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A new method for preparing alumina nanofibers by electrospinning technology

Weimin Kang, Bowen Cheng, Quanxiang Li, Xupin Zhuang and Yuanlin Ren
Textile Research Journal 2011 81: 148 originally published online 1 September 2010
DOI: 10.1177/0040517510377831

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Original article
Textile Research Journal
81(2) 148–155

A new method for preparing alumina ! The Author(s) 2011

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nanofibers by electrospinning technology DOI: 10.1177/0040517510377831
trj.sagepub.com

Weimin Kang, Bowen Cheng, Quanxiang Li, Xupin Zhuang

and Yuanlin Ren

Abstract
A new method for synthesizing alumina (Al2O3) nanofibers through the electrospinning method was reported. The
spinning solutions of anhydrous aluminium chloride/polyvinylpyrrolidone (AlCl3/PVP), which were prepared by the sol-gel
process of the mixture of AlCl3, PVP, ethanol and redistilled water, were electrospun to form AlCl3/PVP organic-
inorganic hybrid fibers. Alumina nanofibers with average diameters of 100–800 nm were obtained by calcinations of
the as-prepared fibers. The fibers were characterized by SEM, TG-DTA, FTIR, XPS and XRD. The results showed that
with the increase of the concentration of spinning solution, the diameter of fibers also increased, and that the diameter of
fibers decreased with the increase of the applied voltage and calcination temperature. The uncrystalline Al2O3, g-Al2O3
and a-Al2O3 were obtained after calcinations of about 5 h at 450, 900 and 1100  C, respectively.

Keywords
Electrospinning, sol-gel process, alumina, nanofibers, AlCl3/PVP, calcination

evaporation,11 anodisation,12 sputtering,13 and sol–gel

Introduction
Alumina fibers have been attracting broad interests due
to their high strength and elastic modulus, corrosion
resistance, low thermal conductivity, chemical stable-
ness, and good electrical insulation.1–3 Alumina fibers
have previously been prepared by many workers using
melt cooling and sol–gel methods.4,5 They have been
widely used in multiple areas, including high tempera-
ture insulating materials, reinforcement materials of
metals, ceramics, polymers, and catalysts or absor-
bents for scavenging precious or heavy metals.6–8 It is
also used for adsorption/chemisorptions of heavy toxic
metal ions, such as arsenic or arsenate. While alumina
are more preferable in many cases as fibers down to
nanometer scale will provide benefits of lower dosage
and better compatibility with matrix when used as fil-
lers, and also higher adsorbing capability or more sur-
face active sites when employed as absorbents or
catalysts, due to their well-defined size, large surface
area to volume ratio.9,10 However, most of the previous
works for the synthesis of nanoscale alumina are
focused on the preparation of alumina in the form
of particles or films by methods such as thermal
processes.14
The electrospinning technique becomes increas-
ingly popular for the preparation of nanofibers.15–17
Electrospinning occurs when the electrical forces at
the surface of the drop overcome the surface tension.
When this happens, the solution or melt is ejected as an
electrically charged jet and shoots towards the oppo-
sitely charged electrode. Upon reaching the collector
surface, it gets neutralized and collects as dry nanofi-
bers. Initially, this technique was used for the prepara-
tion of polymer nanofibers.18–24 Recently, a new
method to produce inorganic oxide nanofibers has
been found by using electronspun fibers of polymer/
inorganic composite as the precursor, and the final
oxide fibers can be obtained by calcinations of the
Tianjin Polytechnic University, China.
Corresponding author:
Bowen Cheng, Tianjin Polytechnic University, 63 Chenglin Road,
Hedong District, Tianjin, 300160, China
Email: bowen63@126.com

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Kang et al.
composite fibers. Many kinds of inorganic oxide nano-
fibers including NiO,25 TiO2,26 ZrO2,27 SnO2,28 CeO2,29
and other oxide materials,30–39 have been successfully
produced in recent years. Dai et al. reported the syn-
thesis of alumina-borate composite fibers by electro-
spinning a viscous mixture of aluminum acetate and
10% aqueous solution of poly (vinyl alcohol) (PVA).40
In previous research,41,42 alumina nanofibers were
prepared by an electrospinning technique using differ-
ent solutions from a combination of PVA and polyeth-
ylene oxide (PEO) as a polymer precursor, and
aluminium acetate and aluminium nitrate as alumina
precursor. However, all these types of solutions are
based on water as solvent, and the formability of
them is low because the volatility of water is too
slow. Thus, the air was often warmed to increase the
evaporation rate of the water during the electrospin-
ning process. In this work, high quality alumina nano-
fibers were prepared by an electrospinning method
using economic sol-gel spinning solutions of AlCl3/
polyvinylpyrrolidone (PVP) as presurors. Some influ-
ence factors were also explored to continuously pro-
duce alumina nanofibers. The proposed method may
potentially be applied for continuous production of
high quality aluminum oxide nanofibers in industry.
Experimental
Materials
Polyvinylpyrrolidone (PVP, Mn ¼ 1,300,000) was pur-
chased from Boai NKY Pharmaceuticals Ltd. (Henan,
P.R. China) and anhydrous aluminium chloride (AlCl3,
99.7%) was obtained from Tianjin No. 3 Chemical
Reagent Plant. Redistilled water and ethanol (EtOH,
99%) were supplied by Tianjin Motian Membrane
Eng. and Tech Co., Ltd and Tianjin No.1 Chemical
Reagent Plant respectively.
Preparation of AlCl3/PVP spinning solution
First, 3.0 g of PVP were dissolved in EtOH to obtain
solutions at the concentration of 5 wt%, 6 wt% and
7 wt%, respectively. Then 2.0 g of AlCl3 were dissolved
in 8.0 mL water and were subsequently dropped slowly
into one of the PVP solutions, prepared with different
concentrations, while stirring for 4 h. Thus, the viscous
sol-gel spinning solutions of AlCl3/PVP were obtained.
Preparation of alumina nanofibers
The spinning solution was placed in a hypodermic syr-
inge and was delivered to the blunt needle tip (nozzle
diameter of approxaimately 0.8 mm) at a flow rate
of 5 mL/h via a mirco-syringe pump (WZ-500C2,
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149
Zhejiang, China) at a fixed collecting distance (23 cm)
between the tip of the syringe and rotating collector.
The positive terminal of a high voltage power
(DC60000-1mA, Tianjin, China) was applied to the
needle of the syringe via an alligator clip delivering an
applied voltage (25–40 kV). The AlCl3/PVP organic-
inorganic hybrid fibers were prepared by subjecting
the solution to a high electrical potential of hot air
and dried in a vacuum at 100  C for 24 h, and were
then sintered in a muffle furnace at 450, 900 and
1100  C for 5 h in air to obtain alumina fibers.
Characterization
The morphology of the prepared nanofibers was
observed under a scanning electron microscope
(SEM) (FEI, QUANTA200) after spraying a thin
layer of gold. The nanofibers’ diameter distributions
were calculated based on the SEM photos. For each
sample, six photos were used to measure the diameter
distributions with Image-Pro plus 6.0 software.
Infrared spectra were obtained on a FT-IR spectro-
photometer (Bruker, Tensor 37) with a resolution of
1 cm1, KBr wafers were used, and the weight percent-
age of nanofibers in KBr was about 0.5%. X-ray pho-
toelectron spectroscopy (XPS) spectra were recorded
using K-alpha X-ray photoelectron spectroscopy
employing a monochromated Al-Ka X-ray source
(h ¼ 1486.6 eV), survey spectra were recorded with a
pass energy of 200 eV, and high resolution spectra
with a pass energy of 50 eV (Thermo Fisher). The
base pressure in the sample analysis chamber was set
at 3  107 Pa. X-ray diffraction (XRD) patterns of
these materials were recorded using a diffractometer
(D/max 2500  , Japan) with a Geiger counter, con-
nected to a computer. Scans were made from 10 to
80 (2) at a speed of 2 min1.
Results and Discussion
SEM characterization of the AlCl3/PVP composite
and alumina nanofibers
The concentration of solutions is a variable that has a
dramatic effect on the results of electrospinning trials.43
In this research, electrospinning solutions of AlCl3/PVP
with a concentration of PVP from 5 wt% to 7 wt%
were easily electrospun into fibers. However, AlCl3/
PVP hybrid fiber can hardly be obtained beyond this
range. The relationship between the concentration
of PVP and the diameter distribution of AlCl3/PVP
hybrid fibers is shown in Figure 1. It can also be
found that much finer fiber could be gained when the
concentration of the solution is much lower. This is
probably because a higher viscosity results in a larger
150 Textile Research Journal 81(2)

40
(a)

Diameter distribution (%)

30

20

10

0
500 1000 1500 2000 2500
Diameter (nm)

35
(b)
30

Diameter distribution (%)

25

20

15

10

0
1000 2000 3000 4000 5000 6000
Diameter (nm)

30
(c)
25
Diameter distribution (%)

20

15

10

0
500 1000 1500 2000 2500 3000
Diameter (nm)

Figure 1. SEM photos of AlCl3/PVP hybrid fibers electrospun from spinning solutions containing 5 wt% (a), 6 wt% (b) and 7 wt%
(c) PVP solution. The applied voltage was 30 kV.

fiber diameter and the solution viscosity is proportional
to the polymer concentration.
The critical value was chosen as 25 kV to overcome
the surface tension force of the solution, and the fiber
diameter showed a slight tendency to decrease with the
increase of the applied voltage when other parameters
were fixed, as shown in Figure 2. Generally, as the
applied voltage carried by the needle of the syringe
increased, higher elongation forces were imposed to
the spinning solution under the electrical field, resulting
in thinner fiber diameters.44
SEM photos of the alumina nanofibers sintered at dif-
ferent temperatures for 5 h were presented in Figure 3.
As can be readily seen, the fibrillar attributes observed in
the spun hybrid fibers were fully retained in the fired
samples, with considerable decrease in the fiber diame-
ter. It can be seen from Figure 1a, that the prepared
fibers with diameter of 1–2 m had a cylindrical
structure and smooth surface due to the amorphous
nature of AlCl3 and PVP composites. While the diameter
of the fibers decreased after calcinations because of the
decomposition of AlCl3 and PVP, alumina nanofibers
with average diameters of 100–800 nm were obtained.
Also with the calcination temperature increasing from
450  C to 1100  C (Figure 3), the average diameter of
aluminum oxide nanofibers continuously decreased,
which indicated that most organic groups in the fibers
were completely removed.
Thermogravimetric analysis of AlCl3/PVP composites
The thermal decomposition of hybrid nanofibers could
be largely divided into three degradation steps (shown
in Figure 4a). The first weight loss of about 25%, from
25 to 250  C, mainly involved dehydration of the hybrid
fibers. The second weight loss of about 40%, started at

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Kang et al. 151

35
(a)
30

Diameter distribution (%)

25

20

15

10

0
500 1000 1500 2000 2500
Diameter (nm)
35
(b)
30

Diameter distribution (%)

25

20

15

10

0
600 800 1000 1200 1400 1600 1800 2000
Diameter (nm)

(c) 25
Diameter distribution (%)

20

15

10

0
500 1000 1500 2000 2500 3000
Diameter (nm)

40
(d)
35
Diameter distribution (%)

30

25

20

15

10

0
400 600 800 1000 1200 1400 1600 1800 2000
Diameter (nm)

Figure 2. SEM photos of AlCl3/PVP hybrid fibers electrospun from spinning solution containing 5wt% PVP solution under various
applied voltage: 25 kV (a), 30 kV (b), 35 kV (c) and 40 kV (d).

250  C, was predominantly due to decomposition of
PVP. The following weight loss of about 10%, from
450 to 600 C, corresponded to further degradation of
the unsaturated backbone residues (Al(OH)xCl3-x). As
shown in the differential thermal analysis (DTA) curve,
the prominent exothermic peak at about 336  C was
associated with the decomposition of PVP which was
in agreement with the weight loss of about 40% in the
thermogravimetric (TG) curve (Figure 4b). Another
exothermic peak was observed at 517.01  C, which
was associated with degradation of unsaturated back-
bone residues. This degradation accompanied the for-
mation of Al2O3. After 600  C, there was no change in
weight loss, which indicated that the decomposition of

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152 Textile Research Journal 81(2)

30
(a)
25

Diameter distribution (%)

20

15

10

0
400 600 800 1000 1200 1400 1600 1800 2000
Diameter (nm)

40
(b)
35

Diameter distribution (%)

30

25

20

15

10

0
200 400 600 800 1000 1200 1400 1600
Diameter (nm)
50
(c)
40
Diameter distribution (%)

30

20

10

0
200 400 600 800 1000 1200
Diameter (nm)

Figure 3. SEM photos of the alumina fibers sintered at various temperatures: 450  C (a), 900  C (b) and 1100  C (c). The PVP
concentration of the spinning solution was 5 wt% and the applied voltage was 30 kV.

PVP had been completed and Al2O3 had formed.

15 120 However, there were still prominent endothermic peak
and exothermic peak from 600 to 1400  C, which were
a – TG 100
10
analyzed as phase transition, melting and recrystalliza-
Exothermic

b – DTA tion of alumina crystals.

Heat flow (W/g)

80
Weight (%)

5 60
0
–5
0 200 400 600 800 1000 1200 1400
Figure 4. Thermogravimetric curve (a) and differential thermal
curve (b) of AlCl3/PVP hybrid fibers from spinning solution
containing 5 wt% PVP solution at 30 kV.
FTIR spectra analysis
40
Figure 5 showed the FTIR spectra of the AlCl3/PVP
20
hybrid fibers and alumina fibers. It can be seen clearly
from Figure 5a that two strong bands appeared around
0 3000 cm1 and 1600 cm1 in AlCl3/PVP hybrid fibers,
which could be assigned to the bending and
stretching vibration of CH and C¼O groups in
PVP molecule, respectively. The presence of a broad
band in the region of 500–1000 cm1 corresponding
to the stretching vibration mode of Al–O may be

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Kang et al. 153

due to the formation of Al(OH)xCl3-x when AlCl3 was

1100°C (d)
dissolved in the water.45 From the IR spectra of the alu-
900°C (c)
450°C (b) mina fibers (Figure 5b, c and d), it is easily found that the
100°C (a) band in the region of 500–1000 cm1, corresponding to
Al–O bond becomes stronger and the two bands at 1600
C–H C =O and 3000 cm1 in the spectrum of the AlCl3/PVP hybrid
fibers disappeared when calcination temperature was
over 450  C, suggesting that the PVP components were
O – AI– O
decomposed completely and the alumina was formed.
The peak at about 2350 cm1 should be attributed to
CO2 absorbed from the air by the nanofibers because
of their large surface area to volume ratio.

3900 3600 3300 3000 2700 2400 2100 1800 1500 1200 900
Wavenumber (cm–1)
Figure 5. FTIR spectra of the AlCl3/PVP hybrid fibers (a) and
alumina nanofibers prepared by calcination at 450  C (b), 900  C
(c), and 1100  C (d) for 5 h. The PVP concentration of the spin-
ning solution was 5 wt% and the applied voltage was 30 kV.
600 XPS analysis
Figure 6 shows the XPS spectra of nanofibers sintered at
900  C for 5 h. It can be seen that in the whole region of 0–
1400 eV, the characteristic peaks of Al2p, C1s and O1s are
presented (shown in Figure 6a). As shown in Figure 6b, the
peak at the binding energy of 74.42 eV corresponds to Al2p.
The peak of Al2p shows only one symmetric component

(a)
80,000 O1s

60,000
Counts / s

40,000

C1s
Al2s
20,000 Al2p

0
1400 1200 1000 800 600 400 200 0
Binding energy (eV)

(b) 4000 (c) 16000

Al2p
O1s
3500 74.42 14000
532.58
3000 12000
2500 10000
Counts / s
Counts / s

2000 8000
1500 6000
1000
4000
500
2000
0
0
65 70 75 80 85 525 530 535 540 545
Binding energy (eV) Binding energy (eV)

Figure 6. XPS spectra of Al2O3 nanofibers sintered at 900  C for 5 h: (a) survey spectrum; (b) high-resoluion XPS spectrum of Al2p;
(c) high-resoluion XPS spectrum of O1s. The PVP concentration of the spinning solution was 5 wt% and the applied voltage was 30 kV.

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154
and has no shoulder peak, which illustrates that the alumi-
num-containing compound is Al2O3. In Figure 6c, the
characteristic peak of O1s is at 532.58 eV, which can be
attributed to the lattice oxygen in Al2O3. The peak at the
binding energy of 285.36 eV corresponds to free carbon
that was formed by the decomposition of PVP due to the
calcine time being insufficient. The atomic percent and the
surface atomic ratios calculated for Al2O3 determined by
XPS are reported in Table 1. It was clearly seen from Table
1 that the Al/O ratio is close to 2:3.
X-ray diffraction
Figure 7 shows the XRD curve for the alumina fibers
after calcination at 450  C, 900  C, and 1100  C for 5 h
in air, respectively. When calcinating the AlCl3/PVP
hybrid fibers at 450  C, the obtained alumina fibers
were not fully crystallized, which was suggested by its
poorly developed XRD pattern in Figure 7a. It can
be seen clearly from Figure 7b that there are seven
reflection peaks centering at 2y of 19 (111), 32
(220), 37 (311), 39 (222), 46 (400), 61 (511), 67
(440), respectively after calcination at 900  C, which
could be indexed exactly as g-Al2O3. However, when
the calcination temperature was increased to 1100  C,
Table 1. Atomic percent of the Al2O3 nanofibers
Elements Atomic % Atomic Ratios
Al/O
Al 31.49 2:2.9
O 45.62
C 22.89
a– A12O3
g– A12O3
1100°C (c)
900°C (b)
450°C (a)
10 15 20 25 30 35 40 45 50 55 60 65 70 75 80
2q (°)
Figure 7. XRD spectra for the alumina nanofibers obtained
at 450  C (a), 900  C (b) and 1100  C (c). The PVP concentration
of the spinning solution was 5 wt% and the applied voltage
was 30 kV.
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Textile Research Journal 81(2)
the intensity of its characteristic peaks was enhanced
remarkably, and the nine reflection peaks can be seen
to have appeared at 2y of 25 (012), 35 (104), 37 (110),
42.5 (113), 52 (024), 57 (116), 61 (018), 65 (214)
and 67 (300), respectively (shown in Figure 7c),
which could be exactly indexed as a-Al2O3.
Conclusions
Alumina nanofibers with diameter of 100–800 nm were
successfully fabricated by electrospinning technique
using economic AlCl3/PVP solution as presurors.
Analytical tools, such SEM, TG-DTA, FTIR, XPS and
XRD, were employed to carry out systematic structural
and microstructural characterization of alumina fibers.
This investigation showed that the uncrystalline Al2O3,
g-Al2O3 and a-Al2O3 nanofibers of high quality could be
obtained by calcinations of the AlCl3/PVP hybrid fibers
for 5 h at 450, 900, and 1100  C, respectively.
Funding
This work was supported by the National
Science Foundation of Tianjin (grant number
09JCYBJC04500).
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