Diamond Light Source - Annual Review 2022/23

62 63 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 2 / 2 3 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 2 / 2 3 Soft CondensedMatter Group Robert Rambo, Science Group Leader T he Soft Condensed Matter (SCM) Group is comprised of the High Throughput SAXS (B21), the Multimode Infrared Imaging and Microspectroscopy (MIRIAM) (B22), SAXS and Diffraction (I22) and the Circular Dichroism Microspectroscopy (B23) beamlines, co-located in zones 3 and 4 of Diamond. This unique portfolio of instruments enables studies of amorphous to noncrystalline materials at nano- to meso- scale resolutions that include two-dimensional thin-films (photovoltaics, OLEDs), living mammalian cells, three-dimensional matrices (e.g. metal- organic frameworks, gels andwaxes) andmicro/nano-particles (e.g. micro/nanoplastics) in any condensedmatter states. SCM science is “the science that underpins continued improvements to quality of life” and was critical to the rapid development of the COVID vaccines from Pfizer-BioNTech and Moderna. The SCM user community is international, nearly 70% of our peer-reviewed allocated beamtime were awarded to users from the United Kingdom where the remaining time is shared largely between member states of the European Union, United States, China, Canada, Japan, Israel, and Australia. In the last year, the SCM Group contributed to 132 scientific publications covering a broad range of disciplines including chemistry, material science, chemical engineering, physics and astronomy, biochemistry, genetics and molecular biology and engineering. SCM group now provides off-line CD, InfraRed and SAXS measurement via peer-reviewapplications and rapidaccess.The SCMGroupmaintains adedicated laboratory space for visiting users. The laboratory houses vital equipment for sample preparation and analysis such as a centrifuge, a biosafety level 2 facility, spectroscopy equipment and the ability to work with different gases plus a cell culture lab for mammalian tissues (associated to B22). We acquired a new mass photometer by Refyn for single particle mass characterisations to complement our size-exclusion chromatography coupled, multi-angle light scattering (MALS) system (Wyatt and Agilent). In addition, we now house two incubators for supporting plant-based experiments. In collaboration with the DIAD beamline headed by Dr. Sharif Ahmed, SCM group will play a central role in building the food sciences and security user community at Diamond. Diamond-II Machine Physics group has identified lattice dipole- quadrupoles (DQ) as suitable soft photon sources for B22 and B23. B22 shall see a significant increase in the available terahertz radiationwith an~1.3x increase in flux across the terahertz-to-infrared range producing one of the largest broad band sources spanning 3 decades in wavelengths for vibrational microscopy and imaging. Currently, we are investigating bespoke vacuumvessel designs for extracting the radiation and new front-end mirrors for directing the radiation through the existing port that separates the beamline from the synchrotron storage ring. A new cohort of students joined our existing SCM doctoral students which now include the Universities of Pisa (Italy), Surrey and Chalmers, Southampton, King’s College London, Imperial, Sheffield, Reading, Leeds Cambridge, and Durham. SCMprovided several training workshops including the popular S4SAS meeting led by I22. B22 organised an advanced hyperspectral analysis and data processing training workshop with Soleil and Lubjiana University using machine learning software (Quasar) in IR image and spectroscopy analysis and B21 hosted a series of online, small group data analysis sessions for users which is now a routine part of our user program. In addition, we hosted the FoodBioSystems DTP partner event in October 2022. The event introduced Diamond’s capabilities and resources to a new user community and included Aberystwyth University, Brunel University, Cranfield University, Queen’s University Belfast, University of Reading and University of Surrey. The event attracted ~70 attendees and featured speakers from eBIC (Dr. Yuriy Chaban and Dr. Alisa Powell), I18 (Dr. Konstantin Igniatev) and DIAD (Dr. Sharif Ahmed). B21 Update B21 studies noncrystalline, randomly oriented particles using high- throughput approaches. SAXS measurements can be made 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 machines in conditions that are comparable to their liquid, hydrated environment. B21 started two major upgrades to be completed by 2023: 1) an automation project that will enable high-throughput studies of semi-solid materials and 2) WAXS detector upgrade. B21 pioneered mail- in SAXS services for UK and EU users. Prior to the COVID restrictions, mail-in experiments were limited to biological, liquid samples but was expanded to general soft condensed matter samples. The automation project will enable higher throughput of semi-solid materials using a 6-axis Meca500 robotic arm available through mail-in and peer-review proposals. The WAXS detector upgrade will be provided by an in-vacuum Eiger 1M detector. The increased, observed scattering range will further support SCM experiments on B21 whilst also adding additional capabilities to the sample environment unit (SEU). Currently, B21 experiments are performed at fixed temperatures (<60 ℃ ), the new SEU will allow for routine measurements between (-4 and 120 ℃ ), ideal for studying phase behaviour of proteins, waxes, gels and other polymer blends. In 2021, B21 commissioned a new SEU that enabled simultaneous UV- visible light illumination of the sample during X-ray exposure which has now produced its first paper examining time-resolved, photo-switchable polymers for solar fuels (Tyagi et al, JACS Au 2022, 2, 12, 2670-2677). B22 Update The Multimode Infrared Imaging and Microspectroscopy (MIRIAM) beamline, B22, is used to assess the molecular composition and microscopic 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 2-D detectors that seamlessly cover the whole IR range, from near-IR to mid-IR and further into 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 IR microprobe for in situ drug response, an important tool in anti-cancer research. This past year, B22 provided nano- and micro-spectroscopy imaging experiments studying detection of volatile acetone by MOFs (10.1002/ admi.202201401) as molecular sensors, understanding host-parasite interactions at cellular and subcellular levels using infrared microspectroscopy imaging (10.3390/cells11050811) , following the photo-oxidation catalysis of methane to methanol (a key reaction for increasing energy density) (10.3390/ cells11050811) and application of terahertz spectroscopy for studying zeolitic imidazole framework (ZIF-71), a large, 816-atom porous nanomaterial ideal for gas capture, catalyst and molecular sensing (10.1021/acs.jpclett.2c00081) . B22 acquired two new team members, Dr. Hendrik Vondracek and Dr. Vishnu Muruganandan. Dr. Vondracek will be the Senior Support Scientist overseeing the new atomic force microscopy coupled to IR end-station. Dr. Vondracek was a post-doctoral fellow at the IR beamline (SISSI) at Elletra (Triesta, Italy) with experience in s-SNOM as well as THz research in biological/ biofunctionalised system ( new and enhanced technical capabilites at B22, respectively). Collaborative calls for IR nanospectroscopy in photothermal tapping and contact modes, plus scattering-SNOM. AFM-IR will be available during the ongoing commissioning of the instrument aiming to a dedicated call for commissioning/collaborative users in early 2024. In addition, B22 published a technical development paper on the application of deformable mirrors to improving the synchrotron source for illumination in IR hyperspectral imaging by Focal Plane Array detector (10.1364/OL.456049) . This work demonstrated the potential of beamshaping using a double set of deformable mirrors that will be further developed in collaboration with the machine learning group at STFC (SciM, headed by Dr. Jeyan Thiyagalingam) and Dr. Muruganandan, our new post-doctoral research fellow. Dr. Muruganandan has experience in telescope-based image-processing algorithms for star tracker and multispectral camera, including adaptive optics and algorithms to image and characterise artificial satellites B23 Update B23 is our beamline for synchrotron radiation Circular Dichroism (CD) and Mueller Matrix Polarimetry (MMP). B23 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. The beamline operates two end-stations:moduleAandB to accommodate a variety of sample environments. Module A operates in the 170-500nm region (125- 500nm for gas phase) utilising an automated 6-cell turret for protein UV denaturation and/or thermal stability assays, a motorised XY stage to accommodate either microfluidic chips for the separation of proteins by diffusion or a custommade 96-cell multiplate to characterise the biomolecules conformational behaviour and ligand binding screening. Since 2020, module B operating in the 190- 650nm spectral region is equipped with the Mueller Matrix Polarimeter (MMP) to study the optical (linear dichroism (LD), circular birefringence (CB)) and chiroptical properties (circular dichroism (CD), and circular birefringence (CB)) of thin films of chiral materials such as polymer, biopolymers, optoelectronics, hydrogels, and twisted liquid crystals. For optoelectronic materials, the measurement of CD at 50micron 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 for MMP measurements. MMP 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. B23, through the PBS Prof. Giuliano Siligardi and Dr. Tamás Jávorfi (senior beamline scientist), participate in an international collaboration, The Chiral Materials Team, which was awarded the 2022 Horizon Prize (Stephanie L Kwolek Award) by the Royal Society of Chemistry. The award recognises their discovery that chiral organic materials can control photon and electron spin to high degree, an important attribute for future computer memory, 3D displays and other spintronic devices. This discovery was made possible through the world-leading MMP instrument uniquely operating at B23. B23 will see the installation of a new monochromator in 2023 that was designed in-house with our engineering support groups and Dr. Tamás Jávorfi and Dr. Giuliano Siligardi (PBS). The upgrade will improve beam stability and spatial resolution for imaging experiments. I22 Update The Small Angle Scattering and Diffraction beamline (I22) offers combined Small and Wide Angle X-ray Scattering (SAXS and WAXS) studies on a range of 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. 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) provides a Xenocs Xeuss 3.0 instrument operating with an in-vacuum Eiger-2R 1M detector. The facility accepts Peer-reviewed Panel (PRP) proposals for 25% of its available time with the remaining time dedicated to University of Leeds and sample environment development (SED). The SED laboratory is supported by Dr. Paul Wady and is key to enabling new science within the SCM group. SED has already supported experiments studying iron oxide formation on electrode surfaces (Cambridge University), using an acoustic cell to investigate crystal nuclei (Univeristy of Leeds) and cubosome formation and application to targeting cancer cells (University of Leeds). I22 began an automation project in 2022 that will use robotics to measure samples stored in a sample hotel co-located at the beamline. The beamline end-station required significant renovation to accommodate cabling, sample hotel and tracks that mobilise the robotic arm. This automation project will store ~5.000 samples in capillaries or DSC pans and take advantage of camera lengths during unsociable hours. Users often require different camera lengths depending on the hierarchical scale under investigation. In some cases, on-site users may have a camera length configuration required by a queued sample and the automation will be designed to efficiently take advantage of on-site user specific camera configurations. Attendees to the S4SAS conference in September 2022.