NanoMAX Beamline Research Articles

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.

Nanofocused x-ray photon correlation spectroscopy

Here, we demonstrate an experimental proof of concept for nanofocused x-ray photon correlation spectroscopy, a technique sensitive to nanoscale fluctuations present in a broad range of systems. The experiment, performed at the NanoMAX beamline at MAX IV, uses a novel event-based x-ray detector to capture nanoparticle structural dynamics with microsecond resolution. By varying the nanobeam size from σ=88 nm to σ=2.5μm, we quantify the effect of the nanofocus on the small-angle scattering lineshape and on the diffusion coefficients obtained from nano-XPCS. We observe that the use of nanobeams leads to a multifold increase in speckle contrast, which greatly improves the experimental signal-to-noise ratio, quantified from the two-time intensity correlation functions. We conclude that it is possible to account for influence of the high beam divergence on the lineshape and measured dynamics by including a convolution with the nanobeam profile in the model.Received 17 December 2021Revised 19 May 2022Accepted 16 June 2022DOI:https://doi.org/10.1103/PhysRevResearch.4.L032012Published by the American Physical Society under the terms of the Creative Commons Attribution 4.0 International license. Further distribution of this work must maintain attribution to the author(s) and the published article's title, journal citation, and DOI.Published by the American Physical SocietyPhysics Subject Headings (PhySH)Physical SystemsNanoparticlesSynchrotron radiation & free-electron lasersTechniquesCoherent X-ray scatteringX-ray photon correlation spectroscopyCondensed Matter, Materials & Applied PhysicsPolymers & Soft Matter

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.

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.

Extreme-resolution synchrotron X-Ray fluorescence mapping of ore samples

In order to maximise profit and sustainability of a mining operation, knowledge of the chemistry, mineralogy, texture, and structure of the ore is essential. Continuous advancements in analytical techniques enable studying these features with increasing detail. Synchrotron radiation X-ray fluorescence is unparalleled in its simultaneously high spatial resolution and detection range. Yet, its application in ore geology research and the mining industry is still in its infancy. This study investigated opportunities of extreme-resolution synchrotron X-ray fluorescence mapping of ore samples. Analysis was performed at the NanoMAX beamline at the MAX IV synchrotron facility in Lund, Sweden. The samples investigated are from the Liikavaara Östra Cu-(W-Au) deposit, northern Sweden. Analysis covered areas of several hundreds of μm2 in grains of molybdenite, pyrite, and native Bi. Key results included successful mapping of the lattice-bound distribution of Re, Se, and W in molybdenite at 200 nm spot/step size and detection of nanometre inclusions of Au in native Bi at 50 nm spot/step size. Challenges were encountered concerning data acquisition and processing. In order to achieve satisfactory resolution of both light and heavy elements and to limit mapping artefacts, repeated scans of the same area with varied experimental parameters and very thin (quasi-2d) samples are required. For complex geological samples, the software used for analysing spectral data (PyMCA) requires a considerable degree of human examination, which may be a source of error. Overall, synchrotron X-ray fluorescence mapping has a strong analytical potential for ore geology research, in analysing and imaging trace elements that would constitute potential by-products in mining operations. Detailed knowledge of how trace elements occur in the ores will inform the development of appropriate metal extraction programs thus ensuring that a larger part of the ore may then be utilized.

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, asgeneral control systems are designed to cover a wide set of instruments andtechniques, 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.

Direct Three-Dimensional Imaging of an X-ray Nanofocus Using a Single 60 nm Diameter Nanowire Device

Nanoscale X-ray detectors could allow higher resolution in imaging and diffraction experiments than established systems but are difficult to design due to the long absorption length of X-rays. Here, we demonstrate X-ray detection in a single nanowire in which the nanowire axis is parallel to the optical axis. In this geometry, X-ray absorption can occur along the nanowire length, while the spatial resolution is limited by the diameter. We use the device to make a high-resolution 3D image of the 88 nm diameter X-ray nanofocus at the Nanomax beamline, MAX IV synchrotron, by scanning the single pixel device in different planes along the optical axis. The images reveal fine details of the beam that are unattainable with established detectors and show good agreement with ptychography.

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.

High resolution strain mapping of a single axially heterostructured nanowire using scanning X-ray diffraction

Axially heterostructured nanowires are a promising platform for next generation electronic and optoelectronic devices. Reports based on theoretical modeling have predicted more complex strain distributions and increased critical layer thicknesses than in thin films, due to lateral strain relaxation at the surface, but the understanding of the growth and strain distributions in these complex structures is hampered by the lack of high-resolution characterization techniques. Here, we demonstrate strain mapping of an axially segmented GaInP-InP 190 nm diameter nanowire heterostructure using scanning X-ray diffraction. We systematically investigate the strain distribution and lattice tilt in three different segment lengths from 45 to 170 nm, obtaining strain maps with about 10−4 relative strain sensitivity. The experiments were performed using the 90 nm diameter nanofocus at the NanoMAX beamline, taking advantage of the high coherent flux from the first diffraction limited storage ring MAX IV. The experimental results are in good agreement with a full simulation of the experiment based on a three-dimensional (3D) finite element model. The largest segments show a complex profile, where the lateral strain relaxation at the surface leads to a dome-shaped strain distribution from the mismatched interfaces, and a change from tensile to compressive strain within a single segment. The lattice tilt maps show a cross-shaped profile with excellent qualitative and quantitative agreement with the simulations. In contrast, the shortest measured InP segment is almost fully adapted to the surrounding GaInP segments.

Metal-Assisted Chemical Etching and Electroless Deposition for Fabrication of Hard X-ray Pd/Si Zone Plates.

Zone plates are diffractive optics commonly used in X-ray microscopes. Here, we present a wet-chemical approach for fabricating high aspect ratio Pd/Si zone plate optics aimed at the hard X-ray regime. A Si zone plate mold is fabricated via metal-assisted chemical etching (MACE) and further metalized with Pd via electroless deposition (ELD). MACE results in vertical Si zones with high aspect ratios. The observed MACE rate with our zone plate design is 700 nm/min. The ELD metallization yields a Pd density of 10.7 g/cm, a value slightly lower than the theoretical density of 12 g/cm. Fabricated zone plates have a grid design, 1:1 line-to-space-ratio, 30 nm outermost zone width, and an aspect ratio of 30:1. At 9 keV X-ray energy, the zone plate device shows a first order diffraction efficiency of 1.9%, measured at the MAX IV NanoMAX beamline. With this work, the possibility is opened to fabricate X-ray zone plates with low-cost etching and metallization methods.

Coherent Bragg imaging of 60 nm Au nanoparticles under electrochemical control at the NanoMAX beamline.

Nanoparticles are essential electrocatalysts in chemical production, water treatment and energy conversion, but engineering efficient and specific catalysts requires understanding complex structure-reactivity relations. Recent experiments have shown that Bragg coherent diffraction imaging might be a powerful tool in this regard. The technique provides three-dimensional lattice strain fields from which surface reactivity maps can be inferred. However, all experiments published so far have investigated particles an order of magnitude larger than those used in practical applications. Studying smaller particles quickly becomes demanding as the diffracted intensity falls. Here, in situ nanodiffraction data from 60 nm Au nanoparticles under electrochemical control collected at the hard X-ray nanoprobe beamline of MAX IV, NanoMAX, are presented. Two-dimensional image reconstructions of these particles are produced, and it is estimated that NanoMAX, which is now open for general users, has the requisites for three-dimensional imaging of particles of a size relevant for catalytic applications. This represents the first demonstration of coherent X-ray diffraction experiments performed at a diffraction-limited storage ring, and illustrates the importance of these new sources for experiments where coherence properties become crucial.

Combining Nanofocused X-Rays with Electrical Measurements at the NanoMAX Beamline

The advent of nanofocused X-ray beams has allowed the study of single nanocrystals and complete nanoscale devices in a nondestructive manner, using techniques such as scanning transmission X-ray microscopy (STXM), X-ray fluorescence (XRF) and X-ray diffraction (XRD). Further insight into semiconductor devices can be achieved by combining these techniques with simultaneous electrical measurements. Here, we present a system for electrical biasing and current measurement of single nanostructure devices, which has been developed for the NanoMAX beamline at the fourth-generation synchrotron, MAX IV, Sweden. The system was tested on single InP nanowire devices. The mechanical stability was sufficient to collect scanning XRD and XRF maps with a 50 nm diameter focus. The dark noise of the current measurement system was about 3 fA, which allowed fly scan measurements of X-ray beam induced current (XBIC) in single nanowire devices.

NanoMAX beamline, a nanoprobe beamline for scattering and imaging at MAX IV

NanoMAX beamline, a nanoprobe beamline for scattering and imaging at MAX IV

Initial Operation of the NanoMAX Beamline at MAX IV

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