Authors Accepted Manuscript

A review of the magnetic properties, synthesis

methods and applications of Maghemite

H. Shokrollahi

www.elsevier.com/locate/jmmm

PII: S0304-8853(16)31339-7
DOI: http://dx.doi.org/10.1016/j.jmmm.2016.11.033
Reference: MAGMA62107
To appear in: Journal of Magnetism and Magnetic Materials
Received date: 5 July 2016
Revised date: 24 October 2016
Accepted date: 4 November 2016
Cite this article as: H. Shokrollahi, A review of the magnetic properties, synthesis
methods and applications of Maghemite, Journal of Magnetism and Magnetic
Materials, http://dx.doi.org/10.1016/j.jmmm.2016.11.033
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 A review of the magnetic properties, synthesis methods and applications of Maghemite

H. Shokrollahi

Electroceramics Group, Materials Science and Engineering Department, Shiraz University of

Technology, Shiraz, Iran

Tel/Fax: 0098-713-7270047, Email: shokrollahi@sutech.ac.ir

Abstract

It must be pointed out that maghemite Fe2O3 with a cubic spinel structure is a crucial

material for various applications, including spin electronic devices, high-density magnetic

recording, nano-medicines and biosensors. This paper has to do with a review study on the

synthesis methods, magnetic properties and application of maghemite in the form of one-

dimensional (1D) nanostructured materials, such as nanoparticles, nanotubes, nano-rods, and

nanowires, as well as two-dimensional (2D) thin films. The results revealed that maghemite is

widely used in the biomedical applications (hyperthermia, magnetic resonance imaging and drug

delivery) and magnetic recording devices. The unmodified and Co/Mn modified maghemite thin

films prepared by the dc-reactive magnetron sputtering show the excellent values of coercivity

2100 Oe and 3900 Oe, respectively, for the magnetic storage application. The super-

paramagnetic particles with 7 nm size and the saturation magnetization of 80 emu/g prepared by

the established thermolysis method are good candidates for bio-medical applications.

Keywords: Maghemite, Spinel, Thin film, Nanoparticle,

1. Introduction

1
It is noteworthy that among different types of magnetic materials, magnetic ceramics have

various advantages, as compared to metallic and alloy magnetic materials, including high

electrical resistivity, ease of synthesis, as well as resistance to corrosion and wear [1, 2]. Among

magnetic ceramics, iron oxide has been utilized in various fields and applications as it can exist

in several phases such as magnetite, hematite and maghemite Fe2O3 . Magnetite and

maghemite are two main classes of iron oxide with interesting magnetic properties which are

good candidate for various applications, including magnetic recording devices, high-frequency

switch modes, electromagnetic absorbers and especially biomedical applications [3-10].

Recently, the nanostructured iron oxides in the form of nanoparticles, nanorods, nanotubes, and

thin films have received special attention among researchers in different areas. To the best of my

knowledge, there is no review paper on the structural, magnetic and synthesis methods, as well

as applications of maghemite, as compared to magnetite. For this reason, this paper attempts to

present an overview of the synthesis methods, structural studies and magnetic properties of

maghemite, especially for data recording and biomedicine applications.

The basic distinguishable properties of iron oxide phases are particular magnetic behavior,

originating from the vacancies and valance states of iron in sub-lattices. Magnetite (Fe3O4), the

most magnetic naturally occurring mineral on Earth, is a soft ferrimagnetic material with small

magnetic anisotropy at room temperature. It has the highest saturation magnetization at room

temperature (84 emu/g) among different iron oxides. Fe2O3 is a very common mineral on the

earths surface with a soft ferrimagnetic property at room temperature and a Curie temperature of

928 K. Like magnetite, it exhibits the cubic spinel structure with small magnetic anisotropy due

to no orbital angular momentum. Unlike magnetite, which is a semiconductor, the maghemite is

expected to be an insulator [2]. From the viewpoint of the magnetism, the super-exchange

2
interactions between magnetic ions in the tetrahedral and octahedral sites result in a

ferrimagnetic ordering in magnetite and maghemite.

Magnetite and maghemite are utilized in magnetic recording devices, whereas hematite is the

most stable state of all and is commonly used in the sensor application [11, 12].Both maghemite

and magnetite exhibit a spinel crystal structure, whereas the latter contains both Fe2+ and Fe3+

cations. In maghemite all the iron cations are in the trivalent state, and the charge neutrality of

the cell is guaranteed by the presence of the cation vacancies [13].

The name, maghemite, was first proposed in 1927. It is a combination of the first syllables of

magnetite, which has the same structure, and hematite, which has the same composition.

Maghemite is a member of the family of iron oxides. It has the same spinel ferrite structure as

magnetite and is also ferrimagnetic. Maghemite has relatively high magnetization, octahedral

vacancies, and bio-compatibility [14]. The octahedral vacancies are the suitable position for the

accepting of certain cations which have the strong tendency toward the octahedral site (Ni2+,

Gd3+, Mg2+) [15].

The Fe2O3 polymorphic nature has been known for a long time. Fe2O3 is the second

polymorph that occurs in nature like the mineral maghemite. Fe2O3 is an inverse spinel with

a cubic unit cell (a) 8.351 (Fig. 1a). Like Fe3O4, it contains cations in the tetrahedral A and

octahedral B positions, yet there are vacancies (), usually in octahedral positions, to compensate

for the increased positive charge (Fig. 1b).When the vacancies are randomly distributed, the

space group is Fd3m . Stoichiometry can be formally described by the formula

FeA Fe5 3
B
13 O4 [16, 17]. Fe2O3 is considered as a defective spinel 13 Fe833O4 , which

represents vacancies on the cation sites.

2. Magnetic Properties

3
Admittedly, maghemite Fe2O3 is the second most stable polymorphofiron oxide. Unlike

antiferromagnetic hematite Fe2O3 , maghemite exhibits ferrimagnetic ordering with a net

magnetic moment (2.5 B /unit formula) and high Curie temperature (950 K), and due to its

chemical stability and low cost has led to its wide application as a magnetic pigment in the

electronic recording media [4] since the late1940s. Based on the materials preparation and purity,

the saturation magnetization ( MS ) and coercivity ( H C ) of bulk maghemite are 74-80 emu/g and

HC 50 800 G at room temperature, respectively. Its MS is lower than that of the magnetite (92

emu/g) and is higher than that of the hematite (0.1-0.4 emu/g), whereas its coercivity is the same

as that of the magnetite (50-800G) and lower than that of the hematite (1000-5000G). Fe2O3

is one of the first and experimentally most researched materials for the purpose of building the

super-paramagnetic theory. The ultrafine particles of maghemite like hematite show super-

paramagnetism [1].

Yoon et al. synthesized the maghemite nanoparticles with 13.9 nm with the super-paramagnetic

behavior at 300 K. The saturation magnetization was 68 emu/g, which was slightly smaller than

that for the bulk material (74 emu/g)[18]. Dutta and his co-workers presented the nearly

spherical particles of Fe2O3 of 7 nm in diameter. The MS 80 emu/g in these nanoparticles is

equal to the bulk value with negligible coercivity and no exchange bias is below the blocking

temperature ( TB 100 K ). This suggests that these nanoparticles are near perfect crystals without

any significant disorder [19]. Guivar and his collogues investigated the super-paramagnetic

particles with average sizes of 5.7 nm by use of the magnetite precursor of ferric chloride and

ferrous chloride[20]. The precursors were fully oxidized by adjusting the pH =3.5 at about 80 C

in an acid medium. Figure 2 shows the Mossbauer spectroscopy at room temperature (RT) and

4
77 K of the nano-metric Fe2O3 sample, revealing the intermediate super-paramagnetic

relaxation effect. At RT, the fitting was carried out using one distribution of hyperfine fields and

one doublet representing the super-paramagnetic particles. At 77 K, the spectrum was adjusted

by using one distribution of the hyperfine fields of Fe3+. This shows five peaks whose centers

were calculated through five Gaussian curves obtaining 51.3, 48.6, 43.2, 23.4 and 17.1 T,

respectively. In the Mssbauer spectra the TB can be obtained when the area of the distribution is

50% of the super-paramagnetic area. Hence, at 77 K the total area of the two principal peaks

gives 71.4 % assumed to maghemite without relaxation, and the remaining peaks give 28.6%;

then the TB is nearly 100 K [20]. Can et al. investigated the magnetic behavior of the single

domain size of Fe3O4 , Fe2O3 and Fe2O3 nanoparticles by considering the intra-particle

interactions. The magnetic formations in both sites, tetrahedral and octahedral symmetries, of the

Fe3O4 nano-particles were constructed from the nonequivalent and different cations. However,

for Fe2O3 and Fe2O3 , the asymmetry or symmetry can be the result of the non-equivalency

of the magnetic moment of the same cations of each sub lattice [21]. Deng found that the Co

content of 6-18 wt% and heat treatment dominates coercivity, while Mn leads to a better heat

treatment response of the media. The low-level Zn doping enhanced the magnetization and

reduced the temperature coefficient of coercivity. Thus, these modified maghemite non-acicular

particulates are also candidates for ultra-high-density recording purposes [15]. Anantharaman

found that the octahedral vacancies are the suitable position for the accepting of certain cations

which have a strong tendency to the octahedral site (Ni2+, Gd3+, Mg2+). The doped maghemite

prepared using acicular ferrous oxalate dihydrate precursors showed higher saturation

magnetization, as compared to the undoped one. 2 at% Mg2+ increases MS from 77 to 100 emu/g

5
and H C from 250 to 269Oe. In addition, 2 at% Ni2+ increases MS from 77 to 83 emu/g and

reduces H C from 250 to 224Oe [15]. Mozaffariet al. substituted Zn2+ into the maghemite by the

co-precipitation method. They showed that the Zn ions up to 0.11 increase the saturation

magnetization of maghemite and make it into super-paramagnetic particles. The Curie

temperature first decreases and then increases. A further increase in the Curie temperature up to

680 C was found for x 0.66 due to the migration of some Zn2+from A to B sites in the spinel

[22]. Regarding the application of the nano-magnetic particles, the major challenge is a reduction

in the saturation magnetization with an increase in the surface to the volume ratio. In this area,

Coey proposed the magnetic core-shell structure[23, 24]. In a deep research done by Kubickova

and his co-workers, they synthesized three maghemite nanoparticles (NPs) by the thermal

decomposition. The well-crystalline NPs are Np7, d XRD ~6.6 nm, d TEM ~6.5 nm (Fig. 3a) and two

samples with the same NPs sizes but different internal structures (Np15a d XRD ~7.2, d TEM ~15 nm

(Fig. 3b); Np15b d XRD ~7.4, d TEM ~14.1 nm (Fig. 3c)). The Np15a sample has the structural core-

shell structure (Fig. 3e) and the Np15b has the stacking faults in the center of the particle (Fig.

3f).

Regarding the well-crystalline NPs (Fig. 3d) there are not any core-shell structures, surface spin

disordering and internal stacking faults. This depicts for the NPs with high crystallinity that the

crystallite size is near the particle size and that the MS is higher than the other samples ( MS ~67.5

emu/g). Also, for the sample with the core shell structure the MS is at the lowest level ( MS ~51

emu/g) [25].

3. Synthesis methods

6
A miscellany of methods such as the co-precipitation, solgel synthesis, micro emulsion, flow

injection synthesis, flame spray pyrolysis, decomposition of organic precursors at high

temperatures, and oxidation of magnetite nano-particles have been reported to prepare

maghemite nano-particles [18]. Maghemite is a metastable phase of ferric oxide at room

temperature and above 450 C , and it is transformed into the stable -phase. Therefore, it can

only be prepared at temperatures below 450 C by the oxidation of magnetite or dehydration of

ferric hydroxides. Due to the low-temperature preparation, the crystallized particles are poorly

formed, and the Fe3+ cations and the vacancies are distributed in a disordered way [26].

The synthesis method remarkably affects the cation distribution, purity, shape and particle sizes

of maghemite and therefore properties and application of this material. Recently, Shokrollahi et

al. have presented various internal parameters, including site preference, enthalpy formation,

entropy and bonding energy on the cation distribution and particle size of spinels [27].

Maghemite tends to be prepared by a variety of methods, such as (a) the oxidation of magnetite

in air and/or oxygen atmosphere, (b) the dehydration of FeOOH and (c) the iron salts in a

solution. Kandori and co-workers [28] have observed a maximum value for the size of

FeOOH particles in the presence of EDTA (Ethylenediaminetetraacetic acid) at low

concentrations. In this case, the mechanism of the chelation of organic ions with metal ions,

which prevents the nucleation, leads to larger particles. It should be mentioned that the

adsorption of these ions on the nuclei produced by hydrolysis inhibits the growth of the nuclei.

Magnetic fluids, with particles smaller than 3 nm, can be produced in the presence of citrate ions

during the crystal growth of Fe2O3 , which are suitable for biomedical applications. Without

citrate, the mean diameter is about 8 nm. For low proportions of citrate (R < 2%) the size

decreases only gradually with R, but for R > 2%, the decrease is rather strong. For R = 3%, the

7
size is about 2 nm. Above 4%, the agglomerates of very fine particles are formed. For the fine

particles, the saturation is difficult to achieve [29]. Among different chemical methods, the co-

precipitation is a simple and low-cost method for the production of maghemite. Recently, Nurdin

et al.have achieved the saturation magnetization value of the maghemite nanoparticles produced

by the chemical co-precipitation of about 32.18 emu/g at room temperature, which is lower than

that of the bulk maghemite (74 emu/g) [30]. The morphology of powders was carried out by

TEM (Fig. 4a). It is clear that the maghemite nanoparticles are almost spherical. The size

distribution of particles has been presented in Fig. 4b. Due to the dipoledipole interaction

between the particles and the agglomeration effect, a few larger particles are found. The

average diameter of the particles is about 9.5 nm. Industrially, maghemite particles are usually

prepared from acicular goethite ( FeOOH ) particles via thermal dehydration to hematite,

followed by the partial reduction of magnetite and reoxidation to maghemite [31].

Woo et al. created a novel and cheap synthetic procedure, which is a combination of the solgel

reaction in reverse micelles and crystallization by reflux for the preparation of hematite and

maghemite nano-rods: the rod-shaped hematite (the ferromagnetic behavior from 5 to 300 K,

HC 53 Oe, Mr 0.28 emu/g at room temperature) (Fig. 5a)and the maghemite nano-rods(Fig.

5b) (the super-paramagnetic behavior with a blocking temperature at around 130 K, a diameter

of 5 nm and lengths of 16 and 17nm, respectively) [32].

Wu and his colleagues developed a simple and inexpensive method for the preparation of stable

and magnetic Fe2O3 short nanotubes (SNTs) [33]. The TEM image of the as-prepared

Fe2O3 SNTs contains fine nanotubes with an average size of 500 nm (Fig. 6b).The starting

materials were prepared by the hydrothermal treatment of iron (III) chloride with sulfate and

8
phosphate additives. Then powders were annealed in a tubular furnace at 300 C under a

continuous hydrogen flow for 5 h. The starting materials ( Fe2O3 ) had MS 0.5 emu/g,

Mr 0.16 emu/g and HC 1030 Oe at RT. The as-synthesized SNTs ( Fe2O3 ) with

MS 27.3 emu/g, M r 6 emu/g and HC 100 Oe were ferromagnetic at RT, which may have

potential applications in biotechnology, biomedicine, and fundamental science (Fig. 6a).This

result indicates that the coercivity of Fe2O3 SNTs mainly originates from the small nano-

crystallines with relatively high shape anisotropy. The different valence states and cation

distribution can express the difference in the magnetic properties [33].

Choiet al. synthesized the ultrafine magnetic particles of maghemite by using the iron precursors

of FeCl3 6H2O and FeCl2 4H2O [34]. Choi and co-workers utilized different ratios of iron/oleic

acid to control the particle size. They obtained the smallest particles of maghemite at a ratio of

1/3. The mean particle size was about 6 nm. The low value of MS 50.3 emu/g, HC 21.8 Oe,

Mr 0.7 emu/g and TB 138 K at RT. The major problem with this method was the broadness of

the particles. For this reason, they could not achieve super-paramagnetic particles (the nonzero

coercivity), indicating that some large ferrimagnetic nanoparticles also exist [35].

Wang et al prepared various nanotubes at 500 C for 2 h without a magnetic field and with a 12

T in the thermal decomposition process [36]. Magnetic fields were applied perpendicularly and

parallel to the anodic aluminum oxide (AAO) membrane plane. They showed that the application

of the magnetic field can promote the transformation of magnetite to maghemite. They revealed

i) the magnetic field can enhance the nucleation rate of magnetic materials, ii) the Curie

temperature for Fe2O3 is 590 C ( at 500 C ), therefore G M is negative and the total

free energy ( G T G M ) is reduced because of the external magnetic field,iii) Fe2O3 is

9
formed at 500 C due to the thermal decomposition of Fe NO3 3 and then Fe2O3 is

transformed into Fe2O3 in the presence of a high magnetic field. The results showed that

when the magnetic field is perpendicular to the membrane plane, the MS (46.1 emu/g), M r (2.35

emu/g) and H C (28 Oe) are higher than the others at room temperatures [36]. Drofeniket al.

successfully synthesized maghemite nano-sheets from the FeO OH precursor with a high

tendency to form the 2D morphology particles. At elevated temperatures, the FeO OH

particles can be transformed by the thermal dehydroxilation to the spinel maghemite [37].

The mono-dispersed maghemite nanoparticles of uniform size (102 nm) with a fast and

economical chemical procedure can be easily synthesized in a short reaction time (30 min) and at

such low temperatures as 130 C by the thermal decomposition of iron pentacarbonyl with

dimethylsulfoxide (DMSO) serving as the oxidizing agent and oleic acid as the surfactant to

maintain a narrow size distribution [38]. Maghemite thin films are widely used in the magnetic

recording due to the fact that they are easy to erase and rewrite with high storage, less access

time and that they are relatively inexpensive. They have a greater available signal-to-noise ratio

than the particulate media. Nowadays, for high-capacity hard disks, the coercivity of the thin

film maghemite with high corrosion resistance must be 1200 Oe in spite of the metallic alloys

Co-Ni-Cr, Co-Cr-Ta, which lack the corrosion resistance [39].

A great number of investigators have attempted to prepare maghemite and magnetite thin films

for data recording by different methods but their coercivity is smaller than 800 Oe. The methods

include reactive deposition [40], reactive sputtering [41-44], spray-pyrolysis by ultrasonic-pump

[45] and spray-spin-coating [46]. Spry-pyrolysis is one of the most important methods to produce

the films with high coercivity. Chang et al. synthesized maghemite films, 3 m in thickness, by

10
the spray-pyrolysis of nitrates onto the heated substrates of polycrystalline alumina, magnesium

oxide (MgO (100) and glass with different Co and Mn contents [39]. They achieved the highest

value of coercivity (1300 Oe), Ms= 5000 G and squareness of 0.61 with the composition of 12

wt% Co and 14.4 wt% Mn on alumina after annealing. The coercivity was found to arise from

the single domain particles of 50 nm. The obtained thin films are appropriate for magnetic

recording applications. In most cases, super-paramagnetic maghemite particles are synthesized

by wet chemical methods. Vollathet al. presented the microwave plasma process (0.915 GHz)of

nano-crystalline maghemite Fe2O3 using chloride ( FeCl3 ) or carbonyl ( Fe3 CO 12 ) as the

precursor with the super-paramagnetic behavior and particle sizes between 5-10 nm [47]. A

microwave plasma enhances the kinetics of chemical reactions at low temperature as a result of

the promotion of the interaction of the charged particles, including electrons, ions, or radicals in

the plasma with the uncharged species. The obtained small magnetization, as compared to

theoretical values and various chemical methods, is caused by the lattice disorder, leading to the

nonstandard distribution of the Fe3+ ions to the octahedron and tetrahedron sites. Prado and his

co-workers increased the magnetic anisotropy of maghemite nanoparticles by increasing the

surface anisotropy from the magnetic interaction of the complexes with the particles [48]. They

synthesized 5 nm Fe2O3 nanoparticles with the [ CoII TPMA C12 ] complex (TPMA: tris(2-

pyridylmethyl)amine) with the coercivity of 839 Oe, as compared to 62 Oe, which is 13 times.

The observed effect necessarily results from the magnetic interaction of the complexes with the

particles, leading to an increase in the magnetic anisotropy. The strong influence of the

molecular component on the nanoparticle comes from the covalent linking of the two species

through the oxo-bridges and the resulting magnetic interaction. The obtained nanoparticles are

suitable for magnetic recording and some medical applications. The high-quality pure maghemite

11
with an average particle size of 19 nm was prepared by a simple solgel self-combustion process

and achieved only with a gel pH value of 7 and with a primer temperature between 290 and 325

C( H C =280G, MS =78 emu/g). This shows that a perfect collinear structure is present in the

particles, as confirmed by the ratio MS MS (bulk) 0.95 ( MS (bulk) = 82emu/g) [49]. The sol-gel

method as a simple and economical way has been chosen to synthesize the high-quality

maghemite thin film. The Iron (III) nitrate nonahydrate has been used as a precursor with

different molarities. The largest value of coercivity (482.32 Oe) with an average crystallite size

of 13.3 nm due to the domain behavior makes maghemite a suitable candidate in the high-density

magnetic recording [50]. The maghemite nanoparticles were synthesized by a new synthetic

route using triethylamine as a co-precipitation agent in the presence of the organic ligand LCH3 .

This method indicates that the nanoparticles have a mean diameter of 3.9 nm by TEM and a

narrow size distribution. The saturation magnetization and the anisotropy constant were about

17emu/g at 3 K, and K 2.6 105 erg/cm3 [51].Horner synthesized the maghemite nanoparticles

with co-precipitation followed by the hydrothermal process. The hydrothermal method leads to

the formation of large particles10110 nm with good mono-dispersity [52].

Industrially, maghemite particles tend to be prepared at 2 steps. At the first step, magnetite is

synthesized by the chemical co-precipitation of ferric and ferrous ions in an alkali solution, and

at the second step magnetite is oxidized by aeration at 200400 C . Darezereshki developed a

simple-single step method to prepare Fe2O3 nano-particles with an average size of 10 nm. In

this method the organic solvents and heat treatment are not required. Pure maghemite can be

prepared without hematite and magnetite impurities [53]. The usual technique for maghemite

requires 2 steps. At first the magnetite nanoparticles are synthesized by co-precipitation in the

alkaline solution of ferrous and ferric cations. Then these particles are oxidized in air between

12
100 and 250 C . Recently, Janotet al. have synthesized the maghemite nanoparticles of about 15

nm by the one-step ball-milling of the iron powder in water ( 2Fe 3H2O Fe2O3 3H2 ) with

good crystallinity and Fe2+ content below 1% [54].

4. Application

It must be stated that some applications of maghemite, especially in the form of super-

paramagnetic nanoparticles are in ferro-fluids, high density magnetic storage, high-frequency

electronics, high-performance permanent magnets, magnetic refrigerants, magnetic resonance

imaging (MRI) contrast enhancement [14, 55], bio-magnetic separations, hyperthermia treatment

or magnetic drug targeting [56]. Among various applications, maghemite is widely used in

medicine and data storage. Recently, maghemite nanoparticles have been used to clean up the

Cr(VI)[57], As (V) [58] and Mo (VI) [59] contamination from waters.

Aliahmad et al. developed a modified co-precipitation synthesis of the divalent/trivalent iron

salts using aqueous ammonium hydroxide ( NH3 H2O ) to produce super-paramagnetic Fe3O4

and Fe2O3 nanoparticles. The size control and size distribution are a great challenge in nano-

medicine. Due to the good size distribution and size control, Fe2O3 with the average size of

22 nm has been reported to be applicable as a material for use in drug delivery systems (DDS),

magnetic resonance imaging (MRI), and cancer therapy [60]. Tietze obtained similar results in

the study of the drug delivery application of the maghemite super-paramagnetic nanoparticles

[61]. In this area, Bandhu et al. prepared the maghemite nanoparticles ( Fe2O3 ) by the co-

precipitation method. To obtain the bio-functionalized magnetic nanoparticles for magnetically

controlled drug delivery, the prepared nanoparticles are successfully coated with the pepsin, bio-

compatible polymer and digestive enzyme [62].

13
Numerous researchers have obtained the smaller particle sizes which are also suitable for

biomedical applications. Mzquiz-Ramos et al. successfully synthesized the super-paramagnetic

maghemite nanoparticles with a mean diameter of 10 nm by the chemical co-precipitation

followed by heat treatment. The obtained particles are good candidates for cancer treatment by

magnetic hyperthermia at 362 kHz and 0.2 kAm-1 up to 49 C [63]. Maghemite nanoparticles

covalently coated with polyethylene glycol have been investigated by Hergtaet al. The extremely

high values of the specific loss power in the order of the 600 W/g result for 400 kHz and 11

kA/m make it possible for hyperthermia [64]. Maghemite nanoparticles due to high saturation

magnetization and biocompatibility are good candidates for hyperthermia treatment. Pure and

highly crystalline Fe2O3 nano-crystals (NCs) (6 nm) in the aqueous solutions of poly (vinyl

pyrrolidone), such as pristine NCs form the aggregates of about 150 nm. These particles exhibit a

high transversal relaxivity ( r2 466 mM1s1 ) about four times higher than that of the

commercial Feridex magnetic resonance imaging (MRI) contrast agent. The important result of

this is a reduction in the MRI measurements [65].

The Fe2O3 nanoparticles (5 nm) synthesized by the continuous laser pyrolysis of Fe CO 5

vapors were prepared. The laser pyrolysis technique seems to be a good alternative to the co-

precipitation method for producing the MRI contrast agents [66]. A novel method has been

described by Chen et al for the preparation of super-paramagnetic mesoporousmaghemite

Fe2O3 /silica ( SiO2 ) composite microspheres to allow for the rapid magnetic separation of
DNA from the biological samples [67]. Maghemite nanoparticles are also used in the magneto-

rheological fluids as a magneto-mechanical sensor. Maghemite nanoparticles with an average

size of 10.6 nm in the form of maghemite-Kerosene Ferro-fluid are used as magneto-rheological

fluids [68]. In the application of the maghemite nanoparticles, the surface stabilization is very

14
important. Desautels and his collogues discovered an interfacial monolayer of CuO in the Cu-

coated- Fe2O3 nanoparticles, which stabilized the disordered surface spins of the maghemite

nanoparticles [69]. In other investigations Albornoz et al. developed a matrix containing

maghemite with polyvinyl alcohol (PVA). In other words, to control the stabilization and the

performance of nano-metric maghemite particles, the nanoparticles are dispersed in a polymeric,

glassy or ceramic matrix. In some cases the surface modification follows specific purposes [70].

Cappelletti et al. presented the surface modified maghemite nanoparticles with a thermo-

sensitive organic shell of poly (N-isopropylacrylamide) (PNIPAm). The thermally responsive

polymers can collapse or expand on heating [71]. Nowadays, the magneto-optic sensors are

being produced widely from maghemite. Recently, the maghemitesilica gel nano-composites

with a suitable magneto-optical response for the magnetic field sensing applications have been

prepared. The magnetic and magneto-optical responses correlate well for those samples with a

maghemite conversion higher than 50%, reaching a Verdet constant of 950 rad T 1 m1 and a

specific Faraday rotation at 0.12 T of 19 rad m1 for the 72% conversion yield [72].

The Fe2O3 SiO2 nano-composite aerogels, which are light, porous and transparent and

magnetic materials, are synthesized. The composite, with 10.4wt% of iron oxide, has a specific

Faraday rotation of 29.61/cm at 0.6 T and is used in optical fiber sensors, optical isolators and

magnetic data storage [73]. Fe2O3 has been widely used in audio recording as a magnetic

recording material [74]. About 90% of the audio/video and computer diskettes use needle-shaped

maghemite in the particulate or thin films. This material has a suitable hysteresis loop with a

good combination of saturation magnetization, coercivity and squareness. The single domain

acicular shape is required to optimize the coercivity and better alignments of particles for

recording. Also, it is used as a potential catalyst in petrochemical industry. The Polymer nano-

15
composites containing maghemite exhibit super-paramagnetism and are potential materials for

magnetic refrigeration.

A crucial property for magnetic recording application is the coercivity. This property can be

increased by the shape anisotropy through the acicular particle forms and/or magneto-crystalline

anisotropy through the nonzero angular momentum ion doping like Co2+ doping and/or surface

anisotropy via the absorption of Co2+ in the surface of the particles [26].

In has been indicated that the coercivity of maghemite thin films increases noticeably about 1-4

times, making it suitable for recording materials [75]. The coercivity of the previously studied

undoped Fe2O3 thin films which have been studied is only 200 to 800 Oe. Obviously, it is too

low to meet the future demand for high-density recording. The coercivity of the thin films can be

increased from 1000 to 2100 Oe by being doped with some modifiers like Co, Ti, Os to enhance

the magneto-crystalline anisotropy. Present authors have reported that the Co/Mn modified

Fe2O3 thin films prepared by the dc-reactive magnetron sputtering are found to have the

coercivity of up to 3900 Oe. In this area, Chang and et al. synthesized the undoped thin

Fe2O3 films on the Si substrate under the well-controlled O 2 partial pressure by the dc-

reactive magnetron sputtering Fe3O4 phase for 10 minutes at 360 C . The coercivity was

increased 1-4 times to 640 - 2100 Oe. The residual stress was due to the mismatch in the thermal

expansion coefficient between films and Si substrate [75]. Table 1lists some important magnetic

nanoparticles, including the nano-sphere, nanotube and nanowire, as well as the thin films

produced by different methods.

5. Conclusion

16
It has been concluded that maghemite is widely used in the biomedical applications and magnetic

recording devices. The super-paramagnetic behavior with relatively high saturation

magnetization for biomaterial applications has been achieved by the co-precipitation,

hydrothermal, spray-pyrolysis, sol-gel, thermal decomposition and established thermolysis

methods. The highest value of saturation magnetization has been achieved by the established

thermolysis procedure. In addition, thin films, nanotubes and nanowires with suitable coercivity

can be used for data storage applications. The results showed that the Co/Mn-doped maghemite

thin films produced by the dc-reactive magnetron sputtering have the highest value of coercivity

(3900 Oe). Furthermore, the results demonstrated that the saturation magnetization is less than

the theoretical value due to the spin surface effects and lattice disordering (the nonstandard

distribution of the Fe3+ ions to octahedron and tetrahedron sites).

Acknowledgment

The author wishes to thank Shiraz University of Technology.

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Figure 1.(a) The crystal packing in the structure of Fe2O3 , the view onto (100). (b)The

schematic representation of the nonequivalent sites of Fe in the structure of Fe2O3

[reproduced with permission from ref. 17].

22
Fig. 2. The Mssbauer spectra of the maghemite nanoparticles at RT and 77 K [reproduced with

permission from ref. 20].

Fig. 3. The upper row:the HR-TEM images of the samples, a) Np7 with d XRD ~6.6, d TEM ~6.5 nm;

b) Np15a with d XRD ~7.2, d TEM ~15 nm; c) Np15a with d XRD ~7.2, d TEM ~15 nm. The bottom row:

different internal structures of particles, d) without surface disordering and stacking fault, e) with

surface disordering, f) with internal stacking faults [reproduced with permission from ref. 25].

Fig. 4. a) The TEM images of the maghemite nanoparticles, b) Dynamic light scattering or

hydrodynamic size [reproduced with permission from ref. 30].

Fig. 5. The TEM images of (a) hematite, and (b) maghemitenano-rods [reproduced with

permission from ref. 32].

Fig. 6. TEM image and magnetic hysteresis loops at T = 300 K for the starting materials and as-

prepared Fe2O3 SNTs [reproduced with permission from ref. 33].

Table. 1. Saturation magnetization (emu/g) and coercivity (Oe) at room temperature for sphere

diameter (nm), tube length, rod section and film thickness obtained by different methods.

Synthesis method Shape Hc Ms Ref.

Co-precipitation Spherical - 68 13.9 [10]

Established Spherical ~0 80 7
[11]
thermolysis procedure

Co-precipitation Spherical ~0 5.7 [12]

Co-precipitation Spherical - 32.18 15-20 [22]

23
Thermal decomposition Spherical - 67.5 6.5 [17]

Sol-gel reaction in reverse Nano-rod ~0 - 5 17

[24]
micelles

Hydrothermal Short nano-tube 100 27.3 400-500 [25]

Co-precipitation spherical 21.8 50.3 6 [27]

Thermal Nano-tube 28 46.1 2d

[28]
decomposition

Spray-pyrolysis Thick Film 1300 5000a 3e [31]

Chemical reaction in Spherical 839 - 5

[40]
microwave plasma

Solgel self-combustion Spherical 280 78 19 [41]

Sol-gel Thin film 482.32 - 13.3 [42]

Co-precipitation Spherical - 17b 3.9 [43]

DC-reactive magnetron Thin film 2100 230c - [67]

sputtering

DC-reactive magnetron Thin film 3900 - - [67]

sputtering

a) G, b) at 3 K, c) emu/cm3, d) m, e) m

Highlights

Among iron oxides, maghemite is one of the most important magnetic ceramics
Maghemite is widely sued in magnetic recording and biomedicine
This paper attempts to give an overview on the some important areas
They contain synthetic methods, magnetic study, structural study and applications

24
a b

Fig. 1

25
Fig. 2

26
Fig. 3

27
Fig. 4

28
Fig. 5

29
Fig. 6

30