Simultaneous Atomic Force—scanning Electrochemical Microscopy (Afm-Secm) Imaging of Copper Dissolution

Abstract

Combined atomic force-scanning electrochemical microscopy (AFM-SECM) has been explored for monitoring copper ions generated by dissolution of copper samples while recording induced changes in topography. Released Cu 2+ ions were detected via reduction to metallic copper at the AFM tip-integrated electrode followed by subsequent re-dissolution in bulk solution by anodic stripping voltammetry. Copper crystals electrodeposited on gold substrates were used as model systems to demonstrate the laterally resolved analysis of topographical changes and the simultaneous measurement of localized cation release, which was anodically activated upon exposure to acidified chloride-containing solution. Finally, the potential of AFM-SECM for monitoring spatially resolved corrosion processes with sub-micrometer resolution was illustrated using a pure copper sample.

Importance of Mass Transport and Spatially Heterogeneous Flux Processes for in Situ Atomic Force Microscopy Measurements of Crystal Growth and Dissolution Kinetics

“…19 An exception is integrated electrochemical (IE)-AFM, 6,26 or equivalently combined scanning electrochemical microscopy (SECM)-AFM, which allow the solution conditions to be changed rapidly and significantly, while changes in the substrate are mapped as the process comes back to equilibrium. [27][28][29] Such studies are relatively rare.…”

Digital Holographic Study of pH Effects on Anodic Dissolution of Copper in Aqueous Chloride Electrolytes

“…Copper is one of the most important materials in the industry owing to its relatively noble properties. The anodic polarization of copper in acidic, neutral, and alkaline chloride media has received considerable attention in the literature [1][2][3][4][5][6][7][8][9][10][11][12][13][14]. As the electro-dissolution of Cu is found to be complex, the various mechanisms proposed can be applied for chloride electrolytes.…”

Investigating Pitting Corrosion of Stainless Steel and Aluminium Using Scanning Vibrating Electrode Techniques and Electrochemical Noise Measurement

“…The values of the potential drop or probe peak signal as extracted from the line maps which are used for computation of the calibration factor (CF) for the different electrolytes. An initial probe reading before sudden drop = 174.6*10 -9 V, applied current = 0.025mA=25µA and applied current density = 79.46598856mA/cm 2 were utilized to obtain the CF in accordance with OEM recommendation (0-150mA/cm 2 ) within which a linear relationship exist between the measured probe output and the local current density [9] 2 /V; The SVET test commenced with the performance of a PIS calibration using line scan rather than the conventional area scan. Probe peak output signal voltage values were averaged to reduce the error associated with inconsistent readings of probe signal.…”

“…Some of these techniques include atomic force microscopy (AFM) [7], [8], scanning electrochemical microscopy (SECM) [9], scanning tunneling microscope (STM) [10], electrochemical noise (ECN) [11], [12], Electrochemical Impedance spectroscopy (EIS) [13], and Scanning reference electrode technique (SRET) [15]. The Scanning vibrating electrode technique (SVET) [16], adopted in this study belong to this SRET group, all of which function under the principle of their ability to pick up little changes in electrochemical activity within a localised pit and amplifying it [18], [19].…”