Piezocatalysis, a new catalysis technology much relying on catalyst's piezoelectric property, attracts unprecedented research enthusiasm for applications in energy conversion and chemical synthesis, such as hydrogen peroxide production. However, the reported piezocatalytic activities are not ideal and one of the reasons is the unsatisfactory piezoelectricity, urging researchers to explore new and efficient piezocatalysts. Herein, the MAX phase materials (Ti₃AlC₂, Ti₃AlCN, and Ti₃SiC₂) are employed as piezocatalysts for hydrogen peroxide (H₂O₂) and reactive oxygen species generation. Results suggest that Ti₃SiC₂ possesses the highest piezocatalytic activity with a notable H₂O₂ yield of 871.0 μmol/g/h accompanied with small amount of reactive oxygen species, while the Ti₃AlC₂ and Ti₃AlCN deliver relatively lower H₂O₂ yields of 810.6 and 835.6 μmol/g/h in pure water, respectively. A series of characterizations and analysis have been employed to understand the insights of piezocatalytic activity difference and reaction mechanism. The enhanced peizocatalytic activity of Ti₃SiC₂ can be traced to its notable piezoelectric property and reduced electronic transfer resistance as well as the improved free charge density, all of which are favorable factors benefiting the piezocatalytic H₂O₂ generation. Moreover, H₂O₂ production via piezocatalysis stems from both oxygen reduction and water oxidation.