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Hybrid composites forms an important field of research in the area of composite science and engineering as it gives the advantage of avoiding complex lay-up designs and provides better tuning compatibility to get desired properties in comparison with their mono-fiber counterpart. Further, utilization of composites for low temperature structures has been hindered by inconsistency of material property data and not much is reported on thermal characteristics of hybrid composites at cryogenic temperatures. This research work is focused on development of carbon-glass epoxy hybrid composite and to study the thermal behavior of these materials in comparison to its mono-fiber counterparts especially at cryogenic temperatures. The objectives are classified into the following three parts: Development of a hybrid composite with urethane modified epoxy matrix system (toughening agent used is Propyltrimethoxysilane (PTMO) and Toluene Di-Isocyanate (TDI) is added to get the polyurethane structure), for cryogenic applications. Study and understand the limitations and complexities of the experimental methodologies involved in evaluating the thermal properties of these materials namely thermal conductivity, coefficient of thermal expansion and specific heat. Finally to look into the appropriate theoretical calculations and experimental results to understand the variations, if any, for these materials. Specifically the following contributions are reported in this thesis: Evaluated the modified matrix system for its physical and mechanical properties at 20K. Specimens were prepared with D638 ASTM standard, modified to suit pin loading configuration in the cryostat/Instron machine. After assessing the suitability of the matrix system, mono fibre composites of different types were made and evaluated their thermal properties viz, coefficient of thermal expansion, thermal conductivity and specific heat down to 20K. Based on the results of the above, a hybrid composite configuration was evolved which exhibits optimal thermal characteristics at low temperatures and its characterization for various thermal properties at cryogenic temperatures was carried out. Comparisons of the experimental results were made with macro-mechanical model and micro-mechanical model (rule of mixtures) of composite materials. The present work throws light to the fact that hybrid polymer matrix composites can very well be considered for cryogenic applications where the combination or trade off between properties like strength to conductivity ratio, modulus to conductivity ratio and low cost is to be made. The mechanical properties of hybrid composites also need to be studied to complement the study on thermal properties reported in this thesis. It is essential to have a complete understanding of behaviour of these materials at cryogenic temperatures with respect to both thermal and mechanical properties as it is evident from the available literature that the emerging demands are multi-disciplinary in nature. The present research work is aimed at highlighting the use of hybrid composites to achieve the desirable thermal properties and thereby inviting the attention of scientists and engineers who are engaged in the design of cost effective structures and appliances for cryogenic environments to focus on further research to develop