A novel sol-gel process is used to synthesize mesoporous silica-alumina catalysts with controlled pore size distribution without using templates or pore-regulating agents. The nitrogen sorption analysis shows that the synthesized materials have high specific surface area in the range 587-692 m(2)/g and similar mesoporous distribution within 2-11 nm. Ultrasound is applied to prepare precursor silica-alumina Sol with narrow particle diameter distribution. By calculation, it is found that ultrasonic treatment is able to provide 22.94 kJ/mol energy, which is just in accordance with the weak bond's bonding energy. Based on the calculation result, it is proposed that the role of ultrasonic treatment followed by acid peptization is to provide energy to break down the weak bonds. After gelation, the regular and close packing of similar-sized sot particles is capable of formation of controlled-sized interstices which are the precursors of mesopores. Solid-state Al-27 MAS NMR and TEM are used to characterize the samples' structure and particle morphology. They show that most of the aluminum is located in the tetrahedral position in the present materials. According to TEM results, it is shown that the synthesized materials have spherical particles with size of about 15 nm.