Surfactants organize to form various mesophases of lyotropic liquid crystal (LLC) in the presence of water. In the literature, some acids, salts, and ionic liquids have also been used to form ordered LLC mesophases. In this thesis, two dimensional (2D) singleicrystalline gold (Au) nano- and microplates and reduced graphene oxide (RGO) thin films have been synthesized using LLC mesophases. Stable LLC mesophases have been formed using 10-lauryl ether (C12EO10), an oligo-type surfactant, and sulfuric acid (H2SO4), a strong acid. Au plates with various anisotropic structures, such as triangular, truncated triangular, hexagonal, and gear-like, have been synthesized by a photochemical method in the presence of LLC mesophase. Most importantly, Au plates up to 39 μm in width have been obtained in the confined space of the LLC medium. The thickness of the obtained Au plates varies from 50 nm to 150 nm. The size and/or morphology of Au products synthesized in LLC medium depends on the power of the light source, the irradiation time, the amount of Au precursor added, the addition of different capping agents, and various inorganic salts. Additionally, spin-coated RGO thin films have been synthesized using the LLC mesophase for use as a transparent and conductive electrode in various electrochemical devices. The LLC mesophase has improved the sheet resistance values of RGO thin films. RGO thin films with a sheet resistance of 31 kΩ/sq and an optical transmittance of 92% at 550 nm have been achieved at the high thermal annealing temperature under an inert atmosphere.