We report about the experimental work related to hierarchical structures at the Diamond I13L beamlines. The I13-2 Imaging and I13-1 Coherence beamlines provide imaging with micro- and nano-resolution. The Diamond II upgrade for the synchrotron source and the OCTOPI upgrade for I13L provide new opportunities for expanding the existing scientific areas in multiscale and operando imaging. We describe the scientific research benefitting from the instrumental upgrade. Comparable recording times across all length scales will enable hierarchical operando imaging. With the implementation of automated high-throughput data acquisition and analysis, large numbers of samples will be analyzed.
We present the most recent advances in fast X-ray grating interferometer and their applications. A dedicated setup for rapid scanning with a single grating and using filtered broadband illumination of an undulator source has been implemented. With this setup tomographic scans can be achieved within minutes. Larger number of samples can be measured and chemical processes can be studied. Improvements in the data processing technique will be presented. We will also describe the new capabilities and applications.
We report about multiscale tomography with high throughput at the Diamond beamline I13L. The beamline has the purpose of multi-scale and operando imaging and consists of two independent branchlines operating in real and reciprocal space. The imaging branch -called Diamond-Manchester branchline- hosts micro-tomography, grating interferometry and a full-field microscope. For rapid recording a broad spectrum of the undulator radiation is used either with band-passing the light with a combination of a filter and a deflecting mirror or using a multilayer monochromator. For all the methods similar recording times can be achieved, with typical scanning times of some minutes and covering the resolution range from microns to the 100nm range. Most recently a robot arm has been installed to increase the throughput to 300 samples per day. The system is now implemented for user operation in remote operation mode for the micro-tomography setup and can be expanded to the two other experiments. The instrumental capabilities are applied on various topics such as the study of biodiversity of insects or the structural variations of electrode materials in batteries. Fast recording with dedicated sample environments (not using the sample changing robot) enables operando studies in many areas, the charging/discharging cycles on batteries, the degradation of teeth enamel under various conditions or loading brine sandstone mixtures with CO2, to name some examples. For imaging with highest spatial resolution we managed to improve significantly the recording speed of ptycho-tomography, which is now in the order of hours and will be reduced further. We demonstrated in the past 2-D recording with 10kHz and expand the instrumental capability with specific hardware dependent triggering and scanning schemes. We expand the research program for multi-scale imaging across both branchlines (imaging and coherence branchlines) with first studies such as batteries, brain research, concrete.
We report about our current capabilities and future plans in multi-scale imaging with high recording speed. For micro-tomographic imaging an automated system is used measuring up to 300 samples per day. For sub-micron and nano measurements the so-called polychromatic ‘pink beam’ is employed. The larger energy bandwidth compared to monochromatic beam permits recording times similar to microtomography. For highest resolution namely ptychography the acquisition time for tomographic scans is currently in the order of hours and below an hour in the near future. The current multi-scale science and the scientific perspective with the Diamond beamline I13L upgrade will be presented.
X-ray Grating Talbot Interferometer (XGTI) is already routinely used for quantitative phase contrast imaging of soft tissue samples. XGTI can be realized using various measurement techniques, depending on the X-ray source used, the required spatial resolution and the speed of acquisition. The phase-stepping measurement technique, which is commonly used for XGTI data acquisition, needs multiple acquisitions for a single projection. For fast imaging the Moiré technique, a single-shot technique, is often preferred. However, it requires two gratings which increases the dose on the sample. We have therefore examined the Spatial Harmonic Imaging (SHI) technique which is low-dose and single-shot, using the I13-2 Diamond-Manchester Beamline at Diamond Light Source (DLS). The DLS I13-2 beamline is equipped with a Double Crystal Monochromator (DCM) and a Multi-Layer Monochromator (MLM) to deliver monochromatic beam, which work at the energy bandwidths (ΔE/E) of 10-4 and 10-2, respectively. However, the disadvantage of using these monochromators, especially for fast imaging, is loss of X-ray flux. It has already been shown that XGTI can work with an energy bandwidth (ΔE/E) of 10-1. Our aim is to develop a single phase grating interferometer with pink beam from an undulator source, with X-ray mirror optics and multiple absorption filters, to obtain maximum possible flux with sufficient coherence and monochromaticity. We demonstrate performance with optimized beamline parameters for a photon energy of 15 keV with some demonstrative image reconstructions.
The DIAMOND beamline I13L is dedicated to multi-scale and multi-modal imaging in real and reciprocal space. The beamline consists of two independently operating experimental stations, located at a distance of more than 200 m from the source. The Imaging Branch performs micro-tomography with in-line phase contrast in the 6-30 keV energy range. In addition, a grating interferometry setup and a full-field microscope for nano-tomography are currently implemented. Other techniques providing high-resolution three-dimensional information, in particular coherent X-ray diffraction, are hosted on the Coherence Branch. All imaging methods are tested to operate with large energy bandwidths and therefore shorter exposure times. To this end, two options are currently used: the so-called ‘pink-beam’ mode using a reflecting mirror and X-ray filters and monochromatic mode using a multilayer monochromator. The operation mode enables science for in-situ and operando studies across a wide range of scientific areas.
The Diamond Beamline I13L is dedicated to micro- and nano- imaging, with two independently operating branchlines. The imaging branch preforms imaging in real space, with In-line phase contrast imaging and grating interferometry at micrometre resolution and full-field transmission microscopy up to 50nm spatial resolution. Highest spatial resolution is achieved on the coherence branchline, where diffraction imaging methods such as Ptychography and Bragg-CDI are performed. The article provides an update about the experimental capabilities at the beamline with an emphasis on the rapidly evolving ptychography capabilities. The latter has evolved to an user-friendly method with non-expert users able to explore their science without any specific a-priory knowledge.
X-ray grating interferometry (XGI) is a phase-contrast imaging technique that allows for a quantitative measurement of the refractive index with high density resolution in a model-independent manner—i.e. without a priori knowledge of the specimen composition. However, the retrieval of the X-ray wavefront phase shift relies on the accurate measurement of the interference pattern phase shift, making XGI vulnerable to phase wrapping when the interference pattern phase shift, related to the derivative of the wavefront phase shift, is large. Standard procedure for avoiding phase wrapping involves submerging the specimen in a water bath to reduce the mismatch of the index of refraction at the boundaries, but this requires a top-down rotation stage and is susceptible to gas bubble formation inside the water bath. Our team has presented an algorithm to remove phase wrapping artifacts for cylindrically shaped specimens that is applied to the phase-retrieved sinogram. This algorithm models and replaces phase-wrapped data to prevent the spread of “cupping” artifacts due to the integration of the differential phase during reconstruction. We give a criterion for selecting the modeling parameters so that the resulting measurement of the index of refraction matches the results of measurements without phase wrapping. We also apply this technique to cases where phase wrapping occurs at multiple interfaces. This algorithm allows for XGI measurements without a water bath and top-down rotation stage at synchrotron and laboratory facilities, especially as sensitivity increases.
Preserving the coherence and wavefront of a diffraction limited x-ray beam from the source to the experiment poses stringent quality requirements on the production processes for X-ray optics. In the near future this will require on-line and in-situ at-wavelength metrology for both, free electron lasers and diffraction limited storage rings. A compact and easy to move X-ray grating interferometry (XGI) setup has been implemented by the Beamline Optics Group at PSI in order to characterize x-ray optical components by determining the aberrations from reconstructing the x-ray wavefront. The XGI setup was configured for measurements in the moire mode and tested with focusing optic at Swiss Light Source, Diamond Light Source and LCLS. In this paper measurements on a bendable toroidal mirror, a zone plate, a single and a stack of beryllium compound refractive lenses (CRL) are presented. From these measurements the focal position and quality of the beam spot in terms of wavefront distortions are determined by analysing the phase-signal obtained from the XGI measurement. In addition, using a bendable toroidal mirror, we directly compare radius of curvature measurements obtained from XGI data with data from a long-trace profilometer, and compare the CRL wavefront distortions with data obtained by ptychography.
The Diamond Beamline I13L is dedicated to imaging on the micro- and nano-lengthsale, operating in the energy range
between 6 and 30keV. For this purpose two independently operating branchlines and endstations have been built. The
imaging branch is fully operational for micro-tomography and in-line phase contrast imaging with micrometre
resolution. Grating interferometry is currently implemented, adding the capability of measuring phase and small-angle
information. For tomography with increased resolution a full-field microscope providing 50nm spatial resolution with a
field of view of 100μm is being tested. The instrument provides a large working distance between optics and sample to
adapt a wide range of customised sample environments. On the coherence branch coherent diffraction imaging
techniques such as ptychography, coherent X-ray diffraction (CXRD) are currently developed for three dimensional
imaging with the highest resolution.
The imaging branch is operated in collaboration with Manchester University, called therefore the Diamond-Manchester
Branchline. The scientific applications cover a large area including bio-medicine, materials science, chemistry geology
and more. The present paper provides an overview about the current status of the beamline and the science addressed.
The phase-stepping (PS) mode of X-ray Grating Talbot interferometer (XGTI) data processing technique can yield
high-spatial resolution images, albeit with lower throughput since each projection of a tomogram requires at least five
phase-stepping images. To overcome this problem, we can use a setup with only a single phase grating in combination
with a high-resolution detector system and a Spatial Harmonic Imaging (SHI) technique. The latter technique makes use
of the fact that a Talbot interferogram consists of carrier frequency spectrum of the grating overlapping with the sample
spectrum and by Fourier transforming the interferogram we can separate the two. The disadvantage of this is that the
spatial resolution is inferior. In this manuscript we will compare these two single grating data processing techniques
using a single data set measured with mouse embryo heart and discuss advantages and disadvantages of each technique.
These two techniques can be used as complementary; one for high resolution, and the other for high-speed 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
The initial result of using a single 2-D checkerboard phase-grating Talbot interferometer as a feed-back loop sensor
element of an adaptive x-ray mirror system is reported. The test was performed by measuring the surface profile of a
deformable Pt coated Silicon mirror at five different actuation states. The reflected beam was detected at the fractional
Talbot distance of a π/2 phase grating. The measured interferograms were de-convolved using the spatial harmonic
imaging technique to extract the phase and amplitude of the reflected wavefront. The wavefront was then propagated to
the mirror center to retrieve the surface profile of the mirror. The activation of a single actuator was easily detected from
the reconstructed surface profile of the mirror. The presented results indicate that the single phase-grating x-ray Talbot
interferometer is capable of sensing nano-meter scale profile changes of an adaptive mirror.
Kirkpatrick-Baez (K-B) mirrors [1] are sophisticated x-ray micro- and nano-focusing tools for synchrotron radiation applications. A prototype of a modular x-ray K-B mirror mount system has been designed and tested at an optics testing beamline, 1-BM at the Advanced Photon Source (APS), Argonne National Laboratory (ANL). This compact, costeffective modular mirror mount system is designed to meet challenging mechanical and optical specifications for producing high positioning resolution and stability for various scientific applications with focused hard x-ray beams down to the 100-nanometer scale. The optomechanical design of the modular x-ray K-B mirror mount system as well as the preliminary test results of its precision positioning performance are presented in this paper.
Here we report on the effort to develop a hard x-ray grating interferometry technique for application to hard x-ray optics
and wavefront characterization at the Advanced Photon Source (APS), Argonne National Laboratory, USA. We will
mention the motivation for developing an x-ray interferometer at the APS and discuss the design of the interferometer.
We will also describe the efforts in fabricating 2-D gratings and a new type of grating having nanometer periods for
high-energy x-ray applications. The preliminary results obtained using x-ray Talbot interferometers built at APS, using a
broadband (pink) beam and a monochromatic beam demonstrate the importance of this tool as a metrology instrument
for optics and beam wavefront diagnostics.
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