Liu next played O-Ren Ishii, one of the major villains in Quentin Tarantino's 2003 film, Kill Bill. She won an MTV Movie Award for "Best Movie Villain" for the part. Subsequently, Liu appeared on several episodes of Joey with Matt LeBlanc, who played her love interest in the Charlie's Angels movies. She also had smaller roles as Kitty Baxter in the film Chicago, and as a psychologist opposite Keira Knightley in the thriller Domino. In 2006, she played leading lady and love interest to Josh Hartnett in the crime thriller Lucky Number Slevin. Other appearances include a cameo on the animated shows Futurama (as herself in the episodes "I Dated a Robot" and "Love and Rocket" and The Simpsons (on the season sixteen episode "Goo Goo Gai Pan"), a guest host on an episode of the NBC sketch show Saturday Night Live in 2000 (musical guest" Jay-Z), and the voice of Elise in SSX Tricky.

In April 2006, the documentary Freedom's Fury premiered, with Liu as executive producer. The film dramatizes the Hungarian Revolution of 1956, climaxing with the infamous water polo showdown between Hungary and the Soviet Union at the 1956 Melbourne Olympics, known as the 'Blood in the Water match'.

Her film 3 Needles was released on December 1, 2006. In the film, she plays Jin Ping, an HIV-positive Chinese woman. Liu agreed to star in the film for lower than usual pay because she wanted to spread awareness about the way AIDS is improperly treated in China and Thailand.

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