X. Yuan et al. / Journal of Alloys and Compounds 680 (2016) 604e611
605
an onyx mortar and sieving with the 300 mesh sieve. Subsequently,
the powders were equally divided into four parts and each was
added into a stainless steel mould to cold-press into a cuboids
monolith under a pressure of 10.0 MPa for 2.0 min. Finally, the
2
polymer/SiO monolith was transferred into a horizontal ceramic
tube furnace and subjected to the thermal treatment in Ar atmo-
ꢀ
sphere at x C (x ¼ 1200, 1300, 1400 or 1500) for 2 h with a heating
ꢀ
ꢁ1
2
rate of 1 C min , to generate SiC/SiO monolithic ceramic. The
monoliths pyrolyzed at different temperatures were denoted as
SiC/SiO -1200, SiC/SiO -1300, SiC/SiO -1400 and SiC/SiO -1500,
respectively.
2
2
2
2
2.3. Characterization
2
Scheme 1. Schematic illustration of the ordered inter-filled SiC/SiO composite.
Powder small-angle X-ray diffraction (SA-XRD) and wide-angle
X-ray diffraction (WA-XRD) patterns were achieved using a Philipps
X’Pert PRO X-ray diffraction system (Cu K radiation, 0.15406 nm).
a
absorption performances were investigated at X-band. The results
clearly indicated that the combination of the specific structure and
high crystallinity SiC can be contributed to an enhanced microwave
absorption property. To find the optimal reflection loss (RL) and
matching thickness, the quarter-wavelength thicknesses and
impedance match degree plots were constructed and the relevant
loss mechanisms were proposed herein.
The surface morphology was investigated by a field emission
scanning electron microscope (FE-SEM, S4700). Transmission
electron microscopy (TEM) measurement was conducted on a FEI
T20 microscope operated at 200 kV. Nitrogen adsorption-
desorption isotherm measurements were performed on a Micro-
ꢀ
metitics ASAP 2020 volumetric adsorption analyzer at ꢁ196 C. The
mechanical compressive strength of the monoliths was evaluated
using a universal tensile testing machine (SHIMADZU Universal
Testing Machine AGS-X 5kN) at room temperature. Direct current
2
. Experimental details
(
DC) conductivity was performed with a standard two lines method
2
.1. Chemicals
using the DC Source (Precise Current Source by Keithley, 6220,
USA). The dielectric properties were measured by a vector network
analyzer (VNA, MS4644A, Anritsu, Atsugi, Japan) in X-band
Triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-
poly(ethylene oxide) copolymer Pluronic P123 (M
EO20PO70EO20) was purchased from Sigma-Aldrich. Polycarbosilane
PCS) was obtained from lab of ceramic fiber and composites, Na-
w
¼ 5800,
(8.2e12.4 GHz) using the wave-guide method. The as-prepared
sample was placed vertically in the center of test chamber during
measurement.
(
tional University of Defense Technology, China. Others chemicals
were purchased from Shanghai Reagents Co., Ltd. All chemicals
were used as received state without any further purification. High-
purity argon (99.99%) was used in their as-received state during the
ceramic preparation.
3
. Results and discussion
3
.1. Morphology and microstructure
The synthetic approach for the ordered mesoporous inter-filled
2.2. Synthesis of mesoporous SBA-15 and SiC/SiO
2
monolithic
2
SiC/SiO monoliths was shown in Scheme 1. The microsturctures of
composites
the SBA-15 were shown in Fig. S1 in the SI. The SBA-15 exhibited 2-
D P6mm hexagonal symmetry with a specific surface area of
2
ꢁ1
and an average pore diameter of 8.9 nm (shown in
Mesoporous silica SBA-15 was prepared by hydrothermal syn-
thesis method according to established procedures [17], using P123
as structure directing agent and TEOS as a precursor. A detailed
explanation on the synthesis and characterization of the meso-
porous SBA-15 were given in the Support Information (SI).
573 m
g
Table 1). These results indicated that the SBA-15 had good ordered
mesoporous structure, high specific surface area and narrow pore-
size distribution.
The typical cross-section SEM images of SiC/SiO
were shown in Fig. 1. The samples of SiC/SiO -1200, SiC/SiO
and SiC/SiO -1400 all exhibited interconnected particles with a
uniform size of about 1.0 m (shown in Fig. 1aec). The morphol-
2
monoliths
The SiC/SiO
2
monoliths were synthesized by a combined process
2
2
-1300
of nanocasting and cold-pressing. A flow chart of the synthesis
2
procedure was shown in Scheme 1. In a typical process, 4.0 g of SBA-
m
ꢀ
1
5 was placed in a flask, dried at 150 C under a vacuum for 4.0 h
ogies of these monoliths were similar to that of the SBA-15, which
and cooled down to room temperature (RT), and then added in the
solution of 5.0 g PCS and 45.0 ml THF to stir for 6.0 h. After that, the
THF solvent was removed under vacuum to generate a powdery
mixture. The fine powdery mixtures were obtained by grinding in
confirmed that the SiC grains were restricted into channels of the
SBA-15 [25,27]. When the calcination temperature was 1500 C, the
as-prepared composite was constructed from unconnected parti-
cles (shown in Fig. 1d). Meanwhile, there were many big pores in
ꢀ
Table 1
Textural data of the samples.
BET (m2
g
ꢁ1
)
Pore volume (cm3
g )
ꢁ1
Pore size (nm)
Compression strength (MPa, RT)
Sample
SBA-15
S
573.0
25.3
38.5
60.7
15.6
1.0
e
8.9
e
e
SiC/SiO
SiC/SiO
SiC/SiO
SiC/SiO
2
-1200
-1300
-1400
-1500
43.8
52.0
68.5
39.2
2
2
2
0.1
0.13
e
3.8
4.0
e