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Materials Today: Proceedings 2 (2015) 1136 – 1142

4th International Conference on Materials Processing and Characterization

Study of microstructure, mechanical properties and wear rate of

high leaded tin bronze after multidirectional forging

Rahul Guptaa, Sanjay K Panthib, Sanjay Srivastavac

a
Ph.D Scholar, Department of Material Science & Metallurgical Engineering, Maulana Azad National Institute of Technology, Bhopal, 462003,
India
b
Scientist, Advanced Materials and Processes Research Institute (AMPRI), Bhopal, 462024, India
c
Associate Professor, Department of Material Science & Metallurgical Engineering, Maulana Azad National Institute of Technology, Bhopal,
462003, India

Abstract

In this work, the change in microstructure, mechanical properties and wear rate of high leaded tin bronze alloy was studied after
multidirectional forging (MDF) process. The total equivalent strain of 0.75 was applied. During MDF process improved ultimate
tensile strength, hardness and wear rate along with maintained ductility was reported. The initial average grain size of 120 nm
was refined to the final average grain size of 37 nm. The transmission electron microscope, scanning electron microscope and
optical microscope was used for microstructure observation of the sample without MDF, MDF and wear worn surfaces.

© 2014 The Authors. Elsevier Ltd. All rights reserved.

© 2015 Elsevier Ltd. All rights reserved.
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Selection and peer-review
peer-review under responsibility
under responsibility of thecommittee
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International the 4th International conference
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Materials Processing and Characterization.
Characterization.

Keywords: Multidirectional forging; high leaded tin bronze; mechanical properties; microstructure; wear

1. Introduction
The high leaded tin bronze alloy has been extensively used in automotive, agricultural, rail road, mining, off
highway equipments [1]. Severe plastic deformation for the fabrication of improved mechanical properties materials
refers to various experimental techniques such as high pressure torsion (HPT), equal channel angular pressing
(ECAP), multidirectional forging (MDF), accumulative roll bonding (ARB), cyclic extrusion and compression *
Corresponding author. Tel.: +0-000-000-0000 ; fax: +0-000-000-0000 .
E-mail address: rahulgupta087@gmail.com

2214-7853 © 2015 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the conference committee members of the 4th International conference on Materials Processing
and Characterization.
doi:10.1016/j.matpr.2015.07.023
 Rahul Gupta et al. / Materials Today: Proceedings 2 (2015) 1136 – 1142 1137

(CEC), repetitive corrugation and straightening (RCS) and twist extrusion (TE) [2,3]. MDF is a repeatition of free
forging operation multiple times including setting and pulling operations with the change in direction of applied load
[4]. Gao and Cheng [5] reported improvement in the mechanical and tribological properties of the commercial
aluminum bronze alloy after equal channel angular extrusion at high temperature. Prasad [6] monitored dry sliding
wear rate of the leaded tin and aluminum bronzes by using pin on disc machine for different sliding speeds and
applied pressure and also studied the frictional heating and surface roughness during the wear. The study results no
direct correlation between wear response and mechanical properties of the sample. Keshavamurthy et al. [7]
measured tribological properties of Al 2024-TiB2 composite after applying hot forging operation. The aim of present
work is to study the effect of MDF on microstructure, mechanical properties and wear behavior of the alloy.

Table 1. Chemical composition of alloy (wt. %)

Cu Pb Zn Sb Ni P Fe As Bi Sn Si Al Mn

Bal. 20.58 3.52 0.25 0.63 0.02 0.2 0.03 0.003 5.044 <0.001 <0.001 <0.001
____________________________________________________________________________________________________________________

2. Experimental

The high leaded tin bronze alloy was MDFed; chemical composition is shown in table 1. Before MDF the alloy
was heat treated at 300o C for 1 hour by using muffle furnace followed by water quenching. The initial average grain
size of 120 nm was found after heat treatment. The rectangular specimen of 56.5 mm x 56.5 mm x 50 mm was
machined from heat treated alloy and MDFed at room temperature by using MDF die.

The MDF was initiated by inserting the samples inside the die between the top punch and bottom punch and force
downed perpendicularly by altering the direction of loading along three orthogonal directions from pass to pass at an
angle of 90o i.e. in order of z to x, x to y, y to z axes several times as shown in figure 1. The MDF was applied upto
9 pass at constant pressing speed of 10mm min-1 by using 200 tons capacity press. The total equivalent strain of 0.75
was applied in 3 MDF cycles.

The MoS2 lubricant was used to reduce the friction between die and specimen contact points during forging. The
tensile tests were carried out at room temperature on the specimens with 24 mm gauge length, and 6 mm gauge
diameter at constant tensile rate of 0.5 mm/min by applying Tinius Olsen H50K-S universal testing machine. The
vicker’s micro hardness was measured for the sample without MDF and MDF to 9 pass at room temperature under
applied indenter load of 1 kg and dwell time of 10 seconds, the average of 6 indents readings was taken as final
hardness. The microstructure characterization of MDF sample was performed by using high resolution transmission
electron microscope (HRTEM, JEM-2100, JEOL, Japan) operated at 200 kV and optical microscope (OM). For
TEM thin slices of the sample were prepared. The samples for OM were polished and etched in a solution of
ammonia hydroxide (NH4OH) 25 ml, hydrogen peroxide 3% (H2O2) 25-50 ml and distilled water 25 ml. A dry
sliding adhesive wear test was performed by using pin on disc wear testing machine. The wear test was executed on
stationary cylindrical pin specimens of 8 mm diameter and 30 mm length.

The samples was tested against the rotating disk (EN31) of 60 HRC hardness, for different sliding distances at
room temperature with 34 mm track radius, 10 N load and 150 rpm sliding speed. Before starting the test pin contact
surfaces were polished by using 600 grits polishing paper, cleaned with acetone before and after every test. The
wear rate was determined by weight loss method. The weight of pins was measured before and after every wear test
by using electronic balance machine. The temperature near the specimen and disc contact point was measured by
using pen type thermometer. The microstructure of the worn surfaces was observed by using scanning electron
microscope (JEOL JSM 6390A) at an accelerating voltage of 20 kV prior to SEM observation the samples were
cleaned with acetone.
1138 Rahul Gupta et al. / Materials Today: Proceedings 2 (2015) 1136 – 1142

Fig.1. MDF processing of high leaded tin bronze alloy.

3. Results and Discussion

3.1 Microstructure Evolved

3.1.1 Optical Micrographs

The optical micrographs of the sample without MDF and MDF to 9 pass is shown in figure 2. It can be observed
that the lead shows extremely low solid solubility in tin and copper and dispersed throughout the matrix as small
sized lead globules and occurs as a separated particle [6,8,9] marked by sign L in figure 2 (a). The primary α phase
marked by sign A is a solid solution of tin in copper provides support to copper tin intermetallic compound marked
by the sign B is shown in figure 2 (a) [9]. Figures 2 (a) and 2 (b) explains that the increase in the applied strain with
number of MDF pass distributes the coarser lead particles, α phase and copper tin compound into finer size. The
number and size of deformed particles increases within the same area of observation due to the uniformity applied
strain during MDF.

20 μm
20 μm

Fig.2. Optical micrographs of sample (a) without MDF; (b) MDF to 9 pass.

3.1.2 TEM microstructure

The TEM image of the sample without MDF is shown in figure 3 (a) reveals equiaxed grains of average 120 nm
sizes. The 120 nm grains was refined to average size of 37 nm after nine MDF pass can be seen in figure 3 (c). The
 Rahul Gupta et al. / Materials Today: Proceedings 2 (2015) 1136 – 1142 1139

grain of lead rich phases was also identified at certain locations. The lead particles are placed at the surrounding of
grain boundaries and within the grain [9]. The lead rich phase was found to be layered at an average distance of 0.56
μm as shown in figure 3 (b) marked by the arrow signs. The microstructures figure 3 (c) reveals with the increase in
the applied strain up to 0.75 the intermixing of phases, primary α phase, copper tin intermetallic compound (β phase)
and lead rich phases was obtained. MDF results a sandwich structure of Cu-Pb-Sn phases with the increase in
applied strain. The intermixed layers structure with an average thickness of 84 nm was observed after nine MDF
pass as shown in figure 3 (c).

Fig.3. TEM images of (a) and (b) sample without MDF; (c) MDFed sample after 9 pass.

3.2. Strength, hardness and ductility

Figure 4 reveals improvement in ultimate tensile strength of differently MDFed alloy. The initial ultimate strength
of 122.4 MPa was improved to 264.5 MPa after nine MDF pass, which was about 2.16 times higher than the sample
without MDF. The vicker’s micro hardness was also improved during MDF pass as shown in figure 4. The hardness
of the alloy was increased from 63 HV to 146 HV after nine pass, which was about 2.3 times higher than the
hardness of sample without MDF. The increase in strength and hardness was credited to grain refinement during
MDF. The strengthening and hardening through grain refinement was described by the hall petch equations, σy = σ0
+ kD-1/2 and Hv = H0 + kD-1/2 , which states that the yield strength σy and room temperature hardness H v both are
inversely proportional to the average grain size (D) of the material [10]. The grains size of the alloy was refined
1140 Rahul Gupta et al. / Materials Today: Proceedings 2 (2015) 1136 – 1142

during MDF pass as shown in the figure 3 (a) and 3 (c). Thus the strength and hardness was improved after MDF. In
addition, It is known from literature [11] that the strength and hardness of the alloy is directly proportional to the
volume fraction of the second phase particles. The optical microstructure shown in the figure 2 (b) reveals dispersed
distribution of second phase particles and increase in the volume fraction of the second phase particles after nine
MDF pass. Thus the strength and hardness increases with the increase in volume fraction. The result of change in %
elongation with the number of MDF pass is shown in figure 4. The alloy ductility after 9 pass was 12.67% which
was maintained as compared to the initial ductility 12.28%.of sample without MDF. Thus, the ductility of the alloy
was maintained during MDF and with the increase in strength and hardness.

Fig.4. Changes in ultimate tensile strength (UTS), % elongation and hardness with the number of MDF pass.

3.3 Wear rate

The wear rate of the alloy for different sliding distance is shown in the figure 5 (a). The wear rate of sample
without MDF and MDF was decreased with the increase in sliding distance. For small distance alloy shows less wear
rate which was regularly increased with the increase in sliding distances. The alloy after 3, 6, 9 MDF pass shown
improved wear resistance can be seen in figure 5 (a). The wear rate of MDF specimen was further more decrease as
compared to the sample without MDF. The hardness and refined grain structure obtained during MDF results in
decrease of wear rate of MDF samples as shown in figure 5 (a). The effect of decrease in wear rate with the hardness
can be explained according to the Archard’s law [5], Q = K LN / H, Where Q is volumetric wear loss, which is
inversely proportional to the hardness H of the wear surface, L is total sliding distance, N is applied load and K is
friction coefficient. The improvement in hardness of the alloy was achieved by the grains and crystal refinement,
thus improved hardness increases wear resistance of the alloy. Also at slower speed of 150 rpm the conditions for the
formation of lead film on the wear surface was not favorable, since the iron grasping between the sliding pin and the
rotating disk is negligible and the formation of lead lubricating film without iron pick up results higher wear rate and
material removes as chip off hence higher wear rate was resulted [6, 12] can be seen in figure 5 and 6. The
phenomenons of chip off remain continues for all the samples and wear rate increases. For 9 pass sample chip off
can be seen in figure 6 (b). Also slow speed due to less frictional heating results less temperature can be seen in
figure 5 (b), which continuously increases due to increase in frictional heating. The frictional heating temperature
was increased continuously for 3, 6, and 9 pass specimens which was due to increase in hardness of the alloy during
MDF.
 Rahul Gupta et al. / Materials Today: Proceedings 2 (2015) 1136 – 1142 1141

Fig.5. (a) Wear rate of sample without MDF and MDF to 3, 6, and 9 passes for different sliding distances; (b) average temperature close to the
wear surface of sample without MDF and MDF to 3, 6, and 9 passes for different sliding distances.

b a b

50 μm 50 μm

Fig.6. Optical micrographs of wear surfaces of the alloy (a) metal removal as chip off (marked by sign C) at 150 rpm speed for sample without
MDF; (b) metal removal as chip off (marked by sign C) at 960 m sliding distance after 9 pass.

4. Conclusions

The grain refinement from 120 nm size to 37 nm during MDF results improvement in ultimate strength, hardness
and wear rate of the alloy along with the maintained ductility. The strength of the alloy after nine MDF pass was
2.16 times improved and the hardness was 2.3 times improved the initial values. The grain and crystals refinement
of the composite alloy results fine dispersion of the constituents alloy members with the increase in MDF passes.
The increase in alloy hardness during MDF improved its dry sliding adhesive wear resistance with the changing
sliding distance. The wear rate of alloy was decreased with the increase in the sliding distance. The temperature
produced near to the wear surface was also increased but not considerably. The material wears as a chip off due to
low sliding speed and reported higher wear rate. Hence MDF can be a proficient process to improve the alloy
mechanical properties along with wear rate.
1142 Rahul Gupta et al. / Materials Today: Proceedings 2 (2015) 1136 – 1142

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