Abstract This work provides data on strategies for single GdSrFeO 4 phase solid state synthesis. Earlier works have shown that under the solid-state synthesis conditions, the GdSrFeO 4 preparation is hampered by the formation of non-target product: Gd 2 SrFe 2 O 7 . This work approach led to the solid-phase synthesis GdSrFeO 4 scheme change. GdSrFeO 4 was characterized by X-Ray, scanning electron microscopy/energy dispersive X-ray spectroscopy, dilatometry and complex thermal analysis methods. GdSrFeO 4 is stable in the wide range of studied temperatures 40–1,400°C in air. The sintering start temperature was determined to be 985°C. GdSrFeO 4 has a thermal expansion coefficient of 30 × 10 −6 K −1 . The thermal stability is excellent for further investigation and potential for application of the materials as SOFC, for example. The study of catalytic stability of the obtained GdSrFeO 4 is to be a subject of future work as well.