Metals and Materials International (2021) 27:4841–4853

https://doi.org/10.1007/s12540-020-00739-0

Influence of Dispersoid Content on Compressibility, Sinterability

and Mechanical Behaviour of ­B4C/BN Reinforced Al6061 Metal Matrix
Hybrid Composites Fabricated via Mechanical Alloying
Sudipta Chand1 · Polymersetty Chandrasekhar1 · Sudesna Roy1 · Saranjit Singh1

Received: 27 March 2020 / Accepted: 21 April 2020 / Published online: 18 May 2020
© The Korean Institute of Metals and Materials 2020

Abstract
In the present work, x wt% ­B4C (x = 2, 4, 6, 8) and 2 wt% BN reinforced aluminum 6061 metal matrix hybrid composites
were synthesized by mechanical milling for 10 h. The milled powders were consolidated by cold uniaxial compaction at
various compression pressure (200–800 MPa) and then sintered at various temperatures (400–600 °C). Microstructural
characterization of the milled powders and the fabricated composites were performed by X-ray diffraction, scanning electron
microscope, and energy dispersive spectroscopy techniques. The effect of B ­ 4C/BN reinforcements on the densification of
the milled powders was studied in terms of compressibility and sinterability. The mechanical properties, specifically the
green compressive strength, and hardness of the composites were also investigated. The empirical relations formulated by
Heckel, Panelli-Filho, and Ge were used to plot the compressibility curves of the developed composites to study the com-
pressibility behavior of the milled powders. The densification co-efficient (K) of the powders and sinterability behavior of
the composites decreased with an increase in ­B4C reinforcement. ­B4C particles prevented the grain growth by seizing the
grain boundary, resulting in refinement of grains and enhancement in mechanical properties The maximum compressive
strength of 249 MPa and hardness of 184 HV was observed for the sample Al6061–8 wt% B ­ 4C–2 wt% BN compressed at
800 MPa and sintered at 600 °C.

Keywords Powder metallurgy · Metal matrix composites · Compressibility · Sinterability · Boron carbide · Aluminium
alloy

1 Introduction automotive, aerospace, and defense sectors. The Al-MMC

possesses an excellent combination of physical and mechani-
Metal matrix composites (MMC) with ceramic reinforce- cal properties such as high stiffness, specific strength, wear
ments have evolved as one of the most researched topics resistance, thermal and electrical conductivities [4–6]. Alu-
in the last decade due to their advanced applications cor- minum 6061 alloy was chosen as a matrix material for this
responding to the monolithic alloys. These MMCs have a research due to its higher strength and corrosion resistance,
variety of applications due to their superior properties like good deformation capability and formability [7, 8]. With
high elastic modulus, wear, fatigue resistance and high ten- these superior properties and technological importance,
sile strength compared to monolithic alloys. To fabricate Al6061 alloy is mainly used in various applications in the
these MMCs various manufacturing processes have been marine and automotive sectors. The major requirement for
developed, such as stir casting, powder metallurgy, pres- fabricating superior MMC is the homogeneous distribution
sure infiltration, etc.[1–3]. Particulate reinforced aluminum of the reinforcement in the matrix material. In particulate
MMC has a wide variety of commercial applications in the reinforced Al-MMC, agglomeration of the particles pos-
sesses a major challenge during the fabrication, which dete-
riorates the physical and mechanical properties. Powder
* Polymersetty Chandrasekhar metallurgy technique is extremely useful to overcome the
csekharfme@kiit.ac.in agglomeration of reinforcement and avoiding any interfacial
1
School of Mechanical Engineering, KIIT Deemed to be reaction between the reinforcement and the matrix mate-
University, Bhubaneswar, Odisha 751024, India rial. Powder metallurgy also helps to add a high amount of

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4842 Metals and Materials International (2021) 27:4841–4853

reinforcement particle and control the microstructural phases Shanmugasunderam et al. [16] processed bulk Al–4Cu
in the MMC. alloy by mechanical alloying (BPR 14:1, 200 RPM,
For synthesizing the reinforcement and matrix material, 30 h) followed by hot pressing. It was observed that rela-
mechanical alloying is most widely used, as it prevents the tive density was > 99.5% and the compression strength
clustering of reinforcement on the matrix, and produces at room temperature was 890 MPa. Microstructure and
uniform dispersion of the dispersoid in the matrix. This mechanical behavior of mechanically alloyed Al–4.5Cu,
uniform distribution of the dispersoid helps to enhance the Al–4.5Cu–10 ZrC (8 µm and 157 µm) composites were
mechanical properties of the MMC. The process of mechani- studied by Kaftelen et al. [17]. The composites were com-
cal alloying consists of imparting a severe plastic deforma- pacted by vacuum hot pressing (70 MPa, 550 °C, 1 h),
tion (SPD) to the elemental powders using the high energy 97% densification was observed. Due to the presence of
ball milling process. This method induces very high strain ZrC particles, enhancement of wear resistance and hard-
on the milled powder resulting in fracture of phase mix- ness was observed. Many researchers have investigated the
tures. Due to SPD, structural refinement occurs which leads dispersion of reinforcements like A ­ l2O3, SiC, TiC, AlN,
to nano grain structures. The mechanical alloying process VC, ­B4C, ­TiB2, ­Si3N4, ­MgB2, and ­AlB2 and even lighter
consists of cold welding and fracturing of powder in the reinforcements like graphite, BN, mica [18–22] on the Al-
high energy ball milling process. Powder morphology evalu- MMC through the mechanical alloying process.
ation of Al–AlN composites was studied by Abdoli et al. [9]. Boron carbide (­ B4C) is chosen as an appropriate rein-
The unreinforced aluminum powder particles did not reach forcement as it is a hard ceramic reinforcing material with
steady-state after 25 h of ball milling. With the addition of high hardness (> 30 GPa), high elastic modulus (445 GPa),
ceramics particles, the powders reached a steady state with high melting point (2450 °C), good thermal stability, high
equiaxed shaped particles. The hard ceramic AlN particles impact and wear resistance, high chemical resistance and
accelerated the fracture of particles, acting as milling agent low density (2.51 g cm−3) which makes it suitable for refrac-
and obtaining equiaxed particles. Powder morphology of tory applications, bulletproof vests and ballistic protection
Al–15 wt% ­Al2O3 and Al–15 wt% SiCp was investigated by of tanks armor [23–25]. Also, because of the high neutron
Ozdemi et al. [10]. The ceramic reinforcement particles were absorption capacity in isotope B ­ 10, it has a wide range of
evenly dispersed in the Al matrix after mechanical alloying. applications in nuclear industries [26]. Since the presence
Samal et al. [11] studied that during mechanical alloying of hard ceramic reinforcement like B ­ 4C in the aluminum
of Al–Cu alloy the particle size reduced from 21 to 3 µm. matrix, it has poor machinability and forgeability due to its
The crystallite size decreases with an increase in milling high hardness and low ductility. Identifying ways to improve
time and was around 21 nm after 10 h of milling. Lattice the toughness, ductility, and machinability became a major
strain increased from 0.935 to 1.35% with an increase in challenge. The above issue can be addressed by using hybrid
milling time. Paul et al. [12] processed A ­ l95–Zn5 alloy by reinforcement for the development of metal matrix hybrid
mechanical milling at BPR: 10:1, 300 rpm, toluene media composites. Some earlier researchers found out that the addi-
and prepared nanofluid with studies of thermal application. tion of graphite as a secondary reinforcement can reduce the
The crystallite size decreased to 4 nm after 10 h of milling. wear rate of the hybrid composites [27]. The major draw-
The lattice strain increased with milling time which attrib- back of graphite reinforcement is the formation of brittle
uted to grain refinement. interfacial phases, reducing the strength of the composites.
The consolidation mechanical behavior of aluminum Graphite also reacts with the aluminum matrix at processing
2024 with M ­ oSi 2 as reinforcement was studied by temperatures [28] Thus, boron nitride (BN) which acts as a
Sameezadeh et al. [13]. Mechanical alloying was used to solid lubricant and has properties like thermal shock resist-
produce Al 2024- ­MoSi2 composites with (0, 1, 2, 3, 4, ance, low density, low strength and toughness, excellent
5 vol% of ­MoSi2) and were cold compacted at 800 MPa machinability is chosen as the secondary reinforcement for
followed by hot pressing at 450 MPa at 450 °C. 97% the hybrid metal matrix composites [29, 30]. The addition of
relative density was observed in the fabricated compos- solid lubricants also enhances the self-lubrication property
ites. Hosseini et al. [14]. fabricated Al6061 alloy rein- which can reduce wear and tear in the composites. It also
forced with A ­ l2O3 (3 vol%) by mechanical alloying and helps to prevent seizing of punch in the compaction die dur-
then hot pressed to study the tribological behavior. Arik ing high-pressure compactions. The relationship between the
[15] fabricated Al-α-Si3N4 (5, 10, 15 wt%) by mechani- powder characteristics and the compaction routes have been
cal alloying (BPR 10:1, 400 RPM, 5 h) followed by studied by various researchers [12, 31–34]. The compac-
compaction at 1000 MPa and sintering at 620, 640, 660, tion and densification behavior of Al–Al2O3 [35], Al–TiC
680 °C. The composite sintered at 680 °C produced good [36], Al–TiO2 [32], and Al–SiC [31] have been studied
mechanical properties, homogeneous distribution and intensively, whereas very limited studies have been made
densification was observed due to mechanical alloying. on Al6061/B4C/BN hybrid composites.

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Metals and Materials International (2021) 27:4841–4853 4843

The present research aims to investigate the microstruc- remaining matrix material. All the elemental powders and
tural characteristics, compressibility, sinterability, and reinforcement are supplied by Lobachemie Pvt. Ltd, Mum-
mechanical properties of the Al6061/B4C/BN hybrid com- bai, India. The composites were fabricated with (2, 4, 6, 8)
posites with (2, 4, 6, 8) wt% of B
­ 4C and 2 wt% BN fabricated wt% of ­B4C and 2 wt% BN in a high energy ball mill. To
through powder metallurgy technique. As boron carbide maintain good wear resistance as well as ductility, ­B4C and
is a hard ceramic material, the addition of a high amount BN content were limited to 8 wt% and 2 wt% respectively
(> 8 wt%) of boron carbide to the aluminum matrix reduces [28]. 2 wt% of BN was carefully chosen to ensure that there
the compressibility and sinterability of the composites is no residual ash to interface with bonding during sinter-
resulting in the reduction of mechanical strength [37]. High ing. The soft alloy matrix was completely embedded by the
content of B­ 4C ceramic particles in the aluminum matrix reinforcement, using the high energy ball milling. The mill-
causes poor wettability, splitting of hard ceramic reinforce- ing experiments were carried out in a four station planetary
ment off the matrix and co-ordination ability between B ­ 4C ball mill (Retsch PM 400). Hardened tungsten carbide balls
reinforcement and aluminum matrix [38, 39]. Thus with a of 10 mm diameter and a total mass of 355.26 g were used.
high content of ­B4C, fabrication of the Al/B4C matrix will Tungsten carbide jars of 250 ml capacity were filled with
be difficult. From the literature review, it was found that 35.52 g of Al6061/B4C/BN powders in the ball to powder
increasing boron carbide content above 8 wt% reduces the ratio (BPR) of 10:1 and toluene ­(C6H5CH3) was added to
ductility of the composites during compressive loading. To avoid any chemical reaction. The milling speed was set to
regain the ductility within the composites, 2 wt% of boron 300 rpm. The mechanical alloying time was limited to 10 h,
nitride (a solid lubricant) was used to ensure that there is as there is a very slight decrease in crystallite size and a very
no residual ash to interface with bonding during sintering. negligible increase in lattice strain during further milling of
The samples were fabricated by mechanical milling and then the powders [36]. However, to avoid overheating, 30 min of
consolidated at various compaction pressures and sintered at cooling was done after each hour of milling. After the mill-
different temperatures. The effect of B­ 4C and BN reinforce- ing process, the powder obtained was dried and transferred
ments on the compressibility, sinterability and mechanical to airtight containers to avoid any oxidation.
properties were studied and the compressibility curves were
plotted using Heckel, Panelli-Filho and Ge equations. 2.1 Compaction and Sintering

Al6061/B4C/BN milled powders were compacted into cylin-

2 Experimental Procedure drical shapes of diameter 25 mm and 5 mm height using
closed circular cavity compaction die sets in a hydraulic
Aluminum 6061 alloy was produced by mixing highly pure compression system with a 100-ton capacity. The walls of
(more than 99%) elemental powders as shown in Table 1. the die were lubricated using zinc stearate and the powders
The base matrix was reinforced using ­B4C and BN powders were compressed at 200, 400, 600, 800 MPa. The green
having an average particle size of 140 and 325 mesh respec- components obtained were further sintered at 400, 500,
tively. The characteristics of B
­ 4C and BN powders are shown 600 °C for 3 h in an endothermic atmosphere with a heating
in Table 2. The pure aluminum was considered as the major rate of 10 °C min−1 and were furnace cooled. Due to shrink-
matrix material and other elements such as iron, magnesium, age after sintering the diameter of the fabricated composite
copper, silicon, chromium, zinc, titanium and manganese as was found to be 24.67 mm. Figure 1 represents the powder

Table 1  Elemental composition Elements Fe Cr Si Cu Mg Mn Ti Zn Al

of aluminum 6061 alloy
Purity 99.6 99 99.5 99 99 99 99 99 99
Element wt% 0.700 0.195 0.600 0.275 1 0.150 0.150 0.250 Bal
Mesh size − 325 − 325 − 325 − 325 − 325 − 325 − 325 − 325 − 325

­ 4C
Table 2  Characteristics of B Reinforcement Mesh size Purity (%) Density Hardness Tensile Young’s Melting
and BN (g cm−3) (GPa) strength modulus point
(MPa) (GPa) (K)

B4C − 325 99 2.51 44 569 472 2780

BN − 140 99 2.30 3 83 100 3400

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4844 Metals and Materials International (2021) 27:4841–4853

Fig. 1  Powder metallurgy process

metallurgy process. Archimedes principle was used to cal- 78.22 confirm the presence of aluminum (JCPDS 85-1327,
culate the actual densities of obtained sintered components. 65-2869). The miller indices of these peaks are found out to
be (111), (200), (220), (311) respectively. At the 2θ angle
2.2 Characterization and Hardness Measurement of 82.44, a small peak of ­B4C crystal was found, which
confirms with JCPDS (75-0424). It was confirmed that
The Al6061/B4C/BN composite samples were finely pol- aluminum matrix and ­B4C phases were formed during the
ished using diamond paste and micro cloth and were mechanical alloying process. A very negligible peak was
observed under field emission scanning electron micro- observed at 2θ angle of 43.88 with miller indices of (101)
scope (Merlin Compact FESEM, Carl Zeiss, Germany) for which confirms the presence of BN (JCPDS-73-2095). The
morphological properties. Energy Dispersive Spectroscopy intensities of the ­B4C and BN peaks were low due to low
(EDS) was to evaluate any microstructural changes in the wt% of BN and B ­ 4C in the aluminum matrix. As the wt% of
metal matrix composite. XRD analysis (Shimadzu XRD- ­B4C is increased, there was a gradual decrease in the inten-
7000) was carried out for the hybrid composites powders sity of aluminum matrix peaks. This is due to the structural
with a scanning range of 2θ = 10° to 90° using Cu Kα refinement and a decrease in the lattice parameter of the alu-
(λ = 1.5406 Å) radiation, operating at 30 mA and 40 kV at minum matrix. From the XRD patterns, it can be confirmed
a scanning speed of 2° per min. Optical microscope (Leica that aluminum, ­B4C, and BN peaks were found, with AlC
Microsystems, Germany) was used to study the grain size and AlN as secondary phases. Peaks for Mg, Si, etc. related
analysis using ASTM E112 three circles method. The hard- to Al6061 alloy were not detected due to low wt% in the
ness of the composite was calculated according to ASTM aluminum matrix.
E381 using Vickers hardness tester at 1 kg load for a dwell X-ray diffraction peak profile analysis is a powerful and
time of 10 s. The average hardness value was taken from 5 simple method in evaluating the broadening of peak with
different indentations. The error was within 5% for the hard- lattice strain and crystallite size due to dislocation. Instru-
ness measurement. mental broadening must be analyzed for accurate analysis
of crystallite size and lattice strain effects. A standard mate-
rial such as A­ l2O3 was used and the diffraction patterns of
3 Results and Discussion the material was analyzed to determine the instrumental
broadening [40] 𝛽hkl , the instrumental corrected broadening
3.1 Evolution of Powder Morphology and Structural of different diffraction peak of Al was calculated using the
Analysis following relation:
]1∕2
The Al6061/B4C/BN powder morphology with a milling
2
(1)
[( ) ( 2 )
𝛽hkl = 𝛽hkl measured − 𝛽hkl instrumental
time of 10 h is presented in Fig. 2. It can be observed that in
Fig. 2a, b due to low B­ 4C content the particles exhibit ductile From the XRD peaks of Al (111), (200), (220), (311),
behavior and the particles changed to flat morphologies due the average crystallite size was calculated based on the
to severe plastic deformation. In Fig. 2c, d, with the increase Debye–Scherrer equation [41].
in wt% of ­B4C reinforcements in the aluminum matrix, the k𝜆
brittle fracturing of the particles becomes a significant pro- D=
𝛽hkl cos 𝜃 (2)
cess that breaks the particles resulting in an almost equiaxed
and spherical shape. where D is the crystallite size, shape factor (k) = 0.90 which
X-ray diffraction of the Al6061/B4C/BN mechanically is a constant, (λ = 1.54) wavelength of X-ray, βhkl is an inte-
milled powders is shown in Fig. 3 for four different compo- gral half-width, θ is the Bragg angle. The crystallite size is
sitions. The peaks at the 2θ angle of 38.47, 44.72, 65.13 and the size of a coherently diffracting domain and is not the

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Metals and Materials International (2021) 27:4841–4853 4845

Fig. 2  Powder morphologies of a 2 wt%, b 4 wt%, c 6 wt% and d 8 wt% ­B4C and 2 wt% BN powders milled for 10 h

same as the particle size [42]. The amount of defects in the time. The crystallite size steadily decreases with an increase
sample is the dislocation density (δ) per unit volume of the in wt% of B ­ 4C reinforcement due to the presence of hard
crystals and presented as: ceramic ­B4C which helps to refine the matrix. The lattice
strain in the Al6061/B4C/BN composite increases with an
1
𝛿= (3) increase in the wt% of B ­ 4C reinforcement. During severe
D2
plastic deformation (SPD), the applied strain is much higher,
where δ is the dislocation density, D is the crystallite size. which reduces the formation of new dislocations. The severe
The lattice strain was calculated using the Williamson Hall plastic deformation also increases the stacking fault energy,
analysis [43]. enhancing the vacancy concentration and the twin formation
[36, 44, 45].
k𝜆
[ ]
𝛽hkl . cos 𝜃hkl = + 4𝜀. sin 𝜃hkl (4) The field emission scanning electron microscope
D (FESEM) micrographs of polished Al6061–8 wt%
where shape factor (k) = 0.90, λ = 1.54 (X-ray wavelength), ­B4C–2 wt% BN is shown in Fig. 4. The figures represent the
D is crystallite size, 𝜃hkl is the Braggs angle, and ε is the distribution of ­B4C and BN reinforcements in the fabricated
lattice strain. The full width half maximum was calculated composites. Better dispersion of B ­ 4C is essential for excel-
based on the 2θ value. The miller indices of Al were used to lent mechanical properties like hardness and wear resist-
plot a linear plot of 𝛽hkl . cos 𝜃hkl with 4𝜀. sin 𝜃hkl . The lattice ance. To analyze the different elements present in Al6061/
strain was calculated from the slope (m = ε). Table 3 repre- B4C/BN hybrid composites, Energy dispersive X-Ray spec-
sents the change in lattice strain, crystallite size, and dislo- troscopy (EDS) was conducted and shown in Fig. 5. EDS
cation density as a function of ­B4C wt% at 10 h of milling image confirms the presence of aluminum, boron, carbon
and some traces of titanium being a compositional material

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4846 Metals and Materials International (2021) 27:4841–4853

Fig. 3  XRD analysis of Al6061/

(111)
B4C/BN mechanically milled
powders ♦ ∗ B4C

(200)
• ΒΝ

(128)
(220 )

(311)
♦

(101)
♦AlC
♦AlN

♦AlC
• ♦ ♦ ∗ ♦ Al
Al6061-8%B4C-2%BN

Intensity (a.u)
Al6061-6%B4C-2%BN

Al6061-4%B4C-2%BN

Al6061-2%B4C-2%BN

20 30 40 50 60 70 80 90
2θ
θ Angle

Table 3  Structural analysis of Al6061–x wt% B

­ 4C–2 wt% BN after of the Al6061 alloy. Also, it is observed that there is no trace
10 h of milling. (x = 2, 4, 6, 8) of oxygen element found in the composites.
Composition Crystallite Disloca- Lattice
size (nm) tion density strain 3.2 Analysis of Compressibility and Sinterability
(δ) × 10–4(nm−2) (ε) × 10–3 Behavior of the Composites
Al6061–2% ­B4C–2% BN 72.23 1.91 1.51
Al6061–4% ­B4C–2% BN 65.36 2.34 1.69
In the powder metallurgy process, the characteristics of
Al6061–6% ­B4C–2% BN 59.78 2.79 1.75
the green compact influence the mechanical and physi-
Al6061–8% ­B4C–2% BN 51.23 3.91 1.89
cal properties of the final product. The characteristics and

Fig. 4  a Polished surface of Al6061–8 wt% ­B4C–2 wt% BN composites compressed at 800 Mpa and sintered at 600 °C and b zoomed view of
the composite

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Fig. 5  EDS analysis and elemental mapping of Al6061–8 wt% B

­ 4C–2 wt% BN hybrid composites

quality of the green compacts are governed by the densi- their morphology, size, shape, formability, porosity, fric-
fication mechanism and the deformation behavior of the tion, distribution of reinforcement particulates, applied
powder during compaction [44, 46]. The compressibility pressure, etc. [34–36, 44–46]. An increase in compres-
of the particle reinforced matrix is comparably lower than sion pressure increases the density by lowering the poros-
the unreinforced matrix, which results in lower strength ity between the particles. To evaluate the compaction and
to support secondary processing methods like extrusion densification behavior of a hybrid composite, empirical
and rolling [44–46]. Therefore, the study on the compress- equations are used to develop relationships between the
ibility of reinforced powders is important to know the den- relative density of the compacted material and the applied
sification process during the high-pressure compactions. pressure. According to the literature survey, Heckel [47],
The compressibility of the powder is directly affected by Panelli Filho [48], and Ge [49] empirical equations can be

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4848 Metals and Materials International (2021) 27:4841–4853

effectively applied to the particle reinforced MMC [12, 35, considering that the hard ­B4C ceramic particles cause a
36, 44, 45, 50]. The compressibility equations are stated detrimental effect of the clustered powder during SPD. To
below: study the compressibility and densification behavior of the
Al6061/B4C/BN hybrid composites, empirical equations
1
( )
Heckel: ln = K1 P + B1 (5) like Heckel, Panelli-Filho, and Ge were used. Figure 6b–d
1−D
shows the compressibility behavior of Al6061/B 4C/BN
hybrid composites compacted at pressures ranging from
1 200 to 800 MPa. The densification co-efficient (K) and ­R2
� � √
Panelli-Filho: ln = K2 P + B2 (6)
1−D values are represented in Table 4. The higher the densi-
fication co-efficient higher the plastic deformation of the
1 material. The correlation coefficient (­ R2) is almost equal to
[ ( )]
Ge: Log ln = K3 log (P) + B3 (7)
1−D unity which implies that the ­B4C particulates influence the
where ­K1, ­K2, ­K3 are densification co-efficient, D is the deformation of the composites. In the heckle equation it
relative density of green compacts. P is the compression can be observed that the R ­ 2 values are almost greater than
pressure and B ­ 1, ­B2, ­B3 are the density of milled powders 0.99 for all the composites in comparison to Panelli-Filho
without any compaction pressure. The mechanism of powder and Ge equations. Thus Heckel equation can be used for
consolidation can be explained in two steps; (1) rearrange- higher accuracy of predictions for the densification rates. It
ment of powders due to sliding mechanism (2) initialization can be observed from Fig. 6 that at lower compaction pres-
of plastic deformation as the compaction pressure increases. sures the compressibility curves converge. This is due to
At the early stage of compression, the powder particles slide a decrease in friction at lower compaction pressures. This
over each other and rearrangement occurs. The sliding of can be a limitation of the empirical equations due to which
these particles found to be limited, with the increase in the accurate densification mechanisms cannot be predicted at
compaction pressure inducing the plastic deformation. In lower compaction pressures. The variation of density with
these stages the powder morphology, distribution and parti- applied compaction pressures shows a good agreement
cle size plays a crucial role in determining the densification between the experimental and the predicted results [12,
behavior of the compacted material. Both the step i.e. rear- 34, 46]. Table 5 and Fig. 7 shows the sinterability of the
rangement of particle and plastic deformation can occur at Al6061/B4C/BN hybrid composites sintered at 400, 500,
the same time. The compaction pressure was varied from 600 °C. The sinterability of the Al6061/B 4C/BN hybrid
200 to 800 MPa with an interval of 200 units. The green composites was evaluated by the following equation:
density of the compacted samples was measured by the (
𝜌 s − 𝜌g
)
Archimedes principle. 𝜓= (8)
𝜌th − 𝜌g
The compaction behavior of the fabricated composites
shows that at the early stage of compaction high densifi- where 𝜓 is the sinterability of the hybrid composites, 𝜌th is
cation is observed. When the hard B ­ 4C ceramic particles the theoretical density, 𝜌s is the sintered density, 𝜌g is the
are added to the Al6061 matrix the disintegration of the green density. The theoretical density of aluminium, ­B4C,
cluster under high compression pressure occurs resulting and BN were considered as 2.7 g cm−3, 2.51 g cm−3, and
in void filling within particles. To enhance the ductility of 2.3 g cm−3 respectively. The density of the sintered com-
the composites boron nitride was added to exhibit good posites increased with an increase in sintering temperature.
compressibility. The densification is improved at the early With an increase in wt% of B ­ 4C particles the sinterability of
stages of compaction because the fine BN particles fill up the composites decreases. The highest sinterability can be
the pores within the aluminum matrix. The low density of observed at a sintering temperature of 600 °C.
the aluminum matrix also helps in restacking and sliding
at early compaction stages. As shown in Fig. 6a with an
increase in B­ 4C wt% the densification rate decreased. This 3.3 Hardness and Compressive Strength
is due to the decrease in the transmission of pressure from
the reinforcement to the aluminum matrix with a network The compressive strength and Vickers hardness of the com-
of pores inside the matrix [33, 46]. The formability of the posites as a function of ­B4C content are shown in Table 6.
aluminum matrix became limited with the formation of a The compressive strength increased from 123 to 249 MPa
network of pores and particle clusters, which reduces the for the composite Al6061–8 wt% ­B4C–2 wt% BN. The
compaction pressure applied to it. The plastic deformation stress–strain curves during compressive loading are shown
behavior has a very negligible contribution to the densifi- in Fig. 8a. The hybrid composites showed ductile behavior
cation mechanism. The above observation can be justified at low ­B4C content and brittle behavior at higher ­B4C con-
tent. BN helped to maintain ductility during the increase of

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(a) (b)

(c) (d)

Fig. 6  a Relative density of the green compacts, compressibility behavior of the Al6061/B4C/BN hybrid composites using various compaction
equations, b Heckel equation, c Panelli-Filho and d Ge equations

Table 4  Analysis of Sl. no. Composition Heckel Panelli Ge

densification co-efficient (K)
and ­R2 values of different K, ­MPa−1 R2 K, ­MPa−0.5 R2 K, ­MPa−1 R2
compaction equations for
1 Al6061–2% ­B4C–2% BN 0.0029 0.992 0.064 0.995 0.328 0.995
Al6061/B4C/BN hybrid
composites 2 Al6061–4% ­B4C–2% BN 0.0027 0.993 0.059 0.994 0.310 0.992
3 Al6061–6% ­B4C–2% BN 0.0025 0.993 0.053 0.975 0.302 0.967
4 Al6061–8% ­B4C–2% BN 0.0023 0.994 0.049 0.983 0.296 0.975

­ 4C content [28]. The increase in strength was attributed to

B content. Maximum hardness of 184 HV was obtained from
the embedding of reinforcement particles to aluminum 6061 Al6061–8 wt% ­B4C–2 wt%BN at a sintering temperature
matrix. Figure 8b shows the Vickers hardness of Al6061/ of 600 °C. The hardness increment was due to grain refine-
B4C/BN metal matrix hybrid composites as a function of ment and uniform distribution of ­B4C and BN in the alu-
sintering temperature and ­B4C content. The graph shows a minum 6061 matrix. The grain size analysis was performed
positive correlation between sintering temperature and ­B4C according to the ASTM E112 three circles method. The

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Table 5  The sinterability behavior of Al6061/B4C/BN hybrid composites sintered for 3 h

Sl. No. Composition Theoretical Green den- Sintered density (𝜌s) Sinterability (𝜓 )
density (𝜌th) sity (𝜌g)
400 °C 500 °C 600 °C 400 °C 500 °C 600 °C

1 Al6061–2% ­B4C–2% BN 2.684 2.475 2.52 2.54 2.57 0.22 0.31 0.45
2 Al6061–4% ­B4C–2% BN 2.681 2.445 2.49 2.52 2.56 0.19 0.32 0.49
3 Al6061–6% ­B4C–2% BN 2.677 2.420 2.46 2.48 2.51 0.16 0.23 0.35
4 Al6061–8% ­B4C–2% BN 2.674 2.400 2.42 2.45 2.48 0.07 0.19 0.29

pile up behind the ­B4C particles. Thus, the uniform distribu-

tion of dislocation enhances the hardness and compressive
strength of the metal matrix hybrid composites [52].

4 Conclusion

The present work elucidates the influence of B ­ 4C and BN

reinforcements on structural characterization, compressibil-
ity, sinterability, and mechanical properties of Al6061/B4C/
BN metal matrix hybrid composites prepared by mechani-
cal milling. The following observations were found in this
study:

• XRD of the milled powders showed that no contamina-

tion was found during the mechanical alloying process.
Fig. 7  Sinterability of the fabricated composites w.r.t sintering tem- EDS results showed some trace of titanium, as it is the
perature and ­B4C content compositional material for Al6061 alloy.
• From XRD analysis it was found that the crystallite
average grain size was found to be 2.98 μm and 3.049 μm size steadily decreases with an increase in wt% of B ­ 4C
for Al6061–8 wt% ­B4C–2 wt% BN hybrid composite sin- reinforcement due to the presence of hard ceramic ­B4C
tered at 500 °C and 600 °C respectively. It can be observed which helps to refine the matrix. The lattice strain in
from Fig. 9 that the hard ­B4C particles prevent the grain the Al6061/B4C/BN milled powders increases with an
growth by seizing the grain boundary by Zenner pinning, increase in wt% of ­B4C reinforcement
which helps in the refinement of grains and enhancement in • The densification co-efficient (K) decreased with
mechanical properties [51, 52]. According to the Hall–Petch an increase in B ­ 4C reinforcement. The densification
and Orowan mechanism, the presence of ­B4C reinforcement improved at the early stages of compaction as the fine BN
and the refinement of grains, there is an enhancement of the particles fill up the pores within the aluminum matrix.
compressive strength of the fabricated material. Precipita- The sinterability of the Al6061/B4C/BN hybrid compos-
tion hardening occurs in the composites as the hard ­B4C ites increased with an increase in sintering temperature
particles prevent the dislocation motion, creating dislocation but decreased with increase ­B4C wt% in the matrix

Table 6  Vickers hardness and Sl. no. Composition Green compressive Vickers hardness (HV)
green compression strength of strength (MPa)
Al/6061/B4C/BN composites at
different sintering temperatures 400 °C 500 °C 600 °C

1 Al6061–2% ­B4C–2% BN 123 128 132 138

2 Al6061–4% ­B4C–2% BN 181 140 149 162
3 Al6061–6% ­B4C–2% BN 204 158 165 177
4 Al6061–8% ­B4C–2% BN 249 168 176 184

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(a) (b)

Fig. 8  a Stress–strain curves during compressive loading and b Vickers hardness of Al6061/B4C/BN composites

­ 4C–2 wt% BN sintered at a 500 °C and b 600 °C.

Fig. 9  Optical micrograph (color image) showing grain size analysis of Al 6061–8 wt% B
(Color figure online)

• The average grain size was found to be 2.98 μm and resistance applications like brake pads, ballistic protec-
3.049 μm for Al6061–8 wt% ­B4C–2 wt% BN hybrid tion of tanks armor, automotive sector and in nuclear
composite sintered at 500 °C and 600 °C respectively. industries
The hard ­B4C particles prevented the grain growth by
seizing the grain boundary by Zenner pinning, which
helps in the refinement of grains and enhancement in Acknowledgements The authors would like to acknowledge Dr. S.K.S
Parashar (Nano Synthesis Lab, School of Applied Science) and School
mechanical properties of Mechanical Engineering, KIIT Deemed to be University, Bhubane-
• The hardness and compressive strength of the composites swar, India for their metal powder synthesis, composite fabrication
increased up to 184 HV and 249 MPa respectively for the and testing facilities.
Al6061–8 wt% ­B4C–2 wt% BN composites due to the
presence of hard ceramic B­ 4C reinforcement. The relative
density of the composites decreased with the increase in
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