A novel compound YBaCo2Fe2O7 was synthesized successfully under low surrounding oxygen partial pressure by selecting raw materials Fe2O3 and Fe to fix the oxygen content to “O7” in YBaCo2Fe2O7. Its oxygen intake/release characteristics were investigated by the thermogravimetric (TG) analysis from room temperature to 1150°C. The YBaCo2Fe2O7 sample exhibits a weak oxygen intake capability at lower temperature 360°C. On the other hand, the oxygen intake/release cycles of YBaCo2Fe2O7 were investigated between 340°C and 410°C. The experimental results show that it has good and stable oxygen intake/release reproducibility, and that its mass change of oxygen reaches 0.6% of its original mass within 40 minutes. However, after partial substitution, the oxygen storage capability of YBaCo2Fe2O7 is worse than YBaCo4O7. The previous results mean that YBaCo2Fe2O7 is not enough as a novel candidate for oxygen storage or separation materials.