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A novel approach to fabricate porous alumina ceramics with excellent

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DOI: 10.1016/j.ceramint.2018.06.106

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 Ceramics International 44 (2018) 16751–16757

Contents lists available at ScienceDirect

Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

A novel approach to fabricate porous alumina ceramics with excellent T

properties via pore-forming agent combined with sol impregnation
technique
⁎
Jingjing Liua, Wenlong Huoa, Bo Rena, Ke Gana, Yuju Lua, Xiaoyan Zhanga, Xinyue Tangb, ,
⁎
Jinlong Yanga,
a
State Key Laboratory of New Ceramics and Fine Processing, School of Materials Science and Engineering, Tsinghua University, Beijing 100084, PR China
b
School of Materials Science and Engineering, Dalian Jiaotong University, Dalian 116028, PR China

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

Keywords: An innovative approach for fabricating porous alumina ceramics (PACs) with improved mechanical and thermal
Walnut shell powders properties using walnut shell powders as pore-forming agent combined with alumina sol impregnation is re-
Porous alumina ceramics ported in the present work. It is demonstrated that uniform distribution of spherical pores can be observed in as-
Alumina sol particles prepared PACs by using above technical route. The decrease of walnut shell powder sizes significantly promotes
Mechanical properties
the enhancement of crushing strength and reduction of thermal conductivity of the PACs. Meanwhile, the im-
Thermal conductivity
pregnated alumina sol is favoring for the formation of spherical micro-pores, then further improves their me-
chanical and thermal insulation performances. The lowest thermal conductivity and highest crushing strength of
resulting sample reach 0.16 W/m K and 29.2 MPa, respectively. This novel method offers new possibilities to
fabricate high-quality PACs.

1. Introduction
Porous alumina ceramics (PACs) are used widely in filtration,
thermal insulators and catalyst fields due to their low thermal con-
ductivity, high melting point and chemical stabilities [1–5]. As for
furnace thermal insulators, alumina hollowsphere bricks are currently
applied owing to their excellent mechanical properties. However, the
relative high thermal conductivity and energy-intensive fabrication
process make them unable to satisfy the ever-increasing request of
modern industry [6,7]. Therefore, it is of great importance to develop a
novel and low-cost PACs with excellent insulation performance and
mechanical strength simultaneously.
Thus far, various methods are employed for preparing alumina or
alumina-based ceramics, including foam-gelcasting [8], sacrificial
templating [9,10] and pore-forming agent (PFA) [11–13]. The last
method is widely used to fabricate porous samples with high porosity or
complex shape because of its simple preparation procedure and high
controllability [14,15]. In addition, the pore structures of porous
ceramics are intrinsically relate to the morphology and elasticity of
PFA, which would largely affect their performances. The traditional
PFA employed to prepare PACs mainly including sawdust [16], rice
husk [17] and polymethylmethacrylate (PMMA) microspheres [18],
etc. Nevertheless, these traditional PFA present some obstacles in pre-
paring porous products with less defect and good materials homo-
geneity due to the considerable spring back effect caused by their high
elasticity [19,20]. Furthermore, the impurities after burn-out may also
deteriorate the high-temperature performances of porous ceramics.
Other than traditional high elasticity PFA, rigid PFA including ceramic
hollow microspheres [21,22] and other particles [23], etc., have been
developed to prepare high performance porous ceramics. In comparison
with high elasticity PFA, rigid PFA exhibits many advantages, namely
low elasticity, low toxicity and effective compatibility with ceramic
paste. Nevertheless, low porosity (about 45–60%) and complex pre-
paration processing are the drawbacks to limit their further application,
thus many researchers have focused on the exploitation of facile, low
cost, and eco-friendly fabrication method in recent years [24,25].
Walnut shell powder is a natural organic matter possessing non-
toxicity after burning and significant level of organics, which has been
widely applied in the filterable, medical and catalytic fields [26,27].
However, the irregular pores after burn-out still present a challenge for
its wider application. To address this problem, in the present work, four
different sizes of walnut shell powders were introduced as the PFA of
PACs. Based on our previous work [28], alumina sol was introduced in
this work during the preparation of PACs to modify the pore structure

⁎
Corresponding authors.
E-mail addresses: txy19942016@163.com (X. Tang), jlyang@mail.tsinghua.edu.cn (J. Yang).

https://doi.org/10.1016/j.ceramint.2018.06.106
Received 31 May 2018; Received in revised form 12 June 2018; Accepted 12 June 2018
Available online 03 July 2018
0272-8842/ © 2018 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
J. Liu et al. Ceramics International 44 (2018) 16751–16757

Table 1
Element compositions of walnut shell powders.
Walnut shells C O Si K Na Ca Other

Mass fraction 64.38 33.85 0.164 0.532 0.140 0.197 0.737

and improve the performance of PACs. The effects of walnut shell

powders sizes on the pore size, pore proportions and pore morphology
were investigated systematically. Also, the roles of pore structures on
thermal conductivity and mechanical properties of PACs were analyzed.

2. Experimental procedures

2.1. Preparation of PACs

Tabular alumina (≤ 74 µm and ≤ 45 µm, Qingdao, China), α-Al2O3

(2 µm, Qingdao, China) and ρ-Al2O3 (5 µm, Zhengzhou, China) were
used as starting materials in this work. Four different sizes of walnut
shell powders (WS, 45 µm; 22 µm; 13 µm and 7 µm, Shijiazhuang,
China) were chosen as PAF and their added volume percentage were
almost same to ensure the same porosity of fired samples. The chemical
compositions of walnut shell powder were listed on Table 1. Poly vinyl
alcohol (PVA), one in liquid form (5 wt% solid content, Beijing, China)
and commercial alumina sol (5 wt% solid content, Handan, China) were
adopted as binder and coating compositions. Fig. 1 gives the micro-
structures of walnut shell powders and alumina sol particles. As can be
seen that the walnut shell powders exhibit irregular morphology with
various sizes, and the alumina sol present perfect spherical particles.
Fig. 2 illustrates the detailed process for fabricating the PACs. Firstly,
the ceramic pastes consisting of tabular alumina, α-Al2O3, walnut shell
powders and deionized water were added into 5 wt% PVA aqueous
solution. The obtained pastes were then put into cold isostatic pressing
mold and pressed under 5 MPa. The green bodies are pre-fired at
1400 °C at a rate of 5 °C/min for 2 h. Most of the pre-fired samples were
immediately heat up to 1600 °C at a rate of 10 °C/min. The other pre-
fired samples were sintered beforehand impregnating alumina sols
under vacuum followed by drying, as described above. Altogether, five
different types samples were obtained by varying the wall shell powder
sizes and whether the as-fired compositions were impregnated before-
hand or not (i.e., WS45: 45 µm; WS22: 22 µm; WS13: 13 µm; WS7: 7 µm
and WS7-5: 7 µm, 5 wt%).
2.2. Characterization methods
Fig. 2. Scheme depicting the experimental procedure for the porous alumina
ceramics production.
ρbulk
Vtotal = 1−
ρtrue (1)
here, Vtotal was the total porosity, ρbulk and ρtrue were the bulk density
and true density of porous alumina ceramics, respectively. Close por-
osity of the obtained alumina samples was calculated according to Eq.
(2):
Vclose = Vtotal − Vopen (2)
where Vclose was the close porosity, Vtotal and Vopen were total porosity and
open porosity of sintered samples, respectively. Microstructures were
characterized with a scanning electron microscopy (SEM, Carl Zeiss,
Jena, Germany). Pore size distribution was characterized by Mercury
Intrusion Porosimetry (Autopore IV9500, Micromeritics Instrument
Corp., USA). Pore shape factor was calculated according to Ref. [29].
Thermal conductivity with dimensions of Φ180 mm × 20 mm were
characterized using a thermal constants apparatus (PBDR-02, Pre-
condar, PR China). Cold crushing strength was determined using cy-
lindrical samples of Φ30 mm × 20 mm according to the GB-T 3997.2-
1998. More than fifteen samples were measured to obtain the average
value. Based on the crushing strength result, Weibull distribution plots
were evaluated as follows:

lnln[1/(1 − F)] = mlnσn−mlnσ0 (3)

Apparent porosity of the obtained alumina samples was measured
according to Archimedes method by distilling deionized water. Total where m was Weibull modulus, σn and σ0 were the crushing strength of
porosity was calculated according to Eq. (1): the nth bar and characteristic crushing strength, respectively.

Fig. 1. SEM micrographs of (a) walnut shell powders and (b) alumina sol particles.

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Table 2 3. Results and discussion

Porosity and bulk density of porous alumina ceramics with different walnut
shell powder sizes. 3.1. Porosity and microstructure of PACs
Properties WS45 WS22 WS13 WS7 WS7-5
Table 2 illustrates the bulk density (BD) and apparent porosity (AP)
Bulk density (g/cm3) 1.25 1.27 1.28 1.29 1.32 of the sintered samples. Apparently, decreasing of walnut shell powder
Apparent porosity (%) 68.6 67.1 66.8 65.9 59.1
sizes (WSPS) has no significant differences on their BD and AP, which is
Close porosity (%) 1.2 1.6 2.2 2.9 8.6
attributed to the incorporation of same volume percentage of walnut
shell powder, an AP value of ~ 68.6%, and a BD value of ~ 1.27 g/cm3
F = (n−0.5)/ N (4) are achieved for samples WS45, WS22, WS13 and WS7. Also, the close
porosity (CP) without obvious change are observed in those samples.
where F was the failure probability estimator, n was the ranking and N Nevertheless, the decreasing of AP and increasing of CP can be found
was the number of samples tested. easily in sample WS7-5 with impregnating 5.0 wt% alumina sol solid
content, the occurrence lied in the fact that the existence of

Fig. 3. SEM micrographs of polish surface of (a) the sample WS45, (b) WS22, (c) WS13, (d) WS7, (e) WS7-5 and (f) high magnification of WS7-5.

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Fig. 5. Thermal conductivity of samples with different walnut shell powder

Fig. 4. Pore size distribution of samples with different walnut shell powder
sizes.
sizes.

WSPS. Clearly, the thermal conductivity of all samples increase as the

nanoparticles leads to the promotion of sintering. The highest close
test temperatures increases due to air trapped in the pores accelerates
porosity of 8.6% is obtained for sample WS7-5.
the motion of air molecule [30,31]. The thermal conductivity at various
Fig. 3 shows the polished surfaces of the samples with different
temperatures is strongly dependent on the WSPS. When the WSPS is
WSPS. In case of sampleWS45, abundant elongated pores with pore size
45 µm, sample WS45 has maximum value of 0.34 W/m K. On de-
of about 60 µm (higher magnification Fig. 3a) are observed. With de-
creasing of WSPS from 45 µm to 7 µm, thermal conductivity of samples
creasing of WSPS from 45 µm to 7 µm, similar microstructures are ob-
decreases from 0.34 W/m K to 0.19 W/m K. After impregnating of alu-
served except for the decreased mean pore size. When 5 wt% alumina
mina sol, sample WS7-5 shows the lowest thermal conductivity of
sol is impregnated, more approximately spherical micro-pores with size
0.16 W/m K, suggesting that as-fabricated PACs could be a promising
of 2–10 µm are observed (Fig. 3e). Alumina nanoparticles can be ob-
thermal insulator.
served at the tip of macro-pores (see Fig. 3f). In comparison with
sample WS7, the mean pore size of sample WS7-5 exhibit an obvious
decrease, due mainly to the promotion of sintering when introduce 3.4. Mechanical properties of PACs
external nanoparticles in matrix.
The above changes of the microstructure and pore structures of
3.2. Pore structures of PACs samples must result in the differences of their mechanical properties.
Fig. 6a gives the load-displacement curves of sintered samples. Ob-
The differences in the above densification and microstructure must viously, the typical curves of porous ceramics with a long distance of
lead to a change of pore structures of the fabricated composites. The elastic region followed by fracture catastrophically are observed for all
results for pore size distribution, mean pore size and pore shape factor samples without impregnating alumina sol. However, a non-linear
measured are summarized in Fig. 4 and Table 3. Clearly, the pore size mechanical behavior up to the peak with a post-peak region appears
distributions are strongly influenced by the WSPS, and all the samples when impregnate alumina sol, which can be attributed to the promo-
appear unimodal pore size distribution. The mean pore size appears tion of pore spherification caused by addition of nano-alumina parti-
decreased trend with decreasing of WSPS, whereas the proportions cles. Due to the stochastic nature of fracture in PACs, their crushing
of < 2 µm micro-pore exhibit an opposite tendency. Thanks to the strength are statistically investigated according to the Weibull dis-
presence of the nano-sized alumina particles during sintering, the tribution analysis, and the result is shown in Fig. 7. As expected, sample
proportions of < 2 µm micro-pore in impregnated sample increases WS45 exhibits the lowest crushing strength of 8.9 MPa and smallest
from 13.35% to 19.27%. With regard to pore shape factor, a smaller Weibull moduli of 6.69, which is attributed mainly to the existence of
decrease of 3.3% is achieved in alumina sol impregnated sample in its largest pore size and irregular pore morphology. Thereafter, the
comparison with the sample WS7. The reduction in mean pore size and strength and Weibull moduli of PACs increase with decreasing of WSPS.
pore shape factor of sample WS7-5 is respond for the decrease of micro- When alumina sol is impregated, the highest crushing strength value of
pores (see Fig. 3 and Table 2). 29.2 MPa and largest Weibull moduli of 18.93 are achieved for sample
WS7-5 due to the almost spherical pore and homogenous micro-
structure. Table 4 compares physical properties of various PACs syn-
3.3. Thermal conductivity of PACs
thesized by using different methods [28,32–34]. Although the similar
porosity was performed by Liao et al. [32], the thermal conductivity in
Fig. 5 gives thermal conductivity of the samples with different
the present work is much lower (~ 36% lower) and the crushing
strength is much higher (~ 700% higher). Note that the performances
Table 3
in present work are also quite excellent comparing with alumina hol-
Pore volume intervals, mean pore size and pore shape factor of samples with
different walnut shell powder sizes.
lowsphere bricks. For example, alumina hollowsphere bricks with
porosity of 62.7% was obtained by using alumina hollow sphere as
Pore size intervals (%) Mean pore size Pore shape factor starting materials. In spite of their samples showed relative high
＜2 µm 2–22 µm ＞22 µm (μm) (a.u.)
crushing strength, their thermal conductivity is quite high (0.93 W/
m K) [28]. Some other investigators also prepare porous alumina
WS45 1.21 25.23 73.56 34.6 1.56 compositions with higher porosity (70.6% or 72.2%), however, the
WS22 6.89 46.34 46.77 24.7 1.53 higher thermal conductivity (0.50 W/m K or 1.03 W/m K) and lower
WS13 9.21 56.37 34.42 14.2 1.51
crushing strength were obtained. As a result, PACs having optical
WS7 13.35 67.39 19.21 7.1 1.48
WS7-5 19.27 68.26 12.47 4.2 1.43 thermal and mechanical properties could be readily fabricated by using
the method proposed in the present work.

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Fig. 6. Mechanical properties of samples with different walnut shell powder sizes: (a) load-displacement curves and (b) cold crushing strength.

composites. Furthermore, the impregnation of alumina sol promotes

Fig. 7. Weibull distribution plots of crushing strength for all samples.
3.5. Discussion
Based on the above experimental results, the heat transfer model for
all investigated samples is proposed and graphically present in Fig. 8.
The sample WS45 are is quite poor insulatable due to their less gas-solid
interfaces, thus leading to a short heat transfer path (Fig. 9a). Mean-
while, the thermal radiation and convection also become greater be-
cause of their large mean pore size. The decreasing of WSPS not only
decrease mean pore size of samples but also increase their gas-solid
interfaces. Consequently, their heat transfer path also become long and
the thermal insulation performances are greatly improved (Fig. 9b). The
above explanation was also confirmed by thermal conductivity result.
Although decreasing of WSPS has a positive influence on the thermal
insulation performance of sintered samples, their pore morphology also
contribute to an obvious decreasing of heat transfer and thermal ra-
diation and convection. Consequently, the lowest thermal conductivity
is achieved for sample WS7-5. Obviously, homogeneous spherical pores
are formed by nano-sized alumina particles attaching on the pore tip, as
a result longer heat transfer path can be obtained, thus restricting the
heat conduction of heat flow. On the other hand, spherical pores are
favorable for decreasing thermal radiation and convection of porous
decreasing of mean pore size, and thus increase the gas-solid interfaces
in matrix, which also extend heat transfer path and reduce thermal
radiation and convection of material. As a consequence, the lower
thermal conductivity is achieved in sample WS7-5 in comparison with
the sample WS7.
Similarly, the change of pore morphology and pore size complicates
the fraction process in samples. For the sample WS45 possessing large
pore size and irregular pore morphology, high stress concentration
around the tip of irregular pore would accelerate the initiation of crack,
thus lead to the lowest strength (Fig. 9a). A slight high fracture load can
be attained for sample WS22; meanwhile, samples containing lower
WSPS show a more fracture load, especially for the sample WS7, which
can be attributed to the increasing of load area per unit (Fig. 9b).
Thanks to the presence of spherical pores caused by impregnating
alumina sol, the crushing strength of sample WS7-5 increases from
21.2 ± 0.3 MPa to 29.2 ± 0.9 MPa. These spherical pores are favor
for decreasing of the stress concentration, which would lead to the in-
creasing of strength, as shown in Fig. 9c.
4. Conclusions
A novel approach to fabricate porous alumina ceramics using
walnut shell powders as pore- forming agent combined with alumina
sol impregnating technology has been successfully reported. The de-
creasing of walnut shell powders size promotes the reduction of pore
size in such compositions. Also, more spherical pores and smaller pore
size are achieved for the alumina sol impregnated samples. These oc-
currences lead to the enhancement of crushing strength and thermal
insulation performance, owing to decreasing of stress concentration and
reduction of heat transfer as well as heat radiative caused by the pre-
sence of spherical micro-pores and smaller pore size. By using of 7 µm
walnut shell powders with impregnating 5 wt% alumina sol, porous
alumina ceramics with excellent properties could be fabricated, whose
thermal conductivity is 0.161 W/m K and crushing strength is
29.2 MPa, providing potential applications in high-temperature furnace
working lining materials.

Table 4
Comparison of physical properties of PACs prepared by using different methods.
Preparation method Apparent porosity Bulk density Crushing strength Thermal conductivity References
(%) (g/cm3) (MPa) (W/m K)

Direct foaming 71.0 0.91 4.2 0.25 [31]

Gel-casting 72.2 1.10 15.5 1.03 [32]
PFAs (sawdust) 70.6 1.09 2 0.50 [33]
Alumina hollowsphere bricks 62.7 1.51 22.5 0.93 [28]
WS7-5 67.7 1.35 29.2 0.161 This work

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J. Liu et al.
Fig. 8. Heat transfer behaviors of samples with (a) irregular large pore sizes, (b) irregular small pore sizes and (c) spherical micro-pores.
Fig. 9. Stress distribution behaviors of samples with (a) irregular large pore sizes, (b) irregular small pore sizes and (c) spherical micro-pores.
Acknowledgements
The authors are grateful for the financially support from the China
Postdoctoral Science Foundation (Grant no. 2018M631492), the China
Postdoctoral Science Foundation (Grant no. 2018M630151), the China
Postdoctoral Science Foundation (Grant no. 2018M63149), the China
Postdoctoral Science Foundation (Grant no. 2018M63154), the
National Natural Science Foundation of China (Grant no. 51572140)
and National Natural Science Foundation of China (NSFC, No.
51702184).
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