Elsevier

Vacuum

Volume 163, May 2019, Pages 236-247
Vacuum

Study of phase transformations, structural, corrosion properties and cytotoxicity of magnetite-based nanoparticles

https://doi.org/10.1016/j.vacuum.2019.02.029Get rights and content

Highlights

  • The experimental series metabolic activity of studies cells.

  • Magnetic nanoparticles based on metal oxides.

  • Oxide nanoparticles were synthesized by a mixture of iron (II) and (III) chloride.

  • Nanoparticles is characteristic of nanoscale ferromagnetic materials.

Abstract

This paper presents the results of the structural, corrosion, magnetic properties and cytotoxicity of magnetite nanoparticles, phase transformations was studied by thermal annealing. It was established that thermal annealing of Fe3O4 nanoparticles led to three stages of phase transformations from magnetite to maghemite, with the subsequent formation of the hematite structure. Increasing annealing temperature lead to a change in the magnitudes of the hyperfine magnetic field, quadrupole displacement and isomeric shift that indicates a change in the crystal structure and annealing of defects, which eventually leads to the ordering of magnetic nanoparticles. Studying the degradation of nanoparticles in PBS solution shows us that a change in the crystal structure as a result of a decrease in the degree of perfection and the formation of amorphous inclusions leads to magnetic disordering and a subsequent change in the magnitude of the hyperfine magnetic field. Cytotoxicity results indicate that nanoparticles do not show cytotoxic activity against tested L929, PC-3 and HeLa cell lines, because in all experimental series metabolic activity of studies cells was not below 70% of control.

Introduction

To date, magnetic nanoparticles based on metal oxides are of great interest, both from the science and industry. There is a huge variety of methods for synthesis of nanoparticles with various geometry and structural properties [[1], [2], [3], [4], [5]]. Chemical methods of precipitation and sol-gel methods are widely used for the synthesis of oxide nanoparticles [[2], [3], [4], [5], [6]]. These methods are based on the simplest chemical reactions of the metal nanoparticles reduction in saturated solutions together with external influences (temperature, vigorous stirring, pressure, etc.) [[7], [8], [9], [10], [11], [12], [13], [14], [15]]. Moreover, in most cases, the obtained colloidal solutions contain precipitate of large agglomerations of particles. To avoid agglomeration of nanoparticles into large clusters, as a rule, organic additives is added in the synthesis process. One of the common additives is graphene [16,17].

The wide application of materials based on metallic nanoparticles is due to high values of specific surface area; specific electronic structure, that is close to the semiconductors, and as a consequence, an unusual combination of electrical, magnetic, optical properties, not typical for massive metal samples [[18], [19], [20], [21], [22]]. Controlling the shape, size, and chemical composition of nanostructures both at the stage of synthesis and in subsequent modification allows one to control their physical properties and opens up new possibilities for their practical application [[23], [24], [25], [26], [27]]. Magnetite Fe3O4 nanoparticles found application in various fields of science and technology [[27], [28], [29]]. Wide interest of these nanoparticles is caused by their adsorption properties, biocompatibility and superparamagnetic properties [[30], [31], [32], [33]]. All these properties make magnetite nanoparticles promising objects for biomedical applications, including magnetic resonance imaging for clinical diagnostics, carriers for targeted drug delivery, for immobilization of anenzymes and etc. However, the efficiency of using magnetic nanoparticles depends on the size effect of nanoparticles, their resistance to external influences, phase transformations, corrosion and degradation resistance, and toxicity of nanoparticles [[34], [35], [36], [37], [38]].

The main features of magnetic nanoparticles based on iron oxide is their resistance to changes in physicochemical properties and structural characteristics under the influence of external factors, such as aggressive media, ionizing radiation, etc. Low toxicity of magnetite nanoparticles and their relative easy dissolving in biological media, as well as their natural excretion over a fast time period (from 7 to 30 days), compared with other nickel-based nanoparticles [39,40], copper [41], iron-nickel [42] makes them the most promising materials for biological and medical applications. Fe3O4 nanoparticles also can be treated by heat for controlled phase transformations of nanoparticles with a change not only of the structural characteristics, but also of magnetic properties [43,44]. By controlling the temperature and heat treatment time, both partial and complete phase transformation of nanoparticles from the magnetite phase to hematite or maghemite can be achieved. At the same time, the formed phases are rather stable and are able to retain their properties for a long time [45,46].

This paper presents the results of a study of the structural, magnetic, corrosion properties and cytotoxicity of Fe3O4 nanoparticles obtained by chemical deposition. The effect of temperature annealing on the phase transformations of nanoparticles that affect the structural and magnetic properties of nanoparticles was evaluated.

Section snippets

Materials and methods

Structural and compositional analysis was done with either a JEOL JEM 2100 LaB6 or ARM200F transmission electron microscope (TEM) operated at 200 kV.

X-ray diffraction analysis was carried out on a D8 ADVANCE ECO diffractometer (Bruker, Germany) using CuKα radiation. In order to identify the phases and study the crystal structure, the software BrukerAXSDIFFRAC.EVAv.4.2 and the international ICDD PDF-2 database were used.

The investigation of magnetic properties was carried out using the

Synthesis and characterization of Fe3O4 nanoparticles

Oxide nanoparticles were synthesized by a mixture of iron (II) and (III) chloride and the addition of ammonium hydroxide. The reaction of iron oxide nanoparticles formation:FeCl2 + 2FeCl3 + 8NH3·H2O → Fe3O4 + 8NH4Cl + 4H2O

FeCl2 (2 M) and FeCl3 (1 M) was dissolved in 2 M HCl. To the solution, 50 ml of NH4OH (0.7 M) was added dropwise through a funnel over a period of 5–10 min, while simultaneously stirring with a magnetic stirrer. After synthesis, the nanoparticles were washed, ultrasonicated

Conclusion

This paper presents the results of the structural, corrosion, magnetic properties and cytotoxicity of magnetite oxide nanoparticles. According to the XRD data, transmission electron microscopy and Mössbauer spectroscopy, the initial nanoparticles are magnetic polycrystalline particles of Fe3O4 magnetite with a highly disordered magnetic texture and the average size of 20–25 nm. As a result of phase transformations studies during thermal annealing, it was found that an increase in temperature

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