Aiming to strengthen the performance of waste activated sludge digestion, pretreatment is a prerequisite for keeping operations within an industrially acceptable time-frame. In this study, the performance of microaeration coupled with thermophilic (MT) pretreatment on waste activated sludge solubilization and acidification was investigated. The results showed that the maximum soluble organics concentrations, including soluble proteins and carbohydrates, reached 2290 mg COD/L in 24 h when the ventilation rate and temperature were 0.05 vvm and 70 degrees C. SDS-polyacrylamide gel electrophoresis (SDS-PAGE) test on pure-culture (E.coli) and scanning electron microscopy analysis indicated that MT pretreatment effectively destroyed microbial cell wall and resulted in an increase in soluble proteins. Polymerase chain reaction-denaturing gradient gel electrophoresis (PCR-DGGE) analysis revealed that MT pretreatment reduced the diversity of the bacterial community during pretreatment. Along with the dissolution of a large quantity of organic matter, microbial species such as Lactococcus and Methyloversatilis bloomed at the end of acidification period, which contributed to SCFAs production. This study revealed that MT pretreatment facilitated the WAS hydrolysis efficiency and enhanced SCFAs (3149 mg COD/L with fermentation for 96 h) production, especially for acetic acid (50%) accumulation, which provides a new perspective for the application and recovery of sludge resources.