Optimizing microwave-assisted synthesis of akermanite nanoparticles using citric acid as a chelating agent: A combined machine learning and experimental approach

Abstract

This study aims to synthesize akermanite (Ca2MgSi2O7) using an eco-friendly and fast microwave-assisted method and understand the effect of using citric acid (CA) as a chelating agent to optimize the calcination temperature for synthesizing pure akermanite nanoparticles (along with a trace amount of merwinite) at low calcination temperatures. This study developed a new predictive model by machine learning-assisted modeling to advance the understanding of relationship between synthesis parameters and the resulting purity and particle size of akermanite. To evaluate the reliability of the developed model in predicting the purity and characteristics of the resultant Ak powder, the crystallization behavior and phase formation sequence of citric acid-containing samples and those without citric acid were experimentally investigated by differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. Following validation and training, the developed model indicates promising effects of citric acid on reducing crystallization temperature, enhancing purity, and decreasing particle size. The synthesized powders were further characterized by field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM) analyses. For the first time, our results addressed the microwave-assisted synthesis as an effective method via experimental evidence and machine learning-assisted modeling that allows for the production of akermanite containing a trace amount of merwinite with the aid of citric acid at a relatively low calcination temperature of 950 °C. In vitro bioactivity evaluation supported the potential suitability of Ak powders for bone tissue engineering applications.