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Response surface method optimization of synthesized superparamagnetic magnetite (Fe3O4) nanoparticles characterized by pulsed IR calibration-free laser-induced breakdown spectroscopy

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Abstract

Magnetite nanoparticles (Fe3O4) are the subject of numerous investigations, particularly regarding synthesis conditions. In this study, we used the Response Surface Method (RSM) to optimize Fe3O4 synthesis conditions by modifying the concentration of iron salts, oxidizing medium and reaction temperature. The samples were characterized by Field Emission Scanning Electron Microscope (FESEM), Vibrating Sample Magnetometer (VSM), X-ray Diffraction (XRD), and Transmission Electron Microscopy (TEM). Ten experimental runs with two independent variables and one categorical variable were proposed using the three-level-three-factor design. The results were statistically analyzed using ANOVA. The analysis confirmed that the response variables were significantly influenced by factors A (concentration of iron), B (concentration of the alkaline), A2, and B2 with a p value less than 0.05. In this work, the Adequate Precision i.e., the signal-to-noise ratio, which should be more than four, were 20.50 and 24.48 for both models indicating an adequate signal to explore the design space. The optimized condition for the smallest particle size with the highest saturation magnetization of 60 emu/g was determined using 0.012 M of iron salts, 0.9 M of an alkaline medium concentration, and a reaction temperature of 70 °C. The mean particle size of nanoparticles was about 9.8 ± 1 nm using the Digitizer Image Analysis software. The calibration-free laser-induced breakdown spectroscopy (CF-LIBS) indicated the plasma temperature was about 5000 ± 200 K, obtained from the slope of the Boltzmann plot and an optimal iron/oxygen ratio of 0.769. This research effectively connects the data obtained by RSM with C-F LIBS.

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Authors and Affiliations

  1. School of Metallurgy and Materials Engineering, Iran University of Science and Technology (IUST), Narmak, Tehran, 16844, Iran

    Maryam Tajabadi

  2. Laser and Nanobiophotonics Lab., Faculty of Biomedical Engineering, Amirkabir University of Technology (AUT), Tehran, Iran

    Mohammad E. Khosroshahi & Hamideh Rezvani Alanagh

  3. Nanobiophotonics and Biomedical Research Laboratory, MIS Electronics Inc., ON, L4B 1B4, Richmond Hill, Canada

    Mohammad E. Khosroshahi

  4. CAS Key Laboratory of Nanosystem and Hierarchical Fabrication, CAS Center for Excellence in Nanoscience, National Center for Nanoscience and Technology, Bei**g, 100190, People’s Republic of China

    Hamideh Rezvani Alanagh

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  1. Maryam Tajabadi
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  2. Mohammad E. Khosroshahi
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  3. Hamideh Rezvani Alanagh
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Contributions

MT contributed to the synthesis of nanoparticles, experimental work, and hel** with the manuscript. MEK contributed to laser spectroscopy, analyzing the results, and manuscript preparation. HRA contributed to the synthesis of nanoparticles and characterization.

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Correspondence to Mohammad E. Khosroshahi.

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Tajabadi, M., Khosroshahi, M.E. & Alanagh, H.R. Response surface method optimization of synthesized superparamagnetic magnetite (Fe3O4) nanoparticles characterized by pulsed IR calibration-free laser-induced breakdown spectroscopy. Appl. Phys. A 129, 439 (2023). https://doi.org/10.1007/s00339-023-06720-z

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