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Effect of ARB Cycle Number and Second Phase Content on Mechanical

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Article  in  Transactions of the Indian Institute of Metals · February 2018

DOI: 10.1007/s12666-018-1281-4

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Trans Indian Inst Met
https://doi.org/10.1007/s12666-018-1281-4
TECHNICAL PAPER
Effect of ARB Cycle Number and Second Phase Content
on Mechanical properties and Microstructure of Pb–Ag
Composite
Maryam Karbasi1 • Eskandar Keshavarz Alamdari2 • Elaheh Amirkhani Dehkordi1
Received: 12 December 2016 / Accepted: 12 January 2018
Ó The Indian Institute of Metals - IIM 2018
Abstract A solid state method has been found for manu-
facturing of lead–silver composites for use as anodes in
electrowinning production. Mechanical properties and
microstructure of composite were characterized via peel-
ing, tensile and microhardness tests, and scanning electron
microscopy, transmission electron microscopy and frac-
tography. Based on the peeling test results, maximum bond
strength was achieved in the presence of 0.125 wt% of Ag
(1.8 N/mm). Best mechanical properties were achieved in
the Pb–0.5 wt% Ag composite after 10 ARB cycles by the
enhanced tensile strength rising up to 50%, yield strength
up to 170%, shear strength up to 63% and hardness up to
2.6 times higher, and the strain decreasing to 68% lower.
These advanced properties led to higher stiffness and
considerable enhancements in dimensional stability of the
anodes and they improved creep characteristics. The
advanced properties of the processed Pb–Ag composite
anodes could be introduced as certification for slower
anode failure, upkeep, surcharge and capital expenditure of
industries with essential lead anode requirement.
Keywords Lead–silver  Composite  Anode 
Accumulative roll bonding (ARB)
& Maryam Karbasi
m_karbasi@cc.iut.ac.ir
1 invention of homogeneous lead anodes is accompanied by
Department of Materials Engineering, Isfahan University of
Technology, Isfahan 84156-83111, Iran
2 cesses, negligible solubility of most elements in melted
Department of Mining and Metallurgical Engineering,
Amirkabir University of Technology, Tehran 15875-4413,
Iran
1 Introduction
Due to high energy consumption, expensive raw materials,
high capital cost, working condition problems, environ-
mental pollution and lack of possibility of recycling of used
materials in pyro-metallurgical processes; substitutions of
hydro-metallurgy have been extended progressively [1].
Electrolysis of aqueous extraction via electrowinning
method is universally accepted hydro-metallurgical indus-
trial technique for high purity mass production of copper
and zinc. In this method, reduced products such as Copper
and Zinc are deposited on the surface of Aluminum cath-
ode and an oxidation reaction take place on anode.
Suitable electrochemical and mechanical properties of
anodic metal are fundamental requirements that must be
considered for its selection [2]. Sulfuric acid based baths in
the presence of Lead (Pb) anodes are generally applied in
hydro-metallurgical techniques, especially in zinc and
copper electrowinning industries. Although, Pb anodes
have been extensively used in sulfuric acid based industrial
processes but their utilization is accompanied with several
disadvantages. Major operational shortages results from
weak mechanical properties of Lead metal. Gradual
deformation of lead anodes during operation leads to
continuous breakage of anodic surface, fresh lead metal
corrosion and increasing anode failure and electrolyte and
metallic product contamination. Accordingly, improve-
ment of mechanical properties of lead anodes is unavoid-
able. Therefore, researchers have added several alloys
elements to lead anodes to achieve this improvement. But,
numerous difficulties such as: complicated casting pro-
lead casting and consequently difficult dispersion of alloy
agents in lead base metal have resulted in very low
123

reliability and control ability of anodes [3]. Though,
nowadays different methods have been examined by
researchers, but essential difficulties and expenditure of
production of homogeneous alloys of composite anodes
prevails [4].
The aim of this paper is to study fabrication of com-
posite lead based anode with similar chemical properties as
RSR’s anode, Texas, USA. Possibility of Pb–Ag anodes
with more Ag content has been investigated. Microstruc-
ture and Mechanical properties of these anodes have also
been examined.
2 Experimental Procedure
Lead ingot (Iranian Lead and Zinc (NILZ) Co, Zanjan,
Iran) with reported Chemical composition in Table 1 have
been utilized for Pb sheet fabrication. Ag (Fluka Co., 97.9
wt%) powders with 1–3 micron initial particle size distri-
bution and partially rounded morphology (Fig. 1a, b) were
used as additive.
ARB procedure was carried out by a laboratory rolling
mill (loading power of 20 tons and rolling speed of 4 mm/
min). Ag powder addition to Pb sheets was done at first
four passes of ARB process and further cycles were con-
tinued for improvement of particle distribution and their
interface in Pb matrix. For composite sheet preparation, the
surface of two strips of 100 mm 9 50 mm 9 3 mm were
cleaned with pure acetone spray and scratched using a
rotating wire brush. After surface treatment, particles were
uniformly dispersed via vibration dispenser between upper
sides of strips in different percentages (0.25, 0.5, and 1
wt% Ag), and then strips were stacked over each other and
fixed at ends. The roll bonding process was carried out
without any lubrication at a loading capacity of 20 tons and
50% reduction. Cold roll bonded strips were cut into half,
cleaned, scratched, powder dispersed, fastened and the
same procedure was repeated up to 4 cycles at room tem-
perature. ARB cycles were repeated without powder
addition up to the defined pass for better distribution at the
second phase. T-Peel test (ASTM: D1876-08) were applied
(via a Hounsfield H10KS tensile testing appliance with
constant cross head speed of 2 mm/min) for assessment of
peeling strength in different reduction and with various
amount of added Ag particles. For each specimen, three
Table 1 Chemical composition of Pb ingot
Element Pb Sn Zn
Percent 99.987 0.0011 0.0041
123
Trans Indian Inst Met
peel tests were carried out and the average peel strength
was calculated. Tensile test samples were prepared from
the rolled strips oriented along the rolling direction via a
wire cutting apparatus corresponding to the ASTM: E8 M
standard. The tensile tests were conducted at ambient
temperature using a Hounsfield H50KS testing instrument
(at a speed of 2 mm/min). To evaluate the creep behavior
and performance of the specimens under shear force, shear
punch tests were performed in the normal direction
according to ASTM: E898. Microhardness of the speci-
mens at the normal direction (ND)-transverse direction
(TD) planes were measured under a load of 15 g using the
Mitutoyo-HM100C system. Microhardness was measured
randomly at 15 different points along the rolled surface for
each specimen and the coefficients of variations were
calculated.
Scanning electron microscopy (SEM) and energy dis-
persive spectroscopy (EDS) were performed using SEM–
EDS LEO1550 and iXRF 5500i at 25 kV to evaluate
additive morphology, powder distribution in the Pb matrix
at ND-TD planes, the bonding conditions of the specimens,
and their fractography at the fractured surface after the
tensile test.
Transmission electron microscopy (TEM) was done by
using the PHILIPS CM120 at 200 kV to examine the
structure of the ARB processed specimens thinned by using
microtome technique in the ND-TD planes. Thin foils for
TEM were prepared using the ultra-microtome sectioning
technique.
3 Results
3.1 Peeling Tests
Changes of average peeling force of roll bonded Pb strips
with different reduction have been reported in Table 2. As
can be seen, critical reduction is 25% and lower reduction
have not resulted in bonding of Pb strips via rolling. The
result indicates that, for low reduction (30%), the perfor-
mance of bonding is not strong but for high reduction
(about 50%), the bonds created are very strong. It should be
noted that in order to achieve good bond strength, an
optimum reduction is between 50 and 60%, and over 60%
reduction lead to sheet failure. This is because, reduction
Ni Sb Bi Ag
0.0003 0.0059 0.0012 0.0004
Trans Indian Inst Met

Fig. 1 Ag powder: a morphology, b EDS analysis

Table 2 Average peeling forces in different reduction

Reduction (%) 20 25 30 40 50 60
Average peeling force (N) Without bonding 5 17 39 53 Sheets failure

more than 50% leads to the rupture of the base metal and
can not lead to higher bond quality. So, optimal average of
peeling force and subsequently suitable bond strength of Pb
sheets via roll bonding can be obtained in 50% reduction.
Because average peel strength in 0.5, 0.375 and 0.25% Ag
samples is very close to average peel strength of pure lead,
those samples can pass acceptable anodes ARB fabrication
parameters [5]. However, average peel strength of 0.625%
Ag sample is very weak compared to the pure lead, so this
sample is not suitable for fabrication as lead anode. Peeling
strength changes with various percentage of added Ag
powders between Pb strips after 50% reduction, shown in
Fig. 2. As can be seen that by addition of 0.125 wt% Ag
Fig. 2 Average of peeling
strength of Pb sheets in the
presence of different amount of 1.8
Ag powder addition
1.6
powder, bond strength increases to a maximum value and
addition of more than 5.0 wt% lead to a significant
reduction in bond strength of lead sheet. For the purpose of
this research, the acceptable bond strength for the com-
posite sheets is defined as the average bond strength which
is approximately equal to or greater than the average bond
strength of pure Pb strips after the same reduction. So, by
adding more than 0.5 wt% Ag, the achieved bond strength
is not suitable. This behavior results from the following
bonding mechanism: when Pb sheet have been rolled, two
phenomena have happened. First; compaction of powder
layers and simultaneously deformation of oxide film under
the normal force of roller. Second; by restricting the
Average of peeling strength (N/mm)

1.4

1.2

0.8

0.6

0.4

0.2
0Wt. %Ag 0.125Wt.%Ag 0.25Wt.% Ag 0.375Wt.%Ag 0.5Wt.%Ag 0.625Wt.%Ag

123

Fig. 3 Tensile engineering
stress–strain curves: a in the
presence of 0.5% Ag after
different ARB pass and b in the
presence of different amount of
Ag compared with Pure Pb
movement of particles, the apparent volume reduction has
stopped and further objected roller force lead to crack
formation in powder layer. By increasing the rolling ten-
sion, powder layer has broken down to smaller parts. Those
can act as micro-punches and micro-extrusion of virgin Pb
metal through the cracks of powder layer at around the
particles takes place and bonding of two sheets is enhanced
[5–7]. Similar behaviors have been recommended by other
researchers [8–10]. By increasing the weight percent of
added Ag powders (more than 0.5 wt%), the thickness of
powder layer have been increased; consequently, suit-
able sheets bonding has been avoided and bonding strength
have been reduced significantly (Table 2 and Fig. 2).
3.2 Tensile Test
Engineering tensile stress–strain curves of Pb sheets and
Pb–0.5 wt% Ag composite sheets after various ARB passes
have been shown in Fig. 3a. The results of tensile stress–
strain tests of Pb–Ag composite anode with different Ag
123
Trans Indian Inst Met
contents after 10 ARB passes have been shown in Fig. 3b.
Results of tensile tests have been summarized in Table 3.
According to tensile test results, by increasing the number
of ARB passes, yield strength (YS) and ultimate tensile
strength (UTS) have increased and simultaneously engi-
neering strain of pure Pb (a, b and c curves) and Pb–Ag (e,
f and g) composite sheets have decreased. This behavior
indicates that deformation resistances of samples under the
tensile tensions conditions has increased by ARB process.
Figure 3a and Table 3 indicate that, the composite, which
has 0.5 wt% Ag in comparison to another one, have the
highest tensile strength and yield strength and the lowest
elongation and higher deformation resistance have been
gained in this sample. Comparison of curves of Fig. 3b
have shown that optimal tensile behavior has been gained
in the presence of 0.5 wt% Ag (curve b). Addition of lower
percent (curve b) and higher percent (curve d) than 0.5%Ag
have led to the weakness in the tensile behavior of samples
in comparison to pure Pb (curve a) after 10 ARB passes.
From one side, low percent of Ag can not act as micro-
Trans Indian Inst Met

Table 3 Tensile test results

Specimen YS increase (times) UTS increase % Elongation
(MPa) (MPa) (%)

Pb-0 pass 0 0 87
Pb-5 pass 1.1 10 75
Pb-7 pass 1.6 30 58
Pb-10 pass 2 38 27
0.5% Ag-5 2.2 8 57
pass
(a)
0.5% Ag-7 2.4 35 44
pass
0.5% Ag-10 2.7 50 28
pass
0.25% Ag-10 2.1 32 42
pass
1% Ag-10 2.2 30 38
pass

Table 4 Hardness tests results (b)

Specimen Hardness (HV) Coefficient of variation Shear Strength (Mpa) Tensile Strength (Mpa)

Pb-0 pass 9.3 0.0008 16

Pb-5 pass 10.7 0.0165 14

Pb-7 pass 15.0 0.0113
12
Pb-10 pass 18.9 0.009
10
0.5% Ag-5 pass 20.6 0.0183
0.5% Ag-7 pass 22.0 0.0133 8

0.5% Ag-10 pass 24.8 0.0108 6

0.25% Ag-10 pass 19.4 0.0102
4
1% Ag-10 pass 20.1 0.0132
2

0
punches effectively. On the other side, high percent of Ag Pb-0pass Pb-10pass Pb-0.5Wt.%Ag-10pass
forms a thick powder layer, and sheet bonding is avoided.
(c)
Low bonding strength directly lead to lower tensile
behavior of sheets with a separated layer forming during Fig. 4 a Strain–time curves, b force–displacement curves, c com-
ARB passes. These results are in good agreement with pared shear strength and tensile strength of pure Pb strips and ARB-
peeling tests results. processed specimens under a constant tension

3.3 Microhardness Tests where r is standard deviation and l is average value of

measured hardness of 15 regions in each sample. In other
Results of hardness tests are important from two points of words, fragmentation of hardness values, around average is
view: average value of hardness and distribution of hard- represented by the coefficient of variations (Table 4) [11].
ness values. In the first case, the average value of hardness According to the results, hardness of Pb sheets and Pb–Ag
is represented as deformation resistance under normal composited sheets have increased and coefficient of vari-
compressive tension of dent and in the second one, ations has decreased by increasing the number of ARB
homogeneity of this behavior is evaluated as criterion, for passes because of better distribution of hardening agent. In
the distribution of reinforcement agents. In order to eval- addition, increasing the added Ag percent has lead to a
uate recent criterion, coefficient of variations has been higher hardness average and a higher coefficient of varia-
calculated as follows: tions. This behavior has resulted from the presence of
r higher amount of Ag (2.5 in Mohs scale) with more
Cv ¼ ð1Þ
l hardness in comparison to pure Pb (1.5 in Mohs scale).

123

Table 5 Shear punch results
Specimen Ultimate shear force (N) Shear strength(MPa)
Pb-0 pass 65.90 6.95
Pb-10 pass 89.61 9.45
0.5% Ag-10 pass 107.65 11.37
3.4 Shear Punch Tests
The amount of displacement of punch under constant ten-
sion (10 MPa) per unit time in shear punch tests is inter-
preted as the deformation of sample in unit time or
deformation rate under constant tension. As can be seen in
Fig. 4a, shear punch test results’ curves are very similar to
creep test results and can be used suitably for evaluating
the behavior of prepared anodes under low gradual tension
[12]. By comparison of Fig. 4a graphs, it is clear that
deformation rate (punch displacement rate) of ARB pro-
cessed samples (b and c curves) is lower than pure Pb
sample (a curve). And the lowest deformation rate has been
obtained in the presence of 0.5% Ag after 10 ARB passes.
This behavior is in good agreement with tensile test results.
In order to evaluate the deformation resistance of sam-
ples under shear tensions, they have been subjected to
constant rate of punch displacement and the required forces
for displacement have been determined and the resulting
graphs are shown in Fig. 4b. Maximum required force for
constant displacement rate of punch in shear punch test has
been recognized as ultimate shear force [13] that has been
calculated by the following equation:
p with distinguishably arranged bright points (Fig. 6b). After
s¼ ð2Þ
pdt
where s is shear tension (MPa), p is force (N), d is average
of punch and matrix diameter (mm) and t is sheet thickness
(mm). By substitution of p with ultimate shear force, shear
Fig. 5 a BSE-SEM micrographs of Pb %0.5Ag-10 pass specimen at ND-TD plane, b EDS pattern of dark regions and c EDS pattern bright
matrix
123
Trans Indian Inst Met
strength of samples can be calculated. Results have been
summarized in Table 5 and the amount of Shear strength in
samples in comparison with ultimate tensile strength is
shown in Fig. 4c. The highest displacement force and shear
strength have been gained in the presence of 0.5% Ag after
10 passes of ARB. These behaviors are in good agreement
with tensile tests results. Conformity of shear strength and
ultimate tensile strength changes, that can be seen in
Fig. 4c is in good agreement with other researchers’ reports
[14, 15].
3.5 Microstructure Observations
In order to evaluate particles distribution in Pb matrix,
BSE-SEM micrographs have been taken of ND-TD cross
section of samples and EDS have been applied for ele-
mental characterization of different gray level regions.
Results of SEM observations are shown in Fig. 5a.
Suitable Ag particle distribution with continuous interfaces
without any gaps or debonding can be seen in Fig. 5a. EDS
results confirm that the dark regions are Ag particles
(Fig. 5b) and bright field is Pb matrix (Fig. 5c). In addition,
presence of Ag peaks in bright gray matrix is interpreted as
the existence of finer Ag particles, which break down
during severe plastic deformation during ARB passes and
get distributed in Pb matrix.
Bright field, SAD patterns and EDS results of TEM
observation of Pb sample before and after 10 ARB passes
are shown in Fig. 6. As seen in Fig. 6a, grain size of Pb
sample is considerably more than 1 lm. Coarseness of
grains in Pb sample has been confirmed by SAD patterns
10 ARB passes on pure Pb, formation of dislocations
(outlined regions) and presence of some black items on
grain boundaries can be clearly observed in Fig. 6c; in
addition, reduction of grain size can be assumed from SAD
Trans Indian Inst Met
Fig. 6 a TEM bright field image of pure Pb, b SAD pattern of pure Pb, c TEM bright field image of Pb-10 pass specimen, d SAD pattern of Pb-
10 pass specimen, e EDS pattern of 1 in Fig. 6c
patterns which show increased number of diffraction spots
with lower intensity and unarranged positioning (Fig. 6d).
Presence of Pb oxide particles on grain boundaries has
been proved by EDS analysis results (Fig. 6e) of black
items on grain boundaries. In comparison to pure Pb,
performing 10 ARB passes in the presence of 0.5 wt% Ag
(Fig. 7a) has led to the formation of lower grain size (ac-
cording to SAD patterns of Fig. 7b), significantly higher
dislocation density and enhanced formation of dislocation
tangles (outlined zones), cells, sub-grains (with settled Ag
particles proved by EDS analysis of Fig. 7c) and Multi-
directional slip bands [15] (observed in gray field of
Fig. 7a).
In order to examine the effects of ARB process on
fracture mechanism of Pb and Pb–Ag samples, SEM
fractography has been performed and SE-SEM micro-
graphs of tensile fracture surface of samples have been
shown in Figs. 8 and 9. Clearly, the pure Pb strip is
123

Fig. 7 a TEM bright field image of 0.5%Ag-10 pass specimen, b SAD pattern of 0.5%Ag-10 pass specimen, c EDS pattern of 1 in a
completely necked and a fractured surface forms as a
narrow linear zone with less than 30 micron width and
without any chance of forming dimples (Fig. 8a). How-
ever, deep equiaxed dimples and shear zones occur in a
typical ductile fracture which happens in the ARB-pro-
cessed specimen [5, 16]. After 5 ARB passes, formation of
dimples (as ductile mechanism feature) and lower reduc-
tion of fractured area and strain during necking stage are
observed (Fig. 8b). By increasing ARB passes to 7 passes,
recent features get enhanced (Fig. 8c). After 10 ARB
passes, fractured surface forms as layers and significant
lower reduction of fracture area is noticed. This behavior,
interpreted as heterogeneous deformation phenomenon,
results in a layered fractured surface and higher deforma-
tion resistance (or in other words, higher dimensional sta-
bility) of ARB processed anodes under tensile conditions
[17]. SE-SEM micrograph of fractured surface of ARB
processed samples in the presence of 0.5 wt% Ag after
different passes have been shown in Fig. 9. As can be seen
in Fig. 9a, fractured surface of Pb–0.5%Ag specimen after
5ARB passes has been formed as a layered structure
(similar to Pb-10 pass). So, formation of a layered structure
during ARB process has been enhanced in the presence of
Ag particles. By increasing ARB passes, bonding of layers
123
Trans Indian Inst Met
improves and in addition to coarse dimples, fine dimples
can also be observed (Fig. 9b). Finally, after 10 ARB
passes in the presence of 0.5 wt% Ag, with substantial
improvement of composite microstructures, shear dimples
[15, 17, 18] are formed on the fractured surface (Fig. 9c).
4 Discussions
In accordance with mechanical characterization of ARB
developed samples by tensile tests (50% higher UTS, 170%
higher YS, strain decreasing to 68% lower), hardness tests
(up to 2.6 times higher), shear punch tests (70% higher
shear strength and significant lesser deformation rate at
same punching condition) and fractography, improvement
of dimensional constancy of ARB processed sample
especially in the presence of Ag particles have been
corroborated.
In additions, the linear part of the stress–strain graphs
corresponds to the stiffness, and are defined as Young
modulus, as can be seen in Fig. 3a and b graphs. Linear
part of ARB-processed anodes are steeper, that can be
described as higher stiffness, lower elasticity and higher
deformation resistance. Higher stiffness of the ARB-
Trans Indian Inst Met
Fig. 8 SE-SEM fractography micrograph: a plain Pb, b Pb after 5 ARB passes, c Pb after 7 ARB passes and d Pb after 10 ARB passes
processed anodes has resulted from the presence of Ag and
broken Pb oxide particles as reinforcement phase, and ARB
process as an anisotropic sever plastic deformation tech-
nique. This conclusion is in agreement with other
researchers’ discussions [19–23], but superior degree of
changes in this research work results from ultimate duc-
tility of Pb in comparison to Al, Cu and Fe base sheets.
Furthermore, numerous stress oscillations can also be
seen in the tensile stress–strain graph of Pb strips (Fig. 3a,
b). This performance has been resulted from counter action
of tensile work hardening (leading to higher requirement of
stress for further elongation) and fast recovery phe-
nomenon (leading to compensation of hard working and
lower stress necessity for further elongation) in the pure Pb
microstructure. As further tension is exerted during the
tensile test, work hardening behavior is established such
that a higher stress is required for the deformation to occur.
On the other hand, the dominant recoverability of the Pb
microstructure effectively compensates for the strain
hardening features [17], so a lower stress suffices for fur-
ther deformation. In the tensile stress–strain curves of pure
Pb, stress oscillations are observed caused by behavior
which has been described above. As mentioned before, the
successfully diminished recovery progress in ARB pro-
cessed anodes caused by strengthening mechanisms results
in the continued work hardening and the disappearance of
stress oscillations.
Distribution of broken down Pb oxide films and Ag
particles at dislocation tangles, cells and sub-grains or
grains boundaries have been observed in TEM results
(Figs. 6, 7). These microstructure features are essential
evidences for the occurrence of strengthening mechanisms
that are described as follows:
The existence of additive particles in the Pb matrix can
perform efficiently by making the movement difficult for
grain boundaries and dislocations [17–19, 24]. Small par-
ticles restrict the movement of grain boundaries by
applying a pinning force which neutralizes the exerted
pressure resulting from rolling, that tends to push the
boundaries away. This effect has a significant hindrance
effect on the recovery of work hardening. This phe-
nomenon can be enhanced by increasing the volume frac-
tion and homogeneity of the dispersed particles. These
have been concluded from tensile strength (Fig. 3 and
Table 3), hardness (Table 4) tests results, BSE-SEM
micrograph (Fig. 5) and fractography results (Figs. 8, 9).
123

Dimensional stability has been amended accompanied with
higher ARB passes, resulting from more homogeneous
particle distribution. Furthermore, second phase particles
are distributed in the ductile Pb matrix. Thus, severe plastic
deformation leads to the pile-up of dislocations around the
particles. These dislocation pile-up can act as tough bar-
riers to dislocation glide, sub-grain formation, and grain
boundary sliding, all of which lead to work hardening and
recovery hindrance [20]. This effect can be improved
efficiently via more homogeneous particles distribution
[17]. Consequently, superior deformation resistance and
extra dimensional stability have been characterized in the
ARB-processed anodes, mainly with higher ARB passes
and in the presence of Ag with micro-punch acting and
enhanced distribution effects [5, 16]. Therefore, YS, UTS,
hardness and shear strength are improved and elongations
are reduced in comparison to the non-rolled Pb strips.
The significant increase of microhardness of the Pb–
0.5%Ag-10pass (Table 4), is the effect of higher hardness
of Ag particles (2.5 in Mohs hardness scale for Ag particles
in comparison to 1.5 in Mohs hardness scale for Pb matrix).
Table 4 indicate that, a lower coefficient of variations is
gained at higher ARB passes due to better distribution of
Ag particles and broken Pb oxide films. By increasing the
Fig. 9 SE-SEM fractography micrograph: a 0.5% Ag-5 pass, b 0.5% Ag-7 pass, c 0.5% Ag-10 pass
123
Trans Indian Inst Met
number of layers of composite formed due to continuous
rolling by ARB, distribution of particles in matrix enhan-
ces, and these results are in good agreement with other
researchers’ reports [23, 25–31]. Continuous acidic solu-
tions’ flow in the industrial electrowinning cells involve
very aggressive working conditions for anodes [32].
Therefore, the hardness improvements gained in ARB
processed anodes can lead to higher surface resistance
against erosion and anode surface decay as reported in
other publications by the authors [7, 8].
Because of very low melting point of lead (599 °K),
accelerated creep rate has been seen at room temperature in
pure Pb samples (see the steep slope of the shear punch
simulated creep graph a in Fig. 4a). This behavior lead to
very high decay rate and failure of lead anodes at the
typical ambient temperature in electrowinning industries
(more than 295 °K). As can be seen in shear punch tests
results (Fig. 4 and Table 5), significant improved shear
yield strength and the higher shear strength have been
gained at the ARB-processed specimens compared to pure
Pb.
In the first creep stage, strain hardening is a major
controlling agent, which in the second stage is balanced by
interaction with recovery phenomenon. The reduced creep
Trans Indian Inst Met
rates of the ARB-processed specimens are resulted from
matrix strengthening due to ARB process work hardening
effects. In addition, presence of second phase decaying
movement of dislocation glide (consequently reduced
Coble creep), sub-grain formation, and grain boundary
sliding are also observed. This mechanism is in good
accord with other research reports [9, 18]. Therefore,
improved shear yield strength can strongly correspond to
the higher creep resistance that not only lead to significant
reductions in maintenance costs [33], but also to consid-
erably enhanced product purity in electrowinning as
examined in other research work of authors [7, 8].
On the other hand, fractured surfaces of tensile-stressed
specimen are observed in Figs. 8 and 9. As seen, hetero-
geneous deformation has happened. This behavior of ARB
process can prevent the recovery phenomenon and
encourage high deformation resistance in manufactured
anodes, that corresponds to the higher dimensional stabil-
ity; another researchers’ reports are in good agreement with
our results [13]. This means lower anodic surface break-
down and reduced decay rate, less sludge formation, lower
bath and production contamination, and reduced mainte-
nance and capital costs in electrowinning industries.
Our results propose that the ARB Technique can be
effectively developed towards improvement of mechanical
and microstructural characteristics of Pb–Ag composite
anode via solid state industrial method.
5 Conclusion
1. Accumulative roll bonding (ARB) could be effectively
developed for fabrication of Pb–Ag composited
anodes.
2. Highest bond strength (1.8 N/mm) at 50% reduction,
could be gained in the presence of 0.125 wt% Ag.
3. Maximum tensile deformation resistance could be
obtained after 10 ARB passes in Pb–0.5%Ag
composite.
4. Based on shear punch tests, Creep resistance could be
improved for Pb–0.5%Ag composite after 10 ARB
passes with up to 63% higher shear strength.
5. Due to suitable distribution of Ag second phases in Pb
matrix, up to 2.6 times higher harness could be gained
in Pb–0.5%Ag composite after 10 ARB passes.
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