Synthesis of NaTi 2 ( PO 4 ) 3 by the Inorganic–Organic Steric Entrapment Method and Its Thermal Expansion Behavior

Crystalline pure NaTi 2 ( PO 4 ) 3 ( NTP ) powder was synthesized at 700°C using a simple and low energy, hybrid inorganic–organic, steric entrapment method. Sodium nitrite (Na NO 2 ) and ammonium phosphate dibasic (( NH 4 ) 2 HPO 4 ) dissolved in water, whereas titanium ( IV ) isopropoxide (Ti[ OCH ( CH 3 ) 2 ] 4 ) hydrolyzed in water. Ethylene glycol ( HOCH 2 CH 2 OH ) was used as a polymeric entrapper and hydrolysis of the Ti source was hindered by its dissolution in isopropyl alcohol. The resulting NTP powder was characterized by thermogravimetric analysis/differential thermal analysis, X‐ray diffractometry, scanning electron microscopy, specific surface area by Brunauer–Emmett–Teller nitrogen absorption, and particle size analysis. Furthermore, C, H, N were measured by the classical Pregl‐Dumas method. The thermal expansion behavior in all { hkl } pole directions was also determined by in situ high‐temperature X‐ray diffraction using synchrotron radiation and was found to be in agreement with other published studies.