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Laboratory practical training on the structural analysis for 3rd year students of the Solid State Physics Chair of MIPT

L.V. Zorina


Program of the practical training:
  1. X-ray diffraction methods in materials research
    1. Debye method: determination of lattice parameters, identification of crystal phases
    2. Laue method: orientation of a single crystal sample
    3. Oscillation method: determination of type of the Brave lattice and the unit cell parameters of a single crystal
  2. X-ray powder diffraction
    1. X-ray phase analysis: computer processing of X-ray diffraction spectra, identification of crystal phases using ICDD database
    2. The quantitative phase analysis with computer programs for full-profile fitting of powder diffraction patterns
    3. Precise determination of lattice parameters
    4. Determination of the size of particles and microstresses in a material
  3. Single crystal structural analysis
    1. Determination of translation periods and space group symmetry
    2. Analysis of Patterson function for solution of simple structures
    3. Application of direct methods for the structure solution
  4. Electron diffraction
    1. Electron diffraction in crystalline and amorphous materials
    2. Diffraction contrast in imperfect crystals
  5. Scanning electron microscopy
    1. X-ray microprobe analysis
    2. Study of surface relief

Practical works:

Work 1.X-ray phase analysis using registration of powder diffraction pattern on X-ray film (Debye Method). (Preparation of a powder sample of a simple cubic crystal; charging of X-ray camera; carrying out X-ray diffraction study by Debye method; X-ray film development; processing of Debye pattern; determination of lattice parameters; calculation of lines intensities.)

Work 2.X-ray powder diffraction: qualitative phase analysis. (Optical scheme of powder diffractometer with Bragg-Brentano geometry; preparation of a powder sample; carrying out X-ray study on powder diffractometer; processing of the received powder diffraction pattern using the standard software package; identification of crystal phase.)

Work 3.X-ray powder diffraction: quantitative phase analysis. (Preparation of a powder sample containing mixture of two phases; carrying out X-ray powder diffraction study; processing of the diffraction pattern using the standard software package; identification of crystal phases; definition of corund numbers for two phases mixed in the sample; calculation of weight constitution of the mixture of two phases; full-profile fitting of X-ray pattern by structures of known phases for definition of quantitative phase ratio.)

Work 4.X-ray powder diffraction: determination of the grains size, measurement of crystal lattice parameters. (X-ray diffraction experiment on a nanocrystal material; analyzing character of diffraction lines spreading; estimation of the size of nanocrystal grains; measurement of Debye spectra from a crystal of cubic symmetry; refining positions of diffraction maxima; application of extrapolation method for precise determination of lattice parameters.)

Work 5.Single crystal X-ray diffraction. Laue and oscillation methods: definition of orientation of single-crystal sample and determination of translation periods in crystal structure. (Preparation of single crystal sample for X-ray study; obtaining Laue diffraction patterns for two various orientations; creation of stereographic projections and definition of rotation matrix in laboratory coordinate system; measurement of oscillation X-ray pattern on oriented crystal; an indexation of diffraction reflections; definition of the translation period along a rotation axis.)

Work 6.Single crystal structural analysis: determination of lattice parameters, space group symmetry and crystal structure of a simple compound. (Preparation of a crystal with simple structure of cubic symmetry for X-ray study; collecting X-ray single crystal diffraction data on diffractometer with the CCD detector; determination of lattice parameters using a set of reciprocal lattice vectors; statistical analysis of reflections intensities; detecting the systematic absences and definition of space group symmetry; determination of crystal density and chemical elemental composition; crystal structure determination).

Work 7.Single crystal structural analysis: application of Patterson function and direct methods for a crystal structure solution. (Preparation of an organic single crystal with simple structure for X-ray study; collecting X-ray single crystal diffraction data; determination of lattice parameters and space group symmetry; application of direct methods for solution of crystal structure; X-ray diffraction experiment on a simple cubic crystal; analysis of Patterson function and structure solution.)

Work 8.Electron diffraction: measurement and indexation of electron diffraction patterns, determination of crystal lattice parameters. Dark-field image: size determination of diffracting objects.

Work 9.Scanning electron microscopy: X-ray microprobe analysis and study of surface structure.

Agarkov D.A. Tel: +7(916)7584930 email: agarkov@issp.ac.ru