic reconstruction are recovered. The second one consists on diminishing the missing wedge inherent to flat sample supports (rotation range ±70deg) by performing dual axis tomography. Both strategies clearly show a spatial resolution and visibility improvement on the reconstructed volumes while complying with radiation dose limitation. Examples of these methods on relevant biological applications will be presented.

Coherent high energy X-ray microscope was employed to study the wide range of natural and artificial mesoscopic materials that are structured on scales of the order of a few to a few hundred nanometers. The microscope operates under a coherent illumination where a diffraction pattern of the specimen is formed in the back focal plane of the condenser and an inverted two-dimensional image of the object is formed by objective lens in the image plane. Functioning at 10 – 30 keV, the microscope consists of the condenser, the objective lens and two X-ray CCD cameras – large area detector for diffraction and high resolution CCD for imaging. Condenser and objective assemblies are comprised of Be parabolic refractive lenses. Switching from the diffraction mode to the imaging is achieved by placing the objective lens into the beam, and the chosen detector. The tunable objective lens offers full-field imaging with variable resolution and field of view. The microscope was applied for study of natural and synthetic opals, metal inverted photonic crystals and colloidal suspensions. The combination of the direct-space imaging and high resolution diffraction provide a wealth of information on their local structure and the long range periodic order. The development of the hard x-ray microscope emerged concomitantly with the realization of the ESRF source upgrade which greatly enhanced brilliance and fraction of coherent light, and this will open entirely new frontiers in materials imaging.

The Diamond Beamline I13L is designed to imaging on the micron- and nano-lengthsale with X-rays of energies between 6 and 30 keV [1]. Two independently operating branchlines and endstations have been built at distance of more than 200m from the source for this purpose. The imaging branch is dedicated for imaging in real space, providing In-line phase contrast imaging and grating interferometry with micrometre resolution and full-field transmission microscopy with 50nm spatial resolution. On the coherence branch coherent diffraction imaging techniques such as ptychography, coherent X-ray diffraction (CXRD) and Fourier-Transform holography are currently developed. Because of the large lateral coherence length available at I13, the beamline hosts numerous microscopy experiments. The coherence branchline in particular contains a number of unique features. New instrumental designs have been employed such as a robot arm for the detector in diffraction experiments and a photon counting detector for diffraction experiments. The so-called ‘mini-beta’ layout in the straight section of the electron storage ring permits modulating the horizontal source size and therefor the lateral coherence length. We will present the recent progress in coherent imaging at the beamline and the sciences addressed with the instrumental capabilities. Reference: [1] C. Rau, U. Wagner, Z. Pesic, A. De Fanis Physica Status Solidi (a) 208 (11). Issue 11 2522-2525, 2011, 10.1002/pssa.201184272

Diffractive X-ray optics, like Fresnel zone plate lenses, are widely employed X-ray optics for collimation and focusing. While they are extremely versatile and easy to use optical elements, they generally suffer from limited efficiency due to limitations in fabrication possibilities. Near-field stacking is an established concept for overcoming fabrication limitations, yet its existing implementations suffer from issues regarding complexity and stability. In this work, an alternative stacking concept is explored, by patterning both the front and back sides of a single membrane. Such double-sided zone plates are shown to exchange conventional zone plate stacks in increasing the efficiency or resolution of conventional zone plate optics. In conventional stacking, they achieve 9.9% focusing efficiency at 9 keV with 30 nm smallest half-pitch and diffraction limited optical performance. Following the blazed stacking scheme, they are shown to provide up to 54.7% diffraction efficiency at 6.2 keV. Finally, using the novel concept of interlaced stacking, they demonstrate the feasibility of large aperture X-ray optics for sub-10 nm X-ray nanofocusing.

Ptychography was used to determine the focus of a Multilayer-Laue-Lens (MLL) at beamline 1-BM at the Advanced Photon Source (APS). The MLL had a record aperture of 102 microns with 15170 layers. The measurements were made at 12 keV. The focal length was 9.6 mm, and the outer-most zone was 4 nm thick. MLLs with ever larger apertures are under continuous development since ever longer focal lengths, ever larger working distances, and ever increased flux in the focus are desired. A focus size of 25 nm was determined by ptychographic phase retrieval from a gold grating sample with 1 micron lines and spaces over 3.0 microns horizontal distance. The MLL was set to focus in the horizontal plane of the bending magnet beamline. A CCD with 13.0 micron pixel size positioned 1.13 m downstream of the sample was used to collect the transmitted intensity distribution. The beam incident on the MLL covered the whole 102 micron aperture in the horizontal focusing direction and 20 microns in the vertical direction. 160 iterations of the difference map algorithm were sufficient to obtain a reconstructed image of the sample. The present work highlights the utility of a bending magnet source at the APS for performing coherence-based experiments. Use of ptychography at 1-BM on MLL optics opens the way to study diffraction-limited imaging of other hard x-ray optics.

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.

Nano-focused hard X-ray probe offers a suite of analytic tools for quantitative characterization of specimen under investigation. Scanning probe operated in a multi-modality imaging mode evokes fluorescence, absorption, phase contrasts, and potentially diffraction contrast as well. Without introducing extra instrumental complexity, ptychography technique can be seamlessly integrated into the scanning probe imaging system, since it shares the same data collection procedure and even shares the exactly the same dataset with absorption- and differential-phase-contrast imaging. We will present our implementation of ptychography method for nano-Mii (Nanoscale Multimodality Imaging Instrument) at the Hard X-ray Nanoprobe (HXN) Beamline of the National Synchrotron Light Source II (NSLS-II). The ptychography reconstruction assist aligning optics to achieve diffraction-limited focus and provide quantitative images with enhanced resolution. The on-the-fly operation mode maximizes the experimental throughput, and make it timely realistic to conduct three-dimensional high-resolution imaging.

The Göttingen Instrument for Nano-Imaging with X-ray (GINIX) is a holography endstation located at the P10 coherence beamline at PETRA III, designed and operated by the University of Göttingen in close collaboration with DESY Photon science Hamburg [1-2]. GINIX is designed as a waveguide based holography experiment with a Kirkpatrick-Baez nanofocus. Its versatility has stimulated a great manifold of imaging modalities. Today, users choose the GINIX setup not only for its few nm coherent waveguide beams (e.g. for ptychography or holography), but also to carry out scanning SAXS measurements to probe local anisotropies with sub-micron real-space and even higher reciprocal space resolution. In addition, it is possible to combine different detectors for e.g. simultaneous SAXS/WAXS and fluorescence measurements [3]. We summarise our ongoing efforts to reduce vibrations in the setup, and present latest experimental results obtained with GINIX, focusing on the unique capabilities offered by its versatile and flexible design. The overview includes results from different imaging schemes such as waveguide based zoom-tomography and user examples in WAXS geometry. We show how to correlate complementary techniques like holography and scanning SAXS and present first results obtained using a new fast sample scanner for Multilayer Zone Plate imaging..

In recent years, ptychography has revolutionized x-ray microscopy in that it is able to overcome the diffraction limit of x-ray optics, pushing the spatial resolution limit down to a few nanometers. However, due to the weak interaction of x rays with matter, the detection of small features inside a sample requires a high coherent fluence on the sample, a high degree of mechanical stability, and a low background signal from the x-ray microscope. The x-ray scanning microscope PtyNAMi at PETRA III is designed for high-spatial-resolution 3D imaging with high sensitivity. The design concept is presented with a special focus on real-time metrology of the sample position during tomographic scanning microscopy.

The ID16A beamline at ESRF offers unique capabilities for X-ray nano-imaging, and currently produces the worlds brightest high energy diffraction-limited nanofocus. Such a nanoprobe was designed for quantitative characterization of the morphology and the elemental composition of specimens at both room and cryogenic temperatures. Billions of photons per second can be delivered in a diffraction-limited focus spot size down to 13 nm. Coherent X-ray imaging techniques, as magnified holographic-tomography and ptychographic-tomography, are implemented as well as X-ray fluorescence nanoscopy. We will show the latest developments in coherent and spectroscopic X-ray nanoimaging implemented at the ID16A beamline

The Hard X-ray Nanoprobe (HXN) at NSLS-II provides a nanoscale 3D multi-modality imaging capability, useful for investigating diverse material systems. The multi-modality scanning-probe imaging utilizes a variety of imaging contrasts such as fluorescence, transmission, scattering, and diffraction. Images taken simultaneously using different contrast mechanisms can provide 3D visualization of a sample, producing complementary information about the sample. Such comprehensive 3D characterizations are extremely useful in studying materials with multiple phases or complex internal structures. An important scientific problem is to investigate phase or grain boundaries of multi-component materials during or after material processing such as sintering, since re-organization of these boundaries due to annealing or phase-separation often result in profound impact on material property or functionality. However, accurate quantification of 3D elemental concentration is hampered by a well-known self-absorption problem, particularly severe for the low energy fluorescence x-rays. Correcting absorption is non-trivial and requires an iterative and three-dimensional solution. In this presentation, we will describe our approach using experimental data taken from mixed ionic ceramic membrane samples and elaborate on how accurate absorption correction led to discovery of a new material phase in this material system.

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.

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.

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.

A new scanning transmission X-ray microscope (STXM) optimized for cryo-spectro-tomography with soft X-rays has been designed, built and commissioned at Canadian Light Source (CLS) beamline 10ID1 (130-2700 eV). It is controlled via a new python-based software package, pySTXM. A liquid N2 goniometer (Gatan 630, -80° to 80°), mounted on a computer controlled (x,y,Theta) tilt stage allows for spectro-tomographic measurements at cryogenic temperatures (-180°C) which reduces radiation damage. The CLS cryo-STXM is unique among the set of soft X-ray STXMs currently installed around the world. Details of the cryo-STXM design and examples of its performance will be presented.

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.

Hard x-ray imaging methods are routinely used in two and three spatial dimensions to tackle challenging scientific questions of the 21st century, e.g. catalytic processes in energy research and bio-physical experiments on the single-cell level [1–3]. Among the most important experimental techniques are scanning SAXS to probe the local orientation of filaments and fluorescence mapping to quantify the local composition. The routinely available spot size has been reduced to few tens of nanometres; but the real-space resolution of these techniques can degrade by (i) vibration or drift, and (ii) spreading of beam damage, especially for soft condensed matter on small length scales. We have recently developed new Multilayer Zone Plate (MZP) optics for focusing hard (14 keV) and very hard (60 keV to above 100 keV) x-rays down to spot sizes presumably on 5 or 10nm scale. Here we report on recent progress on a new MZP based sample scanner, and how to tackle beam damage spread. The Eiger detector synchronized to a piezo scanner enables to scan in a 2D continuous mode fields of view larger than 20μm squared, or for high resolution down to (virtual) pixel sizes of below 2nm, in about three minutes for 255×255 points (90 seconds after further improvements). Nano-SAXS measurements with more than one million real-space pixels, each containing a full diffraction image, can be carried out in less than one hour, as we have shown using a Siemens star test pattern.

We developed a python-based fluorescence analysis package (PyXRF) at the National Synchrotron Light Source II (NSLS-II) for the X-ray fluorescence-microscopy beamlines, including Hard X-ray Nanoprobe (HXN), and Submicron Resolution X-ray Spectroscopy (SRX). This package contains a high-level fitting engine, a comprehensive commandline/ GUI design, rigorous physics calculations, and a visualization interface. PyXRF offers a method of automatically finding elements, so that users do not need to spend extra time selecting elements manually. Moreover, PyXRF provides a convenient and interactive way of adjusting fitting parameters with physical constraints. This will help us perform quantitative analysis, and find an appropriate initial guess for fitting. Furthermore, we also create an advanced mode for expert users to construct their own fitting strategies with a full control of each fitting parameter. PyXRF runs single-pixel fitting at a fast speed, which opens up the possibilities of viewing the results of fitting in real time during experiments. A convenient I/O interface was designed to obtain data directly from NSLS-II’s experimental database. PyXRF is under open-source development and designed to be an integral part of NSLS-II’s scientific computation library.

The understanding of real complex geological, environmental and geo-biological processes depends increasingly on in-depth non-invasive study of chemical composition and morphology. In this paper we used scanning hard X-ray nanoprobe techniques in order to study the elemental composition, morphology and As speciation in complex highly heterogeneous geological samples. Multivariate statistical analytical techniques, such as principal component analysis and clustering were used for data interpretation. These measurements revealed the quantitative and valance state inhomogeneity of As and its relation to the total compositional and morphological variation of the sample at sub-μm scales.