The most common method used for synthesizing inorganic solids is the so-cal
led 'ceramic method' which involves synthesizing at elevated temperatures a
nd leads to thermodynamically stable phases. This method has a serious limi
tation because many inorganic solids of current interest are rather metasta
ble and consequently their preparation requires low temperature methods. In
this article, we have reported some methods of synthesis which also includ
e methods that belong to soft-chemistry routes. The selected examples prese
nted in this paper are: (1) the intercalation and or deintercalation of oxy
gen in oxides by electrochemical oxidation or reduction in aqueous or nonaq
ueous solutions, (ii) the use of chemical agents such as NO2 or borohydride
s for obtaining oxides with tunneled and lamellar structures, (iii) a multi
stage synthesis processing for intercalating, in layered oxygenated materia
ls, anionic species and acrylic monomers and polymers, (iv) the supercritic
al fluid processing for preparing nitrides, carbon-nitrides, lamellar oxide
s and oxy-(hydroxy-) fluorides, and (v) the mechanical alloying for synthes
izing new Mg-based binary intermetallics.