The synthesis of monometallic hydrotalcite-like compounds (MHLC) type Co(II
)-Co(III) materials was achieved by precipitation of a solution of cobalt n
itrate(II) followed by microwave irradiation during the hydrothermal treatm
ent step. The effects of irradiation time, precipitant agent and atmosphere
were studied in order to establish the preparation conditions and the stab
ility of these materials. As expected, these materials required careful pre
paration conditions, mainly a very slow addition of the precursors. NH,OH h
ad to be used as precipitant agent in an air atmosphere. Short microwave ir
radiation times during the hydrothermal treatment provided a better crystal
lization of MHLC. The low stability of these compounds (similar to 200 degr
eesC) was explained by the presence of several Go-complexes between the lay
ers of the laminar structure. X-ray diffraction (XRD), Fourier transform in
frared spectroscopy (FTIR), differential thermal analysis and thermogravime
tric analysis (DTA/TGA), and thermoprogrammed oxidation (TPO) were used as
characterization techniques. (C) 2001 Published by Elsevier Science Ltd.