General strategy for fabricating thoroughly mesoporous nanofibers

Article abstract of DOI:10.1021/ja508840c

Recently, preparation of mesoporous fibers has attracted extensive attentions because of their unique and broad applications in photocatalysis, optoelectronics, and biomaterials. However, it remains a great challenge to fabricate thoroughly mesoporous nanofibers with high purity and uniformity. Here, we report a general, simple and cost-effective strategy, namely, foaming-assisted electrospinning, for producing mesoporous nanofibers with high purity and enhanced specific surface areas. As a proof of concept, the as-fabricated mesoporous TiO₂ fibers exhibit much higher photocatalytic activity and stability than both the conventional solid counterparts and the commercially available P25. The abundant vapors released from the introduced foaming agents are responsible for the creation of pores with uniform spatial distribution in the spun precursor fibers. The present work represents a critically important step in advancing the electrospinning technique for generating mesoporous fibers in a facile and universal manner.

Full text of DOI:10.1021/ja508840c

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A General Strategy for Fabricating Thoroughly Mesoporous Nanofibers
Huilin Hou, Lin Wang, Fengmei Gao, Guodong Wei, Bin Tang, Weiyou Yang, and Tom Wu
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A General Strategy for Fabricating Thoroughly Mesoporous
Nanofibers
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†,‡
†
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†
‡
,†
Huilin Hou, Lin Wang, Fengmei Gao, Guodong Wei, Bin Tang, Weiyou Yang,* * ꢀandꢀTomꢀ
,
§
Wu, * ꢀ
†
Institute of Materials, Ningbo University of Technology, Ningbo, 315016, P.R. China
‡
Research Institute of Surface Engineering, Taiyuan University of Technology, Taiyuan, 030024, P.R. China
§
Materials Science and Engineering, King Abdullah University of Science and Technology (KAUST), Thuwal 23955-6900,
Saudi Arabia.
Supporting Information Placeholder
we report a general strategy, namely foaming-assisted electro-
spinning, for the synthesis of mesoporous fibers. TiO and TiO
ABSTRACT: Recently, preparation of mesoporous fibers has
attracted extensive attentions because of their unique and broad
applications in photocatalysis, optoelectronics and biomaterials.
However, it remains a great challenge to fabricate thoroughly
mesoporous nanofibers with high purity and uniformity. Here, we
report a general, simple and cost-effective strategy, namely
foaming-assisted electrospinning, for producing mesoporous
nanofibers with high purity and enhanced specific surface areas.
2
2
-
based composites are chosen as the examples to demonstrate the
versatile and general nature of our approach. The resultant meso-
porous fibers exhibit much better performance compared to the
conventional nanofibers and the commercially available P25
product, suggesting their very promising application prospect. The
present work might open new doors for the exploration of meso-
porous nanofibers with high photocatalytic activities.
2
As a proof of concept, the as-fabricated mesoporous TiO fibers
exhibit much higher photocatalytic activity and stability than both
the conventional solid counterparts and the commercial available
P25. The abundant vapors released from the introduced foaming
agents are responsible for the creation of pores with uniform
spatial distribution in the spun precursor fibers. The present work
TiO mesoporous nanofibers were fabricated by calcination
of precursor fibers, which were obtained by electronspinning the
2
solution of polyvinylpyrrolidone (PVP), tetrabutyl titanate
(TBOT), and foaming agent diisopropyl azodiformate (DIPA).
The raw materials of TBOT (Aladdin, Shanghai, China), PVP
(MW≈1300000, Aladdin, Shanghai, China) and DIPA (Adamas,
Shanghai, China) were commercially available and directly used
without further purification. Absolute ethyl alcohols and acetic
acid were used as the solvents to homogenously mix TBOT, PVP
and DIPA. In a typical experiment, PVP, TBOT and solvents were
firstly mixed by vigorously stirring for 6 h. PVP is used here to
tune the viscosity of the solution. DIPA of 10 wt% was then add-
ed into the above solution with further magnetic stirring for 2 h.
The resultant solution was transferred into a plastic syringe with a
stainless steel nozzle (anode, diameter: 0.22 mm). The tip of the
stainless steel nozzle was placed in the front of a metal cathode
represents
a
critically important step in advancing the
electrospinning technique for generating mesoporous fibers in a
facile and universal manner.
Mesoporous materials are of great interest in the fields of ca-
talysis, selective adsorption and host/guest supports, owing to
their high specific surface areas as compared to their conventional
1
solid counterparts. Recently, preparation of mesoporous mi-
cro/nanofibers has particularly attracted extensive attentions be-
cause of their broad applications in photocatalysis, optoelectronics
(
collector) with a typically fixed distance of 20 cm between the
2
and biomaterials. Besides the intrinsic porous characteristics, the
nozzle and the collector. An electrical potential of 18 kV was
applied for electrospinning the precursor fibers, and then the
products were dried in oven at 60 °C. Subsequently, the precursor
fibers were positioned in a quartz crucible and annealed in a tube
furnace at 550 °C in air for 2 h, before cooling to the ambient
temperature. For comparison, a control experiment was also car-
ried out without the foaming agent addition in the initial solutions,
and the details are shown in Table S1 (Supporting Information).
The resultant products were referred as Sample A1 and A2, re-
spectively. To show the universality of this technique for generat-
1D mesoporous nanofibers provide efficient paths for the electron
transportation and possess a robust geometry to maintain the func-
3
tionalities. Up to date, several methods have been invented to
4
fabricate mesoporous nanofibers, such as hydrothermal route,
5
6
template-assisted process, electrospinning technique, structure-
selective synthesis and so on. However, it still remains a great
7
challenge to fabricate thoroughly mesoporous nanofibers with
satisfied purity and uniformity in a simple and universal manner.
Electrospinning is a versatile, simple and cost-effective strat-
egy for producing 1D nanostructures of a wide range of materials
ing mesoporous fibers, TiO
were also synthesized with the similar experimental procedures.
Zinc acetate (Zn(Ac) ), copper acetate (Cu(Ac) ) and ferric acety-
lacetonate (Fe AcAc) were used as the raw materials in the syn-
thesis of TiO /ZnTiO , TiO /CuO and TiO /Fe hybrid nano-
2
-based hybrid mesoporous nanofibers
8
with tunable diameters and morphologies. However, most of the
reported works were focused on the fabrication of conventional
solid fibers without any pores. Can we advance the facile tech-
nique of electrospinning to create mesoporous fiber structures?
Such a breakthrough will lead to the fabrication of mesoporous
fibers with enhanced specific surface areas in a controlled man-
ner. This is the primary motivation behind the present work. Here,
2
2
2
3
2
2
2 3
O
fibers, respectively. Dimethylformamide (DMF) was added to
improve the solubility of precursors during the preparation of the
solutions. The detailed compositions of the initial solutions were
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shown in Table S2 (Supporting Information), and the resultant
process, indicating their high structural robustness. Figure 1(d)
presents the typical XRD pattern of the calcined products of Sam-
ple A1. All the peaks can be indexed to the anatase TiO (JCPDS,
No. 21-1272), suggesting the pure phase of the resultant fibers.
The sharp diffraction peaks indicate that the products are highly
crystalline.
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products were referred as Samples B-D, respectively. The details
for structure characterization and photocatalytic performance
measurement of the mesoporous fibers were shown in the Sup-
porting Information.
2
Nitrogen adsorption measurements (Figure 1(e) revealed that
the products exhibit the type IV isotherm behavior with H3 hyste-
resis, implying that the obtained fibers are mesoporous with a
BET surface area of ~64.9 m /g. The distribution of Barrett–
Joyner–Halenda (BJH) pore sizes (Figure 1(f)) determined from
the adsorption branches are peaked at ~16 nm.
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A control experiment without the foaming agent added in the
initial solutions (see Sample A2 in Table S1, Supporting Infor-
mation) was carried out to isolate the effect of the foaming agent
of DIPA on the formation of the porous fibers. The as-spun poly-
mer fibers are similar to those of Sample A1 (Figure S3(a-b),
Supporting Information). However, their calcined products pre-
sent the ordinary solid nanofibers (Figure S3(c-d), Supporting
Information), which are quite different from the mesoporous
structures synthesized with the 10 wt% foaming agents, suggest-
ing that the introduced foaming agents are critical for the for-
mation the mesoporous structures. The XRD pattern (Figure
S3(e), Supporting Information) discloses that the as-prepared
2
Sample A2 is also pure anatase TiO , implying that the foaming
agent has no effect on the compositions of the resultant products.
However, the calcined fibers of Sample A2 shows a BET surface
2
area of ca. 11.9 m /g (Figure S3(f), Supporting Information),
2
which is about 6 times lower than that of Sample A1 (64.9 m /g).
Table S3 in Supporting Information summarizes the surface prop-
erties of the Samples A1 and A2. Sample A1 possesses much
higher pore volume than A2, implying that the foaming agent of
DIPA is responsible for the formation of the mesopores within the
fibers. This comparison unambiguously suggests: i) the foaming
agents play a critically important role on the formation of the
mesoporous fibers, which helps create the pores throughout the
entire body of fibers with uniform spatial distribution; ii) the
foaming agents significantly enhance the BET Surface area of the
resultant fibers.
Figure 1. (a-b) Typical SEM images of the TiO
nanofibers under different magnifications. (c) A representative
TEM image of a single mesoporous TiO nanofiber. The inset is
the corresponding SAED pattern recorded from the marked area
of A in (c). (d) A typical XRD pattern of Sample A1 after calcina-
2
mesoporous
2
tion. (e) Nitrogen adsorption-desorption isotherm of the TiO
mesoporous nanofibers. (f) Corresponding pore size distribution.
2
The formation mechanism of the mesoporous fibers could be
explained as follows (schematically shown in Figure S4(a), Sup-
porting Information). First, the DIPA, the foaming agent, is as-
sembled into the precursor fibers (Step I). Since the DIPA is dis-
solved in the solutions before electrospinning, the foamer is dis-
tributed homogenously within the fibers. The homogeneous dis-
tribution of DIPA is consistent with elemental mapping data and
the formation of uniform porous structure throughout the fiber
body. During the calcination process under air at 550 °C (Step II),
SEM was employed to characterize the spun precursor fibers
and their corresponding calcined products. The as-spun precursor
fibers of Sample A1 have smooth surfaces with average diameter
of ~1 µm and lengths up to several hundred of millimeters. The
corresponding elemental mappings show uniform spatial distribu-
tion of Ti, N and O (Figure S1, Supporting Information). Figure
1(a) shows the typical SEM images of the calcined fibers (also see
Figure S2(a-c), Supporting Information). All the precursor nano-
fibers have been completely converted into mesoporous nano-
fibers with a high purity. The fiber diameter is reduced to ~600
nm, mainly owing to the elimination of PVP and the formation of
the DIPA foamer, with the chemical formula of C
completely decomposed into vapor phases (e.g. CO
O), which cause the formation of the pores within the fibers.
8
H
14
N
2
O
4
, is
2
, NO
2
and
crystalline TiO
shows a representative cross-section SEM image of the TiO
2
after the high-temperature treatment. Figure 1(b)
mes-
H
2
This is confirmed by the thermal analysis of the as-spun
PVP/TBOT/DIPA fibers of Sample A1 (Figure S4(b), Supporting
Information). The initial slight weight loss in the low temperature
range (35-130 °C) is owing to the residual solvent decomposition
and volatilization. The 10 % weight loss between 130 °C and 180
2
oporous nanofibers, disclosing that the fibers possess a thoroughly
porous structure with homogeneous pores.
Figure 1(c) provides a representative TEM image of a single
TiO nanofiber, further confirming that densely distributed pores
2
exist throughout the fiber body. The SAED pattern (the inset in
Figure 1(c)) recorded at the marked area in Figure 1(c) suggests
2
that the obtained product is anatase TiO (JCPDS, No. 21-1272)
with a polycrystalline nature. Furthermore, the EDS spectrum
discloses that the fibers possess only Ti and O (Figure S2(d),
Supporting Information). Although the DIPA foamer contain N,
we did not detect any N in the calcined fibers. We should also
mention that many long mesoporous fibers survived the scratch-
ing and ultrasonic treatments during the TEM sample preparation
°
C is caused by the decomposition of DIPA (DSC exdothermic
peak at ~160 °C), which results in the formation of mesoporous
precursor nanofibers. The 40% weight loss at the higher tempera-
tures (300 - 480 °C) should be attributed to the decomposition of
PVP (DSC endothermic peak at 420 °C). Finally, the DSC
exdothermic peak at 500 °C is attributed to the TiO crystalliza-
2
tion. In contrast, as shown in Figure S4(b), there are only two
exothermic peaks observed for Sample A2, which are related to
2
PVP decomposition and TiO crystallization. These data suggest
2
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that the introduction of the DIPA foaming agents notably affects
the thermal behaviors of as-spun fibers.
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Figure 2. (a) The hydrogen production photocatalyzed by the as-
fabricated mesoporous TiO nanofibers, solid TiO nanofibers and
P25 under different irradiation time. (b) Results of reusability
experiments for photocatalytic H generation using the present
2
2
Figure 3. (a1-c2) Typical SEM images of the hybrid mesoporous
nanofibers of TiO /ZnTiO (a1-a2), TiO /CuO (b1-b2) and
TiO /Fe . (a3-c3) Typical TEM images of individual mesopo-
2
three photocatalysts. (c) Schematic illustration of mesoporous
fibers with enhanced photocatalytic activities.
2
3
2
2
2 3
O
rous nanofibers from Samples B, C and D, respectively. (a4-c4)
Representative XRD patterns recorded from the calcined products
of Samples B, C and D.
The as-fabricated TiO
2
mesoporous nanofibers (Sample A1)
and solid TiO nanofibers (Sample A2), as well as the commercial
2
P25, were used as the photocatalysts for evaluation of their photo-
catalytic properties. The surface properties of P25 are shown in
Table S3, Supporting Information. Figure 2(a) plots the evolution
of hydrogen produced from the aqueous suspensions of the three
photocatalysts (their average hydrogen production rates are shown
in Figure S5, Supporting Information). It is clear that the hydro-
Now we come to the point on the versatile and universal
characteristics of the present foaming-assisted electrospinning
technique for producing mesoporous nanofibers. Three TiO -
2
based hybrid materials are chosen as the examples (see Table S2,
Supporting Information). Figure 3(a1-c2) displays the representa-
tive SEM images of the calcination products corresponding to the
as-spun precursor fibers of Sample B, C and D (i.e., using zinc
acetate, copper acetate and ferric acetylacetonate as the precur-
sors, respectively) (Figure S6, Supporting Information), suggest-
ing that the precursor fibers have been completely converted to
mesoporous fibers (Figure S7, Supporting Information). Close
observations on the cross sections (Figure S7, Supporting Infor-
mation) indicate that all the fibers are thoroughly mesoporous.
Figure 3(a3, b3 and c3) depict the typical TEM images of Sample
B, C and D, respectively, further confirming their thoroughly
mesoporous nature (also see Figure S8-10(a), Supporting Infor-
mation). Figure 3(a4, b4 and c4) displays the typical XRD pat-
terns corresponding to Sample B, C and D. These experimental
gen evolution rate of the TiO
2
mesoporous nanofibers (ca. 399.2
-
1 -1
µmol g h ) is much higher than those of solid counterpart (ca.
-
1
-1
-1 -1
1
56.9 µmol g h ) and P25 (ca. 197.8 µmol g h ), suggesting that
the creation of pores in/on the fibers by the foaming agents signif-
icantly improves the photocatalytic activity of TiO . More inter-
estingly, the hydrogen production rate of thoroughly mesoporous
TiO nanofibers is higher than most values reported for solid and
porous TiO nanofibers (see Table S4, Supporting Information).
To further investigate their reusability and stability, these three
photocatalysts were recovered and reused for photocatalytic H
production under the similar conditions. As shown in Figure 3(b),
there is nearly no loss of H evolution rate for both mesoporous
and solid TiO fibers photocatalysts, whereas the activity of P25
evidently declined after 3 cycles. This confirms that the obtained
mesoporous TiO fibers are much more stable with a higher pho-
tocatalytic activity than the commercial product of P25. To ac-
count for the high performance of mesoporous TiO fibers, a
2
2
2
2
2
2
results suggest that the obtained three samples are TiO
2 3
/ZnTiO ,
TiO /CuO and TiO /Fe hybrid fibers, respectively, which are
2
2
2 3
O
2
consistent with the SAED analyses (Figure S8(b), Figure S9(b)
and Figure S10(b), Supporting Information). The EDS analyses
2
(
Figure S8(c), Figure S9(c) and Figure S10(c), Supporting Infor-
schematic diagram is illustrated in Figure 3(c). First, the one-
dimensional (1D) fibers could remarkably inhibit the agglomera-
tion of nanoparticles, which contributes to the stable photocatalyt-
mation) disclose the presence of Zn, Cu, and Fe elements, respec-
tively, besides Ti and O, consistent with the expected composi-
tions. The HRTEM images (Figure S8(d-f), Figure S9(d-f) and
Figure S10(d-f), Supporting Information) further confirm that the
9
ic performance. Second, the columnar mesoporous architecture
possesses the interconnected channels, which offers more active
sites to adsorb reactants, e.g. water and MeOH groups. Finally,
the mesoporous channels existing throughout the fibers allow the
2 3 2 2 2 3
synthesis products are TiO /ZnTiO , TiO /CuO and TiO /Fe O
hybrid fibers. The results of BET surface areas and the pore sizes
distribution measurements (Figure S11, Supporting Information)
indicate that these three products also display the type IV-like
10
effective transportation of gaseous products. In other words, the
morphology of the 1D mesoporous fibers is beneficial to the par-
ticipation materials moving easily into/out of the framework,
yielding a high reaction rate. These synergetic effects as men-
tioned above are responsible for the much improved photocatalyt-
ic properties of the mesoporous fibers with high activity and sta-
bility.
isotherm with H3 hysteresis, and the BET surface areas are ~37.8,
2
5
0.7 and 35.9 m /g for TiO
2
/ZnTiO
3
, TiO
2
/CuO and TiO
2
/Fe
2
O
3
hybrid fibers with average pore sizes of 17.1, 16.2 and 38.3 nm,
respectively. The surface properties of the three hybrid products
are summarized in Table S5, Supporting Information. These re-
3
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sults demonstrate that diverse materials can be fabricated simply
by using the corresponding raw materials, suggesting the versatili-
ty and universality of the present foaming-assisted electrospinning
technique for the fabrication of mesoporous fibers.
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In summary, we have demonstrated a novel and general
strategy, namely foaming-assisted electrospinning, for producing
mesoporous nanofibers. This universal method is effective for
generating thoroughly mesoporous fibers with high purity and
remarkably enhanced specific surface areas. As a proof of con-
1
6
2
cept, the as-fabricated mesoporous TiO fibers exhibit a much
higher photocatalytic activity and stability than both the conven-
tional solid counterparts and the commercial available P25. The
release of vapor phases from the introduced foaming agents is
responsible for the creation of pores in/on the polymeric precursor
fibers, leading to the formation of mesoporous structures. Our
work opens new doors for the exploration of thoroughly mesopo-
rous fibers, and the novel synthesis will advance such materials
towards the high-performance applications as photocatlysts and
catalyst supports.
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(10) (a) Yu, J. C.; Wang, X.; Fu, X. Chem. Mater. 2004, 16, 1523. (b)
2
ASSOCIATED CONTENT
Supporting Information
Guo, C.; Ge, M.; Liu, L.; Gao, G.; Feng, Y.; Wang, Y. Environ. Sci. Tech-
nol. 2009, 44, 419. (c) Zhou, W.; Li, W.; Wang, J.; Qu, Y.; Yang, Y.; Xie,
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Supplementary to the section of experimental procedure, addi-
tional date including SEM, TEM, XRD, TG-DCS and BET of the
example products，and schematic illustration for the formation of
mesoporous nanofibers. These materials are available free of
charge via the Internet at http://pubs.acs.org.”
9
280.
AUTHOR INFORMATION
Corresponding Author
*Email : weiyouyang@tsinghua.org.cn (W. Yang)；
tao.wu@kaust.edu.sa (T. Wu)
Notes
The authors declare no competing financial interests.
ACKNOWLEDGMENT
This work was supported by the 973 program (Grant No.
2
(
012CB326407), National Natural Science Foundation of China
NSFC, Grant Nos. 51372122 and 51372123) and Outstanding
Innovation Project for Graduate Student in Shanxi Province
Grant No. 20133040).
(
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