I13-1-Coherence
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Valerio
Bellucci
,
Marie-Christine
Zdora
,
Ladislav
Mikes
,
Šarlota
Birnšteinová
,
Peter
Oberta
,
Marco
Romagnoni
,
Andrea
Mazzolari
,
Pablo
Villanueva-Perez
,
Rajmund
Mokso
,
Christian
David
,
Mikako
Makita
,
Silvia
Cipiccia
,
Jozef
Ulicny
,
Alke
Meents
,
Adrian P.
Mancuso
,
Henry N.
Chapman
,
Patrik
Vagovic
Diamond Proposal Number(s):
[17739]
Open Access
Abstract: The characterisation of fast phenomena at the microscopic scale is required for the understanding of catastrophic responses of materials to loads and shocks, the processing of materials by optical or mechanical means, the processes involved in many key technologies such as additive manufacturing and microfluidics, and the mixing of fuels in combustion. Such processes are usually stochastic in nature and occur within the opaque interior volumes of materials or samples, with complex dynamics that evolve in all three dimensions at speeds exceeding many meters per second. There is therefore a need for the ability to record three-dimensional X-ray movies of irreversible processes with resolutions of micrometers and frame rates of microseconds. Here we demonstrate a method to achieve this by recording a stereo phase-contrast image pair in a single exposure. The two images are combined computationally to reconstruct a 3D model of the object. The method is extendable to more than two simultaneous views. When combined with megahertz pulse trains of X-ray free-electron lasers (XFELs) it will be possible to create movies able to resolve 3D trajectories with velocities of kilometers per second.
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May 2023
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B16-Test Beamline
DIAD-Dual Imaging and Diffraction Beamline
E01-JEM ARM 200CF
E02-JEM ARM 300CF
I08-Scanning X-ray Microscopy beamline (SXM)
I12-JEEP: Joint Engineering, Environmental and Processing
I13-1-Coherence
I13-2-Diamond Manchester Imaging
I14-Hard X-ray Nanoprobe
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Open Access
Abstract: Hard dental tissues possess a complex hierarchical structure that is particularly evident in enamel, the most mineralised substance in the human body. Its complex and interlinked organisation at the Ångstrom (crystal lattice), nano-, micro-, and macro-scales is the result of evolutionary optimisation for mechanical and functional performance: hardness and stiffness, fracture toughness, thermal, and chemical resistance. Understanding the physical–chemical–structural relationships at each scale requires the application of appropriately sensitive and resolving probes. Synchrotron X-ray techniques offer the possibility to progress significantly beyond the capabilities of conventional laboratory instruments, i.e., X-ray diffractometers, and electron and atomic force microscopes. The last few decades have witnessed the accumulation of results obtained from X-ray scattering (diffraction), spectroscopy (including polarisation analysis), and imaging (including ptychography and tomography). The current article presents a multi-disciplinary review of nearly 40 years of discoveries and advancements, primarily pertaining to the study of enamel and its demineralisation (caries), but also linked to the investigations of other mineralised tissues such as dentine, bone, etc. The modelling approaches informed by these observations are also overviewed. The strategic aim of the present review was to identify and evaluate prospective avenues for analysing dental tissues and developing treatments and prophylaxis for improved dental health.
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Apr 2023
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I13-1-Coherence
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Diamond Proposal Number(s):
[30097]
Open Access
Abstract: Ptychography is a form of lens-free coherent diffractive imaging now used extensively in electron and synchrotron-based X-ray microscopy. In its near-field implementation, it offers a route to quantitative phase imaging at an accuracy and resolution competitive with holography, with the added advantages of extended field of view and blind deconvolution of the illumination beam profile from the sample image. In this paper we show how near-field ptychography can be combined with a multi-slice model, adding to this list of advantages the unique ability to recover high-resolution phase images of larger samples, whose thickness places them beyond the depth of field of alternative methods.
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Apr 2023
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I13-1-Coherence
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Savvas N.
Savvides
,
Mattia F.
Gerli
,
Antonio
Citro
,
Lorenzo
Massimi
,
Charlotte K.
Hagen
,
Marco
Endrizzi
,
Alessia
Atzeni
,
Alberto
Astolfo
,
Michela
Esposito
,
Olumide K.
Ogunbiyi
,
Mark
Turmaine
,
Elizabeth S.
Smith
,
Silvia
Cipiccia
,
Christoph
Rau
,
Peng
Li
,
Roberto
Lutman
,
Giulia
Selmin
,
Natalie
Durkin
,
Soichi
Shibuya
,
Marianna
Scuglia
,
Marco
Pellegrini
,
Paolo
De Coppi
,
Alessandro
Olivo
Abstract: Tissue engineering (TE) holds promise for generating lab-grown patient specific organs which can provide: (1) effective treatment for conditions that require volumetric tissue transplantation and (2) new platforms for drug testing. Even though volumetric structural information is essential for confirming successful organ maturation, TE protocol designs are currently informed through destructive and 2D construct assessment tools (e.g. histology). X-ray phase-contrast computed-tomography (PC-CT) can generate non-destructive, high resolution, 3D density maps of organ architecture. In this work, PC-CT is used as new imaging tool for guiding two TE protocols currently at the in-vitro testing stage. The first (1) involves cell-repopulation of an oesophageal scaffold, with the aim of using the regenerated construct for treating long-gap oesophageal atresia, whilst for the second (2) a lung-derived scaffold is populated with islets for regenerating a pancreas, with the “repurposed” lung offering a platform for diabetes drug testing. By combing 3D images and quantitative information, we were able to perform comprehensive construct evaluation. Specifically, we assessed volumetrically: (1) the cell-distribution within the regenerated oesophagi and (2) islet integration with the vascular tree of the lung-derived scaffold. This new information was proven to be essential for establishing corresponding TE protocols and enabled their progression to more advanced scale-up models. We are confident that PC-CT will provide the novel insights necessary to further progress TE protocols, with the next step being in-vivo testing. Crucially, the non-destructive nature of PC-CT will allow in-vivo assessments of TE constructs following their implantation into animal hosts, to investigate their successful integration.
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Apr 2023
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I13-1-Coherence
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Diamond Proposal Number(s):
[28831]
Open Access
Abstract: Diffractive optical elements such as periodic gratings are fundamental devices in X-ray imaging – a technique that medical, material science, and security scans rely upon. Fabrication of such structures with high aspect ratios at the nanoscale creates opportunities to further advance such applications, especially in terms of relaxing X-ray source coherence requirements. This is because typical grating-based X-ray phase imaging techniques (e.g., Talbot self-imaging) require a coherence length of at least one grating period and ideally longer. In this paper, the fabrication challenges in achieving high-aspect ratio nanogratings filled with gold are addressed by a combination of laser interference and nanoimprint lithography, physical vapor deposition, metal assisted chemical etching (MACE), and electroplating. This relatively simple and cost-efficient approach is unlocked by an innovative post-MACE drying step with hexamethyldisilazane, which effectively minimizes the stiction of the nanostructures. The theoretical limits of the approach are discussed and, experimentally, X-ray nanogratings with aspect ratios >40 are demonstrated. Finally, their excellent diffractive abilities are shown when exposed to a hard (12.2 keV) monochromatic X-ray beam at a synchrotron facility, and thus potential applicability in phase-based X-ray imaging.
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Jan 2023
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I13-1-Coherence
I13-2-Diamond Manchester Imaging
Optics
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Open Access
Abstract: I13 is a 250 m long hard X-ray beamline for imaging and coherence experiments at the Diamond Light Source [1]. The beamline comprises two independent experimental branches: one for imaging in direct space using X-ray microscopy and one for imaging in reciprocal space using coherent imaging techniques. The mechanical stability is very important for implementation of increased capabilities at latest generation of long beamlines [2]. Therefore, the beam stability monitoring is essential part of the day-to-day operation of the beamlines as well as for analysis of mechanical instability sources for the Diamond II upgrade. In this paper we present the setup developed to measure mechanical stability of beamline based on optical autocollimator.
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Dec 2022
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I13-1-Coherence
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Open Access
Abstract: The study aims to investigate the effect of ionising radiation on the structure of the chromosomes after lose-dose X-ray irradiation. The first aim was to investigate the changes that occurred in the molecular environment of the chromosomes after radiation exposure using Fluorescence Lifetime Imaging Microscopy (FLIM). The study’s second aim was to measure the mass of the human chromosomes and produce ‘X-ray karyotypes’ of each spread, plotting the measured mass against the number of base pairs using the X-ray ptychography technique. The purpose was to observe the changes in the mass of the X-ray induced chromosomes.
A complete set of 46 human metaphase chromosomes in one frame is known as ‘spread’. Exponentially growing cells were irradiated with X-ray doses at 0.1 Gy (Gray), 0.5 Gy and 1 Gy, followed by chromosome preparation from the irradiated as well as non-irradiated cells. DNA specific stain, 4’,6-diamidino-2-phenylindole (DAPI), was used to stain the chromosomes during the analysis.
Using FLIM, a significant reduction in the DAPI lifetime values (2.8 ± 0.03 ns) was observed in the heterochromatin region of heteromorphic chromosomes 1, 9, 15, and 16 compared to the non-heterochromatin region of the chromosomes (2.88 ± 0.02 ns) present in the non-irradiated chromosome spreads. Furthermore, in the case of irradiated chromosomes, the heterochromatic regions of chromosomes showed statistically significant reduced lifetime values, with the difference ranging between ~260 picoseconds (ps) to ~290 ps compared to the non-irradiated chromosomes. This indicates that chromosomes might have undergone chemical perturbations. However, DAPI lifetime values were not significantly different between low-dose radiations. Therefore, low-dose irradiation is thought to induce an adaptive or hermetic response under certain conditions. However, the sensitivity of the FLIM could assist in the early detection of epigenetic variations that occur in the structure of chromosomes due to radiation/diseases.
Key results were obtained from the Diamond Light Source (Harwell), I-13-coherence beamline by imaging metal-stained and unstained human chromosome spreads at room temperature to determine the gain or loss of genetic material upon low-level X-ray irradiation doses due to radiation damage. The obtained better resolution phase-contrast images of chromosome spreads gave the distribution of electron density which correlates with the mass of the chromosomes. The masses of non-irradiated and irradiated chromosomes were karyotyped to observe the difference in the masses. Therefore, the mass of the human genome can be determined using phase-contrast X-ray ptychography.
The X-ray ptychography results are fascinating. The importance of this research lies in developing a new and improved technique to image and weigh individual chromosomes that will benefit medicine in diagnosing cancer and other health problems from patient samples.
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Nov 2022
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I13-1-Coherence
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Diamond Proposal Number(s):
[25873, 25442]
Abstract: Solar energy powered interfacial evaporation is the most meaningful strategy for energy utilization, water desalination and mineral purification. It can achieve high efficiency, low-density energy and sustainable harvest and utilization. However, the microstructure and surface/interface design still lead to a balance between solar-thermal conversion, water conduction and thermal management, which also determines the efficiency of photothermal interfacial evaporation. Here, a free-standing, ultra-thin carbon film with a tunable nanopore diameter was prepared and used as a blackbody layer for solar photothermal evaporation. By the three-dimensional reconstruction methods, the effect of pore structure on interfacial evaporation is systematically studied. HPCF with an average pore size of about 300 nm exhibited outstanding photothermal evaporation performance, reaching up to 1.96 kg m−2 h−1 with excellent stability. Ultra-hydrophobic, optically enhanced absorption graphene array is constructed on the carbon film surface through femtosecond laser nano processing, further increasing the evaporation rate to 2.12 kg m−2 h−1 (1 sun) and 5.55 kg m−2 h−1 (3 suns).
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Oct 2022
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I13-1-Coherence
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Diamond Proposal Number(s):
[24079]
Open Access
Abstract: The structure and function of solid catalysts are inseparably linked at length scales from nm to cm and beyond. Hard X-ray tomography offers unique potential for spatially-resolved characterization by combining flexible spatial resolution with a range of chemical contrasts. However, the full capabilities of hard X-ray tomography have not been widely explored in the catalysis community. This review highlights modern advances in hard X-ray tomography using synchrotron radiation. Case studies from model to technical scale illustrate the bright future of X-ray tomography in catalysis research.
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Aug 2022
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I13-1-Coherence
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Abstract: In this work, a characterization and optimization of phase-sensitive X-ray imaging techniques with a focus
on the field of laboratory astrophysics is given. Here, the advent of hard X-ray free electron lasers offers
novel opportunities as single-pulse imaging with sub-picosecond temporal resolution becomes possible. The
use of phase-sensitive techniques is often mandatory as micro- and nanoscopic samples show little or no attenuation
contrast. In order to fully benefit from the short pulse lengths at X-ray free electron lasers, these
methods should be reconcilable with single-exposure acquisition schemes. This task is complicated by zeroes
in the respective transfer functions of the imaging systems. Therefore, direct inversions are typically not
possible and sophisticated algorithms are required for the image reconstruction. Overall, this thesis mainly
focuses upon the grating-based X-ray imaging technique, also known as Talbot interferometry. For comparison,
propagation-based phase contrast imaging will also be considered. The investigations are divided into
analytical considerations, numerical simulations, and experimental implementations of the respective imaging
techniques.
An analytical examination of the image formation within a Talbot interferometer is presented. This process
can become complicated, especially for applications in X-ray microscopes. Here, transverse shifts of the
interference pattern in general depend nonlinearly on the phase differences across the X-ray wave field. Existing
reconstruction methods on the basis of deconvolutions then rely on idealized conditions, thus limiting
the experimental applicability of the method. In addition, the achievable spatial resolution of Talbot interferometry
in single-exposure applications is typically limited to the demagnified fringe period of the interference
pattern.
In order to resolve the limitations regarding the applicability, three novel reconstruction methods for Talbot
interferometry are conceptualized and implemented: the design of a beam-splitting diffraction grating featuring
only two diffraction orders, a two-stage deconvolution approach, and a statistical image reconstruction
method based on an analytical forward model of the imaging process and a regularized maximum likelihood
approach. The three schemes are validated on the basis of simulated data. They all prove advantageous when
the premises for standard deconvolution-based reconstructions are not met. The statistical image reconstruction
technique seems most promising as it achieves the best reconstruction quality at low photon numbers and
also circumvents the abovementioned limitations regarding the spatial resolution.
Building up on the simulative studies, two experimental realizations of Talbot interferometry at synchrotron
light sources are presented. In the first experiment, the single-exposure phase imaging capabilities
of Talbot interferometry in conjunction with the statistical image reconstruction method are investigated and
characterized on the basis of simple test samples. The broadened experimental applicability is demonstrated
through the retrieval of Fresnel diffraction images in an X-ray projection microscope. While a comparative
implementation of propagation-based phase contrast imaging at the same instrument still yields a superior
spatial resolution, the mitigation of limitations due to the fringe period is also verified experimentally. In the
second experiment, single-exposure phase imaging with both the grating-based and the propagation-based
approach is employed in order to monitor the moistening process of wood on the level of single wood cells...
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Aug 2022
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