Ultralow-dielectric-constant (k) porous SiCOH films have been prepared using 1,2-bis(triethoxysilyl)ethane, triethoxymethylsilane, and a poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer template by means of spin-coating. The resulting films were characterized by cross-section scanning electron microscopy, small-angle x-ray diffraction, atomic force microscopy, Fourier-transform infrared spectroscopy, nanomechanical testing, and electrical measurements. Thermal treatment at 350°C for 2 h resulted in the formation of ultralow-k films with k of $2.0, leakage current density of 3 9 10 À8 A/cm 2 at 1 MV/cm, reduced modulus (E r ) of $4.05 GPa, and hardness (H) of $0.32 GPa. After annealing between 400°C and 500°C for 30 min, the resulting films showed fluctuant k values of 1.85 to 2.22 and leakage current densities of 3.7 9 10 À7 A/cm 2 to 3 9 10 À8 A/cm 2 at 0.8 MV/cm, likely due to the change of the film microstructure. Compared with 350°C annealing, higher-temperature annealing can improve the mechanical strength of the ultralow-k film, i.e., E r % 5 GPa and H % 0.56 GPa after 500°C annealing.