I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[28557]
Open Access
Abstract: Swelling of shale in response to interaction with water is an important consideration within subsurface energy systems. In the case of waste disposal, swelling can provide important barriers around the waste and enhance the sealing ability of rocks. For shale gas exploration purpose, however, swelling may cause wellbore instability. Therefore, a careful study of shale swelling is critical for subsurface energy related applications. Here, the swelling effects of shale were imaged at nanoscale using an advanced synchrotron Transmission X-ray Microscopy (TXM) imaging technique for the first time, with a spatial resolution down to 40.9 nm. Organic matter and clays within the analysed sample were observed to display large swelling effects which resulted in a 50% reduction in porosity. Strain maps generated using Digital Volume Correlation (DVC) show deformation and significant strain were mostly localized to between the contact boundaries of sharp brittle minerals and softer organic matter and clays. This is the first study, to our knowledge, to directly image the swelling deformation of shale at the tens of nanometer scale and provide local information on the strain evolution.
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Jul 2023
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[25756]
Open Access
Abstract: Caries is a chronic disease that causes the alteration of the structure of dental tissues by acid dissolution (in enamel, dentine and cementum) and proteolytic degradation (dentine and cementum) and generates an important cost of care. There is a need to visualise and characterise the acid dissolution process on enamel due to its hierarchical structure leading to complex structural modifications. The process starts at the enamel surface and progresses into depth, which necessitates the study of the internal enamel structure. Artificial demineralisation is usually employed to simulate the process experimentally. In the present study, the demineralisation of human enamel was studied using surface analysis carried out with atomic force microscopy as well as 3D internal analysis using synchrotron X-ray tomography during acid exposure with repeated scans to generate a time-lapse visualisation sequence. Two-dimensional analysis from projections and virtual slices and 3D analysis of the enamel mass provided details of tissue changes at the level of the rods and inter-rod substance. In addition to the visualisation of structural modifications, the rate of dissolution was determined, which demonstrated the feasibility and usefulness of these techniques. The temporal analysis of enamel demineralisation is not limited to dissolution and can be applied to other experimental conditions for the analysis of treated enamel or remineralisation.
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May 2023
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[28574]
Open Access
Abstract: We present a flyscan compatible acquisition scheme for three-modal X-Ray Computed Tomography (CT) with two-dimensional phase sensitivity. Our approach is demonstrated using a “beam tracking” setup, through which a sample’s attenuation, phase (refraction) and scattering properties can be measured from a single frame, providing three complementary contrast channels. Up to now, such setups required the sample to be stepped at each rotation angle to sample signals at an adequate rate, to prevent resolution losses, anisotropic resolution, and under-sampling artefacts. However, the need for stepping necessitated a step-and-shoot implementation, which is affected by motors’ overheads and increases the total scan time. By contrast, our proposed scheme, by which continuous horizontal and vertical translations of the sample are integrated with its rotation (leading to a “cycloidal-spiral” trajectory), is fully compatible with continuous scanning (flyscans). This leads to greatly reduced scan times while largely preserving image quality and isotropic resolution.
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Dec 2022
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I13-2-Diamond Manchester Imaging
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Lorenzo
Massimi
,
Samuel J.
Clark
,
Sebastian
Marussi
,
Adam
Doherty
,
Saurabh M.
Shah
,
Joachim
Schulz
,
Shashidhara
Marathe
,
Christoph
Rau
,
Marco
Endrizzi
,
Peter D.
Lee
,
Alessandro
Olivo
Diamond Proposal Number(s):
[23760]
Open Access
Abstract: In this work, the application of a time resolved multi-contrast beam tracking technique to the investigation of the melting and solidification process in metals is presented. The use of such a technique allows retrieval of three contrast channels, transmission, refraction and dark-field, with millisecond time resolution. We investigated different melting conditions to characterize, at a proof-of-concept level, the features visible in each of the contrast channels. We found that the phase contrast channel provides a superior visibility of the density variations, allowing the liquid metal pool to be clearly distinguished. Refraction and dark-field were found to highlight surface roughness formed during solidification. This work demonstrates that the availability of the additional contrast channels provided by multi-contrast X-ray imaging delivers additional information, also when imaging high atomic number specimens with a significant absorption.
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Jul 2022
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E01-JEM ARM 200CF
I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[29256, 30666]
Open Access
Abstract: Dental caries is a widespread disease that damages teeth by heterogeneous dissolution. Conventional histology identifies different zones within carious lesions by their optical appearance, but fails to quantify the underlying nanoscale structural changes as a function of specific location, impeding better understanding of the demineralisation process. We employ detailed collocative analysis using different imaging modalities, resolutions and fields of view. Focused ion beam-scanning electron microscopy (FIB-SEM) reveals subsurface 3D nanostructure within milled micro-sized volumes, whilst X-ray tomography allows less destructive 3D imaging over large volumes. Correlative combination of these techniques reveals fine detail of enamel rods, inter-rod substance, sheaths, crystallites and voids as a function of location. The degree of enamel demineralisation within the body of the lesion, near its front, and at the surface is visualized in 3D. We thus establish the paradigm of dental 3D nano-histology as an advanced platform for quantitative evaluation of caries-induced structural modification.
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Jun 2022
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I13-2-Diamond Manchester Imaging
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Saranarayanan
Ramachandran
,
Yi
Zhong
,
Stuart
Robertson
,
Christoforos
Panteli
,
Shuibao
Liang
,
Fan
Wu
,
Renqian
Zhou
,
Shashidhara
Marathe
,
Zhaoxia
Zhou
,
Andrew S.
Holmes
,
Sarah J.
Haigh
,
Changqing
Liu
,
Wajira
Mirihanage
Diamond Proposal Number(s):
[24151]
Abstract: Self-Propagating Exothermic Reactive (SPER) bonding with lead-free solders is potentially attractive for microelectronics assembly due to its highly localised heating and minimal thermal loading of the components and substrates. The transient dynamics of melting, wetting, solidification and defect formation during SPER bonding were observed using in-situ synchrotron X-ray imaging with sub-millisecond temporal resolution and the results were further analysed using electron microscopy and thermal modelling. In-situ imaging revealed the preferential melting of the solder and subsequent wetting of the substrate. Numerous air bubbles were observed to form at the bonding interface. The distribution of these bubbles was found to vary with the thermal conductivity and wettability of the substrates. These bubbles appear to reduce the effectiveness of bonding by promoting the formation of cracks and voids within the solder joint. Our results show that metallisation layers on the bonding substrate can influence the dynamics of melting for the solder materials and thereby directly influence the reliability of SPER interconnects.
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Apr 2022
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[24233, 25431]
Open Access
Abstract: Oleofoams are a novel, versatile, and biocompatible soft material that finds application in drug, cosmetic or nutraceuticals delivery. However, due to their temperature-sensitive and opaque nature, the characterization of oleofoams’ microstructure is challenging. Here, synchrotron X-ray microcomputed tomography and radiography are applied to study the microstructure of a triglyceride-based oleofoam. These techniques enable non-destructive, quantitative, 3D measurements of native samples to determine the thermodynamic and kinetic behavior of oleofoams at different stages of their life cycle. During processing, a constant bubble size distribution is reached after few minutes of shearing, while the number of bubbles incorporated keeps increasing until saturation of the continuous phase. Low amounts of solid triglycerides in oleofoams allow faster aeration and a more homogeneous microstructure but lower thermodynamic stability, with bubble disproportionation and shape relaxation over time. Radiography shows that heating causes Ostwald ripening and coalescence of bubbles, with an increase of their diameter and sphericity.
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Jan 2022
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I13-2-Diamond Manchester Imaging
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Open Access
Abstract: Full-field transmission X-ray microscopy (TXM) is a very potent high-resolution X-ray imaging technique. However, it is challenging to achieve fast acquisitions because of the limited efficiency of the optics. Using a broader energy bandwidth, for example using a multilayer monochromator, directly increases the flux in the experiment. The advantage of more counts needs to be weighed against a deterioration in achievable resolution because focusing optics show chromatic aberrations. This study presents theoretical considerations of how much the resolution is affected by an increase in bandwidth as well as measurements at different energy bandwidths (ΔE/E = 0.013%, 0.27%, 0.63%) and the impact on achievable resolution. It is shown that using a multilayer monochromator instead of a classical silicon double-crystal monochromator can increase the flux by an order of magnitude with only a limited effect on the resolution.
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Dec 2021
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[23760]
Abstract: We present a dynamic implementation of the beam-tracking x-ray imaging method providing absorption, phase, and ultrasmall angle scattering signals with microscopic resolution and high frame rate. We demonstrate the method’s ability to capture dynamic processes with 22-ms time resolution by investigating the melting of metals in laser additive manufacturing, which has so far been limited to single-modality synchrotron radiography. The simultaneous availability of three contrast channels enables earlier segmentation of droplets, tracking of powder dynamic, and estimation of unfused powder amounts, demonstrating that the method can provide additional information on melting processes.
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Nov 2021
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I13-1-Coherence
I13-2-Diamond Manchester Imaging
Data acquisition
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Christoph
Rau
,
Shashidhara
Marathe
,
Andrew J.
Bodey
,
Malte
Storm
,
Darren
Batey
,
Silvia
Cipiccia
,
Peng
Li
,
Ralf F.
Ziesche
,
Mohamed
Al-Hada
,
Sven L. M.
Schroeder
,
Gunjan
Das
,
Anjali
Goswami
Open Access
Abstract: We report about multiscale tomography with high throughput at the Diamond beamline I13L. The beamline has the purpose of multi-scale and operando imaging and consists of two independent branchlines operating in real and reciprocal space. The imaging branch -called Diamond-Manchester branchline- hosts micro-tomography, grating interferometry and a full-field microscope. For rapid recording a broad spectrum of the undulator radiation is used either with band-passing the light with a combination of a filter and a deflecting mirror or using a multilayer monochromator. For all the methods similar recording times can be achieved, with typical scanning times of some minutes and covering the resolution range from microns to the 100nm range. Most recently a robot arm has been installed to increase the throughput to 300 samples per day. The system is now implemented for user operation in remote operation mode for the micro-tomography setup and can be expanded to the two other experiments. The instrumental capabilities are applied on various topics such as the study of biodiversity of insects or the structural variations of electrode materials in batteries. Fast recording with dedicated sample environments (not using the sample changing robot) enables operando studies in many areas, the charging/discharging cycles on batteries, the degradation of teeth enamel under various conditions or loading brine sandstone mixtures with CO2, to name some examples. For imaging with highest spatial resolution we managed to improve significantly the recording speed of ptycho-tomography, which is now in the order of hours and will be reduced further. We demonstrated in the past 2-D recording with 10kHz and expand the instrumental capability with specific hardware dependent triggering and scanning schemes. We expand the research program for multi-scale imaging across both branchlines (imaging and coherence branchlines) with first studies such as batteries, brain research, concrete.
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Oct 2021
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