Owing to the increasing competition and time-to-market pressure, new products and new process technologies are constantly developed and ramped-up in high-tech industries. To ensure operational quality and manufacturing excellence, process validation is a critical procedure. However, little research has been done on process validation in high-tech industries. This study aims to develop a systematic process validation procedure, on the basis of UNISON decision analysis framework and international standards, and construct a set of validation indices that are appropriate for high-tech industry. To estimate the validity of this approach, an empirical study was conducted in a liquid crystal production plant for their process validation and the results showed practical viability of this approach. Similar approaches can also be developed for other high-tech industries to enhance operational quality.