Using Deben µXCT Stages to Characterize Multiple Engineering and Natural Materials at The University of Oxford Materials Department

2 May 2017
Weylan Kiam-Laine
Microbiologist

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Deben, a leading provider of in-situ testing stages together with innovative accessories and components for electron microscopy, reports on how the Marrow group in the Materials Department at the University of Oxford applies Deben’s mechanical stage for in situµXCT studies of multiple engineering and natural materials.

Professor James Marrow leads a research group specializing in the structure-property relationship of a broad range of engineering and natural materials. Based in the Materials Department at the University of Oxford, Marrow's team use high resolution X-ray computed tomography to make in situ studies of three-dimensional deformation and damage (e.g. digital volume correlation), with a particular interest in materials for energy. Research in engineering materials for energy generation is not a quick-fix topic. New materials can take from 15-20 years to come into use and then are expected to be in service for 40-80 years. The key physical mechanisms that determine manufactured performance, and how these properties age in service, are not very well understood, and mistakes in materials selection can have enormous financial and social implications. Prediction is a major challenge and thus a deep understanding of the fundamental mechanisms of materials aging and how it affects damage tolerance is essential to identify and avoid potential “cliff-edges” in future materials performance.

Testing is based in house and using the Diamond Light Source synchrotron x-ray facility at Harwell. The range of materials studied is quite remarkable; from graphite and ceramic composites for nuclear energy to interfacially-toughened polymer composite laminates for aerospace; from the study of eggs shells to samples of human bone. With experiments running from a few hours to several days, it does not come as a surprise to learn that the CT facility is running 24/7. The micro CT system is a ZEISS Xradia 510 Versa. This provides a two-stage magnification technique to enable high resolution at a distance (RaaD). In the first stage, the sample image is enlarged through geometric magnification as with conventional micro-CT. In the second stage, a scintillator converts X-rays to visible light, which is then optically magnified. Reducing dependence upon geometric magnification enables the Versa to maintain submicron resolution at large working distances, which is essential for in situ observations of mechanical testing.

The figure shows a silicon-carbide ceramic composite that is designed for future accident tolerant nuclear fuels. In situ mechanical loading has been applied to create an internal pressure, which eventually initiates cracks from the larger pores within its woven structure. The digital volume correlation analysis of the tomographs reveals cracks as strains (color), and the sequence and pattern of their nucleation and growth is used to test high fidelity models that predict how changes in microstructure affect the structural integrity of the material.

The Deben Microtest CT tensile stages for µXCT systems allow samples to be examined using customized load cells in the range from 150 N up to 5000 N (5kN). Custom versions are available with Peltier heating & cooling from -20 °C to +160 °C, extended stroke and travel. To obtain full details of the Deben applications and product portfolio, please visit www.deben.co.uk

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X-Ray Diffraction and SpectroscopyX-Ray diffraction & spectroscopy are used in material characterization to discern the structure and elemental composition of a sample. X-Ray diffractometers (XRD) are superior instruments in elucidating the dimensional atomic structure of crystalline materials, including powders, thin films and single crystals. For large unit cells or ordered macromolecules, consider small-angle X-ray scattering (SAXS). X-ray spectroscopic techniques include X-ray fluorescence (XRF) and X-ray photoelectron spectroscopy (XPS), both providing simple and accurate methods for determining the elemental composition of a material. Energy dispersive (EDXRF) and wavelength dispersive (WDXRF) XRF spectrometers are available, as well as handheld/portable devices. High-resolution, 3D microstructure characterization of materials can be achieved with X-ray microscopes combining sub-micron resolution imaging with 3D computed tomography. Find the best XRD and XRF spectrometers in our peer-reviewed product directory: compare products, check customer reviews and receive pricing direct from manufacturers.Light MicroscopyLight microscopes or optical microscopes are used to visualize microscale objects under magnification, including cells, clinical specimens and materials. Lab equipment for light microscopy includes confocal microscopes, fluorescence microscopes, zoom and stereo microscopes. Microscope slides and imaging reagents are available for visualizing samples, as well as various microscope stages and incubators for large or temperature-sensitive samples. Find the best light microscopes in our peer-reviewed product directory: compare products, check customer reviews and receive pricing direct from manufacturers.Electron MicroscopyElectron microscopes (EM) are used to create high-resolution images of samples at the nanoscale by means of an accelerated beam of electrons as a source of illumination. Types of electron microscope include scanning electron microscopes (SEM), transmission electron microscopes (TEM), scanning transmission electron microscopes (STEM) and cryo-electron microscopes. Focused ion beam (FIB) microscopes are useful for modifying or milling a sample surface with nanometer precision, as well as imaging. Find the best electron microscopes in our peer-reviewed product directory: compare products, check customer reviews and receive pricing direct from manufacturers.Polymeric MaterialsPolymeric materials are widely used in industries ranging from biomedical devices to packaging and electronics. Research into these materials focuses on their properties, including strength, flexibility, and degradation. Advances in polymer science have enabled the development of more sustainable and high-performance materials. Explore the best polymeric material products in our peer-reviewed product directory; compare products, check reviews, and get pricing directly from manufacturers.NanomaterialsNanomaterials such as carbon nanotubes, fullerenes and nanoparticles are a group of materials that measure between 1-1000nm for a single unit. Analysis techniques include AFM, electron microscopy and super resolution microscopy.Silicon
Using Deben µXCT Stages to Characterize Multiple Engineering and Natural Materials at The University of Oxford Materials Department