Using diffraction losses of X-rays in a single crystal for determination of its lattice parameters as well as for monochromator calibration.

A way has been developed to measure the unit-cell parameters of a single crystal just from an energy scan with X-rays, even when the exact energy of the X-rays is not well defined due to an error in the pitch angle of the monochromator. The precision of this measurement reaches da/a ∼ 1 × 10-5. The method is based on the analysis of diffraction losses of the beam, transmitted through a single crystal (the so-called `glitch effect'). This method can be easily applied to any transmissive X-ray optical element made of single crystals (for example, X-ray lenses). The only requirements are the possibility to change the energy of the generated X-ray beam and some intensity monitor to measure the transmitted intensity. The method is agnostic to the error in the monochromator tuning and it can even be used for determination of the absolute pitch (or 2θ) angle of the monochromator. Applying the same method to a crystal with well known lattice parameters allows determination of the exact cell parameters of the monochromator at any energy.

X-ray reflectivity from curved surfaces as illustrated by a graphene layer on molten copper.

The X-ray reflectivity technique can provide out-of-plane electron-density profiles of surfaces, interfaces, and thin films, with atomic resolution accuracy. While current methodologies require high surface flatness, this becomes challenging for naturally curved surfaces, particularly for liquid metals, due to the very high surface tension. Here, the development of X-ray reflectivity measurements with beam sizes of a few tens of micrometres on highly curved liquid surfaces using a synchrotron diffractometer equipped with a double crystal beam deflector is presented. The proposed and developed method, which uses a standard reflectivity θ-2θ scan, is successfully applied to study in situ the bare surface of molten copper and molten copper covered by a graphene layer grown in situ by chemical vapor deposition. It was found that the roughness of the bare liquid surface of copper at 1400 K is 1.25 ± 0.10 Å, while the graphene layer is separated from the liquid surface by a distance of 1.55 ± 0.08 Šand has a roughness of 1.26 ± 0.09 Å.

Towards high-quality nitrogen-doped diamond single crystals for X-ray optics.

In this manuscript, characterization of single-crystalline (111) plates prepared from type-Ib diamonds with a nitrogen content of 100-150 ppm by means of high-resolution rocking-curve imaging (RCI) is reported. Contrary to common opinion regarding the intrinsically poor diffraction quality of type-I diamonds, RCI showed the presence of nearly defect-free areas of several millimetres squared in the central part of the diamond plates. The observed broadening of the rocking curves is a result of the cutting and polishing processes, causing strains around the edges of the plates and rare defects. An improvement of the preparation technique will thus allow single-crystalline diamond plates to be made for Laue and Bragg monochromators and beam splitters from type-Ib material with areas large enough to be used as optical elements at fourth-generation synchrotron facilities.

Impact of beryllium microstructure on the imaging and optical properties of X-ray refractive lenses.

Beryllium is one of the most transparent materials to hard X-ray radiation and, as a direct consequence, it is the main material for the fabrication of X-ray refractive optics and instrumentation for synchrotron radiation sources and free-electron laser facilities. However, it is known that almost all beryllium currently in use is polycrystalline material. In this paper, the influence of the microstructure of different beryllium grades on the optical properties of X-ray refractive lenses is studied. The experiments were performed at the ESRF ID06 beamline in X-ray coherent transmission microscopy mode in the near- and far-fields. Two sets of refractive lenses made of beryllium O-30-H and IS-50M grades with different internal microstructure were used. It was found that both beryllium grades have a strongly inhomogeneous structure, which inevitably produces speckle patterns under coherent illumination in imaging experiments. It was shown that fine-grained beryllium O-30-H is better suited for imaging applications, whereas beryllium IS-50M with a relatively large grain microstructure is more appropriate for focusing and collimation of X-rays. A discussion on the requirements for X-ray optical materials used at the third- and fourth-generation synchrotrons is also presented.

Diamond refractive micro-lenses for full-field X-ray imaging and microscopy produced with ion beam lithography.

We demonstrate that ion-beam lithography can be applied to the fabrication of rotationally parabolic refractive diamond X-ray micro-lenses that are of interest to the field of high-resolution X-ray focusing and microscopy. Three single half-lenses with curvature radii of 4.8 µm were produced and stacked to form a compound refractive lens, which provided diffraction-limited focusing of X-ray radiation at the P14 beamline of PETRA-III (DESY). As shown with SEM, the lenses are free of expressed low- and high-frequency shape modulations with a figure error of < 200 nm and surface roughness of 30 nm. Precise micro-manipulation and stacking of individual lenses are demonstrated, which opens up new opportunities for compact X-ray microscopy with nanometer resolution.

Investigation of `glitches' in the energy spectrum induced by single-crystal diamond compound X-ray refractive lenses.

Single-crystal diamond stands out among all the candidate materials that could be exploited to fabricate compound refractive lenses (CRLs) owing to its extremely stable properties. Among all related experimental features, beam divergence, χ-angles relative to the incoming beam in Eulerian geometry and different positions of the X-ray beam relative to the lens geometry may influence the transmission energy spectrum of CRLs. In addition, the orientation of the single-crystal diamond sample may also affect the glitches significantly. To verify these initial assumptions, two experiments, an energy scan and an ω-scan, were set up by employing a polished diamond plate consisting of five biconcave lenses. The results show that beam divergence does not affect the spectrum, nor do χ-angles when ω is set to zero. Nevertheless, different incident positions have an appreciable effect on the transmission spectrum, in particular the `strengths' of the glitches. This is attributed to absorption. The ω-scan setup is capable of determining the so-called orientation matrix, which may be used to predict both `energy positions' and `strengths' of the glitches.

CRL-based ultra-compact transfocator for X-ray focusing and microscopy.

A new ultra-compact transfocator (UCTF) based on X-ray compound refractive lenses (CRLs) is presented. The device can be used to change the number of one- and two-dimensional focusing CRLs by moving the individual parabolic lenses one-by-one independently, thus providing permanent energy and focal-length tunability for scanning and full-field X-ray microscopy applications. The small overall size and light weight of the device allow it to be integrated in any synchrotron beamline, while even simplifying the experimental layout. The UCTF was tested at the Excillium MetalJet microfocus X-ray source and at the P14 EMBL (PETRA-III) beamline, demonstrating high mechanical stability and lens positioning repeatability.

Optical performance and radiation stability of polymer X-ray refractive nano-lenses.

Full-field X-ray imaging and microscopy with polymer compound refractive nano-lenses is demonstrated. Experiments were carried out at beamline ID13 at the European Synchrotron and yielded a resolution of 100 nm. The lenses were demonstrated to be functioning even after an absorbed dose of ∼107 Gy. This article also discusses issues related to lens aberrations, astigmatism and radiation stability, and thus ways of improving the lens further are considered. Polymer nano-lenses are versatile and are promissing for nano-focusing and compact X-ray microscopy.

Linear parabolic single-crystal diamond refractive lenses for synchrotron X-ray sources.

Linear parabolic diamond refractive lenses are presented, designed to withstand high thermal and radiation loads coming from upgraded accelerator X-ray sources. Lenses were manufactured by picosecond laser treatment of a high-quality single-crystal synthetic diamond. Twelve lenses with radius of curvature at parabola apex R = 200 µm, geometrical aperture A = 900 µm and length L = 1.5 mm were stacked as a compound refractive lens and tested at the ESRF ID06 beamline. A focal spot of size 2.2 µm and a gain of 20 were measured at 8 keV. The lens profile and surface quality were estimated by grating interferometry and X-ray radiography. In addition, the influence of X-ray glitches on the focusing properties of the compound refractive lens were studied.

Protective radiolucent aluminium oxide coatings for beryllium X-ray optics.

Beryllium, being one of the most transparent materials to X-ray radiation, has become the material of choice for X-ray optics instrumentation at synchrotron radiation sources and free-electron laser facilities. However, there are concerns due to its high toxicity and, consequently, there is a need for special safety regulations. The authors propose to apply protective coatings in order to seal off beryllium from the ambient atmosphere, thus preventing degradation processes providing additional protection for users and prolonging the service time of the optical elements. This paper presents durability test results for Be windows coated with atomic-layer-deposition alumina layers run at the European Synchrotron Radiation Facility. Expositions were performed under monochromatic, pink and white beams, establishing conditions that the samples could tolerate without radiation damage. X-ray treatment was implemented in various environments, i.e. vacuum, helium, nitrogen, argon and dry air at different pressures. Post-process analysis revealed their efficiency for monochromatic and pink beams.

Optical performance of materials for X-ray refractive optics in the energy range 8-100†keV.

A quantitative analysis of the crucial characteristics of currently used and promising materials for X-ray refractive optics is performed in the extended energy range 8-100 keV. According to the examined parameters, beryllium is the material of choice for X-ray compound refractive lenses (CRLs) in the energy range 8-25 keV. At higher energies the use of CRLs made of diamond and the cubic phase of boron nitride (c-BN) is beneficial. It was demonstrated that the presence of the elements of the fourth (or higher) period has a fatal effect on the functional X-ray properties even if low-Z elements dominate in the compound, like in YB66. Macroscopic properties are discussed: much higher melting points and thermal conductivities of C and c-BN enable them to be used at the new generation of synchrotron radiation sources and X-ray free-electron lasers. The role of crystal and internal structure is discussed: materials with high density are preferable for refractive applications while less dense phases are suitable for X-ray windows. Single-crystal or amorphous glass-like materials based on Li, Be, B or C that are free of diffuse scattering from grain boundaries, voids and inclusions are the best candidates for applications of highly coherent X-ray beams.

30-Lens interferometer for high-energy X-rays.

A novel high-energy multi-lens interferometer consisting of 30 arrays of planar compound refractive lenses is reported. Under coherent illumination each lens array creates a diffraction-limited secondary source. Overlapping such coherent beams produces an interference pattern demonstrating strong longitudinal functional dependence. The proposed multi-lens interferometer was tested experimentally at the 100 m-long ID11 ESRF beamline in the X-ray energy range from 30 to 65 keV. The interference pattern generated by the interferometer was recorded at fundamental and fractional Talbot distances. An effective source size (FWHM) of the order of 15 µm was determined from the first Talbot image, proving the concept that the multi-lens interferometer can be used as a high-resolution tool for beam diagnostics.

Lens coupled tunable Young's double pinhole system for hard X-ray spatial coherence characterization.

We have implemented a modified Young's double slit experiment using pinholes with tunable separation distance coupled with compound refractive lens for hard X-ray spatial coherence characterization. Varying distance between the apertures provides a high sensitivity to the determination of spatial coherence across a wide range of experimental parameters. The use of refractive lenses as a Fourier transformer ensures far field registration conditions and allows the realization of a very compact experimental setup in comparison with the classical Young technique and its derivatives. The tunable double aperture interferometer was experimentally tested at the ESRF ID06 beamline in the energy range from 8 to 25 keV. The spatial coherence and the source size were measured by evaluating the visibility of the interference fringes at various separation distances between the apertures and this value agrees very well with the data obtained by other techniques. The proposed scheme can be used for comprehensive characterization of the coherence properties of the source on low emittance synchrotrons in the hard X-ray region.

Large-acceptance diamond planar refractive lenses manufactured by laser cutting.

For the first time, single-crystal diamond planar refractive lenses have been fabricated by laser micromachining in 300 µm-thick diamond plates which were grown by chemical vapour deposition. Linear lenses with apertures up to 1 mm and parabola apex radii up to 500 µm were manufactured and tested at the ESRF ID06 beamline. The large acceptance of these lenses allows them to be used as beam-conditioning elements. Owing to the unsurpassed thermal properties of single-crystal diamond, these lenses should be suitable to withstand the extreme flux densities expected at the planned fourth-generation X-ray sources.

Highly porous nanoberyllium for X-ray beam speckle suppression.

This paper reports a special device called a `speckle suppressor', which contains a highly porous nanoberyllium plate squeezed between two beryllium windows. The insertion of the speckle suppressor in an X-ray beam allows manipulation of the spatial coherence length, thus changing the effective source size and removing the undesirable speckle structure in X-ray imaging experiments almost without beam attenuation. The absorption of the nanoberyllium plate is below 1% for 1 mm thickness at 12 keV. The speckle suppressor was tested on the ID06 ESRF beamline with X-rays in the energy range from 9 to 15 keV. It was applied for the transformation of the phase-amplitude contrast to the pure amplitude contrast in full-field microscopy.

X-ray harmonics rejection on third-generation synchrotron sources using compound refractive lenses.

A new method of harmonics rejection based on X-ray refractive optics has been proposed. Taking into account the fact that the focal distance of the refractive lens is energy-dependent, the use of an off-axis illumination of the lens immediately leads to spatial separation of the energy spectrum by focusing the fundamental harmonic at the focal point and suppressing the unfocused high-energy radiation with a screen absorber or slit. The experiment was performed at the ESRF ID06 beamline in the in-line geometry using an X-ray transfocator with compound refractive lenses. Using this technique the presence of the third harmonic has been reduced to 10(-3). In total, our method enabled suppression of all higher-order harmonics to five orders of magnitude using monochromator detuning. The method is well suited to third-generation synchrotron radiation sources and is very promising for the future ultimate storage rings.

RETRACTED: Anohova et al. The Dosidicus gigas Collagen for Scaffold Preparation and Cell Cultivation: Mechanical and Physicochemical Properties, Morphology, Composition and Cell Viability. Polymers 2023, 15, 1220.

The Polymers Editorial Office retracts the article, "The Dosidicus gigas Collagen for Scaffold Preparation and Cell Cultivation: Mechanical and Physicochemical Properties, Morphology, Composition and Cell Viability" [...].

Efficient focusing of 8 keV X-rays with multilayer Fresnel zone plates fabricated by atomic layer deposition and focused ion beam milling.

Fresnel zone plates (FZPs) recently showed significant improvement by focusing soft X-rays down to ~10 nm. In contrast to soft X-rays, generally a very high aspect ratio FZP is needed for efficient focusing of hard X-rays. Therefore, FZPs had limited success in the hard X-ray range owing to difficulties of manufacturing high-aspect-ratio zone plates using conventional techniques. Here, employing a method of fabrication based on atomic layer deposition (ALD) and focused ion beam (FIB) milling, FZPs with very high aspect ratios were prepared. Such multilayer FZPs with outermost zone widths of 10 and 35 nm and aspect ratios of up to 243 were tested for their focusing properties at 8 keV and shown to focus hard X-rays efficiently. This success was enabled by the outstanding layer quality thanks to ALD. Via the use of FIB for slicing the multilayer structures, desired aspect ratios could be obtained by precisely controlling the thickness. Experimental diffraction efficiencies of multilayer FZPs fabricated via this combination reached up to 15.58% at 8 keV. In addition, scanning transmission X-ray microscopy experiments at 1.5 keV were carried out using one of the multilayer FZPs and resolved a 60 nm feature size. Finally, the prospective of different material combinations with various outermost zone widths at 8 and 17 keV is discussed in the light of the coupled wave theory and the thin-grating approximation. Al2O3/Ir is outlined as a promising future material candidate for extremely high resolution with a theoretical efficiency of more than 20% for as small an outermost zone width as 10 nm at 17 keV.

The Dosidicus gigas Collagen for Scaffold Preparation and Cell Cultivation: Mechanical and Physicochemical Properties, Morphology, Composition and Cell Viability.

Directed formation of the structure of the culture of living cells is the most important task of tissue engineering. New materials for 3D scaffolds of living tissue are critical for the mass adoption of regenerative medicine protocols. In this manuscript, we demonstrate the results of the molecular structure study of collagen from Dosidicus gigas and reveal the possibility of obtaining a thin membrane material. The collagen membrane is characterized by high flexibility and plasticity as well as mechanical strength. The technology of obtaining collagen scaffolds, as well as the results of studies of its mechanical properties, surface morphology, protein composition, and the process of cell proliferation on its surface, are shown in the given manuscript. The investigation of living tissue culture grown on the surface of a collagen scaffold by X-ray tomography on a synchrotron source made it possible to remodel the structure of the extracellular matrix. It was found that the scaffolds obtained from squid collagen are characterized by a high degree of fibril ordering and high surface roughness and provide efficient directed growth of the cell culture. The resulting material provides the formation of the extracellular matrix and is characterized by a short time to living tissue sorption.

Self-assembly of colloidal cubes via vertical deposition.

The vertical deposition technique for creating crystalline microstructures is applied for the first time to nonspherical colloids in the form of hollow silica cubes. Controlled deposition of the cubes results in large crystalline films with variable symmetry. The microstructures are characterized in detail with scanning electron microscopy and small-angle X-ray scattering. In single layers of cubes, distorted square to hexagonal ordered arrays are formed. For multilayered crystals, the intralayer ordering is predominantly hexagonal with a hollow site stacking, similar to that of the face centered cubic lattice for spheres. Additionally, a distorted square arrangement in the layers is also found to form under certain conditions. These crystalline films are promising for various applications such as photonic materials.