Fe2O3
Review: Nanostructure, Synthesis Methods, and Applications
Novita1, Ramlan2, Marzuki Naibaho3, Masno
Ginting4, Syahrul Humaidi5,
Tulus Na Duma6
Department
of Physics, Universitas Sumatera Utara, Indonesia1,5,6
Department
of Physics, Universitas Sriwijaya, Indonesia2
Research
Center for Advanced Materials, National Research, and Innovation Agency (BRIN),
Indonesia3,4
Email:
[email protected]1,
[email protected]2,
[email protected]3,
[email protected]4,
[email protected]5,
[email protected]6
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Keywords |
|
ABSTRACT |
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Fe2O3,
Nanostructures, Synthetic Methods, Applications. |
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Iron sand,
which contains magnetite iron ore, exhibits unique magnetic properties when
exposed to magnetic fields. Iron ore content, including α-Fe2O3, FeTiO3,
Magnetite (Fe3O4), and others, provides potential uses in various industries
such as electronics, energy, chemical, ferrofluids, catalysts, and
biomedicine. The location of the discovery of iron sand can affect its
mineral characteristics and geological conditions. This research aims to
develop innovative synthesis methods to produce hematite nanomaterials from
iron sand. Nano-size hematite nanoparticles exhibit unique characteristics,
including an increase in specific surface area that is beneficial in
applications such as gas sensors, catalysts, lithium-ion batteries, and the
manufacture of permanent magnets. Through a literature review, this article
presents comprehensive insights into the characteristics of iron sand,
variations in synthesis methods, and the structure of hematite nanoparticles.
Applications of hematite nanoparticles in water treatment, catalysis, and
energy storage are also detailed. This article is expected to contribute to
the development of innovative nanomaterial technologies as well as explore
the potential of iron sand resources for wider industrial applications. |
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INTRODUCTION
Iron sand is one type of sand containing magnetite iron ore.
The iron ore content in this sand gives it unique properties in the form of
magnetic properties. When exposed to external magnetic fields, iron sand can
exhibit magnetic behavior and even attract metal objects. This phenomenon makes
iron sand not only an object of geological exploration, but also a valuable
resource in industrial contexts such as, electronics, energy, chemistry,
ferrofluids, catalysts, and biomedicine
Iron sand contains various magnetic minerals such as
α-Fe2O3, FeTiO3, SiO2, Magnetite (Fe, Maghemite) γ-Fe2O3, Alumina
(Al2O3), and Rutile (TiO2). Iron sand can also
contain impurities such as clay, non-metallic minerals, or organic material.
Iron sand generally has a black or dark brown color, reflecting a significant
magnetite content. The size and shape of iron sand grains can vary this is due
to deposition processes such as erosion or transport by water. The
characteristics of iron sand may vary depending on the mineral composition and
geological conditions in which iron sand is found Kandungan
Senyawa Ki
Iron sand can be found in various locations around the
world. Iron sand mines are often located in coastal areas, rivers, or lakes
that are places of deposition of sedimentary material. In its use, iron sand
found in nature needs to be synthesized first to produce pure hematite content
Current research highlights an innovative synthesis method
that can produce nanomaterials from pure hematite. Hematite in the nanoscale
has shown unique and distinct characteristics compared to its bulk form. With nanosize, the specific surface area of hematite can
increase significantly while maintaining its magnetic properties. The wider
surface provides benefits in a variety of applications such as gas sensors,
catalysts, lithium-ion batteries, and pigments, and can also be utilized in the
manufacture of permanent magnets
By reviewing the latest literature and research, this review
article will compile a comprehensive understanding of the characteristics of
iron sand based on the location of its discovery, explore various methods that
can be used to produce hematite nanoparticles, and decipher the structure of
hematite nanoparticles. Various applications of hematite nanoparticles will
also be discussed to determine their development. This article is expected to
provide new insights into the potential of iron sand resources and contribute
to the development of innovative nanomaterial technologies.
METHODS
This literature research method review will begin by
investigating the various literature sources that have been presented to
understand the characteristics of iron sand based on the location of its
discovery. Consideration will be given to the content of magnetic minerals and
impurities in iron sand, as well as variations in grain size and shape affected
by the deposition process. Next, research will focus on innovative synthesis
methods to produce hematite nanomaterials from iron sand. The analysis will cover
the unique characteristics of hematite at the nanoscale, with an emphasis on
increasing the specific surface area and maintaining its magnetic properties.
This article will compile a comprehensive understanding of the structure of
hematite nanoparticles and present various applications of hematite
nanomaterials, such as gas sensors, catalysts, lithium-ion batteries, and
permanent magnet manufacturing. This literature review is expected to provide
new insights into the potential of iron sand resources and contribute to the
development of innovative nanomaterial technologies, especially in the context
of water treatment, catalysis, and energy storage.
RESULTS
Coastal
Areas
Coastal areas are known
as places where the process of material deposition by seawater occurs. The
deposition of material by seawater will affect the concentration of iron
minerals. Therefore, iron sand in coastal areas has a high iron content. In
addition to iron minerals, iron sand in coastal areas can also contain
additional minerals such as ilmenite, magnetite, or other metal minerals.
Comparison of iron sand characteristics of coastal areas in Indonesia can be
seen in Table 1
Iron sand in coastal
areas occurs due to rocks containing iron minerals eroded by sea waves and
carried to the coast. In addition, the process of weathering and erosion also
plays a role in forming iron mineral particles that are free from the original
rock. The accumulation of iron sand along the coast or coastline occurs with
the help of tides
Table 1.
Comparison of iron sand characteristics of coastal areas in Indonesia
|
Location Name |
Dominant Minerals |
Additional Minerals |
Physical, Mechanical, and Chemical Properties |
Reference |
|
Sunur Beach, West Sumatra |
Magnetite, Hematite,
and Ilmenite |
Quartz, and anapit |
Magnetic granules are
large, multidomain, and mineral growth modes form lamellae. |
(Fatni Mufit et al., 2006) |
|
South Coast of West
Java |
Magnetite, Hematite |
Silicon, Graphite, Clinoferrosilite |
Not explained further |
(Setianto et al.,
2017) |
|
Sampulungan Beach, South Sulawesi |
Magnetite |
Titanium, Chromium,
Vanadium, and Manganese |
It is ferrimagnetic,
multidomain magnetic grain, and fine magnetic fraction. |
(Tiwow et al., 2018) |
|
Keumumu Beach, Aceh |
Magnetite |
Silica, Calcium,
Aluminum, Potassium, and Titanium |
The sand fraction is
very fine, rounded and well rounded. |
(Purnawan et al.,
2018) |
|
Puntaru Beach, East Nusa Tenggara |
Magnetite |
Aluminum, Silica, and
Potassium |
Softmagnetic, and ferrimagnetic |
(Karbeka et al.,
2020) |
|
Ivory Coast, East
Nusa Tenggara |
Magnetite, and
Hematite |
Aluminum, Silica,
Potassium, and Titanium |
Not explained further |
(Fithriyani et al.,
2018) |
|
North Coast, Central
Java |
Hematite, maghemite |
Titanomagnetite, and titanohematite |
Fine grain, and
pseudo-single domain (PSD) |
(Yulianto et al.,
2003) |
|
Kata Beach, West
Sumatra |
Hematite |
Carbon, Aluminum,
Silica, Calcium, and Manganese |
Black, Difficult to
reduce, and softmagnetic. |
(Rianna et al., 2018) |
River
Iron sand in rivers
generally has varying grain sizes, depending on the process of transportation
and deposition by water. The size of sand grains in rivers is usually smaller
than the size of sand grains in coastal areas. This can occur due to the
process of transportation by water until it arrives at the river can break the
grain. The color of iron sand in rivers can vary, but usually has a brighter
color than the color of iron sand in coastal areas
Iron sand is often
unevenly distributed along river flows due to the deposition process. The
deposition process can lead to the deposition of iron sand in certain areas
such as, river bends and prominent plains along the flow. In addition, strong
river currents can transport and precipitate different iron particles in
different parts of the water flow. The iron sand content in the river has
impurities such as clay, non-metallic minerals, or organic material
Table 2.
Comparison of the characteristics of river iron sand in Indonesia
|
Location Name |
Dominant Minerals |
Additional Minerals |
Physical, Mechanical, and Chemical Properties |
Reference |
|
Batang Kuranji River, West Sumatra |
Albite, magnetite |
Quartz, halloysite,
saponite, and pyrophyllite |
Ferromagnetic
minerals |
(Afdal &; Niarti, 2013) |
|
Central Lampung |
Ilmenite, and
Potassium Chloride |
Not explained further |
Antiferromagnetic |
(Puspitarum
et al., 2019) |
|
Tor River, Papua |
Magnesioferrite |
Augit-aluminian |
Magnetization is high
saturation, and coercive field is low. |
(Togibasa
et al., 2018) |
|
Sompang River, East Lombok |
Silica |
Aluminum, Carbon,
Sodium, and Potassium |
It is finely grained,
and has a smaller size than river sand |
(Meiliyadi
et al., 2022) |
|
Bah Bolon River,
North Sumatra |
Magnetite, Hematite,
and Maghemite |
Titanium, Aluminum,
Copper. Manganese, Silica, Vanadium |
It is soft magnet,
and high saturation. |
(Novita et al., 2023) |
Based on research that
has been done, the mineral content in iron sand in rivers has a more unique
diversity than the mineral content in iron sand in coastal areas. This can
occur because the iron sand in the river has mixed with various minerals during
the transportation process by water.
Hematite Nanostructure (α-Fe2O3)
Hematite (α-Fe2O3) has properties that are difficult to
corrode so it is suitable for applications such as gas sensors, catalysts, lithium-ion
batteries, and pigments, it can also be used in the manufacture of permanent
magnets. At high temperatures, the α-Fe
Figure
1. (a) Corundum structure of hematite
(α-Fe2O3); (b) Rhombohedral shape of hematite crystal lattice (α-Fe2O3)
To produce α-Fe 2O3 nanoparticles is carried out using
several methods, including the sol-gel method, from which the
particle size of α-Fe2O3 between 10 – 20
nm, the hydrothermal method with a particle size of 30 nm, the ball miling method, with a particle size of 99.14 μm –
93.34 μm, and the coprecipitation method, with a
particle size of 22.8899 nm
Various nanostructures have been studied on hematite by
varying the synthesis process. The nanostructures formed during the synthesis
and fabrication process also depend on different factors such as synthesis
methods, types of precursors, stabilizers, substrates, and not to mention their
parameters, for example, temperature and time variations in the synthesis
process. Nanostructures are useful for a wide range of applications due to
their unique structure and optical and electrical behavior. The nanostructure
of α-Fe2O3is nanorods, as shown in Figure 2, micro-cubes, nanowires, nanotubes,
nanoflakes, flower-shaped hematite, nanoparticles, and nanorod arrays
Figure
2. Nanostructure of α-Fe2O3; (a) microcubes, (b) nanowires, (c)
nanotubes, (d) nanoflakes, (e) nanorods, (f) microstructure orientation, (g) sea-urchin
shaped, and (h) worm-shaped.
Hematite nanostructure synthesis
Coprecipitation
Iron
sand is separated by impurities using neodymium magnets. The result is then
dissolved into HCl, with the reaction:
Fe2O3 + 6HCl → 2FeCl3 +
3H2O
Stirred
and heated at 80oC using a magnetic stirrer at a speed of 350 rpm for 2 hours.
Precipitation is carried out by dripping ammonium hydroxide (NH4OH)
dissolved to pH 6 and forming a precipitate by the reaction:
2FeCl3 + 3H2O + 6NH4OH → 2Fe (OH)3 +
6NH4Cl + 3H2O
The resulting precipitate
is washed with equates and dried in a memmert oven at
100°C for 19 hours, with the reaction:
2Fe (OH)3+6NH4OH+3H2O→
2FeOOH+6NH4Cl+5H2O
The dried sample is ground and then calcined. The synthesis
process using the coprecipitation method can be seen in Figure 3. The weakness of the
coprecipitation method is that the grain size distribution of nanoparticles
tends to be large, as well as the polydisversiveness
of small particles. Nanoparticles are easily agglomerated the synthesis of
nano-hematite using the coprecipitation method has been reported in various
studies. A comparison of the results of each study that has been conducted can
be seen in Table 3.
Figure 3. Flow of the coprecipitation method
Table 3.
Comparison of research results using the coprecipitation method
|
Coprecipitation Variation |
Particle Size and Shape |
Physical, Mechanical, and Chemical
Characteristics |
Influence of Process Parameters |
Ref. |
|
FeCl precursor3and
NH4OH precipitator |
Hexagonal
crystal structure, polygonal morphology, average particle size 10-25 nm. The
surface area of the particle is about 17.937 m2/g. |
The average
pore diameter is 85.67 nm, and the total pore volume is 0.2699 cm3/g.
It has a band gap of 1.8 eV. |
This
method promises to narrow the band gap in the iron oxide system. |
(Parvathy
Namboothiri &; Vasundhara, 2023) |
|
FeCl precursors3and
NaOH precipitators |
The
crystal measures 41.7 nm, the average particle size of 50-150 nm is
spherical. |
Agglomeration
occurs, and it is chemically stable. |
Temperature
affects the formation of nanophases. |
(Gobinath et al., 2015) |
|
FeCl precursor3and
NH4OH precipitator |
The
rhombohedral/hexagonal crystal structure measures 16-44 nm. |
Agglomeration
occurs, has seven phonon modes, crystals are formed at low temperatures. |
The
concentration of precursors affects the size, crystallinity, morphology, and
formation of clots. |
(Fouad
et al., 2019) |
|
FeCl precursor3and
NH4OH precipitator |
The
particles are 30 nm in size, shaped like a ball with the formation of
clusters, hexagonal crystal structure. |
Bandgap
energy 2.58 eV. |
Nano-hematite
powder has a uniform size when calcined at 500oC. |
(Farahmandjou &; Soflaee,
2015) |
|
FeCl precursor3and
NH4OH precipitator |
The
smallest particle size is 21 nm, spherical. |
It has
a band gap of 2.09 eV. |
An
increase in the concentration of precursors leads to an increase in
nanoparticle size. |
(Lassoued et al., 2017) |
Gel Insoles
The
sol-gel method is a synthesis method that requires chemical engineering. The
term sol-gel comes from two words, namely: 1) sol refers to a precursor
solution that will be used as the starting material for the synthesis of Fe2O3
nanoparticles; and 2) gel refers to the form of the final product of
synthesized nanoparticles in the form of gels. The sol-gel method is commonly
used to synthesize ceramic materials and is not suitable for synthesizing oxide
nanoparticles, so additional modifications are needed in using this method. The
sol-gel method is a chemical method that has a complex procedure. Many
synthesis parameters must be observed
Table 4.
Process Parameters of Gel Soles
|
Process Stages |
Process Objectives |
Process Parameters |
|
Chemical Solutions |
Forming Gels |
Precursor type, Solvent type, Water content,
Precursor concentration, Temperature, and pH |
|
Aging |
Let the gel sit to change properties |
Time, Temperature, Fluid composition, Aging environment |
|
Drying |
Removing water from the gel |
Drying method (ovaporative,
supercritical, and freeze drying), Temperature, Pressure, Time |
|
Calcining |
Changes the physical/chemical properties of
solids, often resulting in crystallization and densification |
Temperature, Time, Gas (inert or reactive) |
The
sol-gel method has several disadvantages, namely: 1) it produces a lot of
alcohol during the calcination process, 2) it requires additional heat
treatment at high temperatures, and 3) the nanoparticle permeability is high,
and the bonding power of nanoparticles is weak
Hydrothermal
Hydrothermal
is formed from the words hydro which means water and thermal which means heat. So the hydrothermal method is a method that uses water and
heat whose properties convert solutions into crystals. The hydrothermal method
must be performed in a closed system to prevent solvent loss when heated above
its boiling point
Hydrothermal
synthesis is widely used in the manufacture of metal oxides. Metal oxide
synthesis can occur in two stages. The first stage is hydrolysis of the salt
solution to produce metal hydroxide. The second stage is that the hydroxide
will be dehydrated to produce the desired metal.
Water is
the most effective solvent in dissolving ionic compounds at high temperatures
and pressures. Water can also act as a pressure transmission and as a precursor
solvent, so the resulting powder can be amorphous or crystalline. The
advantages of the hydrothermal method include being able to produce crystalline
products that can be achieved at low enough temperatures with a high degree of crystallity, can reduce agglomeration between particles, can
produce a relatively uniform particle size distribution, high product purity,
relatively cheaper, directly formed powder from solution, shape and particle
sizes can be controlled from the initial material and different hydrothermal
conditions, The reactivity of the
resulting powder is high, and allows the synthesis of compounds that have
oxidation numbers that are difficult to obtain, especially transition groups
In addition,
hydrothermal also has a drawback, that is, the initial solubility must be known,
hydrothermal slurry is corrosive, and the use of high-pressure vessels will be
dangerous in case of accidents
Figure 4. The process of synthesis of hydrothermal methods
with various precursors
Good
crystals can be obtained by adding a mineralizer. Mineralizer serves to
increase the polarity of water to increase the solubility of a dissolved
substance. Compounds used as mineralizers should not be seen in reactions, and
commonly used compounds are alkaline bases, NaOH, and KOH
Table 5.
Comparison of research results using hydrothermal methods
|
Hydrothermal Variations |
Particle Size and Shape |
Physical, Mechanical, and
Chemical Characteristics |
Influence of Process
Parameters |
Ref. |
|
Anionic, cationic, and nonionic surfactants. Temperature 180oC. |
Spherical particle shapes with a diameter ranging from 15-205
nm. |
Single-domain magnetic behavior, coercivity of 225 Oe, high stability, and thermal conductivity of 0.4787 W/mK. |
The type and concentration of surfactants can affect the
colloidal stability and thermal stability of nanoparticle suspensions. |
(Kongsat et al., 2021) |
|
PVP surfactants and NaAc precipitants.
Temperature 200oC. |
The average particle size is 40 nm with a spherical shape. |
The highest capacitance is 340.5 F/g at a current density of 1
A/g, remanent magnetization is 0.02 emu/g, coercivity is 66.8 Oe, and a long cycle life. |
The concentration of the precursor affects the quality of the
size and dispersion of the resulting hematite |
(M. Zhu et al., 2012) |
|
Fe sulfate heptahydrate solution Fe2 (SO4)3.7H2O Temperature 160oC. |
Spherical in shape, and the average size is 8 nm. |
It is superparamagnetic with blocking temperature T B = 52 K and
irreversibility temperature T irr = 103 K.
Magnetization Ms = 3.98 emu/g and magnetic moment mp = 657 B. |
The magnetization properties of hematite nanoparticles are
influenced by the crystallinity and surface of the nanoparticles. |
(Tadic et al., 2014) |
|
Fe (III) nitrate solution. Temperature 100oC. |
The average particle size is 20-60 nm. |
A low pH produces a positive potential value, while a pH of 7
produces a negative value |
The size of the synthesized particles increases with the
reaction time. Particle size affects colloidal behavior to absorption and
aggregation processes. |
(Colombo et al., 2015) |
|
Hierarchical nanostructures with various glycine-free and
glycine-assisted morphologies. |
The diameter of the particles is on average 20-80 nm, spherical
in shape. |
Ferromagnetic, coercivity Hc
= 3725 Oe. |
Glycine in hydrothermal reactions can increase the coercivity
value up to 3 times. |
(Trpkov et al., 2018) |
|
Precursors of iron and sodium acetate. Temperature 180oC. |
The size of 50 nm irregular nanoparticles, such as plates with a
thickness of 10 nm and a diameter of 50-80 nm, a 3D ellipsoid with a length
of 3.5 nm and a diameter of 1.5 m |
Coerciveness of irregular nanoparticles Hc
= 73 Oe, nanoplates Hc =
689 Oe, and 3D ellipsoid Hc
= 2688 Oe. Indicates a low level of cytotoxicity. |
The anisotropic form influences the increase in coercivity in
hematite nanoplates, their structure and morphology. |
(Tadic, Trpkov, et al., 2019) |
Sonication
The
sonication method is the easiest and most effective method for large-scale
production with precise size control, high morphology, and crystallinity. In
research using ultrasonic sonochemical methods
obtained polyhedron monodispersa hematite
nanoparticles with uniform shape, particle size of about 14nm at a temperature
of 500oC
Figure 5. Synthesis process sonication method
Applications of Hematite
(α-Fe2O3) Nanoparticles
Hematite nanoparticles (α-Fe2O3) have potential applications
in various fields of advanced nanotechnology, such as electronics, optical
devices, photonics, and microwave absorbers. Much research has focused on
hematite nanoparticles (α-Fe2O3) both undoped and doped as solar
photoelectrochemical cell (PEC) materials
Hematite nanoparticles (α-Fe2O3) are
also suitable for photocatalytic applications because they are environmentally
friendly, cost-effective, and have chemical stability over a wide pH range. The
size of the diameter and porosity of the hematite nanorod
Hematite nanoparticles (α-Fe2O3) can also be applied as
microwave absorbers on aircraft walls. By utilizing the potential of natural
sand in East Java, a prototype of a microwave absorbing coating based on Mhexaferite BaFe12-xZnxO19 has been successfully made, by
making it a coating for paint composite materials on the interior walls of the
aircraft. The use of hematite nanoparticles as microwave absorbers is also
supported by the results of research conducted by Rianna
et al using natural iron sand
Barium hex ferrite is an ideal material to dampen
electromagnetic interference (EMI) caused by malfunctions in electronic
equipment. One of the ingredients for making Barium hexaferrite is hematite
(α-Fe2O3)
Hematite nanoparticles as water and sewage treatment have
been reported in research by Kefeni et al. Based on
the research that has been done, hematite nanoparticles have succeeded in
removing Al, Mg, Mn, Zn, Ni, Ca, and Na metals. The adsorption and
precipitation properties possessed by hematite can help in the process of
cleaning water from heavy metals and other solutes. This is also reinforced by
the findings of Aal et al which show that hematite nanoparticles can absorb Cu,
Ni, Co, Cd, and Pb ions
In the medical field, hematite nanoparticles also show no
less unique abilities, one of which is their use as a delivery drug. Hematite
nanoparticles can be coated with drug compounds to be then directed to specific
locations in the body using external magnetic fields. External magnetic fields
can also generate heat through magnetic hysteresis in magnetic hyperthermia
therapy to damage cancer cells. In addition, the unique magnetic properties that
hematite nanoparticles possess can help in medical imaging techniques such as
magnetic resonance (MRI) by increasing image contrast
Figure 6. Applications and methods of synthesis of hematite
nanoparticles
CONCLUSION
Based on the literature that has been described, it can be
concluded that iron sand can be further utilized in producing a variety of
minerals, especially hematite. The characteristics of iron sand used can be
influenced by the location where iron sand is found. In addition, the synthesis
method plays an important role in determining the physical, mechanical, and
chemical properties of hematite nanoparticles from iron sand. The structure of
hematite nanoparticles, especially at the level of crystallinity and surface
morphology has an impact on the performance and application of hematite
nanoparticles. Hematite nanoparticles have demonstrated their capabilities in a
wide range of applications, including water and environmental treatment,
catalysts, and energy storage.
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