In this paper the effect of ammonium hydroxide addition to the solution of metallic oxide on sol gel preparation process of YBCO is studied with differential thermal analysis, thermal graviometry and X-ray diffraction. Two samples with and without ammonium hydroxide. Ammonium hydroxide prevents both barium nitrate precipitate during the gel preparation and also unwanted reaction as well as increasing homogeneous product. After drying the gel, the samples heated up to 1050°C in DTA apparatus in order to find more accurate the type and the temperature of reaction during the preparation process. After the initial reactions in the samples, Y2Cu2O5 and 123 phases are created in the range of 780-840°C and then the 123 phase is strengthened at 900-950°C. As shown in X-ray data, 123 was the only phase after this range. In addition ammonium hydroxide support and increase the creation of 123 phase at lower temperature.