Monday's handover of the "toi moko" follows years of campaigning by New Zealand officials and Maori elders.
It has been held at the Museum of Rouen in northern France since 1875.
More than 300 such heads have been returned from several countries since New Zealand began requesting their return.
French museum officials say they have no idea how the "toi moko" - which is intricately tattooed and has one damaged eye socket - came to be in their possession.
Until 1996, it had been on public display alongside the museum's prehistoric collection, said museum director Sebastien Minchin.
"As was done at the time, they compared the 'savage' from the other side of the world with our local cavemen," he told the Associated Press news agency.
It is thought to be one of some 15 similar relics in French possession and one of about 500 around the world.
'Killed to order'New Zealand first began requesting their return in the 1980s, but France's laws on cultural artefacts meant it could not give up the Maori heads in its possession.
In 2007, Rouen's council voted to send theirs back, but were overruled by the Ministry of Culture, which feared it could set a precedent for countries to reclaim their historical artefacts.
A traditional ceremony with incantations will be carried out in Rouen's town hall on Monday to hand the head over to representatives of Wellington's Te Papa museum, who are touring Europe collecting the relics.
New Zealand's Dominion Post newspaper reported that the delegation would be bringing home nine heads in total.
"The French government have provided Te Papa, on behalf of Maori, the ability to bring these ancestors home," Maori leader Michelle Hippolite told the paper.
"This momentous occasion is filled with joy but is also a time for reflection on the journeys of these tupuna [ancestors]."
The Maori traditionally kept tribal heads as war trophies, but they later became much sought after by Western explorers.
They were in such demand that men were believed to have been killed specifically for their heads and slaves were said to have been tattooed and then killed.
Once back in New Zealand, DNA tests will be carried out on the remains where necessary to determine the correct ancestral lands for a proper burial.
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