I12-JEEP: Joint Engineering, Environmental and Processing
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Imogen
Cowley
,
Harry E.
Chapman
,
Sebastian
Marussi
,
Xianqiang
Fan
,
David
Rees
,
Tristan
Fleming
,
Yunhui
Chen
,
Alexander
Rack
,
Robert C.
Atwood
,
Martyn A.
Jones
,
Samuel J.
Clark
,
Chu Lun Alex
Leung
,
Peter D.
Lee
Diamond Proposal Number(s):
[28804]
Open Access
Abstract: In situ synchrotron studies of Directed Energy Deposition (DED) additive manufacturing provide unique process insights, using high-resolution spatial and temporal observations to reveal melt pool dynamics, phase evolution, and defect formation mechanisms. However, capturing these phenomena under industrially relevant conditions remains a challenge. Here, a second-generation DED apparatus is presented that replicates industrially relevant process conditions whilst enabling multi-modal in situ monitoring, including synchrotron X-ray radiography and diffraction, infrared (IR) imaging, inline coherent imaging (ICI), and optical imaging. The equipment, termed the Blown-powder Additive Manufacturing Process Replicator-II (BAMPR-II), also facilitates a range of unique process adaptations including the application of heat, magnetic fields, and ultrasound. Two case studies are described demonstrating how BAMPR-II reveals the underlying phenomena controlling DED, including: (1) simultaneous X-ray and ICI imaging to capture cracking mechanisms during DED; and (2) X-ray imaging of DED illustrating how magnetic fields can control flow in the melt pool.
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Feb 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Da
Guo
,
Chengbo
Zhu
,
Harry E.
Chapman
,
Kai
Zhang
,
Wei
Li
,
Shishira
Bhagavath
,
Robert
Atwood
,
Stefan
Michalik
,
Dmitry G.
Eskin
,
Iakovos
Tzanakis
,
Chu Lun Alex
Leung
,
Peter D.
Lee
Diamond Proposal Number(s):
[34549]
Open Access
Abstract: Directed energy deposition (DED) additive manufacturing (AM) can fabricate, repair, and join near-net-shaped components for high-performance engineering applications, including biomedical, energy, and transport sectors. The broader adoption of DED remains constrained by the limited number of alloys available that can be reliably manufactured without imperfections, hence limiting mechanical properties. Here, we designed an Al-Ni-Ce-Mn-Fe AM alloy that can achieve an ultra-fine microstructure (<5 μm), uniform distribution of intermetallics, low residual stress (<32 MPa), and superior mechanical properties in as-built DED components. Compared to DED AlSi10Mg in the as-build state using the same conditions, the yield increased by 70%, and the ultimate tensile strength by 50%. DED-AM involves rapid cooling and complex thermal conditions, which largely influence the property of the final components. Post-characterization cannot capture the time resolved thermal behavior, hence offer limited mechanism-based guide for alloy design. In this study, we develop a novel multimodal characterization methodology for correlative in situ X-ray imaging, X-ray diffraction, and infrared imaging, enabling quantification of the in situ thermal-related behavior, including phase evolution, temperature distribution and stress accumulation during DED. We elucidated key mechanisms driving the structure refinement and stress development in this alloy. The insights gained into the interplay between alloy composition, thermal-related behavior, and performance under specific AM conditions informs next-generation material design tailored for AM technologies.
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Jan 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[31855]
Open Access
Abstract: Directed energy deposition (DED) laser additive manufacturing (AM) is a promising technique for building complex components and performing repair applications. However, large defects can form through coalescence of argon bubbles from the feedstock powder, potentially reducing end-component mechanical performance. Here, we used correlative high-speed synchrotron X-ray and infrared imaging, coupled with multiphysics modelling to develop a strategy to control defect formation. We demonstrate that the bubble dynamics can be controlled by appropriately modulating the laser power, temporarily disrupting the Marangoni flow, enabling bubble release. The bubble control mechanisms discovered here provide a way to achieve defect-lean AM.
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Sep 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[26767]
Open Access
Abstract: Lithium ion batteries are pivotal for clean energy storage and mitigating climate change. In this study, we employ operando synchrotron X-ray computed tomography to investigate the dynamic evolution of battery cathode microstructure. We focus on tracking changes in porosity and pore size distribution at the microscale and cathode thickness at the macroscale during the lithiation and delithiation processes within a commercially configured battery. Image quality was enhanced using both conventional image processing methods and a Super-Resolution Convolutional Neural Network (SRCNN) model. Our findings revealed a slight increase in the cathode solid volume fraction and specific surface area as the battery transitioned from its pristine state to fully lithiated, followed by a reduction during delithiation. This behavior was attributed to the expansion of the cathode material and phase transitions during lithiation, which split larger pores into smaller ones, as evidenced by the increase in surface area. Cathode thickness also exhibited expansion during lithiation and contraction during delithiation. These results offer valuable insights into the structural changes that contribute to battery aging, helping researchers better understand how these different parameters change over time. This understanding is crucial for designing more durable and sustainable batteries in the future, both in terms of specific design and material selection, to enhance resistance during charge and discharge cycles to improve performance and longevity.
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Apr 2025
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[19354]
Open Access
Abstract: Laser powder bed fusion (LPBF) of Polyamide 12 (PA12) using a near-infra-red (NIR) beam is largely unexplored; therefore, the beam-matter interaction, evolution mechanisms of the melt pool and defects remain unclear. Here, we employed a combination of in situ synchrotron X-ray imaging, ex situ materials characterisation techniques, and high-fidelity process simulations to study these behaviours during LPBF of PA12. Our results demonstrate that the NIR absorption of PA12 can be improved by 600 times through powder surface modification with C, P and Al species. In situ X-ray images reveal that the PA12 powders undergo melting, viscous merging, volume expansion, warping, solidification, and shrinkage before forming a solid track. Our results uncover the bubble evolution mechanisms during LPBF of PA12. During laser scanning, the high-energy laser beam produces organic substances/vapours which are trapped inside bubbles during viscous merging. These bubbles continue to shrink due to vapour condensation as the polymer cools under a cooling rate range of 200 - 600 K s−1. Using the collected data, we have developed a data-driven bubble shrinkage criterion to predict the bubble shrinkage coefficient using the bubble half-life, improving the build quality of LPBF polymeric parts.
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Feb 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[29851]
Open Access
Abstract: Irregular Li heterostructure growth at the interphase between the solid electrolyte and anode reduces solid-state Li metal battery (SSLMB) performance, but the fundamental cause is still elusive. Measuring and imaging Li+ ion diffusion in operando inside an SSLMB using a commercially standard cell configuration are extremely challenging because the ultra-light Li element exhibits a minute signal-to-noise ratio using most x-ray-related characterization methods, and the weak x-ray signals of Li+ are buried by strong signals of other heavy transition metal elements in the cathode and battery enclosure. Here, we pioneer novel operando correlative imaging of coupling x-ray Compton scattering with computed tomography (XCS-CT), which is able to quantify the interplay between spatially resolved Li+ ion diffusion kinetics and Li0 metal structure growth at the interphases of both the anode and cathode sides inside a full-cell SSLMB using a solid polymer electrolyte (SPE) and commercially standard cell configuration during (dis)charging. We show a 61% increase in the efficiency of extracting Li+ ions from the cathode LiNi0.6Mn0.2Co0.2O2 to the anode during charging at 0.1 C compared with at 1 C due to restricted Li+ ion diffusion at the higher rate inside SSLMB. However, this led to the formation of a more irregular interfacial morphology, consisting not only of Li0 dendrites, but also sub-surface pore formation at the anode/SPE interphase. We find that surprisingly, the irregular Li0 structure initiation and growth are accelerated during the first Li stripping step, not the Li plating step, and the root cause is the onset imbalance of Li+ ion diffusion and redox reactions between the anode and cathode. These insights highlight the benefits of asymmetric charging and discharging rates as a promising solution to improving SSLMB performance with SPEs. The operando correlative XCS-CT imaging technique has the potential to study the relationship between active ion concentrations and buried morphological changes for a variety of battery chemistries.
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Feb 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Lorna
Sinclair
,
Oliver
Hatt
,
Samuel J.
Clark
,
Sebastian
Marussi
,
Elena
Ruckh
,
Robert C.
Atwood
,
Martyn
Jones
,
Gavin J.
Baxter
,
Chu Lun Alex
Leung
,
Iain
Todd
,
Peter D.
Lee
Diamond Proposal Number(s):
[20096]
Open Access
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Jul 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[29851, 23400]
Open Access
Abstract: Understanding the correlation between chemical and microstructural properties is critical for unraveling the fundamental relationship between materials chemistry and physical structures that can benefit materials science and engineering. Here, we demonstrate novel in situ correlative imaging of the X-ray Compton scattering computed tomography (XCS-CT) technique for studying this fundamental relationship. XCS-CT can image light elements that do not usually exhibit strong signals using other X-ray characterization techniques. This paper describes the XCS-CT setup and data analysis method for calculating the valence electron momentum density and lithium-ion concentration, and provides two examples of spatially and temporally resolved chemical properties inside batteries in 3D. XCS-CT was applied to study two types of rechargeable lithium batteries in standard coin cell casings: (1) a lithium-ion battery containing a cathode of bespoke microstructure and liquid electrolyte, and (2) a solid-state battery containing a solid-polymer electrolyte. The XCS-CT technique is beneficial to a wide variety of materials and systems to map chemical composition changes in 3D structures.
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Jul 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[29851]
Open Access
Abstract: The formation of heterogeneous Li structures at the anode/solid polymer electrolyte (SPE) membrane interphase of solid-state Li-metal batteries (SSLMBs) is one of the key factors that impede SSLMB performance. The relationship between Li+-ion transport kinetics and Li0 structural evolution at the buried interphase is critical but challenging to characterize. Here, we report an operando correlative X-ray Compton scattering and computed tomography imaging technique that quantifies the changes of Li+-ion concentrations in the bulk cathode, SPE membrane, and anode of the SSLMB full cell using a commercially standard configuration. We then visualize Li+-ion concentration distributions as well as Li0 microstructures at the buried anode/SPE interphase. Mechanistic analyses show that the Li-stripping step forms more irregular interfacial Li morphologies at the expense of bulk anode volume shrinkage compared to the Li-plating step during the first cycle.
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May 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[22053, 30735, 31855]
Open Access
Abstract: Synchrotron X-ray imaging has been utilised to detect the dynamic behaviour of molten pools during the metal additive manufacturing (AM) process, where a substantial amount of imaging data is generated. Here, we develop an efficient and robust deep learning model, AM-SegNet, for segmenting and quantifying high-resolution X-ray images and prepare a large-scale database consisting of over 10,000 pixel-labelled images for model training and testing. AM-SegNet incorporates a lightweight convolution block and a customised attention mechanism, capable of performing semantic segmentation with high accuracy (∼96%) and processing speed (< 4 ms per frame). The segmentation results can be used for quantification and multi-modal correlation analysis of critical features (e.g. keyholes and pores). Additionally, the application of AM-SegNet to other advanced manufacturing processes is demonstrated. The proposed method will enable end-users in the manufacturing and imaging domains to accelerate data processing from collection to analytics, and provide insights into the processes’ governing physics.
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Mar 2024
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