Imaging and Microscopy Group Update 2023-24

The Imaging and Microscopy Group at Diamond

DIAD

The DIAD (Dual Imaging and Diffraction) beamline is a pioneering facility designed to provide simultaneous imaging and diffraction capabilities for advanced material and biological research. The beamline features a unique dual-beam setup, where one beam is optimised for high-resolution imaging, allowing for detailed visualisation of internal features and defects, while the other beam is tailored for diffraction, providing insights into the crystalline structure and phase composition. This dual capability facilitates comprehensive analysis, making it possible to correlate structural properties with material performance and behaviour under various conditions. It supports both static and dynamic studies, enabling time-resolved experiments that can capture the evolution of materials under stress, temperature changes, and other environmental factors.

DIAD is particularly well-suited for studies in materials science, engineering, geology, and biology, where understanding the interplay between microstructure and macroscopic properties is crucial. Researchers can use the beamline to investigate a wide range of phenomena, from the mechanics of new alloys and composites to the behaviour of biological tissues and the microstructure of natural minerals.

The Joint Engineering, Environmental and Processing (JEEP) beamline produces high energy X-rays (53-150 keV) enabling imaging and diffraction of large or dense samples. I12 continued its exciting science programme, collaborations, and development. New research carried out at the I12 involved real-time in situ observation of chemical processes using synchrotron X-ray powder diffraction and Raman spectroscopy and joint experiments with ISIS neutron facility in the areas of material, life, and heritage sciences.

A number of new developments offer new capabilities for users. A high speed camera for fast X-ray imaging and tomography which will replace the older equipment and provide a gain in both frame rate and sensitivity, keeping I12 at the cutting edge. A new stage for in situ experiments was also implemented enabling mechanical characterisation during experiments.

The I13-2 Diamond Manchester Imaging beamline is focussed on micro-and nano-tomography and provides, in connection with the I13-1 Coherence beamline, multiscale imaging capabilities over three orders of magnitude in resolution. The beamline operates in the 8-30 keV energy range, offering a variety of imaging capabilities including in-line phase contrast imaging, full-field microscopy and grating interferometry. In-line phase contrast is typically applied to millimetre-sized objects, with zooming capability using different detector objectives. Over the last year the high-throughput capability has been increased, improving the gripper mechanism of the sample changer robot and measuring up to 100 samples per eight hour shift. The grating interferometer allows measurement of the refractive index of materials with high sensitivity, important in particular for the segmentation of data. With the full-field microscope, we achieve 80nm resolution on 80μm samples and with data collection times of a few minutes. Work is ongoing to improve the Zernike phase contrast imaging method for the collection of high quality data with high contrast. The I13 OCTOPI upgrade project describes the ambitions for multiscale and operando imaging, and we are currently improving the instrumentation in sight of the Diamond-II upgrade.

I13-1 coherence beamline is a hard X-ray beamline, operating in the 6-20 keV range. The beamline specialises in high-speed, multiscale and multimodal coherent diffraction imaging and ptychography in both transmission and Bragg geometries. These methods provide nanoscale resolutions with a quantitative phase contrast and can often be combined with other methods, such as tomography and XANES, and complementary signals, such as fluorescence and diffraction mapping. The beamline supports users from all backgrounds and a wide range of research areas, from materials science to bio-imaging, allowing the community to apply these powerful analytical tools to their specific scientific challenge.

In recent years there has been a big effort at the beamline to increase the scanning speeds and imaging throughput. This is particularly important as we look towards the Diamond-II upgrade and the increase in source brilliance. Recent publications from the beamline are beginning to demonstrate how our developments open the possibility for in operando studies and imaging of larger volumes of material at the nanoscale, with applications across the life and physical sciences.

The Scanning X-ray Microscopy beamline (I08) is for morphological, elemental and chemical speciation on a broad range of organic-inorganic interactions in a 250 - 4400 eV photon energy range, and sample investigations under ambient conditions. I08 has a range of applications including biological and biomedical sciences, earth and environmental science, geochemistry, and materials science. I08 has improved and partially automated and simplified user operation and current developments look to enable more in situ and in operando research.

The new soft X-ray spectro- and tomo-ptychography branchline I08-1 (operating iin the 250-2000 eV photon energy range) is growing in capabilities and has been enthusiastically received by initial users with clear benefits for experiments for many experiments transitioning from I08 to I08-1. Key developments for I08-1, such as providing access to the carbon edge for ptychographic studies are well under way and key developments focus on multi-dimensional spectroscopic ptychographic imaging of light elements including variable polarisation of X-rays.

I14, the Hard X-ray Nanoprobe beamline, provides a focussed beam of 50 nm for high resolution imaging of a wide range of samples using multiple techniques including X-ray fluorescence, diffraction, X-ray Absorption Near Edge Structure (XANES), differential phase contrast imaging and ptychography. The beamline continues to improve the data processing workflows, providing live processing pipelines to enable fast visualisation of results. Recent developments have further optimised the tomography capabilities, from maple mounting through to reconstruction tools, allowing easier three dimensional imaging of morphologies and elemental distributions. The beamline has a strong focus on in situ characterisation and provides environments for gas flow, heating, liquid and electrochemistry, while the flexible endstation space enables integration if customised user sample environments.

The electron Physical Science Imaging Centre (ePSIC) at Diamond consists of two transmission electron microscopes, a JEOL ARM 200 and a JEOL GRAND ARM 300, which were brought to Diamond through a collaboration with Johnson Matthey and the University of Oxford respectively. The ARM 200 is a state-of-the-art probe-corrected analytical microscope capable of X-ray spectroscopy and atomic resolution electron energy loss spectroscopy with a recently upgraded Gatan Continuum K3 spectrometer. The ARM 300 is a dedicated imaging instrument aligned across a wide range of accelerating voltages (30 - 300 keV) and is equipped with an Oxford Instruments X-Max 100 EDX detector. It is both probe- and imaging-corrected and has numerous detectors, including a small pixel array (512 x 512) fast direct electron detector for low voltage work and a large pixel array (4K x 4K) fast direct electron detector for high voltage imaging. These combined capabilities make this a unique resource for electron microscopy within the UK. With in situ sample holders, users at ePSIC can perform variable temperature measurements from 100 to 1600 K, apply electrical bias to samples during imaging and transfer samples anaerobically into the microscope. For TEM sample preparation ePSIC runs a JEOL 4700F focused ion beam microscope with in situ lift out and anaerobic transfer capability. The state-of-the-art instrumentation available at ePSIC attracts both established electron microscopists looking to develop new techniques, and scientists with limited previous electron microscopy experience interested in the atomic structure of their samples.