Spectroscopic Methods for Materials Characterization

Mentor:Dmitri Podgorny
Revision:15 Dec 2013

Course Summary

Experimental studies carried out by spectroscopic methods and techniques for analyzing the information obtained can be given strong modern analytical framework for the creation of new materials and focus on the development of physical foundations of new materials. The main purpose of discipline, "Spectroscopic methods for analysis of materials is the preparation of literate and educated professionals who know the methods of studying the elemental, chemical and molecular composition, structural perfection of the surface of interphase boundaries and nanostructures, methods, materials metrology. This discipline has a practice-oriented focus. The purpose of discipline Teach the basics of modern spectroscopic methods of analysis of materials, such as Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XRF), secondary ion mass spectrometry (SIMS), scanning ion microscopy (SIM). Allows us to investigate the elemental, chemical composition, atomic structure, structural perfection of the surfaces of solids, surface layers, phase boundaries and nanostructures. Ensure understanding of the possibilities of spectroscopic methods, their precision, sensitivity, and applicability of the locality for the study of nanomaterials. Learned to plan, organize and carry out spectroscopic and microscopic studies, process and analyze the information.

Course Format

Hours of lecture Hours of discussion Hours of class preparation Hours total
34 15 47 96

Please note that students are expected to study outside of class for three hours for every hour in class.

Course Content

The plan is to work through the following topics:

  1. Classification of methods for studying the surface and subsurface layers of solids
    • Relevance of spectroscopic studies of solids at this time. Methods Related to the spectroscopic class. Conditional division of methods into groups according to their abilities. Parameters of the Classification and comparative characteristics of the experimental methods of investigation and analysis of structural materials. Examples of classification methods
    • Destructive and non-destructive methods of analysis. Used types of sounding effects and their influence on surface and subsurface layers of solids. Rationale for the use of high and ultrahigh vacuum
    • Rationale of experimental methods of spectroscopic analysis of solids. Analysis of the impact of macro-and micro- and nano- in mechanical, physical, surface and other properties of structural nanomaterials as objects of spectroscopic studies. Notation. LS- and jj-bond
  2. Methods of electron spectroscopy. Auger electron spectroscopy (AES)
    • Methods of electron spectroscopy. Physical basis of the method of the AES. The mechanism of the Auger process. Coster - Kroning transitions. The energies of Auger transitions. The dependence of the energies of the dominant Auger transitions from the atomic number. Chemical shifts
    • Probability KLL - transitions in hydrogen-like atom. The width of atomic levels. The fine structure of Auger lines. The peaks of plasmon losses, ionization losses. Escape depth of Auger electrons
    • A quantitative analysis, the method of measurement standards, the method of elemental sensitivity factors. Getting concentration profiles using the AES. Application of AES (practical examples)
    • Apparatus for AES. Types of energy analyzers (analyzer with a retarding field analyzer of cylindrical mirror type, concentric semispherical analyzer). Sources of electrons (thermal emission and field emission). Requirements for the energy resolution, absolute and relative resolution, the resolving power. Vacuum pumps and systems spectrometers
    • Supplement information obtained by the spectroscopic method AES. Planning and organization of complex material science studies of the structure and properties of materials, depending on the perfection of their surfaces. Preparation of atomically clean surfaces
  3. X-ray photoelectron spectroscopy (XPS)
    • Physical basis of XPS method and the experimental technique. X-ray radiation, monochromatization. Energy analyzer (magnetic and electrostatic, dispersion and nondispersion). Electron multiplier. The resolving power of the method. The calibration spectra (internal standard, external standard from the surface of the additive)
    • Basic laws of XPS spectra: influence of oxidation, the dependence of the nearest environment and additive binding energy. The theory of chemical shift in the XPS spectra. Multiples splitting and X-ray satellites
    • X-Ray semi-quantitative analysis. Determination of the thickness of the thin film on the surface of the material on the corner of photoelectrons escape. Getting concentration profiles using the XPS. Practical application of the method XPS
    • Comparative characteristics of methods AES and XPS. Ultraviolet photoelectron spectroscopy. The energy spectrum and angular distribution of electrons. Investigation of the structure of the valence band, surface states of solids. Obtaining information on the chemical adsorption
  4. Methods of ion spectroscopy. Secondary ion mass spectrometry (SIMS)
    • Secondary ion emission. Construction of SIMS (ion source, quadrupole and magnetic mass-analyzer). Type the primary beam. Rate of sputtering. The interference of the masses. Qualitative analysis, deciphering the mass spectra
    • Concentration depth profiles of elements. The instrument factors influencing the depth resolution in the measurement of concentration profiles. Ion-matrix effects nfluence on the resolution of depth profiles. Quantitative processing SIMS. The coefficient of relative sensitivity. Bulk doping. Practical application of the method of SIMS
    • Physical basis of the method. Construction of SIM. Type the primary beam. Rate of sputtering. Obtaining an SIM image. The principles of the image contrast.


Primary textbooks:

  1. D. Briggs and M. P. Seah. Practical Surface Analysis, Auger and X-ray Photoelectron Spectroscopy. Wiley, Chichester; New York : Aarau, volume 1 edition edition, November 1990.
  2. D. P. Woodruff and T. A. Delchar. Modern Techniques of Surface Science. Cambridge University Press, Cambridge; New York, 2 edition edition, April 1994.

Additional textbooks:

  1. John F. Watts and John Wolstenholme. An Introduction to Surface Analysis by XPS and AES. Wiley, Chichester, West Sussex, England; New York, 2nd edition edition, May 2003.
  2. A. W. Czanderna. Methods of Surface Analysis. North Holland, January 1984.
  3. J. M. Walls. Methods of Surface Analysis: Techniques and Applications. Cambridge University Press, Cambridge Cambridgeshire; New York, 1st edition edition, January 1989.

Homework Assignments

Weekly, 15 problem sets in total, due at the beginning of the lecture. You may also submit via e-mail before the due date/time. It is of outmost importance that you invest your own effort into solving problems. Should you consult any sources, please provide references. Homework assignments should be typed. Legible handwritten assignments are acceptable.


Midterm exam 30%
Final exam 70%