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  • Synthesis and Characterization of Magnetite Nanoparticles Via The Chemical Co Precipitation Method

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    Akef Afaneh
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    This document describes an experiment to synthesize and characterize magnetite (Fe3O4) nanoparticles via chemical co-precipitation. Key steps include: (1) mixing FeCl3 and FeCl2 solutions and adjusting pH to 10 with ammonia, producing black Fe3O4 particles; (2) characterizing the nanoparticles using Fourier-transform infrared spectroscopy to identify functional groups. The experiment aims to produce magnetite nanoparticles for applications in areas like biomedicine, using a simple co-precipitation method to control particle size and properties.

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    Synthesis and characterization of magnetite nanoparticles via the chemical co precipitation method

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    This document describes an experiment to synthesize and characterize magnetite (Fe3O4) nanoparticles via chemical co-precipitation. Key steps include: (1) mixing FeCl3 and FeCl2 solutions and adjusting pH to 10 with ammonia, producing black Fe3O4 particles; (2) characterizing the nanoparticles using Fourier-transform infrared spectroscopy to identify functional groups. The experiment aims to produce magnetite nanoparticles for applications in areas like biomedicine, using a simple co-precipitation method to control particle size and properties.

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    28 views4 pages

    Synthesis and Characterization of Magnetite Nanoparticles Via The Chemical Co Precipitation Method

    Uploaded by

    Akef Afaneh
    This document describes an experiment to synthesize and characterize magnetite (Fe3O4) nanoparticles via chemical co-precipitation. Key steps include: (1) mixing FeCl3 and FeCl2 solutions and adjusting pH to 10 with ammonia, producing black Fe3O4 particles; (2) characterizing the nanoparticles using Fourier-transform infrared spectroscopy to identify functional groups. The experiment aims to produce magnetite nanoparticles for applications in areas like biomedicine, using a simple co-precipitation method to control particle size and properties.

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    © All Rights Reserved
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    of 4

    PHYS. CHEM.

    CHEMISTRY DEPARTMENT

    EXPERIMENT 10

    Synthesis and characterization of magnetite


    nanoparticles via the chemical co-precipitation method

    1.1. Introduction

    Magnetic particle sizes from nanometer to micrometer are attractive


    materials not only in the field of magnetic recording but also in the areas
    of biological and medical applications. One of the promising particles is
    the iron oxide nanoparticle of various kinds and derivatives: magnetite
    (Fe3O4), maghemite (γ-Fe2O3), and hematite (α-Fe2O3). These are widely
    used as materials for drug carrier, drug release, cancer therapy. Magnetic
    nanoparticles have intensive interest because of their outstanding
    properties and potential applications in various fields, such as ferrofluids,
    catalysts, colored pigments, high-density magnetic recording media, and
    medical diagnostics. However, many properties of these magnetic
    nanoparticles are size-dependent. For example, when the size of the
    magnetic nanoparticles is below 10 nm, they become superparamagnetic
    at room temperature.

    Magnetite (Fe3O4) has been widely studied in recent years due to its
    interesting magnetic properties and many potential applications,
    PHYS. CHEM. CHEMISTRY DEPARTMENT

    especially being an ideal candidate for biological applications, both as a


    tag for sensing and as an actively agent for antitumor therapy. Fe3O4
    nanoparticles are normally obtained by various chemical-based synthetic
    methods, including coprecipitation, the reverse micelle method,
    microwave plasma synthesis, sol–gel techniques, freeze drying,
    ultrasound irradiation, hydrothermal methods, laser pyrolysis techniques,
    and thermal decomposition of organometallic and coordination
    compound. However, in most of these approaches, the sizes of the as-
    synthesized products are below 30 nm and their size-distribution can only
    be controlled to few extents.

    Coprecipatation technique, which is the most convenient method and it is


    a very common reaction for the synthesis of NPs, for example, Fe3O4.
    Besides the preparation of NPs, this technique can also can be used to
    form shells on preformed cores. In the typical coprecipitation reaction, the
    feature of different solubility of salts in water is taken advantage of. As
    reagents, two or more water-soluble salts are used that react with each
    other. One or more salts that are water-insoluble are formed in the liquid
    phase. When the concentration of this product crosses the solubility
    product value in the reaction media precipitation takes place.
    PHYS. CHEM. CHEMISTRY DEPARTMENT

    2.1. Chemicals and reagents

    Anhydrous FeCl3 98%, FeCl2·4H2O, NaOH pellets were used as received, NH4OH
    solution (25 wt.%).

    2.2. Synthesis of magnetite (Fe3O4)

    Firstly, FeCl3·6H2O (4 ml, 2 M) and FeCl2·4H2O (2 ml, 2 M) were mixed and stirred
    for 45 min at 30 °C. The molar ratio of Fe (III)/Fe (II) was kept 2. Under N 2 gas
    atmosphere, ammonia solution (100 ml, 1 M) was added dropwise to the previous
    solution and pH of the mixture was adjusted to 10. The solution was stirred for about
    1 h until black Fe3O4 particles appeared. The product was filtrated and rinsed with
    distilled water and methanol until neutral filtrate was obtained. The produced Fe 3O4
    NPs were eventually dried at 60 C for 24 h. The following reaction describes the
    formation of Fe3O4 NPs[1].

    Fe (aq
    2 3 
    )  2Fe .(aq )  8OH ( aq )  Fe 3 O 4 ( S )  4H 2 O ( l )
    PHYS. CHEM. CHEMISTRY DEPARTMENT

    3.1. Characterization of the magnetite nanoparticles of


    magnetite (Fe3O4)

    The magnetite nanoparticles were first characterized for the functional groups by a
    FT-IR spectrometer a wave-number range of 4000–400 cm−1.

    3.2. Results and discussion

    BANDS(cm-1 ) FUNCTIONAL TYPE OF INTENSITY


    GROUP VIBRATION

    References

    1. Al-saida, B., et al., Enhanced dual catalytic activities of silver-


    polyaniline/titanium dioxide magnetic nanocomposite. Journal of
    Photochemistry and Photobiology A: Chemistry, 2020. 392: p. 112423.

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