There's a famous folk tale that the Maharal created a golem, some sort of human shaped creature. The tale has it that he created it using practical Kabbalah.
The gemarra even describes amoraim creating a humanoid using Sefer Yetzira. However, the gemarra doesn't use the word golem.
The word, as I understand it, refers simply to a formless mass. It's used by the Mishnah to chastise uncivilized individuals. What's the earliest usage of the word golem to refer to a humanoid created by humans?