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Damage and molecular changes under a laser beam in SEM‐EDX/MRS interface: a case study on iron‐rich particles
Author(s) -
Worobiec A.,
Darchuk L.,
Brooker A.,
Potgieter H.,
Van Grieken R.
Publication year - 2011
Publication title -
journal of raman spectroscopy
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.748
H-Index - 110
eISSN - 1097-4555
pISSN - 0377-0486
DOI - 10.1002/jrs.2789
Subject(s) - raman spectroscopy , scanning electron microscope , particle (ecology) , energy dispersive x ray spectroscopy , laser , materials science , evaporation , particle size , analytical chemistry (journal) , chemistry , optics , composite material , oceanography , physics , chromatography , thermodynamics , geology
The control of damage to individual environmental particles by a laser beam during Raman spectroscopy carried out in ambient air is generally well understood. The nature and control of damage under vacuum conditions (e.g. in the scanning electron microscopy with energy X‐ray detection combined with micro‐Raman spectroscopy—interfaced SEM‐EDX/MRS) are more complex and less well comprehended. The physical and chemical processes that affect the damage caused to small particles by lasers still remain somewhat unclear, but certainly the atmosphere (vacuum/air) and the beam intensity have very significant influences. Furthermore, it has been determined that some particles (e.g. haematite), although stable under an electron beam, are damaged by the laser beam, hampering their analysis. Additionally, when simultaneous analyses by SEM/EDX and MRS are considered, the correct choice of the collection surface plays a crucial role. As a result, the following collection substrates were tested to determine their influence on the laser beam damage process to the particle: silver and aluminium foils and silicon wafers. A test study was performed using artificial examples of haematite (Fe 2 O 3 ) particles. Exposure of Fe 2 O 3 particles in vacuum to 514‐ and 785‐nm laser radiation often leads to their melting, transformation and evaporation. The dependence of the damage caused by the laser beam on the particle structure is reported here. Molecular and crystallographic changes have also been revealed. Formation of magnetite (as an effect of re‐crystallisation) and Raman inactive structures was detected. Copyright © 2010 John Wiley & Sons, Ltd.