Taking to the court on Tuesday (January 1st), Serena and Roger - along with his Switzerland team-mate Belinda Bencic - will go head-to-head in a match that has been compared to the iconic 1973 Battle Of The Sexes.
Leading 4-1 in the first set, Williams looked set to be cruising to a comfortable victory until her 21-year-old opponent hit back to win the next five games and take the opener.
Federer and Williams, of course, won't be the only players on the court in a mixed doubles match.
The result meant Switzerland beat the U.S. 2-1 overall, with Williams having beaten Bencic 4-6 6-4 6-3 and Federer easily seeing off Tiafoe 6-4 6-1 in their earlier singles clashes. And his partner, Bencic, also won her match putting the finishing touch over the British team in Group B.
"It's great to back out here, I love playing Down Under here in Perth and in Australia, some of my best memories are here" Williams told Channel Nine after the match.
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"I can not imagine having two sets of twins!" "She played really well".
Williams has already declared her intent to get a selfie with Federer to post on Instagram.
"You know I've been training offseason to be ready for Roger, so not sure how I'm going to do but we'll see", Williams said.
The 37-year-olds have won 43 Grand Slam singles titles between them.
"I'm happy in all aspects of my game that things were working - foot work, offensive play, serve, return - it was all there".
Federer's sublime touch at the net proved decisive as he moved closer to a record third Hopman Cup title.
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Switzerland lead Group B at the tournament, followed by Greece and Great Britain, with the U.S. bringing up the rear.
An early break in the final set to Williams was crucial as she used her big serve to hold Bencic at bay and win 4-6, 6-4, 6-3.
Federer's response? "It's the age of social media", he said, laughing at the prospect of Williams' plan.
"I don't know her that well", he said.
Federer echoed Williams' excitement, assuring fans the two sides will be playing to win - and that such a competition might only come around once in their careers.
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