Various electroplating/electroforming processes have been used for years to produce nickel‐cobalt components for applications from space industry to tool refurbishing. The mechanical properties (hardness, strength, etc.) are drastically affected by the nickel to cobalt ratio of the alloy, as well as the amount of organic additives and trace contaminants present in the plating tank. Traditionally, chemical or optical methods were used for characterizing the constituents of the resulting deposit. In this paper we present the usefulness of nuclear methods of analysis based on accelerated ion beams for performing both qualitative and quantitative compositional characterization of such alloys. Samples of electroformed materials were prepared in a nickel sulfamate bath with nickel‐cobalt ratios ranging between 70:30 (or 2.33:1) and 80:20 (or 4:1) atomic percent. The samples were analyzed using PIXE (Proton Induced X‐Ray Emission) with proton beam of 1 MeV and RBS (Rutherford Backscattering Spectrometry) with 6 MeV nitrogen beam.

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