Improvement of the saturation magnetisation using Plackett–Burman design and response surface methodology: superparamagnetic iron oxide nanoparticles synthesised by co-precipitation under nitrogen atmosphere

• Published in: Journal of materials science. Materials in electronics 2021-05, Vol.32 (10), p.13673-13684
• Main Authors: Köçkar, Hakan, Karaagac, Oznur
• Format: Article
• Language: English
• Subjects: Biomedical materials; Characterization and Evaluation of Materials; Chemistry and Materials Science; Coercivity; Coprecipitation; Crystallites; Design of experiments; Fourier transforms; Ion concentration; Iron oxides; Magnetic measurement; Magnetization; Materials Science; Nanoparticles; Optical and Electronic Materials; Optimization; Parameters; Reaction time; Regression analysis; Response surface methodology; Saturation; Synthesis
• ISSN: 0957-4522; 1573-482X
• DOI: 10.1007/s10854-021-05945-z

Superparamagnetic iron oxide nanoparticles (SPIONs) are highly promising materials especially for biomedical applications. Under study, Plackett–Burman (PB) design and subsequent response surface methodology (RSM) from design of experiments were successfully employed for the improvement of saturation magnetisation, M s of SPIONs with zero coercivity, H c . Regression analysis has also been applied to evaluate the M s of the SPIONs. Twelve experiments from PB design were conducted on the synthesis of the nanoparticles by co-precipitation under nitrogen atmosphere. The effects of simultaneously varying independent parameters; Fe 2+ /Fe 3+ molar ratio (MR), total iron ion concentration (TIC), base concentration (BC), reaction time (RTi), stirring rate (SR), and reaction temperature (RTe) on maximum M s response with zero coercivity, H c were studied with the RMS. The most effective and interactive factor for maximum M s with zero H c is found to be the MR. Characterisations of the nanoparticles were performed by vibrating sample magnetometry, X-ray diffraction technique and Fourier transform infrared spectroscopy. After experimental process optimisation, the M s of the synthesised SPIONs were increased from 52.6 to 67.2 emu/g with zero H c . The optimal sample was also shown to be iron oxide with the crystallite size of 10 nm. The linear regression was successfully estimated the M s value (66.7 emu/g) using optimal conditions. The experimental results and predicted values were found to be very close to each other. The results demonstrated that optimal values for the synthesis parameters can be efficiently used for the synthesis of SPIONs with maximum M s .