Highly ordered supermicroporous silica (space group 2D-
p6
mm) was prepared using gemini surfactant [C
8H
17-N
+(CH
3)
2-(CH
2)
2-N
+(CH
3)
2-C
8H
17]·2Br
- (denoted C
8-2-8) with a short spacer group (
s = 2) as the structure-directing agent and sodium silicate as the precursor. The samples were characterized by small-angle X-raydiffraction, transmission electron microscopy, and N
2 adsorption-desorption. The results showed that thepore structure of the resulting silica belongs to the two-dimensional hexagonal structure (space group 2D-
p6
mm) with a pore size of ca. 1.40 nm (in the supermicroporous range). The high-quality supermicroporoussilica was formed at a low molar ratio of C
8-2-8 to sodium silicate (0.08:1), indicating that the ability ofself-assembly of C
8-2-8 is stronger than that of corresponding monovalent surfactants (single chain, singlehead group). For supermicroporous materials, the methods for calculating surface area and pore size arecritically compared. The surface area was found to be about 1000 m
2/g by the
s plot method. The pore sizeobtained with the HK model was in the range of 1.36-1.62 nm.