Here's the results of some research I did into the early appearances of Mister Freeze. I was curious and looked into this after watching an episode Batman Caped Crusader, 2.08 Zero Hour.
Four of Mister Freeze's first six appearances in comic books were reprinted in Batman Arkham: Mister Freeze. This collection is available on Hoopla at the time I am writing this. Mister Freeze is the only supervillain in these stories.
- Batman 121 (Feb 1959)
- Detective Comics 373 (Mar 1968)
- Batman 308 (Feb 1979)
- Batman 375 (Sep 1984)
- World's Finest 275 (Jan 1982)
His only other appearance up to 1984 was in a story called Who Killed Batman. There were several supervillains in this story. It doesn't look like Mister Freeze was the primary villain, if there was one, in this story. Who Killed Batman was reprinted in Batman: The Strange Deaths of Batman which is not currently available on Hoopla.
- Batman 291 (Sep 1977)
- Batman 292 (Oct 1977)
- Batman 293 (Nov 1977)
- Batman 294 (Dec 1977)
Mister Freeze had an Earth-2 counterpart who never appeared in a comic book but was mentioned once, in The Brave and the Bold 182 (Jan 1982).
Other stories in which Mister Freeze appeared (post-COIE) that caught my eye
- Batman: Legends of the Dark Knight 190-191: Cold Snap
- Batman: Legends of the Dark Knight 192-196: Snow
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