Soft Condensed Matter Group Update 2023-24

The 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 and waxes) and micro/nano-particles (e.g. micro/nanoplastics) in any condensed matter 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 with 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 151 scientific publications covering a broad range of disciplines including chemistry, material science, chemical engineering, physics and astronomy, biochemistry, genetics and molecular biology and engineering.

In addition, SCM group provides off-line CD, InfraRed and SAXS measurements via peer-review applications and rapid access. The SCM Group maintains a dedicated laboratory space for visiting users. The laboratory houses vital equipment for sample preparation and analysis such as a centrifuges, 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 maintain the Refyn mass photometer for single particle mass characterisations to complement our size-exclusion chromatography coupled, multi-angle light scattering (MALS) system (Wyatt and Agilent) and house two incubators for supporting plant-based experiments.

A new cohort of students joined our existing SCM doctoral students which now include the Universities of Surrey and Chalmers, Southampton, King’s College London, Imperial, Sheffield, Cranfield, Reading, Leeds Cambridge, University College London and Durham. SCM provided 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.

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 completed its WAXS detector upgrade with installation of 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 °C), the new SEU allows for routine measurements between (-4 and 120 °C) where temperature ramping can be programmable and tightly controlled through active cooling. The new SEU is ideal for studying phase behaviour of proteins, waxes, gels and other polymer blends. In addition, a new SEC-SAXS cell is being designed that will reduce sample dilution with a > 10-fold decrease in background scatter. B21 also welcomes a new post-doctoral research associate, Barbara Gerbelli, PhD. Dr Gerbelli will oversee the B21 automation project and provides expertise in lipid nanoparticles.

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 2D 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’s PBS, Dr Gianfelice Cinque and Beamline Scientist, Dr Mark Frogley, were award the Royal Society of Chemistry Dalton Horizon prize for research on functional materials in collaboration with Professors Martin Schroder and Sihai Yang of the University of Manchester. The research investigated gas-solid interactions using a novel sample environment at Diamond. Dr Frogley has led a project at Diamond for developing sample environments that utilise aggressive gases at high temperatures that improved signal-to-noise ratio by greater than 20x.

B22 continues to develop a novel optical system for beam-shaping led by Dr Vishnu Muruganandan. In collaboration with SciML and Ada Lovelace Centre, this work aims to improve the beam quality for hyperspectral microscopy, increasing the overall field of view and sensitivity of the instrument. We expect the deformable mirror project to be accessible to users in 2024. Finally, our upgrade in IR nanospectroscopy in photothermal tapping and contact modes, plus scattering-SNOM is completed and the instrument is available to users through our standard Peer-review Proposal calls.

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: module A and B to accommodate a variety of sample environments. Module A operates in the 170-500nm region (125- 500nm for gas phase) utlising 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 custom made 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 50 micron 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.

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, purchased through an Engineering and Physical Sciences Research Council (EPSRC) grant a liquid-metal jet SAXS instrument (Xenocs Xeuss 3.0) with an in-vacuum Eiger-2R 1M detector that is now fully enrolled in the Diamond User program. The facility accepts peer-reviewed panel (PRP) and rapid access proposals for experiments 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.

I22 installed a new Vortex-60EX silicon drift fluorescence detector that is permanently installed at the beamline. The instrument is available on demand and adds additional elemental information to complement micro-focus mapping SAXS experiments. The X-ray fluorescence detector can also aid in improve background corrections for samples that contain substantial fluorescence when measurements are performed above their absorption edges.

B21: Intercepting the Inflammation Signal

B22: Good vibrations again: MOFs may be the key to scavenging mechanical energy

B23: Bleomycin: cancer drug with a hidden flaw

I22: Cooking Residues Can Cling on to Indoor Pollutants

LabSAXS: From Greenhouse Gas to Green Synthesis: CO₂ as a Raw Material for Next-Generation Polymers