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J. Mater. Sci. Technol., 2014, 30(7), 661e665

Processing of B4C Particulate-reinforced Magnesium-matrix


Composites by Metal-assisted Melt Infiltration Technique
Yantao Yao, Liqing Chen*
State Key Laboratory of Rolling and Automation, Northeastern University, Shenyang 110819, China
[Manuscript received January 14, 2014, in revised form March 1, 2014, Available online 24 June 2014]

In fabricating magnesium-matrix composites, an easy and cost-effective route is to infiltrate the ceramic preform
with molten Mg without any external pressure. However, a rather well wettability of molten Mg with ceramic
reinforcement is needed for this process. In order to improve the wettability of the metal melt with ceramic
preform during fabricating composites by metal melt infiltration, a simple and viable method has been
proposed in this paper where a small amount of metal powder with higher melting point is added to the
ceramic preform such that the surface tension of the Mg melt and the liquidesolid interfacial tension could be
reduced. By using this method, boron carbide particulate-reinforced magnesium-matrix composites (B4C/Mg)
have been successfully fabricated where Ti powder immiscible with magnesium melt was introduced into B4C
preform as infiltration inducer. The infiltration ability of molten Mg to the ceramic preform was further studied
in association with the processing conditions and the mechanism involved in this process was also analyzed.

KEY WORDS: Magnesium-matrix composites; Boron carbide; Melt infiltration; Microstructure; Mechanism

1. Introduction and hybrid reinforcements were synthesized by Sankaranar-


ayanan et al.[11] through disintegrated melt deposition technique
Light-weight particulate-reinforced magnesium-matrix com- (DMD) followed by hot extrusion and the effect of ball milling
posites are gradually finding wide applications as promising the hybrid reinforcements on the microstructure and mechanical
structural and functional materials in electronic, aeronautical and properties of this kind of composites was also evaluated. Among
aerospace fields, since they possess high specific strength and these routes, metal melt infiltration into ceramic preform is
stiffness, excellent wear-resistant ability, good electrical and recognized as having merits in low cost, high efficiency, near
thermal conductivities, and vibration-damping capacity[1e4]. net-shape, availability of composites with high ceramic volume
As for the fabrication of magnesium-matrix composites, fraction and received much attention in recent years[12,13].
several routes have been utilized to synthesize magnesium- However, the prerequisite for effective infiltration of metal melt
matrix composites, which mainly include powder metallurgy[5], into the ceramic preform is good wettability of metal melt to the
stir casting[6] and infiltration technique with or without the aid of ceramic particulate[2]. Generally, the wettability between ceramic
pressure[7,8]. Recently, Habibi et al.[9] utilized powder metallurgy and magnesium melt is not so well and the infiltration process is
route using microwave assisted rapid sintering technique fol- unlikely to occur unless the fabrication temperature is extremely
lowed by hot extrusion to synthesize magnesium nano- high, e.g. in conventional ceramic/magnesium systems as Mge
composites in order to enhance the strength and ductility of TieC, MgeTieB, MgeB4C. Thus, promotion of the infiltration
magnesium simultaneously. Interpenetrating metal-matrix com- ability becomes a critical issue in fabricating magnesium-matrix
posites were prepared by Scherm et al.[10] through infiltrating of composites by using this technique.
porous ceramic performs by a pressure supported casting process The usual way to enhance the wettability of metal melt to the
and the microstructure was also characterized by using different ceramics is to raise the temperature much higher than the melting
experimental methods. Composites containing pure magnesium point. Undoubtedly, this method is suitable for the non-volatile
molten metal and can not be used for volatile metal, e.g. Mg and
Zn. In this paper, an effective way to improve the wettability of the
*
Corresponding author. Tel.: þ86 24 83681819; Fax: þ86 24 23906472;
E-mail address: lqchen@mail.neu.edu.cn (L. Chen). metal melt with ceramic preform was proposed in fabricating
1005-0302/$ e see front matter Copyright  2014, The editorial office of magnesium-matrix composites via pressureless infiltration technique
Journal of Materials Science & Technology. Published by Elsevier by adding small amount of metal particles with high melting point.
Limited. All rights reserved. As an illustrative case, this conception was demonstrated in
http://dx.doi.org/10.1016/j.jmst.2014.06.005 fabricating B4C/Mg composite by magnesium melt infiltration
662 Y. Yao and L. Chen: J. Mater. Sci. Technol., 2014, 30(7), 661e665

into B4C ceramic preform where some amount of Ti particles had


been added, and the mechanism of effective infiltration involved
in this process was also analyzed. Since B4C has a lower density
(2.52 g/cm3), even when the B4C takes 50% volume fraction, the
composite system B4C/Mg is extra-light and the density is only
about 2 g/cm3, much lighter than that of pure aluminum, a little
higher than that of magnesium. It is worth noting that such a high
volume fraction of ceramics in this composite system will bring
about excellent wear resistance[14], so it will find wide applica-
tions in aeronautical and aerospace industries.

2. Experimental

The raw materials used in fabricating boron carbide reinforced Fig. 1 SEM micrographs of the as-fabricated B4C/Mg composites at
973 K for 120 min.
magnesium composites were listed in Table 1 where the B4C
particulate has mean sizes of 28, 10 and 5 mm, respectively, and
Ti particulate has an average size of 25 mm. The magnesium preform of B4C when the heating temperature is at 953, 973, and
ingot was used as infiltration metal and it has a commercial 993 K for different holding time under the flowing argon at-
purity of 99.95%. mosphere. It is noticeable that the infiltration process of mag-
There are two main steps in fabricating B4C/Mg composites, i.e. nesium melt into B4C preform does not occur without the
preparation of the B4C preform and spontaneous infiltration of addition of Ti particulate into B4C preform. This implies that the
magnesium melt into B4C ceramic preform. Firstly, Ti powder of Ti particulate plays a predominant role in this process. That is to
different volume fraction (0%, 2%, 4%, 6% and 8%) was added say, the B4C/Mg composites can be successfully fabricated with
into B4C powder. After adding a certain amount of binder and fully the existence of Ti as an infiltration inducer.
mechanical blending, the mixed Ti and B4C powders were then Fig. 1 shows the typical SEM micrograph of the as-prepared
cold compacted into green body of cylindrical shapes (16 mm in B4C/Mg composites at 973 K for 120 min. The original pre-
diameter, height variable) in a steel mould with various relative form has a 4% volume fraction of Ti particles and a relative
densities of 50%, 55% and 60%. The compacted preform together density of 60%. It can be seen in Fig. 1 that B4C particles with an
with a pure magnesium ingot on it was put into a graphite mould. irregular shape were uniformly distributed in the magnesium-
Several small holes were drilled at the bottom of the graphite matrix and very few Ti particles were found due to its extremely
mould in order to release the air during fabricating the B4C/Mg low volume fraction. Fig. 2 shows the XRD spectrum of the as-
composites. The infiltration process was carried out in an electric fabricated B4C/Mg composites corresponding to Fig. 1 and it
furnace under the presence of a flowing argon (99.999% purity) contains four phases, i.e. B4C, Mg, MgB2 and SiC. The presence
atmosphere. The chamber of the furnace was degassed prior to of Mg and B4C phases confirms that magnesium melt has
heating and then backfilled with Ar. The infiltration system was infiltrated into the B4C preform under the present processing
finally heated up to temperatures of 953, 973 and 993 K, respec- conditions. No Ti peak was detected owing to its low addition
tively, at a rate of 10 K/min. At each temperature, the holding time and SiC was introduced as impurities during the blending of
was all set as 90, 120 and 150 min. After that, the samples were starting powders or the polishing of B4C/Mg composites samples
cooled with the furnace down to the room temperature. using silicon carbide paper. Besides, there is a weak peak cor-
Metallographic microscopy (LEICA Q550IW), scanning elec- responding to MgB2 trace phase. It was reported that B4C par-
tron microscopy (SEM, FEI Quanta 600) and X-ray diffractometer ticles were easily oxidated during mixing the starting materials
(XRD, X’Pert Pro) were used to characterize the microstructures and an amorphous B2O3 surface layer was produced. After that,
and the phases of the as-infiltrated composites. The specimens an interfacial reaction of B2O3 with magnesium melt occurred
were sectioned and polished in the infiltration direction in order to and rod-like MgB2 produced[15].
measure the infiltration distance to analyze the influence of pro- It is obvious that the processing parameters, e.g. Ti content,
cessing parameters on the infiltration dynamics. heating temperature, holding time and relative density, have
much influence on the fabricating process and thus the materials
3. Results and Discussion

3.1. Microstructure and phase analysis

As expected, with the aid of Ti particulate in B4C preform the


magnesium melt can spontaneously infiltrate into the ceramic

Table 1 Raw materials used in fabricating B4C/Mg composites

Materials Particle size (mm) Purity (%)

B4C 28 94.66
10 94.55
5 93.78
Ti 25 99.5
Mg (ingot) e 99.95
Fig. 2 XRD spectrum of the as-fabricated B4C/Mg composites.
Y. Yao and L. Chen: J. Mater. Sci. Technol., 2014, 30(7), 661e665 663

Fig. 3 Curves showing infiltration distances of magnesium melt versus holding time at 973 K (a), heating temperature with the holding time of 120 min
(b), relative density of preform at 973 K for 120 min (c) and B4C particle size at 973 K for 120 min (d) in fabricating B4C/Mg composites.

performance. For these reasons, a further study was carried out in their influence on the infiltration process. When the B4C powder
order to have a detailed understanding of the infiltration process with particle size of 5 mm was used, the process of magnesium
under the presence of Ti particles as infiltration inducer. melt infiltration into B4C ceramic powder did not take place. It is
obvious in Fig. 3(d) that a larger infiltration distance can be
3.2. Influence of processing parameters on infiltration ability obtained with larger B4C particle size. In other words, when the
particle size of B4C powder is comparable to that of Ti particles,
In order to study the infiltration ability or infiltration distance the infiltration process is prone to occur.
of magnesium melt in the ceramic preform, several processing
parameters were taken into account in analyzing the infiltration 3.3. Mechanism of infiltration process
process. The experimental results were collected in Fig. 3
showing the infiltration distance versus various processing pa- For MgeB4C system, the infiltration of magnesium melt
rameters for preparing the composites. For the infiltration of into B4C preform depends largely on the wettability between
magnesium melt into B4C preform, the infiltration process is them. The capillarity acts as the driving force without any
unlikely to occur when no Ti was added into B4C particles, even external applied pressure. The wettability of a liquid with a solid
at a rather high temperature or for extended time. Moreover, is generally measured by the contact angle q. And the angle q
despite of all the other factors, the more the amount of Ti is related to the surface tension gl/g of the interface of liquid
addition is, the greater the infiltration distance is. In Fig. 3(a), and gas, which can be expressed by the YoungeKelvin equa-
one can see that the infiltration distance increases with increasing tion[16]:
the holding time, but the discrepancy of the infiltration distance
at 120 min and 150 min is not evident, which means that 2gl=g cos q
extending holding time is not needed for fabricating B4C/Mg p ¼ (1)
r
composites in view of efficiency. While in Fig. 3(b) the infil-
tration distance also increases when the processing temperature where p is the capillary force and r the radius of the pores within
is raised. Fig. 3(c) demonstrates that a preform with higher the preform. Eq. (1) indicates that a liquid can wet a solid only
relative density can lead to a larger infiltration distance. when the contact angle q is less than 90 , i.e. cosq is positive. In
It is well known that the particulate size of the raw powder more detail, when the contact angle is smaller and the liquidegas
materials is of great importance in the preparation of particulate- surface tension is greater, or the pore radius is smaller, the
reinforced metal-matrix composites by spontaneously pressure- penetration is easier to occur.
less infiltration technique. In this study, three kinds of particle A schematic representation of the spontaneous infiltration
size, 5 mm, 10 mm and 28 mm, of B4C powder were used to study process is illustrated in Fig. 4 with the existence of Ti particles as
664 Y. Yao and L. Chen: J. Mater. Sci. Technol., 2014, 30(7), 661e665

Fig. 4 Schematic illustrations showing the infiltration of magnesium melt into a porous preform containing Ti particulates by capillarity in fabricating
B4C/Mg composites.

infiltration inducer. It can be seen that the magnesium melt with different amount of Ti under the condition at 993 K for
penetrated into the ceramic preform along the pores between Ti 120 min where the relative density of the preform is 50%. It can
and B4C particles by the capillarity. Once the magnesium melt be seen that homogeneous distribution of the ceramic rein-
come across Ti particulate, the infiltration of magnesium melt forcement B4C in the microstructure could be obtained when the
into the B4C preform is accelerated. The B4C/Mg composites volume fraction of Ti was 8%. In fact, when the volume fraction
were finally fabricated after the magnesium melt infiltrated into of Ti reaches 6% or above, B4C/Mg composites could be
the full B4C ceramic preform. fabricated with uniform microstructures and more infiltration
Generally, the wettability of magnesium melt with B4C is not distance, which can be seen in Fig. 3. For the composites B4C/
so well that the penetration proceeds at an extremely low rate. Mg containing 8 vol.% addition of Ti powder, the density was
This can be observed in the experiment without Ti added to the measured to be 2.147 g/cm3 according to Archimedes’s princi-
B4C particles. Some research indicates that a suitable third metal ple, which is much lighter than aluminum. The hardness of the
can be added to decrease the surface tension of the melt and the as-fabricated B4C/Mg composites was also measured in the
liquidesolid interfacial tension, thus to improve the wetta- range of 110  2 HB by using Full-Automatic Rockwell Type
bility[17,18]. As described in Ref.[19], a sessile drop technique was Hardness Tester, about 3e3.6 times higher than that of pure
utilized to study the wetting behavior of copper alloys on SiC magnesium.
substrates and the results showed that Ti and Cr are effective
elements to improve the wettability owing to lowering the 4. Conclusions
interfacial energy or promoting the chemical reaction. Moreover,
the metal to be used mostly tends to be chemically active. For (1) By introducing a small amount of metal powder Ti with
example, minor magnesium in aluminum matrix composites higher melting point than Mg to the B4C ceramic preform
plays an important role in improving the wettability of the as infiltration inducer, B4C/Mg composites could be easily
aluminum melt and reinforcement through aiding the reaction at and cost-effectively prepared by Mg melt infiltration tech-
the surface of the reinforcement particles and forming new nique. The mechanism involved in this process is that the
compounds at the interface[20]. In this study, however, the infil- wettability of magnesium melt to B4C ceramic preform is
tration mechanism differs from that. Ti has higher melting point largely improved by reducing the surface tension of the melt
than magnesium and is immiscible with magnesium. When it and the liquidesolid interfacial tension.
was added, the surface tension of the melt or liquidesolid (2) In fabricating B4C/Mg composites by metal-assisted melt
interfacial tension would be reduced. Thus, the wettability of the infiltration technique, there are several factors that have
melt and preform can be improved and it could lead to the influences on the process, including fabricating or heating
penetration of the melt into ceramic preform at the same time. temperature, holding time, relative density of the ceramic
In order to obtain a more uniformly distributed B4C particu- preform and particle sizes of the starting powders.
late-reinforced magnesium-matrix composites, numerous infil- Generally, these factors will play positive roles in melt
tration experiments have been conducted to have an optimal infiltration ability, i.e. with increasing the heating
processing condition. As an illustrative case, Fig. 5 shows the temperature, holding time or the relative density of the
optical micrographs of the as-fabricated B4C/Mg composites ceramic preform, the infiltration distance is increased.

Fig. 5 Optical micrographs showing the microstructures of the B4C/Mg composites containing 2 vol.% (a) and 8 vol.% (b) of Ti particulates as
infiltration inducer.
Y. Yao and L. Chen: J. Mater. Sci. Technol., 2014, 30(7), 661e665 665

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Zhang, and Mrs Yanhua Zhang, Institute of Metal Research,
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