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82 items found (0 items not approved), displaying 51 to 60.[First/Prev] 2, 3, 4, 5, 6, 7, 8, 9 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I15-1-X-ray Pair Distribution Function (XPDF)	Insight into the atomic scale structure of CaF2-CaO-SiO2 glasses using a combination of neutron diffraction, 29Si solid state NMR, high energy X-ray diffraction, FTIR, and XPS Louis Forto Chungong , Mark A. Isaacs , Alexander Morrell , Laura A. Swansbury , Alex C. Hannon , Adam F. Lee , Gavin Mountjoy , Richard A. Martin Biomedical Glasses 5, 112 - 123 DOI: 10.1515/bglass-2019-0010 Diamond Proposal Number(s): [16079] Open Access Show Abstract ▼ Abstract: Bioactive glasses are important for biomedical and dental applications. The controlled release of key ions, which elicit favourable biological responses, is known to be the first key step in the bioactivity of these materials. Properties such as bioactivity and solubility can be tailored for specific applications. The addition of fluoride ions is particularly interesting for dental applications as it promotes the formation of fluoro-apatite. To date there have been mixed reports in the literature on how fluorine is structurally incorporated into bioactive glasses. To optimize the design and subsequent bioactivity of these glasses, it is important to understand the connections between the glass composition, structure and relevant macroscopic properties such as apatite formation and glass degradation in aqueous media. Using neutron diffraction, high energy X-ray diffraction, 29Si NMR, FTIR and XPS we have investigated the atomic scale structure of mixed calcium oxide / calcium fluoride silicate based bioactive glasses. No evidence of direct Si-F bonding was observed, instead fluorine was found to bond directly to calcium resulting in mixed oxygen/fluoride polyhedra. It was therefore concluded that the addition of fluorine does not depolymerise the silicate network and that the widely used network connectivity models are valid in these oxyfluoride systems.	Jan 2019
I07-Surface & interface diffraction	Hydrophobicity of surface-immobilised molecules influences architectures formed via interfacial self-assembly of nucleoside-based gelators Maria Galini Faidra Angelerou , Bin Yang , Thomas Arnold , Jonathan Rawle , Maria Marlow , Mischa Zelzer Soft Matter 34 DOI: 10.1039/C8SM01868E Diamond Proposal Number(s): [16246] Open Access Show Abstract ▼ Abstract: Surface-mediated self-assembly has potential in biomaterial development but underlying rules governing surface–gelator interactions are poorly understood. Here, we correlate surface properties with structural characterization data of nucleoside-based gels obtained by GISAXS and GIWAXS and find that hydrophobicity descriptors (log[thin space (1/6-em)]P, polar surface area, aromaticity) are key predictors for the gel structures formed.	Dec 2018
I22-Small angle scattering & Diffraction	From structure to function: pH-switchable antimicrobial nano-self-assemblies Mark Gontsarik , Anan Yaghmur , Qun Ren , Katharina Maniura-Weber , Stefan Salentinig Acs Applied Materials & Interfaces DOI: 10.1021/acsami.8b18618 Diamond Proposal Number(s): [17191] Show Abstract ▼ Abstract: Stimuli-responsive nanocarriers based on lipid self-assemblies have the potential to provide targeted delivery of antimicrobial peptides, limiting their side effects while protecting them from degradation in the biological environments. In the present study, we design and characterize a simple pH-responsive antimicrobial nanomaterial, formed through the self-assembly of oleic acid (OA) with the human cathelicidin LL-37 as model for an amphiphilic antimicrobial peptide. Colloidal transformations from core-shell cylindrical micelles with a cross-section diameter of ~ 5.5 nm and a length of ~ 23 nm at pH 7.0, to aggregates of branched thread-like micelles at pH 5.0 were detected using synchrotron small angle X-ray scattering, cryogenic transmission electron microscopy, and dynamic light scattering. Biological in vitro assays using an Escherichia coli bacteria strain showed high antimicrobial activity of the positively charged LL-37/OA aggregates at pH 5.0, which was not caused by the pH conditions themselves. Contrary to that, negligible antimicrobial activity was observed at pH 7.0 for the negatively charged cylindrical micelles. The nanocarrier’s ability to switch its biological activity ‘on’ and ‘off’ in response to changes in pH could be used to focus the antimicrobial peptides’ action to areas of specific pH in the body. The presented findings contribute to the fundamental understanding of lipid-peptide self-assembly, and may open up a promising strategy for designing simple pH-responsive delivery systems for antimicrobial peptides.	Dec 2018
I22-Small angle scattering & Diffraction	A guide to high-efficiency chromium (III)-collagen cross-linking: Synchrotron SAXS and DSC study Yi Zhang , Tim Snow , Andrew J. Smith , Geoff Holmes , Sujay Prabakar International Journal Of Biological Macromolecules 126, 123-129 DOI: 10.1016/j.ijbiomac.2018.12.187 Diamond Proposal Number(s): [18388] Show Abstract ▼ Abstract: The inefficiency of the chromium (III)-collagen cross-linking reaction during conventional leather processing results in severe environmental pollution from the waste chromium in the effluent. A mechanistic study using synchrotron-based small-angle X-ray scattering (SAXS) and differential scanning calorimetry (DSC) on ThruBlu tanned leather, revealed the effect of chromium sulphate and its pre-treatments on collagen structure and stability. By pre-treating with complexing agents such as sodium formate and disodium phthalate, as well as nanoclay (sodium montmorillonite), the uniformity through bovine hide collagen matrix were improved significantly. These pre-treatments effectively reduce the reactivity of chromium during its cross-linking reaction with collagen while retaining its bound water. However, collagen pre-treated with a covalent cross-linker (glutaraldehyde) results in a decrease in both chromium-collagen cross-linking and bound water while improving uniformity. These molecular-level insights can be developed into metrics to guide us towards a more sustainable future for the leather industry.	Dec 2018
B16-Test Beamline	Probing the complex thermo-mechanical properties of a 3D-printed polylactide-hydroxyapatite composite using in situ synchrotron X-ray scattering Tan Sui , Enrico Salvati , Hongjia Zhang , Kirill Nyaza , Fedor S. Senatov , Alexei I. Salimon , Alexander M. Korsunsky Journal Of Advanced Research DOI: 10.1016/j.jare.2018.11.002 Diamond Proposal Number(s): [17541, 21312] Open Access Show Abstract ▼ Abstract: Polylactide (PLA)-hydroxyapatite (HAp) composite components have attracted extensive attentions for a variety of biomedical applications. This study seeks to explore how the biocompatible PLA matrix and the bioactive HAp fillers respond to thermo-mechanical environment of a PLA-HAp composite manufactured by 3D printing using Fused Filament Fabrication (FFF). The insight is obtained by in situ synchrotron small- and wide- angle X-ray scattering (SAXS/WAXS) techniques. The thermo-mechanical cyclic loading tests (0-20MPa, 22-56°C) revealed strain softening (Mullins effect) of PLA-HAp composite at both room and elevated temperatures (<56°C), which can be attributed primarily to the non-linear deformation of PLA nanometre-scale lamellar structure. In contrast, the strain softening of the PLA amorphous matrix appeared only at elevated temperatures (>50°C) due to the increased chain mobility. Above this temperature the deformation behaviour of the soft PLA lamella changes drastically. The thermal test (0-110°C) identified multiple crystallisation mechanisms of the PLA amorphous matrix, including reversible stress-induced large crystal formation at room temperature, reversible coupled stress-temperature-induced PLA crystal formation appearing at around 60°C, as well as irreversible heating-induced crystallisation above 92°C. The shape memory test (0-3.75MPa, 0-70°C) of the PLA-HAp composite demonstrates a fixing ratio (strain upon unloading/strain before unloading) of 65% and rather a ∼100% recovery ratio, showing an improved shape memory property. These findings provide a new framework for systematic characterisation of the thermo-mechanical response of composites, and open up ways towards improved material design and enhanced functionality for biomedical applications.	Nov 2018
I15-1-X-ray Pair Distribution Function (XPDF)	The antimicrobial efficacy of hypoxia mimicking cobalt oxide doped phosphate-based glasses against clinically relevant Gram positive, Gram negative bacteria and a fungal strain Farah N. S. Raja , Tony Worthington , Mark A. Isaacs , Louis Forto Chungong , Bernard Burke , Owen Addison , Richard Martin Acs Biomaterials Science & Engineering DOI: 10.1021/acsbiomaterials.8b01045 Diamond Proposal Number(s): [16079] Show Abstract ▼ Abstract: Bioactive phosphate glasses are of considerable interest for a range of soft and hard tissue engineering applications. The glasses are degradable and can release biologically important ions in a controlled manner. The glasses can also potentially be used as an antimicrobial delivery system. In the given study, novel cobalt doped phosphate-based glasses, (P2O5)50(Na2O)20(CaO)30-x(CoO)x where 0 ≤ x (mol%) ≤ 10, were manufactured and characterised. As the cobalt oxide concentration increased the rate of dissolution was observed to decrease. The antimicrobial potential of the glasses was studied using direct and indirect contact methods against both Escherichia coli (NCTC 10538) Staphylococcus aureus (ATCC 6538) and Candida albicans (ATCC 76615). The results showed a strong, time dependent and strain specific, antimicrobial activity of the glasses against microorganisms when in direct contact. Antimicrobial activity (R) ≥ 2 was observed within 2 hours against Escherichia coli whereas similar effect was achieved in 6 hours against Staphylococcus aureus and Candida albicans. However, when in indirect contact, the dissolution products from the bioactive glasses failed to show antimicrobial effect. Following direct exposure to the glasses for 7 days, osteoblast-like SAOS-2 cells showed a 5-fold increase in VEGF mRNA whilst THP-1 monocytic cells showed a 4-fold increase in VEGF mRNA expression when exposed to 10% CoO doped glass compared with the cobalt free control glass. Endothelial cells stimulated with conditioned medium taken from cell cultures of THP-1 monocytes exposed to 10% CoO doped glass showed clear tube–like structure (blood vessel) formation after 4 hours	Nov 2018
I15-Extreme Conditions	Residual strain mapping through pair distribution function analysis of the porcelain veneer within a yttria partially stabilised zirconia dental prosthesis Alexander J. G. Lunt , Philip Chater , Annette Kleppe , Nikolaos Baimpas , Tee K. Neo , Alexander M. Korsunsky Dental Materials DOI: 10.1016/j.dental.2018.11.013 Diamond Proposal Number(s): [9106] Show Abstract ▼ Abstract: Objective. Residually strained porcelain is influential in the early onset of failure in Yttria Partially Stabilised Zirconia (YPSZ) – porcelain dental prosthesis. In order to improve current understanding it is necessary to increase the spatial resolution of residual strain analysis in these veneers. Methods. Few techniques exist which can resolve residual stress in amorphous materials at the microscale resolution required. For this reason, recent developments in Pair Distribution Function (PDF) analysis of X-ray diffraction data of dental porcelain have been exploited. This approach has facilitated high-resolution (70 μm) quantification of residual strain in a YPSZ-porcelain dental prosthesis. In order to cross-validate this technique, the sequential ring-core focused ion beam and digital image correlation approach was implemented at a step size of 50 μm. This semi-destructive technique exploits microscale strain relief to provide quantitative estimates of the near-surface residual strain. Results. The two techniques were found to show highly comparable results. The residual strain within the veneer was found to be primarily tensile, with the highest magnitude stresses located at the YPSZ-porcelain interface where failure is known to originate. Oscillatory tensile and compressive stresses were also found in a direction parallel to the interface, likely to be induced by the multiple layering used during fabrication. Significance. This study provides the insights required to improve prosthesis modelling, to develop new processing routes that minimise residual stress and ultimately to reduce prosthesis failure rates. The PDF approach also offers a powerful new technique for microscale strain quantification in amorphous materials.	Nov 2018
I18-Microfocus Spectroscopy	In situ synchrotron x‐ray diffraction characterization of corrosion products of a ti‐based metallic glass for implant applications Petre Flaviu Gostin , Owen Addison , Alexander P. Morrell , Yue Zhang , Angus J. M. C. Cook , Alethea Liens , Mihai Stoica , Konstantin Ignatyev , Steven R. Street , Jing Wu , Yu-Lung Chiu , Alison Davenport Advanced Healthcare Materials 33 DOI: 10.1002/adhm.201800338 Diamond Proposal Number(s): [13963] Show Abstract ▼ Abstract: Ti‐based bulk metallic glasses are under consideration for implants due to their high yield strength and biocompatibility. In this work, in situ synchrotron X‐ray diffraction (XRD) is used to investigate the corrosion products formed from corrosion of Ti40Zr10Cu34Pd14Sn2 bulk metallic glass in artificial corrosion pits in physiological saline (NaCl). It is found that Pd nanoparticles form in the interior of the pits during electrochemical dissolution. At a low pit growth potential, the change in lattice parameter of the Pd nanoparticles is consistent with the formation of palladium hydride. In addition, a salt layer very close to the dissolving interface is found to contain CuCl, PdCl2, ZrOCl2∙8H2O, Cu, Cu2O, and several unidentified phases. The formation of Pd nanoparticles (16 ± 10 nm at 0.7 V vs Ag/AgCl) containing small amounts of the other alloying elements is confirmed by transmission electron microscopy. The addition of albumin and/or H2O2 does not significantly influence the nature of the corrosion products. When considering the biological compatibility of the alloy, the biological reactivity of the corrosion products identified should be explored.	Sep 2018
I12-JEEP: Joint Engineering, Environmental and Processing I13-2-Diamond Manchester Imaging	Laser-matter interactions in additive manufacturing of SS316L and 13-93 bioactive glass revealed by in situ X-ray imaging Chu Lun Alex Leung , Sebastian Marussi , Michael Towrie , Jesus Del Val Garcia , Robert C. Atwood , Andrew J. Bodey , Julian R. Jones , Philip J. Withers , Peter D. Lee Additive Manufacturing DOI: 10.1016/j.addma.2018.08.025 Diamond Proposal Number(s): [13641, 15250] Open Access Show Abstract ▼ Abstract: Laser-matter interactions in laser additive manufacturing (LAM) occur on short time scales (10-6 - 10-3 s) and have traditionally proven difficult to characterise. We investigate these interactions during LAM of stainless steel (SS316 L) and 13-93 bioactive glass powders using a custom built LAM process replicator (LAMPR) with in situ and operando synchrotron X-ray radiography. This reveals a range of melt track solidification phenomena as well as spatter and porosity formation. We hypothesise that the SS316 L powder absorbs the laser energy at its surface while the trace elements in the 13-93 bioactive glass powder absorb the laser energy by radiation conduction. Our results show that a low viscosity melt, e.g. 8 mPa s for SS316 L, tends to generate spatter with a diameter up to 250 µm and an average spatter velocity of 0.26 m s-1 and form a melt track by molten pool wetting. In contrast, a high viscosity melt, e.g. 2 Pa s for 13-93 bioactive glass, inhibits spatter formation by damping the Marangoni convection, forming a melt track via viscous flow. The viscous flow in 13-93 bioactive glass resists pore transport; combined with the reboil effect, this promotes pore growth during LAM, resulting in a pore size up to 500 times larger than that exhibited in the SS316 L sample.	Aug 2018
B21-High Throughput SAXS	Pectin conformation in solution Katerina Alba , Richard J. Bingham , Patrick A. Gunning , Peter J. Wilde , V. Kontogiorgos The Journal Of Physical Chemistry B DOI: 10.1021/acs.jpcb.8b04790 Diamond Proposal Number(s): [17074] Show Abstract ▼ Abstract: The interplay of degree of methylesterification (DM), pH, temperature, and concentration on the macromolecular interactions of pectin in solution has been explored. Small angle X-ray scattering complemented by atomic force microscopy and molecular dynamics were employed to probe chain dimensions and solution structure. Two length scales have been observed with the first characterising chain clustering with a size ranging between 100-200 nm. The second level of structure arises from single biopolymer chains with radius of gyration between ~6-42 nm. The development of a range of macromolecular dimensions in vitro and in silico shows chain flexibility increases with DM and at acidic pH whereas hydrogen bonding is the responsible thermodynamic driving force for cluster formation. High methyl pectins create structures of lower fractal dimension with less efficient packing. This work unveils pectin conformations covering most of its industrially and biologically relevant environments, enabling rational design of advanced biomaterials based on pectin.	Jul 2018

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