I08-1-Soft X-ray Ptychography
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Abstract: The scales of butterflies display a vast array of vivid colors. However, the exact mechanisms behind these colours are not yet fully understood. Butterfly scales consist of intricate nanostructures that in- teract with light through interference, diffraction, and scattering. Additionally, the nanostructures on butterfly scales vary in pigment density across different species.
A combination of 'pigment effects' and ‘structural effects’ gives rise to the vivid colors observed on a butterfly’s wings. Variations in pigment density have been correlated with specific nanostructures. However, the interplay between pigmentation and nanostructures - how they influence each other - remains largely unexplored. Hence, our work aims to perform a detailed examination of the distribution of various matrix components within butterfly scales, leading to a deeper understanding of not only their colour, but also their role in guiding nano- structure growth.
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Jul 2025
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I08-1-Soft X-ray Ptychography
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Abstract: When an object is illuminated by a source, the resulting exit wave is a complex function intricately connected to the object's structure. Generally speaking, the wave's modulus corresponds to the object's transmittance, while its phase represents the cumulative phase shift relative to free space, caused by the object's refractive index as the wave traverses it. Therefore, to fully characterise the object, both the modulus and phase of the exit wave are required. However, detectors only measure the intensities (the modulus squared) of the waves striking the detector. The modulus can thus be easily obtained by taking the square root of the measured intensity. The phase, on the other hand, is much more challenging to determine. Any potential phase configuration could theoretically produce the same measured intensity, leading to what is known as the 'Phase Retrieval Problem', whereby the true phases that were lost during the experiment are not easily recovered. Ptychography offers a possible solution to the phase retrieval problem. Multiple diffraction intensity patterns are obtained by scanning a finite probe over an extended specimen with sufficient overlap between adjacent illumination positions. Combined with suitable iterative reconstruction algorithms, these measured diffraction patterns can be effectively utilised to accurately determine both the amplitude and phase of the object's exit wave, providing a robust approach that significantly enhances the ability to retrieve complete structural information about a specimen. Ptychography can be combined with X-ray absorption spectroscopy by using an X-ray beam of tuneable energies at each scan position. The diffraction patterns are now collected when the X-rays are scanned over absorption edges of specific elements, providing chemical information, in addition to high resolution reconstructions. This method has been dubbed 'Spectro-Ptychography'. Our work aims to push the limits of ptychography by employing it to analyse various butterfly scales. These scales are intricate self-assemblies of proteins that form complex structures. Beyond exhibiting pigment colour—where specific compounds absorb particular wavelengths of light—butterfly scales are also remarkable examples of structural colour, where their unique structures manipulate light in specific ways. We will showcase the application of spectro-ptychography on butterfly scales and demonstrate how we extracted detailed 3D spatial and chemical information from the dataset, aiding in our understanding of both 'pigment colour' and 'structural colour'.
Preliminary results reveal distinct chemical variations in the carbon and oxygen signatures across different regions of a butterfly scale. By segmenting the scale into defined classes, we gain deeper insights into the chemical compositions of each specific segment, enhancing our understanding of its complex structure.
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Feb 2025
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I08-1-Soft X-ray Ptychography
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Diamond Proposal Number(s):
[32984, 33254]
Abstract: Magnetic materials underpin our high-tech lifestyles and will play key roles in the production of clean energy and next-generation computing technologies. Studying natural magnetic materials can offer insights into animal behaviour, the role of Earth’s magnetic field over time and the formation of the solar system itself. The behaviour of magnetic materials is governed by their underlying magnetisation configuration, including magnetic domains (local areas of uniform magnetisation) and defects such as domain walls.
With magnetic systems varying from the macroscopic scale down to single atoms, and occurring in everything from natural magnetite through to carefully designed topological chiral magnets, researchers require an array of techniques to study them. Exploring magnetic textures on the order of the magnetic exchange length requires spatial resolutions of tens of nanometres or lower.
However, while using a combination of high spatial resolution soft X-ray imaging and electron microscopy allows the analysis of thin samples (≲300 nm) and surfaces, investigation of thicker samples has been limited to hard X-ray dichroic imaging, limiting studies to thin films for most materials, including transition metal magnets.
In work recently published in Physical Review X, an international team of researchers led by Dr Claire Donnelly of the Max Planck Institute for Chemical Physics of Solids has developed a soft X-ray imaging technique for thicker magnets, closing this “thickness gap”. Their work reveals previously inaccessible magnetic textures, and is an exciting development with a range of applications, including the study of naturally occurring magnetic rocks, transition-metal based permanent magnets for energy harvesting, and chiral magnets for spintronics.
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Aug 2024
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I08-1-Soft X-ray Ptychography
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Jeffrey
Neethirajan
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Benedikt J,
Daurer
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Marisel
Di Pietro Martinez
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Ales
Hrabec
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Luke
Turnbull
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Rikako
Yamamoto
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Marina
Raboni Ferreira
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Ales
Stefancic
,
Daniel A.
Mayoh
,
Geetha
Balakrishnan
,
Zhaowen
Pei
,
Pengfei
Xue
,
Liao
Chang
,
Emilie
Ringe
,
Richard
Harrison
,
Sergio
Valencia
,
Majid
Kazemian
,
Burkhard
Kaulich
,
Claire
Donnelly
Diamond Proposal Number(s):
[32984, 33254]
Open Access
Abstract: Imaging of nanoscale magnetic textures within extended material systems is of critical importance to both fundamental research and technological applications. While high-resolution magnetic imaging of thin nanoscale samples is well established with electron and soft x-ray microscopy, the extension to micrometer-thick systems currently requires hard x rays, which limits high-resolution imaging to rare-earth magnets. Here, we overcome this limitation by establishing soft x-ray magnetic imaging of micrometer-thick systems using the pre-edge phase x-ray magnetic circular dichroism signal, thus making possible the study of a wide range of magnetic materials. By performing dichroic spectroptychography, we demonstrate high spatial resolution imaging of magnetic samples up to 1.7 μm thick, an order of magnitude higher than conventionally possible with soft x-ray absorption-based techniques. We demonstrate the applicability of the technique by harnessing the pre-edge phase to image thick chiral helimagnets, and naturally occurring magnetite particles, gaining insight into their three-dimensional magnetic configuration. This new regime of magnetic imaging makes possible the study of extended non-rare-earth systems that have until now been inaccessible, including magnetic textures for future spintronic applications, non-rare-earth permanent magnets for energy harvesting, and the magnetic configuration of giant magnetofossils.
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Aug 2024
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E01-JEM ARM 200CF
I08-1-Soft X-ray Ptychography
I13-2-Diamond Manchester Imaging
I14-Hard X-ray Nanoprobe
I18-Microfocus Spectroscopy
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Cyril
Besnard
,
Ali
Marie
,
Sisini
Sasidharan
,
Petr
Buček
,
Jessica M.
Walker
,
Julia E.
Parker
,
Matthew C.
Spink
,
Robert A.
Harper
,
Shashidhara
Marathe
,
Kaz
Wanelik
,
Thomas E. J.
Moxham
,
Enrico
Salvati
,
Konstantin
Ignatyev
,
Michal M.
Klosowski
,
Richard M.
Shelton
,
Gabriel
Landini
,
Alexander M.
Korsunsky
Diamond Proposal Number(s):
[27749, 30684, 30691, 31005, 29256, 23873]
Open Access
Abstract: Caries, a major global disease associated with dental enamel demineralization, remains insufficiently understood to devise effective prevention or minimally invasive treatment. Understanding the ultrastructural changes in enamel is hampered by a lack of nanoscale characterization of the chemical spatial distributions within the dental tissue. This leads to the requirement to develop techniques based on various characterization methods. The purpose of the present study is to demonstrate the strength of analytic methods using a correlative technique on a single sample of human dental enamel as a specific case study to test the accuracy of techniques to compare regions in enamel. The science of the different techniques is integrated to genuinely study the enamel. The hierarchical structures within carious tissue were mapped using the combination of focused ion beam scanning electron microscopy with synchrotron X-ray tomography. The chemical changes were studied using scanning X-ray fluorescence (XRF) and X-ray wide-angle and small-angle scattering using a beam size below 80 nm for ångström and nanometer length scales. The analysis of XRF intensity gradients revealed subtle variations of Ca intensity in carious samples in comparison with those of normal mature enamel. In addition, the pathways for enamel rod demineralization were studied using X-ray ptychography. The results show the chemical and structural modification in carious enamel with differing locations. These results reinforce the need for multi-modal approaches to nanoscale analysis in complex hierarchically structured materials to interpret the changes of materials. The approach establishes a meticulous correlative characterization platform for the analysis of biomineralized tissues at the nanoscale, which adds confidence in the interpretation of the results and time-saving imaging techniques. The protocol demonstrated here using the dental tissue sample can be applied to other samples for statistical study and the investigation of nanoscale structural changes. The information gathered from the combination of methods could not be obtained with traditional individual techniques.
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Jul 2023
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I08-1-Soft X-ray Ptychography
I14-Hard X-ray Nanoprobe
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Cyril
Besnard
,
Ali
Marie
,
Sisini
Sasidharan
,
Petr
Buček
,
Jessica
Walker
,
Julia E.
Parker
,
Thomas E. J.
Moxham
,
Benedikt
Daurer
,
Burkhard
Kaulich
,
Majid
Kazemian
,
Richard M.
Shelton
,
Gabriel
Landini
,
Alexander M.
Korsunsky
Diamond Proposal Number(s):
[30684, 31005]
Open Access
Abstract: This study reports the characterisation of human dental enamel caries using synchrotron nanoscale correlative ptychography and spectroscopic mapping in combination with scanning electron microscopy. A lamella ̴2.4 µm thick was extracted from a carious enamel region of a tooth using focused ion beam-scanning electron microscopy and transferred to two synchrotron beamlines to perform hard X-ray nano-fluorescence spectroscopy simultaneously with differential phase contrast mapping at a beam size of 50 nm. Soft X-ray ptychography data was then reconstructed with a pixel size of 8 nm. The two dimensional variation in chemistry and structure of carious enamel was revealed at the nanoscale, namely, the organisation of hydroxyapatite nano-crystals within enamel rods was imaged together with the inter-rod region. Correlative use of electron and X-ray scanning microscopies for the same sample allowed visualisation of the connection between structure and composition as presented in a compound image where colour indicates the relative calcium concentration in the sample, as indicated by the calcium Kα fluorescence intensity and grey scale shows the nanostructure. This highlights the importance of advanced correlative imaging to investigate the complex structure-composition relationships in nanomaterials of natural or artificial origin.
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Oct 2022
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I08-1-Soft X-ray Ptychography
I08-Scanning X-ray Microscopy beamline (SXM)
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Diamond Proposal Number(s):
[22398]
Open Access
Abstract: Sustainability, environmental and safety concerns raised by the increasing demand of batteries are driving research towards post-lithium technologies. Rechargeable Zn batteries are strong candidates, but still not practically viable, owing to the extensively studied, but poorly understood unstable behavior of Zn metal upon discharge-charge cycling. This limiting factor warrants more fundamental investigations and the present report provides the lacking molecular-level information on the Zn-based compounds forming at the electrode/electrolyte interface as a result of electrochemical cyclic in weakly acidic aqueous electrolyte. The results are obtained using ex situ X-ray absorption spectromicroscopy maps, modelled mathematically and complemented with cyclic voltammetry, symmetric-cell tests and electron microscopy. We have identified the role of the zincate precipitation resulting from local alkalinization during recharge, combined with additional zincate formation and decomposition to zinc oxide during discharge. The mathematical model allowed a transparent interpretation of morphochemical changes observed. The synergy of these processes leads to electrochemical localization effects, resulting in the formation of a complexly structured and low conductive ZnO-based template, that might play a role in driving shape changes.
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Mar 2022
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