Diamond Annual Review 2020/21

102 103 D I A M O N D L I G H T S O U R C E A N N U A L R E V I E W 2 0 2 0 / 2 1 D I A M O N D L I G H T S O U R C E A N N U A L R E V I E W 2 0 2 0 / 2 1 Soft CondensedMatter Group Robert Rambo, Science Group Leader T he Soft CondensedMatter (SCM) Group at Diamond Light Source is comprised of the HighThroughput Small Angle X-ray Scattering (SAXS) (B21), theMultimode Infrared Imaging andMicrospectroscopy (MIRIAM) (B22), SAXS and Diffraction (I22) and the Circular Dichroism (CD) Microspectroscopy (B23) beamlines at Diamond Light Source. This unique portfolio of instruments enables studies of non-crystalline materials at micro to meso-scale resolutions that include two-dimensional thin-films (photovoltaics), living mammalian cells, three- dimensional matrices (e.g. metal-organic frameworks, gels andwaxes) and nano-particles in non-crystalline states. The SCMgroup nowoffers mail-in services for SAXS and CDmeasurements throughUAS (User Administration System) announcements. In addition, I22, B22 andB23 offer off-line access to IRmicroscopy and imaging, CD spectroscopy and SAXSmeasurements. In the last year, the SCM Group contributed to 172 scientific publications, a 30.3% increase over 2020 with B21 increasing their publications to a new record of 83. SCM publications covered many aspects of healthcare including use of metal-organic frameworks in drug release, anti-microbial films and peptoids, diagnostic imaging and vaccine stabilisation at room temperature. Further publications looked at contributing factors associated with prominent diseases such as the role of intrinsically disordered proteins associated with Helicobacter pylori (stomach disease) and hepatitis C virus (liver disease), as well as specific proteins in Vibrio cholera (cholera), dengue virus, cancer, tuberculosis, infertility, Pseudomonas aeroginosa (disease associated with cystic fibrosis), heart disease, Alzheimer’s disease and malaria. Outside of healthcare, SCM instruments were critical to investigations examining self-assembled systems that included innovations in liquid crystals, nano-tubes, hydrogels, light-sensitive and functionalised graphene thin-films, nano-structured cages for carbon capture and industrial processes and improving perovskite stability in solar photovoltaics. The 2020 COVID-19 working restrictions created many challenges for our scientific community. In response, B21 and B23 optimised for mail-in experiments in support of COVID research, whereas B22 and I22 quickly invested in infrastructure to support both mail-in and remote experiments. At the start of the 2020 academic year, a new cohort of students joined our existing SCM doctoral students, which now include the Universities of Pisa (Italy), Surrey and Chalmers, Southampton, College London, Imperial, Sheffield, Reading, Leeds and Durham. SCMprovidedseveraltrainingworkshopsviaonlineplatforms including the popular S4SAS meeting led by I22, which had the prominent SAXS Professor Otto Glatter as keynote speaker. B22 organised a series of training workshops using machine learning software (Quasar) in infrared image analysis and B21 hosted a series of online, small group data analysis sessions for users, which is now a routine part of our user programme. 2020 has been a transformative year for all beamlines in SCM. B21’s mail-in services motivated a new web-interface for users to schedule and manage mail- in experiments through ISPyB. This will be extended to B23 and I22 in 2021. B23 increased its capacity to perform high-throughput CD experiments including automated thermal studies. I22 developed new sample environments for mail- in and remote experiments allowing users to set-up experiments for 1,000s of liquid and solid samples. B21 update B21 studies noncrystalline, randomly oriented particles using high- throughput approaches. SAXSmeasurements can bemade on any type of sample and in any physical state. The life sciences community comprises our largest user group since such measurements provide the opportunity to study biological machinesinconditionsthatarecomparabletotheirliquid,hydratedenvironment. During 2020, B21 provided over 70mail-in experiments that included research in COVID-19, RNA helicases, antibody complexes, gelation, photocatalysis, gelation, statins, stress proteins, oncogenes and biotech industry. In planning for Diamond-II (proposed upgrade programme), B21 commissioned the design and manufacturing of a new sample delivery environment that exploits laminar liquid flow. Radiation damage is a major contributor to measurement error in SAXS. Under the flow conditions used in size-exclusion chromatography coupled SAXS, the liquid flows much slower at the walls of the capillary used in the actual X-ray scattering measurement. The slow flowing liquid with protein leads to deposition of protein on the walls of the capillary (fouling) during X-ray exposure, contributing significantly to measurement background thus reducing the instrument’s sensitivity. The new co-flow device creates a flow of inert liquid around the sample that pushes the sample away from the walls of the capillary, thereby eliminating fouling. It can be expected that the performance of B21 in Diamond-II will lead to significant capillary radiation induced fouling. B22 update The Multimode Infrared Imaging and Microspectroscopy (MIRIAM) beamline B22 is used to assess the molecular composition andmicroscopic spatial distribution of a sample at the highest, optically-achievable resolution in the infrared (IR). B22 operates two end stations for scanning IR spectro-microscopy and IR imaging, with a suite of single and 2D detectors that seamlessly cover the whole IR range, fromnear-IR to mid-IR and further into terahertz (THz). B22 has been used in the analysis of inorganic-organic combinations in biomineralogy or composite materials, chemical degradation in conservation and archaeology, as well as studying live mammalian cells under the IRmicroprobe for in situ drug response, an important tool in anti-cancer research.This past year, B22 provided nano- andmicro-spectroscopy imaging experiments on rubber composites, pluripotent stem cells in cardiomyocytes, macrophage phenotyping, spinal cords, retinas and photovoltaics. In 2020, scientists from the University of Manchester led by Dr Martin Schröder developed a new separation method based on metal-organic frameworks (MOFs) to separate xylene isomers at low temperatures. Currently, industrial-scale xylene isomer separation requires fractional crystallisation at moderately high temperatures (>220 K). Xylenes are critical compounds inmany industrial sectors where lower temperature separation methods will lead to major reductions in energy consumption and waste. Dr Schröder’s group showed that bymodulating the chemical environment and internal pore size of MOFs, the MOFs can be used to effectively discriminate xylene isomers. B22 used its THz spectroscopy capabilities to look inside theMOFs and showdefinitive and specific uptake of xylenes in the non-crystalline material. The beamline made major changes in support of remote experiments with new IT hardware and changes in working protocols. B22 continues with collaborative calls for IR nanospectroscopy in photothermal mode (AFM-IR) by synchrotron radiation (SR). This cutting-edge method is suitable for molecular analysis of submicron to micron scale organic matter and biomaterials - from mammalian cells to microplastic - with exceptional sub-micron resolution (i.e. up to 100 times below the IR wavelength scale). However, B22 will be commissioning a new AFM end station (summer 2021) that will allow tapping AFM-IR and scattering Scanning Optical Microscopy (s-SNOM) measurements by SR. The modernisation will improve data acquisition rates and spatial resolution, allowing IR nanospectroscopy to be performed at tens of nanometers resolution. B23 update The B23 synchrotron radiation Circular Dichroism (CD) beamline uses circularly polarised light to characterise the structure-architecture of complex chiral materials in solution and in solid-state thin films. Chiral materials have a handedness (like our right and left hands that are not superimposable) and absorb differently the circularly polarised light, generating CD fingerprint ID spectra. For optoelectronic materials, the measurement of CD at 50 μm of spatial resolution can inform about the homogeneity of the supramolecular structure, which is strictly related to their efficacy. For biological samples, CD is also used to monitor in microfluidic chips structural changes, drug binding, protein instabilities as a function of temperature, pressure, ionic strength, surfactant, pH, ligand interactions and ageing. Pioneered by the B23 team, CD Imaging (CDi) technology exploits a highly collimated, synchrotron microbeam for scanning thin-films of solid materials. Unlike absorption, CDi can inform on the homogeneity of the chiral supramolecular structure. Led by Dr Jessica Wade (Imperial College London), new research in polymers showed that large-scale chiral properties can emerge from self-assembling of achiral polymers doped with small chiral molecules. This represents a breakthrough in material engineering for spintronic devices and high-performance electronic displays. CDi at B23 is the only synchrotron- based instrument with the required sensitivity to guide the researchers on how to improve the properties of chiral materials. Combined with Diamond’s high- resolutionmicroscopy, B23 is a unique worldwide facility for material science and life sciences. I22 update The Small Angle Scattering and Diffraction beamline (I22) offers combined SmallandWideAngleX-rayScattering(SAXSandWAXS)studiesonarangeof low order biological, natural and synthetic samples. I22 excels at providing structural information on partially ordered materials, ranging from colloidal nanoparticles and thin-films to large hierarchical structures such as bone. During COVID-19 restrictions, I22 supported 18 individual user visits distributed as 10 remote and eight on-site visits. However, in support of mail-in operations, I22 supported 45 additional user visits utilising bespoke sample environments for high-throughput experiments on solid and liquid samples. I22 completed its major Beam Condition Optics (BCO) upgrade project allowing for precise and stable control of a microfocus X-ray beam for SAXS. The new optical layout has significantly reduced divergence for microfocus experiments and has provided access to much lower q (scattering vectors) than previously available. The upgrade has been a step change in mapping experiments particularly examining deformation in bones and eye lenses. I22 upgraded its bimorph mirror controller in 2020 to complement the BCO upgrade and also sought approval of a new double crystal monochromator (DCM) to upgrade its original 2007 DCM. The new DCM is due for installation in June 2021 along with an upgraded, in-vacuumWAXS detector. The I22 Principal Beamline Scientist Dr Nick Terrill, in collaboration with Prof Michael Rappolt from the School of Food Science and Nutrition at the University of Leeds, manage an Engineering and Physical Sciences Research Council (EPSRC) grant to support an offline SAXS facility at Diamond. The Multi-User Facility for SAXS/WAXS (DL-SAXS) now has an installed Xenocs Xeuss 3.0 instrument operating with an Eiger-2R 1M detector. The facility is under commissioning and will accept a limited number of users in 2021.This instrument will be critical to the SCM Sample Environment Development Laboratory for independent development/testing of sample environments prior to beamtime. Studying materials under intended use, such as lubricants under frictional strain or simply the stretching of a novel bioengineered material requires bespoke sample environments. Testing these sample environments prior to beamtime drives innovation and optimises the available beamtime.