Front. Mater. Sci.

2012, 6(2): 128141

DOI 10.1007/s11706-012-0167-3

REVIEW ARTICLE

Solgel auto-combustion synthesis of spinel-type

ferrite nanomaterials

Andris SUTKA and Gundars MEZINSKIS ()

Department of Silicate, High Temperature and Inorganic Nanomaterials Technology, Institute of Silicate Materials,
Riga Technical University, 14/24 Azenes Str., Riga, LV-1048, Latvia

Higher Education Press and Springer-Verlag Berlin Heidelberg 2012

ABSTRACT: Recent developments and trends of solgel auto-combustion method for

spinel ferrite nanomaterial synthesis are briey discussed and critically analyzed. The
analysis of various parameters of reaction which could be used for better understanding
of synthesis process and control of microstructure and property of spinel ferrite
nanopowder products was the main objective of this review article. Special attention was
paid to variety of particle size and phase purity. For these purposes the correlation
between complexant, oxygen balance and combustion process chemical additives, as
well as heating mechanism and atmosphere, was established. These results are relevant
from standpoints of both application and processing of ferrites.

KEYWORDS: ferrite, synthesis, solgel, auto-combustion, nanomaterial

Outline 1 Introduction

1 Introduction The spinel ferrites are unique materials exhibiting

2 The solgel auto-combustion process for spinel ferrite ferrimagnetic and semiconductor properties and can be
synthesis considered as magnetic semiconductors [1]. These materi-
2.1 The inuence of complexant/fuel agents als has been extensively used in several applications
2.2 Oxygen balance including recording heads, antenna rods, loading coils,
2.3 Combustion process chemical additives to facilate microwave devices, core material for power transformers
the auto-combustion reaction in electronics and telecommunication applications [24].
2.4 The inuence of atmosphere Nanosized ferrites may have extraordinary electric and
2.5 Heating mechanism magnetic properties that are comparatively different from
3 The new approach for the synthesis of 1D structures microstructured materials, tailoring them to modern
4 Conclusions technologies, as well as providing novel applications
Acknowledgements such as ferrouids [4], magnetic drug delivery [5], high
References density information storage [6], photocatalysis [7], gas
sensors [8], etc.
The spinel ferrite structure (Fig. 1) can be described as
cubic close packed arrangement of oxygen atoms in which
32 oxygen ions forms a unit cell. Layers of oxygen ions
Received February 28, 2012; accepted April 12, 2012 contain 64 tetrahedral (A) sites and 32 octahedral (B) sites.
E-mail: gundarsm@ktf.rtu.lv To provide electrical neutrality of the lattice the 8
 Andris SUTKA et al. Solgel auto-combustion synthesis of spinel-type ferrite nanomaterials 129

has shown great potential in the preparation of spinel type

ferrite nanomaterials. Generally, this method can be
considered as solution combustion technique [20]. During
the last decade, the application of the solgel combustion
method for the synthesis of nanosized spinel ferrite
powders has been used in an increasing intensity (Fig. 2).
It has been employed for the synthesis of more than 20
different spinel ferrite compounds MFe2O4, where M could
be Ni, Zn, Co, Cu, Li, Mg, Cd, Mn ion or its combination
[2132]. Recently this method also shows option to
synthesize advanced spinel ferrite one-dimensional (1D)
and two-dimensional (2D) nano-structures [3334].
Obtained products are usable for electronic [35] and
biological applications [36], high density magnetic [37]
and radar absorbing materials [38], and materials for
magnetoelectric composites [39]. These materials also
show gas and humidity sensing behaviour [4041], as well
as catalytic [42] and photocatalytic activity [43].
Fig. 1 Schematic representation of spinel structure.

tetrahedral and 16 octahedral sites are occupied by divalent

or trivalent ions, so unit cell contains eight formula AB2O4
units [9]. Distribution of divalent and trivalent cations
between the tetrahedral and octahedral sites in spinel
ferrites can be expressed with formula (MFe1 )
[M1 Fe1 + ]O4, where M represents a divalent cation and
is the inversion degree [10]. The normal spinel structure
with = 1 has A-sites occupied by divalent cations, while
B-sites by trivalent cations. In the inverse spinel structure
with = 0, divalent cations occupy B-sites, while the
trivalent cations are being distributed among A and B sites. Fig. 2 Number of papers on solgel auto-combustion method to
In a mixed spinel structure with between 1 and 0, both the synthesize nanosized ferrite powders published per year (data
summarized from Scopus database).
tetrahedral and octahedral sublattice sites are occupied by
divalent and trivalent ions [11].
In spite of a large number of papers on spinel ferrite
Studies of spinel structure ferrite nanoparticle synthesis
synthesis by the use of solgel auto-combustion method,
methods have lead to the development of different
no reviews could be found in the literature analysing
chemical synthesis techniques, which have a common
inuence of complexant/fuel agents, oxygen balance,
feature that all reagents are mixed in atomic or molecular
additives to improve the auto-combustion reaction, inu-
level. Most popular methods of bottom-up synthesis
ence of reaction atmosphere, and heating mechanism. In
approach mentioned above are co-precipitation [12], sol
this paper, recent approach for the synthesis of 1D
gel method [13], microemulsion method [14], hydrother-
structures of spinel ferrites is briey summarized.
mal [15], spray pyrolysis [16], reverse micelle [17],
precursor [18], etc. Complex schedules and low production
rate are common problems of these wet-chemical methods 2 The solgel auto-combustion process for
[19]. spinel ferrite synthesis
Solgel auto-combustion synthesis method (also called
low-temperature self-combustion, auto-ignition or self- This method involves exothermic and self-sustaining
propagation, as well as gel-thermal decomposition) where thermally-induced anionic redox reaction of xerogel,
the chemical solgel and combustion process is combined which is obtained from aqueous solution containing
130 Front. Mater. Sci. 2012, 6(2): 128141
desired metal salts (oxidizer) and organic complexant
(reductant) [44]. Combustion reaction of reactant mixtures
Fig. 3 Combustion reaction of reactant mixture. (Reproduced
with permission from Ref. [45], Copyright 2005 Elsevier)
Fig. 4 SEM images of the sample powders after auto-combustion amplied 500, 5000, 8000, and 10000, respectively. (Reproduced with
permission from Ref. [50], Copyright 2006 Elsevier)
is shown in Fig. 3 [45]. Proportions between complexant
and salts are usually calculated according to the valences of
the reacting elements in order to supply the relation of
oxidizer/reductant equal to 1 [46]. The nitrate salts are
favoured as precursors, because they serve as water-soluble
low temperature NO3 oxidant source for synthesis [32].
In some cases, metal nitrates and complexant are directly
mixed together by intensive stirring and heating without
adding water. Metal nitrates possess hygroscopicity;
consequently, they easily absorb moisture and become
slurry. This variety of the solgel auto-combustion is called
ash-combustion method [4748].
Rapid evaluation of a large volume of gases accom-
panying by a great mass loss during the xerogel
combustion leads to the formation of ferrite nanopowders.
Evolution of gases limits the occurrence of agglomeration
[4950]. The scanning electron microscopy (SEM) images
of ferrite nanopowders after auto-combustion are shown in
Fig. 4 [50].
The direct transformation of crystalline ferrite from
 Andris SUTKA et al. Solgel auto-combustion synthesis of spinel-type ferrite nanomaterials
xerogel during combustion is surely due to the heat
generated from the exothermic reaction [51]. Flame
temperature during combustion could vary from 600C to
1350C. The ow chart of the processing steps is illustrated
in Fig. 5, and the schematic diagram of combustion
synthesis device is shown in Fig. 6 [52].
The advantages of solgel auto-combustion include:
good chemical homogeneity (mixing of cations of desired
composition at molecular level); high product purity and
crystallinity; ne particle size and narrow particle size
distribution; it is easy to control stoichiometry; dopants can
be easily introduced into the nal product; simple
equipment and preparation process; low processing time;
low external energy consumption (process initiates at low
temperatures) and multiple steps are not involved [5355].
As we will see in next sub-sections, electromagnetic
properties, as well as particle size and distribution of
obtained ferrite products synthesized by solgel combus-
tion depends on type of organic chelating agent (complex-
ant), complexant to metal salt ratio (oxygen balance), pH
value of solution, ambient atmosphere, heat source and
conditions. Additionally, in some cases chemical additives
such as NH4OH or NH4NO3 are used to modify the nature
of combustion reaction.
2.1 The inuence of complexant/fuel agents
It is important to select appropriate complexant additives
for phase formation by the auto-combustion method.
Complexant agents can effectively chelate metal ions
with varying ionic sizes, which helps in preventing their
selective precipitation to maintain compositional homo-
geneity among the constituents [51]. They also serve as
reductant being oxidized by nitrate ions, thus working as
fuel. Good complexant should react non-violently and
Fig. 5 Flow chart of processing steps.
131
produce nontoxic gases [56]. For example hydrazine is
carcinogenic, thus as complexant is used rarely [49].
All of the complexants differ in the complex ability,
reducing power and the amounts of the gasses that
generate, which obviously affects the properties of the
reaction product (Table 1). Various reaction conditions
inuence defect concentration in the spinel ferrite lattice,
thus could have an impact on charge carrier transport
properties, as well as magnetic domain wall movement.
This is very important for different spinel ferrite applica-
tions.
From literature survey it could be concluded that for
spinel ferrite synthesis various kinds of complexant agents
were used (Table 2). Most popular complexants are urea
(CO(NH2)2), glycine (NH2CH2COOH) and citric acid
(C6H8O7). Complexant agents, which contain carboxylate
groups or amine groups, are essential in the water-soluble
complex precursor synthesis route. Citric acid contains
carboxylate groups, glycine carboxylate and aliphatic
amine groups, while urea contains aliphatic amine groups
[51].
Numerous researches have shown inuence of type of
complexant on obtainable spinel ferrite products [51,57
62]. Hwang et al. investigated relationships on spinel
ferrite properties obtained by solgel auto-combustion by
using glycine, urea and citric acid [52]. It has been found
that from these three precursors, combustion reaction rate
increases in order glycine > urea > citric acid. By using
these three complexants, glycine, urea, and citric acid,
reactions stop at 180C, 280C, and 500C, respectively.
Also, citric acid shows much atter weight loss on TGA
plot. Single phased spinel ferrite was obtained when
glycine was used, but in case of urea and citric acid traces
of impurity phases were detected. Also, by using urea and
citric acid, there is higher carbon content after combustion
132 Front. Mater. Sci. 2012, 6(2): 128141

Table 1 Complexant inuence on obtainable spinel ferrite products

Complexant transferred phenomena Inuence on obtainable products
Complexation ability Stoichiometry of spinel ferrite com-
pounds
Combustion ame temperature Particle size, crystallinity and phase
purity
Amount of gases generated Particle growth, agglomeration and
segregation

Fig. 6 Schematic diagram of the combustion synthesis device: reaction in comparison with glycine. Increase of phase
reactant mixture (A); porcelain crucible (B); thermocouple (C);
hot-plate (D). (Reproduced with permission from Ref. [52], purity and crystallinity is attributed to the generation of
Copyright 2005 Elsevier) larger amount of heat during combustion. In the same time,

Table 2 List of fuels used for spinel ferrite synthesis by solgel auto-combustion
Complexant Structural formula Molecular weight Total valence Decomposition temperature

Citric acid 192.12 + 18 175C

Urea 60.06 +6 135C

Glycine 75.07 +9 262C

Hydrazine 32.05 +4 250C

Ethylene glycol 62.07 + 10 163C

Carbohydrazide 90.08 +8 153C

Alanine 89.09 + 15 314C

Acetic acid 60.05 +8 400C

Acrylic acid 72.06 + 12 440C

 Andris SUTKA et al. Solgel auto-combustion synthesis of spinel-type ferrite nanomaterials
Fig. 7 SEM images showing the morphology of the powder of (a) urea and (b) glycine. (Reproduced with permission from Ref. [60],
Copyright 2010 Elsevier)
faster chemical reaction and higher heat generated tends to
particle growth and agglomeration. Specic area of
products obtained with corresponding complexants
decreases in order urea > citric acid > glycine. The same
contributions were observed in other works, where citric
acid and urea [59], citric acid and glycine [51,61] or urea
and glycine [60] were compared. For example, as shown in
Fig. 7, products synthesized by using urea consist from
agglomerates of primary particles but the powder synthe-
sized with glycine show presence of pre-sintered secondary
particle agglomerates [60].
When comparing combustion heat of these three
complexants, observed relationships become clear. Glycine
combustion heat ( 3.24 kcal/g) is more negative than urea
( 2.98 kcal/g) or citric acid ( 2.76 kcal/g) [63]. Also,
energy released from reaction between ammonia (released
from glycine or urea decomposition) and NOx from the
decomposition of metal nitrates is much higher than that
released from reaction between hydrocarbonaceous frag-
ments and oxygen [52].
However, citric acid is most frequently used in
producing in large variety of ferrites with solgel auto-
combustion method. It is inexpensive and is a more
effective complexing agent than hydrazine and glycine in
producing ne ferrite powder with smaller particle size.
Also, it should be mentioned that the use of citric acid as
complexing agent is often accompanied with the addition
of certain amounts of NH4OH. The use of specic
additives, called drying control chemical additives
(DCCAs), is widely accepted practice preparing solgel
monoliths and coatings. DCCAs help to overcome drying
stresses and contribute to the porosity and strength of the
solgel network. The term combustion process chemical
133
additive (CPCA) seems to be appropriate describing the
modifying nature of NH4OH additive. CPCA inuence on
reaction process and properties of spinel ferrite powder
products obtained with solgel auto-combustion will be
discussed in Section 2.3.
2.2 Oxygen balance
Oxygen balance is ratio between complexant and salts.
According to the principles used in propellant chemistry,
the oxidizing and reducing valences of various elements
are considered as follows: VC = 4; VH = 1; VO = 2; VN = 0,
VM = 2 or 3, etc. Thus total valences of metal salts should
be balanced by total valences in the complexant [64]. For
example, in case of NiFe2O4 when metal nitrates as
Ni(NO3)2, Fe(NO3)3 and citric acid are used, the total
valences are 10, 15 and + 18, respectively. Hence the
stoichiometric composition requires that 40 + 18n = 0 or
n = 2.22 mol of citric acid. For instance, to prepare
NiFe2O4, the reactants Ni(NO3)2, Fe(NO3)3 and citric acid
should be combined in a molar proportion of 122.22
[65]. The total valences for different complexant agents are
shown in Table 2.
In some cases non-stoichiometry between metal and
complexant valences is preferable. Adjustment of the
complexant to metal nitrate ratio allows for control of the
ame time and its effect on the formation and growth of the
phase and on the particle agglomeration states [45].
It was found that with increase excess of complexant in
the gels, the combustion reaction needs oxygen to be
supplied externally, thus reaction rate and temperature is
reduced. Moreover, if increase the amount of complexant,
larger volume of gases is produced, and reaction heat could
134 Front. Mater. Sci. 2012, 6(2): 128141
be carried out to form system by convection. This will
reduce chance of particles to contact, growth and sinter to
each other, which may produce powder with high specic
surface area [46,66]. It should be mentioned that this could
increase fraction of super paramagnetic particles what is
preferable for specic spinel ferrite applications [6768].
In the same time, due to lower reaction rate and
temperature, particles with lower crystallinity and phase
purity will form [69].
For decient complexant content, the heat generated is
not enough due to lack of reductant in the system, and thus
reaction rate and temperature are also reduced, resulting in
the decrease of particle sizes and the increase of specic
surface area [46,70]. In comparison with complexant
excess systems, less amount of carbon content in the
nal product could be observed. From this point of view, it
is more suitable for method modifying when producing of
smaller particles is goal of the work.
2.3 Combustion process chemical additives to facilate the
auto-combustion reaction
In order to improve combustion of the gel different CPCA
such as NH 4 NO 3 [46,52], NH 4 OH [7173] and
C2H4(NH2)2 [50] or combination of different complexants
are used [62,7478]. Appropriate amount of NH4NO3 can
be added to the reactant mixture to compensate loss of
NO3 during dehydration process [52].
CPCA, ammonia (NH4OH), is added when citric acid as
complexant is used. Ammonia increases metal cation
chelating with citrates [71], which could help to control
oxygen balance [71] and develop porous three-dimensional
(3D) network structures in nitrate-citrate xerogels [73].
Added amount of ammonia is controlled by pH value of the
solution. It was found that Fe3+ has achieved complete
complexation with citrates only when pH value is
approached above 3 [71]. From that one could conclude
that without ammonia, citric acid works only as a fuel. Poor
chelation of metal ions with citrates could lead to the
imperfect 3D net-structured gel and therefore the oxidant
nitrate involved in the xerogel is easily decomposed both
during drying and auto-combustion processes. This will
decrease amount of the heat generated due to lack of
oxidant, thus delaying formation of desired ferrite
compounds [71]. Optimal pH value equal to 6 for spinel
ferrite formation was found by Waqas et al [72]. It was
observed that with increasing pH to 6, decomposition of
citric acid containing xerogels occurs at 220C in single
step and results in monophasic spinel ferrite formation.
As we remember from Section 2.1, decomposition of
citrate-nitrate xerogels without ammonia completely pro-
ceeds only at 500C. Nitrate-citrate xerogels without
ammonia have been ignited in the localized manner and
resulted in formation of amorphous powder. Xerogels
obtained from solutions with pH > 7 prevented the process
of spontaneous ignition therefore partially crystalline
powders were obtained [72]. However, in most investiga-
tions for spinel ferrite synthesis from nitrate-citrate gels,
pH equal to 7 was chosen. Yue et al. found that when the
pH value was higher than 4, the crystallized NH4NO3
phase appeared, which was decomposed to NH3, NOx and
H2O during drying process, and due to gas liberation, 3D
xerogel network structures formed, as shown in Fig. 8 [73].
For pH = 2 and 3, gels exhibited dense microstructures in
which only few pores existed in gel structure. As pH value
increased, the network structures developed in the gels. At
pH = 6 and 7, the 3D networks were completely formed.
Due to porous network, more oxygen is introduced in the
xerogels. The oxygen accelerates the combustion process,
thus increasing combustion temperature and rate. The
porous network structures make the xerogel burn rapidly
and violently. Moreover, decomposition of NH4NO3
produced O2, thus accelerating the combustion process.
Higher pH values of mixed solutions are expected for the
synthesis of ferrite compounds with increased magnetic
initial permeability. In the same time, with increasing pH
value, crystallite size increases, and that was attributed to
higher combustion temperature [73].
With the addition of ethylene glycol into complexant and
nitrate solution, decrease of ignition temperature and
increase of heat evaluation could be expected, which may
help to form monophasic spinel ferrites [79]. Ethylene
glycol works as gelating reagent [76]. Addition of ethylene
glycol leads to the formation of an organic ester, thus bonds
between complexant and ethylene glycol is formed through
the esterication reaction [7576]. Polymerization is
facilitated by heating and results in the formation of
homogeneous polymer network with metal ions uniformly
distributed throughout the organic matrix [7576].
2.4 The inuence of atmosphere
Ambient atmosphere can play important role on nature of
combustion reaction. It was found that the mass-changing
rate in nitrogen nearly twice of that in air atmosphere. This
phenomenon was attributed to the supply of additional
nitrogen to the gel, and formation of NO3 ions acting as
oxidant [50]. However, in some cases oxidation-reduction
 Andris SUTKA et al. Solgel auto-combustion synthesis of spinel-type ferrite nanomaterials 135

Fig. 8 SEM images of dried gels prepared from solutions with pH values of (a) 2, (b) 3, (c) 4, (d) 5, (e) 6, and (f) 7. (Reproduced with
permission from Ref. [73], Copyright 2004 Elsevier)
136 Front. Mater. Sci. 2012, 6(2): 128141

reaction could be restrained in nitrogen [80]. Also, the

temperature for the spinel ferrite formation after combus-
tion reaction is lower in air than in nitrogen [50].
After combustion in helium atmosphere the as-
synthesized powder characterizes with higher content of
impurities, due to release of certain amount of reactive
gases before the combustion reaction [52].

2.5 Heating mechanism

Characteristics of spinel ferrite powders are inuenced by

the change of heating source used for combustion reaction
of xerogels [62,81]. As heating source, external heat or
microwaves could be used.
Applying external heat for the combustion initiation,
different heating devices such as mufe [45] or hot plate
[70] may be used, thus changing external conditions. Costa
et al. compared two different external heating methods:
mufe and hot plate [81]. The reaction rate is slower and
temperature higher when ignition is induced in mufe due
to differences on oxygen availability. Employing hot plate
during combustion reaction, pure spinel type structure
developed while products formed in mufe revealed
hematite as the secondary phase. Also, powders obtained
on hot plate characterizes with lower particle and
agglomerate sizes and higher specic surface area, as
shown in Fig. 9 [81].
The heating mechanism in microwave processing is
fundamentally different from that in conventional proces-
sing. Microwave radiation is absorbed and converted to Fig. 9 Transmission electron microscopy images of the pow-
thermal energy. Heat is generated from inside the xerogel, ders synthesized by combustion reaction with two different
heating conditions: (a) in mufe; (b) on plate. (Reproduced with
in contrast with conventional heating methods in which
permission from Ref. [81], Copyright 2002 Springer Netherlands)
heating proceeds from surface [49]. Advantages of
microwave heating are fast reaction kinetics and cleanness,
particle counterparts [83]. 1D structured magnetic materi-
and moreover it is cheap and ecological [82]. It was also
als could be used as building blocks for next generation
revealed that microwave power and exposure time could
electromagnetic devices and gas sensors [8485]. For
inuence the crystallinity and formation of the ferrite phase
example, microstructure of gas sensors based on tubes
[62].
consists from network of interconnected channels as shown
in Fig. 10, which increases gas access ability [84]. The
3 The new approach for the synthesis of 1D unique structural characteristics as shape anisotropy and
structures high aspect ratio of 1D structures enhance magnetic
permeability, resonance frequency and mechanical proper-
By using solgel auto-combustion method, not only spinel ties of spinel ferrites [85].
ferrites in form of spherical particles, but also 1D structures Polycrystalline ferrite bres ~0.5 m in diameter can be
can be synthesized. Recently, microscale and nanoscale prepared from citrate-nitrate gels by the immersion of a
brous materials have drawn a great interest and stimulated glass rod into gel and then pulling it out by hand. The gel
intensive researches because of their novel properties that bres were dried in vacuum and then calcined in ambient
are signicantly different from those of their bulk or atmosphere [8586]. The bres obtained with procedure
 Andris SUTKA et al. Solgel auto-combustion synthesis of spinel-type ferrite nanomaterials 137

Fig. 10 Schematic diagrams showing the gas sensor sample based on (a) 1D structures and (b) nanoparticles. (Reproduced with
permission from Ref. [84], Copyright 2007 Elsevier)

Fig. 11 SEM images of (a) a NiFe2O4 ne bre and (b) the surface morphology of the NiFe2O4 bre. (Reproduced with permission from
Ref. [86], Copyright 2007 Springer Netherlands)

mentioned above are shown in Fig. 11 [86].
It has been shown that the spinnability of the gels is
affected by viscosity, solution pH and citric acid to nitrate
ratio. The spinel ferrite bres with a hollow structure can
also be obtained by controlling chemical composition and
heating rate of gel bres [83].
4 Conclusions
By choosing appropriate complexing agent, oxygen
balance value or concentration and type of chemical
additives, as well as heating source and atmosphere, it has
been possible to control system stability, xerogel micro-
structure, reaction temperature and rate and volume of
gases generated. It will inuence phase purity, crystallinity,
defect concentration, particle and agglomerate size and
specic surface area, thus affecting electromagnetic
properties of spinel ferrite products.
Most commonly used complexant for spinel ferrite
synthesis is citric acid which in combination with ammonia
provides optimal combination of properties. Ammonia
increases metal cation chelating with citrates, which could
help to control oxygen balance and develop porous 3D
network structures in nitrate-citrate xerogels. Adjustment
of the oxygen balance i.e. complexant to metal salt ratio
allows to control reaction rate. Either excess or decient
complexant system is characterized with lower reaction
rate and temperature, which is attributed to the lack of
reductants or oxidants. This reduces chance of particles to
grow and sinter to each other, but in the same time, lower
crystallinity and phase purity are obtained. Reaction
initiation in xerogel lm on hot plate in air could be the
most preferable for small crystalline particle synthesis with
high purity due to oxygen availability and increase of the
138 Front. Mater. Sci. 2012, 6(2): 128141
reaction rate.
By using solgel auto-combustion method, 1D spinel
ferrite structures can be synthesized enhancing magnetic
permeability, resonance frequency and mechanical
properties, as well as widening application area of the
products.
Acknowledgements Authors acknowledge to the kind help of Baiba
Dzerve from the University of Latvia for image drawing and design. The
study has been supported by the European Social Fund within the project of
Support for the Implementation of Doctoral Studies at Riga Technical
University.
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