H. Roggendorf et al., STRUCTURAL CHARACTERIZATION OF CONCENTRATED ALKALINE SILICATE SOLUTIONS BY SI-29-NMR SPECTROSCOPY, FT-IR SPECTROSCOPY, LIGHT-SCATTERING, AND ELECTRON-MICROSCOPY - MOLECULES, COLLOIDS, AND DISSOLUTION ARTIFACTS, Glass science and technology, 69(7), 1996, pp. 216-231
Sodium and potassium silicate solutions (water glass; molar ratios SiO
2:Na2O = 2.0 and 3.3, SiO2 content = 25 wt%; molar ratios SiO2:K2O = 3
.3 and 4.0, SiO2 content = 25 and 20 wt%, respectively) were prepared
and characterized, e.g. by Si-29-NMR spectroscopy, FT-IR spectroscopy,
Raman spectroscopy, or dynamic light scattering. One type of sodium s
ilicate solution (molar ratio SiO2:Na2O = 2.0) was prepared by three d
ifferent methods from different precursors (two glasses with different
chemical compositions and quartz). The structure of these concentrate
d alkaline silicate solutions is determined by the ''molecular'' and t
he ''colloidal'' fraction of silica. For the investigation of the mole
cular silicate components the Si-29-NMR spectroscopy and the FT-IR spe
ctroscopy yielded the most valuable results. Dynamic light scattering
allowed to detect minute amounts of artefacts (possibly remnants of th
e dissolving species) of the production process with diameters > 100 n
m. By filtering off these artefacts it was possible to characterize th
e colloidal fraction of the sodium silicate solutions. Monomodal parti
cle size distributions with maxima at 30 to 35 nm were found. The solu
tions with the higher sodium contents have the smaller particles. Elec
tron microscopy supported the light scattering results concerning the
particle sizes and gave an impression that the major part of silica is
present in colloidal form. The preparation method had almost no influ
ence on the molecular structure of the alkaline silicate solutions. Th
is and the monomodal size distributions of the colloids can be interpr
eted by the assumption of a (metastable) equilibrium state.