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Instruments / Technical Area	Publication Details	Published
I22-Small angle scattering & Diffraction	Tailoring viscoelastic properties of dynamic supramolecular poly(butadiene)-based elastomers M. Hyder , A. D. O'Donnell , A. M. Chippindale , I. M. German , J. L. Harries , O. Shebanova , I. W. Hamley , W. Hayes Materials Today Chemistry 26 DOI: 10.1016/j.mtchem.2022.101008 Diamond Proposal Number(s): [22909] Open Access Show Abstract ▼ Abstract: The discovery and development of new adhesive materials is critical for real-world applications of polymeric composite materials. Herein, we report the design and synthesis of a library of structurally related phase-separated supramolecular polyurethanes whose mechanical properties and adhesive characteristics can be enhanced through minor structural modifications of the polymer end-group. The interplay between phase separation of the hard domain polar end-groups and soft polybutadiene domains, coupled with tuneable self-assembly afforded by the polar end-groups, gives rise to a class of materials with tuneable mechanical properties. Exceptionally strong supramolecular adhesives and mechanically robust self-healing elastomers were identified. The mechanical properties were investigated through tensile testing. Finally, rheological analysis of the supramolecular materials was used to identify suitable healing and adhesive temperatures in addition to elucidate the supramolecular polyurethanes' thermal-responsive nature.	Dec 2022
I02-Macromolecular Crystallography I03-Macromolecular Crystallography I22-Small angle scattering & Diffraction	Tropocollagen springs allow collagen fibrils to stretch elastically James S. Bell , Sally Hayes , Charles Whitford , Juan Sanchez-Weatherby , Olga Shebanova , Nick J. Terrill , Thomas Sorensen , Ahmed Elsheikh , Keith M. Meek Acta Biomaterialia 8 DOI: 10.1016/j.actbio.2022.01.041 Diamond Proposal Number(s): [11316, 8458] Show Abstract ▼ Abstract: The mechanical properties of connective tissues are tailored to their specific function, and changes can lead to dysfunction and pathology. In most mammalian tissues the mechanical environment is governed by the micro- and nano-scale structure of collagen and its interaction with other tissue components, however these hierarchical properties remain poorly understood. In this study we use the human cornea as a model system to characterise and quantify the dominant deformation mechanisms of connective tissue in response to cyclic loads of physiological magnitude. Synchronised biomechanical testing, x-ray scattering and 3D digital image correlation revealed the presence of two dominant mechanisms: collagen fibril elongation due to a largely elastic, spring-like straightening of tropocollagen supramolecular twist, and a more viscous straightening of fibril crimp that gradually increased over successive loading cycles. The distinct mechanical properties of the two mechanisms suggest they have separate roles in vivo. The elastic, spring-like mechanism is fast-acting and likely responds to stresses associated with the cardiac cycle, while the more viscous crimp mechanism will respond to slower processes, such as postural stresses. It is anticipated that these findings will have broad applicability to understanding the normal and pathological functioning of other connective tissues such as skin and blood vessels that exhibit both helical structures and crimp.	Jan 2022
I22-Small angle scattering & Diffraction	I22: SAXS/WAXS beamline at Diamond Light Source – an overview of 10 years operation Andrew Smith , S. G. Alcock , L. S. Davidson , J. H. Emmins , J. C. Hiller Bardsley , P. Holloway , M. Malfois , A. R. Marshall , C. L. Pizzey , S. E. Rogers , O. Shebanova , T. Snow , J. P. Sutter , E. P. Williams , N. J. Terrill Journal Of Synchrotron Radiation 28 DOI: 10.1107/S1600577521002113 Open Access Show Abstract ▼ Abstract: Beamline I22 at Diamond Light Source is dedicated to the study of soft-matter systems from both biological and materials science. The beamline can operate in the range 3.7 keV to 22 keV for transmission SAXS and 14 keV to 20 keV for microfocus SAXS with beam sizes of 240 µm × 60 µm [full width half-maximum (FWHM) horizontal (H) × vertical (V)] at the sample for the main beamline, and approximately 10 µm × 10 µm for the dedicated microfocusing platform. There is a versatile sample platform for accommodating a range of facilities and user-developed sample environments. The high brilliance of the insertion device source on I22 allows structural investigation of materials under extreme environments (for example, fluid flow at high pressures and temperatures). I22 provides reliable access to millisecond data acquisition timescales, essential to understanding kinetic processes such as protein folding or structural evolution in polymers and colloids.	May 2021
I22-Small angle scattering & Diffraction	Extending synchrotron SAXS instrument ranges through addition of a portable, inexpensive USAXS module with vertical rotation axes Brian R. Pauw , Andrew Smith , Tim Snow , Olga Shebanova , John P. Sutter , Jan Ilavsky , Daniel Hermida-Merino , Glen J. Smales , Nicholas J. Terrill , Andreas F. Thünemann , Wim Bras Journal Of Synchrotron Radiation 28 DOI: 10.1107/S1600577521003313 Open Access Show Abstract ▼ Abstract: Ultra-SAXS can enhance the capabilities of existing synchrotron SAXS/WAXS beamlines. A compact ultra-SAXS module has been developed, which extends the measurable q-range with 0.0015 ≤ q (nm−1) ≤ 0.2, allowing structural dimensions in the range 30 ≤ D (nm) ≤ 4000 to be probed in addition to the range covered by a high-end SAXS/WAXS instrument. By shifting the module components in and out on their respective motor stages, SAXS/WAXS measurements can be easily and rapidly interleaved with USAXS measurements. The use of vertical crystal rotation axes (horizontal diffraction) greatly simplifies the construction, at minimal cost to efficiency. In this paper, the design considerations, realization and synchrotron findings are presented. Measurements of silica spheres, an alumina membrane, and a porous carbon catalyst are provided as application examples.	May 2021
I22-Small angle scattering & Diffraction	Pressure and temperature dependence of local structure and dynamics in an ionic liquid Filippa Lundin , Henriette Wase Hansen , Karolina Adrjanowicz , Bernhard Frick , Daniel Rauber , Rolf Hempelmann , Olga Shebanova , Kristine Niss , Aleksandar Matic The Journal Of Physical Chemistry B DOI: 10.1021/acs.jpcb.1c00147 Diamond Proposal Number(s): [20249] Show Abstract ▼ Abstract: A detailed understanding of the local dynamics in ionic liquids remains an important aspect in the design of new ionic liquids as advanced functional fluids. Here, we use small-angle X-ray scattering and quasi-elastic neutron spectroscopy to investigate the local structure and dynamics in a model ionic liquid as a function of temperature and pressure, with a particular focus on state points (P,T) where the macroscopic dynamics, i.e., conductivity, is the same. Our results suggest that the initial step of ion transport is a confined diffusion process, on the nanosecond timescale, where the motion is restricted by a cage of nearest neighbors. This process is invariant considering timescale, geometry, and the participation ratio, at state points of constant conductivity, i.e., state points of isoconductivity. The connection to the nearest-neighbor structure is underlined by the invariance of the peak in the structure factor corresponding to nearest-neighbor correlations. At shorter timescales, picoseconds, two localized relaxation processes of the cation can be observed, which are not directly linked to ion transport. However, these processes also show invariance at isoconductivity. This points to that the overall energy landscape in ionic liquids responds in the same way to density changes and is mainly governed by the nearest-neighbor interactions.	Mar 2021
I22-Small angle scattering & Diffraction	Programming gels over a wide pH range using multicomponent systems Santanu Panja , Olga Shebanova , Andrew Smith , Bart Dietrich , Dave John Adams Angewandte Chemie International Edition DOI: 10.1002/anie.202101247 Diamond Proposal Number(s): [27906] Open Access Show Abstract ▼ Abstract: Multicomponent hydrogels offer a tremendous opportunity to prepare useful and exciting materials that cannot be accessed using a single component. Here, we describe an unusual multi‐component low molecular weight gelling system that exhibits pH‐responsive behavior involving cooperative hydrogen bonding between the components, allowing it to maintain a gel phase across a wide pH range. Unlike traditional acid‐triggered gels, our system undergoes a change in the underlying molecular packing and maintains the β‐sheet structure both at acidic and basic pH. We further establish that autonomous programming between these two gel states is possible by an enzymatic reaction which allows us to prepare gels with improved mechanical properties.	Feb 2021
I15-Extreme Conditions I22-Small angle scattering & Diffraction	In situ observation of nanolite growth in volcanic melt: A driving force for explosive eruptions Danilo Di Genova , Richard A. Brooker , Heidy M. Mader , James W. E. Drewitt , Alessandro Longo , Joachim Deubener , Daniel R. Neuville , Sara Fanara , Olga Shebanova , Simon Anzellini , Fabio Arzilli , Emily C. Bamber , Louis Hennet , Giuseppe La Spina , Nobuyoshi Miyajima Science Advances 6 DOI: 10.1126/sciadv.abb0413 Diamond Proposal Number(s): [17615, 20447] Open Access Show Abstract ▼ Abstract: Although gas exsolution is a major driving force behind explosive volcanic eruptions, viscosity is critical in controlling the escape of bubbles and switching between explosive and effusive behavior. Temperature and composition control melt viscosity, but crystallization above a critical volume (>30 volume %) can lock up the magma, triggering an explosion. Here, we present an alternative to this well-established paradigm by showing how an unexpectedly small volume of nano-sized crystals can cause a disproportionate increase in magma viscosity. Our in situ observations on a basaltic melt, rheological measurements in an analog system, and modeling demonstrate how just a few volume % of nanolites results in a marked increase in viscosity above the critical value needed for explosive fragmentation, even for a low-viscosity melt. Images of nanolites from low-viscosity explosive eruptions and an experimentally produced basaltic pumice show syn-eruptive growth, possibly nucleating a high bubble number density.	Sep 2020
I22-Small angle scattering & Diffraction	Pluronic F127 thermosensitive injectable smart hydrogels for controlled drug delivery system development Bana Shriky , Adrian Kelly , Mohammad Isreb , Maksims Babenko , Najet Mahmoudi , Sarah Rogers , Olga Shebanova , Tim Snow , Tim Gough Journal Of Colloid And Interface Science DOI: 10.1016/j.jcis.2019.12.096 Diamond Proposal Number(s): [18402] Show Abstract ▼ Abstract: Understanding structure-property relationships is critical for the development of new drug delivery systems. This study investigates the properties of Pluronic smart hydrogel formulations for future use as injectable controlled drug carriers. The smart hydrogels promise to enhance patient compliance, decrease side effects and reduce dose and frequency. Pharmaceutically, these systems are attractive due to their unique sol-gel phase transition in the body, biocompatibility, safety and injectability as solutions before transforming into gel matrices at body temperature. We quantify the structural changes of F127 systems under controlled temperature after flow, as experienced during real bodily injection. Empirical formulae combining the coupled thermal and shear dependency are produced to aid future application of these systems. Induced structural transitions measured in-situ by small angle x-ray and neutron scattering reveal mixed oriented structures that can be exploited to tailor the drug release profile.	Dec 2019
	In situ mechanical behavior of regenerating rat calvaria bones under tensile load via synchrotron diffraction characterization Ameni Zaouali , Baptiste Girault , David Gloaguen , Fabienne Jordana , Marie-José Moya , Pierre-Antoine Dubos , Valerie Geoffroy , Matthias Schwartzkopf , Tim Snow , Himadri Gupta , Olga Shebanova , Konrad Schneider , Baobao Chang Residual Stresses 2018 DOI: 10.21741/9781945291890-19 Show Abstract ▼ Abstract: The major challenge of Research in bone surgery is to develop strategies to repair large bone defects. Bone grafting technique is the gold standard to fill and heal these kind of defects. This work address the evolution of the mechanical properties as regard to bone regeneration microstructure. Managing such a time dependent (different regeneration step) and spatially resolved (strain field across natural/reconstructed bone interface) process is achieved through a quantitative analysis of the mechanical strain distribution supported by the mineral part of bone architecture (hydroxyapatite – Hap) and crystal microstructural features (size distribution, spatial pattern). SAXS/WAXS (Small- and Wide- Angle X-ray Scattering) experiments will highlight strain distribution respectively in the reconstructed bone’s collagen fibrils and minerals, through mechanical state mapping over a surgically created defect under in situ tensile testing on samples harvested at different regeneration stages.	Oct 2018
I02-Macromolecular Crystallography I22-Small angle scattering & Diffraction	The hierarchical response of human corneal collagen to load J. S. Bell , Sally Hayes , C. Whitford , J. Sanchez-Weatherby , O. Shebanova , C. Vergari , C. P. Winlove , N. Terrill , T. Sorensen , A. Elsheikh , K. M. Meek Acta Biomaterialia DOI: 10.1016/j.actbio.2017.11.015 Diamond Proposal Number(s): [12810, 11316] Open Access Show Abstract ▼ Abstract: Fibrillar collagen in the human cornea is integral to its function as a transparent lens of precise curvature, and its arrangement is now well-characterised in the literature. While there has been considerable effort to incorporate fibrillar architecture into mechanical models of the cornea, the mechanical response of corneal collagen to small applied loads is not well understood. In this study the fibrillar and molecular response to tensile load was quantified using small and wide angle X-ray scattering (SAXS/WAXS), and digital image correlation (DIC) photography was used to calculate the local strain field that gave rise to the hierarchical changes. A molecular scattering model was used to calculate the tropocollagen tilt relative to the fibril axis and changes associated with applied strain. Changes were measured in the D-period, molecular tilt and the orientation and spacing of the fibrillar and molecular networks. These measurements were summarised into hierarchical deformation mechanisms, which were found to contribute at varying strains. The change in molecular tilt is indicative of a sub-fibrillar “spring-like” deformation mechanism, which was found to account for most of the applied strain under physiological and near-physiological loads. This deformation mechanism may play an important functional role in tissues rich in fibrils of high helical tilt, such as skin and cartilage.	Nov 2017

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