In situ characterization of stresses, deformation and fracture of thin films using transmission X-ray nanodiffraction microscopy.

The use of hard X-ray transmission nano- and microdiffraction to perform in situ stress and strain measurements during deformation has recently been demonstrated and used to investigate many thin film systems. Here a newly commissioned sample environment based on a commercially available nanoindenter is presented, which is available at the NanoMAX beamline at the MAX IV synchrotron. Using X-ray nanoprobes of around 60-70 nm at 14-16 keV and a scanning step size of 100 nm, we map the strains, stresses, plastic deformation and fracture during nanoindentation of industrial coatings with thicknesses in the range of several micrometres, relatively strong texture and large grains. The successful measurements of such challenging samples illustrate broad applicability. The sample environment is openly accessible for NanoMAX beamline users through the MAX IV sample environment pool, and its capability can be further extended for specific purposes through additional available modules.

In situ characterization of stresses, deformation and fracture of thin films using transmission X-ray nanodiffraction microscopy. Corrigendum.

Errors in variable subscripts, equations and Fig. 8 in Section 3.2 of the article by Lotze et al. [(2024). J. Synchrotron Rad. 31, 42-52] are corrected.

X-ray in-line holography and holotomography at the NanoMAX beamline.

Coherent X-ray imaging techniques, such as in-line holography, exploit the high brilliance provided by diffraction-limited storage rings to perform imaging sensitive to the electron density through contrast due to the phase shift, rather than conventional attenuation contrast. Thus, coherent X-ray imaging techniques enable high-sensitivity and low-dose imaging, especially for low-atomic-number (Z) chemical elements and materials with similar attenuation contrast. Here, the first implementation of in-line holography at the NanoMAX beamline is presented, which benefits from the exceptional focusing capabilities and the high brilliance provided by MAX IV, the first operational diffraction-limited storage ring up to approximately 300 eV. It is demonstrated that in-line holography at NanoMAX can provide 2D diffraction-limited images, where the achievable resolution is only limited by the 70 nm focal spot at 13 keV X-ray energy. Also, the 3D capabilities of this instrument are demonstrated by performing holotomography on a chalk sample at a mesoscale resolution of around 155 nm. It is foreseen that in-line holography will broaden the spectra of capabilities of MAX IV by providing fast 2D and 3D electron density images from mesoscale down to nanoscale resolution.

Dose-efficient multimodal microscopy of human tissue at a hard X-ray nanoprobe beamline.

X-ray fluorescence microscopy performed at nanofocusing synchrotron beamlines produces quantitative elemental distribution maps at unprecedented resolution (down to a few tens of nanometres), at the expense of relatively long measuring times and high absorbed doses. In this work, a method was implemented in which fast low-dose in-line holography was used to produce quantitative electron density maps at the mesoscale prior to nanoscale X-ray fluorescence acquisition. These maps ensure more efficient fluorescence scans and the reduction of the total absorbed dose, often relevant for radiation-sensitive (e.g. biological) samples. This multimodal microscopy approach was demonstrated on human sural nerve tissue. The two imaging modes provide complementary information at a comparable resolution, ultimately limited by the focal spot size. The experimental setup presented allows the user to swap between them in a flexible and reproducible fashion, as well as to easily adapt the scanning parameters during an experiment to fine-tune resolution and field of view.

Design and performance of a dedicated coherent X-ray scanning diffraction instrument at beamline NanoMAX of MAX IV.

The diffraction endstation of the NanoMAX beamline is designed to provide high-flux coherent X-ray nano-beams for experiments requiring many degrees of freedom for sample and detector. The endstation is equipped with high-efficiency Kirkpatrick-Baez mirror focusing optics and a two-circle goniometer supporting a positioning and scanning device, designed to carry a compact sample environment. A robot is used as a detector arm. The endstation, in continued development, has been in user operation since summer 2017.

Complete alignment of a KB-mirror system guided by ptychography.

We demonstrate how the individual mirrors of a high-quality Kirkpatrick-Baez (KB) mirror system can be aligned to each other to create an optimally focused beam, through minimizing aberrations in the phase of the ptychographically reconstructed pupil function. Different sources of misalignment and the distinctive phase artifacts they create are presented via experimental results from the alignment of the KB mirrors at the NanoMAX diffraction endstation. The catalog of aberration artifacts can be used to easily identify which parameter requires further tuning in the alignment of any KB mirror system.

Contrast - a lightweight Python framework for beamline orchestration and data acquisition.

The emergence of fourth-generation synchrotrons is prompting the development of new systems for experimental control and data acquisition. However, as general control systems are designed to cover a wide set of instruments and techniques, they tend to become large and complicated, at the cost of experimental flexibility. Here we present Contrast, a simple Python framework for interacting with beamline components, orchestrating experiments and managing data acquisition. The system is presented and demonstrated via its application at the NanoMAX beamline of the MAX IV Laboratory.

NanoMAX: the hard X-ray nanoprobe beamline at the MAX IV Laboratory.

NanoMAX is the first hard X-ray nanoprobe beamline at the MAX IV laboratory. It utilizes the unique properties of the world's first operational multi-bend achromat storage ring to provide an intense and coherent focused beam for experiments with several methods. In this paper we present the beamline optics design in detail, show the performance figures, and give an overview of the surrounding infrastructure and the operational diffraction endstation.

Ptychographic characterization of a coherent nanofocused X-ray beam.

The NanoMAX hard X-ray nanoprobe is the first beamline to take full advantage of the diffraction-limited storage ring at the MAX IV synchrotron and delivers a high coherent photon flux for applications in diffraction and imaging. Here, we characterize its coherent and focused beam using ptychographic analysis. We derive beam profiles in the energy range 6-22 keV and estimate the coherent flux based on a probe mode decomposition approach.

Focus characterization of the NanoMAX Kirkpatrick-Baez mirror system.

The focusing and coherence properties of the NanoMAX Kirkpatrick-Baez mirror system at the fourth-generation MAX IV synchrotron in Lund have been characterized. The direct measurement of nano-focused X-ray beams is possible by scanning of an X-ray waveguide, serving basically as an ultra-thin slit. In quasi-coherent operation, beam sizes of down to 56 nm (FWHM, horizontal direction) can be achieved. Comparing measured Airy-like fringe patterns with simulations, the degree of coherence |µ| has been quantified as a function of the secondary source aperture (SSA); the coherence is larger than 50% for SSA sizes below 11 µm at hard X-ray energies of 14 keV. For an SSA size of 5 µm, the degree of coherence has been determined to be 87%.

Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction.

In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br(-) + hv → Br + e(-) and e(-) + Ag(+) → Ag(0). The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s(-1) and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

Compound focusing mirror and X-ray waveguide optics for coherent imaging and nano-diffraction.

A compound optical system for coherent focusing and imaging at the nanoscale is reported, realised by high-gain fixed-curvature elliptical mirrors in combination with X-ray waveguide optics or different cleaning apertures. The key optical concepts are illustrated, as implemented at the Göttingen Instrument for Nano-Imaging with X-rays (GINIX), installed at the P10 coherence beamline of the PETRA III storage ring at DESY, Hamburg, and examples for typical applications in biological imaging are given. Characteristic beam configurations with the recently achieved values are also described, meeting the different requirements of the applications, such as spot size, coherence or bandwidth. The emphasis of this work is on the different beam shaping, filtering and characterization methods.

Achieving hard X-ray nanofocusing using a wedged multilayer Laue lens.

We report on the fabrication and the characterization of a wedged multilayer Laue lens for x-ray nanofocusing. The lens was fabricated using a sputtering deposition technique, in which a specially designed mask was employed to introduce a thickness gradient in the lateral direction of the multilayer. X-ray characterization shows an efficiency of 27% and a focus size of 26 nm at 14.6 keV, in a good agreement with theoretical calculations. These results indicate that the desired wedging is achieved in the fabricated structure. We anticipate that continuous development on wedged MLLs will advance x-ray nanofocusing optics to new frontiers and enrich capabilities and opportunities for hard X-ray microscopy.

Scanning WAXS microscopy of regenerated cellulose fibers at mesoscopic resolution.

In this work, regenerated cellulose textile fibers, Ioncell-F, dry-wet spun with different draw ratios, have been investigated by scanning wide-angle X-ray scattering (WAXS) using a mesoscopic X-ray beam. The fibers were found to be homogeneous on the 500 nm length scale. Analysis of the azimuthal angular dependence of a crystalline Bragg spot intensity revealed a radial dependence of the degree of orientation of crystallites that was found to increase with the distance from the center of the fiber. We attribute this to radial velocity gradients during the extrusion of the spin dope and the early stage of drawing. On the other hand, the fiber crystallinity was found to be essentially homogeneous over the fiber cross section.

Versatility of a hard X-ray Kirkpatrick-Baez focus characterized by ptychography.

In the past decade Kirkpatrick-Baez (KB) mirrors have been established as powerful focusing systems in hard X-ray microscopy applications. Here a ptychographic characterization of the KB focus in the dedicated nano-imaging setup GINIX (Göttingen Instrument for Nano-Imaging with X-rays) at the P10 coherence beamline of the PETRA III synchrotron at HASLYLAB/DESY, Germany, is reported. More specifically, it is shown how aberrations in the KB beam, caused by imperfections in the height profile of the focusing mirrors, can be eliminated using a pinhole as a spatial filter near the focal plane. A combination of different pinhole sizes and illumination conditions of the KB setup makes the prepared optical setup well suited not only for high-resolution ptychographic coherent X-ray diffractive imaging but also for moderate-resolution/large-field-of-view propagation imaging in the divergent KB beam.

Quantitative biological imaging by ptychographic x-ray diffraction microscopy.

Recent advances in coherent x-ray diffractive imaging have paved the way to reliable and quantitative imaging of noncompact specimens at the nanometer scale. Introduced a year ago, an advanced implementation of ptychographic coherent diffractive imaging has removed much of the previous limitations regarding sample preparation and illumination conditions. Here, we apply this recent approach toward structure determination at the nanoscale to biological microscopy. We show that the projected electron density of unstained and unsliced freeze-dried cells of the bacterium Deinococcus radiodurans can be derived from the reconstructed phase in a straightforward and reproducible way, with quantified and small errors. Thus, the approach may contribute in the future to the understanding of the highly disputed nucleoid structure of bacterial cells. In the present study, the estimated resolution for the cells was 85 nm (half-period length), whereas 50-nm resolution was demonstrated for lithographic test structures. With respect to the diameter of the pinhole used to illuminate the samples, a superresolution of about 15 was achieved for the cells and 30 for the test structures, respectively. These values should be assessed in view of the low dose applied on the order of approximately 1.3x10(5) Gy, and were shown to scale with photon fluence.

Structure of cellulose in birch phloem fibres in tension wood: an X-ray nanodiffraction study.

BACKGROUND: To gain a better understanding of bark layer structure and function, especially of the phloem fibres and their contribution to the posture control of trees, it is important to map the structural properties of these cells. The role of bark can also be linked to the reaction wood formation and properties which are essential when it comes to studying the questions related to tree growth. To offer new insights into the role of bark in the postural control of trees, we studied the micro- and nanoscale structures of the phloem and its nearest layers. This study is the first time, in which phloem fibres in trees have been extensively examined using X-ray diffraction (XRD). We determined the orientation of cellulose microfibrils in phloem fibres of Silver birch saplings by using scanning synchrotron nanodiffraction. The samples consisted of phloem fibres extracted from tension, opposite and normal wood (TW, OW, NW). RESULTS: Using scanning XRD, we were able to obtain new information about the mean microfibril angle (MFA) in cellulose microfibrils in phloem fibres connected to reaction wood. A slight but consistent difference was detected in the average MFA values of phloem fibres between the TW and OW sides of the stem. Using scanning XRD, different contrast agents (intensity of the main cellulose reflection or calcium oxalate reflection, mean MFA value) were used to produce 2D images with 200 nm spatial resolution. CONCLUSIONS: Based on our results, the tension wood formation in the stem might be related to the structure and properties of phloem fibres. Thus, our results suggest that the nanostructure of phloem fibres is involved in the postural control of trees containing tension and opposite wood.

Correction: Strain mapping inside an individual processed vertical nanowire transistor using scanning X-ray nanodiffraction.

Correction for 'Strain mapping inside an individual processed vertical nanowire transistor using scanning X-ray nanodiffraction' by Dmitry Dzhigaev et al., Nanoscale, 2020, 12, 14487-14493, DOI: 10.1039/D0NR02260H.

First ptychographic X-ray computed tomography experiment on the NanoMAX beamline.

Ptychographic X-ray computed tomography is a quantitative three-dimensional imaging technique offered to users of multiple synchrotron radiation sources. Its dependence on the coherent fraction of the available X-ray beam makes it perfectly suited to diffraction-limited storage rings. Although MAX IV is the first, and so far only, operating fourth-generation synchrotron light source, none of its experimental stations is currently set up to offer this technique to its users. The first ptychographic X-ray computed tomography experiment has therefore been performed on the NanoMAX beamline. From the results, information was gained about the current limitations of the experimental setup and where attention should be focused for improvement. The extracted parameters in terms of scanning speed, size of the imaged volume and achieved resolutions should provide a baseline for future users designing nano-tomography experiments on the NanoMAX beamline.

Strain mapping inside an individual processed vertical nanowire transistor using scanning X-ray nanodiffraction.

Semiconductor nanowires in wrapped, gate-all-around transistor geometry are highly favorable for future electronics. The advanced nanodevice processing results in strain due to the deposited dielectric and metal layers surrounding the nanowires, significantly affecting their performance. Therefore, non-destructive nanoscale characterization of complete devices is of utmost importance due to the small feature sizes and three-dimensional buried structure. Direct strain mapping inside heterostructured GaSb-InAs nanowire tunnel field-effect transistor embedded in dielectric HfO2, W metal gate layers, and an organic spacer is performed using fast scanning X-ray nanodiffraction. The effect of 10 nm W gate on a single embedded nanowire with segment diameters down to 40 nm is retrieved. The tensile strain values reach 0.26% in the p-type GaSb segment of the transistor. Supported by the finite element method simulation, we establish a connection between the Ar pressure used during the W layer deposition and the nanowire strain state. Thus, we can benchmark our models for further improvements in device engineering. Our study indicates, how the significant increase in X-ray brightness at 4th generation synchrotron, makes high-throughput measurements on realistic nanoelectronic devices viable.