Reigning featherweight champ Volkanovski stepped up a division to fight Makhachev for the lightweight title in February and lost by decision, and when Makhachev's original opponent Charles Oliveira pulled out 12 days ago, he stepped up again.
The packed Etihad Arena was treated to a short but intriguing battle that burst into life when Makhachev landed a kick to Volkanovski's head, and he followed his opponent to the mat and landed nine unanswered punches before referee Marc Goddard jumped in to stop the fight at 3:06 in the first round.
The knockout was the first suffered by Volkanovski since May 2013, when he lost to Corey Nelson in only his fourth professional MMA fight.
In the co-main event, Khamzat Chimaev put his name firmly in the middleweight title picture with a win over Kamaru Usman, but he was pushed him all the way before edging a majority decision on the judges' scorecards.
Chimaev dominated former welterweight champ Usman in the opening round, but the 36-year-old Nigerian managed to keep the fight on the feet in the second and pressed all the way to the end of the third before coming up short.
