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Fe–Ni alloy with a Ni content of 36% by mass exhibits the smallest coefficient of thermal expansion and is known as invar alloy.1–4) In the field of electronic communication devices, such as semiconductor lead frames and the package components of optical fibers, Fe–36 mass% Ni alloy has been widely used as a material with low thermal expansion.5) Invar alloys are produced by melting and casting methods and by rolling, but these manufacturing processes limit the form and accuracy of the dimensions of the products. If these invar alloys can be produced by electrodeposition, the range of products that could be formed by deposition will increase and the manufacturing cost will decrease.6) For example, in the vacuum deposition of an organic electroluminescence layer in a smartphone, the metal mask is set Effects of Electrolyte Composition and Additives on the Formation of Invar Fe–Ni Alloys with Low Thermal Expansion Electrodeposited from Sulfate Bath