Surface vs bulk analysis The value of solid state materials characterisation techniques, including: • Sample size • Site specific analysis • Surface vs bulk composition The student should be able to  Describe why surfaces can have different composition from bulk materials  Understand that a single technique is often not sufficient for fully characterizing a material  Understand that there are a very large number of techniques that give subtly different information about a solid sample

Surface vs bulk analysis The value of solid state materials characterisation techniques, including: • Sample size • Site specific analysis • Surface vs bulk composition The student should be able to  Describe why surfaces can have different composition from bulk materials  Understand that a single technique is often not sufficient for fully characterizing a material  Understand that there are a very large number of techniques that give subtly different information about a solid sample

Energy & Wavelength Dispersive Spectroscopy • Electron-specimen interactions II • Characteristic X-rays • X-ray detection in WDS and EDS • Spectral features • Quantification The student should be able to  Describe the signals generated when an electron beam hits a solid sample – continuous and characteristic X-Rays  Recognise and identify features in an EDS spectrum and explain the source of artefacts  Describe the advantages/disadvantages of EDS vs WDS  Understand the first approximation of quantification and explain why it is insufficient (and what steps are taken to address this, ie ZAF corrections)  Suggest suitable sample preparation routes for microanalysis of various samples

Electron Back Scatter Diffraction • Components of EBSD instruments • EBSP generation • Sample preparation The student should be able to  Describe the source of EBSP and orientation contrast imaging  Suggest suitable sample preparation routes for EBSD analysis of various samples

Focussed Ion Beam • Basic components of FIB and dual beam instruments • Sectioning and imaging generation • FIB preparation of TEM samples The student should be able to  Describe the basic operation of a dual beam FIB instrument  Suggest possible applications to a variety of samples

Surfaces • Concept of surfaces • Ideal vs real surfaces • Surface relaxation and reconstruction • Interfaces The student should be able to  Describe the ways in which a surface may be terminated.  Describe how relaxation and reconstruction of surfaces can minimise the surface free energy.  Recognise that real surfaces can be much more complex than idealised single crystal surfaces.  View interfaces as another type of surface.  Recognise that the surface region may differ from the bulk in both structure and composition.

X-ray photoelectron spectroscopy • Information content • Survey and Core-level scans • Spectral interpretation • Instrument design • Sampling depth • Sample preparation The student should be able to  Describe the type of information available from an XPS spectrum.  Understand that XPS probes a very shallow surface region, and be able to identify ways of increasing or decreasing the surface sensitivity.  Explain why XPS is a UHV technique and how this impacts sample preparation.  Identify spectral lines in an XPS spectrum and assign them to their transitions.  Be able to distinguish between photoelectron and Auger electron peaks.  Identify the major components of an XPS spectrometer.  Understand what needs to be done to analyse insulting samples and how this affects data analysis.  Quantify a survey XPS spectrum to provide atomic concentration information.  Quantify a core level XPS spectrum to determine chemical state information.  Understand how the thickness of thin overlayers may be calculated.

X-ray photoelectron spectroscopy • Information content • Survey and Core-level scans • Spectral interpretation • Instrument design • Sampling depth • Sample preparation The student should be able to  Describe the type of information available from an XPS spectrum.  Understand that XPS probes a very shallow surface region, and be able to identify ways of increasing or decreasing the surface sensitivity.  Explain why XPS is a UHV technique and how this impacts sample preparation.  Identify spectral lines in an XPS spectrum and assign them to their transitions.  Be able to distinguish between photoelectron and Auger electron peaks.  Identify the major components of an XPS spectrometer.  Understand what needs to be done to analyse insulting samples and how this affects data analysis.  Quantify a survey XPS spectrum to provide atomic concentration information.  Quantify a core level XPS spectrum to determine chemical state information.  Understand how the thickness of thin overlayers may be calculated.

Synchrotron methods • Synchrotron light sources • Insertion devices • Types of experiments possible with synchrotron light • X-ray absorption spectroscopy • Synchrotron IR spectroscopy The student should be able to  Explain the differences between X-rays produced at a synchrotron and with a laboratory source.  Describe the types of devices used for producing synchrotron light.  Explain how the tunability of synchrotron X-rays provide more information than a lab XPS.  Explain how XAFS and XANES provide information about short-range order.  Qualitatively describe the steps involved in data reduction for XANES and XAFS.  Explain why synchrotron IR gives higher sensitivity.  Explain how XRD using synchrotron X-rays differs from a conventional lab source.  Describe the information provided by small and wide angle X-ray scattering (SAXS/WAXS).

Transmission Electron Microscopy • The transmission electron microscope: general function, apertures, resolution, lens errors, specimen preparation • Reciprocal lattice concepts, diffraction, Ewald sphere, , bright field (BF) and dark field (DF) image, selected-area diffraction (SAD), convergent-beam electron diffraction (CBED), Kikuchi lines • Image Contrast, two beam theory, • High resolution transmission electron microscopy (HRTEM) • Scanning transmission electron microscopy and High angle annular dark field (STEM & HAADF) image • Electron energy-loss spectroscopy (EELS) and Energy-filted TEM (EFTEM) • Cryogenic TEM (Cryo-TEM) • Electron tomography The student should be able to  Understand the operation of a TEM and how to obtain a selected area diffraction patterns (SADPs), convergent-beam electron diffraction (CBED) & bright field (BF) and dark field (DF) images  Construct a cubic reciprocal lattice  Understand the kinematical theory of electron diffraction, construct the Ewald sphere, construct cubic diffraction patterns and index a given cubic pattern  Understand the formation of Kikuchi lines  Understand the theory of image contrast, and how to achieve two beam condition  Understand the theory of HRTEM and STEM, and explain the difference between high resolution transmission electron microscopy and atomic resolution scanning transmission electron microscopy images. • Understand the theory of Electron energy-loss spectroscopy (EELS) and Energy-filted TEM (EFTEM), and explain the difference between Energy-dispersive x-ray spectroscopy (EDXS) and Electron energy-loss spectroscopy (EELS)  Discuss other techniques, such as cryo-TEM, electron tomography, and in-situ TEM