For a sample of an inorganic powder, select a materials characterisation techniq

Question

For a sample of an inorganic powder, select a materials characterisation technique or combination of techniques which could give you information on each the following:

(a) Particle size, particle shape and agglomeration state;

(b) Whether the particles are amorphous or crystalline and, if crystalline, the exact crystal structure;

(c) Whether the particles contain crystalline defects;

(d) The chemical composition of the bulk and surface of the particles;

(e) The chemical bonding in the particles.

In each case, as well as listing an appropriate technique or techniques, describe them in terms of their sample preparation requirements, data output/data analysis and limitations due to analytical resolution.

Explanation / Answer

a) Particle size and size distribution:

      i) Photon correlation spectroscopy

      ii) Laser diffractometry

      iii) Transmission Electron Microscopy (TEM)

      iv) Scanning Electron Microscopy (SEM)

       V) Atomic force microscopy

b) X-Ray Diffraction Technique (Powder XRD and single crystal XRD).

C) X-Ray Diffraction Techniques--Convergent-beam electron diffraction (CBED) for the analysis of stacking faults and antiphase boundaries, Large-angle convergent-beam electron diffraction (LACBED) is performed to detect crystal defects like point defects, perfect and partial dislocations, stacking faults, antiphase boundaries and grain boundaries.

d) chemical composition of the bulk and surface of the particles :

    i)Auger electron spectroscopy and energy dispersive X-ray analysis (EDXA) or energy dispersive X-ray microanalysis (EDXMA).

    ii) Electron spectroscopy for chemical analysis (ESCA)

   iii) X-ray fluorescence (XRF)

e) chemical bonding in the particles :

   X-ray photo electron spectroscopy(XPS)/ Infrared spectroscopy(IR)

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