Laboratory practical training on the structural analysis for 3rd year students of the Solid State Physics Chair of MIPT
ProgramProgram of the practical training:
Work ¹1.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 ¹2.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 ¹3.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 ¹4.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 ¹5.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 ¹6.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 ¹7.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 ¹8.Electron diffraction: measurement and indexation of electron diffraction patterns, determination of crystal lattice parameters. Dark-field image: size determination of diffracting objects.
Work ¹9.Scanning electron microscopy: X-ray microprobe analysis and study of surface structure.
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