Chronocoulometry for quantitative control of mass removal in micro-structures and sensors

In this work, tungsten wires have been etched in a KOH electrolyte solution. Based on the oxidation state of the electrolytic dissolution reaction's product and time integration of the Faradaic current produced during the reaction, this method is capable of providing a direct measurement of the change in mass of a structure from anodic dissolution. To assess the application of this process for controlled mass removal spanning sub-micrograms to milligrams, two experimental studies and accompanying uncertainty analyses have been undertaken. In the first of these, 5 tungsten wires of length 30 mm were used to remove mass values ranging from 50 to 350 μg. Uncertainty estimates indicate relative combined standard uncertainties of less than 0.3% in the mass changes determined from the measurement of Faradaic current. Comparison of the mass change determined using the electrolytic method, and using a precision ultra-microbalance agreed within this uncertainty. The charge-based method was then applied to modify the dynamic characteristics of a quartz tuning fork oscillator. In these experiments, tungsten fiber attached to one tine of the oscillator was etched in 5 μg increments up to 120 μg of total removed mass. In general, frequency shifts of 2.8 Hz · μg(-1) were observed, indicating sub-microgram resolution for the characterization of probes based on frequency shift and charge-based mass measurement. Taken together, this study provides the basis for a precision method for determining changes in mass based on electrical measurements from an electrochemical system. The utility of this technique is demonstrated through controlled modification of the dynamic properties of a mechanical oscillator.