Hindawi Journal of Nanomaterials Volume 2024, Article ID 9577778, 9 Pages

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Hindawi

Journal of Nanomaterials
Volume 2024, Article ID 9577778, 9 pages
https://doi.org/10.1155/2024/9577778

Research Article
Crystallographic, Morphological, Magnetic, and Thermal
Characterization of Superparamagnetic Magnetite Nanoparticles
(Fe3O4) Synthesized by Chemical Coprecipitation Method and
Calcined at 250°C for 4 hr

Md. Abdus Sabur and Md. Abdul Gafur


Pilot Plant and Process Development Centre, Bangladesh Council of Scientific and Industrial Research (BCSIR), Dhanmondi,
Dhaka 1205, Bangladesh

Correspondence should be addressed to Md. Abdus Sabur; [email protected]

Received 16 October 2023; Revised 27 December 2023; Accepted 8 January 2024; Published 22 January 2024

Academic Editor: Xiaoqian Wang

Copyright © 2024 Md. Abdus Sabur and Md. Abdul Gafur. This is an open access article distributed under the Creative Commons
Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.

Magnetite nanoparticles (Fe3O4) were prepared by chemical coprecipitation method using ferric chloride (FeCl3) and heptahydrate
ferrous sulfate (FeSO4·7H2O) salts employing sodium hydroxide (NaOH) as a precipitant. To determine the size, shape, and
chemical makeup of the produced magnetite nanoparticles, the generated powders were examined by transmission electron
microscope, scanning electron microscope, atomic force microscope, and X-ray diffractometer. It was found that the magnetite
powder had made a face-centered cubic crystal structure and spherical-like particle form with particle diameters of about 30 nm.
The magnetic properties of magnetite nanoparticles were evaluated using a vibrating sample magnetometer. The obtained super-
paramagnetic properties of the produced nanoparticles, with saturation magnetization and coercivity of 50.75 emu/g and 30.09 Oe,
respectively, allow them for applications in drug delivery, MRI contrast agent, catalysis, degradation of antibiotics, antibacterial
activity, removal of heavy metals and organic dyes, etc.

1. Introduction still much to learn about the development of such scalable


synthesis and, consequently, large-scale production.
Applications involving iron oxide nanoparticles (IONPs) are Highly monodisperse IONPs of tunable size can be pro-
receiving a lot of interest in industries that need a lot of them, duced utilizing techniques that thermally decompose precur-
like agriculture and biomass recovery [1–3] and wastewater sors as ferric acetylacetonates in high-boiling-point organic
treatment [4]. Higher quality requirements for IONPs lead to solvents [17–19], and instances of scalable synthesis are known
their use in catalysis [5], batteries [6], and particularly in to exist [20]. An in-depth understanding of the particle gener-
biomedicine [7–9], where they are used for drug delivery ation mechanism during thermal decomposition syntheses
[10], cancer treatment using magnetic hyperthermia [11, 12], was achieved because of the relatively long reaction times (of
and as a contrast agent for MRI [13, 14]. the order of an hour) that allow for thorough examination
The oxide phase, particle shape, size and size distribution, during the synthesis [21–23]. However, because these synthe-
internal composition (such as impurities and grain boundaries), ses require high temperatures (often > 250°C) and expensive
and surface chemistry all have a significant impact on how well chemicals, they are labor and resource-intensive (particularly
they work. Therefore, each application needs a customized syn- for large-scale manufacturing). In addition, if IONPs need to
thetic process that can consistently produce the needed IONPs be disseminated in aqueous solutions, thermal decomposition
in amounts greater than the lab scale. The numerous investiga- syntheses necessitate postprocessing processes, such as purifi-
tions on IONP syntheses [9, 14–16] demonstrate that there is cation and phase transfer, typically after a time-consuming
2 Journal of Nanomaterials

ligand exchange step. This is true for the majority of biological produced by mixing 100 ml 0.4 M FeCl3 with 100 ml 0.2 M
applications, where the regularly employed compounds for FeSO4·7H2O as a precursor. The ions Fe3+ and Fe2+ are
thermal breakdown also face significant difficulties due to created when the FeCl3 solution and FeSO4 solution react.
strict regulatory oversight. Water-based syntheses are, there- As a precipitating agent, a 3 M solution of NaOH was added
fore, preferred. This is one of the reasons that the coprecipita- drop-by-drop to the salt solutions while being stirred con-
tion of iron salts in aqueous solutions, or the simultaneous tinuously until the pH reached 12 and heated the solution at
precipitation of ferrous and ferric ions started by the addition 80°C for 60 min. Then, with the help of a magnetic stirrer hot
of a base, is the most widely used method for synthesizing plate and a molar ratio of 2 : 1, Fe3+ and Fe2+ react with
IONPs. The availability of inexpensive chemicals and straight- NaOH solution to produce coal-black Fe3O4 particles as a
forward experimental techniques at moderate temperatures precipitate. After that, the material was continuously rinsed
(100°C) without harmful byproducts are further factors con- in distilled water until it achieved a pH level of 7 to obtain the
tributing to the success of coprecipitation synthesis. pure Fe3O4 nanoparticles. Finally, particles were calcined for
The benefit of the coprecipitation method is that it gives a 4 hr at 250°C.
crystallite size in the small range contrasted with other syn-
thesis processes based on the precipitating agent selected 2.3. Characterization Techniques
during the reaction. Likewise, the crystallite size and mor- 2.3.1. XRD. The crystallographic properties of Fe3O4 were
phology of the material produced utilizing this technique can identified by recording X-ray powder diffraction patterns
be controlled using capping agents. Higher yield, high prod- (XRD) of powder samples using a Rigaku Smart Lab SE
uct purity, the lack of necessity to use organic solvents, easily X-ray Diffractometer equipped with a CuKα radiation source
reproducible, and low cost are some of the common advan- (λ = 1.5406 Å). Analysis was carried out at 25°C, 40 kV, and
tages of this method [24, 25]. However, the properties of the 50 mA. The 2θ measured range was 20°–70°, at 0.01° steps,
produced particles, such as size, shape, and composition, are with a scan speed of 25.00°/min.
highly dependent on the reaction parameters such as tem-
perature, pH, ionic strength, nature of the basic solution, and 2.3.2. SEM. The morphology of Fe3O4 nanoparticles was
so on. observed using the JEOLUSER 7610F SEM, which operated
Due to variability in IONP core sizes and the existence of at 10 kV. SEM images were analyzed with ImageJ software to
agglomerates, coprecipitation syntheses are known to pro- calculate the particle size distribution of the dried nanoparticles.
duce particles with a high polydispersity and a relatively low
magnetism [16]. The stability and use of the IONPs are now 2.3.3. TEM. The morphology of the Fe3O4 nanoparticles was
complicated by these agglomerates. The simultaneous nucle- analyzed by TEM using a high-resolution LIBRA 120 Plus
ation and development of particles, as well as the existence of Carl Zeiss microscope. TEM images were analyzed with
intermediary phases before or during the production of the ImageJ software to calculate the particle size distribution of
desirable magnetic phases, such as magnetite (Fe3O4) or the dried nanoparticles.
maghemite (γ-Fe2O3), are likely to cause variations in core
2.3.4. AFM. AFM images were performed by CSI AFM nano-
size [26, 27]. According to the synthesis circumstances (pre-
observer microscopy in an oscillating mode using silicon
cursors utilized and their concentration, temperature, pH,
cantilevers with a typical resonant frequency of 138.228
order of reagent and stabilizer addition, etc.), the particle
kHz, scanning speed of 750 mIn/s, resolution of 512 × 512,
formation mechanism is still up for debate and is predicted
and scan size of 5 × 5 µm. The AFM data were analyzed using
to vary [28, 29].
the Gwyddion software.
In this study, sodium hydroxide (NaOH) was used as a
precipitating agent together with ferric and ferrous salts to 2.3.5. VSM. The magnetic properties of Fe3O4 nanoparticles were
create magnetite nanoparticles. The nanoparticles were then measured using VSM in the quantum design physical property
analyzed using X-ray diffractometer (XRD), scanning elec- measurement system DYNACOOL at room temperature with a
tron microscope (SEM), transmission electron microscope magnetic field in the range of −15,000 to 15,000 Oe. About
(TEM), atomic force microscope (AFM), vibrating sample 12.3 mg of dried samples were used for these measurements.
magnetometer (VSM), and thermal analysis (TG-DTA) to
study the crystallographic, morphological, magnetic, and ther- 2.3.6. TG-DTA. The thermogravimetric and differential thermal
mal properties of superparamagnetic magnetite nanoparticles. analysis TG-DTA curves of Fe3O4 nanoparticles were obtained
from EXSTAR 6000, TG/DTA 6300 thermal analyzer with a
2. Experimental Details heating rate of 20°C/min. The mass of the solid specimen was
about 15.032 mg and the whole measurements were carried
2.1. Materials. All of the chemical reagents utilized during the out in a nitrogen atmosphere.
synthesis were analytical grade and did not require any additional
purification. Anhydrous ferric chloride (FeCl3), ferrous sulfate 3. Result and Discussion
heptahydrate (FeSO4·7H2O), and sodium hydroxide (NaOH)
were purchased from Merck (India) with a purity ≥98%. 3.1. XRD Analysis. The XRD pattern of Fe3O4 nanoparticles
is shown in Figure 1. This pattern is used to determine the
2.2. Synthesis of Magnetite Nanoparticles. Using the copreci- crystal structure, lattice parameter, crystallite size, and crystal
pitation approach, magnetite nanoparticles (Fe3O4) were defects of Fe3O4 nanoparticles. In the XRD patterns, the
Journal of Nanomaterials 3

1,200 311 The microstrain of a crystalline solid is calculated using


the following formula:
1,000
β
ϵ¼ ; ð4Þ
Intensity (cps)

800
4tanθ
600 220 440
222
where ϵ is the microstrain of the crystal, β is the FWHM, and
400 400 θ is the angle of diffraction. The average microstrain of Fe3O4
nanoparticles is found to be 0.0133 ppm (Table 1).
200 The crystallite size of Fe3O4 nanoparticles has a signifi-
cant impact on their magnetic characteristics, such as the Ms,
0
20 25 30 35 40 45 50 55 60 65 70
Mr, and Hc. Regardless of the shape and crystal structure of
the particles, the Ms, Mr, and Hc rise with increasing crystal-
2θ (degree)
lite size up to the critical limit [33]. The XRD data suggested
FIGURE 1: XRD pattern of Fe3O4 nanoparticles. that due to smaller crystallite size, the Fe3O4 nanoparticles
are superparamagnetic as well as have smaller Ms and Hc.
most intense XRD peak appears at 2θ = 35.65°, representing 3.2. SEM/EDAX Analysis. SEM images are used to examine
the (311) plane of Fe3O4 nanoparticles. Fe3O4 nanoparticles the surface detail, shape, and average size of the synthesized
show strong peaks at 2θ = 30.25, 35.65, 36.37, 43.15, and Fe3O4 nanoparticles. Figure 2(a) displays an FESEM image
62.78, respectively, confirming the existence of diffraction of Fe3O4 nanoparticles. The SEM image of the synthesized
planes for magnetite at 220, 311, 222, 400, and 440. These Fe3O4 nanoparticles shows that they have a rough surface
peaks have a cubic form and a crystalline structure that are and a cavity-like structure. The average particle size of Fe3O4
typical of magnetite. As a result, the diffractogram of Fe3O4 nanoparticles is about 63 nm, which is determined using
nanoparticles meets the magnetite standard JCPDS 65-3107 ImageJ software [34]. The histogram (Figure 2(b)) displays
(magnetite) requirements [30, 31]. the size distribution of the nanoparticles, where the average
The lattice parameter of the cubic crystal system is deter- diameter of the synthesized nanoparticles is determined to be
mined using the following formula: 63.19 Æ 7.12 nm. The EDAX spectrum of Fe3O4 nanoparticles
reveals the presence of iron and oxygen (Figure 2(c)).
h2 þ k 2 þ l 2
a2 ¼ ; ð1Þ
d2 3.3. TEM Analysis. The TEM images are taken to determine
the morphology, shape, and size of the Fe3O4 nanoparticles.
where a is the lattice parameter, h, k, and l are the Miller Figure 3(a) illustrates the TEM image of Fe3O4 nanoparticles
indices, and d is the interplanar spacing. The calculated that were calcined at 250°C. The HR-TEM image (Figure 3(b))
average lattice parameter of Fe3O4 nanoparticles is 8.398 displays tiny aggregated particles with a mean diameter of
Å (Table 1). about 30 nm that are resolved using ImageJ software [34].
The crystallite size is calculated using Debye–Scherrer’s The histogram (Figure 3(c)) displays the size distribution of
formula given below: the nanoparticles, where the average diameter of the produced
nanoparticles is determined to be 29.56 Æ 7.9 nm. The major-
Kλ ity of the nanoparticles have a size distribution between 25
D¼ ; ð2Þ and 35 nm. The selective area electron diffraction (SAED)
βcosθ
pattern of Fe3O4 nanoparticles demonstrates the presence of
concentric rings connected to several diffraction planes, indi-
where D is the average size of the crystallite, λ is the wave- cating that produced Fe3O4 nanoparticles are polycrystalline
length of X-ray radiation, β is the full peak width at half- (Figure 3(d)).
maximum (FWHM), and θ is the angle of diffraction. The
average crystallite size of Fe3O4 nanoparticles is 17.698 nm 3.4. AFM Analysis. The morphology and the average size of
[32], and 34.862 nm for the most intense peak (Table 1). Fe3O4 nanoparticles are evaluated by AFM. Before the micros-
The number of dislocations in a unit volume of crystal- copy analyses, one to two droplets of 0.1 mg/ml nanoparticles
line materials is determined according to the Segal method as were deposited on a mica surface and left to dry at room
follows: temperature. Topography, amplitude, and phase contrast
images from different regions over the sample surface are
1
δ¼ ; ð3Þ obtained and analyzed using the Gwyddion software [35];
D2 some representative micrographs are shown in Figure 4(a)–
4(c), respectively. Typical AFM images of magnetic nanopar-
where δ is the dislocation density, and D is the crystallite size. ticles (Figure 4) suggest that nanoparticles have a nearly
The calculated average dislocation density of Fe3O4 nano- spherical shape with an average diameter of 51.93 nm as
particles is 3.219 × 1016 line/m2 (Table 1). well as have a single phase of Fe3O4 nanoparticles. Particle
4 Journal of Nanomaterials

TABLE 1: Crystallographic properties of Fe3O4 nanoparticles.


S. no. 2θ (°) hkl d (Å) Lattice parameter (Å) Crystallite size (nm) Dislocation density (line/m2) Microstrain (ppm)
1 30.25 220 2.952 8.349 19.534 2.620 × 1015 0.0071
2 35.65 311 2.516 8.344 34.862 8.227 × 1014 0.0033
3 36.37 222 2.468 8.549 2.599 1.480 × 1017 0.0446
4 43.15 400 2.095 8.380 12.057 6.878 × 1015 0.0081
5 62.78 440 1.479 8.366 19.439 2.646 × 1015 0.0035
Average 8.398 17.698 3.219 × 1016 0.0133

18
16

Frequency of distribution (%)


14
12
10
8
6
4
2
0
40 45 50 55 60 65 70 75 80
Particle size (nm)
ðaÞ ðbÞ

2,000
OKa

1,800
1,600
1,400
Counts

1,200
FeLa

1,000
CKa

800
ClKb
FeLI

600
FeKa
NaKa

FeKesc
ClKa

FeKb

400
200
0
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
(KeV)
ðcÞ
FIGURE 2: (a) FESEM image of Fe3O4 nanoparticles, (b) size distribution of Fe3O4 nanoparticles, and (c) EDAX image of Fe3O4 nanoparticles.

size and surface roughness of Fe3O4 nanoparticles are shown This is because when magnetite nanoparticles are smaller
in Table 2. than the critical size of the magnetic domain size, they exhibit
superparamagnetic characteristics [36–38]. The superpara-
3.5. VSM Analysis. The magnetic characteristics of Fe3O4 magnetism and saturation magnetization (Ms) values in the
nanoparticles are evaluated using a VSM. Figure 5 shows nanosized magnetite samples are lower than the bulk magne-
the hysteresis loops of the Fe3O4 nanoparticles recorded at tite value of 92 emu/g [39]. The saturated magnetization value
room temperature, and Table 3 lists the values for the mag- of Fe3O4 nanoparticles is 50.75 emu/g. The decrease in satu-
netic properties. The magnetization curve for the synthesized ration magnetization with smaller magnetite particle sizes has
magnetite nanoparticles described in this study demonstrates been explained in several ways. One aspect has to do with the
minimal values of remnant magnetization and coercivity spin disorder layer, which grows as crystallite size decreases.
field as well as very little hysteresis behavior for the samples. The result of a dipolar interaction between magnetite nano-
This demonstrates that superparamagnetic characteristics particles can also be used to explain another explanation for
are present in the produced particles at normal temperatures. the decrease in the magnetic moment. The uneven shape of
Journal of Nanomaterials 5

ðaÞ ðbÞ

10
Frequency of distribution (%)

0
15 20 25 30 35 40 45 50
Particle size (nm)
ðcÞ ðdÞ
FIGURE 3: (a) TEM image of Fe3O4 nanoparticles, (b) HRTEM image of Fe3O4 nanoparticles, (c) size distribution of Fe3O4 nanoparticles, and
(d) SAED pattern of Fe3O4 nanoparticles.

ðaÞ ðbÞ
FIGURE 4: Continued.
6 Journal of Nanomaterials

ðcÞ
FIGURE 4: (a) AFM image (topography) of Fe3O4 nanoparticles, (b) AFM image (amplitude) of Fe3O4 nanoparticles, and (c) AFM image
(phase) of Fe3O4 nanoparticles.

TABLE 2: Particles size and surface roughness of Fe3O4 nanoparticles.


Average particle size (nm) RMS roughness (nm) Grain-wise RMS (nm) Mean roughness (nm) Skewness
58.043 20.6954 20.6954 11.4536 3.43140

60
Ms
40
Magnetization, H (emu/g)

20
Mr

0
Hc

–20

–40

–15,000–10,000 –5,000 0 5,000 10,000 15,000


Magnetic field, B (Oe)

FIGURE 5: B–H (hysteresis) curve of Fe3O4 nanoparticles.

TABLE 3: Magnetic properties of Fe3O4 nanoparticles.


Saturation magnetization (emu/g) Remnant magnetization (emu/g) Coercivity (Oe)
50.75 3.03 30.09

magnetite particles may affect the value of saturation magne- the A and B sites may also contribute to the decline in satura-
tization as a contribution from surface anisotropy. Since all tion magnetization [40–42].
the produced samples are virtually spherical, surface anisot- A long-range magnetic dipole–dipole interaction between
ropy should be expected to have little effect. The inadequate the assemblies of superparamagnetic nanoparticles is not present,
crystallization of magnetite during reaction synthesis may be as shown by the disappearance of hysteresis at a small retentivity
the cause of a further drop in Ms. Changes in the population of of 3.03 emu/g and coercivity (Hc) of 30.09 Oe (Figure 5). This
Journal of Nanomaterials 7

30 °C
2.200 100.0
99.9%

2.000 10.00
9.2%
95.0
1.800 181 °C
90.4%
0.00
1.600 2.6% 625 °C 0.4% 90.0
180 °C 87.8%
90.4%
1.400
625 °C
–10.00 999 °C 85.0
87.8%
DTG (mg/min)

1.200 87.4%

TG (%)
DTA μV

1.000 80.0
–20.00
648 °C
0.800 –19.07 μV
324 °C 75.0
0.600
86 °C –23.73 μV
–30.00
–27.46 μV

0.400 74 °C 70.0
0.370 mg/min
–40.00
0.200
65.0
0.000
292 °C 937 °C
–50.00 0.041 mg/min 0.013 mg/min
–0.200 60.0
100 200 300 400 500 600 700 800 900 1,000
Temp. (°C)

FIGURE 6: TG-DTA curve of Fe3O4 nanoparticles.

indicates that when exposed to a magnetic field, the produced 4. Conclusion


magnetite quickly demonstrated magnetization.
The chemical production of magnetite nanoparticles was carried
3.6. TG-DTA. The produced Fe3O4 nanoparticles were sub- out by a simple and facile coprecipitation in an aqueous solution
jected to synchronized thermogravimetric and differential using iron salt as a precursor. TEM image shows that the syn-
TG-DTA, which was carried out in a nitrogen atmosphere thesized magnetite nanoparticles have a spherical particle form
with an increment of 20°C/min and temperatures ranging with an average diameter of about 30 nm, while SEM and AFM
from 25 to 1,000°C. Three predictable weight losses have image shows bigger particle sizes because particles agglomerated
been identified, according to the TG graph (Figure 6). The due to calcination at 250°C for 4 hr. The iron oxide crystal phase
temperature between 30 and 180°C causes a major weight loss could be face-centered cubic magnetite (Fe3O4), according to
of about 9.2%, which is caused by the evaporation of absorbed XRD results. Because there was little coercitivity for the hyster-
water. The second weight loss is caused by the degradation of esis cycles, measurements of magnetization as a function of the
unrefined material, e.g., NaOH and occurs in the temperature field revealed superparamagnetism behavior in the material.
range of 180–625°C. The third weight loss confirms the for- The average diameter of synthesized magnetite nanoparticles
mation of corresponding metal oxide and the spinel phase. proved to be perfect for applications in drug delivery, MRI
There is no weight loss above 625°C, i.e., TGA curves remain contrast agents, catalysis, degradation of antibiotics, antibacte-
steady, which indicates the absolute volatility of water, the rial activity, removal of heavy metals and organic dyes, etc.
completion of the crystallization route, and the immediate
formation of pure materials. DTG curve (Figure 6) shows Data Availability
that the decomposition of absorbed water molecules occurs The data used to support the findings of this study are
at 86°C, where the maximum decomposition rate is about included in the article.
0.37 mg/min. The DTA curve generally shows that the pre-
pared materials undergo both exothermic and endothermic Conflicts of Interest
reactions. The DTA curve (Figure 6) revealed that three endo-
thermic peaks occur at 86°C due to dehydration and 324 and The authors affirm that they have no known financial or
618°C due to the decomposition of anhydrous precursor, interpersonal conflicts that would have appeared to have
respectively [43]. an impact on the research presented in this study.
8 Journal of Nanomaterials

Acknowledgments [13] Y. Bao, J. A. Sherwood, and Z. Sun, “Magnetic iron oxide


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