Design and Development of Instrumentations for the Preparation of Platinum Single Crystals for Electrochemistry and Electrocatalysis Research. Part 1: Semi-Automated Crystal Growth

In this contribution, we report on a novel design of semi-automated system for the growth of spherical platinum (Pt) single crystals. The system is based on the flame fusion methodology, where the crystal melting/solidification process is controlled by the vertical movement of a hydrogen-oxygen flame by using an actuator. The paper systematically examines the impact of several process variables on the crystal growth. First, the hydrogen-oxygen flame is optimized through control of the gas flow rate and the mixing ratio to ensure the formation of high-quality platinum single crystals. The procedure of crystal growth is documented in a step-by-step manner, starting with cleaning of the Pt wire, followed by the initial formation of metallic sphere, and ending with repetitive zone refining combined with chemical etching. The equilibrium shape of the platinum single crystals is discussed, and the individual low and high Miller index facets identified and visualized. The critical step in the single-crystal growth, the repetitive zone refining, is semi-automated in order to ensure the highest quality crystals and reproducibility, and to minimize any human error.