Optimizing the synthesis of cobalt aluminate pigment using fractional factorial design

Abstract

The increasing use of experimental design techniques comes from the growing need to optimize products and processes while minimizing costs and maximizing efficiency, productivity and quality of products. Ceramic pigments have wide application in ceramic industries in which the quality and advanced properties of materials are widely investigated. However, studies are required to improve the procedure for obtaining cobalt aluminate (CoAl2O4) using the Complex Polymerization Method (CPM). With the objective of optimizing this method, a 2(5-2) fractional factorial design was performed using data from UV–vis spectroscopy analysis as a response surface. To determine the best conditions for obtaining (CoAl2O4) in this study, five factors were chosen as input variables at levels determined for this study: citric acid concentration (stoichiometric), pyrolysis time (h), temperature (°C), calcination heating time and rate (°C/min). Through statistical application in the process of obtaining CoAl2O4, it was possible to study which of these factors may have greater influence in optimizing the synthesis. The precursor powders were characterized using TG/DSC thermogravimetric analysis, and the calcined powders were analyzed using X-ray diffraction (XRD) and energy dispersive scanning electron microscopy (SEM/EDS) to confirm the structural and morphological aspects of CoAl2O4. It was found that with increased calcination temperature 700°C<800°C<900°C, the UV–vis bands decreased with increasing absorbance intensity, and with increasing pyrolysis time (h), there is a proportional increase in the UV–vis bands. The model was generated with the conditions proposed in this study due to the determination coefficient of 99.9%, variance (R2), and satisfactory response surfaces, thus obtaining optimization of the process according to the needs and applicability in the ceramic industry of pigments.