Titanium diboride reinforced Aluminum composite as a robust material for automobile

applications

Srisaran Venkatachalam1*, S.Baskaran1, R.S.Karrthik1, Deepak B. Thimiri Govinda Raj2,3, T.

Ramesh Kumar 4
1
Department of Mechatronics, Bannari Amman Institute of Technology, Sathyamangalam,
Tamil Nadu – 638401, India
2
Oslo University Hospital, Oslo, Norway
3
Envirotransgene® Biosolutions Global, Chennai, India
4
Department of Mechanical Engineering, Bannari Amman Institute of Technology,
Sathyamangalam, Tamil Nadu – 638401, India

* Corresponding author: srisaran@bitsathy.ac.in

Abstract: Aluminum composites are largely used in automobile industries in light of their
lightweight and corrosion free characteristics. In this work, Titanium diboride (TiB2) particles
were reinforced in Aluminum (Al) metal matrix via in-situ salt metal reaction technique. The
composite samples were prepared by reinforcing TiB2 particles of 4% and 8% (by wt.) in Al
6061 alloy matrix and subsequently the composites were characterized for their
microstructure, tensile strength, hardness and wear resistance. The Aluminum 6061 alloy is
found to have tensile strength 114 N/mm2, hardness 30 (Rockwell number) and wear loss of
159 m. It was observed that the mechanical properties of TiB2 reinforced Al 6061 alloys,
especially tensile strength and hardness have been improved to 172 N/mm2 and 54,
respectively, up on addition of 8% TiB2. Moreover, the samples having highest weight
percentage of reinforcement show remarkable wear resistance by pin-on-disc method. Thus
TiB2-Aluminum composites are in foster competition with high performance materials used
as disc brake in automobiles.

Keywords: Metal matrix composites, aluminum alloys, tensile strength, wear resistance,
hardness, and microstructure

1. Introduction

Among automobile manufacturers, in recent times, a paramount importance has been given
to less fuel consumption of the vehicles by utilizing lightweight and high strength materials.
New materials have therefore been evolved to meet many of the challenges presented by
the demands of consumers and legislators[1]. As recently as twenty years ago the
bodywork, chassis and transmission of the average vehicle consisted almost entirely of steel
and cast iron. Now many new materials are being used by the automobile industry non-
ferrous metals, plastics, ceramics and new types of steel and rubber[2]. The exceptional
properties of these materials have made major contribution to passenger comfort and safety,
to the lifespan of the components and to fuel economy.

In the case of conventional materials like steel there are lots of problems like heavy weight,
corrosion, wear resistance, vibration, manufacturing problems. Metal matrix composites are
today widely used to design the automobile components in view of their better performance

1
compared to other composites. Because of improved physical, mechanical, tribological and
thermal characteristics of metal matrix composites those problems can be solved to some
extent[1].

Metal matrix composites (MMCs) have been used commercially in the automotive market for
nearly twenty years[3]. In comparison with conventional polymer matrix composites, MMCs
are resistant to fire, can operate in wider range of temperatures, do not absorb moisture,
have better electrical and thermal conductivity, are resistant to radiation damage, and do not
display out gassing [2]. On the other hand, MMCs tend to be more expensive, the fiber-
reinforced materials may be difficult to fabricate, and the available experience in use is
limited[4].

MMCs are made by dispersing a reinforcing material into a metal matrix. The reinforcement
surface can be coated to prevent a chemical reaction with the matrix[3]. For example, carbon
fibers are commonly used in Aluminum matrix to synthesize composites showing low density
and high strength. However, carbon reacts with Aluminum to generate a brittle and water-
soluble compound on the surface of the fiber. This work demonstrates that Aluminum matrix
composites can be used as brake rotor rather than grey cast iron in automobiles.

2. Experimental

The elemental composition of the raw material (Al 6061 alloy) was experimentally
determined using optical emission spectroscopy (OES). Prior to the analysis, the surface of
the sample was polished. A spark was introduced on the specimen’s polished surface while
it is flooded with Argon gas. As a consequence, the sample surface evaporates and emits
light (photons). The signals are then recorded by an optical spectrometer which provides a
quantitative elemental analysis of the metal sample.

For microstructure analysis, the specimen preparation undergoes the following steps (i)
grinding with SiC abrasive paper of 240 grit -1200 grit, (ii) polishing by diamond paste on
rotating cloth wheel, (iii) etching the specimen using the reagent (a mixture of 1g of sodium
hydroxide pellets and 4g of potassium permanganate in 100ml distilled water), (iv) washing
in acetone and drying. The metallographic images were obtained using optical microscope
using objective lens of magnification100.

Uniaxial tensile test was performed to obtain mechanical parameters such as ultimate
strength, yield strength, % elongation, % area of reduction and Young’s modulus. In
general, the tensile testing is carried out by applying longitudinal or axial load at a specific
extension rate to a standard tensile specimen with known dimensions till failure. Figure 1
depicts a schematic diagram of the specimen with its dimensions used for tensile test. The
gauge length was 30 mm and cross sectional area perpendicular to the load direction was 7
mm.

Figure 1 Dimensions of the specimen for tensile test

2
The specimen is placed in the machine between the grips and an extensometer. Once the
machine is started it begins to apply an increasing load on specimen. The applied tensile
load and extension were recorded during the test for the calculation of stress and strain. This
method not only records the change in length of the specimen but also all other extending or
elastic components of the testing machine and its drive systems including any slipping of the
specimen in the grips.

Hardness of the samples was measured using indentation based Rockwell method. It
consists of indenting the test material by a hardened steel ball indenter. The indenter (1/16”
steel ball) is forced into the test material under a preliminary minor load F0 (10Kgf). When
equilibrium has been reached, an indicating device, which follows the movements of the
indenter and so responds to changes in the depth of penetration of the indenter, is set to a
datum (zero reference) position. While the minor load is still applied, an additional major load
(100 kgf) was applied which resulting increase in penetration. At equilibrium, the major load
was removed while the maintaining the minor load. In fact, removal of the additional major
load allows a partial recovery, thereby reducing the depth of penetration. The major load
removed is related to the Rockwell hardness number.

The dry sliding wear test was performed using a pin-on-disk method at the room
temperature. Before conducting the tests, sample surfaces are polished and cleaned with
acetone and dried. Materials were tested in pairs under nominally non-abrasive conditions.
Both wear and coefficient of friction were measured with electronic sensors and
subsequently recorded on PC for further investigations. Usually, the amount of wear
depends upon a number of factors such as applied load, sliding speed, sliding distance,
environment and material properties. Two specimens are required for the test: a pin with a
flat tip made up of composite material and a flat circular disc made up of chromium steel.
The size of the pin was 6 mm width, 6 mm thickness and 50 mm long, whereas the disc was
160 mm in diameter and thickness of 10 mm. The pin was positioned perpendicular and
forced against the revolving disc specimen with a required load. So that the wear track on
the disc is a circle, involving multiple wear passes on the same track. The DUCOM software
and data acquisition system allows measuring applied test load, speed and friction. The disc
slides over the bottom surface of specimen and wear take place.

3. Results and Discussion

3.1 Composite fabrication

Table 1 displays the elemental composition of Aluminum (Al 6061) alloy sample obtained
from optical emission spectroscopy
Table 1 Chemical Composition of Al 6061 Alloy

Elements Mg Si Fe Mn Cu Cr Zn Ni Ti Al
% 1.03 0.65 0.173 0.349 0.52 0.006 0.007 0.043 0.023 97.2

The major constituent of the raw material matrix is Aluminum (Al) 97.2% along with fractions
of Magnesium (Mg)~1.03 %, Silicon(Si) ~0.65%,Copper (Cu) ~0.52%, Manganese (Mn)

3
~0.349%, Iron (Fe) ~0.173 % and traces of Chromium (Cr), Zinc (Zn), Nickel (Ni) and
Titanium (Ti) <0.1 %.

Aluminum (Al) matrix composite materials were fabricated via stir casting in which the
dispersed phase is mixed with a molten matrix metal by means of mechanical stirring [5].
The liquid composite material is then cast by conventional methods and then subsequently
processed by conventional metal forming technologies. One such sample after casting is
shown in Figure 2.

Figure 2 Photograph of casted Al 6061 alloy sample

In this work, the particulates were synthesized through a chemical reaction process as
shown in Figure 3.

Figure 3 Fabrication of in-situ composite using Halide salts and Aluminum alloy
matrix

The reaction undergoes between the titanium containing K2TiF6 and the boron containing
KBF4 salts in the presence of molten Aluminum 6061 alloy, as follows in equation 1:

K2TiF6 - Ti + Al 6061 = Al-TiB2 (1)

KBF4 - B

During the in-situ reaction process, the elements Ti and B are introduced from the two salts
into the molten Aluminum and made to react within it. The salts are mixed in stoichiometry to
form TiB2 as it is the only inter-metallic phase to be formed by the reaction.

3K2TiF6 + 22Al + 6KBF4 3Al3Ti + 3AlB2 + 9KAlF4 + K3AlF6 + Heat (2)

4
3Al3Ti + 3AlB2 12Al + 3TiB2 (3)

Based on the molecular weight of the constituents, the reinforcement weight can be
calculated as follows,
𝑥 × 𝑑𝑖𝑒 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦
𝑅𝑒𝑖𝑛𝑓𝑜𝑟𝑐𝑒𝑚𝑒𝑛𝑡 𝑤𝑒𝑖𝑔ℎ𝑡 = 100−𝑥
(4)

Where ‘x’ refers to the reinforcement weight in % and die capacity is 1250g.

The amount of salt needed can be estimated from the expressions below,

𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐾2 𝑇𝑖𝐹6 ×𝑟𝑒𝑖𝑛𝑓𝑜𝑟𝑐𝑒𝑚𝑒𝑛𝑡 𝑤𝑒𝑖𝑔ℎ𝑡

𝐾2 𝑇𝑖𝐹6 = 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑇𝑖𝐵2
(5)

2.4 ×𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐾𝐵𝐹4 ×𝑟𝑒𝑖𝑛𝑓𝑜𝑟𝑐𝑒𝑚𝑒𝑛𝑡 𝑤𝑒𝑖𝑔ℎ𝑡

𝐾𝐵𝐹4 = 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑇𝑖𝐵2
(6)

The atomic weight of the constituents which are present in the reinforcement is listed in the
Table 2.
Table 2 Atomic Weight of Constituents

Elements Atomic weight (g/mol)

Al 26.9815
Ti 47.867
K 39.0983
F 18.9984
H 1
B 10.81
O 16

The molar weight of the constituents which are present in the reinforcement is listed in the
Table 3.
Table 3 Molar Weight of Reinforcement

Salts Molar weight (g/mol)

K2TiF6 240.054
KBF4 125.9029
TiB2 69.49
For producing in-situ composite, Aluminum stir casting equipment is used. Wolfra coating is
applied on the surface of the furnace in order overcome unwanted chemical reactions with
the previously casted particles inside the furnace. Al 6061 is supplied in the form of rods at
810°C then the pre-weighed salts are added into the molten aluminum alloy and stirred
continuously. The process is continued for about 40 minutes, the salts synthesized internally
with molten alloy and finally it is allowed to solidify in order to get TiB2-Al composite. The
required specimens are prepared for evaluation of mechanical properties. Usually, the size
of the particulates is more than 1 μm, such that it strengthens the composite in two ways. In
the first one, particulates carry the load along with the matrix materials, whereas the second

5
one involves formation of incoherent interface between the particulates and the matrix. A
larger number of dislocations are generated at the interface, eventually the material gets
strengthened. The degree of strengthening depends not only on the amount of particulate
(volume fraction), but also on its distribution, size, shape of the particulates and so on.

3.2 Microstructure

Figure 4 shows metallography optical microscopy images of the cast Al 6061 alloy matrix
(4a) and composites (4b, 4c, & 4d) reinforced with different weight percentage of TiB2. The
process of cooling during solidification results in the formation of eutectic phase in the
Aluminum matrix. As shown by arrows in Figure 4a, two distinct phases has been identified:
the primary phase Aluminum, and dendrite like structures are seem to be eutectic mixture
[5]. The secondary phase could occur due to the presence excess of silicon and magnesium
in the raw material, thereby forming stable binary or ternary compounds such as Mg 2Si or
Fe3SiAl2, respectively [5].

a) b)

50 m 50 m

c) d)

50 m 10 m

Figure 4 Optical microscopy images acquired from a) cast Al 6061 alloy, b) Al-4%TiB2, c) Al-
8%TiB2 and d) Al-8%TiB2 (magnified)

Upon addition of salts (K2TiF4 and KBF4) to the Aluminum alloy during stir casting process,
reinforcing TiB2 particles were formed instantly as detailed in equations (3) and (4). From the
figures 4b, 4c, and 4d, it can be seen that the reinforcement particles are discontinuous,
randomly dispersed with varying sizes of non-uniform shapes, but well-distributed over the Al
6061 alloy matrix. This homogeneous distribution was due to well controlled parameters
namely the stir rate and stir time during the casting process. Furthermore, the existence of
needle like structures could originate from formation of intermediate compound Al3Ti.

6
3.3 Hardness

The Rockwell hardness values of the Al 6061 alloy and its composites with TiB2 are shown in
the Table 4 and in Figure 5.

Table 4 Hardness Values of the Al 6061alloy and its composites

Composite samples Rockwell hardness number
Al 6061 alloy, no reinforcement 30
Al-4%TiB2 43
Al-8%TiB2 54
Al-12%TiB2 56*

The Rockwell’s hardness number of casted alloy matrix is found to be about 30, which is
then augmented to 43 by adding 4 % weight of reinforcement. Thus, the significant
improvement in the hardness of the composite when compared with the Al 6061 alloy can be
attributed to the presence and distribution of TiB2 particles in the matrix. It can be noted that
the increment in hardness number is not a linear function of weight percentage of
reinforcement. At higher fractions of reinforcement, distribution of the secondary phase may
not be homogeneous, and thus leading to segregate as local agglomerates/islands.

Figure 5 Hardness of Al alloy and its composite with TiB2

3.4 Tensile Strength

Table 5 shows the tensile strength of the Aluminum alloy and composite. For comparison,
the tensile strength of grey cast iron has also been included.

Table 5 Tensile strength of the Aluminum composites against grey cast iron

Composite samples Tensile strength (N/mm2)

Al 6061 alloy 114
Al-4%TiB2 156
Al-8%TiB2 172
Al-12% TiB2 178
Grey iron 284

7
The Al 6061 alloy possesses tensile strength of 114 N/mm2, which is almost 60 % lower than
the tensile strength of grey cast Iron. For certain applications say automobile brake drum or
rotor, the material should possess tensile strength as strong as grey cast Iron. However, Iron
has several drawbacks namely heaviness and prone to corrosion. By incorporating TiB2
particles in the Al alloy matrix, the tensile strength has been significantly increased gradually
with increase in weight fraction of the reinforcement. A graphically representation of the
evolution of the tensile strength is shown in Figure 6. Similar to hardness, tensile strength
does not vary significantly between the weights fractions of 8% and 12%. It is not negligible
to ignore the segregation of agglomerates at that composition. The mechanical properties
can be further improved by optimizing the experimental conditions that determines the
segregation of the agglomerates[6].

Figure 6 Tensile strengths of Al 6061 alloy, it composite with TiB2 and grey cast iron

The tensile strength test specimens for unreinforced Al 6061 alloy and composite
materials are shown in the Figure 7.

Figure 7 Photograph showing specimens after tensile strength test

3.5 Wear behavior

Using the pin-on-disc method, the wear loss was measured by pressing the sample onto a
rotating disc under a defined load [7]. Throughout the measurement, the following
parameters were set: the wear track diameter as 80 mm, sliding speed as 1 m/s, disc
rotation speed as 240 rpm, and load as 10N. The results are obtained by conducting test for
a selected time and load. Each sample is tested for duration of 1000 seconds. Figure 8
illustrates the wear characteristics of Al 6061 alloy, Al-4%TiB2 and Al-8%TiB2 specimens,
under dry sliding conditions.

8
 180
Al 6061 alloy
160 Al 6061 alloy + 4% TiB2

140 Al 6061 alloy + 8% TiB2

120
Wear (m)
100

80

60

40

20

0
0 5 10 15 20
Time (min)

Figure 8 Wear characteristics of Al 6061 and itsTiB2 reinforced composites

It is well known that the wear depends on the hardness and strength of the
material[8]. During dry sliding conditions, the specimens experience a relative motion against
the disc under load, thereby causing the wear loss. Table 6 shows the maximum wear loss
values for the Al alloy and the composite materials obtained after 16.667 minutes.

Table 6 Wear of Aluminum alloy and its composites

samples Wear (m)
Al 6061 alloy 159.7
Al-4%TiB2 101.72
Al-8%TiB2 85.04
Al-12% TiB2 80.03

More addition of the TiB2 particulates will reduce the wear loss in the materials. Having
known that the specimen dimensions length, width, and thickness 50x6x6 mm, sliding
distance 1000 m, velocity 1m/s, and load applied 10N. The wear rate can be calculated by
using the following relation (equation 7),

𝑤𝑒𝑎𝑟 𝑙𝑜𝑠𝑠 (𝑔)

𝑤𝑒𝑎𝑟 𝑟𝑎𝑡𝑒 = 𝑔 (7)
𝑆𝑙𝑖𝑑𝑖𝑛𝑔 𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 (𝑚)×𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑤𝑜𝑟𝑛 𝑜𝑢𝑡 𝑚𝑎𝑡𝑒𝑟𝑖𝑎𝑙 ( )×𝑙𝑜𝑎𝑑 𝑎𝑝𝑝𝑙𝑖𝑒𝑑 (𝑁)
𝑚𝑚3

The wear rate for the unreinforced alloy and the composite materials are shown in Table 7.

Table 7 Wear Rate of Aluminum alloy and its composites

Composite samples Wear rate (mm3/N-min)
Al 6061 alloy 0.016
Al-4%TiB2 0.01
Al-8%TiB2 0.008
Al-12%TiB2 0.005
Grey iron 0.001

9
3.6 Analysis of Variance and Linear Regression Analysis

Analysis of Variance (ANOVA) reveals the most influencing design factors that affect the
performance characteristics. Table 8 summarizes the results of ANOVA performed using
Minitab software.

Source DF Adj. SS Adj. MS F-Value P-Value

Regression 2 2498.41 1249.20 785.09 0.025
Hardness (Rockwell) 1 11.47 11.47 7.21 0.227
Wear (μm) 1 76.58 76.58 48.13 0.091
Error 1 1.59 1.59
Total 3 2500.00

The ANOVA was executed for the confidence level 95% and significance level 5%. The p-
value of the wear parameter is less than 0.1 and the hardness parameter is 0.3. It means
that wear parameter has higher percentage of impact than the hardness parameter.

The linear regression equation was formulated by using Minitab statistical software. By this
analysis, the correlation between predicted variable and the response variable can be
identified. In our study, the tensile strength is taken as response variable, whereas the
hardness and wear as predicted variable.

Tensile Strength (N/mm2) = 185.0 + 0.678 Hardness (Rockwell) - 0.5722 Wear (m) (8)

The positive and negative signs of the equation 8 correspond to changes in tensile strength
of the composite. The positive sign indicated increase in tensile strength and negative sign
indicated decrease in tensile strength. The results observed from experimental tensile
strength were compared with regression tensile strength and found an error less than 5%.
Thus, regression tensile strength was closely similar to experimental tensile strength with
minimum error and hence the developed model has well suitable to analyze the mechanical
properties of the composite materials.

4. Conclusion

Aluminum alloy can be successfully reinforced with Titanium diboride particles through in-
situ salt-metal reaction method. Strengthening of composite is due to dispersion
strengthening and particle reinforcement. Tensile strength and Hardness of the composite
has increased with the increase in percentage of Titanium diboride reinforcement, whereas
wear has decreased significantly. The increased percentage of titanium diboride from 4% to
8% reinforcement in the molten aluminum alloy, the mechanical properties hardness, tensile
strength and tribological property wear are affected. Thus Al-TiB2 composites are one
among the new materials that have come to occupy important fields such as aerospace,
defence, automobile, biomaterial as well as sports and leisure.

References

[1] A. Belhocine, A. R. A. Bakar, and M. Bouchetara, “Thermal and structural analysis of

disc brake assembly during single stop braking event,” Aust. J. Mech. Eng., vol. 14, no.
1, pp. 26–38, Jan. 2016.

10
[2] C. S. Ramesh, A. Ahamed, B. H. Channabasappa, and R. Keshavamurthy,
“Development of Al 6063–TiB2 in situ composites,” Mater. Des., vol. 31, no. 4, pp. 2230–
2236, Apr. 2010.
[3] D. B. Miracle, “Metal matrix composites – From science to technological significance,”
Compos. Sci. Technol., vol. 65, no. 15, pp. 2526–2540, Dec. 2005.
[4] N. B. Dhokey and K. K. Rane, “Wear Behavior and Its Correlation with Mechanical
Properties of TiB2 Reinforced Aluminium-Based Composites,” Advances in Tribology,
2011. [Online]. Available: https://www.hindawi.com/journals/at/2011/837469/cta/.
[Accessed: 07-Aug-2018].
[5] T. V. Christy, N. Murugan, and S. Kumar, “A Comparative Study on the Microstructures
and Mechanical Properties of Al 6061 Alloy and the MMC Al 6061/TiB2/12p,” J. Miner.
Mater. Charact. Eng., vol. 09, p. 57, Jan. 2010.
[6] M. K. Surappa, “Aluminium matrix composites: Challenges and opportunities,” Sadhana,
vol. 28, no. 1–2, pp. 319–334, Feb. 2003.
[7] N. B. Dhokey, “Effect of KBF4 and K2TiF6 on precipitation kinetics of TiB2 in aluminium
matrix composite,” Adv. Mater. Lett., vol. 2, Sep. 2011.
[8] M. . M. Siva, R. Rajesh, S. Pugazhendhi, M. Sivapragash, and R. R. Neelarajan,
“Analysis of Microstructural, Corrosion and Mechanical Properties of Aluminium Titanium
Diboride Particles (Al-TiB2) Reinforced Metal Matrix Composites (MMCs),” Indian J. Sci.
Technol., vol. 9, no. 43, Nov. 2016.

11