The effects of different mixtures of organic structure-directing agents (OSDAs) on the formation of SAPO-34 structure have been investigated. Different OSDAs, namely, triethylamine (TEA), tetraethylammonium hydroxide (TEAOH), and morpholine (Mor) and their combinations were used to synthesize SAPO-34 by a hydrothermal method. The template concentration was optimized by eliminating the competing phases to obtain the purest form of SAPO-34 phase. The as-synthesized samples were analyzed by XRD, FE-SEM/EDS, FT-IR, surface area/pore volume measurements, NH3-TPD, TG/DTA, and 29Si NMR MAS. The selection of template notably impacts the crystal size and physicochemical characteristics of as-synthesized SAPO-34. The sample prepared with 3 Mor : 3 TEA : 1 TEAOH exhibited the highest total acidity, smallest crystal size below 3 µm, and high surface area up to 697 m²/g.