Phase equilibria in the La1−xCaxFeO3−δ (LCF) system were assessed at temperatures below 1350°C in both simulated air and argon atmospheres using a combination of differential scanning calorimetry, thermogravimetric analysis, scanning electron microscopy, and high‐temperature X‐ray diffraction. The solubility limit of Ca in the perovskite structure was determined to be 38% A‐site substitution. A high‐temperature orthorhombic to rhombohedral transition was identified and the dependence on oxygen partial pressure and effect on thermal expansion were characterized. A partial, pseudobinary LaFeO3–CaFeO2.5 phase diagram is presented that is based on these analyses combined with data available in the open literature.

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