A high temperature superconductor of type TI2Ba2Ca2Cu3O10+5 has been prepared using the Freeze-Drying Method (TDM), and studied the physical properties through; the lodometric Titration, X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), and the resistivity measurement. The synthesis process of freeze-drying method starts from mixing the salts; T1NO3, Ba(NO3)2, Ca(NO3)24H2O, Cu(NO3)-3H20, according to their atomic percentages and dissolved in distilled water. The solution, then, sprayed in liquid nitrogen as droplets by using a glass spray system, then the droplets were dried by using freeze dryer plant to produce the powders. The freeze dryer that used in this work was designed locally in the Solid State Physics laboratory under vacuum (10"1 - 10"2 mbar) and low temperature (230 K) to produce a fine powder. The powder undergoes thermal treatment in two stages, first, a decomposition process to evolve the nitrates from the powder and, second, the sintering process in order to forming the superconducting phase. High homogeneity and very fine powder was produced with high transition temperature (Tc= 123 K).