Materials and Design 56 (2014) 353358

Contents lists available at ScienceDirect

Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Compressive properties of closed-cell aluminum foams with different

contents of ceramic microspheres
Xingchuan Xia a,, Xiaowei Chen a, Zan Zhang a, Xu Chen a, Weimin Zhao a, Bo Liao a, Boyoung Hur b
a
b

School of Materials Science and Engineering, Hebei University of Technology, Tianjin 300130, China
School of Nano Advanced Materials Science and Engineering, Gyeongsang National University of South Korea, Republic of Korea

a r t i c l e

i n f o

Article history:
Received 5 September 2013
Accepted 18 November 2013
Available online 26 November 2013
Keywords:
Aluminum foam
Melt foaming method
Compressive property
Ceramic microspheres

a b s t r a c t
In this paper, closed-cell aluminum foams with different kinds and contents of ceramic microspheres are
obtained using melt-foaming method. The distribution and the effects of the ceramic microspheres on the
mechanical properties of aluminum foams are investigated. The results show that both kinds of ceramic
microspheres distribute in the foams uniformly with part in the cell wall matrix, some in adhere to the
cell wall surface and part embed in the cell wall with portion surface exposed to the pores. Ceramic
microspheres have an important effect on the yield strength, mean plateau stress, densication strain
and energy absorption capacities of aluminum foams. Meanwhile, the content of ceramic microsphere
in aluminum foams should be controlled in order to obtain good combination of compressive strength
and energy absorption capacity. The reasons are discussed.
2013 Elsevier Ltd. All rights reserved.

1. Introduction
Closed-cell aluminum foams are a class of novel materials with
continuous metallic matrix being separated by equally distributed
gas bubbles. Compared with commercial available bulk alloys, they
have many excellent properties, such as ultra-low density, good
energy absorption property, high electromagnetic shielding effect,
excellent sound-absorbing property and good damping
performance [1]. Many kinds of metallic foams (e.g. aluminum,
magnesium, titanium, nickel and steel) have been developed for
energy-absorbing applications as they have a distinct advantage
over solid metals in this respect, the related energy-absorbing
characteristics of these materials have also been widely researched
[2,3]. Among these kinds of metallic foams, aluminum foams, due
to their lightweight and good energy absorption performance, have
been drawing much attention in construction, automotive and
aerospace applications. Meanwhile, with the development of
preparation methods, aluminum foams have been widely used as
structural and functional materials. However, in these elds
commercially pure aluminum foams were rarely used because of
their lower mechanical properties [4,5]. A few researchers have focused on this phenomenon and Huang et al. investigated the effect
of Sc elements on the quasi-static compressive behaviors of Al
foams and the results showed that minor Sc additions and subsequent proper heat treatment could dramatically improve the

Corresponding author. Tel.: +86 22 60204477; fax: +86 22 60202414.

E-mail address: xc_xia@hebut.edu.cn (X. Xia).
0261-3069/$ - see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.matdes.2013.11.040

compressive yield strength of Al foams [6]. In our previous research Mn particles was introduced into commercial pure aluminum foam to improve its compressive properties [7]. These are
useful and effective ways to obtain high-strength aluminum foams.
However, as it is known that AlSc alloys are expensive, resulting
in increased production costs. Although Mn particles are much
cheaper than AlSc alloy, they need an intermediate preparation
process, leading to energy consumption. Recently, ceramic microspheres, by-products of pulverized coal combustion in thermal
power plant boiler, have been drawing a lot of attention in the respect of metal matrix syntactic foams (MMSFs) [8,9], owning to
their low density, insulating heat, saving energy, good owability
and high mechanical features. Millions tons of ceramic microspheres powder are generated in coal based thermal power plants
every year and only a small portion is being utilized [10]. Metal
matrix syntactic foams (MMSFs) using ceramic microspheres as
pore generation agent or thickening agent have been proved to
possess excellent compressive properties compared with conventional aluminum foams [812].
Metal matrix syntactic foams (MMSFs), mainly fabricated
through melt inltration of technique, resulting in conned foam
dimensions and the porosity of the foams fabricated through melt
inltration is less than 65% [1315], to the best of our knowledge.
Researchers have investigated the micro-architecture and compressive deformation behavior of Al-alloy and microspheres hybrid
Al-foam prepared through stir casting technique using CaCO3 as
foaming agent [12]. 30 vol.% of cenospheres were added into the
melt mixture as thickening agent, it was conrmed that the

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X. Xia et al. / Materials and Design 56 (2014) 353358

closed-cell foams possessed higher plateau strength and energy

absorption capacity than conventional aluminum foams [12]. It is
signicant to produce hybrid metal foams through conventional
casting method which is widely used in the industrial production
of aluminum foams and the products have a greater range in respect of the dimensions. However, we should note that only xed
percentage of microspheres was added into the melt as thickening
agent. While, from the engineering application view point, the effect of ceramic microspheres contents on the variation of compressive properties, the distribution of the ceramic microspheres and
the optimal content in the foam have to be investigated and found.
Unfortunately few literatures focused on this region and further research is needed.
In the present experiment, closed-cell aluminum foams containing different kinds and contents of ceramic microspheres were
prepared through melt foaming method. The effects of ceramic
microspheres on the compressive properties were investigated
experimentally and the optimal contents of the ceramic microspheres were found.

2. Experimental methods and materials

Melt foaming method was applied to fabricate closed-cell Al
foams with different types and contents of ceramic microspheres.
The raw materials used in the present experiment were commercially pure aluminum ingots (with the purity of 99.5%), Ca granules
(commercially pure, granularity between 1 and 2.5 mm, thickening
agent), TiH2 (commercially pure, 300 20 mesh, foaming agent)
and two types of ceramic microspheres QK150 and QK300, with
the compositions of SiO2 60 wt%, Al2O3 40 wt% and Fe2O3
0.5 wt% (supplied by Sun Microsphere Co., Ltd., China). The size
ranges of QK150 and QK300 are 45150 lm and 150300 lm
respectively. In addition, the compressive strengths are 17.24 and
14.48 MPa, respectively. Detailed preparation process mainly
includes the following steps: (1) melting certain quantity of
commercially pure aluminum (1 kg) in a low carbon steel
crucible to a xed temperature; (2) adding certain quantity of Ca
granules (thickening agent, 2 wt%) with the stirring speed of
450 rpm for 6 min and different contents (0%, 2.5%, 5.0%, 12.5%

Table 1
Detailed specimens structural parameters.
Types

No.

Length/mm

Width/mm

Height/mm

Volume/mm3

Weight/g

Porosity (%)

QK150

2.51
2.52
5.01
5.02
12.51
12.52
20.01
20.02

25
25
25
25
25
25
25
25

25
25
25
25
25
25
25
25

25
25
25
25
25
25
25
25

15,625
15,625
15,625
15,625
15,625
15,625
15,625
15,625

10.9917
11.4574
10.5438
10.7994
10.8164
10.6876
12.2705
12.4959

0.7395
0.7284
0.7501
0.7440
0.7436
0.7467
0.7091
0.7038

QK300

2.51
2.52
5.01
5.02
12.51
12.52
20.01
20.02

25
25
25
25
25
25
25
25

25
25
25
25
25
25
25
25

25
25
25
25
25
25
25
25

15,625
15,625
15,625
15,625
15,625
15,625
15,625
15,625

9.0889
9.1023
9.2763
8.9086
8.5124
8.8920
8.9926
9.1691

0.7846
0.7842
0.7801
0.7888
0.7982
0.7892
0.7868
0.7827

Original

O-1
O-2

25
25

25
25

25
25

15,625
15,625

10.6302
10.9997

0.7480
0.7393

Fig. 1. Macroscopic and fracture morphologies of QK150 (a) and QK300 (b) ceramic microspheres.

X. Xia et al. / Materials and Design 56 (2014) 353358

and 20.0%, hereinafter refer to vol.% unless otherwise specied) of

QK150 or QK300 ceramic microspheres (preheated at 600 C in a
furnace to avoid broken when being introduced into the aluminum
melt) to the melt accompanied by stirring with the speed of
800 rpm for 2 min; (3) adding certain amount of TiH2 (commercially pure, 300 20 mesh, 0.6 wt%) to the melt accompanied by
stirring and holding for some time, with the stirring speed of
1500 rpm for 40 s and holding time of 2 min; (4) cooling the ux
in the air after it was foamed. During the whole procedures except
for the last step the temperature of the melt was controlled at
680 5 C. Buoyant method was applied to eliminate the broken
hollow microspheres from a batch. Specimens for ceramic microspheres morphology and distributions observation were prepared
by electro-discharging machine, metallographic mosaic machine
and band saw, briey in the following steps: Surfaces of specimens
for investigation of the sphere distribution were rstly cut by electro-discharging machine. After that specimens were sealed with
ureaformaldehyde molding powder by metallographic mosaic
machine, leaving the cross section for investigation of the sphere
distribution. The other connecting surfaces were cut by band saw
to satisfy the size requirements of SEM. Then specimens were nally ground using 2000 grit emery paper, polished using 0.25 lm diamond paste, ultrasonically cleaned by acetone for 5 min and at last
dried by cold owing air. Hitachi S4800 scanning electron microscope (SEM) was used to examine the distributions of the ceramic
microspheres.
Specimens were machined by electro-discharging machine into
the size of 25  25  25 mm3 to ensure there were at least 7 cells
in every direction to avoid size effect. Porosities of the foams were
deduced from weights and volumes of the foams (it should be
emphasized that the density of the matrix containing some microspheres in cell walls was selected as 2.70 g/cm3) [12]. Analytical
balance (with precision of 0.0001 g) and electronic caliper were
used to measure the weights and accurate dimensions of the
foams, respectively. Uniaxial compression tests were performed
by using a SUNS electron universal material testing machine
(according to China Standard GB/T7314-2005 [16]). All tests were

355

applied under displacement control with a constant cross-head

speed of 6.0 mm/min (with the initial strain rate of 4  103/s) at
room temperature. The displacement measurements were taken
from the crosshead displacement of the machine corrected for
the compliance of the load frame and load cell. Vaseline was used
to minimize the friction between specimen and plates. Stress
strain was deduced from the recorded loaddisplacement data
which was recorded using a data acquisition unit and a personal
computer. Mean intercept technique were used to determine the
macroscopic pore size and extrapolation method was used to
determine the densication strain [17]. For each test parameters,
two specimens were compressed to ensure the reproducibility
and the average data were used, detailed parameters are shown
in Table 1.

3. Results and discussion

3.1. Morphology observation
Fig. 1 shows the typical macroscopic and fracture morphologies
of QK150 and QK300 ceramic microspheres respectively. From the
observation of more than 1000 microspheres and shown in Fig. 1a,
the QK150 microspheres can divide into three categories: category
A has small size and smooth surface (marked as 1), accounting for
about 10% (by number); category B possesses rough surface and
large range of sizes (marked as 2), accounting for about 75% (by
number); category C (marked as 3) is somewhere between the rst
two categories, accounting for about 15% (by number). While for
the QK300 microspheres (as show in Fig. 1b), almost no category
A was observed and their surfaces are rougher than the QK150
microspheres. In addition, more tiny holes appear in the surface,
leading to their lower compressive properties (as described in
Section 2). Under higher magnication we can see that there are
cellular structures in both of the microspheres walls and some
much smaller pores embedded in them and no obvious cracks
are observed.

Fig. 2. Specimen images of foams with 2.5 vol.% QK150 ceramic microspheres.

Fig. 3. Typical ceramic microspheres distribution and existence state in the foam with 2.5 vol.% QK150 ceramic microspheres.

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X. Xia et al. / Materials and Design 56 (2014) 353358

Fig. 4. Stressstrain curves of all specimens containing different contents of QK150 (a) and QK300 (b), the average results and energy absorption properties of specimens with
different contents of QK150 (c) and QK300 (d) ceramic microspheres.

3.2. Distribution of microspheres

Fig. 2 shows representative specimen images (with 2.5% QK150
ceramic microspheres) with dimension, porosity and pore size of
25  25  25 mm3, 75% and 2  4 mm respectively. It is clear that
the pores are spherical and isolated, the pore structure on the cross
section is homogeneous and the pores are closed-cell. Fig. 3a and b
shows typical ceramic microspheres distribution and existence
state in the foams (with 2.5% QK150 ceramic microspheres). Ceramic microspheres were mixed uniformly and present in the cell
wall, cell edges or cell wall faces (as shown in Fig. 3a). We can

see that ceramic microspheres mainly exist in the following states

from Fig. 3a. Some totally embed in the cell wall (ellipses marked
areas, dened as state A). Part of them adhere to the cell wall surface with most of their surfaces exposing to cells, which could easily be conrmed (circles marked areas, dened as state B). Another
part with more volume embedding in the cell walls, leaving rough
surface exposing to the cells (squares marked areas, dened as
state C) and it is a direct reection of the drainage phenomenon
of the solidication of the foams. When foaming is done, the microsphere would try to move upward and thus helps in hindrance of
melt drainage due to gravity through the cell walls or cell edges.

X. Xia et al. / Materials and Design 56 (2014) 353358

357

Fig. 5. Variation of the densication strain, mean plateau strength and yield strength with different contents of QK150 (a) and QK300 (b) ceramic microspheres (Note: lines
were added as guidelines only).

The downward movement of melt causes a fraction of microspheres towards the cell wall boundary. Microspheres with smooth
surface can easily be pushed into the pores with small part of them
adhere to the cell wall (state B). While microspheres with rougher
surface possess greater opportunities leave in cell walls or with
more volume embedding in cell walls. Fig. 3b shows the representative structure of the QK150 microspheres in the foam cell wall
under higher magnication. It is clear that the microsphere maintain the original morphology and no obvious cracks and aluminum-penetration can be observed. Similar situation is also found
in the foams with QK300 ceramic microspheres. It should be noted
that the amount of ceramic microspheres with states B and C
increased more than state A as the content of ceramic microspheres increasing, regardless of QK150 or QK300. In addition,
most of the ceramic microspheres exist in foams are spherical during the preparation process. This indicates that melt foaming
method and the preheated technology are effective and suitable
to prepare closed-cell aluminum foams with ceramic microspheres. It is important to note that though aluminum melts have
been thickened before ceramic microspheres being introduced into
the melts, not all the microspheres are kept in the cell walls and
only part of them could act as strengthening phases.
3.3. Energy absorption characteristics
Energy absorption capacity (E) is an important aspect to evaluate the properties of metal foams. The energy absorption capacity
(E) of closed-cell AZ31 aluminum foams was calculated according
to Eq. (1):

rde

where W is the energy absorption capacity, r is the stress where the

stain is e.
Fig. 4a and b shows the engineering stress-engineering strain
compression curves of all the specimens under quasi-static compression tests. Fig. 4c and d shows the average values (obtained
from Fig. 4a and b) and the energy absorption capacities of specimens with different types and contents of ceramic microspheres.
In all cases the curves display an initial linear deformation region
(I) where stress increased linearly to the rst peak (dened as yield
strength), followed by a plastic plateau stage (II) where stress
slightly increased as the strain increasing, then a densication
stage (III) where stress raises sharply with strain increasing
slightly. The trends are similar to those of other Al/Mg alloy foams
[18,19]. Meanwhile, energy absorption capacity is an important aspect to evaluate the properties of metal foams and it could be seriously inuenced by yield strength, plateau stress and densication

strain. It is necessary to consider their modication from the application point. Thus, we mainly focus on the effect of ceramic microspheres on the compressive yield strength, mean plateau stress
(dened as the average value of the stress with the strain between
0.05 and 0.55.) and the densication strain of aluminum foams.
The yield strength of the foams with QK150 ceramic microspheres
contents of 0%, 2.5%, 5.0%, 12.5% and 20% are about 2.97, 8.02 (value range: 7.019.03), 7.83 (value range: 7.518.15), 6.22 (value
range: 5.816.63) and 6.66 (value range: 6.137.19) MPa, respectively. For the mean plateau stresses of these foams (shown in
Fig. 4c and d) are around 4.86, 11.47, 11.09, 8.65 and 9.46 MPa
and the average densication strains (shown in Fig. 4c and d) are
about 0.55, 0.59, 0.65, 0.59 and 0.64 respectively (As shown in
Fig. 5a). This indicates that QK150 ceramic microspheres have an
important effect on the foams yield strength, mean plateau
strength and densication stress under compression state. The
yield strength of the foam improves about 2 times of the original
ones, especially when the contents are 2.5% and 5.0%. Similar phenomenon appears on mean plateau stress of the foams. As for
densication strain, QK150 ceramic microspheres enhance the
densication strain of the foams. All of these reasons result in higher energy absorption capacity of the foams containing different
contents of QK150 ceramic microspheres (as shown in Fig. 4a)
and the energy absorption capacity increased with the strain
increasing like other foams [7,12]. It is interesting that there are
similar variation tendency regardless of yield strength, mean plateau stress, densication strain and energy absorption capacity of
the foams with different contents of QK150 ceramic microspheres.
That is the values increased to a high level and then decreased
moderately to a lower level (higher than the original foam) as ceramic microspheres content increasing. From the perspective of energy absorptive capacity, foams with QK150 contents of 2.5% and
5.0% possess better performance compared with others. This is because of the presence of hard ceramic microspheres will increase
the overall bulk hardness of the material, leading to higher yield
strength and mean plateau stress. In addition, it has been found
that the addition of ceramic microspheres has a signicant effect
on the mechanical properties of Al composites by the load transfer
from matrix to the reinforcement [20]. In addition, the energy
absorption capacity decreased with more content of microspheres.
It should be noted that foams with 20.0% microsphere content have
little higher yield strength, mean plateau strength and energy
absorption capacity than the 12.5% foam, it is mainly due to the
former possess lower porosity (as shown in Figs. 5a and 4a). For
foams with different contents of QK300 ceramic microspheres,
the variation tendency of yield strength, mean plateau stress and
energy absorption capacity are similar with the foams with
QK150 ceramic microspheres (as shown in Figs. 4b and 5b).

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X. Xia et al. / Materials and Design 56 (2014) 353358

However, there are some distinctions, e.g. specimens with QK300

possess higher porosities than the QK150 specimens under present
preparation process and the energy absorption capacity of
specimens with 2.5% QK300 is higher than others. It is clear that
the microspheres improved compressive properties of the original
specimen. Meanwhile, compared with the results of other
experiments, microsphere-containing specimens possess higher
compressive yield strength, mean plateau stress and energy
absorption capacity than commercially pure aluminum foams
[4,7,21,22] even though the microsphere-containing specimens
possess higher or similar porosities, meaning ceramic microspheres have apparent enhancement to aluminum foams.
4. Conclusions
Closed-cell aluminum foams with different kinds and contents
of ceramic microspheres were fabricated by melt-foaming method
using Ca as thickening agent and TiH2 as foaming agent. The effects
of ceramic microspheres on the compressive properties of Al foams
were studied and the results were summarized as follows: The distribution of ceramic mcirospheres was uniform in the cell walls
and they were mainly distributed in the foams with part in the cell
wall matrix, some in adhere to the cell wall surface and part embed
in the cell wall with portion surface exposed to the pores. The addition of ceramic microspheres prominently improved the yield
strength, mean plateau stress, densication strain and energy
absorption capacity of original foams. In order to guarantee the
optimal energy absorption capacity the content of both types of
ceramic microspheres should be limited.
Acknowledgements
The present authors wish to thank the nancial support
provided by 863 project of China (No. 2013AA031002), Major
Project of China (2013ZX04004027), the 100 Talents Project of
Hebei Province of China (Grant No. E2012100009), Natural Science
Foundation of Hebei Province of China (Nos. E2012202017 and
E2010000121), Science and Technology Research of Hebei Province
for Youth fund (No. 2011182). Science and Technology Project of
Hebei Province (13211008D).
References
[1] Banhart J. Manufacture, characterisation and application of cellular metals and
metal foams. Prog Mater Sci 2001;46:559632.

[2] Dannemann KA, Lankford Jr J. High strain rate compression of closed-cell

aluminium foams. Mater Sci Eng A 2000;293:15764.
[3] Mukai T, Kanahashi H, Miyoshi T, Mabuchi M, Nieh TG, Higashi K.
Experimental study of energy absorption in a closed-cell aluminum foam
under dynamic loading. Scripta Mater 1999;40:9217.
[4] Kennedy AR, Asavavisitchai S. Effects of TiB2 particle addition on the
expansion, structure and mechanical properties of PM Al foams. Scripta
Mater 2004;50:1159.
[5] Davydov VG, Rostova TD, Zakharov VV, Filatov YuA, Yelagin VI. Scientic
principles of making an alloying addition of scandium to aluminum alloys.
Mater Sci Eng A 2000;280:306.
[6] Huang L, Wang H, Yang DH, Ye F, Lu ZP. Effects of scandium additions on
mechanical properties of cellular Al-based foams. Intermetallics
2012;28:716.
[7] Xia XC, Feng H, Zhang X, Zhao WM. The compressive properties of closed-cell
aluminum foams with different Mn additions. Mater Des 2013;51:797802.
[8] Orbulov IN. Compressive properties of aluminium matrix syntactic foams.
Mater Sci Eng A 2012;555:526.
[9] Tao XF, Zhang LP, Zhao YY. Al matrix syntactic foam fabricated with bimodal
ceramic microspheres. Mater Des 2009;30:27326.
[10] Guo RQ, Rohatgi PK, Nath D. Preparation of aluminium-y ash particulate
composite by powder metallurgy technique. J Mater Sci 1997;32:39714.
[11] Rabiei A, ONeill A. A study on processing of a composite metal foam via
casting. Mater Sci Eng A 2005;404:15964.
[12] Mondal DP, Jha Nidhi, Gull Bilal, Das S, Badkul Anshul. Microarchitecture and
compressive deformation behavior of Al-alloy (LM13)-cenosphere hybrid Alfoam prepared using CaCO3 as foaming agent. Mater Sci Eng A
2013;560:60110.
[13] Kiser M, He MY, Zek FW. The mechanical response of ceramic microballoon
reinforced aluminum matrix composites under compressive loading. Acta
Mater 1999;47:268594.
[14] Balch DK, ODwyer JG, Davis GR, Cady CM, Gray GT, Dunand DC. Plasticity and
damage in aluminum syntactic foams deformed under dynamic and quasistatic conditions. Mater Sci Eng A 2005;391:40817.
[15] Tao XF, Zhao YY. Compressive behavior of Al matrix syntactic foams
toughened with Al particles. Scripta Mater 2009;61:4614.
[16] China Standard GB/T 73142005. Metallic materials-compression testing at
ambient temperature. General administration of quality supervision,
inspection and quarantine of the Peoples Republic of China, Standardization
administration of the Peoples Republic of China. 2005.
[17] Francesca Campanaa and Daniela Pilone. Effect of heat treatments on the
mechanical behaviour of aluminium alloy foams. Scripta Mater 2009; 60:679
82.
[18] Yamada Y, Shimojima K, Sakaguchi Y, Mabuchi M, Nakamura M, Asahina T,
et al. Effects of heat treatment on compressive properties of AZ91 Mg and
SG91A Al foams with open-cell structure. Mater Sci Eng A 2000;280:2258.
[19] Kanahashi H, Mukai T, Yamada Y, Shimojima K, Mabuchi M, Aizawa T, et al.
Experimental study for the improvement of crashworthiness in AZ91
magnesium foam controlling its microstructure. Mater Sci Eng A
2001;308:2837.
[20] Ramachandra M, Radhakrishna K. Synthesis-microstructure-mechanical
properties-wear and corrosion behavior of an AlSi (12%)-yash metal
matrix composite. J Mater Sci 2005;40:598997.
[21] Andrews E, Sanders W, Gibson LJ. Compressive and tensile behaviour of
aluminum foams. Mater Sci Eng A 1999;30:11324.
[22] Edwin Raj R, Parameswaran V, Daniel BSS. Comparison of quasi-static and
dynamic compression behavior of closed-cell aluminum foam. Mater Sci Eng A
2009;25:115.