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Sonodynamic therapy (SDT) typically suffers from compromised anticancer efficacy owing to the low reactive oxygen species (ROS) yield and complicated tumor microenvironment (TME) which can consume ROS and support the occurrence and development of tumors. Herein, ultrathin‐FeOOH‐coated MnO2 nanospheres (denoted as MO@FHO) as sonosensitizers which can not only facilitate ultrasound (US)‐triggered ROS but also tune the TME by hypoxia alleviation, H2O2 consumption as well as glutathione (GSH) depletion are designed. The FeOOH coating will boost the production yield of singlet oxygen (1O2) and hydroxyl radicals (•OH) by inhibiting the recombination of US‐initiated electron–hole pairs and Fenton‐like reaction, respectively. Additionally, the catalase‐like and GSH peroxidase‐like activities of MO@FHO nanospheres enable them to break the TME equilibrium via hypoxia alleviation and GSH depletion. The combination of high ROS yield and fundamental destruction of TME equilibrium results in satisfactory antitumor outcomes, as demonstrated by the high tumor suppression efficacy of MO@FHO on MDA‐MB‐231‐tumor‐bearing mice. No obvious toxicity is detected to normal tissues at therapeutic doses in vivo. The capability to modulate the ROS production and TME simultaneously can afford new probability for the development of advanced sonosensitizers for synergistic comprehensive cancer therapy. [ABSTRACT FROM AUTHOR]

Metal oxides hold great promise as robust sonosensitizers for sonodynamic therapy (SDT). However, they usually suffer from limited production yield of reactive oxygen species (ROS) due to the fast recombination of ultrasound‐triggered electrons and holes. Herein, porous lanthanum (La)‐doped MnO2 (LMO) nanoparticles are firstly developed as promising sonosensitizers in SDT. The strategic introduction of La dopants greatly promotes the separation efficiency of ultrasound‐triggered electrons and holes of MnO2, endowing them with significantly improved ROS yield. Consequently, the LMO with polyethylene glycol decoration exhibits good SDT activity toward breast cancer cells. This work highlights the doping strategy for the development of enhanced ROS production of metal oxide sonosensitizers for SDT. [ABSTRACT FROM AUTHOR]