The broad theme of the present research investigation is on the preparation and characterization of the ultra thin films. The emerging field of nano science and technology demands the realization of different materials in nanometer dimension and a comprehensive understanding of their novel properties. Especially, the properties of the semiconducting materials in the nano dimensions are quite different from their bulk phase. A phase transition from semimetalic to semiconducting nature occurs at a thickness < 5nm of Sb ultra thin films. These facts emphasize the need for preparing these materials as nano layers and studying their properties as a function their size. Among the various characterization methods available to study the structure and the interfaces, Raman spectroscopy has proved to be a useful technique. In addition to revealing the structural information, Raman spectroscopy can bring out the quantum size effects in the lattice vibrational spectra of lower dimensional solids, stress state of the film in the initial growth stages, chemical nature of materials etc. Raman spectroscopy studies on the quantum structure of Ge and Sb are limited. This is attributed to the two serious limitations of the conventional backscattering of Raman signal. 1. The back scattered Raman signal intensity from the ultra thin layer could be below the detection limit. 2. The lower penetration depth of the lasers could inhibit the information from the buried layers. These limitations could be overcome to a major extent by employing an optical interference technique called IERS. This is basically an anti-reflection structure consisting minimum of three layers. These three layers are essential for achieving the interference conditions. The thicknesses of each layer were calculated using a matrix method. IERS structure consists of 1. A reflecting layer at the bottom of the stack (Platinum or Aluminum) 2. The second layer which is grown above the reflecting layer is a transparent dielectric layer, which introduces the necessary phase shift and hence it is called phase layer.(SiO2 or CeO2) 3. The top ultra thin layer which is to be investigated (Ge or Sb), is grown over the dielectric film and it is the layer which absorbs the most of the incident exciting light and it is called the absorbing layer. In this trilayer structure the thickness of the phase layer and the absorbing layer are adjusted in such a way that the light reflected from the air-ultra thin layer interface and the dielectric-reflector interface are equal in amplitude but opposite in phase. This leads to the destructive interference and a perfect anti-reflection condition is achieved. This enhances the near surface local field and results in the enhanced Raman signal. Regarding the reflection layer, thermally evaporated Al films were used. But the surface studies revealed a large surface roughness of 2.7nm for area of 2 µm×2µm. Also Al is known to react with oxygen and formation of an oxide layer is favored. In an effort to overcome these problems, a platinum layer was chosen instead of Al as a reflecting layer. Dual ion beam sputter deposition was employed to prepare the platinum films and to study the surface property of the films prepared at different secondary ion current density. Thus the process parameters to get the Pt film with the required surface properties were optimized. To prepare the required phase layer, optical thin films of Ceria were used. The optical and structural property of ceria is found to be sensitive to the process parameters. Hence a new deposition technique for preparing the CeO2 thin films was adopted. This technique is called Dual ion beam Sputter Deposition (DIBSD). This technique involves, two ion sources (Kaufman type). One source is used to sputter the target, which is called the primary ion source and the other one is used to assist the growing film, which is called the secondary ion source. Both argon and oxygen were fed into the secondary ion source and oxygen ions in the mixture of the gases (Ar +O2) react with the growing film and the oxygen stoichiometry in the film is maintained. Also the secondary ion bombardment of the growing film helps in the densification and it leads to the increase in the refractive index of the ceria films. The films were found to grow with a preferential orientation along (111) direction. The optical properties of the films were studied by using the transmission spectra of the films from the spectrophotometer. Powder X-Ray diffraction, and Raman spectroscopy, were employed to study the structural properties. Atomic Force Microscopy was used to examine the surface topography and to estimate the surface statistics. A stress free ceria film with a high refractive index of 2.36 at 600nm was prepared for a secondary ion beam current density of 150µA/cm2 and a beam energy of 150 eV. Raman spectra and X-ray diffraction data of these films have revealed the formation of point defects in these films as a function of secondary ion current density. Germanium (Ge) ultra thin layers were prepared by using Ion Beam Sputter Deposition (IBSD) as this technique has a good control over the rate of deposition apart from various other advantages. The Ge ultra thin films were prepared on the multilayer stacks with Al or Pt as a reflecting layer. The germanium films were prepared for the various thicknesses ranging from 1-10 nm. These films were prepared on the multilayer stack of reflecting layer and phase layer. The films were prepared for the different substrate temperatures from 40 °C to 300 °C. The films thus prepared have been analyzed by Interference Enhanced Raman Spectroscopy (IERS) for the structural and quantum size effects, by RBS for the thickness and to study interface diffusion, and Atomic Force Microscopy (AFM) for the analysis of nano structure of the grown films and also for the surface statistics. The thickness of the Ge films was found to be same as that had been calculated from the rate of deposition of the films. The films showed increase in the grain sizes with increase in the thickness of the films. The nanostructure of the films from AFM images confirms this observation. IERS of the films shows the transition from the compressive to stress free nature of the film for the nominal thickness of 1 & 2 nm. The quantum size effects of the films show the asymmetric broadening and peak shift and these observations were studied using the spatial correlation model. The TEM studies on the samples with Pt as a reflecting layer show influence of the underlying layer of CeO2 by the formation Moiré fringes. Antimony (Sb) films were prepared for the different thicknesses (3-10nm) and at different substrate temperatures (40 °C - 200 °C) on the Pt/CeO2 multilayer stacks as the absorbing layer. IERS studies on the films were performed and the results are as follows. Sb films show crystallization with increase in thickness from 3nm to 4nm. The films show amorphous to crystalline transition for the substrate temperature of 200 °C. Quantum size effects on the samples due to the phonon confinement were analyzed by the spatial correlation model. The atomic force microscopic measurements for the nanostructural information on the samples showed that the grain sizes of the films increase with increase in the thickness. Also the surface morphology shows a definite change in the features for the transition of amorphous to crystallization phase. Chapter 1 introduces the importance of Ge and Sb in the present day technologies. The current state of research on these two materials has been discussed. The importance of ceria and Pt films has been highlighted in the context of IERS and for the applications elsewhere. The advantages and disadvantages of ion beam sputter deposition have been described. The importance of Raman spectroscopy as a characterization tool for the nano structures has been shown in this chapter along with an introduction on Raman spectroscopy. Also, the importance of the other complimentary characterization techniques has been discussed. Chapter 2 presents the experimental details used to deposit and characterize the thin films. Details of IBSD and DIBSD processes are given. The characterization pertaining to structural, surface, optical and compositional properties are dealt in detail. Method to compute the optical constants of a transparent film is also given. Chapter 3 presents the properties of reflecting layers. Structural, surface and the compositional (presence of Ar ion) properties of the DIBSD platinum thin films are presented. Chapter 4 presents the optical, structural and surface properties of DIBSD ceria thin films as a function of process parameters. Chapter 5 deals with the growth and Raman analysis of ultra thin Ge films with Al and Pt as reflecting layers. Chapter 6 deals with the growth and Raman analysis of ultra thin Sb films. Chapter 7 gives the summary of the thesis and the future scope of the work.