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Phase equilibrium diagrams have been constructed from experimental data for the systems Sb 2 O 4 -NaSbO 3 , Sb 2 O 4 -KSbO 3 , and Sb 2 O 4 -NaSbO 3 -NaF. The system Sb 2 O 4 -NaSbO 3 contains only an intermediate pyrochlore type solid solution with a maximum melting point of 1490 °C at a Na:Sb atom ratio of 3:5. The Sb 2 O 4 -KSbO 3 system contains in addition to the pyrochlore phase a compound 3K 2 O • 5Sb 2 O 5 which melts congruently at about 1450 °C and two polymorphs of K 2 O • 2Sb 2 O 5 . The low temperature form of K 2 O • 2Sb 2 O 5 was found to be monoclinic P2 1 /c with a = 7.178, b = 13.378, c = 11.985 A, β = 124°10'. The melting point of Sb 2 O 4 was found to be 1350 ± 5 °C and NaSbO 3 and KSbO 3 both melt congruently at 1555 ± 5 °C and 1410 ± 5 °C respectively. The previously reported cubic form of KSbO 3 was found to be a K + deficient phase stabilized by reaction with atmospheric moisture. A similar cubic phase which appears to be a good Na + ion conductor can be synthesized in the ternary system NaSbO 3 -Sb 2 O 4 -NaF.

Phase equilibria and crystal growth in the alkali antimonate systems Sb2O4-NaSbO3, Sb2O4-KSbO3, and Sb2O4-NaSbO3-NaF