Iron-cobalt alloys have been extensively studied as potential hard disk drive write head materials due to their potentially high saturation flux densities (~2.4T), low coercivities and ease of deposition. Iron-cobalt plating solutions have, however, been shown to have stability issues, necessitating that they be used at low pH or that a stabilizing agent be added to the solution. The purpose of this thesis is to evaluate the stability of a dibasic ammonium citrate plating solution and to characterize the deposits which result from its use. The plating solutions are found to be less stable than previously claimed. The solutions are oxidized by dissolved oxygen, which leads to a valence change in the iron ions and eventually the formation of iron oxide/hydroxide precipitates. These effects are exacerbated by heating or the application of a voltage across the solution. Deposits plated from the solution are fine grained (<40nm) and compact through their thickness. While normally deposited as the equilibrium BCC phase, metastable phases are deposited at elevated temperatures, high pH or in the absence of a stabilizing agent. A metastable phase which is isomorphous to α-Mn is deposited at elevated temperatures. This phase transforms to the BCC phase when annealed at >174ºC and is highly textured. Its presence is detrimental to deposit coercivity.