Hard X-ray imaging and tomography at the Biomedical Imaging and Therapy beamlines of Canadian Light Source.

The Biomedical Imaging and Therapy facility of the Canadian Light Source comprises two beamlines, which together cover a wide X-ray energy range from 13 keV up to 140 keV. The beamlines were designed with a focus on synchrotron applications in preclinical imaging and veterinary science as well as microbeam radiation therapy. While these remain a major part of the activities of both beamlines, a number of recent upgrades have enhanced the versatility and performance of the beamlines, particularly for high-resolution microtomography experiments. As a result, the user community has been quickly expanding to include researchers in advanced materials, batteries, fuel cells, agriculture, and environmental studies. This article summarizes the beam properties, describes the endstations together with the detector pool, and presents several application cases of the various X-ray imaging techniques available to users.

Hard X-ray operation of X-ray gas monitors at the European XFEL.

X-ray gas monitors (XGMs) are operated at the European XFEL for non-invasive single-shot pulse energy measurements and average beam-position monitoring. The underlying measurement principle is the photo-ionization of rare gas atoms at low gas pressures and the detection of the photo-ions and photo-electrons created. These are essential for tuning and sustaining self-amplified spontaneous emission (SASE) operation, machine radiation safety, and sorting single-shot experimental data according to pulse energy. In this paper, the first results from XGM operation at photon energies up to 30 keV are presented, which are far beyond the original specification of this device. Here, the Huge Aperture MultiPlier (HAMP) is used for single-shot pulse energy measurements since the standard X-ray gas monitor detectors (XGMDs) do not provide a sufficient signal-to-noise ratio, even at the highest operating gas pressures. A single-shot correlation coefficient of 0.98 is measured between consecutive XGMs operated with HAMP, which is as good as measuring with the standard XGMD detectors. An intra-train non-linearity of the HAMP signal is discovered, and operation parameters to mitigate this effect are studied. The upper repetition rate limit of HAMP operation at 2.25 MHz is also determined. Finally, the possibilities and limits for future XGM operation at photon energies up to 50 keV are discussed.

The concept for hard X-ray beamline optics at SLS 2.0.

In the scope of the latest upgrade of the Swiss Light Source, five hard X-ray beamlines will be constructed or rebuilt. To use synergies between these beamline projects, a concept is developed here for hard X-ray beamlines that is tailored to the new storage ring. Herein, this concept is described from the source, via the front end, to the beamline optics. The latter will be outlined in detail, including a new and modular concept for hard X-ray monochromators, focusing optics and heat-load management. With a simple, easy-to-operate and robust beamline design, the new beamlines will greatly profit from the increased brilliance of the new storage ring. The performance increase is up to four orders of magnitude, while the beamline concept allows for the broad application of experimental techniques, from propagation-based methods, such as phase-contrast tomography, to imaging techniques with nanometre resolution. At the same time, spectroscopy experiments are possible as well as high-performance serial X-ray crystallography.

Advanced spectroscopic investigation of colour centres in LiF crystals irradiated with monochromatic hard x-rays.

Nominally-pure lithium fluoride (LiF) crystals were irradiated with monochromatic hard x-rays of energy 5, 7, 9 and 12 keV at the METROLOGIE beamline of the SOLEIL synchrotron facility, in order to understand the role of the selected x-ray energy on their visible photoluminescence (PL) response, which is used for high spatial resolution 2D x-ray imaging detectors characterized by a wide dynamic range. At the energies of 7 and 12 keV the irradiations were performed at five different doses corresponding to five uniformly irradiated areas, while at 5 and 9 keV only two irradiations at two different doses were carried out. The doses were planned in a range between 4 and 1.4 × 103Gy (10.5 mJ cm-3to 3.7 J cm-3), depending on the x-ray energy. After irradiation at the energies of 7 and 12 keV, the spectrally-integrated visible PL intensity of the F2and F3+colour centres (CCs) generated in the LiF crystals, carefully measured by fluorescence microscopy under blue excitation, exhibits a linear dependence on the irradiation dose in the investigated dose range. This linear behaviour was confirmed by the optical absorption spectra of the irradiated spots, which shows a similar linear behaviour for both the F2and F3+CCs, as derived from their overlapping absorption band at around 450 nm. At the highest x-ray energy, the average concentrations of the radiation-induced F, F2and F3+CCs were also estimated. The volume distributions of F2defects in the crystals irradiated with 5 and 9 keV x-rays were reconstructed in 3D by measuring their PL signal using a confocal laser scanning microscope operating in fluorescence mode. On-going investigations are focusing on the results obtained through thisz-scanning technique to explore the potential impact of absorption effects at the excitation laser wavelength.

Resonant inelastic X-ray scattering endstation at the 1C beamline of Pohang Light Source II.

An endstation for resonant inelastic X-ray scattering (RIXS), dedicated to operations in the hard X-ray regime, has been constructed at the 1C beamline of Pohang Light Source II. At the Ir L3-edge, a total energy resolution of 34.2 meV was achieved, close to the theoretical estimation of 34.0 meV, which considers factors such as the incident energy bandpass, intrinsic analyzer resolution, geometrical broadening of the spectrometer, finite beam-size effect and Johann aberration. The performance of the RIXS instrument is demonstrated by measuring the RIXS spectra of Sr2IrO4. The endstation can be easily reconfigured to measure energy-integrated intensities with very low background for diffuse scattering and diffraction experiments.

Design and modeling of a Laue lens for radiation therapy with hard x-ray photons.

We have designed and modeled a novel optical system composed of a Laue lens coupled to an x-ray tube that produces a focused beam in an energy range near 100 keV (λ= 12.4 picometer). One application of this system is radiation therapy where it could enable treatment units that are considerably simpler and lower in cost than present technologies relying on linear accelerators. The Laue lens is made of Silicon Laue components which exploit the silicon pore optics technology. The lens concentrates photons to a small region thus allowing high dose rates at the focal area with very much lower dose rates at the skin and superficial regions. Monte Carlo simulations with Geant4 indicate a dose deposition rate of 0.2 Gy min-1in a cylindrical volume of 0.7 mm diameter and 10 mm length, and a dose ratio of 72 at the surface (skin) compared to the focus placed 10 cm within a water phantom. Work is ongoing to newer generation crystal technologies to increase dose rate.

Hard X-ray nanoprobe scanner.

X-ray scientists are continually striving to improve the quality of X-ray microscopy, due to the fact that the information obtained from X-ray microscopy of materials can be complementary to that obtained from optical and electron microscopes. In contrast to the ease with which one can deflect electron beams, the relative difficulty to deflect X-ray has constrained the development of scanning X-ray microscopes (SXMs) based on a scan of an X-ray small probe. This restriction has caused severe complications that hinder progress toward achieving ultimate resolution. Here, a simple and innovative method for constructing an SXM equipped with a nanoprobe scanner is proposed. The nanoprobe scanner combines X-ray prisms and advanced Kirkpatrick-Baez focusing mirrors. By rotating the prisms on the order of degrees, X-ray probe scanning with single-nanometre accuracy can be easily achieved. The validity of the concept was verified by acquiring an SXM image of a test pattern at a photon energy of 10 keV, where 50 nm line-and-space structures were resolved. This method is readily applicable to an SXM with a single-nanometre resolution and will assist effective utilization of increasing brightness of fourth-generation synchrotron radiation sources.

A new imaging technology based on Compton X-ray scattering.

A feasible implementation of a novel X-ray detector for highly energetic X-ray photons with a large solid angle coverage, optimal for the detection of Compton X-ray scattered photons, is described. The device consists of a 20 cm-thick sensitive volume filled with xenon at atmospheric pressure. When the Compton-scattered photons interact with the xenon, the released photoelectrons create clouds of secondary ionization, which are imaged using the electroluminescence produced in a custom-made multi-hole acrylic structure. Photon-by-photon counting can be achieved by processing the resulting image, taken in a continuous readout mode. Based on Geant4 simulations, by considering a realistic detector design and response, it is shown that photon rates up to at least 1011 photons s-1 on-sample (5 µm water-equivalent cell) can be processed, limited by the spatial diffusion of the photoelectrons in the gas. Illustratively, if making use of the Rose criterion and assuming the dose partitioning theorem, it is shown how such a detector would allow obtaining 3D images of 5 µm-size unstained cells in their native environment in about 24 h, with a resolution of 36 nm.

Impact of real mirror profiles inside a split-and-delay unit on the spatial intensity profile in pump/probe experiments at the European XFEL.

For the High-Energy-Density (HED) beamline at the SASE2 undulator of the European XFEL, a hard X-ray split-and-delay unit (SDU) has been built enabling time-resolved pump/probe experiments with photon energies between 5 keV and 24 keV. The optical layout of the SDU is based on geometrical wavefront splitting and multilayer Bragg mirrors. Maximum delays between Δτ = ±1 ps at 24 keV and Δτ = ±23 ps at 5 keV will be possible. Time-dependent wavefront propagation simulations were performed by means of the Synchrotron Radiation Workshop (SRW) software in order to investigate the impact of the optical layout, including diffraction on the beam splitter and recombiner edges and the three-dimensional topography of all eight mirrors, on the spatio-temporal properties of the XFEL pulses. The radiation is generated from noise by the code FAST which simulates the self-amplified spontaneous emission (SASE) process. A fast Fourier transformation evaluation of the disturbed interference pattern yields for ideal mirror surfaces a coherence time of τc = 0.23 fs and deduces one of τc = 0.21 fs for the real mirrors, thus with an error of Δτ = 0.02 fs which is smaller than the deviation resulting from shot-to-shot fluctuations of SASE2 pulses. The wavefronts are focused by means of compound refractive lenses in order to achieve fluences of a few hundred mJ mm-2 within a spot width of 20 µm (FWHM) diameter. Coherence effects and optics imperfections increase the peak intensity between 200 and 400% for pulse delays within the coherence time. Additionally, the influence of two off-set mirrors in the HED beamline are discussed. Further, we show the fluence distribution for Δz = ±3 mm around the focal spot along the optical axis. The simulations show that the topographies of the mirrors of the SDU are good enough to support X-ray pump/X-ray probe experiments.

Sensitive and Stable 2D Perovskite Single-Crystal X-ray Detectors Enabled by a Supramolecular Anchor.

Perovskite X-ray detectors have been demonstrated to be sensitive to soft X-rays (<80 keV) for potential medical imaging applications. However, developing X-ray detectors that are stable and sensitive to hard X-rays (80 to 120 keV) for practical medical imaging is highly desired. Here, a sensitive 2D fluorophenethylammonium lead iodide ((F-PEA)2 PbI4 ) perovskite single-crystal hard-X-ray detector from low-cost solution processes is reported. Dipole interaction of organic ions promotes the ordering of benzene rings as well as the supramolecular electrostatic interaction between electron-deficient F atoms with neighbor benzene rings. Supramolecular interactions serve as a supramolecular anchor to stabilize and tune the electronic properties of single crystals. The 2D (F-PEA)2 PbI4 perovskite single crystal exhibits an intrinsic property with record bulk resistivity of 1.36 × 1012 Ω cm, which brings a low device noise for hard X-ray detection. Meanwhile, the ion-migration phenomenon is effectively suppressed, even under the large applied bias of 200 V, by blocking the ion migration paths after anchoring. Consequently, the (F-PEA)2 PbI4 single crystal detector yields a sensitivity of 3402 µC Gy-1 air cm-2 to 120 keVp hard X-rays with lowest detectable X-ray dose rate of 23 nGyair s-1 , outperforming the dominating CsI scintillator of commercial digital radiography systems by acquiring clear X-ray images under much lower dose rate. In addition, the detector shows high operation stability under extremely high-flux X-ray irradiation.

Shack-Hartmann wavefront sensors based on 2D refractive lens arrays and super-resolution multi-contrast X-ray imaging.

Different approaches of 2D lens arrays as Shack-Hartmann sensors for hard X-rays are compared. For the first time, a combination of Shack-Hartmann sensors for hard X-rays (SHSX) with a super-resolution imaging approach to perform multi-contrast imaging is demonstrated. A diamond lens is employed as a well known test object. The interleaving approach has great potential to overcome the 2D lens array limitation given by the two-photon polymerization lithography. Finally, the radiation damage induced by continuous exposure of an SHSX prototype with a white beam was studied showing a good performance of several hours. The shape modification and influence in the final image quality are presented.

X-ray photon diagnostics at the European XFEL.

The European X-ray Free-Electron Laser (European XFEL) (Altarelli et al., 2006; Tschentscher et al., 2017), the world's largest and brightest X-ray free-electron laser (Saldin et al., 1999; Pellegrini et al., 2016), went into operation in 2017. This article describes the as-built realization of photon diagnostics for this facility, the diagnostics commissioning and their application for commissioning of the facility, and results from the first year of operation, focusing on the SASE1 beamline, which was the first to be commissioned. The commissioning consisted of pre-beam checkout, first light from the bending magnets, X-rays from single undulator segments, SASE tuning with many undulator segments, first lasing, optics alignment for FEL beam transport through the tunnel up to the experiment hutches, and finally beam delivery to first users. The beam properties assessed by photon diagnostics throughout these phases included per-pulse intensity, beam position, shape, lateral dimensions and spectral properties. During this time period, the machine provided users with up to 14 keV photon energy, 1.5 mJ pulse energy, 300 FEL pulses per train and 4.5 MHz intra-bunch train repetition rate at a 10 Hz train repetition rate. Finally, an outlook is given into the diagnostic prospects for the future.

Idea of thin-film beam splitters for two-colour beamlines.

The idea to split soft X-ray and hard X-ray beams on the same axis into different directions is presented. A thin-film beam splitter can serve this purpose. Performances of thin-film beam splitters made of carbon and aluminium were examined. The idea of thin-film beam splitters expands possibilities in the design of two-colour beamlines.

Operation of X-ray gas monitors at the European XFEL.

X-ray gas monitors (XGMs) are operated at the European XFEL for non-invasive single-shot pulse energy measurements and average beam position monitoring. They are used for tuning and maintaining the self-amplified spontaneous emission (SASE) operation and for sorting single-shot experimental data according to the pulse-resolved energy monitor data. The XGMs were developed at DESY based on the specific requirements for the European XFEL. In total, six XGM units are continuously in operation. Here, the main principle and experimental setup of an XGM are summarized, and the locations of the six XGMs at the facility are shown. Pulse energy measurements at 0.134 nm wavelength are presented, exceeding 1 mJ obtained with an absolute measurement uncertainty of 7-10%; correlations between different XGMs are shown, from which a SASE1 beamline transmission of 97% is deduced. Additionally, simultaneous position measurements close to the undulator and at the end of the tunnel are shown, along with the correlation of beam position data simultaneously acquired by an XGM and an imager.

Hard X-ray self-seeding commissioning at PAL-XFEL.

A wake monochromator based on a large-area diamond single crystal for hard X-ray self-seeding has been successfully installed and commissioned in the hard X-ray free-electron laser (FEL) at the Pohang Accelerator Laboratory with international collaboration. For this commissioning, the self-seeding was demonstrated with a low bunch charge (40 pC) and the nominal bunch charge (180 pC) of self-amplified spontaneous emission (SASE) operation. The FEL pulse lengths were estimated as 7 fs and 29.5 fs, respectively. In both cases, the average spectral brightness increased by more than three times compared with the SASE mode. The self-seeding experiment was demonstrated for the first time using a crystal with a thickness of 30 µm, and a narrow bandwidth of 0.22 eV (full width at half-maximum) was obtained at 8.3 keV, which confirmed the functionality of a crystal with such a small thickness. In the nominal bunch-charge self-seeding experiment, the histogram of the intensity integrated over a 1 eV bandwidth showed a well defined Gaussian profile, which is evidence of the saturated FEL and a minimal electron-energy jitter (∼1.2 × 10-4) effect. The corresponding low photon-energy jitter (∼2.4 × 10-4) of the SASE FEL pulse, which is two times lower than the Pierce parameter, enabled the seeding power to be maximized by maintaining the spectral overlap between SASE FEL gain and the monochromator.

An X-ray gas monitor for free-electron lasers.

A novel X-ray gas monitor (XGM) has been developed which allows the measurement of absolute photon pulse energy and photon beam position at all existing and upcoming free-electron lasers (FELs) over a broad spectral range covering vacuum ultraviolet (VUV), extreme ultraviolet (EUV) and soft and hard X-rays. The XGM covers a wide dynamic range from spontaneous undulator radiation to FEL radiation and provides a temporal resolution of better than 200 ns. The XGM consists of two X-ray gas-monitor detectors (XGMDs) and two huge-aperture open electron multipliers (HAMPs). The HAMP enhances the detection efficiency of the XGM for low-intensity radiation down to 105 photons per pulse and for FEL radiation in the hard X-ray spectral range, while the XGMD operates in higher-intensity regimes. The relative standard uncertainty for measurements of the absolute photon pulse energy is well below 10%, and down to 1% for measurements of relative pulse-to-pulse intensity on pulses with more than 1010 photons per pulse. The accuracy of beam-position monitoring in the vertical and horizontal directions is of the order of 10 µm.

FEL performance achieved at PAL-XFEL using a three-chicane bunch compression scheme.

PAL-XFEL utilizes a three-chicane bunch compression (3-BC) scheme (the very first of its kind in operation) for free-electron laser (FEL) operation. The addition of a third bunch compressor allows for more effective mitigation of coherent synchrotron radiation during bunch compression and an increased flexibility of system configuration. Start-to-end simulations of the effects of radiofrequency jitter on the electron beam performance show that using the 3-BC scheme leads to better performance compared with the two-chicane bunch compression scheme. Together with the high performance of the linac radiofrequency system, it enables reliable operation of PAL-XFEL with unprecedented stability in terms of arrival timing, pointing and intensity; an arrival timing jitter of better than 15 fs, a transverse position jitter of smaller than 10% of the photon beam size, and an FEL intensity jitter of smaller than 5% are consistently achieved.

The SASE1 X-ray beam transport system.

SASE1 is the first beamline of the European XFEL that became operational in 2017. It consists of the SASE1 undulator system, the beam transport system, and the two scientific experiment stations: Single Particles, Clusters, and Biomolecules and Serial Femtosecond Crystallography (SPB/SFX), and Femtosecond X-ray Experiments (FXE). The beam transport system comprises mirrors to offset and guide the beam to the instruments and a set of X-ray optical components to align, manipulate and diagnose the beam. The SASE1 beam transport system is described here in its initial configuration, and results and experiences from the first year of user operation are reported.

SwissFEL Aramis beamline photon diagnostics. Erratum.

The list of authors in the paper by Juranic et al. (2018) [J. Synchrotron Rad. 25, 1238-1248] is corrected.

Measurement of the absolute number of photons of the hard X-ray beamline at the Linac Coherent Light Source.

X-ray free-electron lasers provide intense pulses of coherent X-rays with a short pulse duration. These sources are chaotic by nature and therefore, to be used at their full potential, require that every X-ray pulse is characterized in terms of various relevant properties such as intensity, photon energy, position and timing. Diagnostics are for example installed on an X-ray beamline to specifically monitor the intensity of individual X-ray pulses. To date, these can however only provide a single-shot value of the relative number of photons per shot. Here are reported measurements made in January 2015 of the absolute number of photons in the hard X-ray regime at LCLS which is typically 3.5 × 1011 photons shot-1 between 6 and 9.5 keV at the X-ray Pump-Probe instrument. Moreover, an average transmission of ≉62% of the hard X-ray beamline over this energy range is measured and the third-harmonic content of ≉0.47% below 9 keV is characterized.