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25 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3 [Next/Last]

Instruments / Technical Area	Publication Details	Published
B16-Test Beamline	In situ X-ray diffraction and thermal simulation of material extrusion additive manufacturing of polymer Weiguang Wang , Yanhao Hou , Jiong Yang , Zhengyu Yan , Fengyuan Liu , Cian Vyas , Wajira Mirihanage , Paulo Bartolo Materials & Design 245 DOI: 10.1016/j.matdes.2024.113255 Diamond Proposal Number(s): [14099] Open Access Show Abstract ▼ Abstract: Material extrusion additive manufacturing (AM) has gradually become a dominant technology for the fabrication of complex-designed thermoplastic polymers that require a higher level of control over the morphological and mechanical properties. The polymer internal crystal structure formed during the AM process can present significant impacts on the mechanical properties of the individual filaments, as well as the whole structure. Currently, limited details are known about the crystal structure evolution during the material extrusion AM processes of polymers. A novel in situ synchrotron X-ray diffraction (XRD) experimental configuration was developed enabling us to capture the material evolution data throughout the extrusion AM process. The in situ time-resolved data was analysed to reveal nucleation and crystallization sequences during the continuous deposition, with the aid of both complimentary numerical simulations and post-process (ex situ) characterisations. The thermal simulations supported the prediction of the filament temperature profile over time and location during the AM process, while ex situ characterisations validated the correlation between polymer crystallinity (resulting from printing parameters) and corresponding mechanical properties. The results obtained from varied process parameters suggest that the processing temperature has a dominant influence on the crystal microstructure evolution compared to the deposition velocity. A lower processing temperature just above the melting temperature permitted favourable crystallization conditions. The overall analysis demonstrated prospects for enhancing polymer AM, to engineering mechanically hierarchical structures through correlative investigations.	Sep 2024
I12-JEEP: Joint Engineering, Environmental and Processing	An in situ imaging investigation of the effect of gas flow rates on directed energy deposition 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 Materials & Design 108 DOI: 10.1016/j.matdes.2024.113183 Diamond Proposal Number(s): [20096] Open Access	Jul 2024
I13-2-Diamond Manchester Imaging	In situ X-ray imaging of hot cracking and porosity during LPBF of Al-2139 with TiB2 additions and varied process parameters David T. Rees , Chu Lun Alex Leung , Joe Elambasseril , Sebastian Marussi , Saurabh Shah , Shashidhara Marathe , Milan Brandt , Mark Easton , Peter D. Lee Materials & Design 15 DOI: 10.1016/j.matdes.2023.112031 Diamond Proposal Number(s): [19354, 22976] Open Access Show Abstract ▼ Abstract: Laser powder bed fusion (LPBF) additive manufacturing of 2XXX series Al alloys could be used for low volume specialist aerospace components, however, such alloys exhibit hot cracking susceptibility that can lead to component failure. In this study, we show two approaches to suppress the formation of hot cracks by controlling solidification behaviour using: (1) TiB2 additions; and (2) optimisation of LPBF process parameters. Using high-speed synchrotron X-ray radiography, we monitored LPBF of Al-2139 in situ, with and without TiB2 under a range of process conditions. In situ X-ray radiography results captured the crack growth over 1.0 ms at a rate of ca. 110 mm s-1, as well as pore evolution, wetting behaviour and build height. High-resolution synchrotron X-ray computed tomography (sCT) was used to measure the volume fraction of defects, e.g. hydrogen pores and microcracks, in the as-built LPBF samples. Our results show adding TiB2 in Al-2139 reduces the volume of cracks by up to 79 % under a volume energy density of 1000 to 5000 J mm-3, as well as reducing the average length, breadth, and surface area of cracks.	Jun 2023
I08-1-Soft X-ray Ptychography I14-Hard X-ray Nanoprobe	Nanoscale correlative X-ray spectroscopy and ptychography of carious dental enamel 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 Materials & Design 375 DOI: 10.1016/j.matdes.2022.111272 Diamond Proposal Number(s): [30684, 31005] Open Access Show Abstract ▼ 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.	Oct 2022
E01-JEM ARM 200CF I13-2-Diamond Manchester Imaging	Hierarchical 2D to 3D micro/nano-histology of human dental caries lesions using light, X-ray and electron microscopy Cyril Besnard , Ali Marie , Petr Buček , Sisini Sasidharan , Robert A. Harper , Shashidhara Marathe , Kaz Wanelik , Gabriel Landini , Richard M. Shelton , Alexander Korsunsky Materials & Design 394 DOI: 10.1016/j.matdes.2022.110829 Diamond Proposal Number(s): [29256, 30666] Open Access Show Abstract ▼ 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.	Jun 2022
I13-2-Diamond Manchester Imaging	Fundamental study of multi-track friction surfacing deposits for dissimilar aluminum alloys with application to additive manufacturing Malte Soujon , Zina Kallien , Arne Roos , Berit Zeller-Plumhoff , Benjamin Klusemann Materials & Design 214 DOI: 10.1016/j.matdes.2022.110786 Diamond Proposal Number(s): [22346] Open Access Show Abstract ▼ Abstract: Friction surfacing is an emerging solid-state coating technology based on frictional heat induced plastic deformation at the tip of a consumable metallic stud that allows to deposit layers with a fine-grained recrystallized microstructure at temperatures below the melting point. The generation of sound, defect-free metallurgical joints between multiple adjacent overlapping friction surfacing deposits, also referred to as multi-track friction surfacing, from dissimilar aluminum alloys is the focus of this experimental work. An extensive volumetric defect analysis is carried out for various overlap configurations, including post-processing strategies in order to assess the inter-track bonding integrity using microscopic characterization techniques and micro-computed tomography. The effect of layer arrangement and overlap distance on the volumetric defect formation in both inter-track and layer-to-substrate interface is quantified and discussed. Post-processing via hybrid friction diffusion bonding process demonstrates a significant reduction in defect volume ratio, proving higher material efficiency. The gained knowledge was used to successfully build a multi-track multi-layer friction surfacing stack, demonstrating the suitability of this process for large-scale additive manufacturing components. The subsequent mechanical analysis reveals excellent homogeneous isotropic tensile properties of the additive structure in the range of the base material tensile strength.	May 2022
B16-Test Beamline	Strain mapping of silicon carbon suspended membranes Gerard Colston , Oliver Newell , Stephen D. Rhead , Vishal A. Shah , Maksym Myronov Materials & Design 55 DOI: 10.1016/j.matdes.2021.110135 Diamond Proposal Number(s): [11773, 10303] Open Access Show Abstract ▼ Abstract: The alloy silicon carbon (Si1-yCy) has various strain engineering applications. It is often implemented as a dopant diffusion barrier and has been identified as a potential buffer layer for cubic silicon carbide (3C-SiC) heteroepitaxy. While suspended membranes formed from thin films of semiconductor (Ge and 3C-SiC) and dielectric (Si3N4) materials have been well studied, pseudomorphic, defect-free epilayers under high levels of tensile strain have received little attention. Often, tensile strain is a desired quality of semiconductors and enhancing this property can lead to various benefits of subsequent device applications. The strain state and crystalline tilt of suspended Si1-yCy epilayers have been investigated through micro-X-ray diffraction techniques. The in-plane tensile strain of the alloy was found to increase from 0.67% to 0.82%. This strain increase could reduce the C content required to achieve suitable levels of strain in such alloys and further strain enhancement could be externally induced. The source of this strain increase was found to stem from slight tilts at the edges of the membranes, however, the bulk of the suspended films remained flat. The novel process utilised to fabricate suspended Si1-yCy thin-films is applicable to many other materials that are typically not resistant to anisotropic Si wet etchants.	Sep 2021
I11-High Resolution Powder Diffraction	Effects of vacuum on gas content, oxide inclusions and mechanical properties of Ni-based superalloy using electron-beam button and synchrotron diffraction Liang Zheng , Guoqing Zhang , Michael Gorley , Tung Lik Lee , Zhou Li , Chengbo Xiao , Chiu C. Tang Materials & Design 22 DOI: 10.1016/j.matdes.2021.109861 Diamond Proposal Number(s): [10597] Open Access Show Abstract ▼ Abstract: The effects of vacuum induction melting (VIM) vacuum (<1 Pa to 100Pa) on gas content, oxide inclusions and mechanical properties of Ni-based superalloy K4648 has been investigated by electron beam (EB) button experiment under high vacuum (10-3 Pa) and high resolution synchrotron X-ray powder diffraction (SXPD). The results indicated that VIM remelting vacuum drop has obvious effect on the existing form of trace oxygen. The total amount of oxygen did not increase significantly but a dramatic increase in the amount of oxide inclusions by 1-2 orders of magnitude was found. The inclusions are mainly oxides including Al2O3, Cr2O3, Ni(Al,Cr)2O4 and complex oxides or sulfides. Remelting under 100-110Pa has no significant effect on mechanical properties such as stress rupture life and tensile strength but decreased ductility obviously. In comparison to the normal vacuum counterpart, the tensile elongation and impact ductility of the alloy remelted under lower vacuum level decreased by 67% and 40%, respectively. This study reveals the relationship between the vacuum level and mechanical properties of superalloys and highlights the trace amount of oxide inclusions which should be considered as one of the key issues for the cleanliness of superalloys apart from the typical measurement of the gas content only.	Jun 2021
I15-Extreme Conditions	Solidification microstructure and residual stress correlations in direct energy deposited type 316L stainless steel Da Guo , Kun Yan , Mark D. Callaghan , Dominik Daisenberger , Mark Chatterton , Jiadong Chen , Andrew Wisbey , Wajira Mirihanage Materials & Design DOI: 10.1016/j.matdes.2021.109782 Diamond Proposal Number(s): [20605] Open Access Show Abstract ▼ Abstract: Localized fluctuation in residual stress distribution for direct energy deposited 316L stainless steel thin plate was revealed through high-energy synchrotron X-ray diffraction. The macroscopic residual stress levels are changed steadily across the article according to the characteristic cooling rates, as implied by the measured dendrite arm lengths. Localized fluctuations of residual stress in the length scale, between 500 to 600 µm, coincides well with the morphological variations of the solidification microstructure that formed during direct energy deposition. Computations indicate a greater propensity for related mesoscopic thermal gradient fluctuations along the solidification front of the moving melt pool. Novel perspectives on residual stress across multiple length-scales and its relevance to the formation of solidification microstructure in metal additive manufacturing is analysed by considering the experimental results.	May 2021
B16-Test Beamline	Analysis of in vitro demineralised human enamel using multi-scale correlative optical, scanning electron microscopy and high-resolution synchrotron wide-angle X-ray scattering Cyril Besnard , Robert A. Harper , Enrico Salvati , Thomas E. J. Moxham , Leon Romano Brandt , Gabriel Landini , Richard M. Shelton , Alexander M. Korsunsky Materials & Design DOI: 10.1016/j.matdes.2021.109739 Diamond Proposal Number(s): [19192] Open Access Show Abstract ▼ Abstract: Enamel caries is a highly prevalent disease that involves demineralisation of the enamel structure. In this study, we report the analysis of artificially demineralised human enamel slices etched using lactic acid (2 % v/v) in comparison with healthy enamel using correlative techniques of optical and electron microscopy, as well as scanning diffraction. Demineralisation of the enamel was characterised within the micron to sub-micron scale. The structure of the healthy enamel was investigated using focused ion beam - scanning electron microscopy (FIB-SEM) and compared with an etched sample to reveal structural differences. Additional chemical analysis using energy-dispersive X-ray spectroscopy (EDS) was performed and a decrease in the Ca/P atomic % ratio was found in etched samples in comparison with healthy enamel, suggesting more loss of calcium compared with phosphorus. Synchrotron wide-angle X-ray scattering (WAXS) was performed on the samples to reveal the differences in the diffraction patterns before and after etching in terms of lattice structure and preferred orientation (texture). Texture maps were extracted from diffraction analysis at 500 nm spatial resolution. These maps were correlated with the dimension of the enamel structure. The multi-scale correlative approach provided insights into the demineralisation-induced enamel structure alteration at a resolution approaching 500 nm.	Apr 2021

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