The product of T20 consists of smooth and nonuniform spheres. No real fibers or linear shapes were seen in the images, suggesting that the cotton-like bundles observed in the growth medium were basically loose particle agglomerates. Surface corrugation and nonuniform shapes develop as a result of irregular condensation. With T80 surfactant, the output is mostly ill-shaped agglomerates of preformed spheres that cause combined intra- and interparticle textures. Part of the irregular shapes is contributed
by precipitation from the thick film grown at the interface. This film was shown in an earlier study to be amorphous with low surface area properties [37]. Figure 10 SEM (left) and TEM (right) images of samples prepared using nonionic surfactants. (a) MS5a using Tween 20 and (b) MS5b using Tween 80. According to N2 sorption isotherms (Figure 6a), the Tween-based products have mesoporous structures with a shallow Selleckchem RO4929097 capillary condensation
step indicating a nonuniformity in pore sizes. As seen in Table 2, the average pore size for the T20 product is 3.0 nm which is larger than both the TEOS-based gyroids (MS6b, 2.64 nm) and TBOS-based fibers see more (MSF, 2.35 nm) but has surface area and pore volume properties inferior to the MSF product. An additional capillary condensation step at p/p0 = 1 was seen for the T80 product as a result of the textural porosity generated from the interparticle spaces in the Selleck Belinostat random agglomerates observed in the SEM image (Figure 10b). This shifts the average pore size to a higher value (3.7 nm), combining the structural intraparticle mesopores and the pheromone larger size textural interparticle pores. Such interparticle spaces were not seen in the T20 product because the particles of T80 silica are smaller and aggregated and would therefore provide an additional textural porosity. The XRD patterns of Tween-based silica in Figure 7b show poorly ordered structures (MS5a and MS5b). The T20 silica shows an amorphous response without any peak reflection, while the T80 product exhibits a single broad diffraction
peak characteristic of a mesopore system lacking enough order. This structure was further confirmed by TEM images. Figure 10a clearly shows that T20 silica has irregular porous regions characteristic of an amorphous structure. Conversely, the T80, which showed a small reflection in the XRD pattern, displays some domains of ordered assemblies appearing as long wormhole-like channels along the c-axis (Figure 10b). These results suggest that acidic interfacial growth with neutral surfactants produces mesoporous structure with poor channel arrangement. This structure is similar to MSU-X materials prepared with Tween surfactant by the S0I0 route under neutral and mixing conditions [50]. It is interesting to note that silica prepared with TEOS-T80 system (sample MS5b) has properties very close to the TEOS-CTAB system (sample MS4); both have poor order and wormlike mesopores.