There was evidence found in New Mexico that the Native Americans had discovered it as early as 3600 B.C.
Like xmanmonk said, ears of popcorn have been found in New Mexico that were 4,000 years old. Popcorn was widely used in the 16th century as a part of Aztec ceremony and as food. It may have first been introduced into European culture when Cortez came into contact with it in the early 16th century through contact with the Aztec.
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