Ceramics International 44 (2018) 10984–10989

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Ceramics International
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Short communication

Solution blow spun spinel ferrite and highly porous silica nanofibers T
a a a
Rosiane Maria da Costa Farias , Lucas Leite Severo , Danubia Lisboa da Costa ,
Eliton Souto de Medeirosb, Gregory M. Glennc, Lisiane Navarro de Lima Santataa,
Gelmires de Araújo Nevesa, Ruth Herta Goldschmidt Aliaga Kiminamid,
⁎
Romualdo Rodrigues Menezesa,
a
Unidade Acadêmica de Engenharia de Materiais, Universidade Federal de Campina Grande, Av. Aprígio Veloso 882, Campina Grande 58109-970, PB, Brazil
b
Laboratory of Materials and Biosystems, Universidade Federal da Paraíba, Cidade Universitária, João Pessoa 58059-900, PB, Brazil
c
Bioproduct Chemistry and Engineering, Western Regional Research Center, United States Department of Agriculture, Agricultural Research Service, Albany, CA 94710,
United States
d
Departamento de Engenharia de Materiais, Universidade Federal de São Carlos, Rod. Washington Luis, km 235, São Carlos 13565-905, SP, Brazil

A R T I C LE I N FO A B S T R A C T

Keywords: The novelty of this work is the production of nano- and submicrometric silica and spinel-ferrite fibers using the
Silica solution blow spinning (SBS) method. A pseudo-core-shell method for the production of large surface area silica
Spinel ferrite fibers is also reported. Silica fibers present mean diameters and specific surface areas ranging from 280 nm to
Solution blow spinning 640 nm and from 140 m2/g to 630 m2/g, respectively, while spinel-ferrite fibers of nickel ferrite and nickel-zinc
Ceramic nanofibers
ferrite show mean diameters of 180 nm. Spun materials display a cotton-like morphology and are produced at
Fiber spinning
higher output rates than those achieved by current spinning technologies.

1. Introduction controlled release processes [14–16]. However, porous silica nano-

One-dimensional nanostructures such as nanowires, nanofibers,
nanotubes, and nanoribbons have attracted considerable attention in
recent years due to their high specific surface area [1–3]. Ceramic na-
nofibers have several potential applications, including tissue en-
gineering, catalysis, separation/filtration, sensors, optical and energy
devices, etc. [4–8]. Several methods have been used to produce ceramic
nanofibers; however, disadvantages that limit the commercial applic-
ability of these materials are the use of highly toxic solvents to dissolve
precursors and polymers, high electric voltages and low fiber output
[4]. Alternatively, solution blow spinning (SBS) has emerged as an ef-
ficient fiber spinning technique [9] without these disadvantages, and
presenting low cost, simplicity and high fiber production rates. Re-
cently, SBS was successfully used in the production of ceramic nano-
and submicrometric fibers of mullite, YBCO,TiO2 and ZnO [10–13].
However, no study has so far addressed the use of SBS to produce spinel
ferrite and silica nanofibers, despite the high technological importance
of these materials.
Nanostructured silica materials have been studied due to their high
specific surface area and hydrothermal stability [14]. Mesoporous silica
displays a high efficiency and large capacity for sorption processes and
is widely applied in separation/purification treatments, catalysis and
particles have the disadvantage of easy agglomeration. On the other
hand, mesoporous silica nanofibers retain their large specific surface
area and prevent agglomeration due to their fibrousness [15]. More-
over, silica-based nanofiber systems such as mats, membranes or
cotton-like structures are flexible materials that present low resistance
to mass transport or diffusion [17], which are important features for
most mesoporous silica applications.
Nickel and nickel-zinc ferrites (NiFe2O4, (NiZi)Fe2O3) are magnetic
spinel materials widely used in many industrial applications that re-
quire high resistivity and low eddy current loss, at high frequency,
hardness, chemical and thermal stability [18–20]. Nanostructured one-
dimensional spinel ferrites have attracted considerable interest because
of the reduced energy losses compared with bulk powders [21], and
possible uses in ultrahigh-density data storage devices, sensor tech-
nology, spintronic devices, and heterogeneous catalysis.
Therefore, the development of cost effective techniques for fabri-
cating 1D highly porous silica and nanostructured ferrites is of great
technological and commercial interest. In this context, spinel ferrites
and highly porous silica submicrometric and nanometric fibers were
produced for the first time by SBS and by pseudo-core-shell SBS, re-
spectively.

⁎
Corresponding author.
E-mail addresses: romualdomenezes@gmail.com, romualdo.menezes@ufcg.edu.br (R.R. Menezes).

https://doi.org/10.1016/j.ceramint.2018.03.099
Received 4 October 2017; Received in revised form 12 March 2018; Accepted 12 March 2018
Available online 15 March 2018
0272-8842/ © 2018 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
R.M. da Costa Farias et al. Ceramics International 44 (2018) 10984–10989

2. Experimental procedure

Tetraethyl orthosilicate, TEOS, Si(OC2H5)4 (Aldrich, 99%), zinc ni-

trate hexahydrate, Zn(NO3)2·6H2O (Isofar, 98.0%), nickel nitrate hex-
ahydrate, Ni(NO3)2·6H2O (Isofar, 98.0%), and iron nitrate nonahydrate,
Fe(NO3)3.9H2O (Isofar, 98.0%) were used as precursors for the pro-
duction of fibers. Tetrahydrofuran, THF (Proquimios, 99.9%), ethanol
(Cinética, 99.5%) and N,N-dimethylformamide, DMF
(Cinética, > 99.0%) were used as solvents. Polyvinyl chloride, PVC
(Norvic SP 100, average Mw ~ 50,360) and polyvinylpyrrolidone, PVP
(Aldrich, average Mw ~ 1300,000) were used as polymers.
Hydrochloric acid, HCl, 37% (Fmaia, 36.5–38.0%), and Kolliphor® P
188, (Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly
(ethylene glycol)) (Sigma, Reference 15759) were used as additives.
Silica precursor solutions were prepared as follows. (i) Two solution
were prepared separately for the fibers designated Silica-PVC, and were
then combined under vigorous stirring at room temperature, until a
clear sol was obtained – 1.0 g of PVC were dissolved in 7 ml of THF in
the first solution; and 2.5 ml of TEOS and 30 μl of HCl were dissolved in
3 ml of THF in the second solution. (ii) To form a solution for the fibers
designated Silica-PVP, .5 g of PVP were dissolved in 10 ml of ethanol
and vigorously stirred at room temperature, until a clear sol was ob-
tained, after which 0.8 ml of TEOS and 100 μl of HCl were added to the
solution. (iii) Two solutions were prepared separately for the fibers
designated Silica-PVP-KP188, and then combined under constant stir-
ring at 40 °C – the first solution contained 0.42 g of Kolliphor P188,
1.125 ml of TEOS, and 100 μl of HCl dissolved in 10 ml of ethanol; and
the second contained 1.5 g PVP dissolved in 10 ml ethanol. (iv) Two
solutions were prepared separately for the fibers designated Silica-Core-
Shell: one was used as the precursor for the core and the other for the
shell – 0.5 g of PVP was dissolved in 10 ml of ethanol for the core so-
lution, and 0.5 g of PVP, .8 ml of TEOS and 100 μl of HCl were dissolved
in 10 ml of ethanol for the shell solution. The methodology used for the
production of the fibers designated Silica-Core-Shell was defined as a
pseudo-core-shell method. The core-shell nozzle was used as a metering Fig. 1. Cotton-wool-like morphology of: a) silica fibers (Silica-PVP), and b) spinel ferrite
system rather than for producing clad-core fibers, because the two fibers (Ni-Ferrite); apparent volume (ml) (in a graduated test tube) of: c) 0.0078 g of silica
precursor solutions were mixed together at the outlet of the nozzles. fibers (Silica-PVP), and d) 0.4813 g of spinel ferrite fibers (Ni-Ferrite); and e) silica fibers
Spinel ferrite precursor solutions were prepared as follows. (i) For present flexibility and deformation capability under manual pressure.
the fibers designated Ni-Ferrite, 1.0 g of PVP were dissolved in 10 ml of
a solvent (8 ml of ethanol and 2 ml of DMF) and stirred at room tem- specific surface area was determined by the Brunauer-Emmett-Teller
perature until a clear sol was obtained, after which 100 μl of HCl, (BET) method (pore volume was determined at P/Po = 0.98),
0.8080 g of iron nitrate and 0.2908 g of nickel nitrate were added to the (Micromeritics, ASAP 2020). At least 100 fibers were measured using
solution under continuous stirring. (ii) For the fibers designated NiZn- ImageJ software to determine the mean diameter. Statistical analyses
Ferrite, 1.0 g of PVP was dissolved in 10 ml of solvent (8 ml of ethanol were performed at a 5% level of significance.
and 2 ml of DMF) and stirred at room temperature, after which 100μl of
HCl, 0.8080 g of iron nitrate, 0.1454 g of nickel nitrate and 0.1487 of
zinc nitrate were added to the solution, which was stirred until a clear 3. Results and discussion
sol was obtained.
The spinning apparatus used in this study, which was described in Fired fibers present a cotton-wool-like morphology (see Fig. 1). All
an earlier paper [11], consists of a SBS nozzle, an injection pump (KD the silica fibers produced exhibit the morphology shown in Fig. 1, as
Scientific, USA), a tubular furnace to provide a heating zone, and a well as high flexibility and high volume yield, such as depicted in Fig. 1.
heated collection chamber. The precursor solution of the fibers desig- The flexibility of silica fibers is highlighted by the deformation and
nated Silica-Core-Shell was processed using a SBS core-shell nozzle, and recovery capability (Fig. 1e), and their high volume yield can be ob-
the spinning process involved the use of two injection pumps. The served through the large volume occupied by a small amount of mass,
processing conditions were as follows: an injection rate of 7.2 ml/h and such as that shown in Fig c). These characteristics are very interesting
air pressure of 345 kPa were used for the Silica-PVC solutions and features for membrane applications. Ferrite fibers presented a lower
ferrite precursor solutions; and an injection rate of 6.6 ml/h and air volume yield (Fig. 1d); however, these fibers displayed a morphology
pressure of 345 kPa were used for the other Silica precursor solutions. that is interesting for use in electromagnetic wave absorption applica-
In the core-shell spinning, the core and the shell solutions were pro- tions, as well as in catalysts.
cessed under the same conditions. Silica fibers were fired at 700 °C, Fig. 2 shows SEM micrographs of silica and ferrite fibers, while
applying a heating rate of 10 °C/min, while the ferrite fibers were fired Fig. 3 shows fiber diameter distributions. Silica-PVC fibers have a
at 600 °C, applying a heating rate of 5 °C/min. A holding time of nonwoven fabric characteristic and consist of interconnected fibers,
120 min and an air atmosphere were used during calcinations. while silica fibers produced from PVP consist of more stretched fibers
The fibers were characterized by scanning electron microscopy that are less interconnected. These fibrous arrangements may be at-
(SEM) (LEO, 1430), transmission electron microscopy (TEM) (FEI tributed to higher turbulence during spinning (drying and drawing) of
TECNAI), X-ray diffraction (XRD) (Cu Kα) (Shimadzu, XRD 6000) and Silica-PVC fibers, due to the higher volatility of THF compared to that

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Fig. 2. SEM micrographs of silica fibers: a) Silica-PVC, b) Silica-PVP, c) Silica-PVP-KP188, d) Silica-Core-Shell; e) Ni-Ferrite, and f) Ni-Zn Ferrite.
of alcohol.
The mean diameter of Silica-PVC (Table 1) is higher than the mean
diameters (Tukey test) of all the silica fibers produced using PVP
(p < 0.001 for all comparisons); while the mean diameters of silica
fibers produced with PVP do not differ statistically (Tukey test, p ran-
ging from 0.8144 to 0.9966). The fiber diameter distributions also
follow this behavior, and the distributions of PVP derived silica fibers
differ statistically (Mann-Whitney test, p < 0.001) from that of Silica-
PVC fiber, which is broader and contains fibers with diameters larger
than 1 µm. However, the Silica-Core-Shell fiber presents a broader
diameter distribution than the Silica-PVP fiber (Mann-Whitney test,
p < 0.005) and the Silica-PVP-KP188 fiber (Mann-Whitney test,
p < 0.022). This indicates that the core-shell nozzle did not affect the
mean diameter of spun fiber, but had a small impact on the morphology
of the final material.
SEM micrographs (Fig. 2) show that nanometric and submicro-
metric spinel ferrite fibers were successfully produced for the first time
Fig. 3. Fiber diameter distribution of spun fibers: a) silica fibers; b) ferrite fibers.
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Ceramics International 44 (2018) 10984–10989
by SBS. Spun fibers presented some beads and beaded fibers, but were
homogenous and uniform. The mean diameter and diameter distribu-
tion of Ni-Ferrite fibers (Table 1) did not differ statistically from the
mean diameter (t-test, p = 0.2646) and diameter distribution (Mann-
Whitney test, p = 0.1684), respectively, of the NiZn-Ferrite fibers.
Spinel ferrite fibers have a rough appearance, while silica fibers
have a smooth appearance, because ferrite fibers are composed of larger
particles, such as depicted in TEM micrographs (Fig. 4). Spinel ferrite
fibers are composed of crystalline particles with mean diameters of
22 nm (SD = 8 nm) and 39 nm (SD = 18 nm) for Ni-Ferrite and NiZn-
Ferrite fibers, respectively. These mean diameters are differ statistically
(t-test, p < 0.001) indicating that the presence of Zn influences the
particle size of ferrite fibers.
Silica fibers are noncrystalline materials composed of particles of a
few nanometers in size. Silica-PVP, Silica-PVC and Silica-PVP-KP188
display the same morphology as that illustrated in Fig. 4. The Silica-
Core-Shell does not present a core-shell morphology because the
R.M. da Costa Farias et al. Ceramics International 44 (2018) 10984–10989

Table 1
Physical characteristics of the spun fibers.

Samples Mean diameter ( ± standard deviation) (μm) Minimum-maximum diameter (μm) BET surface area (m2/g) Pore volume (cm3/g)

Silica-PVC 0.640 ( ± 0.345) 0.194–1.694 141.02 0.4146

Silica-PVP .287 ( ± 0.106) 0.113–0.689 197.66 0.1233
Silica-PVP-KP188 0.281 ( ± 0.112) 0.088–0.653 315.17 0.1835
Silica-Core-Shell 0.262 ( ± 0.159) 0.074–0.865 633.62 0.3527
Ni-Ferrite 0.189 ( ± 0.073) 0.090–0.461 24.25 –
NiZn-Ferrite 0.178 ( ± 0.079) 0.079–0.717 26.84 –

nozzles were used as a metering system for the precursors rather than
for the production core-shell structures. However, its fiber morphology
is different from that of the other silica-based fibers, containing a large
amount of mesopores (pore size of 2–50 nm), with a mean pore size of
18 nm, ranging from 7 to 38 nm. There was good interaction and mis-
cibility between the inner and outer spinning solutions, because the
same type of solvent and polymer were used, but the viscosity of the
inner solution was lower. A perfect co-spinning process did not take
place during spinning, and the inner and outer solutions mixed together
to form polymer/solvent-rich regions (inner solution), but poor in or
without TEOS, albeit without compromising the fiber structure. Fur-
thermore, during the spinning process, TEOS hydrolyzed rapidly and
condensed in the shell/outer region of the fiber, due to the heating
process. This occurred in parallel with the drying of the fiber surface,
hindering the formation of solvent and polymer-rich regions on the
fiber surface. After firing, the polymer and solvent-rich regions gener-
ated pores, like those depicted in Fig. 4, which enhanced the specific
surface area of the material without requiring the addition of a por-
osifier.
The XRD patterns of the fired fibers (Fig. 5) indicate that the silica

Fig. 4. TEM micrographs of: a) Silica-PVP, b) Silica-Core-Shell, c) Ni-Ferrite, d) NiZn-Ferrite.

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Fig. 5. XRD patterns of silica and spinel ferrite fibers.
fibers are noncrystalline, such as those shown in Fig. 4, and that the
ferrite fibers have typical spinel reflections: [2 2 0], [3 1 1], [2 2 2], [4
0 0] and [4 2 2]. The Ni-Ferrite also displayed a [5 1 1] reflection and
the NiZn-Ferrite a [3 3 3] reflection. The reflections of Ni-Ferrite and
NiZn-Ferrite are in agreement with JCPDS card nos. 86-2267 and 52-
0278, respectively. Both fibers showed the development of secondary
phases, such as iron oxide (Fe2O3), JCPDS card no. 33–0664, and zin-
cite, (ZnO), JCPDS card no. 36-1451. This can be attributed to the short
stirring time of 2 h during the mixing of the precursors.
Silica fibers presented large surface areas (Table 1) ranging from
140 to 630 m2/g, which is consistent with values reported for meso-
porous silica materials [14,15,20]. The surface area of Silica-Core-Shell
was larger than that of Silica-PVP-KP188, indicating that the pseudo-
core-shell method used was highly efficient in generating fibers with
large specific surface areas, without the use of additives such as sur-
factants, structure directing agents or specific pore-generating agents.
The Silica-PVC fibers showed the highest pore volume, which may
be attributed to their larger diameter and to the high volatility of the
solvent used. THF quickly evaporated across the heated working dis-
tance used. However, these fibers were thicker and this combination
generated a dry outer region layer, while the core still contained a large
amount of solvent. As the spinning and drying process continued, the
heated solvent expanded and evaporated opening pores through the
fibers. On the other hand, when ethanol was used, the fibers were
considerably thinner and the evaporation rate of the solvent was lower.
This enabled simultaneous fiber stretching and gradual solvent drying.
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Ceramics International 44 (2018) 10984–10989
Moreover, when solvent evaporates slowly, polymer chains and silica
structures are brought closer together due to the capillary forces, con-
tributing to reduce the pore volume.
Spinel ferrite fibers also presented a large specific surface area
(Table 1), which was ascribed to their morphology and the high spin-
ning rates, making the resulting spinel fibers potential materials for
applications that require large surface areas, such as catalysts, bioma-
terials and ferrimagnetic membranes. Large surface area ferrimagnetic
materials are generally produced when nanostructured powders are
obtained, however, such materials have a strong tendency for particle
agglomeration, significantly decreasing their specific surface are.
However, the ferrite fibers produced here were nanostructured and
retained their large specific surface areas, with no tendency for ag-
glomeration/aggregation. Studies on nickel and nickel-zinc ferrite na-
noparticles [21–25] presented BET surface areas, for the nanoparticles,
ranging from 3 to 200 m2/g, depending on the size and porosity of the
particles. There is a concentration of these surface area values in the
range of 10–50 m2/g, and of particles mean size in the range of
5–25 nm. However, BET surface area of 6 m2/g was shown for ferrites
with particles size of 190 nm [26] and surface area of 25 m2/g for na-
noferrites with crystallite size of 36 nm [27], which demonstrated that
the produced nanofibers (mean diameter of 180 nm and crystallite size
of 22–40 nm) have BET area similar to those of nanostructured ferrite
powders, but without the disadvantages of this type of material, such as
agglomeration/aggregation tendency.
4. Conclusions
The production of nanometric and submicrometric silica and spinel-
ferrite fibers by means of solution blow spinning is reported here for the
first time. Uniform, homogenous, large surface area silica fibers were
obtained without requiring high voltage. The morphological char-
acteristics of the silica fibers were dependent on the solvent-polymer
system used in the spinning process. The more efficient system to
achieve large surface areas was the PVP-ethanol, and the pseudo-core-
shell method was the more appropriate route for spinning large surface
area (600 m2/g) mesoporous silica nanofibers. High surface area
(25 m2/g) nanostructured spinel-ferrite fibers were also produced by
SBS at high output rates, using precursor solutions prepared with PVP
and a mixture of ethanol/DMF as solvent.
Acknowledgments
The authors would like to thank the Brazilian research funding
agency CNPq (National Council for Science and Technology), grant nos.
310932/2015-7 and 201821/2015-0, for its financial support; and Dr.
Marcelo Strozi Cilla for performing the TEM and BET analyses.
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