Abstract
This work compares the electrochemical windows of polished and unpolished boron doped diamond (BDD) electrodes with hydrogen and oxygen terminations at a series of temperatures up to 125 °C. The experiment was run at 5 bar pressure to avoid complications due to bubble formation. An alternative method for determining the electrochemical window is compared to the most commonly used method, which defines the window at an arbitrary current density cut-off (Jcut-off) value. This arbitrary method is heavily influenced by the mass transport of the electrolyte and cannot be used to compare electrodes across literature where different Jcut-off values have been used. A linear fit method is described which is less affected by the experimental conditions in a given measurement system. This enables a more accurate comparison of the relative electrochemical window from various diamond electrode types from reported results. Through comparison of polished and unpolished BDD electrodes, with hydrogen and oxygen surface terminations, it is determined that the electrochemical window of BDD electrodes narrows as temperature increases; activation energies are reported.
Highlights
This work compares the electrochemical windows of polished and unpolished boron doped diamond (BDD) electrodes with hydrogen and oxygen terminations at a series of temperatures up to 125 °C
The Cyclic voltammetry (CV) measurements are repeated with each electrode over the temperature range 21–125 °C, to identify how the electrochemical window of BDD is affected by temperature
The extent of the hydrogen and oxygen terminations imparted by the processes described in “BDD surface preparation” section were qualitatively assessed with contact angle measurements
Summary
This work compares the electrochemical windows of polished and unpolished boron doped diamond (BDD) electrodes with hydrogen and oxygen terminations at a series of temperatures up to 125 °C. A linear fit method is described which is less affected by the experimental conditions in a given measurement system This enables a more accurate comparison of the relative electrochemical window from various diamond electrode types from reported results. An alternative approach introduced by Olson and Bühlmann has been considered, which was designed to address the inconsistencies that occur when defining the electrochemical window of an electrode by using Jcut-off values[8] In this method, linear fits are made of the three sections of the CV curve, before and after the oxidation. This method more closely resembles the method of defining the limits of detection of ion-selective electrodes recommended by IUPAC8,9 These methods are compared and contrasted with the aim of setting a standard approach for the determination of electrochemical windows from experimental data. Through use of a buffer system, pH 7, we have fixed the pH throughout the experiments
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