In this paper, results are presented from the characterisation of Redlen Technologies high-flux-capable Cadmium Zinc Telluride (HF-CZT) hybridised to the HEXITECMHz ASIC, a novel 1 MHz continuous X-ray imaging system. A 2 mm thick HF-CZT HEXITECMHz detector was characterised on the B16 Test Beamline at the Diamond Light Source and displayed an average FWHM of 850 eV for monochromatic X-rays of energy 20 keV. Measurements revealed a shift in the baseline of irradiated pixels that results in a movement of the entire spectrum to higher ADU values. Datasets taken to analyse the effect's dynamics showed it to be highly localised and flux-dependent, with the excess leakage current generated equivalent to per-pixel shifts of similar to 543 pA (8.68 nA mm(-2)) at a flux of 1.26x10(7) ph s(-1) mm(-2). Comparison to results from a p-type Si HEXITECMHz device indicate this `excess leakage-current' effect is unique to HF-CZT and it is hypothesised that it originates from trapping at the electrode-CZT interface and a temporary modification of the potential barrier between the CZT and metal electrode.

Hard X-ray microscopes with 20–30 nm spatial resolution ranges are an advanced tool for the inspection of materials at the nanoscale. However, the limited efficiency of the focusing optics, for example, a Fresnel zone plate (ZP) lens, can significantly reduce the power of a nanoprobe. Despite several reports on ZP lenses that focus hard X-rays with 20 nm resolution – mainly constructed by zone-doubling techniques – a systematic investigation into the limiting factors has not been reported. We report the structural effects on the focusing and imaging efficiency of 20–30 nm-resolution ZPs, employing a modified beam-propagation method. The zone width and the duty cycle (zone width/ring pitch) were optimized to achieve maximum efficiency, and a comparative analysis of the zone materials was conducted. The optimized zone structures were used in the fabrication of Pt-hydrogen silsesquioxane (HSQ) ZPs. The highest focusing efficiency of the Pt-HSQ-ZP with a resolution of 30 nm was 10% at 7 keV and >5% in the range 6–10 keV, whereas the highest efficiency of the Pt-HSQ-ZP with a resolution of 20 nm was realized at 7 keV with an efficiency of 7.6%. Optical characterization conducted at X-ray beamlines demonstrated significant enhancement of the focusing and imaging efficiency in a broader range of hard X-rays from 5 keV to 10 keV, demonstrating the potential application in hard X-ray focusing and imaging.

Objective. The radiation response of alanine is very well characterized in the MV photon energy range where it can be used to determine the dose delivered with an accuracy better than 1%, making it suitable as a secondary standard detector in cancer radiation therapy. This is not the case in the very low energy keV x-ray range where the alanine response is affected by large uncertainties and is strongly dependent on the x-ray beam energy. This motivated the study undertaken here.Approach. Alanine pellets with a nominal thickness of 0.5 mm and diameter of 5 mm were irradiated with monoenergetic x-rays at the Diamond Light Source synchrotron, to quantify their response in the 8-20 keV range relative to60Co radiation. The absorbed dose to graphite was measured with a small portable graphite calorimeter, and the DOSRZnrc code in the EGSnrc Monte Carlo package was used to calculate conversion factors between the measured dose to graphite and the absorbed dose to water delivered to the alanine pellets. GafChromic EBT3 films were used to measure the beam profile for modelling in the MC simulations.Main results. The relative responses measured in this energy range were found to range from 0.616 to 0.643, with a combined relative expanded uncertainty of 3.4%-3.5% (k= 2), where the majority of the uncertainty originated from the uncertainty in the alanine readout, due to the small size of the pellets used.Significance. The measured values were in good agreement with previously published data in the overlapping region of x-ray energies, while this work extended the dataset to lower energies. By measuring the response to monoenergetic x-rays, the response to a more complex broad-spectrum x-ray source can be inferred if the spectrum is known, meaning that this work supports the establishment of alanine as a secondary standard dosimeter for low-energy x-ray sources.

Spectroscopic X-ray imaging techniques including Compton X-ray Imaging, X-ray Fluorescence Imaging and Hyperspectral X-ray Tomography require energy-resolving detectors capable of operating at high incident X-ray fluxes to make time resolved measurements. HEXITECMHz, operates at a continuous 1 MHz frame rate and can make fully spectroscopic measurements at >10(6) ph s(-1) mm(-2). This is enabled by an integrating Front End, in-pixel digitisation and high-speed serialisers. A 300 mu m thick p-type Si HEXITECMHz detector was characterised on the B16 Test Beamline at the Diamond Light Source and are the first measurements taken at a 1 MHz frame rate. At 10 keV and 15 keV) the device displayed average FWHM of 656 eV and 682 eV respectively, with minimal changes in spectroscopic performance over similar to 8 h. Analysis of charge-sharing events show low charge loss and a linear energy-signal response. Higher-flux measurements illustrated the capability of the ASIC to operate as a photon-counting device.

The HEXITEC MHz ASIC is the next generation of the STFC's High Energy X-ray Imaging Technology (HEXITEC). With a ×100 increase in the camera frame rate to 1 MHz, the new ASIC is capable of delivering fully spectroscopic X-ray imaging at photon fluxes of 2×10 6 photons s -1 mm -2 . The improved flux capability ensures the relevance of the technology at a new generation of difraction-limited storage ring (DLSR) synchrotrons as well as enabeling dynamic spectroscopic imaging with sub-keV energy resolution to be carried out on millisecond timescales. In this paper preliminary results from X-ray testing of a 0.3 mm thick p-type Si sensor and 2.0 mm thick HF-CdZnTe sensor at the Diamond Light Source Synchrotron are presented for the first time. Each module consists of 80 × 80 pixels on a 250 μm pixel pitch operated at a temperature of 20°C and a frame rate of 1 MHz. For these preliminary measurements, testing was completed using a prototype test system which limited readout to a portion of the 1 MHz output sampled over an SPI test interface at ∼50 Hz. Despite this limitation these measurements allow the spectroscopic performance of the ASIC to be characterised ahead of the full DAQ system. The prototype detectors were characterised using monochromatic X-rays with energies 12–35 keV at fluxes of (0.6 – 2.5) × 10 6 photons s -1 mm -2 . At an X-ray energy of 12 keV, the energy resolution of the p-type Si and HF-CdZnTe detectors were measured to be 1.0 keV and 1.1 keV respectively. At the higher energies of 20 keV and 35 keV the energy resolution in the HF-CdZnTe was measured to be 1.2 keV and 1.4 keV respectively.

Visible light optical elements such as lenses and mirrors have counterparts for X-rays. In the visible regime, a variable focusing power can be achieved by an Alvarez lens which consists of a pair of inline planar refractors with a cubic thickness profile. When the two refractors are laterally displaced in opposite directions, the parabolic component of the wavefront is changed resulting in a longitudinal displacement of the focus. This paper reports an implementation of this concept for X-rays using two planar microfabricated refractive elements. The Alvarez X-ray lens can vary the focal distance of an elliptical X-ray mirror or a planar compound X-ray lens over several millimetres. The study presents the first demonstration of an Alvarez X-ray lens which adaptively corrects defocus and astigmatism aberrations of X-ray optics. In addition, the Alvarez X-ray lens eliminates coma aberration in an elliptical mirror, to the lowest order, when combining the lens with an adjustment of the pitch angle of the mirror.

Confocal micro-X-ray fluorescence analysis (CMXRF), using polycapillary optics, is a powerful technique for the non-destructive investigation of the three-dimensional elemental distribution of samples from many different research areas, including biology, cultural heritage and material science. To solve the problem of the quantitative interpretation of CMXRF measurements, voxTrace introduces a new fundamental Monte-Carlo ray-tracing approach, to simulate the measured spectra. This enables the consideration of effects such as secondary excitation, elastic and inelastic scattering. Furthermore, measurements with step sizes between measurement points smaller than the average confocal volume can be interpreted without complicated sample reconstruction algorithms. Solving this problem of high computational effort, in reasonable timescales, is made feasible by the effective use of graphics processing units (GPU) with CUDA.

Extrusion based additive manufacturing (AM) has gradually became a dominant technology for the fabrication of complex-designed thermoplastic polymers that require higher level of control over the morphological and mechanical properties. Internal crystal structure formed during the additive process can present significant impacts on the mechanical properties of the individual fibres, as well as the whole structure. To address the limited current understanding related to the polymer crystal structure formation during the extrusion based AM processes, a novel in situ synchrotron X-ray diffraction configuration has been developed. Experimental results obtained from different AM process parameters reveal strong evidence that temperature has a more dominant influence on the crystal microstructure compared with deposition velocity, and lower extrusion temperature just above the melting temperature provide better crystallisation conditions and thus lead to enhanced mechanical properties. This research opened novel prospects for enhancing polymer additive manufacturing, and revealed a new approach to engineering mechanically hierarchical structures.

Aberrations introduced during fabrication degrade the performance of X-ray optics and their ability to achieve diffraction limited focusing. Corrective optics can counteract these errors by introducing wavefront perturbations prior to the optic which cancel out the distortions. Here we demonstrate two-dimensional wavefront correction of an aberrated Kirkpatrick-Baez mirror pair using adaptable refractive structures. The resulting two-dimensional wavefront is measured using hard X-ray ptychography to recover the complex probe wavefield with high spatial resolution and model the optical performance under coherent conditions. The optical performance including the beam caustic, focal profile and wavefront error is examined before and after correction with both mirrors found to be diffraction limited after correcting. The results will be applicable to a wide variety of high numerical aperture X-ray optics aiming to achieve diffraction limited focussing using low emittance sources.

Speckle-based at-wavelength metrology techniques now play an important role in X-ray wavefront measurements. However, for reflective X-ray optics, the majority of existing speckle-based methods fail to provide reliable 2D information about the optical surface being characterized. Compared with the 1D information typically output from speckled-based methods, a 2D map is more informative for understanding the overall quality of the optic being tested. In this paper, we propose a method for in situ 2D absolute metrology of weakly focusing X-ray mirrors. Importantly, the angular misalignment of the mirror can be easily corrected with the proposed 2D processing procedure. We hope the speckle pattern data processing method presented here will help to extend this technique to wider applications in the synchrotron radiation and X-ray free-electron laser communities.

Advances in accelerator technologies have enabled the continuous development of synchrotron radiation and X-ray free electron laser (XFEL) sources. At the same time, it has been critical to perform in-situ wavefront sensing to aid delivery of high-quality X-ray beams to the end users of these facilities. The speckle-based scanning technique has obtained popularity due to its high spatial resolution and superior sensitivity compared to other wavefront sensing methods. However, these advantages often come at the expense of longer data acquisition times since multiple images have to be collected to derive the necessary wavefront information. Whereas initial speckle tracking techniques could obtain wavefront information relatively quickly, the installation of additional hardware was routinely required to do so. Here, we propose a novel speckle-based approach, termed Alternating Speckle Tracking (AST), to perform fast wavefront sensing within a conventional beamline setup. The wavefront information derived from the new technique has proven to be valuable for many applications that require temporal resolution. Importantly, both horizontal and vertical wavefront information can be simultaneously derived by moving the speckle generator along the diagonal direction. We expect this method will be widely used by the synchrotron radiation and XFEL community in the future.

Ptychography is a scanning coherent diffraction imaging technique that provides high-resolution imaging and complete spatial information of the complex probe and object transmission function. The wavefront error caused by aberrated optics has previously been recovered using ptychography when a highly coherent source is used, but has not been demonstrated with partial coherence due to the multi-modal probe required. Here, we demonstrate that partial coherence can be accounted for in ptychographic reconstructions using the multi-modal approach and assuming that decoherence arises from either the probe or the object. This equivalence recovers coherent (or single state) reconstructions of both the probe and the object even in the presence of partial coherence. We demonstrate this experimentally by using hard x-ray ptychography with a partially coherent source to image a Siemens star test object and to also recover the wavefront error from an aberrated beryllium compound refractive lens. The source properties and resolving capabilities are analyzed, and the wavefront error results are compared with another at-wavelength metrology technique. Our work demonstrates the capability of ptychography to provide high-resolution imaging and optics characterization even in the presence of partial coherence.

27 Technical RepoRT Refractive Optics for Modifying X-Ray Wavefronts DaviD LaunDy,1 Thomas moxham,1,2 vishaL Dhamgaye,3 hossein KhosroabaDi,1 oLiver Fox,1 anD KawaL sawhney1 1Diamond Light Source, Didcot, UK 2Department of Engineering Science, University of Oxford, Oxford, UK 3Synchrotron Utilisation Section, Raja Ramanna Centre for Advanced Technology, Indore, India Introduction Diamond Light Source (DLS) is the UK synchrotron light source with over 30 beamlines, many operating in the X-ray part of the spectrum. The facility has an Optics Group with active research in areas such as modelling of beamlines, development of X-ray optics, and X-ray beam characterization using techniques such as X-ray wavefront measurements. Many optics developments have benefited from using the DLS test beamline, B16 [1], a versatile dipole magnet beamline, for developing techniques and for optics test experiments. A recent project has been the development of microfabricated refractive structures for modifying the X-ray wavefront to extend and improve the performance of beamline optics. At a synchrotron radiation source, X-radiation is emitted by relativistic electrons in the storage ring passing through regions with high magnetic fields. The electromagnetic (em) radiation field emitted by different electrons in the source is uncorrelated and if the spatial distribution of the source is sufficiently large, perfect X-ray focusing optics will produce a direct image of the electrons in the source. With the latest generation of SR facilities—the so-called 4th generation—the electron spatial distribution at the source is small (of order 10 μm rms in both horizontal and vertical directions) and the radiation field at beamline optics becomes highly correlated in the transverse direction. At a focal plane, where these correlated fields overlap, the intensity distribution is determined by interference and for "ideal" focusing optics, interference at the center of the focus is entirely constructive and the focus size is determined by the diffraction limit. In this highly correlated regime, a useful concept is that of the wavefront of the em field [2]. The wavefront is a surface given by the locus of the point at which the phase of the em field is constant. For slowly varying field amplitude and a wavefront that is locally smooth, the wavefront propagates along its normal direction. The wavefront error can be defined as the displacement along the wavefront normal of the actual from the ideal wavefront. In Cartesian coordinates x y ( , , ) z with the z axis pointing along the optical axis, the wavefront error can be expressed as a function of the two transverse coordinates w x y ( , ) . Wavefront error is generated as the em wave encounters optical elements in the beamline such as, for example, monochromators, X-ray mirrors, refractive lenses, and X-ray windows and is given by the variation in the accumulated X-ray path-length. In the case of reflecting optics, the wavefront error is directly related to the figure error h x y ( , ) as shown in Figure 1, by θ = w x y h x y x y ( , ) 2 ( , ) sin( ( , )) (1) where θ x y ( , ) is the local incidence angle on the mirror. For refractive optics, the wavefront error is given by the path-length change δ = w x y E t x y ( , ) ( ) ( , ) where δ E ( ) is the X-ray energy-dependent real part decrement of the refractive index and t x y ( , ) is the error in the thickness profile of the refractor. For a constant amplitude monochromatic beam, the complex em field can be obtained directly from the wavefront error up to a constant phase factor by π λ = i w x y E E 0 exp[ 2 ( , ) / ] where λ is the wavelength of the radiation. The field obtained can be propagated to

Experiments involving the irradiation of water contained within magnesium hydroxide and alumina nanoparticle sludges were conducted and culminated in observations of an increased yield of molecular hydrogen when compared to the yield from the irradiation of bulk water. We show that there is a relationship linking this increased yield to the direct nanoscale ionization mechanism in the nanoparticles, indicating that electron emission from the nanoparticles drives new radiative pathways in the water. Because the chemical changes in these sludges are introduced by irradiation only, we have a genuinely unstirred system. This feature allows us to determine the diffusivity of the dissolved gas. Using the measured gas production rate, we have developed a method for modelling when hydrogen bubble formation will occur within the nanoparticle sludges. This model facilitates the determination of a consistent radiolytic consumption rate coinciding with the observations of bubble formation. Thus, we demonstrate a nanoscale radiation effect directly influencing the formation of molecular hydrogen.

Germanium micro-strip sensors were selected as the sensor technology to take data in energy dispersive X-ray spectroscopy experiments at the Extremely Brilliant Source (EBS) in Grenoble (FR). It is important for this experimental technique to use sensors with a large uniform area and a fine pitch. The former determines the range of energy detectable with a single sensor. The latter improves spectral resolution. A high stopping power is also important to perform studies with hard X-rays. The device under test in this measurement was a germanium micro-strip sensor made of 1024 strips with 50 mu m pitch. The bulk was 1.5 mm thick. The sensor was assembled into a prototype cryostat part of the XH detector system. The device was tested at the B16 beamline at the Diamond Light Source (DLS) in Didcot (UK). The objective of the test-beam was to characterise charge-sharing between strips. In fact, this effect limits the spectral resolution of the device. To carry out this test, the sensor was scanned over a subset of strips with micro-focused X-rays under different settings. These were beam energy and intensity, sensor temperature and bias voltage. Results are presented in this paper. It was measured that the full width half maximum of the charge-sharing profile across different strips was similar to 90 mu m for settings which were indicative of the experimental conditions at the EBS. This was a signal current per unit area on the sensor of similar to 1.66x10(-8) A/mu m(2), a bias voltage of -180 V and a temperature of -159 degrees C.

A newly supplied 80 x 80 chromium compensated GaAs sensor with a matrix of 80 x 80 pixels on a 250 mu m pixel pitch has been characterised utilising microbeam mapping techniques at the Diamond Light Source. The GaAs:Cr sensor was mounted to a HEXITEC DAQ system before raster scanning an X-ray beam with area 25 x 25 mu m(2) in steps of 25 mu m, providing sub-pixel resolution spectroscopic imaging. Scans were performed with incident X-ray energies ranging from 12 to 45 keV. Following processing of the data in MatLab 2019b an analysis of defects previously observed in etched GaAs wafers occurred. Findings indicate the presence of regions with reduced charge collection efficiency where up to 88% of incident events show significant charge loss, and changing charge carrier lifetimes across the sensor.

Cadmium-zinc-telluride (CZT) pixel detectors represent a consolidated choice for the development of room-temperature spectroscopic X-ray imagers, finding important applications in medical imaging, often as detection modules of a variety of new SPECT and CT systems. Detectors with 3-5 mm thicknesses are able to efficiently detect X-rays up to 140 keV giving reasonable room-temperature energy resolution. In this work, the room-temperature performance of 3 mm-thick CZT pixel detectors, recently developed at IMEM/CNR of Parma (Italy), is presented. Sub-millimetre detector arrays with pixel pitch less than 500 µm were fabricated. The detectors are characterized by good room-temperature performance even at high bias voltage operation (6000 V cm-1), with energy resolutions (FWHM) of 3% (1.8 keV) and 1.6% (2 keV) at 59.5 keV and 122.1 keV, respectively. Charge-sharing investigations were performed with both uncollimated and collimated synchrotron X-ray beams with particular attention to recovering the charge losses at the inter-pixel gap region. High rate measurements demonstrated the absence of high-flux radiation-induced polarization phenomena up to 25 × 106 photons mm-2 s-1.

Ptychography is a scanning coherent diffraction imaging technique which provides high resolution imaging and complete spatial information of the complex electric field probe and sample transmission function. Its ability to accurately determine the illumination probe has led to its use at modern synchrotrons and free-electron lasers as a wavefront-sensing technique for optics alignment, monitoring and correction. Recent developments in the ptychography reconstruction process now incorporate a modal decomposition of the illuminating probe and relax the restriction of using sources with high spatial coherence. In this article a practical implementation of hard X-ray ptychography from a partially coherent X-ray source with a large number of modes is demonstrated experimentally. A strongly diffracting Siemens star test sample is imaged using the focused beam produced by either a Fresnel zone plate or beryllium compound refractive lens. The recovered probe from each optic is back propagated in order to plot the beam caustic and determine the precise focal size and position. The power distribution of the reconstructed probe modes also allows the quantification of the beams coherence and is compared with the values predicted by a Gaussian-Schell model and the optics exit intensity.

Gadolinium-based contrast agents (GBCAs) are frequently used in patients undergoing magnetic resonance imaging. In GBCAs gadolinium (Gd) is present in a bound chelated form. Gadolinium is a rare-earth element, which is normally not present in human body. Though the blood elimination half-life of contrast agents is about 90 minutes, recent studies demonstrated that some tissues retain gadolinium, which might further pose a health threat due to toxic effects of free gadolinium. It is known that the bone tissue can serve as a gadolinium depot, but so far only bulk measurements were performed. Here we present a summary of experiments in which for the first time we mapped gadolinium in bone biopsy from a male patient with idiopathic osteoporosis (without indication of renal impairment), who received MRI 8 months prior to biopsy. In our studies performed by means of synchrotron radiation induced micro- and submicro-X-ray fluorescence spectroscopy (SR-XRF), gadolinium was detected in human cortical bone tissue. The distribution of gadolinium displays a specific accumulation pattern. Correlation of elemental maps obtained at ANKA synchrotron with qBEI images (quantitative backscattered electron imaging) allowed assignment of Gd structures to the histological bone structures. Follow-up beamtimes at ESRF and Diamond Light Source using submicro-SR-XRF allowed resolving thin Gd structures in cortical bone, as well as correlating them with calcium and zinc.