Recorded on the Phonautograph, an invention of Édouard-Léon Scott de Martinville (Frenchman of Scottish ancestry).
The device used a boar's bristle attached to a vibrating membrane. It scribed
its vibrations onto a surface coated with lampblack.
Scott de Martinville hoped to invent a playback mechanism, but never
did. Fortunately a few of his recordings survived, and in 2008 some smart fellas in California managed to get a voice from the tracings: probably Scott
de Martinville himself singing (very slowly) the first few notes of "Au clair
de la lune".
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