Determination of phosphorus content from the electrogravimetric response of Ni Players during galvanostatic anodic polarization

Ni P layers demonstrate various favorable functional characteristics, where the P content is the most important property-controlling factor. Therefore, the development of prompt and cost-effective methods for determination of the P quantity in the layer is important. In response to this challenge the current work proposes a simple and low-cost microgravimetric approach for rapid in-situ evaluation of the P content in galvanostatically deposited Ni P layers. The method is based on the application of electrochemical quartz crystal microbalance (EQCM) for electrogravimetric analysis of Ni P anodic dissolution in acidic electrolyte environment. Important factors, including deposition potential, current density and temperature are considered for understanding of the reaction mechanism corresponding to Ni P redox behavior and its gravimetric response. The approach can be realized in a sequential galvanostatic mode, enabling straightforward analysis of the current density impact on the layer composition. The analytical results obtained by means of EQCM are verified by EDX and XPS spectroscopy methods. • EQCM measurements during anodic dissolution were applied for P determination in NiP layers. • Impact factors, like temperature, applied potential and current density) were explored. • The EQCM analysis of the P content show fair agreement with the EDX and XPS analytical data.