In order to solve the crack problem of the traditional ceramic barrier films, RF magnetron co-sputtering method was used for the preparation of TiNx/CFy films on PP substrate. Relative volume ratio of the hard phase TiNx and soft phase CFy was controlled by varying the input RF power ratio between PTFE (Polytetrafluoroe thylene) target and the Ti target. Chemical composition of the composite film was explored using RBS and FTIR, based on which the TiNx volume content in the composite films was calculated. Also, the relationship between the TiNx volume content and OTR and WVTR was established. The results showed that the detailed structure, the volume content of TiNx phase and CFy phase had direct effects on OTR and WVTR values, and also on the flexibility performance of the films. The flexibility and barrier properties of the composite film was the best when the TiNx phase volume content was 0.28.