Ceramics International 46 (2020) 22797–22804

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Ceramics International
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3D printing of porous SiC ceramics added with SiO2 hollow microspheres T

a b,c,∗ a a b a a
Xiaomei Sun , Tao Zeng , Yikai Zhou , Kun Zhang , Guodong Xu , Xiaohong Wang , Su Cheng
a
School of Materials Science and Engineering, Harbin University of Science and Technology, Harbin, 150080, PR China
b
Department of Civil and Environmental Engineering, College of Engineering, Shantou University, Shantou, 515063, PR China
c
Intelligent Manufacturing Key Laboratory of Ministry of Education, Shantou University, Shantou, 515063, PR China

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

Keywords: Porous SiC ceramics were fabricated by 3D printing through selective laser sintering (SLS) and adding hollow
Porous materials spheres (AHS). The process was based on the mullitization of Al2O3 and kaolin, and the SiC particles were
3D printing bonded by the mullite and melted SiO2. The pores were produced by the stacking of SiC particles, debonding of
Adding ceramic hollow spheres epoxy, and adding of SiO2 hollow microspheres. The phase composition, microstructure, porosity, and flexural
Ceramics
strength of the porous SiC ceramics with and without SiO2 hollow microspheres were compared. Additionally,
the effect of the sintering temperature, size, and mass fraction of the SiO2 hollow microspheres on the porous SiC
ceramics was investigated. After the addition of the SiO2 hollow microspheres, an open porosity of 62.51% and
flexural strength of 40.93 MPa were obtained for the porous SiC ceramics. Using the results, three types of
hierarchically porous SiC structures with porosities ranging from 92–97% were manufactured by SLS combined
with AHS.

1. Introduction selective laser sintering (SLS) [24]. Although most of these were
adopted to fabricate dense ceramic parts, direct ink writing can also be
Silicon carbide (SiC) ceramics are promising candidates for high- used to prepare porous ceramics [25,26], especially hierarchical porous
temperature applications because of their good thermal stability, high structures [27,28]. However, the large deformation after printing and
temperature resistance, and excellent anti-oxidation properties [1]. weak bonding between extrusion lines hinders the actual application of
Additionally, porous SiC ceramics have recently attracted increasing direct ink writing in the preparation of porous ceramic parts.
attention owing to their low density, high specific strength, low thermal However, some researchers have used the SLS technology to fabri-
conductivity, and large surface area [2–4]. They have been used in cate porous ceramics. Subramanian et al. [29] manufactured porous
many industrial applications, such as catalyst carriers [5], hot gas filters Al2O3 ceramics using Al as a binder. The porosity of the sintered Al2O3
[6,7], membrane supports [8], and biological bones [9]. Different ceramics was over 60%. Yao et al. [30] fabricated porous Al2O3 using
methods have been used to fabricate porous ceramics, such as pore- indirect SLS and Al reaction bonding. Recently, Chen et al. [31,32]
forming agent addition [10,11], particle stacking [12], foaming [13], manufactured highly porous mullite ceramic foams by SLS. Liu et al.
and freeze-drying [14]. Adding ceramic hollow spheres (AHS) is a [33] prepared highly porous Al2O3 ceramic foams using SLS on Al2O3
modified pore-forming agent addition method that has been developed poly-hollow microspheres. Dong et al. [34] manufactured porous Al2O3
recently [15–17]. In contrast with the conventional methods, AHS al- ceramics with high porosity and strength by SLS. The effect of Al ad-
lows the porosity of the ceramics to be controlled and improves their dition on the microstructure and mechanical properties of the fabri-
mechanical properties. However, because of their inherent brittleness cated porous Al2O3 ceramics was also investigated.
and high hardness, complex porous ceramic parts are difficult to fab- In this work, a novel method is proposed to fabricate porous SiC
ricate by AHS, which inhibits the wide application of this method [18]. ceramics combining SLS and AHS. SLS was used to print the body of
Three-dimensional (3D) printing is a promising technique that has ceramic parts with complex shapes. The addition of SiO2 hollow mi-
been recently applied to prepare complex ceramic parts. Many 3D crospheres not only increased the porosity of the materials but also
printing technologies were proposed to fabricate ceramics, such as strengthened the bonding of the SiC particles. The effects of the sin-
fused deposition modeling [19], stereolithography [20], inkjet printing tering temperature, diameter, and mass fraction of the SiO2 hollow
[21], laminated object manufacturing [22], direct ink writing [23], and microspheres on the microstructure, porosity, and flexural strength of

∗
Corresponding author. Department of Civil and Environmental Engineering, College of Engineering, Shantou University, Shantou, 515063, PR China.
E-mail address: [email protected] (T. Zeng).

https://doi.org/10.1016/j.ceramint.2020.06.047
Received 1 April 2020; Received in revised form 23 May 2020; Accepted 4 June 2020
Available online 09 June 2020
0272-8842/ © 2020 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
X. Sun, et al. Ceramics International 46 (2020) 22797–22804

Table 1
Chemical composition of kaolin.
Content (wt.%)

Al2O3 SiO2 Na2O Others

44.00 54.00 1.45 0.55

Table 2
Size and mass content of the SiO2 hollow microsphere.
Specimen code Mass content Diameter (μm) Open Flexural
(wt.%) porosity (%) strength (MPa)

S0 0 / 44.99 61.93
S5-50 5 50 46.41 46.42
S10-50 10 50 62.51 40.93
S15-50 15 50 60.43 33.13
S20-50 20 50 64.79 37.13
S10-40 10 40 50.99 39.28
S10-60 10 60 63.34 14.83

Fig. 3. XRD patterns of the porous SiC ceramics fabricated at different sintering
temperatures.

fabrication of the ceramics. Al2O3 (99.9%, Yuejiang Co., Ltd.,

Guangdong, China) and kaolin powder (Shuolong Co., Ltd., Hebei,
China) were selected as sintering additives. The chemical composition
of kaolin is shown in Table 1. SiO2 hollow microspheres (Sinosteel Co.,
Ltd., Anhui, China) with size ranging from 40 μm to 60 μm and an
average wall thickness of 1 μm were used as the pore-forming agent. In
SLS, E12 epoxy powder (D50 = 5 μm, Xinxi Co., Ltd., Guangdong,
China) was selected as a binder.

2.2. Preparation of the samples

The printing powders used in SLS were prepared by blending SiC

particles with kaolin, Al2O3, epoxy powders, and SiO2 hollow micro-
spheres for 12 h using a tumbling mixer. The mass ratio of SiC, kaolin,
Al2O3, and epoxy in the printing powders is 6.5:1.5:1.5:0.5. To in-
Fig. 1. Micrograph of the printed sample with SiO2 hollow spheres.
vestigate the effect of the SiO2 hollow microspheres on the porosity and
flexural strength of the porous SiC ceramics, seven groups of printing
powders with different mass fractions (0, 5, 10, 15, and 20 wt%) of SiO2
hollow microspheres of different sizes (40, 50, and 60 μm) were pre-
pared, as shown in Table 2.
The printing powders were processed into printed bodies by an SLS
machine (Wuhan Huake 3D Technology Co., Ltd., China). The SLS
processing parameters were optimized in our previous work [35]. The
main parameters were a laser power of 18 W, scanning velocity of
3600 mm/s, layer thickness of 0.1 mm, scanning spacing of 0.15 mm,
and preheating temperature of 55 °C. During SLS process, the SiO2
hollow spheres were dispersed in the printed samples and retained their
original morphologies. Fig. 1 shows the micrograph of the printed
sample with SiO2 hollow spheres.
After SLS, the printed parts were first heated in air at 600 °C for 1 h
to increase their strength and reduce their close porosities. Then, the
parts were heated in air at a heating rate of 3 °C/min and maintained at
the sintering temperature for 3 h to obtain porous SiC preforms.

Fig. 2. TG curve of the E12 epoxy resin. 2.3. Characterization

The oxidation behavior of the epoxy powder in the air was eval-
the porous SiC ceramics were investigated.
uated by thermogravimetry analysis (TG, STA 409, Netzsch, Germany).
A scanning electron microscope (SEM, JSM-5600LV, Japan) was used to
2. Experimental procedures characterize their morphology. The bulk densities and open porosities
of the porous SiC materials were measured through the Archimedes'
2.1. Raw materials method. Both micro and macro pores were considered in the hier-
archically porous SiC structures. The porosity of the micro pores was
SiC powder (D50 = 37.3 μm, Shantian Co., Ltd.) was used for the measured through Archimedes’ method and that of the macro scale was

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Fig. 4. SEM micrographs of the porous SiC ceramics fabricated at different sintering temperatures: (a) 1200 °C, (b) 1300 °C, (c) 1400 °C, (d) 1500 °C.

Fig. 5. Pore size distribution of porous SiC ceramics prepared at different sintering temperatures: (a) 1200 °C, (b) 1300 °C, (c) 1400 °C and (d) 1500 °C.

predicted. The pore size distribution was determined through analysis 36 mm × 4 mm × 3 mm. Five samples were tested for each group.
of SEM pictures by Image Pro Plus software. The phase and composition
of the samples were characterized by X-ray diffraction (XRD, D/max-γB, 3. Results and discussion
Rigaku, Japan). Three-point bending tests were carried out using a
universal testing machine (INSTRON 3382) with the displacement rate 3.1. Optimization of the sintering temperature
of 0.5 mm/min in accordance with ISO 14704-2000 [36]. The span of
the supports was 30 mm and the size of the samples was Fig. 2 shows the TG curve of the E12 epoxy for a heating rate of

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2 °C/min. As seen, the oxidation begins at 350 °C and completes at

600 °C. Thus, a slow heating rate should be used between these tem-
peratures to avoid the collapse of the green parts while the epoxy
binder burns.
To optimize the sintering temperature, the composition, micro-
structure, porosity, density, and flexural strength of the samples
without SiO2 hollow microspheres were investigated at different tem-
peratures. Fig. 3 shows the XRD patterns of the sintered porous SiC
samples. As observed, the degree of mullitization increased with in-
creasing sintering temperature. No mullite peak was detected in the
XRD pattern of the sample sintered at 1200 °C. When the sintering
temperature increased to 1300 °C, a strong mullite peak was observed,
indicating that mullitization occurred. The mullitization reaction can
strengthen the bonding between the SiC particles. As the sintering
temperature further increased to 1400 °C, the mullite peak strength-
ened, which implies that the mullitization intensified. Additionally, the
Al2O3 peak decreased as the sintering temperature increased. This also
indicates that the degree of mullitization increased. It is also observed
from Fig. 3 that the SiC peak decreased and the SiO2 one increased as
the sintering temperature increased. This is attributed to the oxidation
of the SiC particles accelerating because of the higher temperature.
In the sintered porous ceramic samples, the pores originated from
the stacking of the SiC particles, burnout of the epoxy binder, and
mullitization. Since the size of the epoxy powder is much smaller than
that of SiC, the size of the pores caused by the epoxy burnout should be
smaller than that caused by the SiC particle stacking. Fig. 4 shows the
microstructures of the porous SiC ceramics prepared at different tem-
peratures. A loose structure with a rough fracture surface was observed
in the sample sintered at 1200 °C (Fig. 4(a)). This indicates that the
mullitization was insufficient at this temperature. Fig. 4(b) shows the
fractural morphology of the porous SiC sample prepared at 1300 °C.
Compared with the sample prepared at 1200 °C, the fracture surface of
this sample is clearer, displaying smaller pores. The main reason is that
a higher sintering temperature promotes the formation of mullite, be-
cause more liquid phase is generated. The pores decreased in size be-
cause the liquid phase filled in. This is consistent with the analysis of
Fig. 6. Effects of sintering temperature on the (a) porosity and (b) flexural the pore size distributions for the samples sintered at different tem-
strength of the porous SiC ceramics. peratures in Fig. 5. It is observed that the porous SiC sample prepared at

Fig. 7. SEM micrographs of the porous SiC ceramics with different sizes of SiO2 hollow microspheres: (a) 40 μm, (b) 50 μm, (c) 60 μm, and (d) magnification of (b).

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Fig. 8. (a) Porosity, flexural strength and pore size distribution of the porous SiC ceramics with different sizes of SiO2 hollow microspheres: (b) 40 μm, (c) 50 μm and
(d) 60 μm.

1300 °C exhibited smaller average pores (1.8–5.1 μm) than the other 10 wt% and sintering temperature of 1300 °C. Fig. 7 shows the mi-
samples. An excessive sintering temperature is harmful to the me- crographs of the samples having SiO2 hollow microspheres of different
chanical properties of porous SiC ceramics because of the oxidation of sizes (40 μm, 50 μm, and 60 μm). The samples with smaller (40 μm or
the SiC particles, which generates CO, CO2, or both gases at high 50 μm) SiO2 hollow microspheres have compact structures while that
heating temperatures [11], through the reactions with larger (60 μm) SiO2 hollow microspheres has a loose structure due
to the larger pores generating in the sintering process. Fig. 7(d) is the
SiC + (3/2) O2 → SiO2 + CO  (g ) (1)
enlargement of Fig. 7(b). It is found that the pores derived from SiO2
SiC + 2O2 → SiO2 + CO2  (g ) hollow spheres are smooth while that caused by the stacking of SiC
(2)
particles have sharp shapes. As seen in Fig. 7(d), SiO2 hollow spheres
Then, the gases caused more pores in the samples. did not remain their original shapes due to the mullitization in the post-
Fig. 6(a) depicts the open porosity and bulk density of the samples sintering process. Fig. 8 shows the open porosity, flexural strength and
sintered at different temperatures. When the sintering temperature in- pore size distributions of the samples prepared with 40–60 μm SiO2
creased from 1200 °C to 1500 °C, the open porosity decreased from hollow microspheres. Fig. 8(a) shows the open porosity remarkably
46.43% to 42.92%, whereas the density increased from 1.38 g/cm3 to increased from 50.99% to 62.51% with the increase of the microsphere
1.41 g/cm3. Fig. 6(b) shows the flexural strength of the samples sin- diameter from 40 μm to 50 μm. Then, it increased slightly when the
tered at different temperatures. It can be seen that the flexural strength microsphere diameter further increased to 60 μm. Fig. 8(b)-(d) shows
first increased with increasing sintering temperatures. After reaching the pore size distributions for the sintered samples with 40–60 μm SiO2
the maximum of 61.93 MPa at a sintering temperature of 1300 °C, it hollow microspheres. The sintered samples with 40 μm SiO2 hollow
decreased. This is attributed to both mullitization and SiC oxidation. microspheres possessed smaller pore size distribution. The number of
When the sample was sintered at 1200 °C, mullite was only partly the larger pores in the sintered samples increased as the diameter of the
formed and the other phases were amorphous. After further increasing SiO2 hollow microspheres increased. Fig. 8 also shows the flexural
the sintering temperature to 1300 °C, the mullite crystals grew from strength of the samples prepared with 40–60 μm SiO2 hollow micro-
amorphous phases, and the mullite phase formation was almost com- spheres. The samples with 40 μm or 50 μm SiO2 hollow SiO2 micro-
pleted at 1400 °C. However, the SiC particles were gradually oxidized as spheres have almost the same flexural strength of approximately
the sintering temperature increased, especially above 1300 °C, gen- 40 MPa. This sharply decreased to 14.83 MPa as the diameter increased
erating a large number of pores and reducing the strength of the sam- to 60 μm. The results are summarized in Table 2.
ples. From the above investigations, it is concluded that the optimal
sintering temperature is 1300 °C. 3.3. Effect of the content of SiO2 hollow microspheres

3.2. Effect of the size of the SiO2 hollow microspheres The microstructure and properties of the porous SiC samples were
investigated as a function of the mass fraction of SiO2 hollow micro-
The effect of the size of the SiO2 hollow microspheres on the mi- spheres. The sintering temperature and diameter of the SiO2 hollow
crostructure, porosity, and flexural strength of the sintered porous SiC microspheres for the tested samples were 1300 °C and 50 μm, respec-
samples was investigated using a fixed microsphere mass fraction of tively. Fig. 9 shows the micrographs of the samples prepared with

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Fig. 9. SEM micrographs of the porous SiC ceramics with different mass fractions of SiO2 hollow microspheres: (a) 0 wt%, (b) 5 wt%, (c) 10 wt%, (d) 15 wt% and (e)
20 wt%.

0–20 wt% SiO2 hollow microspheres. It is observed that the structures hierarchically porous SiC structures with porosities of 92–97% were
of the samples with 0–10 wt% SiO2 hollow microspheres are compact fabricated by SLS with the addition of SiO2 hollow microspheres
and then those with larger mass fraction of the SiO2 hollow micro- (Fig. 11). Thus, the combination of SLS and AHS shows great potential
spheres are loose. for preparing highly porous ceramic structures with complex shapes
Fig. 10 shows the open porosity, flexural strength and pore size that can have industrial applications.
distributions of the samples prepared with 0–20 wt% SiO2 hollow mi-
crospheres. It is found from Fig. 10(a) that the open porosity of the
samples increased from 44.99% to 62.51% as the mass fraction of SiO2 4. Conclusions
hollow microsphere increased from 0 wt% to 10 wt%, subsequently
stabilizing at approximately 60%. Fig. 10(b)-(f) shows the pore size A method was proposed for preparing SiC porous ceramics by
distributions for the sintered samples with 0–20 wt% SiO2 hollow mi- combining the SLS technology with the addition of SiO2 hollow mi-
crospheres. The main pore size for all the samples is 1.8–9.8 μm, whose crospheres. It was found that sufficient mullitization occurs at a tem-
percentage is over 80%. Fig. 10 also shows the flexural strength of the perature of 1300 °C, strengthening the bonding between the SiC par-
samples prepared with 0–20 wt% SiO2 hollow microspheres. The flex- ticles. The flexural strength of the porous SiC ceramics increases with
ural strength decreased as the mass fraction of the SiO2 hollow micro- the increases in sintering temperature. However, an excessive sintering
spheres increased. Compared with the samples without SiO2 hollow temperature reduces the strength of porous SiC ceramics because of the
microsphere, the flexural strength of the sample with 10 wt% SiO2 oxidation of the SiC particles. Additionally, it was found that the size
hollow microspheres decreased by approximately 30%. However, the and mass fraction of the added SiO2 hollow microspheres have a great
flexural strength of the sample with 15 wt% SiO2 hollow microspheres influence on the porosity and mechanical properties of the porous SiC
decreased by nearly 50%, from 61.93 MPa to 33.13 MPa. ceramics. As the size of the SiO2 hollow microspheres increases, the
Based on the above measurements, it is concluded that the sample open porosity of the samples first increases and then stabilizes. The
sintered by adding 10 wt% SiO2 hollow microspheres of size 50 μm flexural strength of the sample when the size of the added SiO2 hollow
exhibits the best mechanical properties and high porosity. Using the microspheres is 40 μm or 50 μm is much higher than when it is 60 μm.
optimized components and process parameters, three types of When the mass fraction of the SiO2 hollow microspheres increases from
0 wt% to 20 wt%, the open porosity increases and the flexural strength

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Fig. 10. (a) Porosity, flexural strength and pore size distribution of the porous SiC ceramics with different mass fractions of SiO2 hollow microspheres: (b) 0 wt%, (c)
5 wt%, (d) 10 wt%, (e) 15 wt% and (f) 20 wt%.

Fig. 11. (a) Schematic diagrams and (b) photographs of macro-micro hierarchically porous SiC structures prepared by SLS and AHS.

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