XPS (X ray photoemission spectroscopy) ESCA (Electron XPS（X射线光电子能谱ESCA（电子）.ppt

XPS (X ray photoemission spectroscopy)/ESCA (Electron Spectroscopy for Chemical Analysis) XPS Theoretical consideration Z dependence Main features of XPS Three Step Model Inelastic scattering XPS peak identification Spin-Orbit splitting: Core Level Chemical Shifts Shake-up and shake-off Some general rules Multiplet splitting and shake-up/shake-off lines are generally expected in the paramagnetic states: MnO XPS spectra Multiplet satellite Energy loss lines Energy of Light X-ray tube A common Dual anode X-ray tube X-ray spectrum from x-ray tube Typical X-ray anode material (Mg and Al) X-ray satellites “ghost peaks” Monochromatic X-ray Synchrotron Radiation Sample charging effects Inhomogeneous Surface Charging Charge Compensation Quantitative analysis How to measure the intensity Instrumentation (analyzers) Hemispherical Analyzer Hemispherical Analyzer Angular resolved XPS Surface sensitivity change due to angle and photon energy AES vs. XPS The synchrotron storage ring is a tubular vacuum chamber made to: Hold an electron beam travelling through it at nearly the speed of light. Maintain the high energy of the electron beam. As the accelerating electrons circle the ring at relativistic velocities, they give off intense beams of light including x-rays. By using a monochromator the light will be Monochromatic. Key properties of synchrotron radiation: high intensity tunability in wide range near-coherence polarized. pulsed well collimated NUS has such a source in Singapore! The light for XPS always charges surface positively (shifting of spectrum to higher binding energy) and leads to general instability (spectral noise). For the metal sample, which can be grounded and the charges can be quickly gone. However, for insulator, this effects are serious and need to be treated. C 1s shifts due to the charging For XPS (even AES) never forget ground the sample !!! Charging can even change the line shape due to Inhomogeneous Surface Charging, which have different positive