a r t i c l e i n f o a b s t r a c t
Article history: Porous SiC membrane supports were fabricated from SiC and glass frit at a temperature as low as 850 C
Received 1 August 2016 in air by a simple pressing and heat-treatment process. The effects of the initial SiC particle size and frit
Received in revised form 4 November 2016 content on the porosity, exural strength, and air permeation of the membrane supports were investi-
Accepted 8 November 2016
gated. During heat-treatment, the glass frit transformed to a viscous glass phase, which acted as a bonding
Available online xxx
material between SiC particles and as a protecting layer for severe oxidation of SiC particles. The porosity
of the porous SiC membrane supports could be controlled within a range of 3746% with the present
Keywords:
set of processing conditions. The typical exural strength, permeability, and specic air ow rate of the
Silicon carbide
Membranes
porous membrane supports fabricated using 23 m SiC particles with 15 wt% glass frit were 75 MPa,
Porosity 4.2 1013 m2 , and 32.4 L/min/cm2 , respectively.
Flexural strength 2016 Elsevier Ltd. All rights reserved.
Specic air ow rate
http://dx.doi.org/10.1016/j.jeurceramsoc.2016.11.019
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(1) Chae et al. [30] prepared glass-bonded porous SiC using SiC
powders, a glass frit, and glass microbeads as raw materials and
characterized the exural strength of the porous ceramics. The
typical exural strengths of glass-bonded porous SiC ceramics
were 1923 MPa at 4649% porosity.
(2) Wang et al. [31] prepared glass-bonded porous SiC for vacuum
chuck applications. By adjusting the particle size of SiC powders
and glass frit content, the porosity of the porous SiC ceramics
could be controlled within the range of 3265%. The air perme-
ability and adsorbability were investigated for the glass-bonded
porous SiC ceramics.
2. Experimental procedure puted from the measured ow rate and pressure difference using
Darcys law,
Commercially-available SiC powders with particle sizes of
p/L = Q /A (1)
10 m, 23 m, 35 m (Sinxing Advanced Materials, Hong Kong),
and 65 m (Showa Denko K.K., Tokyo, Japan), and a glass frit bond- where p is the pressure drop from the entrance to the exit of the
ing material (Korea Ceramics Co. Ltd., Gwangju-shi, Gyeonggi-do, sample, L is the thickness of the sample, Q is the ow rate of air
Korea) were used as the starting powders. The chemical compo- through the sample, is the viscosity of air, A is the cross-sectional
sition of the glass frit material was as follows: 73.2% SiO2 , 10.6% area of the sample, and is the permeability.
B2 O3 , 6.4% Al2 O3 , 6.3% Na2 O and 3.5% other materials. The weight The chemical stability of the glass-bonded SiC membrane sup-
fraction of the glass frit was 10, 15, 20, and 25 wt%. To prepare a ports (SC10) with 15 wt% glass frit was evaluated by placing
batch consisting of SiC and glass frit, the SiC powder, glass frit, and samples in glass bottles lled with a pH solution of 3 or 11, respec-
organic binders (polyethylene glycol and polyvinyl alcohol, 5 wt% tively. The pH 3 and 11 solutions were prepared using nitric acid
with respect to ceramic powders) were mixed by ball milling using and ammonia solution with distilled water, respectively. The bot-
SiC media in distilled water in a polypropylene jar for 24 h. The mix- tles were stored at room temperature for 63 days. The strength
ture was dried, sieved, and uniaxially pressed at an applied pressure of the samples subjected to acid or base solution was compared
of 40 MPa. The samples were sintered at 850 C for 2 h with a heat- with an identical unexposed sample (SC10). The glass frit compo-
ing rate of 3 C/min in air without an applied pressure. The number sition in the neck areas after 63-days exposure in an acid or base
after SC denotes the particle sizes of the SiC powders, e.g., SC10 and solution was analyzed using energy dispersive spectroscopy (EDS,
SC65 represent the SiC membrane supports prepared from 10 m JSM-6010PLUS/LA, JEOL, Tokyo, Japan) and compared to that of the
and 65 m SiC powders, respectively. identical, unexposed sample.
The bulk densities of the SiC membrane supports were cal-
culated from the weight-to-volume ratios of the samples. The 3. Results and discussion
porosities of the SiC membrane supports were measured using
Archimedes method. The crystalline phases in the sintered spec- XRD analysis was performed to identify the phases present in
imens were characterized by X-ray diffraction (XRD; D8 Discover, the SiC membrane supports sintered with 1025 wt% glass frits at
Bruker AXS GmbH, Karlsruhe, Germany) of the crushed powders 850 C for 2 h in air. XRD patterns of the SiC membrane supports sin-
using Cu K radiation. tered with 15 wt% glass frit are shown in (Fig. 1). Those of the other
The fracture surface morphology was observed using scanning supports with 10, 20, and 25 wt% glass frit were almost the same for
electron microscopy (SEM, S4300, Hitachi Ltd., Hitachi, Japan). For corresponding specimens in Fig. 1. The glass frit was an amorphous
the exural strength measurements, bar-shaped samples were cut material with no crystallization product after heat-treatment at
to a size of 3 4 35 mm3 and bending tests were performed at a 850 C for 2 h and furnace cooling. All membrane supports consisted
constant crosshead speed of 0.5 mm/min using a three-point bend- of -SiC (6H) and a trace of SiO2 (-cristobalite), which is an oxi-
ing xture with a span of 30 mm. dation product of SiC powders from sintering in air. The intensities
The open porosity and pore size distribution of SiC membrane of the -cristobalite peaks increased with decreasing SiC particle
supports were measured using mercury porosimetry (AutoPore size because of the accelerated oxidation of ner powders at the
IV 9500, Micromeritics, Norcross, GA, USA). The air ux of some sintering temperature.
selected specimens was measured by capillary ow porosimetry Fig. 2 shows the typical microstructures of the SC10 spec-
(CFP-1200-AEL, Porous Materials Inc., Ithaca, NY, USA). The speci- imens with 1025 wt% glass frit. The microstructures show
mens (25 mm in diameter and 3.5 mm thick) were tted between well-developed pore structures in all specimens. Most of the pores
O-rings in the bottom of the chamber and the bottom of the cham- originated from the inter-particle spaces in the green compact.
ber was inserted for capillary ow porosimetry. The ux was then Comparison of Fig. 2(a) and (d) clearly shows that the addition
measured automatically by sensors while incrementally changing of more glass frit produced thick bonding areas and the lling of
the pressure of the regulator. The gas permeability () was com- smaller pores. The glass-bonding phase in the present specimen is
Please cite this article in press as: S.C. Kim, et al., Processing and properties of glass-bonded silicon carbide membrane supports, J Eur
Ceram Soc (2016), http://dx.doi.org/10.1016/j.jeurceramsoc.2016.11.019
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Fig. 2. Typical microstructures of SiC membrane supports prepared from 10 m SiC powders with variation of glass frit content: (a) 10 wt%, (b) 15 wt%, (c) 20 wt%, and (d)
25 wt%.
Fig. 3. Pore size distributions of SC10 specimens with various glass frit content: (a) 10 wt%, (b) 15 wt%, (c) 20 wt%, and (d) 25 wt%.
formed by the following procedure: (1) the glass frit transforms SC10 with 20 wt% and 25 wt% samples showed bimodal pore size
into a viscous glass phase during sintering at 850 C; (2) oxida- distributions (Fig. 3(c) and (d)). The average pore size of the SC10
tion of SiC during sintering in air leads to the formation of the supports with 10, 15, 20, and 25 wt% was 2.5, 3.0, 3.6, and 4.2 m,
cristobalite phase (as conrmed by XRD (Fig. 1)); (3) the oxidation- respectively. Thus, the addition of glass frit in excess of 15 wt% led
derived SiO2 partially dissolves into the viscous glass phase; (4) to partial lling of the pores (Fig. 2(c) and (d)) and resulted in the
the glass phase results in bonding between SiC particles and par- bimodal pore size distribution (Fig. 3(c) and (d)), and an increase in
tially lls smaller pores in the membrane supports. The pore size average pore size.
of the SiC membrane supports increased with increasing glass frit Fig. 4 shows the effect of SiC particle size on the microstructure
content (Fig. 3). The SC10 with 10 wt% and 15 wt% samples showed of the SiC membrane supports with 15 wt% glass frit. As shown
unimodal pore size distributions (Fig. 3(a) and (b)). In contrast, the in Fig. 4, the increase in SiC particle size increased the pore size
Please cite this article in press as: S.C. Kim, et al., Processing and properties of glass-bonded silicon carbide membrane supports, J Eur
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Fig. 4. Typical microstructures of SiC membrane supports prepared from different SiC powders with 15 wt% glass frit: (a) 10 m, (b) 23 m, (c) 35 m, and (d) 65 m.
Fig. 5. Porosity of SiC membrane supports as a function of glass frit content. The SiC Fig. 6. Flexural strength of SiC membrane supports as a function of glass frit content.
membrane supports were sintered at 850 C for 2 h in air. The SiC membrane supports were sintered at 850 C for 2 h in air.
Please cite this article in press as: S.C. Kim, et al., Processing and properties of glass-bonded silicon carbide membrane supports, J Eur
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Fig. 8. Air ux of SiC membrane supports prepared from different SiC powders with
Fig. 7. Flexural strength of SiC membrane supports sintered at 850 C for 2 h in air 15 wt% glass frit as a function of the average pressure across the membrane supports.
as a function of porosity.
(1) The exural strength generally increased with increasing 3655% porosity [23] and 65 MPa at 40% porosity [22]. The ex-
porosity, except the SiC membrane supports with 10 wt% glass ural strength of sodium borate-bonded SiC ceramics was 37 MPa
frit (data in a circle). This trend is very unusual in porous SiC at 52% porosity [26]. The exural strength of cordierite-bonded
ceramics because the exural strength of porous SiC ceramics porous SiC membrane supports was 49 MPa at 38% porosity [27].
generally decreases with increasing porosity [21,22,25,33]. The exural strength of recrystallized SiC ceramics was 45 MPa at
(2) The exural strength increased in the order of 47% porosity [18]. The exural strengths of SiC hollow ber mem-
SC10 > SC23 > SC35 > SC65, indicating that the exural strength branes with inner and outer diameters of 0.8 and 2.0 mm were
of glass-bonded SiC ceramics is primarily dependent on pore 3040 MPa [10]. The exural strength of glass-bonded SiC ceramics
size rather than the porosity in the porosity range of 3746%. with 5 wt% glass frit was 23 MPa at 46% porosity [30]. The ex-
(3) The deviation from the trend, i.e., low strength of SiC mem- ural strengths obtained in SC10 and SC23 specimens with 15 wt%
branes with 10 wt% glass frit (data in a circle), was due to glass frit were 81 and 75 MPa, respectively. The superior strength of
incomplete bonding of SiC grains caused by insufcient glass these glass-bonded SiC membrane supports was attributed to the
frit content. homogeneous microstructure of the membrane supports (Fig. 4)
and formation of strong bonding between SiC and the present glass
According to models proposed by Gibson and Ashby [34] and frit, which was obtained by optimizing the glass frit content and
by Rice [35], the exural strength of porous SiC ceramics decreases glass frit composition.
with increasing porosity. Both models do not expect any depen- Fig. 8 shows the specic ow rate of SiC membrane supports sin-
dence of the strength on pore size, but a variation only with the tered at 850 C for 2 h in air. The specic ow rate of the SC10, SC23,
porosity of the porous ceramics. However, our results (Fig. 7) SC35, and SC65 samples with 15 wt% glass frit at a P of 15 psi were
showed that the strength of glass-bonded SiC supports did not fol- 7.2, 13.4, 16.7, and 34.0 L/min/cm2 , respectively. The ow rate of
low the above models. The average pore sizes of the supports with the glass-bonded SiC membrane supports increased with increas-
15 wt% glass frit were 3.0 m for SC10, 6.3 m for SC23, 7.9 m for ing SiC particle size in the initial composition. The porosities of
SC35, and 12.1 m for SC65, respectively. The exural strength and SC10, SC23, SC35, and SC65 samples were 45%, 42%, 42%, and 38%,
porosity of the SC10, SC23, SC35, and SC65 supports with 15 wt% respectively. In contrast, the average pore sizes of SC10, SC23, SC35,
glass frit were 81 MPa and 45%, 75 MPa and 42%, 71 MPa and 41%, and SC65 samples were 3.0, 6.3, 6.9, and 8.2 m, respectively. Thus,
and 65 MPa and 38%, respectively. The pore size of glass-bonded the SC65 has a lower porosity (38%) and larger pore size (8.2 m)
SiC supports increased with increasing the SiC particle size when than SC10 (45%, 3.0 m). SC65 showed a higher specic ow rate
the same amount of glass frit was added. In contrast, the porosity (34.0 L/min/cm2 and 63.1 L/min/cm2 at a P of 15 psi and 30 psi,
decreased with increasing the SiC particle size. respectively) than SC10 (7.2 L/min/cm2 and 21.0 L/min/cm2 at a P
Our results showed that the strength of glass-bonded SiC sup- of 15 psi and 30 psi, respectively). These ndings indicate that, in
ports increased with decreasing the SiC particle size, i.e., pore size the porosity range of 3845%, the specic ow rate of the glass-
at the same amount of glass frit. These results can be explained bonded SiC supports is primarily dependent on pore size rather
in terms of (i) an increase in strut strength with decreasing the than porosity.
pore-to-pore distance when smaller particles were used for a given The permeabilities of SC10, SC23, SC35, and SC65 were
amount of frit and (ii) a decrease in the critical aw size when 0.24 1012 m2 , 0.42 1012 m2 , 0.52 1012 m2 , and
smaller particles were used [36]. Thus, the exural strength of 1.04 1012 m2 , respectively. Song et al. [37] reported permeabil-
glass-bonded SiC supports was inuenced by pore size as well as ity values in the range of 0.13-0.82 1012 m2 for macroporous SiC
porosity. However, the exural strength of glass-bonded SiC ceram- ceramics with a 6875% porosity range. Eom et al. [38] reported
ics is primarily dependent on pore size rather than the porosity in permeability values in the range of 0.411.89 1012 m2 for macro-
the porosity range of 3746%. Similar trends were also observed in porous SiC ceramics with a porosity of 55.658.4%. Ding et al. [20]
porous liquid phase sintered SiC ceramics [36]. reported permeability values in the range of 0.20.9 1012 m2
There are several reports showing the mechanical properties of for macroporous mullite-bonded SiC ceramics with a porosity
SiC membrane supports. The exural strengths of mullite-bonded of 4557%. Although the processing temperature of the present
SiC ceramics were 314 MPa at 4654% porosity [21], 24 MPa at glass-bonded SiC membrane supports (850 C) was much lower
43% porosity [19], and 37 MPa at 48% porosity [29]. The ex- that the processing temperatures of both macroporous SiC ceram-
ural strengths of silica-bonded SiC ceramics were 630 MPa at ics (17501950 C) [37,38] and the mullite-bonded SiC ceramics
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and 40% degradation of its strength after 63 days of exposure in pH 3 SC10-15 28.74 30.36 38.92 1.18 0.53 0.18 0.07 0.02
and 11 solutions, respectively. To understand the cause of degrada- SC10-15-pH3 29.65 27.08 42.23 0.64 0.26 0.10 0.03 0.01
SC10-15-pH11 27.51 28.99 42.62 0.54 0.24 0.06 0.03 0.01
tion on exural strength, the compositions of bonding areas in the
fracture surfaces were analyzed using EDS after 63 days of exposure
in pH 3 and 11 solutions (Fig. 10) and the results are summarized in
modier in the bonding glass. The weight losses of the SC10-15-pH3
Table 1. As shown in Table 1, the content of alkali (Na, K) and alka-
and SC10-15-pH11 specimens were 0.29 wt% and 0.97 wt%, respec-
line earth (Ca, Ba) elements decreased after 63 days of exposure in
tively, after 63 days of exposure in both pH 3 and pH 11 solutions.
both pH 3 and 11 solutions. Those elements play a role as a glass
The weight loss in the pH 11 solution was greater than that in pH
Fig. 10. Scanning electron micrograph images of glass-bonded SiC membrane supports: (a) SC10 specimen with 15 wt% glass frit (SC10-15), (b) SC10-15 after 63 days of
exposure in a pH 3 solution (SC10-15-pH3), and (c) SC10-15 after 63 days of exposure in a pH 11 solution (SC10-15-pH11). The cross denotes the spot analyzed using EDS
with a spatial resolution of 1 m.
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Korean Ceram. Soc. 46 (2009) 488492.
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