Composite structure with characteristics of high temperature resistance, light weight and high strength is the imperative requirement in aerospace field, which has been extensively applied in engineering. In order to compare effectiveness of two anti-loosing techniques, experimental investigations of bolted structures at room/high temperature are undertaken, random vibration test is adopted as the looseness detecting condition. Fundamental frequency of structure is introduced as indicator of loosening status by comparing its value before and after each step of loading. Application of high temperature adhesive and double nutting, along with different chamfer angles of countersunk bolts are examined for their effectiveness of anti-loosening under random vibration. Results show that application of double nutting or 60°countersunk bolts is more effective under room temperature; high temperature adhesive or 30°countersunk bolts is superior under high temperature circumstances.