This paper deals with the preparation of a family of ionic conductor cerami
cs known as NaSICON (Na Super Ionic CONductor) and with their characterizat
ion. For this family constituted of silicon, sodium, phosphorus and zirconi
um, an original process is proposed to obtain pure ceramics. Precursors are
sodium nitrate, zirconyl nitrate, ammonium phosphate, tetraethoxysilan (TE
OS), nitric acid and ethanol. New compositions unknown in literature (Na3.2
Zr1.9Si1.5P1.5O12 et Na2.8Zr1.8Si1.1P1.9O12) were studied. The thermal deco
mposition of the precursors was performed with a slow heating rate. It was
studied by ATD-ATG and X-ray diffraction. The thermal decomposition leads t
o the oxide at 750 degrees C, which was characterized by X-ray diffraction.