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A method of growing large high‐purity Gd single crystals has been developed utilizing a distillation chamber completely sealed by molten Gd. Resistance ratios [ρ(294 K)/ρ(4.2 K)] up to ∼160 have been attained from a starting point of ∼30 in a single distillation run with the resultant crystal grains approaching a cubic centimeter in volume.