A facile method for the density determination of ceramic thin films using X-ray reflectivity

A fast and non-destructive method based on X-ray reflectivity was developed to determine the density of sol–gel derived ceramic thin films, without prior assumptions on the microstructure of the system. The thin film density is calculated from the critical angle θ c , i.e. the maximum angle at which...

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Bibliographic Details
Published in:Journal of sol-gel science and technology 2014-07, Vol.71 (1), p.118-128
Main Authors: Veldhuis, Sjoerd A., Brinks, Peter, Stawski, Tomasz M., Göbel, Ole F., ten Elshof, Johan E.
Format: Article
Language:English
Subjects:
Angle of reflection
Backscattering
Ceramics
Chemistry
Chemistry and Materials Science
Colloidal gels. Colloidal sols
Colloidal state and disperse state
Composites
Computer simulation
Critical angle
Density
Exact sciences and technology
Film thickness
General and physical chemistry
Glass
Inorganic Chemistry
Interface roughness
Materials Science
Mathematical analysis
Nanotechnology
Natural Materials
Nondestructive testing
Optical and Electronic Materials
Original Paper
Reflectance
Reflectivity
Rutherford backscattering spectroscopy
Scanning electron microscopy
Single crystals
Sol gel process
Sol-gel processes
Substrates
Thin films
X-rays
Yttria stabilized zirconia
Yttrium oxide
Zirconium dioxide
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Summary:A fast and non-destructive method based on X-ray reflectivity was developed to determine the density of sol–gel derived ceramic thin films, without prior assumptions on the microstructure of the system. The thin film density is calculated from the critical angle θ c , i.e. the maximum angle at which total external reflection is still observed, which becomes increasingly difficult for imperfect films. We propose a simple numerical approach, instead of laborious fitting procedures, to determine the thin film density. A pseudo -critical angle, θ pc , was defined by the first minimum in the 3rd derivative of the reflectivity curves. The measured samples were compared with calibration curves obtained from simulations with changing film densities. Although the absolute positions of θ c and θ pc are different, similar shifts are observed with changing density. The accuracy of the described method was validated by determining the density of single crystal substrates (ρ rel  = 100 %) and by Rutherford backscattering spectroscopy in combination with scanning electron microscopy. Varying sample size, film thickness, and film/interface roughness of yttria-stabilized zirconia films were found to have no influence on the final calculated density.
ISSN:0928-0707
1573-4846
DOI:10.1007/s10971-014-3336-2