Nanostructured fluoride powders were prepared by high-energy ball milling u
nder different milling conditions (time and intensity). To investigate the
local structural orders, we combined suitable local probe techniques such a
s Fe-57 Mossbauer spectrometry (MS) and F-19, Ga-69 and Ga-71 nuclear magne
tic resonance (NMR) applied to FeF3 and GaF3 milled samples, respectively.
Both isomer shifts and chemical shifts are consistent with the presence of
only corner-sharing octahedral units in these systems. After analysis of th
e different hyperfine magnetic and quadrupolar parameters, the correspondin
g Mossbauer and nuclear magnetic resonance data were compared to those of c
rystalline and amorphous phases and then mutually compared. Two types of lo
cal structural orders are unambiguously detected and attributed to the pres
ence of crystalline grains and grain boundaries (GB). (C) 2001 Elsevier Sci
ence B.V. All rights reserved.