In this study, synthesis of NASICON powder by coprecipitation and sol-gel processes is described and effect of process conditions and calcination temperature on crystallinity is investigated. X-ray diffraction patterns show that the coprecipitation method leads to formation of NASICON pure phase with a negligible zirconia content and so the powder derived thorough coprecipitation is used for sintering. Sintering is carried out in two methods. In conventional method, NASICON pellets are sintered at different temperatures and holding time. Results reveal that the pellet sintered at 1000 °C for 10 h yields better electrochemical properties. Spark plasma sintering was also performed which results the highest conductivity of 1.7 × 10−3 S cm−1 between all samples at 25 °C.