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Abstract Prussian Blue Analogues are of major interest for their use in alternative battery technologies due to their charge storing ability with a long life cycle. In this work the Prussian Blue Analogue nickel hexacyanoferrate (Ni-HCF) was produced using an all electrochemical method. Creating charge storing materials with electrochemical processes provides a new approach to the development of battery-like materials. These methods have not been commonly employed because the charge storing material yield is not directly known. The charge storage of the Ni-HCF was characterized with two different methods which provided a measure of the electrochemically active Fe present. These were then compared with the Particle Induced X-ray Emission (PIXE) method which measured the total amount of Fe present. By comparing the electrochemical measurement of active Fe to the total Fe as measured by PIXE, the percentage of material that is active in the charge storage was determined. This enables an independent calculation of the specific charge capacity of the material for comparison to other battery technologies. 

The elemental composition of electrodeposited NiFe thin films was analyzed with particle-induced X-ray emission (PIXE). The thin films were electrodeposited on polycrystalline Au substrates from a 100 mM NiSO 4 , 10 mM FeSO 4 , 0.5 M H 3 BO 3 , and 1 M Na 2 SO 4 solution. PIXE spectra of these films were analyzed to obtain relative amounts of Ni and Fe as a function of deposition potential and deposition time. The results show that PIXE can measure the total deposited metal in a sample over at least four orders of magnitude with similar fractional uncertainties. The technique is also sensitive enough to observe the variations in alloy composition due to sample nonuniformity or variations in deposition parameters.