Mesoporous silica crystals have a large variety of structures mainly due to the versatility of their structure template. The configuration and the chemical state of the templating micellar surfactants, together with the kinetic process of silica will determine the final outcome of the synthesis. Increasing the understanding of the complex formation processes involved will enable a possibilityto fine tune the material for specific uses, today focused into the fields of photoniccrystals, drug delivery, catalysis and separation technology.

In this thesis emphasis is put on (1) increasing the understanding the formation mechanism yielding the different species of mesoporous silica crystals through an in depth study of quasicrystallinity (2) Characterization and description of the structural complexity through various characterization techniquesand also by studying the kinetic structural transformation phenomenon related to the minimal G- and D-surfaces. (3) The structural studies of the versatile surfactant liquid crystals for establishing a thermodynamically stable basis to evaluate the kinetic mesoporous silica growth processes. Furthermorethe thesis both enlightens the possibilities of and contributes to the developmentof electron microscopy characterization techniques.

In these studies, electron microscopy is largely employed in the characterization to give a thorough picture of the mesoporous structures. This is combined with the sample preparation techniques cross-section polishing and ionslicing. Low voltage scanning electron microscopy is utilized for studying the surfaces and cross-sections of various materials at the limit of the resolution. Here, a deep understanding of the electron beam-material interaction is used for a better interpretation of the detected signals. Transmission electron microscopyis combined with electron crystallographic reconstruction to yield a three dimensional structural model. For determination of the quasicrystallinity level for a structure of dodecagonal tiling, revealed in the scope of this study,a phason strain analysis was made.