Int J Adv Manuf Technol (2015) 80:1655–1663
DOI 10.1007/s00170-015-7141-z
ORIGINAL ARTICLE
Effect of friction stir processing parameters
on the microstructural and electrical properties of copper
R. M. Leal 1,2 & I. Galvão 1 & A. Loureiro 1 & D. M. Rodrigues 1
Received: 31 January 2015 / Accepted: 12 April 2015 / Published online: 23 April 2015
# Springer-Verlag London 2015
Abstract Friction stir processing (FSP) is an innovative tech-
nology, based on friction stir welding (FSW) operative prin-
ciples, which can be used for changing locally the microstruc-
ture and the mechanical properties of conventional materials.
In this work, the copper alloy C12200 was friction stir proc-
essed using two distinct tools, i.e. a scrolled and a conical
shoulder tool, in order to promote different thermomechanical
conditions inside the stirred volume, and consequently, varied
post-processed microstructures. The influence of the tool ge-
ometry and tool rotation and traverse speeds on the micro-
structural and electrical properties of the processed copper
alloy was analysed. The processing conditions were found to
have an important influence on the electrical conductivity of
the processed material. The differences in electrical conduc-
tivity were explained based on dislocations density effects.
The effect of the dislocations density on electrical conductiv-
ity of the processed material was found to prevail over the
effect of the grain boundaries.
Keywords Friction stir processing . Copper . Microstructure .
Hardness . Electrical conductivity
* D. M. Rodrigues
dulce.rodrigues@dem.uc.pt
1
CEMUC, Department of Mechanical Engineering, University of
Coimbra, Rua Luís Reis Santos, 3030-788 Coimbra, Portugal
2
ESAD.CR, Polytechnic Institute of Leiria, Rua Isidoro Inácio Alves
de Carvalho, 2500-321 Caldas da Rainha, Portugal
1 Introduction
Owing to its good thermal and electrical conductivity, im-
proved plastic properties and excellent corrosion and oxida-
tion resistance, copper is extensively used worldwide. Never-
theless, for some particular applications [1, 2], copper wear
resistance, mechanical strength and fatigue behaviour are still
desirable to be improved. These properties can be improved
by suitable modification of material microstructure, using se-
vere plastic deformation (SPD) techniques, such as friction stir
processing (FSP), as demonstrated by Mishra et al. [3]. Based
on friction stir welding (FSW) principles, this technique
makes use of a non-consumable rotating tool to induce heat
and severe plastic deformation in the material to be processed.
The complex thermomechanical phenomena developed inside
the stirred volume promote strong microstructural modifica-
tions, which, cautiously controlled, enable to enhance partic-
ular mechanical properties of the processed materials. In fact,
the dynamic recrystallization of the plasticised microstructure
leads to significant grain refinement, which impelled the use
of this technique for producing ultra-fine grained structural
metallic materials from aluminium [4–6], magnesium
[7–10], NiAl bronze [11, 12], Ni based super alloys [13],
copper [1] and steel [14]. Furthermore, a large number of
works have also addressed the surface modification of cast
substrates. Grain refinement, dissolution of strengthening
phases and removal of cast porosities were the main improve-
ments achieved by using these techniques for processing sand
cast aluminium [15–19] and magnesium alloys [20].
In-situ production of intermetallic reinforced metal matrix
composites (MMCs) by friction stir processing of elemental
powder mixtures, such as Al-Cu [21, 22], Al-Ti [22, 23] and
Al-Fe [24], or in-situ production of bulk ultra-fine grained
composites by embedding reinforcing particles in metallic
plates, such as SiO2 [25] or SiC [26] in Mg plates, NiTi in
1656
Al plates [27] and Ni powders in Al plates [28], are examples
of other applications of FSP technology. Intermetallic alloys,
with desired portions of Al, Mg and Zn, were also produced
by FSP of sandwich specimens, composed of thin foils of the
different materials, stacked together vertically [29]. In all these
applications, FSP provides (a) severe plastic deformation,
which promotes mixing and refining of composite constituent
phases; (b) elevated temperature, which enables the formation
of intermetallic phases; and (c) hot consolidation, to form fully
dense solids.
Concerning to copper, few research has been carried out on
mechanical and electrical properties enhancement by FSP or
other SPD techniques. In fact, Su et al. [30] friction stir proc-
essed oxygen-free high thermal conductivity copper (C10100)
using a continuous quenching technology with the aim of
enhancing the cooling rates. The production of nanocrystal-
line structures with 174 nm was reported by the authors. In the
same year, Surekha and Els-Botes [1], in FSP of pure copper,
reported sound microstructures for a varied range of process-
ing conditions. According to the authors, the highest mechan-
ical enhancement was obtained for the highest processing
speed. A maximum grain refinement of 84 % relative to the
unprocessed material was achieved, which resulted in a hard-
ness increase of 34 %. These authors also pointed that the
grain refinement did not change the electrical resistivity of
the material. One year later, Xue et al. [31], in FSP of high
pure oxygen-free copper using additional water cooling, re-
ported an important enhancement in the yield and mechanical
strength of the processed material. The formation of an ultra-
fine grained (UFG) structure, with some hundreds of
nanometres, was argued to be on the basis of copper mechan-
ical enhancement.
Most of the research conducted in copper processing by
other SPD methods has also been essentially focused on the
study of the microstructural phenomena occurring during pro-
cessing as well as their effect on the final properties of the
processed structures. A strong enhancement in mechanical
strength, achieved through a wide range of SPD procedures,
such as high-pressure torsion [32], equal-channel angular
pressing [33, 34], multiple channel-die compression [35], el-
liptical cross-section spiral equal-channel extrusion [36],
equal-channel forward extrusion [37], is extensively reported
in literature. Formation of ultra-refined microstructures,
consisting of submicron, or even, nano-sized grains, is argued
in most of the works to be the main cause promoting the
mechanical enhancement of copper. Contrary to most of the
authors working in this field, who have especially emphasised
the mechanical enhancement of processed copper, Zhilyaev
et al. [38] studied the influence of the grain structure on the
electrical properties of pure copper. The electrical conductiv-
ity of pure copper with three different UFG structures,
achieved by combining two distinct SPD techniques, i.e.
high-pressure torsion and equal-channel angular pressing,
Int J Adv Manuf Technol (2015) 80:1655–1663
and that of the unprocessed coarse-grained material were stud-
ied. No significant changes in this property were found by
varying the grain structure of the material.
In current work, copper C12200 was friction stir processed.
The main aim of this investigation was to conduct an in-depth
analysis of the influence of the tool geometry and processing
parameters (tool rotation (ω) and traverse (v) speeds) on the
microstructural, mechanical and electrical properties of the
friction stir processed structures.
2 Experimental methods
Copper C12200, temper class H02, was friction stir processed
in current work. The plates were processed using conical (C)
and scrolled (S) shoulder tools, whose geometry and dimen-
sions are shown in Fig. 1 and Table 1, respectively. A constant
plunge force of 7000 N was used for both tools. Table 2 pre-
sents the full set of processing conditions used in this work:
tool rotation speeds of 400, 750 and 1000 rpm and tool tra-
verse speeds of 160 and 250 mm/min were combined and
tested. As shown in the table, the nomenclature adopted in
the text to classify the processed samples of each series iden-
tifies the tool geometry and the rotation and traverse speeds
used in each processing operation. Thus, C_750_16 labels a
sample processed with the conical tool (C) and rotation and
traverse speeds of 750 rpm and 160 mm/min, respectively.
Table 2 also displays the tool rotation to traverse speeds
ratios (ω/v) since, according to FSW literature [39–43], the
heat input during welding/processing is proportional to this
parameter. Analysing the ω/v values presented in the table, it
is possible to conclude that the 400_25 (ω/v=1.6 rev/mm) and
the 1000_16 (ω/v=6.25 rev/mm) processing conditions pro-
vide the lowest and the highest heat input during processing,
respectively.
Samples for metallographic analysis were prepared accord-
ing to standard practices and etched using a solution of FeCl3
(2.5 g), HCl (15 ml) and H2O (100 ml). Metallographic anal-
ysis was performed using an optical microscope ZEISS HD
100. Vickers microhardness measurements were performed
using a Shimadzu Microhardness Tester, with 200 g load
and 15 s holding time. Transmission electron microscopy
(TEM) observations were also carried out. Thin-foil speci-
mens, with 3 mm diameter, were prepared by double jet thin-
ner electropolishing in orthophosphoric acid (2:1) at room
temperature under 10 V tension. The TEM analyses were
performed in a transmission electron microscope Fei Tecnai
G2 S-Twin. The grain size of the unprocessed and processed
materials was measured using the mean linear intercept meth-
od. Particularly, for UFG microstructures, this method was
complemented by performing hundreds of grain size measure-
ments over several TEM micrographs. The electrical resistiv-
ity was calculated by a four-probe technique using a Lock-in
Int J Adv Manuf Technol (2015) 80:1655–1663
Fig. 1 Conical (a) and scrolled
(b) shoulder FSP tools
(a)
SR830 amplifier and transformed into conductivity according
to International Annealed Copper Standards (IACS). The
measurements were carried out in a temperature range be-
tween 23 and 293 K.
3 Results and discussion
3.1 Morphology and microstructure
The results of the cross-section inspection of all processed
zones are displayed in Table 3 for soundness analysis, i.e. to
detect the presence of any internal discontinuities, such as
voids or cracks, inside the processed volume. From the table,
it can be concluded that all the samples obtained under the
hotter processing conditions (ω/v≥4 rev/mm) and/or using the
scrolled tool displayed sound morphologies. On the other
hand, small internal voids were detected for all the samples
processed with the conical tool under colder processing con-
ditions (ω/v<4 rev/mm). From the pictures of these disconti-
nuities, which are shown in Fig. 2, it is possible to check that
they are located in the processed zone middle thickness. In
FSW with conical tools, this type of discontinuities is com-
mon and currently assigned to inadequate flow of material
around the tool, which prevents the necessary interaction be-
tween the pin and shoulder-driven material flow volumes [44,
45]. Actually, these discontinuities are not observed when
processing under the hotter conditions (ω/v> 4 rev/mm),
which promote the required heat for softening the material
and, consequently, a more efficient material flow inside the
stirred volume.
Table 1 FSP tools characteristics
and tilt angle Processing series Tool characteristics
Shoulder
Geometry
C 6° Conical
S Scrolled
1657
(b)
Comparing the results in Table 3, it is also important to
emphasise the strong influence of the tool shoulder geometry
on the soundness of the processed material. In fact, no impor-
tant discontinuities were observed when processing with the
scrolled tool, independently of the processing parameters in
use. As reported by Leal et al. [46], the scrolled tool induces a
substantial interaction between the pin and shoulder-driven
material flows, avoiding the formation of the same type of
discontinuities registered for the samples processed with the
conical shoulder tool.
The optical microscopy pictures shown in Fig. 3 illustrate
the unprocessed material microstructure (Fig. 3a) as well as
the microstructure of the samples processed using the conical
tool with rotation speeds of 1000 and 750 rpm and traverse
speeds of 160 and 250 mm/min, i.e. samples C_1000_16
(Fig. 3b), C_1000_25 (Fig. 3c) and C_750_25 (Fig. 3d). Im-
portant differences in the grain size and structure of the un-
processed and processed materials are possible to be observed
by comparing the images. In fact, while the unprocessed ma-
terial reveals an equiaxed coarse grain structure with high
density of annealing twins (Fig. 3a), the processed samples
display a recrystallized fine grained structure with no evidence
of the presence of annealing twins (Fig. 3b–d). The presence
of annealing twins in the half hard (H02) unprocessed material
microstructure is an evidence of cold work prior to annealing.
Important differences in grain size between the samples
processed with 1000 and 750 rpm can also be depicted from
the optical micrographs displayed in Fig. 3. On the other hand,
for the samples processed with the same tool rotation speed
(1000 rpm), but with different traverse speeds (160 and
250 mm/min), no important differences in grain size or
Tool tilt angle
Pin
Diameter Diameter Length
14 mm 3 mm 1 mm 2°
14 mm 3 mm 1 mm 0°
1658 Int J Adv Manuf Technol (2015) 80:1655–1663

Table 2 FSP parameters Beyond the very small grain size, which was registered
Processed samples Processing parameters for all the samples processed with the scrolled shoulder tool,
Fig. 5 also shows the presence of cells with high density of
C series S series Rotation Traverse speed ω/v dislocations inside some of the grains. Comparing the three
(rpm) (mm/min) (rev/mm) micrographs, it is also possible to conclude that, although
C_400_25 S_400_25 400 250 1.6
the grain size does not vary significantly with varying pro-
cessing conditions, the density of dislocations inside the
C_400_16 S_400_16 400 160 2.5
grains varies by varying the processing parameters. In fact,
C_750_25 S_750_25 750 250 3
the density of dislocations of the sample processed with the
C_750_16 S_750_16 750 160 4.69
highest ω/v ratio (Fig. 5a) is smaller than that registered for
C_1000_25 S_1000_25 1000 250 4
the samples processed with lower ω/v ratios (Fig. 5b, c).
C_1000_16 S_1000_16 1000 160 6.25
This is due to the higher heat input (high ω) and slower
cooling rates (low v) during processing with high ω/v ratio,
which enabled the annealing of the dynamically recrystal-
structure can be depicted from the images. This assumption lized processed structure.
can be confirmed by analysing Fig. 4, where the average grain Leal et al. [46] and Tronci et al. [47] also studied the use of
size (GS) measured for the unprocessed and processed mate- conical and scrolled tools in FSW of very thin aluminium
rials is plotted as a function of the tool rotation and traverse plates, reporting important improvements in weld strength
speeds. According to the figure, whereas the average grain by welding with the scrolled tool. These authors refer that
size of the unprocessed material was 18 μm, for the materials the scrolled shoulder promotes a strong through-thickness tool
processed with the conical tool, the average grain size is much stirring action, causing more intense deformation of the
smaller and varies according to the tool rotation speed in use. plasticised material. Actually, assuming that the strain rate
Effectively, the average grain size increases exponentially during processing is influenced by the tool rotation speed
with the increase in tool rotation speed, specifically, from [48], and that this parameter was similar when processing with
1 μm, at 400 rpm, to 7 μm, at 1000 rpm. However, for a the conical and scrolled shoulder tools, the only driving force
constant tool rotation speed, no significant differences in grain conducting to the extra grain refinement has to be related to a
size were obtained by varying the traverse speed. higher density of dislocations inside the stirred volume when
From Fig. 4, it is also possible to conclude that the samples processing with the scrolled tool. Large number of disloca-
processed with the scrolled tool had much smaller average tions can still be observed inside the recrystallized grains
grain size than those processed with the conical tool. Owing shown in Fig. 5.
to the extra grain refinement experienced by the material proc- In order to check the previous assumptions, some hardness
essed with the scrolled tool, the microstructural analysis of the measurements were carried out. Figure 6 shows the hardness
S samples was conducted by TEM. Figure 5 shows TEM evolution with the reciprocal of the average grain size square
images of three processed samples, namely, the S_1000_16, root (GS−1/2) for all the C and S samples. The hardness evo-
S_750_16 and S_400_25 samples. Two of these samples are lution was analysed in light of the microstructural properties
representative of the highest (S_1000_16) and the lowest of the processed material, i.e. considering the results displayed
(S_400_25) heat input conditions. An average grain size of in Figs. 3 and 5 as well as in Fig. 7, which illustrates the TEM
0.5 μm was determined for all the processing conditions inspection conducted over the C samples. According to the
(Fig. 4) by performing grain size measurements over a large graph, although an important grain refinement was registered
number of TEM images. for almost all the samples processed with the conical tool

Table 3 Results from cross-

section inspection C series S series

Samples ω/v Inspection results Samples ω/v Inspection results

(rev/mm) (rev/mm)

C_400_25 1.6 Microvoids S_400_25 1.6 No discontinuities

C_400_16 2.5 Microvoids S_400_16 2.5 No discontinuities
C_750_25 3 Microvoids S_750_25 3 No discontinuities
C_1000_25 4 No discontinuities S_1000_25 4 No discontinuities
C_750_16 4.69 No discontinuities S_750_16 4.69 No discontinuities
C_1000_16 6.25 No discontinuities S_1000_16 6.25 No discontinuities
Int J Adv Manuf Technol (2015) 80:1655–1663 1659

Fig. 2 Internal discontinuities in C_400_25 C_400_16 C_750_25

5
the processed C_400_25 (a), C_
400_16 (b) and C_750_25 (c)
materials

(a) (b) (c)

(Fig. 4), a significant hardness increase relative to the unpro-
cessed material was only registered for the samples processed
with lower tool rotation speeds, i.e. 400 and 750 rpm. As
shown in Fig. 3d, for the C_750_25 sample, and in Fig. 7a,
for the C_400_25 sample, these processed materials displayed
important grain refinement relative to the unprocessed copper.
In turn, for the sample processed with 1000 rpm, although the
average grain size was reduced by more than 50 % relative to
the unprocessed material, no important differences in hardness
were registered. In fact, the samples processed with this tool
rotation speed were subjected to high heat input, responsible
for the recovery of the recrystallized grains (Fig. 7b), which,
despite the grain refinement, resulted in processed material
softening to the same hardness values of the half hard (H02)
unprocessed material.
On the other hand, the hardness values shown in Fig. 6 for
the samples processed with the scrolled tool, for which the
highest levels of grain refinement were registered, are in any
case much higher than that of the unprocessed material and
higher than those obtained for the samples processed with the
conical tool under similar processing conditions. The highest
hardness values were registered for the S_400_25 sample, for
which the highest dislocation density was registered (Fig. 5c).
The hardness for the samples processed with higher heat input
conditions, i.e. with 750 and 1000 rpm, is much lower,
denoting the occurrence of softening by recovery after dynam-
ic recrystallization (Fig. 5a, b).
It is also important to stress that, for the scrolled tool proc-
essed materials, the hardness versus GS−1/2 evolution does not
obey the Hall–Petch relationship (see equation in the chart) as

Fig. 3 High magnification Unpprocessed Matterial C_10000_16

micrographs (500×) of the
unprocessed copper (a) and the
C_1000_16 (b), C_1000_25 (c)
and C_750_25 (d) processed
materials

(a) (b)
C_1000_25 C_7550_25

(c) (d)
1660 Int J Adv Manuf Technol (2015) 80:1655–1663

Fig. 6 Hardness evolution with the average grain size

Fig. 4 Evolution of the average grain size with the processing parameters
(tool rotation and traverse speeds)
for the samples processed with the conical tool. This indicates
that the hardness of the conical tool processed copper is main-
ly governed by grain size, but the same is not valid for the
scrolled tool processed materials. In this case, the dislocation
density plays an important role in material strength, which
corroborates the assumption that the scrolled tool induces
higher values of plastic deformation inside the stirred volume
than the conical tool.

Fig. 5 TEM micrographs of the S_1000_116 S_750_16

processed structure of the S_
1000_16 (a), S_750_16 (b) and
the S_400_25 (c) samples

(a) (b)
S_400_255

(c)
Int J Adv Manuf Technol (2015) 80:1655–1663 1661

Fig. 7 TEM micrographs of the C_ 400_25 C_1

1000_25
processed structure of the C_400_
25 (a) and C_1000_25 (b)
samples

(a) (b)

3.2 Electrical conductivity

The electrical conductivity results registered for the unpro-

cessed copper and for S samples processed under three differ-
ent conditions (including the highest (ω/v=6.25) and lowest
(ω/v=1.6) temperature processing conditions) are illustrated in
Fig. 8. More precisely, Fig. 8a, b displays the conductivity
results registered at 23 and 293 K, respectively. The electrical
conductivity in % IACS for the processed samples and for the
unprocessed copper is also given in Table 4. From Fig. 8, it
can be concluded that the electrical conductivity at the lower
temperature of 23 K is considerably higher than at 293 K, for
all the materials. According to the literature, the conductivity
of copper C12200 may range from 92 % IACS, for a percent-
(a) age of phosphorus of 0.015 %, up to 78 % IACS, for percent-
age of phosphorus of 0.05 % [49]. As shown in Table 4, the
conductivity of the unprocessed material studied in current
work is outside this range, which can be attributed to its initial
half hardened condition (H02) and/or to an additional content
of impurities.
Another important conclusion that can also be drawn from
Fig. 8 is that the conductivity of the processed materials is

Table 4 Electrical conductivity at 293 K of unprocessed copper and S

processed material

Samples ω/v Electr. conductivity

(rev/mm)
(Ω.m)−1 ×107 % IACS

C12200 – 3.98 68.6

S_400_25 1.6 3.43 59.2
(b) S_750_16 4.69 3.87 66.7
Fig. 8 Effect of processing conditions on the electrical conductivity of S_1000_16 6.25 4.32 74.6
copper, at 23 K (a) and 293 K (b)
1662
always lower than that of the unprocessed copper, except for
the S_1000_16 sample, which displayed the highest conduc-
tivity values at both temperatures. Moreover, it can also be
observed that the conductivity of the scrolled tool processed
copper increases with increasing values of the ω/v ratio, at
both 23 and 293 K. This increase is especially important at
the very low temperature of 23 K.
The conductivity of any material is well established to de-
pend on the effect of the phonon scattering (Ωp), grain bound-
aries (ΩGB), impurities (ΩI) and defects, such as dislocations,
(Ωd) on electrons mobility. The effect of phonon scattering
becomes negligible at the very low temperature of 23 K,
which justifies the higher conductivity values registered at this
temperature for all the materials. However, neither the effect
of the phonon scattering nor the effect of the impurities may
justify the evolution of the conductivity of the processed ma-
terials with ω/v, since both effects will have a similar weight
on the conductivity for all the materials. So, the evolution has
to be related with the grain boundary and dislocation effects
on conductivity, i.e. with the specific differences in micro-
structure between the different processed materials.
As mentioned above, the conductivity of the scrolled tool
processed materials was found to increase by increasing ω/v.
Although no differences in grain size were registered for the S
processed material with increasing values of ω/v, a decrease in
dislocation density was noticed. In this way, the increase in
conductivity with increasing values of ω/v must be governed
by the dislocation effect, which becomes smaller when the
dislocation density decreases. In fact, the conductivity of the
S_1000_16 material, which was processed under high heat
input conditions, promoting the recovery of the recrystallized
structure, is even higher than that of the coarse-grained and
half hard unprocessed material (Fig. 8). This result indicates
that the dislocation effect on copper C12200 electrical con-
ductivity is stronger than the grain boundary effect.
4 Conclusions
The influence of the friction stir processing parameters on the
microstructural, mechanical and electrical properties of copper
C12200 was studied in current work. The following conclu-
sions were possible to be drawn.
& Tool geometry has strong influence on the soundness of
the processed material. Regardless of the processing con-
ditions, processed material discontinuities can be avoided
by using scrolled shoulder tools.
& Post-processed microstructural characteristics are highly
dependent on the geometry of the processing tool. As
opposed to the conical tool, the scrolled tool enables the
production of extremely refined microstructures,
Int J Adv Manuf Technol (2015) 80:1655–1663
composed of submicron-sized grains (average grain size
of 0.5 μm), for all processing conditions.
& The density of dislocations of the processed grains is
strongly influenced by the ω/v ratio, decreasing for in-
creasing values of this parameter.
& The major factors governing the hardness of the processed
materials vary according to the geometry of the processing
tool. The hardness of the material processed with the con-
ical tool, which ranged from, approximately, 90 to
125 HV0.2, is mainly governed by grain size. On the other
hand, the hardness of scrolled tool processed copper,
which ranged from, approximately, 115 to 130 HV0.2,
strongly depends on the density of dislocations.
& Electrical conductivity of the processed copper is mostly
governed by the density of dislocations inside the grains.
Improvement in the electrical conductivity of the proc-
essed material is possible to be achieved by increasing
the ω/v ratio.
Acknowledgments This research is sponsored by FEDER (Fundo
Europeu de Desenvolvimento Regional) through the program COMPETE
(Programa Operacional Factores de Competitividade) and by national
funds through FCT (Fundação para a Ciência e a Tecnologia), under the
project PEst-C/EME/UI0285/2013. The work is also sponsored by
FEDER funds through the program COMPETE (Programa Operacional
Factores de Competitividade), under the project CENTRO-07-0224-
FEDER-002001 (MT4MOBI). The authors are grateful to Doctor José
Paixão and to the Department of Physics of the University of Coimbra for
the electrical conductivity analysis.
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