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Novel hybrid xerogel materials were synthesized by a sol-gel procedure. <em>n</em><em>-</em>octadecyltriethoxysilane was co-condensed with and without different cross-linkers using <strong>Q<sup>0</sup></strong> and <strong>T<sup>0</sup></strong> mono-functionalized organosilanes in the presence of <em>n</em>-hexadecylamine with different hydroxyl silica functional groups at the surface. These polymer networks have shown new properties, for example, a high degree of cross-linking and hydrolysis. Two different synthesis steps were carried out: simple self-assembly followed by sol-gel transition and precipitation of homogenous sols. Due to the lack of solubility of these materials, the compositions of the new materials were determined by infrared spectroscopy, <sup>13</sup>C and <sup>29</sup>Si CP/MAS NMR spectroscopy and scanning electron microscopy.<strong></strong>