Aa. Rywak et al., SOL-GEL PREPARATION AND CHARACTERIZATION OF MAGNESIUM PEROXIDE, MAGNESIUM-HYDROXIDE METHOXIDE, AND RANDOMLY AND (111) ORIENTED MGO THIN-FILMS, Chemistry of materials, 7(11), 1995, pp. 2028-2038
A H2O2-assisted sol-gel method for the preparation of precursors for f
ormation of thin films of MgO is described. Sols were prepared from th
e addition of Mg(OCH3)(2) to methanolic H2O2. Two such sols, with Mg t
o H2O2 ratios of 1:1 and 1:10, were used to prepare, respectively, ran
dom or (111) oriented MgO thin films on Si(100). The xerogel from a so
l with a 1:10 Mg:H2O2 ratio contained nanocrystalline MgO2 . nH(2)O, w
hereas the xerogel from a comparable sol with a 1:1 Mg:H2O2 ratio cont
ained nanocrystals of MgO2 . nH(2)O, and Mg(OH)(OCH3). The latter comp
ound was the hydrolysis product of methanolic Mg(OCH3)(2) even when tr
eated with up to 4 equiv of water. The thermal decomposition propertie
s of this compound are reported. Using the published method of treatin
g Mg(NO3)(2) with excess 30% H2O2, MgO2 . nH(2)O, with a Mg2+:O-2(2-)
ratio of 1:0.74, was prepared. Based on IR, TGA, and DTA results, it i
s proposed that the material also contained oxide, and possibly hydrox
ide ions for charge balance. These ions were present either in an amor
phous phase, or possibly substituted for O-2(2-) in the MgO2 crystal s
tructure.