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j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

Available online at www.sciencedirect.com

journal homepage: www.elsevier.com/locate/jmrt

An overview of friction stir processing of CueSiC


composites: Microstructural, mechanical,
tribological, and electrical properties

Mohammad Reza Akbarpour a,*, Homayoun Mousa Mirabad b,


Farid Gazani b,1, Iman Khezri b,1, Amirhossein Ahmadi Chadegani b,1,
Ali Moeini c,1, Hyoung Seop Kim d,e,f,**
a
Department of Materials Engineering, University of Maragheh, Maragheh, East Azerbaijan, Iran
b
Department of Materials Science and Engineering, Sharif University of Technology, P.O. Box 11365-9466, Tehran,
Iran
c
Department of Materials Engineering, Isfahan University of Technology, 84156-83111 Isfahan, Iran
d
Department of Materials Science and Engineering, Pohang University of Science and Technology, Pohang 790-784,
South Korea
e
Advanced Institute for Materials Research (WPI-AIMR), Tohoku University, Sendai 980-8577, Japan
f
Institute for Convergence Research and Education in Advanced Technology, Yonsei University, Seoul 03722, South
Korea

article info abstract

Article history: Copper matrix composite reinforced with SiC exhibits high electrical and thermal con-
Received 27 June 2023 ductivity, as well as superior mechanical properties, making it a potential candidate for
Accepted 20 September 2023 thermal management applications. There has been rapid progress in the understanding of
Available online 24 September 2023 CueSiC metal matrix composites during the past decade. To accomplish this, powder
metallurgy, casting, selective laser melting, composite electroforming technology, and
Keywords: electrodeposition methods have been employed. The optimum cutting conditions for
Copper fabrication of CueSiC metal matrix composites are still being explored. In recent years,
Friction stir processing friction stir processing (FSP) has become increasingly popular in the fabrication of com-
Composites posites. FSP is capable of microstructural engineering in CueSiC systems. In light of the
SiC fact that the electrical/thermal conductivity and mechanical performance of CueSiC
Mechanical properties composites depend on microstructural characteristics such as SiC distribution, grain
size, grain orientation, density of dislocations, and bulk density, it seems important to
study the effect of manufacturing conditions on microstructure in detail. In this study, the
influence of FSP parameters such as rotational and traversal speeds, the number of FSP

Abbreviations: AS, Advancing side; BM, Base metal; CTE, Coefficient of thermal expansion; DFSP, Direct Friction stir processing; DRX,
Dynamic recrystallization; EDS, Energy dispersive X-ray spectroscopy; EL, Elongation; FSP, Friction stir processing; FSW, Friction stir
welding; GBS, Grain boundary sliding; HAZ, Heat affected zone; MMC, Metal matrix composites; MGT, Multi groove technique; MG3C,
Multi groove having 3 channels; OIM, Orientation (Imaging) Microscopy; RS, Retreating side; SEM, Scanning electron microscope; SPD,
Severe plastic deformation; SGT, Single groove technique; SQ, Square pins; SZ, Stirring zone; SC, Straight cylindrical; TMAZ, Thermo-
mechanical affected zone; UTS, Ultimate tensile stress; UFG, Ultra-fine grain; YS, Yield strength; 1P, 1 pass of FSP.
* Corresponding author.
** Corresponding author. Department of Materials Science and Engineering, Pohang University of Science and Technology, Pohang
790-784, South Korea.
E-mail addresses: [email protected] (M.R. Akbarpour), [email protected] (H.S. Kim).
1
These authors are equally contributed to this work.
https://doi.org/10.1016/j.jmrt.2023.09.200
2238-7854/© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
1318 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

passes, and the pin profile as well as the characteristics of SiC powder are discussed in
detail with regard to macro- and microstructure, hardness, strength, tribological, and
electrical properties of FSPed CueSiC composites.
© 2023 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

affecting secondary phase distribution and consequently the


1. Introduction matrix properties. The geometry of tools like pins and shoul-
ders, materials characteristics such as base metal and ceramic
Friction stir processing (FSP) is rather a new and complex particle properties, and procedure factors like tool rotational
solid-state technology used for grain refinement, solid-state and travel speed and load directly affect the properties of the
joining, and fabricating surface composites based on funda- surface composite [7,8].
mental principles such as friction stir welding (FSW) [1,2]. FSP The most common methods employed for introducing the
was invented in 1999, 8 years after the invention of the FSW, secondary particles are groove filling [9e12], hole filling
as a localized surface modification, microstructure control, [13e15], direct FSP (DFSP) [16], and sandwich [17,18]. Groove
and property enhancement method [3]. FSP is a material filling (Fig. 2a) was the original method used by Mishra et al. in
processing technique that utilizes a special non-consumable order to fabricate Al-based composites [19]. This method
tool with a shoulder and pin. The shoulder applies pressure produces a narrow groove in the base metal sheet or surface.
to the material, while the pin creates a rotating vortex that After the groove is filled with reinforcements, FSP is utilized to
causes severe plastic deformation and friction. Therefore, it develop the surface composite [20]. In the closed method, the
can be regarded as a material processing technique for severe groove filled with the secondary particles is closed with a pin-
plastic deformation (SPD) [4,5]. Fig. 1 shows a schematic less tool. The friction between the pin-less tool and the base
illustration of the FSP process and related components. During metal surface leads to heat generation, and the surface of the
FSP, heat is generated due to the friction between the top of groove is closed to prevent the secondary particles from flying
the workpiece and the tool shoulder as the pin descends to the out during the FSP process [21].
workpiece and the shoulder contacts the work surface. In the hole filling method (Fig. 2b), tiny holes are created on
Consequently, plastic flow occurs due to material softening the base metal surface and filled with the secondary phase,
from heat generation, leading to different zones with inherent and FSP is carried out to fabricate the surface composite.
microstructural characteristics [6]. Similar to the groove filling method, it can be used with a pin-
In surface composites fabricated using friction stir pro- less FSP tool to close the holes with generated heat, and then
cessing techniques, the type of method employed to insert FSP with a pin tool is performed to fabricate surface composite
secondary phases into the base metal is a critical factor [13].

Fig. 1 e Schematic illustration of the FSP technique (a) and different macrostructural zones created during FSP (b)
(reproduced from Ref. [22]).
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9 1319

Fig. 2 e Schematic illustrations of the FSP process by groove filling method (a) and hole filling method (b).

The FSPed material has limited width for many practical composites and modify mechanical properties like hardness,
applications. The width of the FSPed region could be increased fatigue, tensile strength, wear, and corrosion without
by increasing the pin dimension or using multiple overlapping affecting the bulk material's properties [24,25,37,62,67].
passes. In the case of the increased pin size, the tool and the Whereas multiple reviews on the fabrication of MMCs with
machine need to generate much more torque and power, FSP have been documented, to the best of our knowledge,
respectively; therefore, FPS with multiple passes is a more there has not been a systematic review on the fabrication of
popular method [23e26]. The most common pass patterns in CueSiC MMCs with FSP and the impact of various parameters
the multiple pass method are parallel, raster, and spiral [8,27]. on the microstructure and mechanical characteristics of these
In recent years, the physical and mechanical properties of surface composites. The present study focuses on recent ad-
FSP-processed Cu alloys have been extensively studied [28]. vancements in the development of CueSiC MMCs utilizing
Achieving ultrafine grain microstructure using FSP and active friction stir processing. In this regard, this paper addresses the
cooling has been studied in several works [29e31]. Copper is a characterization of CueSiC MMCs created by FSP and the
promising material for thermal management applications due primary factors that hamper the manufacturing process. In
to its high thermal conductivity, but its high coefficient of the following, the microstructural changes that occur during
thermal expansion (CTE) and low strength limit its applica- the process and the impact of the process parameters and the
tions [32e34]. The mechanical and thermal properties of material characteristics will be discussed in detail. Afterward,
copper can be significantly improved with the incorporation of parameters affecting mechanical properties and tribological
reinforcing particles in Cu-based metal matrix composites characteristics are critically investigated. Overall, this study
(MMCs). primarily analyzes the current development trends and recent
Various secondary particles such as carbides [35e37], sul- advancements in using FSP to produce CueSiC surface MMCs.
fides [38], oxides [39,40] and carbon-based nanomaterials
[41e43] have been added to the Cu matrix so as to improve its
mechanical performance. SiC is a promising candidate among 2. Macrostructural evolution during FSP of
potential secondary particles due to its high elastic modulus CueSiC samples
(~424 GPa) [44], high thermal conductivity (~360 W⁄mK) [45],
low CTE (~5  106 K1) [46], and good chemical inertness During FSP, the samples undergo plastic deformation due to a
[47,48]. Therefore, SiC particles are included as reinforcement combination of frictional heat and the mechanical, to be
in the form of whiskers, particles, and fibers in various com- precise forging, force of the tool. A banded structure forms on
posite materials, including metal matrix composites, to the surface due to friction processing [68]. This corresponds
enhance their mechanical and thermal properties. virtually to the diameter of the shoulder; moreover, the pin's
CueSiC MMCs are fabricated through various solid, liquid, length matched the depth of the microstructural change zone
and solid/liquid state methods. Liquid-state method applica- [26,69,70]. Although all samples (reinforced and unreinforced)
tions are limited due to the accumulation of SiC particles and were produced using identical processing parameters, the
extensive surface reactions at the CueSiC interface. As a appearance of the crowns differs noticeably. The variation in
result, various solid-state methods have been developed to heat generated on the surfaces of processed plates may ac-
fabricate CueSiC MMCs, such as powder metallurgy [49e62] count for the differences in surface characteristics [71,72]. The
and FSP. movement of the plasticized copper outside the tool working
The first use of the FSP method for metal matrix compos- area caused distinctive material outflows, which resulted
ites was conducted by Mishra et al. for AleSiC composites [3]. from lowering the shoulder below the surface of the processed
Based on their work, the fabrication of surface or bulk com- material, to form on the band's edge. The height of the outflow
posites is studied with different approaches to incorporating increased with the path traveled by the tool [26,73].
the ceramic particles into the metal matrix [63e66]. Over the It is crucial to have a smooth crown appearance since
past ten years, much research has been done on FSP as a solid- different internal flaws in the surface composite are caused by
state grain refinement method to produce surface-level surface imperfections in the crown [11,72,74]. Although the
1320 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

Fig. 3 e a) Crown surface of FSPed CueSiC composites, b) heat generation influence on the SZ macrostructure, c) peak
temperature profile in different process parameters (reproduced from Ref. [75]).

banded structure, referred to as an “onion ring”, is evident in crucial for a defect-free SZ zone, so multi-grooved FSP sam-
FSW processing, a smoother crown could be obtained with a ples have smoother crown surfaces [72,78].
multi-groove scheme. The composite plates made using the Heat input during FSP affects grain growth and dynamic
multi-groove approach received more heat than the ones recrystallization, which determine how the FSPed surface will
made using the single-groove technique; hence, they had ultimately be formed [75]. The total heat generation (Q) during
higher heat transfer through the plate depth. Higher heat FSP in its general form is provided below, where the value of
transfer could contribute to a high-temperature gradient “X” is calculated depending on the tool pin profile and is 3 for a
through the plate, allowing suitable mixing of plasticized straight cylindrical pin profile [79].
copper in vertical and rotary routes, resulting in a smooth
2  
crown [71,72]. Additionally, it can be deduced that heat gen- Q¼ pumt R3 þ X  r2  h (1)
3
eration increases incrementally by raising the number of
grooves [72]. Process parameters can affect the heat input, where the Q:u:m:t:R:r and h are input heat, tool rotational
which changes the stirring zone (SZ) shape. As an illuminative speed, friction coefficient, shear strength, pin diameter at the
example, Fig. 3 shows that lowering the rotational speed is top, pin diameter at the root and pin height, respectively [80].
bound to result in a basin-shaped SZ alongside the cavity in It can be deduced from Eq. (1) that the heat input (Q) directly
the RS zone due to low heat input. On the contrary, correlates with rotational speed and reversely relates to pro-
trapezoidal-shaped SZs could be obtained without any cavity cessing speed, as shown by:
at high rotational speed [75]. During the process, it should be
u
noted that “tool dragging” might result from low plastic Qf (2)
n
deformation of the copper and an inadequate amount of
plasticized copper to fill the space behind the pin [26,70,76]. where u and n are the rotational and process speeds, respec-
Heat generation during FSP, overall, is calculated based on tively. Heat input rises as the rotational speed grows or the
friction between the tool shoulder and the plate sample, along process speed declines, leading to a greater peak temperature.
with the amount of plastic deformation [77]. The composites Using K-type thermocouples, the usual temperature distri-
made by the multi-groove technique contain copper between bution profile of the samples has been depicted in the AS and
the successive grooves; therefore, the contact area increases. RS [6,75]. These curves provide crucial details on the highest
These excessive contact areas contribute to heat generation as temperature generated by the processed material as well as
well as the outer edge of grooves, increasing the heat input the rate of heating and cooling during FSP. These rates are of
capable of softening copper at high temperatures and forcing considerable value for controlling grain growth [6,77,81]. It
it to move from the advancing side (AS) toward the retreating was found that the heating rate greatly varies with processing
side (RS) in order to composites fabrication. Sufficient heat is speed and that peak temperature and heat generation
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9 1321

Fig. 4 e Typical defects appearing at the FSW joints: (a) flash, (b) tunnel, (c) keyhole, (d) cavity, (e) groove, and (f) lack of root
penetration (reproduced from Ref. [90]).

strongly depend on the tool's rotating speed. Increasing pro- This action can lead to the flow of material and the production
cessing speed means less time exposure to above recrystalli- of heat due to the friction between the spinning tool and the
zation temperature; thus, with growing rotational and process welding workpieces. The revolving tool retracts once FSW has
speeds, the peak temperature, like heat input, rises and falls, been completed, and a keyhole forms at the weld's end, which
respectively [6,75]. immediately loses its mechanical qualities [83]. Additionally,
Tool tilt angle is another influential factor besides rota- inappropriate process parameters or technical conditions can
tional and processing speeds. The material flow pattern in SZ result in additional welding flaws, including cavities [84],
during FSP, effective stirring action, and frictional forces are tunnels [85], grooves [86], and kissing bonds [87], which are
all enhanced by raising the tool tilt angle from 0 to 2, resulting detrimental to mechanical efficiency [86]. It is determined that
in a considerable change in heat generation [6]. Extensive a number of distinguishing flaws are either flow- or
specific surface contact between the tool and the workpieces geometric-related. The flow-related errors take place beyond
when the tool tilt angle is 0 results in excessive heat buildup the permissible processing zone with values that are deemed
during FSP. The plasticized material is pulled away from the to be either too hot or too cold [88]. For instance, a greater
center of the stir zone by excessive heat in the stir region, welding heat input or a deeper plunge depth might produce
creating FSP zones. Due to effective forging and stirring action, flash flaws that thin the weld and localize stress. Inadequate
the plasticized material flow is sufficient at greater tool tilt material flow induced by less heat input causes interior joint
angles. Less porosity will result from effective forging and flaws, including voids, tunnels, and grooves. Khan et al. [85]
stirring, so fine, homogeneous grains will be developed [75,82]. found that the plunge depth and offset utilized during friction
It is noteworthy that although the peak temperature during stir welding (FSW) of 5083-H116 and 6063-T6 aluminum alloys
FSP reached somewhat between 352 K and 513 K, this amount had a notable influence on the formation of kissing bond and
is below half of the pure copper melting point, which impli- tunnel defects [89]. Untreated surface imperfections can pre-
cates the fact that FSP is a promising solid-state process with a sent significant challenges in terms of stress concentration,
low energy requirement for fabricating surface composites corrosion susceptibility, and surface integrity.
[6,75]. Fig. 4 displays a range of typical faults that manifest at the
Welding defects that can occur during the welding process FSW joints. Welding defects may be categorized into global
weaken the weld and reduce its quality. It is important to and local defects based on their characteristics and kinds.
identify and remove these defects to ensure the quality of the Surface peeling, grooves, tunnels, kissing bonds, lack of root
weld joint. FSP is a variant of FSW that has been altered; penetration, surface damage, and cracks brought on by an
therefore, FSP contains flaws similar to those found in FSW's external source are the major features of global defects,
basic process. In the following paragraph, FSW joint defects whereas keyhole, cavity, and pitting defects are the most
will be interpreted first. common local volume defects [90]. The term “keyhole defect”
During the FSW process, a rotating tool equipped with a refers to a hole that closely resembles the rotating pin's form
shoulder and a pin is inserted into the welding workpieces. and is brought on by a hole that is created when the rotating
1322 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

Fig. 5 e Influence of FSP parameters on the defects.

pin is retracted [88]. Additionally, a high forge load or plunge defect, optimizing the conical angle and top diameter to in-
depth, an overly hot weld, or a smaller shoulder diameter can crease the pin volume may contribute to sufficient material
all cause excessive overflow of materials on the top surface, flow. These materials advanced downward and compressed
which results in a corrugated or ribbon-like pattern along the the pin and workpiece, eliminating flaws and enhancing
RS or AS. This is known as flash [91]. Additionally, grooves or interfacial bonding [103].
cavities may be produced as a result of inadequate material FSP was developed as an extension of the principles un-
flow, low forge pressure, or inadequate heat input [92e94]. A derlying FSW, as previously discussed [19]. Basically, these
cavity is the imperfect connection caused by inadequately two processes have comparable characteristics and micro-
consolidated and forged materials at the RS, and a groove is a structural changes. FSP, however, is used to modify the
continuous dented surface that is characterized by insuffi- structure rather than join or weld two metal sheets together
cient fill with plasticized materials. An interior void running [104]. Most of the flaws in the two processes are the same.
perpendicular to the welding direction is a tunnel flaw that Fig. 5 illustrates the impact of process parameters on the
results from inadequate material flow or a smaller depth of occurrence of defects in FSP. During FSP, the heat produced by
the plunge [95,96]. Lack of root penetration, also known as SPD and frictional contact raises the workpiece's temperature,
incomplete connecting at the rear of the butt-plate, is another causing the material behind the shoulder to excessively
consequence of that. A shorter pin may have also resulted in a soften. The material will burst out as a flash if the shoulder
lack of root penetration [90]. pressure is excessive. This flaw therefore causes the material
Aluminum and magnesium alloys may be repaired using in the SZ to thin [105]. Numerous macro-defects, such as
the benefits of friction stir welding and processing, which are porosity, grooves, fractures, voids, and tunnels, among others,
distinguished by low temperature, severe plastic deformation, may develop during the FSP process as a result of insufficient
and excellent quality [97,98]. Repetitive FSP has been proposed material flow or excessive or inadequate heat input, which are
to address small-scale groove or crack defects in AA2219 FSW primarily impacted by rotational speed (u) and travel speed
joints. To ensure the interface between filler materials and (y). The results reveal that greater tool rotational speeds create
flaws, it is crucial to introduce filler materials for defects of more heat, resulting in increased thermal stress during the
significant size [99,100]. To eradicate significant groove flaws cooling process, whereas lower tool rotational speeds result in
that cannot be addressed by repeating FSW/P, tungsten inert inadequate material flow [106,107]. As a result, processed
gas welding (TIG) and FSW were utilized [101]. To address the workpieces free of flaws can only be created at the optimum
volumetric defects, a combination tool with a consumable pin rotating, plunging, and traversing speeds. For instance,
and a non-consumable outer shoulder was suggested [102]. regarding the AZ91 material, a defect-free sample was pro-
During the repair operation, the shoulder presses against the duced at a ratio of 20 (u ¼ 1200 rpm, y ¼ 60 mm/min) and a
workpiece's surface as the pin is inserted, regulating the shape maximum temperature of 475  C [105].
and performance. Pins of different geometrical dimensions In FSW/FSP-related technologies, the tool is essential for
have an impact on the mechanical and microstructural altering material flow and microstructure, among other pro-
characteristics of joints. For the objective of fixing the keyhole cess parameters. The tool shoulder and pin shape design for
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9 1323

Fig. 6 e a) Grain map of FSPed Cu produced by OIM, b) distribution of the grain size in area fraction and number of fraction
(reproduced from Ref. [125]).

microstructural and mechanical property optimization was affected zone (TMAZ), heat-affected zone (HAZ), and base
the subject of several prior investigations. When it comes to metal (BM) [6,62,116].
tool pins, a tapered tool pin with screw threading offers the Due to severe plastic deformation and frictional heat
best mechanical and microstructural qualities [108]. The tool occurring simultaneously, the stir zone of the specimens
pin thread pitch plays a significant role in producing a process made by FSP had an equiaxed and fine microstructure [73,117].
zone devoid of defects. A stepped, conical, threaded pin en- The FSP process leads to significant plastic deformation of the
hances material flow, enhancing mechanical characteristics material. The grains break down during plastic deformation,
and joint integrity, while effective material flow is provided by creating a lot of low-angle, misoriented grain boundaries and
a polygonal pin profile [109]. Ultimately, defect-free process extremely favorable nucleation locations during recrystalli-
zones were produced using pin profiles that were square [107], zation [118,119]. There appear to be two main causes for var-
conical, triangular [110], straight-cylindrical, tapered-cylin- iations in grain size: (1) heat input that results in annealing,
drical [111], and cubic. Despite the effectiveness of the tool pin leading to grain growth [120,121]; (2) continuous dynamic
design, a shoulder to-pin diameter ratio of 3 could result in the recrystallization brought on by the tool pin's stirring action,
ideal microstructure irrespective of that [112]. producing new nucleation sites and reducing the grain size
[24,62,73,79]. During dynamic recrystallization (DRX), low-
angle boundaries become high-angle ones, and new grains
3. Microstructural evolution during FSP of form at preferred sites [74,119]. Once the fine-grain nuclei
CueSiC samples have begun to form, a microstructure with fine, equiaxed
grains is produced [122e124]. The fine structure produced in
3.1. Microstructural changes in copper matrix the stir zone of the specimens indicates that the second
explanation is prevalent [25,62,73]. Jian-Qing Sua et al. [125]
The FSP process can largely refine the grains at the micro- performed FSP on commercial OFHC (C10100) copper to assess
scopic level. According to various reports, the copper base the properties of microstructures at various positions behind
grain size is between 30 and 65 mm [4,24e26,62,72e75, the pin tool extraction. According to Fig. 6, equiaxed, virtually
79,113e115] while the average grain size in the stirring zone is random-oriented grains surrounded by high-angle boundaries
significantly finer and approximately 21 times smaller make up the resultant microstructures. Most grain sizes are
[4,26,73]. Generally, the samples consist of different parts, between 50 and 300 nm, with average sizes of 109 nm (num-
including the stirring zone (SZ), thermos-mechanically ber-weighted) and 174 nm (area-weighted), respectively [125].
1324 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

Comparing CueSiC samples to pure Cu, the specimens was the most successful [130]. However, because of the severe
manufactured containing SiC reinforcements had smaller wear exhibited with SiC reinforcements, this technique re-
grains than the ones without SiC particles. This is owing to the quires more wear-resistant FSP tools.
nucleation and pinning action of SiC particles, which restrict The process variables have significant effects on how SiC
grain growth and subsequently reduce grain size compared to particles are refined and dispersed during the FSP. The SiC
the FSPed samples without SiC additives [62,73,74]. Moreover, particles could not be sufficiently refined and uniformly
according to the reports, the grain size of the metal matrix dispersed when the tool's traverse speed or rotational speed
nanocomposites manufactured by one-pass FSP is larger than was too low or too high. When the tool's traverse speed was
that of those fabricated by four-pass FSP. An increase in constant but its rotational speed was too slow, the lower
passes results in a larger degree of SiC particle breakup and temperature in the processed zone caused the matrix's poor
dispersion, which enhances the pinning action and inhibits plasticity, which prevented the SiC particles from flowing
dislocation migration. Additionally, the SiC particles break completely with the matrix and distributing evenly. On the
down at higher passes, which increases the number of scat- other hand, when the tool rotated too quickly, the higher
tered particles and amplifies the pinning effect [24e26]. temperature in the processed zone improved the matrix's
Therefore, the grain size in SZ is reduced by fine and highly plasticity, but also reduced the extrusion and shear forces on
distributed SiC particles. According to Barmouz [25], the SiC particles, allowing them to maintain their large size.
increasing the number of passes from 1 to 8 reduces the grain The SiC particles were refined and evenly dispersed when the
size to virtually 800 nm. The pinning effect enhances these tool's rotational speed and traverse speed were matched.
particles' capacity to prevent grain growth despite a sufficient In research conducted by Zahmatkesh et al. [131], APS was
increase in temperature (up to three-fourths of Tm), ultimately employed to deposit reinforcement particles of Al2O3 on the
leading to delaying the grain boundary sliding (GBS). Greater Al2024 substrate. Their findings indicated that using FSP
dynamic recrystallization in SZ, which increases the number technology enhanced Al2O3 dispersion, resulting in fewer
of active nucleation sites and subsequently reduces the grain cluster locations [75]. Due to good forging action, a minor
size, may be another explanation for higher grain refinement adjustment of the tool tilt angle from zero to two degrees
in higher FSP passes [126]. It is noteworthy that although a helps the improvement of the hardness and uniform distri-
sharp decrease in SiC particle size was found at the second bution of SiC particles [81]. Either at fast progress speeds or
pass, the SiC particles fragmentation in higher passes is less low tool rotation speeds, SiC particle agglomeration would
obvious. Similar results have been reported in the case of occur at the sample surface [10]. Agglomerates often have
aluminum alloys with 6 and 3 passes of the FSP process with fewer crack-resistant properties since the matrix does not
particulate SiC additives [127,128]. typically separate the particles from one another. Because
As stated in the preceding section, FSP is a solid-state liquid matrix cannot or only sporadically can enter an
process. Hence, a great advantage of this technology is that agglomeration, material discontinuities are most frequently
no intermetallic compound can be formed after FSP. This found in the center of the agglomerate [26]. The potential for
corresponds to Bauri et al.'s observation of the Al/TiC com- producing undesirable local aggregates of particles, or ag-
posite produced by FSP [128]. Cu composites with SiC rein- glomerates, is a significant technological issue affecting liquid
forcement are considered the finest for electronic packaging matrix technology [74,132,133]. As shown in Fig. 7, a higher
and thermal management use. But two significant issues that traverse speed produced a larger grain size. In other words,
prevent the fabrication of Cu/SiC composites by casting are the SiC particles' tendency to agglomerate rises with
low wettability and a considerable reaction between SiC and increasing the traverse speed.
molten Cu [129]. Cu þ SiC]Cu3Si þ C is the reaction that oc- The uniform distribution of SiC particles within the copper
curs when SiC particles are poured into pure Cu during the matrix's stir zone was attributed to extreme stirring and
casting of the Cu/SiC composite [126]. Properties of compos- adequate material flow, which decreased the probability of
ites such as reduction of thermal conductivity may be agglomeration [62,134]. This corresponds to Kumar et al. [72]
impacted by the formation of intermetallic compounds. findings through EDS mapping. According to Fig. 8, it can be
Nevertheless, the formation of intermetallic compounds is deduced that SiC distribution is more uniform by applying the
not possible due to the lower temperature of FSP in compari- MGT process. In addition, the dispersion of the reinforcement
son to casting [4]. particles is different in each zone. The average fraction of the
reinforcing phase was 9.4% ± 1% in the stirring zone during
3.2. SiC particle distribution by FSP FSP treatment. In the TMAZ, at the edge of the stirring zone, a
larger proportion of the reinforcing phase has been detected,
FSP has recently been researched for composite fabrication, 18.6% 3%, approximately twofold of the SZ. But only in areas
and many reinforcing techniques have been reported in the where the pin-threaded side walls impacted the material high
literature. Miranda et al. [130] exploited three distinct tech- SiC particle contents were observed. Only 2.3% and 0.5% of SiC
niques for incorporating reinforcement into the workpiece. particles were present in the narrow subsurface zone, where
Three different investigated techniques include FSP with the lower flat part of the pin is located, with a thickness of
reinforcement particles inserted in a groove in the workpiece, around 100e120 mm [62,74]. Furthermore, using holes rather
FSP with reinforcement particles evenly distributed across the than grooves could result in a more uniform dispersion of SiC
workpiece before processing, and FSP utilizing a consumable particles, leading to a smaller final grain size.
aluminum rod with holes punched into it. The second tech- The multi-pass FSP decreased cluster size while homoge-
nique, using reinforcing particles applied to the workpiece, nizing the dispersion of reinforcement particles [9]. It could be
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Fig. 7 e SEM images of FSPed samples with rotational speed of 900 rpm and traverse speed of 40 mm/min (a) and 200 mm/
min (b) (reproduced from Ref. [73]).

assumed that the six-pass FSP completely and uniformly uniform SiC dispersion occurs within underwater FSP
dispersed the Nano SiC particles [135]. However, the size of the (UWFSP) conditions despite the peak temperature of in-
agglomerated SiC nanoparticles decreases with the number of process FSP being lower. This is primarily because the
FSP passes, due to the increased material flow that occurs in UWFSP state inhibits the transfer of heat from the SZ to the
the stir zone for specimens treated by consecutive FSP passes. surrounding region while barely affecting the local tempera-
Moreover, further FSP passes may cause material flow and tures around the tool pin. Additionally, having water near the
applied strain to break up the clustered SiC nanoparticles, tool pin concentrates heat around it, enhancing material flow
improving the nanoparticle dispersion [136]. Similar results [140,141]. These facts promote uniform SiC particle dispersion
were found in Al/ZrO2 composites fabricated successfully by and improve the grain structure in 5th pass of UWFSP while
multi-pass FSP [137]. For specimens that have undergone one water is at room temperature or 10  C in comparison with the
and two passes of FSP, large clusters of SiC nanoparticles are air FSP cooling condition [139].
formed at the retreating side of the stir zone due to the The chance of multiple pins applying a load to the SiC
characteristic of material flow during FSP, resulting in brittle particles during the FSP process was greater than it was for a
fracture in these areas. In contrast, during the third pass of single pin. Therefore, compared to the single-pin tool, the
FSP, the SiC clusters can be broken and distributed uniformly multi-pin tool had a greater refining impact on the SiC parti-
[138]. Srivastava et al. [139] investigated the influence of multi- cles. The ideal matching of process parameters was achieved
pass FSP cooling environments on the evolution of micro- with a multi-pin tool as opposed to a single-pin tool at a
structure characteristics. One significant finding is that slower traverse speed when the process parameters were the

Fig. 8 e SEM image and EDS map analysis for the elements Cu, Si and C of Cu/SiC surface composites fabricated by multi-
groove technique (reproduced from Ref. [72]).
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Fig. 9 e Images of the FSP tool using a single pin (a) (reproduced from Ref. [143]), multiple pins (c), and the impact of pin
model on the flow of plastic material (bee) (reproduced from Ref. [142]).

same because the multi-pin tool was better at stirring and after being rubbed and stirred by pin A, flow A and flow B
creating frictional heat [142]. would be stirred again by pin B, and flow C would be stirred
As SiC particles flow with the matrix material during again by pin C as well [142].
composite fabrication, the pin's impact on material flow can
be used to infer its impact on SiC particle dispersion. A model 3.3. Interfacial characteristics of FSPed CueSiC
was developed to study the effect of pins on the plastic flow of composites
material during FSP. Fig. 9 shows the impact of the single and
multiple pin methods on the plastic flow during the FSP pro- The reinforcement-matrix interaction is critical to the per-
cess. In the single-pin method (Fig. 9a and b), the moving pin formance of MMCs. Continuous and robust bonding between
split the plastic flow of material into two pieces, which were matrix and reinforcement results in superior load transfer,
then deposited behind the tool. However, in the multiple-pin electrical, and thermal performance. Inadequate bonding, on
method (Fig. 9cee), the offset pins on the tool caused the the other hand, leads to interface debonding, performance
movement of each pin and tool to be different. Furthermore, degradation, and manufacturing issues. One of the most
the offset pins divided the plastic material flow into many important parameters affecting the mechanical, thermal, and
strands. As can be seen in Fig. 9d and e, the initial pin electrical performance of SiC-reinforced copper composites is
disturbed the plastic flow of the material because the pins the quality of the Cu/SiC interface.
were moving faster than the substance, and subsequent pins Nikolopoulos et al. [144] investigated the wettability of the
repeatedly scraped and stirred it. For instance, immediately CueSiC interface using the sessile drop technique and found
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that the contact angle always remained greater than 90 ,


indicating poor wettability. Additionally, the presence of the 4. Parameters affecting the performance of
reaction zone was reported at temperatures higher than FSPed CueSiC
900  C [145]. As a general rule, the thickness of the reaction
layers increases as time and temperature increase. Moreover, 4.1. Effect of process parameters
according to the CueSiC phase diagram, due to the solubility
of silicon in copper (5% at 850  C [146]), silicon diffuses into Several researchers have discovered through their experi-
copper, and the extra carbon forms a graphite layer [147]. This ments that the rotational and traverse speeds are essential
phenomenon leads to a reduction in the thermal and electrical parameters for the properties and performance of FSPed
conductivity of the CueSiC composites. Fig. 10a and b depicts composites. Optimization of rotational and traverse speeds
the Cu/SiC interface in powder metallurgy obtained from leads to optimal dispersion of the powder and a reduction in
composite sintered at 950  C for 3h. As can be seen, the re- microstructural defects [9,25,73].
action zone is formed due to the high sintering temperature Eq. (1) shows that the tool's rotational speed during the FSP
[148]. Depositing a coating on the reinforcement's surface, process has a direct impact on heat generation. Several
alloying the matrix and optimizing process parameters are the studies have studied temperature shifts due to the higher
most promising methods to address this issue [45,149,150]. rotational speed. This increase in temperature affects grain
As shown in Fig. 3c, the maximum temperature in the FSP growth in samples since dynamic recrystallization occurs
process does not exceed 600  C [75]. Therefore, in the case of during FSP [4,5,75].
FSP-obtained CueSiC MMCs, the formation of a solid solution Raaft et al. [134] reported that increasing the rotational
and reaction zone at the Cu/SiC interface is limited due to the speed from 1200 to 1400 rpm at constant traverse speed leads
lower process temperature. It is noteworthy that there is still a to better graphite distribution and reduced particle agglom-
lack of research on the Cu/SiC interface in FSPed CueSiC eration in the A390 matrix. This phenomenon is attributed to a
composites. higher level of softening at a higher rotational speed, leading
Fig. 10c demonstrates a highly magnified SEM micrograph to more effortless stirring action. According to the Zenner-
of the SZ of the CueSiC composite fabricated via MG3C. It is Holloman parameter [62], if secondary particles are uni-
clear that the metal matrix surrounded the SiC particles, and formly distributed with no agglomeration, the grain size will
the matrix mostly bonded to the particles throughout their decrease drastically due to the pinning effect of the particles.
whole surface. Additionally, the interface is continuous Therefore, increasing rotational speed leads to a trade-off
without any specific pores or defects. By evaluating the EDS between the pinning effect and grain growth. As a result, the
map analysis taken from the SEM image (Fig. 10def), it can be effect of rotational speed on grain size is almost insignificant
deduced that there is no sign of undesirable components or [73]. Fig. 11 shows the effect of traverse speed on the grain size
reaction products at the interface. This analysis suggests that of FSPed Cu and CueSiC samples. As can be seen, the average
a tough interface with high bonding strength can be achieved grain size in the samples with a lower rotational speed is
using FSP [72]. slightly smaller compared to the sample with a higher

Fig. 10 e TEM (a) and HR-TEM (b) micrographs of Cu/SiC interface in powder metallurgy obtained composite sintered at
950  C for 3h (reproduced from Ref. [148]), SEM image and EDS map analysis for the elements Cu, Si and C of Cu/SiC surface
composite fabricated through MG3C (cef) (reproduced from Ref. [72]).
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passes, the time of the stirring action is longer, leading to a


uniform distribution of SiC particles. In contrast, in one pass
of FSP, partial agglomeration of SiC can be observed due to
insufficient stirring action.
As shown in Fig. 13b, e, SiC particles become smaller due to
the multi-pass FSP process. This phenomenon occurs due to
the constant disruption of SiC particles during each pass.
Therefore, grain size drastically decreased in multiple-pass
FSP due to finer SiC particles, higher levels of dispersion,
and an enhanced pinning effect. In the first pass of FSP, high-
strain regions with dislocation walls and sub-grains are
formed. In the second pass, nucleation sites for dynamic
recrystallization are increased due to total high strain and
high strain rate [5]. Barmouz et al. investigated the effect of
the number of passes on the grain size of FSPed CueSiC and
the fabrication of ultra-fine grain (UFG) materials using
multiple-pass FSP [25]. Fig. 13c, f shows the UFG microstruc-
Fig. 11 e Variation of FSPed Cu and CueSiC grain size as a ture fabricated by eight passes of FSP compared to the
function of traverse and rotational speeds [73]. microstructure of the same composite fabricated using one
pass of FSP. The same findings have been reported for
aluminum based MMCs fabricated by FSP [152,153].
Apart from the aforementioned factors, the pin profile
rotational speed. In Cu samples without SiC particles, the significantly influences obtaining finer grains, as thoroughly
primary mechanism for microstructure evolution is heat investigated by Barmouz et al. [113]. According to their find-
generation during the FSP process; therefore, grain growth is ings, SiC particles in SZ were uniformly dispersed due to the
limited at higher traverse speeds, leading to finer grains. straight cylindrical (SC) pin profile. This might be due to the
High rotational speed along with low traverse speed leads unique and uneven geometry of square pins (SQ); SiC particles
to excessive heat input and softening in the stirring zone, are dispersed heterogeneously owing to the tool pin's sharp
resulting in vigorous stirring with the tool pin and the for- corners [154]. In other words, the SC pin profile causes the
mation of the “onion ring” structure in the stirring zone materials around the pin to flow smoothly, which leads to the
(Fig. 12a) [6,72,75]. dispersion of previously segregated SiC particles. The
In CueSiC samples, the primary mechanism for micro- following two factors may illustrate this phenomenon: First,
structure evolution is the pinning effect of the SiC particles. At the smooth pin geometry of the SC tool pin profile at the stir
lower traverse speeds, the SiC particles are dispersed uni- zone results in lower heat generation, which, in turn, slows
formly due to sufficient stirring action in the stirring zone grain growth and results in lower grain growth. Second, su-
(Fig. 12b). The formation of agglomerated SiC particles at perior SiC separation promotes the nucleation of these parti-
higher traverse speeds can be seen in Fig. 12c. The uniform cles, leading to a higher pinning effect, which finally causes a
distribution of the second phase leads to a finer grain size decrease in grain size in the SZ [113].
according to Zenner-Holloman's parameter. As a result, in
FSPed CueSiC samples, increased traversal speed results in 4.2. Influence of SiC content and size
larger grains [62,79,116].
The quantity of FSP passes highly affects the microstruc- The SiC particle volume percentage significantly affects the
ture, mechanical properties, and wear behavior of FSPed grain size of the composite layer [9,62,155]. According to the
composites [113,134,151]. Fig. 13a, d shows the microstructure Zener limiting grain size [10,81] given as dz ¼ 4r/3Vf, where r
of the CueSiC composite with 1 and 8 passes of FSP. In eight and Vf are the corresponding radius and volume fractions of

Fig. 12 e Optical micrographs of FSPed CueSiC composites with different process parameters: (a) 1000 rpm-20 mm/min-1
(reproduced from Ref. [6]), (b) 900 rpm-40 mm/min-2 (reproduced from Ref. [79]), (c) 900 rpm-200 mm/min-2 (reproduced
from Ref. [79]).
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Fig. 13 e Optical micrographs of FSPed CueSiC composites after: (a, b) 1 pass, (d, e) 8 pass of FSP, and FESEM micrographs of
FSPed CueSiC composites after: (c) 1 pass and (f) 8 pass of FSP (reproduced from Ref. [25]).

the second phase particles, when the particle size drops and Further, it is important to note that SiC particles generate
the volume percentage of them grows, the sample grain size locally inhomogeneous deformation that aids in the breakup
reduces [62,74]. Fig. 14a, c demonstrate the effect of SiC par- of the grains [119,127]. Therefore, it might be argued that
ticle volume percentage on the final grain size of the CueSiC reducing the size of SiC particles enhances the nucleation
composite [62]. The specimens with grain sizes of 6.3, 4.2, sites, intensifies the pinning action of particles, and promotes
and 2 mm had volume percentages of 6, 12, and 18%, respec- the breaking up of pre-existing grains [6,62,79]. As an illus-
tively. The grain size was significantly reduced by increasing trative example, SEM images of the FSPed pure Cu and Cu with
the volume percent of reinforcing particles. Because more 5 mm and 30 nm SiC particles in a 12 vol % are displayed in
nucleation sites are available during recrystallization, a Fig. 15a, c. Accordingly, the grain size of the FSPed specimen
greater pinning effect exists at higher particle volume per- was reduced from 10 mm (specimen without SiC) to 5 mm and
centages since more particles are present [62,79]. In other 1.7 mm, respectively. The porosities formed between the Cu
words, by increasing the SiC content, the grain size is drasti- matrix and SiC particles are demonstrated in Fig. 15d [79]. It is
cally reduced due to Ref. [79]. evident that the FSPed samples with SiC particles had an in-
crease in porosity content. The nanoscale SiC particle
1. Creation of more nucleation sites dispersion in the Cu matrix is seen in Fig. 15e. It is obvious that
2. The pinning effect is intensified the SiC additives are well distributed throughout the copper
3. More pre-existing grains are broken up matrix.

Fig. 14 e Optical microstructure of FSPed CueSiC composites containing: (a) 6%, (b) 12%, and (c) 18% volume fraction of SiC
particles (reproduced from Ref. [62]).
1330 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

Fig. 15 e SEM micrograph of FSPed (a) pure Cu, (b) Cu with 12% volume fraction micro-sized SiC particles, (c) Cu with 12%
volume fraction nano-sized SiC particles, (d) CueSiC interfacial bonding and porosities, and (e) high magnification of c
(reproduced from Ref. [9]).

5. Mechanical behavior of FSPed CueSiC 0:5


DsHP ¼ Kd (3)
composites
where DsHP is the increase in yield strength by Hall-Petch, d is
The improvement of copper's mechanical properties is one of the average grain size, and K is a material constant. Hall-Petch
the primary goals followed in developing the CueSiC com- strengthening is highly dependent on the size of the grains
posites. According to studies, SiC can significantly improve within a material. This grain size is influenced by the presence
the hardness, yield stress, and tensile strength of copper when of particle reinforcements, which can act as pinning points,
compared to pure copper. In applications such as mechanical impeding or even preventing the growth of the grains
relays that require high strength and hardness with good [162e164]. To calculate grain size in the Hall-Petch relation,
electrical conductivity, CueSiC composite is one of the best the Zener model [165] provides a theoretical framework for
candidates. Therefore, in this section, strengthening mecha- estimating the average grain size:
nisms of CueSiC MMCs, and the influence of different process
parameters and SiC features on the mechanical properties of 4adp
d¼ (4)
Cu are discussed. 3vP
where a is a proportional constant, dp is the particle diameter,
5.1. Strengthening mechanisms in CueSiC composites and vp is the volume fraction of reinforcement particles. It
should be noted that the strengthening mechanism of Hall
Extensive reviews have been conducted on the strengthening Patch has a greater contribution to the strengthening of the
mechanisms employed to enhance the mechanical properties MMCs in the SPD techniques due to grain refinement during
of MMCs reinforced with particles. The improved mechanical these processes [166].
performance of particle-reinforced MMCs can be attributed to Severe plastic deformation techniques, such as FSP, offer
several strengthening mechanisms, including: (1) Load excellent methods for achieving uniform reinforcement dis-
transfer effect, (2) Orowan strengthening [156], and (3) Hall- tribution and significant grain refinement [167,168]. By sub-
Petch strengthening [157]. Hall-Petch strengthening, also jecting the material to high plastic strain through external
referred to as grain refinement, is a phenomenon in which the deformation, this technique facilitates dynamic recovery and
strength of metals is influenced by the size of their grains recrystallization of the matrix, as well as fragmentation and
[158]. The presence of grain boundaries plays a crucial role in dispersion of nanoparticles [169,170]. Consequently, the ma-
impeding the migration of dislocations [156,159,160]. This ef- trix of the composites exhibits outstanding mechanical per-
fect arises due to the diverse orientations of grains within the formance [171].
metal and the significant lattice disorder, which hinders the The influence of deformation-driven metallurgy (DDM) on
movement of dislocations along a slip plane [161]. The Hall- grain refinement was explored by Xie et al. [172] in graphene
Petch equation, as expressed in Ref. [161], can be stated as nanoplatelets (GNPs)-reinforced aluminum matrix compos-
follows: ites. DDM is a novel severe plastic deformation technique.
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Fig. 16 e Schematic illustration of grain refinement mechanism (reproduced from Ref. [172]).

DDM, along with the accompanying frictional and deforma- SiC can weaken load transfer strengthening, thereby dimin-
tion heat generated, plays a significant role in modifying the ishing the overall strengthening efficiency of SiC. Moreover,
microstructure. They found these GNPs play a crucial role in FSP plays a crucial role in the rapid multiplication of
impeding dislocation movement, leading to localized dislo- geometrically necessary dislocations and the simultaneous
cation aggregation and accelerated dynamic recrystallization nucleation of recrystallized grains. Fig. 16 shows a schematic
during the nucleation stage. Moreover, they introduce a illustration of the grain refinement mechanism. As illustrated,
pinning force that counteracts curvature and dislocation SPD techniques including FSP promote particle fragmentation
driving forces, effectively restraining the growth of recrystal- and dislocation pile-up. The presence of SiC hinders disloca-
lized grains. GNPs are evenly distributed between and within tion movement, resulting in the accumulation of dislocations
the grains. When located at the grain boundaries, these re- in localized regions and the expedited process of dynamic
inforcements demonstrate a noticeable pinning effect on the recrystallization. Furthermore, during the subsequent growth
movement of the grain boundary, effectively impeding its of recrystallized grains, the presence of SiC particles in close
migration. Additionally, they exert an inhibitory effect on the proximity to grain boundaries leads to the phenomenon of
rearrangement of dislocations, further enhancing their Zener pinning, which restricts the motion of the grain
strengthening capabilities [173]. This process ultimately yields boundary. The pinning force exerted by these SiC particles is
grain refinement and nanocrystalline microstructure, which inversely proportional to their average size. The pinning force
improve mechanical properties. It should be noted that the swiftly counterbalances the curvature and dislocation driving
homogenous distribution and fragmentation of the GNPs in- forces, effectively impeding the growth of recrystallized
crease this mechanism. But the excessive fragmentation of grains and ultimately achieving a nano-sized microstructure.
GNPs negatively impacts both the Orowan strengthening
mechanism and the load transfer effect [172]. 5.2. Hardness
Based on the aforementioned discussions and previous
research on grain refinement, a similar outcome can be CueSiC composites were successfully manufactured on the
anticipated for CueSiC composite processed through FSP surface of pure copper using FSP as a low-energy method
[174e178]. As mentioned earlier, friction stir processing has a under various heat input conditions [6,62,75,114]. Generally,
significant impact on the dispersion of SiC particles. This two categories of parameters affect the hardness of FSPed
process leads to the generation of a larger number of active composites: process parameters and material properties.
sites on the SiC particles, facilitating stronger chemical
bonding between SiC and the copper matrix. As a result, the 5.2.1. Effect of process parameters
inhibitory effect of SiC on dislocation rearrangement and Hardness measurement is a critical test to measure the
grain boundary migration in the matrix is strengthened dur- effectiveness of the selection process parameters like FSP
ing recrystallization and growth. As the number of FSP passes passes, tool tilt angle, tool rotation speed, traverse speeds of
rises, there is an observed increase in the fragmentation of SiC the tool pin, tool pin profile, and type of groove technique.
particles. This results in a progressive reduction in the average The number of passes of FSP is among the most critical
size of SiC particles and enhances the inhibitory effect of SiC process parameters. As shown in Fig. 17, increasing the
on grain boundary migration during recrystallization. How- number of passes reduces the size of the SiC additives,
ever, it is crucial to consider that excessive fragmentation of resulting in better dispersion, a noticeable suppression of GBS,
1332 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

Fig. 17 e Hardness profiles of samples FSPed at different conditions such as CueSiC with 6% and 18 vol % micro or nano SiC,
FSPed CueSiC with 1, 4 and 8 pass, FSPed CueSiC with 1, 2 and 3 grooves, SC and SQ tool pin profile and traverse speed of
40, 80 and 200 mm/min.

and a sharp reduction in grain size, leading to higher values of presence of SiC particles. Since the pure copper sheets were
hardness. Moreover, in the high FSP passes, the hardness of previously rolled, they possessed a high density of disloca-
the SZ region is more uniform as a result of well-distributed tions. The FSP process reduces residual stress and dislocation
SiC additives [24,25,74,79]. Another impactful parameter is density in the SZ compared to the BM [9,79]. Because the SiC
the tool rotation speed. Increasing the tool rotation speed particles were successfully dispersed at low traversal speeds,
prevents the accumulation of SiC particles and improves the SZ encountered a strong pinning effect, causing microhard-
distribution of the additives, consequently increasing the ness to increase. However, by increasing the traverse speed,
hardness of the composite [75]. But in some cases, the the SiC particle agglomeration increases; hence, the pinning
microhardness of surface composites decreased with effect of SiC particles declines, leading to a minor increase in
increasing tool rotation speed due to the crushing of SiC par- hardness compared to pure copper [62,73e75,79].
ticles and the increased possibility of agglomeration at very Another important tool parameter is the tool pin profile.
high tool rotation speeds [115]. Investigations have indicated that the straight cylindrical
Furthermore, by increasing the tool tilt angle from zero to profile compared to the square profile improves the surface
two degrees, due to the effect of the frictional forces and heat quality, unifies the dispersion of the SiC particles, and lowers
generation, which improve the compaction and prevent the the heat input because of the smooth geometry, resulting in
accumulation of SiC particles, and improve the distribution of finer grains. All the aforementioned reasons increase the
the particles in the stir zone, the hardness of the composite hardness in the SZ region (Fig. 17) [114].
increases [6,75]. Using a set of blind holes has been introduced as a suc-
In the case of unreinforced copper samples, at low traverse cessful method for fabricating CueSiC composites by the FSP
speeds, the annealing effect is dominant, and despite the process, where uniform dispersion of SiC particles on the
grain size reduction, the hardness is lower than the hardness stirring zone has been achieved [6,75]. The MGT, in compari-
of pure copper [24,73]. However, at high traverse speeds, DRX son with the SGT, showed a more homogeneous SiC particle
prevails over the annealing effect produced as a consequence distribution in the copper matrix. In addition, the hardness of
of lower heat input, higher thermomechanical stress, and a composites made by MGT is higher compared to SGT, which
higher density of dislocations, leading to an increase in increases with the number of grooves. This is because the
microhardness [179]. However, when compared to pure cop- dispersion of SiC particles is more uniform, and as a result, the
per, the CueSiC composite demonstrated increased hardness, pinning effect is more intense (Fig. 17). Also, MGT introduces
which was attributed to the pinning effect caused by the more plastic deformation compared to SGT, generating
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additional dislocations, resulting in increased composite flow. Contrarily, the AS material has a greater temporal rota-
hardness. The hardness improvement was maximized in the tion, a maelstrom-like current flow, and a better distribution
case of the composite developed by three grooves [72]. Ac- of SiC particles [182]. According to Fig. 17, in the constant
cording to the investigations, the optimal parameters of the volume fraction of SiC, the average hardness of micro-sized
FSP process for the CueSiC composite were determined by the SiC composites is lower than that of nano-sized ones. Also,
rotation speed of 500 rpm, the traverse speeds of 50 mm/min, it has been reported that the hardness increases with an
and the tool tilt angle of one degree [6,75]. increment in the SiC volume fraction [181].
As mentioned, the main strengthening mechanisms in the
5.2.2. Effect of FSP zones and SiC parameters FSP process of CueSiC composites are Orowan strengthening,
There are two methods to measure the hardness of the FSPed Hall-Petch strengthening, and the strengthening effect
sample: one is to measure the hardness profile on the surface, resulting from the coefficient of thermal expansion (CTE)
and the other is to measure the cross-sections of the friction differences between the matrix and particles. The most sig-
stir processed zone. The measurements showed a significant nificant contributors to strength among the aforementioned
increase in the hardness of the material subjected to a factors are Orowan strengthening because of the hard SiC
friction-modified zone compared to the hardness of the base particles in the copper matrix and Hall-Petch strengthening
metal, explained by the presence of hard SiC particles and because of the grain refinement dominance in the stirring
grain refinement. In addition, there were variations in the zone. In CueSiC composites, with the increase in the volume
hardness distribution within the stirring zone. In the center of fraction of the SiC additives, the contribution of CTE and
the SZ, the hardness is at its maximum. But the hardness in Orowan reinforcement to strength increases [75].
the narrow subsurface region is slightly lower due to the lower
amount of SiC phase distributed within this zone. But the in- 5.3. Tensile properties
crease in hardness compared to the hardness of the base
metal is due to grain refinement. After the maximum hard- Tensile features of composites include yield strength (YS),
ness of the SZ center, the hardness decreases in the lower part ultimate tensile stress (UTS), and elongation (EL). Elongation,
of the SZ region [26]. Due to grain growth brought on by YS, and UTS of different manufacturing conditions of CueSiC
annealing, the hardness values in the stirring zone's side areas composites are shown in Fig. 18a. In FSPed Cu samples, YS and
have decreased. The stirring motion of the pin causes DRX UTS fell compared to pure copper. Also, in these samples,
that decreases the grain size, increases the dislocations, and elongation increased compared to pure copper. This phe-
ultimately increases hardness. However, the heat input leads nomenon may be due to the annealing and release of residual
to annealing, which reduces the hardness. SZ shows higher compressive stresses in copper during the FSP process. How-
hardness because of the uniform distribution of hard SiC ever, samples reinforced with SiC additives have decreased
particles in the pure copper matrix and the grain size reduc- UTS, YS, and elongation compared to pure copper. Hard SiC
tion caused by grain refinement in SZ. Also, because the SiC particles reduce GBS, plastic deformation, and bonding be-
particles experience different thermal contraction than the tween copper matrix and SiC particles, which reduces elon-
pure copper matrix, quench hardening occurs, increasing the gation. Also, the dimples formed in the composite caused by
hardness of the SZ. Another reason for the increased hardness SiC particles reduce elongation, YS, and UTS [9,25,73]. In
of the SZ region in comparison with the pure copper base another study, unreinforced copper samples showed better
metal is the suppression of GBS caused by the presence of SiC tensile properties in comparison with the as-received copper.
particles [24,25,74,79]. Similar results have also been found in As a result of the grain refinement of FSPed copper, more grain
the FSP-processed Al matrix reinforced with SiC particles boundaries are produced that prevent dislocations from
[74,180]. But in another study, due to the occurrence of DRX in moving during plastic deformation, thereby increasing
the SZ, the microstructure transforms into an equiaxed and strength. In addition, the elongation of FSPed unreinforced
fine structure, improving the hardness of pure copper based copper was improved as well compared to as-received copper.
on the Hall-Petch equation [72]. The Hall-Petch formula states The observed phenomenon of increased elongation can be
that decreasing the SiC particle size decreases the grain size, attributed to the formation of fine grains. Also, the higher
increasing the hardness. Also, hardness increases with proportion of grain boundaries delays crack propagation and
increasing SiC content due to grain size reduction [9,62]. leads to higher elongation [9]. Based on the findings presented
On the surface area, due to the absence of a TMAZ, the in Fig. 18a, it can be observed that the implementation of
grains on the sides of SZ were coarser compared to the SZ multi-pass friction stir processing leads to an improvement in
area, so a significant reduction in hardness can be expected in the tensile properties of CueSiC composites. This improve-
these areas. Still, in the cross-section of the composite, the ment can be attributed to several factors, including a decrease
slope of the reduction in hardness is slight due to the presence in porosity, enhanced bonding between the Cu matrix and SiC
of the TMAZ area [4,6,9,62,79,181]. The next region is called particles, and a more uniform distribution of SiC particles.
HAZ, and due to the absence of SiC particles and plastic Additionally, the multi-pass approach helps to mitigate the
deformation in this region, the grains become significantly agglomeration of SiC particles and promotes grain refinement.
coarser during FSP due to annealing. Therefore, the BM The higher porosity content of the CueSiC composites made
hardness is higher than HAZ [6,29]. Also, there is a slight dif- via multi-pass FSP is bound to decrease UTS compared to pure
ference between the hardness of RS and AS. The hardness of copper [25]. In composites with nano- and micro-sized SiC
RS is lower than that of AS. This phenomenon is attributed to particles, increasing the SiC volume fraction lowers the
the RS material's reduced spinning time and direct current elongation and increases the tensile strength (Fig. 18a). The
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Fig. 18 e (a) Strength and elongation of pure Cu, FSPed Cu, FSPed CueSiC with 6% and 18 %vol micro or nano SiC, FSPed
CueSiC with 1, 4 and 8 pass, FSPed CueSiC with 1, 2 and 3 grooves and (b) average hardness and strength of SPS þ HPT, SPS,
Conventional sintering and 8 pass FSPed CueSiC composite with 20 %vol SiC.

FSPed samples with nano-sized SiC particles had a somewhat crack formation between the SiC particles and Cu grains. Still,
higher tensile strength compared to the samples reinforced the higher strength of samples manufactured by MGT may be
with micro-sized SiC particles due to the smaller grain size. In due to the increased grain refinement, which delays the prop-
general, FSPed samples with SiC particles have higher tensile agation of cracks at larger grain boundaries [5,72,116,151].
and yield strengths than unreinforced copper [9]. Fig. 18b presents a comparison of the microhardness and
As can be seen in Fig. 18a, the strength of the composites strength of CueSiC composites produced by various proced-
fabricated using MGT is higher than that of SGT. Also, the ures, compared to those achieved through FSP process. As can
elongation for both cases shows a significant decrease, result- be seen, although grain refinement occurs in the FSP process,
ing from the SiC particles' presence in the copper matrix, due to the presence of different annealing areas and the uni-
limiting the movement of dislocations during plastic deforma- formity of the structure, the FSPed composite shows low
tion. The reduction in strength stems from the possibility of hardness but it possesses sufficient strength [183].
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5.4. Fracture behavior


6. Tribological behavior of FSPed CueSiC
One of the factors used to determine the initial quality of composites
materials is the way they fracture, along with other factors
like homogeneity and purity, susceptibility to cracking, and Many industrial applications involve the interaction of tool
mechanical properties [184]. Fig. 19 demonstrates the SEM and machine components. Tribological properties are essen-
micrographs of fractured surfaces of FSP-processed samples tial in determining these components' qualities, useable life,
under different routes and with various amounts of SiC and durability. The mechanical and tribological properties of
additives. most metals and alloys are poor under such severe conditions
As can be seen in Fig. 19aed, as-received Cu and FSPed Cu [185e187]. Therefore, novel metal-based materials with
without SiC particles show voids and dimples, which are signs improved properties have been developed to overcome these
of ductile fracture. However, the SEM micrograph taken from challenges, such as composites with hard ceramic particles
the fracture surface of FSPed CueSiC composites indicates developed by friction stir processing [28,188]. In the tribology
small dimples, brittle fracture, and pulling out of the SiC process, parameters including mass loss, wear rate, and co-
particles due to weak interfacial bonding between SiC parti- efficient of friction (COF) are crucial, and by following them,
cles and Cu grains. wear properties can be improved noticeably.
Although the FSPed copper acquires higher ductility
6.1. Wear resistance
compared to the as-received one, the dimples are relatively
deeper in these samples [9,25,72,73]. Since the density of dis-
Researchers have shown that under tribological conditions,
locations is high in the thermo-mechanically affected zone
pure Cu has more weight loss than FSPed CueSiC composites
(TAMZ) due to plastic deformation, they are susceptible to
[4,72,74]. The general reason for this phenomenon is that hard
crack nucleation. Consequently, in the FSPed pure copper,
SiC ceramic particles enhance the microhardness of com-
fracture occurs in the TMAZ zone. But in the FSPed composite
posites. According to the findings by H. R. Akramifard et al. [4],
reinforced with SiC particles, the fracture occurs at the SZ due
the hardness of Cu matrix composites is noticeably enhanced
to the crack starting from the interface between the copper
by increasing the amount of SiC additives, and following
grains and SiC particles [9].
them, the wear rate decreases. Secondly, copper and SiC
Compared to pure copper, the broken surface of 1P features
particles are properly bonded; thus, the bond quality between
a flat zone demonstrating brittle fracture (Fig. 19e). In addi-
the particles and the matrix is essential for wear resistance
tion, the 4 P and 8 P fracture surfaces show voids and dimples
[73,189]. Also, it was demonstrated that SiC nanoparticles
on the surface, which are characteristic of ductile fracture
create a stronger bond with the copper matrix than SiC mi-
(Fig. 19f and g). It is noteworthy that due to the smaller grain
croparticles and positively affect the wear rate [9]. Another
size in these samples, the voids and dimples located on these
reason is the Orowan strengthening mechanism. This
composites' fractured surfaces are smaller than pure copper
strengthening mechanism, due to the fine dispersion of SiC
[25]. In the FSPed composite containing micro-sized SiC par-
particles during friction stir processing, has a critical role in
ticles, the fracture mechanism includes the ductile stretching
the enhancement of wear resistance [4,74,75]. Furthermore,
of the copper matrix, and SiC particles are separating from the
the considerable variation in the CTE of copper matrix and SiC
copper matrix (Fig. 19h). In fact, the weak bonding of the Cu/
additives is crucial in regulating wear rate via composite
SiC interfaces and low mobility of dislocations due to the
strain hardening [72,75]. Apart from the aforementioned rea-
presence of SiC particles are compelling reasons for the low
sons, the majority of reports attribute this to less direct load
plastic deformation of the micro-sized SiC composite that
contact between the worn tool and the Cu/SiC composite than
reduces the elongation [9].
with pure Cu. Due to the load transfer from the Cu matrix
The FSPed composites with nano-sized SiC particles show
grains to the SiC additives and the load-bearing component
a smaller grain size due to the smaller SiC particles (Fig. 19i).
action of them, the direct load is decreased [4,72,74,75,79,190].
Therefore, cracks need more stress for nucleation and growth.
These reasons make FSPed CueSiC composites more resistant
Nano-sized SiC particle dispersion strongly limits the dislo-
to wear than pure copper, which corresponds to the findings
cations' mobility and significantly reduces elongation, there-
of others [9,25,73,189].
fore, the elongation of FSPed composite with nano-sized SiC
One of the key variables affecting the wear rate of FSPed
particles is less than that of FSPed composite with micro-sized
CueSiC composites is the manufacturing parameters. Friction
SiC particles [9]. As shown in Fig. 19j-o, CueSiC composites
stir processing produces a homogeneous dispersion of SiC
fabricated using MGT are more ductile than those made by
particles and a fine grain structure [9,72,189]. When traversing
SGT, and cracks have been formed due to the creation of SiC
speed increases, the hardness enhances owing to decreasing
agglomerates. But with the increase in the number of passes,
the mean grain size [191]. However, as traverse speed in-
the possibility of crack formation between the Cu matrix and
creases excessively, SiC dispersion weakens and agglomer-
SiC particles decreases due to the finer grains and improves
ates, and the hardness decreases [73,79,192]. As mentioned in
the formability [72].
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Fig. 19 e SEM micrographs of fractured surfaces of: (a) as-received Cu, (b) FSP-processed Cu, (c) FSP-processed Cu with SiC
particles, (d) high magnification of (c) (reproduced from Ref. [73]), (e) 1-pass FSPed CueSiC composite, (f) 4-pass FSPed CueSiC
composite, (g) 8-pass FSP-processed CueSiC composite (reproduced from Ref. [25]), (h) FSP-processed Cu with 18% micro-
sized SiC particles, (i) FSP-processed Cu with 18% nano-sized SiC particles (reproduced from Ref. [9]), FSPed CueSiC
composite via SGC technique (j, k), MG2C technique (l, m) and MG3C technique (n, o) (reproduced from Ref. [72]).
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the previous sections, the pin profile affects the FSPed com- Contrarily, FSPed CueSiC composites had smaller fluctua-
posites' various properties [193e196]. Kumar et al. [197] tions as a result of a decrease in the actual contact area be-
investigated the effect of tool pin eccentricity on the proper- tween the composite surface and disk brought on by the
ties of FSPed-copper. They demonstrated that using pin ec- inclusion of SiC particles, which weakened the cohesive con-
centricity during the processing of copper improves grain tact behavior [9,205]. The presence of SiC particles leads to the
refinement and material flow, leading to increased hardness vast early peaks in MMCs generated by enhanced friction force
compared to processing without pin eccentricity. It was also to maintain extremely adhesive contact between the com-
noted that implementing a pin with high eccentricity could posite and counterpart. Later, considerable variations are
lead to overheating, which coarsens the grains and decreases minimized and become almost steady until the end [72,75,79].
the hardness. Square (SQ) pin profiles cause a decrease in Similar results have been found and reported in FSP-
grain size, uniform distribution of SiC in the stirring zone, and processed AleAl2O3 and AleSiC composites, in contrast to
increased hardness and wear resistance of CueSiC FSPed pure aluminum [206]. On the other hand, the SiC particle size
composites. By contrast, a straight cylindrical (SC) pin profile influences the average COF of the composite, so that the COF
leads to slight SiC particle agglomeration [114,198]. Enhancing of the composite with SiC microparticles is lower than the
SiC particle dispersion in the Cu matrix could enhance wear same composite with SiC nanoparticles. The surface of the
resistance. To achieve that, novel techniques such as multi- composites is better covered by nano-size SiC particles, which
pass FSP [24,25,113] and MGT [72] have been suggested and are more numerous than micro-size SiC particles [9].
successfully conducted, illustrating a greater reduction in As previously noted, process factors impact tribological
wear loss or wear rate compared to base metal. More FSP properties. One feature that depends on the process parame-
passes lead to a greater dispersion of SiC and a more uniform ters is the COF. Pin profile is one parameter that is effective for
microhardness distribution. Therefore, it can reduce the average COF. The SC pin profile caused a higher average COF
applied load due to the load distribution between the SiC than the SQ one. When using the SC pin profile during FSP,
particles and reduce the wear rate. Significant enhancement better SiC particle distribution and a massive proportion of
in hardness and consequently wear resistance have also been them acting as obstacles lead to higher resistance of the sur-
observed in some research conducted on the multi-pass FSPed face against the sliding [73]. In a study by M. Barmouz et al.
multi-pass FSP Al-based composites [199e202]. Additionally, [25], the effect of the multi-pass FSP on the average COF of
using many grooves in the FSP reduces the wear rate and copper and SiC-reinforced copper has been investigated
improves wear resistance considerably. In the FSPed matrix (Fig. 20aed). According to their findings, large fluctuations
stir zone, a single groove sample with less reinforcement were diminished for 1P, 4P, and 8P FSP compared to pure
nanoparticle addition exhibited a slight improvement in copper. Thus, the frequency trend becomes more uniform.
hardness because of sufficient grain refinement. Since Indeed, SiC particles reduced the actual contact area, reducing
increased volume fraction of reinforcement and grooves cre- adhesion's effect and COF fluctuation. The dispersion of SiC
ates a consistent dispersion of reinforcement nanoparticles in particles increases as the number of passes rises, further
the FSPed stir zone of the nano-surface composites, the multi- reducing fluctuations due to the greater spreading of the
grooves with higher reinforcement addition indicate better applied load. After then, during more passes, the average
hardness and lowest wear rates [78,203]. At all sliding velocity friction coefficient will decrease [25,207].
conditions, the multi-groove samples showed a decreased Similar outcomes were obtained using a multi-groove
rate of wear, which is attributable to the homogeneous reinforcement technique on CueSiC. Because of the superior
dispersion of SiC nanoparticles in the stir zone, resulting in distribution of SiC particles and a large fraction of them
strengthening mechanisms in the FSPed surface composites. functioning as barriers, resistance to sliding on the surface
Furthermore, the reduction in direct load contact between the increased, leading to fewer fluctuations than with pure copper
hardened disc and matrix was greatly improved by the SiC [72]. The multi-groove technique can decrease the coefficient
nanoparticles. Because of the interfacial bonding and dislo- of friction. Compared to other FSPed samples, Cu reinforced
cation of grain movement, it also increases the capacity of with SiC nanoparticles FSPed by triple grooves indicated a
load-bearing [72,78]. high COF rate, which reduced wear rate compared to the
groove-less, single, and double groove samples at different
6.2. Coefficient of friction (COF) sliding speeds. By interfering with the disruptive movement
and creating a hardening effect with homogenous spreading
The coefficient of friction is one of the parameters for [203], the SiC nanoparticles increased the hardness in the
detecting tribological behavior and wear mechanisms. Many FSPed stir zone [72,78].
investigations showed that FSP-processed CueSiC composites One of the most important criteria in assessing the tribo-
have a higher average COF than pure copper. This result may logical behavior of materials, especially the predominant wear
be due to the presence of SiC reinforcements and their mechanism, is to study the worn surface. As shown in Fig. 21a,
obstacle role in the composite, resulting in higher resistance the worn surface of pure copper notably differs from com-
against surface sliding [4,9,73,75,79]. A closer examination of posite surfaces. It may be accounted for by the fact that the
the friction coefficient diagram corresponding to pure copper low hardness of pure copper causes plastic deformation and
shows significant fluctuations attributed to the severe cohe- significant material removal at its surface, as well as the for-
sive contact between pure copper and its counterpart, severe mation of a smeared layer that creates the tribo-film layer and
material removal action (because particles are absent), high non-uniform wearing; which demonstrates the cohesive wear
direct load, and cohesive wear mechanism [4,9,73,75,204]. mechanism. For FSPed Cu, Fig. 21b shows extensively
1338 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9

Fig. 20 e Coefficient of friction as a function of sliding distance for (a) pure Cu and (bed) 1P, 4P, and 8P, respectively
(reproduced from Ref. [25]).

scratched grooves parallel to each other in the sliding direc- film layer is eliminated from the worn surface of composites
tion, where the sliding wear is dominated by adhesion at the created by multi-pass FSP (single pass and four passes)
wear scar [72,181]. Although both adhesive and abrasive wear (Fig. 21e and f). The worn surface of a CueSiC composite made
mechanisms are seen for pure copper, adhesive wear mech- using a multi-pass FSP process, including segregated particles,
anisms predominate more; since Cu is a ductile and deform- is shown in Fig. 21f. This worn surface may be utilized as ev-
able metal. Despite this, hard SiC particles in FSPed CueSiC idence to validate the abrasive wear mechanism concept for
composites reduce ductility and induce plastic deformation. these composites. The homogeneous dispersion of SiC parti-
As a result, where abrasive wear is the predominant wear cles may explain why worn surfaces of composites made
mechanism, adhesive wear is reduced [72,208]. using multi-pass FSP have a more homogenous morphology
M. Barmouz et al. [9] and S. Cartigueyen et al. [181] have compared to those made with 1P [25].
reported that the FSPed samples containing micro- and nano- Larger craters and delamination are always apparent on
sized SiC particles contain hard SiC particles on their worn the worn surface of pure Cu, which promotes material
surfaces, which may inhibit the generation of severe plastic removal in the form of chunks. Additionally, heat generated at
deformation and material loss (Fig. 21c and d). As shown, the copper-counterpart interface softened the Cu and opened
abrasive wear is the primary wear mechanism in these spec- the path for the hard asperities’ penetration, which aided in
imens because there are no identifiable indications of a the promotion of material removal. However, the worn-out
smeared layer. On these surfaces, homogeneous wear surface appears flat in CueSiC composites made using the
morphology is the result. The increased covering action of SGC and MGC strategies because the grooves and tiny craters
nanoscale SiC particles compared to microscale particles is a are narrow. Fig. 21gei shows the worn surface of CueSiC
notable phenomenon. The results of comparing the wear rate composites fabricated by SGC, MG2C, and MG3C, respec-
and friction coefficient of FSPed specimens with micro- and tively. The wear debris adhered to the surfaces is extremely
nano-sized particles and pure copper back up this assessment obvious. Cutting and asperity penetration were not allowed
of morphology. Additionally, the worn surfaces of the com- due to the high degree of composite hardness. SiC was uni-
posite layers clearly show loose debris fragments [9]. The formly distributed throughout the copper matrix, which
removal and oxidation of the copper matrix and the pulling limited local plastic deformation and hence declined material
out of SiC particles from the FSPed CueSiC composite layer removal [72,210]. L. Feroz Ali et al. [78] reported similar results
during sliding are responsible for the formation of the loose for FSPed WeAleMg composites with the multi-groove tech-
debris particles [209]. nique (MGT). They are shown to cause a change from adhe-
Due to the presence of SiC particles and the increase in sion to an abrasion mode for samples with triple grooves and
microhardness values as compared to pure copper, the tribo- more significant W nanoparticle reinforcement. Due to the
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Fig. 21 e Worn surfaces of a) pure Cu (reproduced from Ref. [9]), b) FSPed Cu, FSPed Cu composite with c) micro and d) nano
SiC particles (reproduced from Ref. [181]), FSPed CueSiC composite fabricated by e) 1 pass, f) 4 pass (reproduced from
Ref. [25]), g) SGC, h) MG2C, and i) MG3C techniques (reproduced from Ref. [72]).

plasticized nature of the material, this condition only causes and the electrical properties of pure copper was examined.
small scratches and no delaminations. The abrasion mode, They studied the electrical conductivity of pure copper with
which further restricts the pulling of the particles, resulted in three different ultra-fine-grained structures made by
extremely low asperities on the surface [211]. combining two distinct SPD techniques (Fig. 22). According to
their research, changing the material's grain structure had no
noticeable impact on electrical performance. Compared to
7. Electrical properties their coarse-grained (CG) equivalent, the electrical conduc-
tivity of ultrafine-grained copper samples does not dramati-
In determining the applications of copper and copper-based cally diminish. They discovered that the electrical
composites, the high electrical conductivity of copper is conductivity of the ECAP þ HPT samples was 91.6% of CG
crucial in many cases. The reinforcement characteristics and copper. This is because electron-phonon scattering, rather
content, as well as the processing route and parameters that than electron scattering on lattice defects, primarily contrib-
affect microstructural features, all play a role in Cu's electrical utes to decreased electrical conductivity at ambient
conductivity. Concerning Cu and Cu-based composites, just a temperature.
few studies have been conducted on the electrical properties' According to R. M. Leal et al. [213], FSP parameters affect
evolution during the FSP or other SPD techniques. In a study the microstructural and electrical properties of copper. Ac-
by Zhilyaev et al. [212], the correlation between grain structure cording to their findings, the electrical conductivity of copper
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Fig. 22 e Microstructure of Cu samples: (a) initial, (b) machining, (c) ECAP þ HPT, and (d) ECAP þ machining, and electrical
conductivity of Cu samples with different microstructures obtained by different severe plastic deformation techniques, and
electrical conductivity of the samples (reproduced from Ref. [212]).

undergoing FSP processing depends on the density of dislo- SiC is a wide band gap semiconductor, and the addition of
cations inside the grains. Processing at higher temperatures SiC to Cu leads to a decrease in the electrical conductivity of
and with high heat input conditions encourages the recovery Cu due to the lower electrical conductivity of SiC (Fig. 23c). It is
of the recrystallized structure, resulting in an electrical con- evident that the electrical conductivity drops as the SiC par-
ductivity that is even higher than that of the coarse-grained ticle content increases but improves with elevated sintering
and unprocessed Cu. Thus, improvement in the electrical temperatures. The electrical conductivity of metals is largely
conductivity of the processed material is achievable by influenced by electron mobility. However, the addition of SiC
increasing the u/v ratios (tool rotation (u) and traverse (v) particles distorted the structure and hindered electron
speeds). Fig. 23a and b demonstrates the effect of processing movement, resulting in reduced conductivity [215e218].
temperature and u/v ratio on the electrical conductivity of Few studies have evaluated the electrical properties of FSP-
unprocessed and FSP-processed samples. processed Cu reinforced by ceramic particles such as SiC. H.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9 1341

Fig. 23 e Effect of processing conditions (w/v) and temperature on the electrical conductivity of copper (C12200 alloy), 23 K (a)
and 293 K (b) (reproduced from Ref. [213]), effects of SiC content and sintering temperature on the electrical conductivities of
Cu/SiC composites (reproduced from Ref. [214]) (c), and electrical resistivity of pure copper and 1P, 4P and 8P FSP-processed
Cu/SiC composite (reproduced from Ref. [25]) (d).

Kumar et al. [219] studied FSPed zirconia-reinforced copper- However, there was only a slight variance in electrical con-
based surface composites. They demonstrated that the elec- ductivity observed in the composites produced with 1, 4, and
trical conductivity of the produced composite was negatively 8-pass FSP. This phenomenon indicates that the semi-
impacted by zirconia dispersed through the copper matrix, conducting behavior and weak interface of Cu/SiC are more
which decreased the electrical conductivity from 99.91% IACS critical than grain size refinement and defect increases in
for pure copper to 69.64% IACS for the Cu/ZrO2 composite scattering electrons in Cu/SiC composites. In conclusion, the
sample. In this case, electrons were scattered due to reduced electrical conductivity of reinforcement and its interfacial
grain boundaries, impurities in the zirconia, and its non- bonding with the matrix are crucial material parameters that
conductive nature. determine the conductivity of a composite. Additionally, the
M.Barmouz et al. [25] prepared Cu/SiC composites by an in- FSP procedure reduced the electrical conductivity of Cu and
situ reaction using multi-pass friction stir processing and reinforced Cu (SiC reinforced Cu in this study) due to scat-
studied the composite's electrical performance. In agreement tering electrons by structural defects such as dislocations and
with research on other Cu-based composites, adding SiC grain boundaries, which all become more prominent as the
particles to the copper matrix using FSP led to a decreased number of FSP passes increases. However, in the FSP process
electrical conductivity compared to pure copper (Fig. 23d). with increased u/v, higher heat input facilitates the recovery
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and recrystallization phenomena, causing only a slight Addressing these challenges is essential for expanding the
reduction in electrical conductivity. applications of these composites and further improving their
properties. Future research in this area is promising and has
the potential to lead to development of new and innovative
8. Conclusions materials with superior performance. This section discusses a
few of the most critical issues and future directions that could
In this study, the fabrication of CueSiC MMCs using the FSP encourage academic and industrial efforts to fabricate high-
technique and various factors that affect, accordingly, the performance CueSiC MMCs.
composite's microstructure, mechanical, tribological, and
electrical properties are reviewed. The conclusions are as 1. The reaction at the Cu/SiC interface has not been fully
follows: investigated with advanced methods. This is a critical
challenge, as the reaction can affect the mechanical and
1. The heat input during the FSP process of Cu/SiC is thermal properties of the composite. Future research
directly affected by process parameters such as the should focus on using advanced methods, such as trans-
rotation and traversing speed of the tool and the num- mission electron microscopy (TEM) and atom probe to-
ber of FSP passes. mography (APT), to study the reaction at the Cu/SiC
2. The microstructure of the FSPed Cu/SiC composites interface. This research will help to improve our under-
consists of refined grains with a uniform distribution of standing of the factors that affect the reaction and how to
fragmented secondary SiC particulates. control it.
3. An increase in the FSP pass number, traverse speed, 2. The effect of metallic coatings on SiC particles is not fully
blind holes, and volume fraction of SiC additives leads understood. This is another critical challenge, as the
to higher values of hardness, YS, and UTS. coating can affect the wettability of the SiC particles in the
4. Reduction in SiC particle size enhances the hardness, Cu matrix and the formation of brittle phases at the
YS, and UTS of the FSPed composites. interface. Future research should focus on investigating
5. Cylindrical pin profile significantly improves the hard- the effects of different metallic coatings on the properties
ness of the SZ region compared to the square pin profile. of FSP-derived CueSiC composites. This research will help
6. The tribological performance of FSPed CueSiC com- develop new methods to improve the performance of these
posites increased by rising SiC content and using many composites.
grooves in the FSP due to improved hardness and 3. The understanding of how SiC particles influence the
decreased wear rate. strengthening of the composite remains somewhat
7. Compared to the SC pin profiles, SQ pin profiles elusive. This is another critical challenge, as the strength-
improved the wear resistance of CueSiC FSPed com- ening mechanisms can affect the mechanical properties of
posites much better. It is because the SC pin profile the composite. Future research should focus on investi-
leads to slight SiC particle agglomeration. gating the strengthening mechanisms in FSP obtained
8. More FSP passes lead to a better dispersion of SiC par- CueSiC composites using advanced techniques.
ticles and a reduced wear rate. 4. Accurately determining the contributions of different
9. The wear resistance improves as traversal speed rises strengthening mechanisms is currently challenging. This
because the mean grain size is getting smaller, leading is due to the complex nature of the FSP process and the
to enhanced hardness. However, as traverse speed in- interactions between the different strengthening mecha-
creases excessively, SiC dispersion weakens. nisms. Future research should focus on developing new
10. The electrical conductivity of Cu is degraded by the methods to accurately determine the contributions of
addition of SiC, which has a low electrical conductivity different strengthening mechanisms.
and increases its content. The FSP process leads to a 5. The influence of manufacturing parameters on wear quali-
slight decrease in the electrical conductivity of Cu/SiC ties is not fully understood. This is a critical challenge, as the
composites due to scattering electrons by structural wear properties of the composite can be affected by the
effects such as dislocations and grain boundaries, processing parameters. Future research should focus on
which are enhanced with increasing FSP pass numbers. investigating the effects of different processing parameters,
In contrast, when FSP is performed with increased/v, such as tool rotational speed, feed rate, and traverse speed,
higher heat input facilitates the recovery and recrys- on the wear properties of FSP obtained CueSiC composites.
tallization phenomena, resulting in a slight reduction in This research will help develop new methods to improve the
electrical conductivity. wear resistance of these composites.
6. The wear mechanisms in CueSiC composites are not fully
understood. This is another critical challenge, as the wear
mechanisms can affect the wear rate and the wear debris
9. Current challenges and future perspective produced. Future research should focus on investigating the
wear mechanisms in CueSiC composites using techniques
Despite the significant progress made in obtaining CueSiC such as scanning electron microscopy (SEM) and energy
surface composites through FSP over the last decade, there dispersive spectroscopy (EDS). This research will help to
are still some challenges that need to be addressed in order to develop new methods to control the wear mechanisms and
further improve the performance of these composites. improve the wear resistance of these composites.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 3 ; 2 7 : 1 3 1 7 e1 3 4 9 1343

7. Since the thermal conductivity is one of the crucial prop- [3] Mishra RS, Mahoney MW, McFadden SX, Mara NA,
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of manufacturing parameters on the thermal performance
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Amirhossein Ahmadi Chadegani: Visualization, Investi- Investigation of mechanical properties of Cu/SiC composite
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Declaration of competing interest Esmailzadeh M, Sabbaghian M, et al. Effect of friction stir
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properties of CueTiC composite. Ceram Int
The authors declare that they have no known competing
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