SMALL-ANGLE X-RAY-SCATTERING EXPERIMENTS IN GRAZING-INCIDENCE ON SOL-GEL COATINGS CONTAINING NANO-SCALED COLLOIDS - A NEW TECHNIQUE FOR INVESTIGATING THIN COATINGS AND FILMS
B. Kutsch et al., SMALL-ANGLE X-RAY-SCATTERING EXPERIMENTS IN GRAZING-INCIDENCE ON SOL-GEL COATINGS CONTAINING NANO-SCALED COLLOIDS - A NEW TECHNIQUE FOR INVESTIGATING THIN COATINGS AND FILMS, Journal of applied crystallography, 30, 1997, pp. 948-956
Small-angle X-ray scattering (SAXS) is generally not applicable to thi
n (similar to 1 mu m) films and coatings because of their weak scatter
ing signal in conventional transmission experiments. This restriction
can be overcome by working in grazing incidence, with an angle of inci
dence ct slightly above the critical angle of total reflection phi(c),
in order to augment the effective X-ray path in the sample. The possi
bilities of this technique are demonstrated by preliminary results obt
ained on glass-like sol-gel coatings containing nano-scaled gold collo
ids. The scattering of the gold colloids was identified by variations
of the X-ray energy near the absorption edge of gold (anomalous SAXS).
It showed the theoretically predicted variation of intensity with ene
rgy. The recorded scattering spectra were corrected for absorption and
refraction effects, whose influences on the spectra are discussed. Ca
lculated size distributions of the colloids from SAXS in grazing incid
ence were compared with results from high-resolution transmission elec
tron microscopy (HTEM) investigations and optical UV-visible spectrosc
opy.