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Microstructural Aspects of the Fabrication of Al/Al2O3 Composite by Friction

Stir Processing

Article  in  Materials · April 2023

DOI: 10.3390/ma16072898

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 materials
Article
Microstructural Aspects of the Fabrication of Al/Al2O3
Composite by Friction Stir Processing
Sergey S. Malopheyev
Citation: Malopheyev, S.S.; Zuiko,
I.S.; Mironov, S.Y.; Kaibyshev, R.O.
Microstructural Aspects of the
Fabrication of Al/Al2 O3 Composite
by Friction Stir Processing. Materials
2023, 16, 2898. https://doi.org/
10.3390/ma16072898
Academic Editors: Zhiwei Liu and
Peng Xiao
Received: 9 March 2023
Revised: 30 March 2023
Accepted: 4 April 2023
Published: 5 April 2023
Copyright: © 2023 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Materials 2023, 16, 2898. https://doi.org/10.3390/ma16072898
, Ivan S. Zuiko , Sergey Yu. Mironov * and Rustam O. Kaibyshev
Laboratory of Mechanical Properties of Nanoscale Materials and Superalloys, Belgorod National Research
University, Pobeda 85, Belgorod 308015, Russia; malofeev@bsu.edu.ru (S.S.M.); zuiko_ivan@bsu.edu.ru (I.S.Z.);
rustam_kaibyshev@bsu.edu.ru (R.O.K.)
* Correspondence: mironov@bsu.edu.ru; Tel.: +7-4722-585456
Abstract: The purpose of this work was the examination of microstructural evolution during the
fabrication of an Al/Al2 O3 composite by friction stir processing (FSP). In order to obtain new insight
into this process, a longitudinal section of the produced composite was studied, and advanced
characterization techniques (including electron backscatter diffraction and microhardness mapping)
were applied. It was found that the reinforcing particles rapidly rearranged into the “onion-ring”
structure, which was very stable against the subsequent dispersion. Specifically, the remnants of the
comparatively coarse-scale particle agglomerations have survived even after 12 FSP passes. Therefore,
it was concluded that three or four FSP passes, which are often applied in practice, are not sufficient to
provide a homogeneous dispersion of the reinforcing particles. It was also revealed that the gradual
distribution of the nanoscale Al2 O3 particles throughout the aluminum matrix promoted a subtle
reduction in both the portion of high-angle boundaries and the average grain size. These observations
were attributed to the particle pinning of grain-boundary migration and dislocation slip.
Keywords: aluminum matrix composite; alumina nanoparticles; friction stir processing; microstructure;
texture; electron backscatter diffraction (EBSD)
1. Introduction
Aluminum matrix composites offer an attractive synergy of properties, including low
density, good strength, and superior thermal stability [1]. Accordingly, these materials are
used for high-performance applications in the transportation sector (particularly in the
automotive industry), specifically for the manufacturing of pistons, brake rotors, connecting
rods, etc. [2]. An important advantage of aluminum matrix composites if compared with
other lightweight composites (such as magnesium or titanium-based) is a reasonably low
price–performance ratio [3].
Friction stir processing (FSP) is sometimes considered a promising technique for
the fabrication of aluminum matrix composites [4–7]. Due to the solid-state nature of
this technology, FSP minimizes interfacial reactions between the reinforcing elements
and the aluminum matrix and thus provides good interfacial bonding between these
two constituents.
The extensive research in this area has conclusively demonstrated the high efficiency
of FSP for the fabrication of aluminum matrix composites [4–7]. Specifically, a wide range
of composites was successfully produced using a variety of both reinforcing particles
and matrix aluminum alloys. The reinforcing elements typically comprise SiC [8–15] or
Al2 O3 [11,16–25] phases but may also involve other particles [26–33]. On the other hand,
the matrix materials included the 1xxx [8,9,16,29], 2xxx [20–22], 5xxx [11,13,27,30,32,33],
6xxx [12,17,23,31], and 7xxx [10,26] series of aluminum alloys.
Moreover, it was found that the agglomeration of the reinforcing particles during
FSP represents an essential problem. Specifically, a single FSP pass is usually not suffi-
https://www.mdpi.com/journal/materials
 Materials 2023, 16, x FOR PEER REVIEW 2 of 14
Materials 2023, 16, 2898 2 of 14

Moreover, it was found that the agglomeration of the reinforcing particles during
cient to producean
FSP represents essential problem.
a homogeneous Specifically,
particle a singleTypically,
distribution. FSP passthree
is usually notpasses
to four suffi- are
cient to produce
applied [11,17–21]. a homogeneous particle distribution. Typically, three to four passes are
applied [11,17–21].
It is important to point out that the distribution of the reinforcing particles throughout
It is important
the FSP-produced to point isout
composites that theexamined
normally distribution of transverse
in the the reinforcing particles
cross section of the
throughout the FSP-produced composites is normally examined in the transverse
processed material. In this context, it is worth noting that the FSP technology for composite cross
section of the
fabrication processed
is based material.
on the In this
preplaced context,strategy.
powder it is worth noting that
According tothe
thisFSP technol- the
technique,
ogy for composite
reinforcing particlesfabrication is based
(or powder) on the preplaced
are distributed powder
throughout thestrategy. According
matrix material to the
from
this technique, the reinforcing particles (or powder) are distributed throughout the ma-
preliminary-drilled grooves, which are preplaced along the FSP path. Hence, it would be
trix material from the preliminary-drilled grooves, which are preplaced along the FSP
useful to also check the particle distribution in the longitudinal section of the composites.
path. Hence, it would be useful to also check the particle distribution in the longitudinal
This approach may provide new insight into microstructural evolution during the FSP
section of the composites. This approach may provide new insight into microstructural
fabrication of aluminum matrix composites and thus improve our understanding of this
evolution during the FSP fabrication of aluminum matrix composites and thus improve
process. This was the objective of the present work.
our understanding of this process. This was the objective of the present work.
2. Materials and Methods
2. Materials and Methods
2.1. Materials
2.1. Materials
The commercial aluminum alloy 5182 was employed as a metal matrix material. The
The commercial aluminum alloy 5182 was employed as a metal matrix material. The
material was manufactured by semi-continuous casting using the casting equipment of
material was manufactured by semi-continuous casting using the casting equipment of
the Joint Research Center “Technology and Materials” at Belgorod National Research
the Joint Research Center “Technology and Materials” at Belgorod National Research
University. The measured chemical composition of the matrix material was Al-4.75Mg-
University. The measured chemical composition of the matrix material was
0.3Mn-0.15Zr-0.1Ti-0.1Cr-0.06Si-0.05Fe (wt. %). The cast ingot was homogenized at 360 ◦ C
Al-4.75Mg-0.3Mn-0.15Zr-0.1Ti-0.1Cr-0.06Si-0.05Fe (wt. %). The cast ingot was homoge-
for 24 h,
nized at sliced
360 °C along its longitudinal
for 24 hrs, sliced along its direction, anddirection,
longitudinal then coldand rolled
thento a total
cold rolledthickness
to a
reduction of 75%. The final thickness of the rolled sheets was 5.2
total thickness reduction of 75%. The final thickness of the rolled sheets was 5.2 mm.mm.
The
Thenanoscale
nanoscale alumina
alumina (Al(Al22OO3)3 powder
) powder was
was used
used as as a reinforcing
a reinforcing phase.
phase. The The powder
powder
particles had a nearly spherical shape and an average diameter
particles had a nearly spherical shape and an average diameter of 20 nm. of 20 nm.
ToTointroduce
introduce thethe Al
Al22OO33 phase
phaseinto intothe
thealuminum
aluminum matrix,
matrix, a series
a series of grooves
of grooves was was
machined
machined within the aluminum workpieces (Figure 1), in which the alumina powder was was
within the aluminum workpieces (Figure 1), in which the alumina powder
filled.
filled.The
The grooves werearranged
grooves were arrangedinina acheckboard
checkboard papattern
ern alongalong
the the
FSPFSP
lineline (Figure
(Figure 1a) 1a)
and
andhad
had aa diameter
diameter of 1.5 1.5 mm
mm and andaadepthdepthofof1 1mm
mm(Figure
(Figure 1b).
1b). TheThe mutual
mutual distance
distance
between
betweenthe thegrooves
grooveswas was3.53.5
mm. mm. TheTheapproximate
approximatevolume
volume fraction of the
fraction of alumina
the aluminapowder
Fpowder
v was evaluated
F v was using the equation
evaluated [9] Fv = [9]
using the equation  VL), Awhere
V/(FAv ×  L  , where
V is theV total volume
is the total of
the grooves,
volume of theA grooves,
is the cross-section area of the stir
A is the cross-section areazone, stir Lzone,
of theand is the length
and L isofthe
thelength
FSP path
(Figure 1a). The calculated volume fraction was ≈ 1%.
of the FSP path (Figure 1a). The calculated volume fraction was ≈1%.

Figure1.1.Schematics
Figure Schematics showing
showing (a)
(a)the
thespatial
spatialarrangement
arrangementofof
thethe
grooves with
grooves Al2Al
with O32powder during
O3 powder during
FSPand
FSP and(b)
(b)the
the dimensions
dimensions of
ofthe
theFSP
FSPworkpieces
workpieceswith drilled
with drilledgrooves. In (a),
grooves. PD,PD,
In (a), ND,ND,
and and
TD are
TD are
the FSP direction, normal direction, and transverse direction, respectively.
the FSP direction, normal direction, and transverse direction, respectively.

2.2. FSP Procedure

The workpieces with the preplaced Al2 O3 powder were subjected to FSP using a
commercial AccuStir 1004 FSW machine. To maintain consistency with scientific literature,
 Materials 2023, 16, x FOR PEER REVIEW 3 of 14

Materials 2023, 16, 2898 3 of 14

2.2. FSP Procedure
The workpieces with the preplaced Al2O3 powder were subjected to FSP using a
commercial AccuStir 1004 FSW machine. To maintain consistency with scientific litera-
the conventional FSP reference frame was used, which included FSP direction (PD), normal
ture, the conventional FSP reference frame was used, which included FSP direction (PD),
direction (ND), and transverse direction (TD), as shown in Figure 1a.
normal direction (ND), and transverse direction (TD), as shown in Figure 1a.
To minimize mechanical abrasion of the FSP tool during FSP, the tool was manufac-
To minimize mechanical abrasion of the FSP tool during FSP, the tool was manu-
tured from a tungsten carbide alloy. The geometry and principal dimensions of the tool are
factured from a tungsten carbide alloy. The geometry and principal dimensions of the
shown in Figure 2a.
tool are shown in Figure 2a.

Figure2.2.(a)
Figure (a)Schematic
Schematic of
of FSP
FSP tool
tooland
and(b)
(b)FSP
FSPthermal cycle
thermal recorded
cycle at the
recorded border
at the of the
border of stir
the zone.
stir zone.

ToToproduce
producea afine-grained
fine-grainedstructure
structureininthe
thealuminum
aluminummatrix,
matrix,aacomparatively
comparatively low
low tool
tool rotation
rotation rate ofrate
500ofrpm
500 was
rpm applied.
was applied. Onother
On the the other hand,
hand, to enhance
to enhance thethe dispersion
dispersion of O
of Al2 3
Al 2O3 powder, the tool translation rate was also selected to be relatively small at 125
powder, the tool translation rate was also selected to be relatively small at 125 mm/min.
mm/min.
Hence, theHence, the toolper
tool advance advance perwas
rotation rotation
250 was
µm. 250 µm.
To examine the effect of multiple passes on microstructural evolution, the work-
To examine the effect of multiple passes on microstructural evolution, the workpieces
pieces with the preplaced Al2O3 powder were subjected to 1, 2, 3, 4, 8, and 12 FSP passes
with the preplaced Al2 O3 powder were subjected to 1, 2, 3, 4, 8, and 12 FSP passes us-
using the same processing variables as indicated above. In an a empt to promote a more
ing the same processing variables as indicated above. In an attempt to promote a more
homogeneous distribution of the reinforcing particles, the upper and bo om parts of the
homogeneous distribution of the reinforcing particles, the upper and bottom parts of the
workpieces (as well as their advancing and retreating sides) were inverted between the
workpieces (as well as their advancing and retreating sides) were inverted between the
passes, while the processing direction was kept the same.
passes,Towhile the processing direction was kept the same.
assist the interpretation of microstructural changes, the FSP thermal cycle was
To assist the interpretation
recorded employing of microstructural
K-type thermocouples placed atchanges,
the border theofFSP
the thermal
stir zone cycle
at thewas
recorded employing K-type thermocouples placed at the border of the
mid-thickness of an FSP workpiece (Figure 2b). The key characteristics of the recordedstir zone at the
mid-thickness
temperature profile included a peak temperature of 422 °C and a relatively slow coolingtem-
of an FSP workpiece (Figure 2b). The key characteristics of the recorded
perature
rate. profile included a peak temperature of 422 ◦ C and a relatively slow cooling rate.

2.3.
2.3.Microstructural
Microstructural Observations
Observations
AsAsdiscussed
discussed in in Section
Section 1, 1, microstructural
microstructuralobservations
observations in in
thethe present
present work
work werewere
focused
focusedon on the
the longitudinal
longitudinal (PD (PD× ×ND)ND) plane
plane of the
of the stir stir
zonezone (Figure
(Figure 1a).examina-
1a). The The exami-
nations involvedoptical
tions involved opticalmicroscopy,
microscopy, microhardness
microhardness mapping,
mapping, andand electron
electron backscatter
backsca er
diffraction
diffraction(EBSD).
(EBSD).
InInall
allcases,
cases, the
the FSP’ed workpieceswere
FSP’ed workpieces weresectioned
sectioned in in half
half along
along the the
FSPFSP centerline,
centerline,
and
andmetallographic
metallographic specimens
specimens werewereprepared
preparedaccording
according toto ASTM
ASTM E3 E3 standards.
standards. TheThe
finalfinal
polishing
polishingstep
stepcomprised
comprisedaalong-term
long-term (up
(up to
to 24-h)
24-h) vibratory
vibratory polishing with
with OPS
OPS suspen-
suspension.
sion.The macro-scale structure was studied using optical microscopy and microhardness
mapping.The macro-scale
The optical structure
observationswas studied using optical
were conducted usingmicroscopy
an opticaland microhardness
microscope Olympus
mapping. The optical observations were conducted using an
GX71 equipped with SIAMS 800 software. The Vickers microhardness measurementsoptical microscope Olym-were
pus GX71 in
performed equipped with with
accordance SIAMS 800 software.
ASTM The Vickers
E92-17 standard microhardness
by applying a loadmeasurements
of 0.2 kg, a dwell
wereofperformed
time 10 s, and ainstep
accordance withmm.
size of 0.25 ASTM E92-17 standard by applying a load of 0.2 kg,
a dwell
The time
grainofstructure
10 s, andwasa step size of 0.25by
investigated mm.EBSD (the basic principles of EBSD are detailed
in Refs. [34,35]) using an FEI Quanta 600 field-emission-gun scanning-electron microscope
(SEM) equipped with TSL OIM software. Orientation mapping was conducted employing a
scan step size of either 0.5 or 0.25 µm. The low-angle boundaries (LABs) were differentiated
from the high-angle boundaries (HABs) using a 15-degree tolerance. The grain size was
measured using the equivalent-circle-diameter approach [35].
 microscope (SEM) equipped with TSL OIM software. Orientation mapping was con-
ducted employing a scan step size of either 0.5 or 0.25 µm. The low-angle boundaries
(LABs) were differentiated from the high-angle boundaries (HABs) using a 15-degree
tolerance. The grain size was measured using the equivalent-circle-diameter approach
Materials 2023, 16, 2898 [35]. 4 of 14

3. Results and Discussion

3. Macro-Scale
3.1. Results and Structure
Discussion
3.1. Macro-Scale Structure
The evolution of the macro-scale structure within the stir zone as a function of the
The evolution of the macro-scale structure within the stir zone as a function of the
number of FSP passes is shown in Figure 3. To assist the interpretation of the macro-scale
number of FSP passes is shown in Figure 3. To assist the interpretation of the macro-scale
structures,
structures,microhardness
microhardness data werealso
data were alsopresented
presentedinin Figures
Figures 4 and
4 and 5. Specifically,
5. Specifically, the the
microhardness
microhardnessmaps in Figure
maps in Figure4 4were
were used
used forfor
thethe examination
examination of theofspatial
the spatial distribution
distribution of
ofAl
Al3 O
3O3powder.
3
powder. By analogy with the work by Zhang et al. [36], microhardness
By analogy with the work by Zhang et al. [36], microhardness profiles were profiles
were
alsoalso measured
measured to quantify
to quantify the dispersion
the dispersion of the reinforcing
of the reinforcing particles
particles through thethrough
matrix the
matrix
material material
(Figure(Figure 5a). Moreover,
5a). Moreover, the average the average microhardness
microhardness of the acquired ofmicrohardness
the acquired mi-
map was also
crohardness shown
map was as a function
also shown as of the number of
a function of the
FSP number
passes inof Figure 5b.
FSP passes in Figure 5b.

Figure
Figure3.3.Optical
Opticalimages
images of
of longitudinal sectionsofofthe
longitudinal sections theprocessed
processed material
material as aasfunction
a function
of theof the
number of FSP passes: (a) 1 pass; (b) 2 passes; (c) 3 passes; (d) 4 passes; (e) 8 passes; and (f) 12
number of FSP passes: (a) 1 pass; (b) 2 passes; (c) 3 passes; (d) 4 passes; (e) 8 passes; and (f) 12 passes.
passes. Selected areas outline microhardness maps shown in Figure 4. In (a), circles indicate the
Selected areas outline microhardness maps shown in Figure 4. In (a), circles indicate the approximate
approximate positions of the initial placement of alumina powder.
positions of the initial placement of alumina powder.

After the first FSP pass, the Al2 O3 powder mainly remained in close proximity to the
areas of initial placement (indicated by circles in Figure 3a). The spatial dispersion of the
reinforcing particles was fairly limited (Figure 3a), thus giving rise to essential variations in
microhardness (Figures 4a and 5a). As a result, the microstructure distribution was fairly
non-uniform (Figures 3a and 4a). Hence, a single FSP pass is obviously not sufficient to
produce a high-quality composite.
Materials 2023, 2023,
Materials 16, x 16,
FOR PEER REVIEW
2898 5 of514of 14

Figure
Figure4. Microhardness
4. Microhardnessmaps
mapsof ofthe
the processed materialasasa afunction
processed material functionof of
thethe number
number of FSP
of FSP passes:
passes:
(a) (a)
1 pass; (b) 2 passes; (c) 3 passes; (d) 4 passes; (e) 8 passes; and (f) 12 passes.
1 pass; (b) 2 passes; (c) 3 passes; (d) 4 passes; (e) 8 passes; and (f) 12 passes.

Essential particle dispersion in the vertical direction was also worthy of remark
(Figure 3a). This observation suggested an extensive vertical material flow within the
stir zone.
After two FSP passes, the macro-scale structure became more uniform (compare
Figure 3a,b). This resulted in a gradual increase in microhardness (Figure 5b). On the
other hand, the reinforcing particles still tended to preferentially concentrate relatively near
their initial placement positions (Figure 4b), thereby leading to essential fluctuations in the
microhardness profile (Figure 5a).
Materials 2023,
Materials 16, 2898
2023, 16, x FOR PEER REVIEW 6 of 14
6 of 14

Figure5.5.Effect
Figure Effectof
ofnumber
number FSP
FSP passes
passeson
on(a)
(a)the
themicrohardness
microhardnessprofile measured
profile across
measured the work-
across the work-
pieces’ mid-thickness and (b) the average microhardness of the acquired microhardness maps. In
pieces’ mid-thickness and (b) the average microhardness of the acquired microhardness maps. In
(b), error bars show the standard deviation. Note: The empty circles in (b) show experimental data
(b), error bars show the standard deviation. Note: The empty circles in (b) show experimental
points.
data points.
After the first FSP pass, the Al2O3 powder mainly remained in close proximity to the
areasTheof third
initialand fourth (indicated
placement FSP passes byresulted
circles ininFigure
the development
3a). The spatialof dispersion
a specific structure,
of the
which consisted of the regular set of vertically oriented particle-rich
reinforcing particles was fairly limited (Figure 3a), thus giving rise to essential bandsvariations
throughout
the
in stir zone (Figure(Figures
microhardness 3c,d). Importantly,
4a and 5a). As theamean
result,spacing between thedistribution
the microstructure bands was was close to
250 µm, i.e., virtually the tool advance per revolution. Therefore,
fairly non-uniform (Figures 3a and 4a). Hence, a single FSP pass is obviously not suffi- the developed structure
represented
cient to produce the so-called
a high-quality“onion-ring”
composite. structure, which is intrinsic to friction stir weld-
ing/processing. In fact, dispersion
Essential particle this structure represents
in the vertical adirection
superposition of material
was also worthy of layers,
remarkwhich
are “cut”3a).
(Figure from theobservation
This initial workpiece
suggested during every single
an extensive verticalrotation
materialof thewithin
flow FSP tool the [37].
stir In
the present case, the development of the “onion-ring” structure implied the formation
zone.
of the After
repeated two sequence
FSP passes, of the
the macro-scale
particle-richstructure became more
and particle-poor uniform
layers, (compare the
i.e., virtually,
Figure 3a,b).of
development This
a newresulted
sort ofinmicrostructural
a gradual increase in microhardness
heterogeneity. (Figure 5b).
The preferential On the
arrangement
ofother hand, the reinforcing
the reinforcing particles as particles still tended
the onion-ring to preferentially
structure concentrate
has been reported relatively
in the scientific
near their initial
literature [38–44]. placement positions (Figure 4b), thereby leading to essential fluctuations
in the
Anmicrohardness
increased fraction profileof (Figure 5a).
the reinforcing particles in either the upper or bottom parts of
the stir zone was also evident (Figuresresulted
The third and fourth FSP passes 3c,d andin4c,d).
the development of a specific
This observation structure, the
likely suggested
which consisted of the regular
importance of vertical material flow. set of vertically oriented particle-rich bands throughout
the With
stir zonethe(Figure
further3c,d). Importantly,
increase the meanofspacing
in the number between
FSP passes, thethe bands was close
“onion-ring” to
structure
250 µm, i.e., virtually the tool advance per revolution. Therefore, the
tended to become less apparent (Figure 3e,f); thus, perhaps evidencing a gradual dispersion developed structure
represented the so-called “onion-ring” structure, which is intrinsic to friction stir weld-
of the coarse-scale particle agglomerations. This resulted in a smoothing of microhardness
ing/processing. In fact, this structure represents a superposition of material layers, which
profiles (Figure 5a) and a gradual increase in the average microhardness (Figure 5b).
are “cut” from the initial workpiece during every single rotation of the FSP tool [37]. In
Remarkably, the latter process tended to saturate (Figure 5b).
the present case, the development of the “onion-ring” structure implied the formation of
On the other hand, it is important to emphasize that the agglomerations of Al O
the repeated sequence of the particle-rich and particle-poor layers, i.e., virtually, the de-2 3
did not disappear completely even after twelve FSP passes (Figure 3f). As a result, the
velopment of a new sort of microstructural heterogeneity. The preferential arrangement
microhardness
of the reinforcing distribution
particles aswas the still not uniform
onion-ring structure(Figure 4f). reported
has been Moreover, in the macro-scale
the scientific
cluster of the reinforcing
literature [38–44]. particles at the root of the stir zone also survived after a very large
number of FSP passes (Figures 3e,f and 4e).
An increased fraction of the reinforcing particles in either the upper or bo om parts
Thus,
of the evenwas
stir zone twelvealsoFSP passes
evident are not
(Figures sufficient
3c,d and 4c,d).toThis
provide an entirely
observation likelyhomogeneous
suggested
distribution
the importance of the
of reinforcing
vertical materialparticles.
flow.
With the further increase in the number of FSP passes, the “onion-ring” structure
3.2. GraintoStructure:
tended become less FSPapparent
without (Figure
Using Reinforcing
3e,f); thus, Particles
perhaps evidencing a gradual disper-
sionToofevaluate the broad
the coarse-scale aspects
particle of grain structure
agglomerations. evolution,
This resulted in aa smoothing
single FSP of pass without
micro-
using reinforcing
hardness profilesparticles
(Figure 5a) wasandapplied.
a gradual Theincrease
typicalinmicrostructure revealed within
the average microhardness the stir
(Figure
5b). is
zone Remarkably,
shown in Figure the la 6a.er process tended to saturate (Figure 5b).
 Thus, even twelve FSP passes are not sufficient to provide an entirely homogeneous
distribution of the reinforcing particles.

3.2. Grain Structure: FSP without Using Reinforcing Particles

To evaluate the broad aspects of grain structure evolution, a single FSP pass without
Materials 2023, 16, 2898 7 of 14
using reinforcing particles was applied. The typical microstructure revealed within the
stir zone is shown in Figure 6a.

Figure6.6.Microstructure
Figure Microstructureproduced
producedafter
afteraasingle
singleFSP
FSPpass
passwithout
withoutusing
usingAlAl
2O2O3powder:
3 powder: (a) (a)EBSD
EBSDmap
map and (b) 111 and 110 pole figures showing crystallographic texture. In (a), grains
and (b) 111 and 110 pole figures showing crystallographic texture. In (a), grains are colored according are colored
according to the transverse direction; LABs and HABs are depicted as white and black lines, re-
to the transverse direction; LABs and HABs are depicted as white and black lines, respectively.
spectively. In (b), SD and SPN show the presumed orientations of shear direction and shear plane
Innormal,
(b), SDrespectively.
and SPN show the presumed orientations of shear direction and shear plane normal,
respectively.
In accordance with expectations, the microstructure was comprised of compara-
In accordance
tively-fine with expectations,
grains (with the average grain the microstructure
size being ~3.5 was µm),comprised
which containedof comparatively-
the es-
fine grains (with the average grain size being ~3.5 µm), which
sential fraction of LABs. This microstructure is typically revealed in FSP’ed aluminum contained the essential
fraction
alloys andof LABs. Thisamicrostructure
is usually ributable to the is development
typically revealed in FSP’ed
of continuous aluminum
dynamic alloys and
recrystalli-
iszation
usually attributable to the development of continuous dynamic recrystallization [6,45,46].
[6,45,46].
Remarkably,
Remarkably, the the measured
measured HAB HAB fraction (≈80%)
fraction(≈80%) waswas somewhat
somewhat higher
higher thanthanthatthat
achievable
achievableduring
during continuous recrystallization(60–70%
continuous recrystallization (60–70% [47,48]).
[47,48]). This
This observation
observation maymay be be
indicative
indicativeof of static
static grain coarsening,which
grain coarsening, whichmay may occur
occur during
during thethe
FSPFSP cooling
cooling cycle cycle
[49],[49],
duetotothe
due therelatively
relatively low cooling
cooling rate
rate(Figure
(Figure2b).2b).
ToToexamine
examine crystallographic
crystallographic texture
textureininthe thestir
stirzone,
zone, thethemeasured
measured orientation
orientation datadata
wererotated
were rotatedinin order
order to to align
align them
them withwiththethe local
local geometry
geometry of the
of the simple-shear
simple-shear strain
strain within
within the stir zone [50]. Specifically, to align the shear direction horizontally,
the stir zone [50]. Specifically, to align the shear direction horizontally, the experimental pole the ex-
perimental
figure pole figure
was rotated ◦ around
by 90was rotated
theby 90° around
normal the normal
direction. Then, direction.
to align the Then,
shear toplane
align normal
the
shear plane normal vertically, the pole figures were additionally
◦ tilted
vertically, the pole figures were additionally tilted by 60 around the transverse direction. by 60° around the
transverse direction. The rotated pole figures were shown in Figure 6b.
The rotated pole figures were shown in Figure 6b. It is seen that the crystallographic texture It is seen that the
crystallographic
within the stir zonetexture within thebystir
was dominated B/Bzone
{112was dominated
} < 110 by B / Borientation,
> simple-shear {112}  110which

issimple-shear orientation,
typically observed which is typically
in friction-stirred observed
aluminum in friction-stirred
alloys [49,50]. aluminum alloys
[49,50].
3.3. Effect of the Reinforcing Al2 O3 Nanoscale Particles on Grain-Structure Evolution
3.3.1. Low-Magnification Overview
A series of low-magnification EBSD orientation maps taken from FSP’ed materials
are shown in Figure 7. In the maps, grains are colored according to their crystallographic
orientations relative to the transverse direction, while black clusters show pixels with a
confidence index below 0.1 (which presumably represent the agglomerations of Al2 O3 ).
It is seen that such clusters are arranged into bands that are oriented nearly vertically
(Figure 7a–d), thus resembling the optical microscopy observations (Figure 3). Moreover,
in good accordance with optical microscopy, the black clusters tended to disappear with
increasing numbers of FSP passes (Figure 7b–f); thus, perhaps evidencing a gradual dis-
persion of the Al2 O3 particles. Of particular interest was the formation of textural bands
after twelve FSP passes (Figure 7f). The possible origin of such bands is considered in
Section 3.3.3.
 3.3. Effect of the Reinforcing Al2O3 Nanoscale Particles on Grain-Structure Evolution
3.3.1. Low-Magnification Overview
A series of low-magnification EBSD orientation maps taken from FSP’ed materials
are shown in Figure 7. In the maps, grains are colored according to their crystallographic
Materials 2023, 16, 2898 8 ofwith
orientations relative to the transverse direction, while black clusters show pixels 14 a
confidence index below 0.1 (which presumably represent the agglomerations of Al2O3).

Figure
Figure7. 7.Low-magnification
Low-magnificationEBSD EBSD maps showinggrain
maps showing grainstructures
structures of of
thethe produced
produced composite
composite as a as a
function
function of the number of FSP passes: (a) 1 pass; (b) 2 passes; (c) 3 passes; (d) 4 passes; (e) 8 passes; and
of the number of FSP passes: (a) 1 pass; (b) 2 passes; (c) 3 passes; (d) 4 passes; (e) 8 passes;
(f) and
12 passes. In the maps,
(f) 12 passes. In the grains
maps, are colored
grains according
are colored to theirtocrystallographic
according orientations
their crystallographic relative to
orientations
therelative
transverse direction, while black clusters show the pixels with a confidence index below
to the transverse direction, while black clusters show the pixels with a confidence index below 0.1. The
reference
0.1. Theframe andframe
reference scale and
of allscale
EBSD maps
of all EBSDaremaps
indicated in (a). Note:
are indicated in (a).The microstructures
Note: within the
The microstructures
selected areas (white rectangles) are shown at higher magnification in Figure 7.
within the selected areas (white rectangles) are shown at higher magnification in Figure 7.

3.3.2. Microstructure Morphology and Grain Size

In this study, no reliable EBSD data were obtained from the coarse-scale particle-
rich bands in Figure 7. Hence, microstructural analysis was focused on the aluminum
 a gradual dispersion of the Al2O3 particles. Of particular interest was the formation of
textural bands after twelve FSP passes (Figure 7f). The possible origin of such bands is
considered in Section 3.3.3.

3.3.2.
Materials 2023, Microstructure
16, 2898 Morphology and Grain Size 9 of 14

In this study, no reliable EBSD data were obtained from the coarse-scale particle-rich
bands in Figure 7. Hence, microstructural analysis was focused on the aluminum matrix. The
matrix. The high-magnification EBSD maps taken from the aluminum matrix after different
high-magnificationnumbers
EBSD mapsof FSPtaken
passesfrom the aluminum
are shown in Figure 8.matrix after LABs
In the maps, different numbers
and HABs of
are depicted
FSP passes are shown in Figure 8. In the maps, LABs and HABs are depicted as red and black
as red and black lines, respectively. The relevant microstructural statistics are given in
lines, respectively. The relevant
Figure 9. microstructural statistics are given in Figure 9.

Figure 8. High-magnification EBSD grain-boundary

Figure 8. High-magnification maps showing
EBSD grain-boundary maps grain structures
showing within within
grain structures the the
aluminum matrix asaluminum
a functionmatrix
of theasnumber
a functionofofFSP
the passes:
number (a) 1 pass;
of FSP (b)(a)
passes: 2 passes; (c)23passes;
1 pass; (b) passes;(c)(d)
3 passes;
4 passes; (e) 8 passes;(d)and (f) 12 passes. In the maps, LABs and HABs are depicted as red and black
4 passes; (e) 8 passes; and (f) 12 passes. In the maps, LABs and HABs are depicted as red and
lines, respectively. The
blackreference frame and
lines, respectively. scale offrame
The reference all EBSD maps
and scale of allare
EBSDindicated in (a). Arrows
maps are indicated in (a). Arrows
exemplify the presumed agglomerations
exemplify the presumed of the Al2O3 powder.
agglomerations of the Al2 O3 powder.
Materials 2023, 16, x FOR PEER REVIEW 10 of 14
Materials 2023, 16, 2898 10 of 14

Effectofofnumber
Figure9.9.Effect
Figure number FSP
FSP passes
passes on
on (a)
(a) average
average grain
grain size
sizeand
and(b)
(b)HAB
HABfraction
fractionwithin
withinthe
the
aluminummatrix
aluminum matrixof ofthe
the produced
produced composite.
composite.

Afterthe
After the first
first and
andsecond
secondFSP FSPpasses,
passes, thethe
important
important microstructural
microstructuralcharacteristic was
characteristic
the the
was development
development of fine-grained
of fine-grained bandsbands(arrows in Figure
(arrows 8a,b). Remarkably,
in Figure such bands
8a,b). Remarkably, such
(as well as the adjacent areas) often exhibited increased LAB content (Figure 8b). These
bands (as well as the adjacent areas) often exhibited increased LAB content (Figure 8b).
observations presumably reflected the influence of the nanoscale Al2 O3 dispersoids.
These observations presumably reflected the influence of the nanoscale Al2O3 disper-
Specifically, it is known that the relatively small (~1 µm in size) agglomerations of the
soids.
nanoscale particles may promote the activation of the mechanism of the particle-stimulated
Specifically, it[6]isand
recrystallization known thusthat the relatively
promote local grain small (~1 µm inOn
refinement. size)
theagglomerations
other hand, theof
the nanoscale particles may promote the activation of the
nanoscale dispersoids per se should retard grain-boundary migration and dislocation mechanism of the parti-
slip.
cle-stimulated recrystallization [6] and thus promote local grain
In the first case, the enhancement of the grain-refinement effect is expected. The second refinement. On the other
hand, the nanoscale dispersoids per se should retard grain-boundary
effect may inhibit the progressive evolution of deformation-induced boundaries, including migration and
dislocation slip. In the first case, the enhancement of the grain-refinement
the LAB-to-HAB transformation; this should result in a decreased HAB fraction in the effect is ex-
pected. The second
microstructure. effect
It was, may inhibit
therefore, the progressive
likely that evolution ofbands
the revealed fine-grained deformation-induced
were associated
boundaries,
with the local including the LAB-to-HAB
concentration of the Al2 O3transformation;
particles. this should result in a decreased
HAB fraction
Therefore, in the
thegradual
microstructure.
dispersion It of
was,
the therefore,
reinforcinglikely thatthroughout
particles the revealed thefine-grained
aluminum
matrix with sequential FSP passes resulted in a steady
bands were associated with the local concentration of the Al2O3 particles. decrease in both grain size and
HAB content (Figures
Therefore, 8c–f and
the gradual 9a,b). Aofgradual
dispersion grain refinement
the reinforcing particleswithin the matrix
throughout of
the alu-
the aluminum-based
minum composites
matrix with sequential FSP with the number
passes resultedofinFSP passesdecrease
a steady has beeninreported
both grain in the
size
scientific
and literature
HAB content [16,17,20,21,51–54].
(Figures 8c–f and 9a,b). A gradual grain refinement within the matrix of
Remarkably, both
the aluminum-based composites above processes
with the tended
number to saturate, and thus
of FSP passes the final
has been effect in
reported was the
comparatively small (Figure 9).
scientific literature [16,17,20,21,51–54]. Moreover, a significant experimental scattering is worthy of
remarking (Figureboth
Remarkably, 9a,b).above
The latter effect tended
processes was likely to due to theand
saturate, macro-scale
thus theinhomogeneity
final effect was
of microstructure distribution, as discussed above.
comparatively small (Figure 9). Moreover, a significant experimental sca ering is worthy
of3.3.3.
remarking (Figure 9a,b).
Crystallographic TextureThe la er effect was likely due to the macro-scale inhomo-
geneity of microstructure distribution, as discussed above.
To investigate the evolution of crystallographic texture, orientation data were derived
from EBSD maps in Figure 7 and rotated in a manner described in Section 3.2. The typical
3.3.3. Crystallographic Texture
examples of rotated pole figures are shown in Figure 10. It is seen that neither the addition
Toreinforcing
of the investigateparticles
the evolution
nor the of crystallographic
number of FSP passes texture,
exertedorientation
a principaldata wereon
influence de-
rived from EBSD
the texture. In all maps
cases, in Figure
it was 7 and rotated
dominated by B/Bin a manner
{112 } < 110 described
> simple-shearin Section 3.2. The
orientations.
typicalConsidering
examples ofthe rotated
formationpole offigures
texturalarebands
shown in Figure
after 12 FSP 10. It is(Figure
passes seen that7f),neither
the crys-the
tallographic
addition of theorientations
reinforcing of particles
the bandsnor were thealso examined.
number To apasses
of FSP first approximation, two
exerted a principal
different types
influence on theof texture.
textural bands
In all could
cases, be it defined in Figure 7f:
was dominated by (i)B the
/ B{green
112} and110(ii)
 the
sim-
blue-to-pink colored ones. The crystallographic orientations of the bands are shown in
ple-shear orientations.
Figure 11.
Materials 2023,
Materials 16, 16,
2023, 2898x FOR PEER REVIEW 11 of 11
14of 14

Figure 10. Images of 111 and 110 pole figures showing crystallographic texture within the alumi-
num matrix of the produced composite as a function of the number of FSP passes: (a) 1 pass; (b) 12
passes. SD and SPN show the presumed orientations of shear direction and shear plane normal,
respectively.

Considering the formation of textural bands after 12 FSP passes (Figure 7f), the
crystallographic orientations of the bands were also examined. To a first approximation,
Figure10.
10.Images
Imagesofof111
111 and110
110 polefigures
figuresshowing
showingcrystallographic
crystallographic texture
texture within
within the alumi-
Figure
two different types of and
texturalpole
bands could be defined in Figure 7f: (i) the greenthe aluminum
and
num matrix of the produced composite as a function of the number of FSP passes: (a) 1 pass; (b) 12
(ii)
matrix
the of the produced
blue-to-pink composite
colored as a function of the number of FSP passes: (a) 1 pass; (b) 12 passes.
passes. SD and SPN show ones. The crystallographic
the presumed orientations of orientations ofand
shear direction the shear
bandsplane
are shown
normal,
SD
in and SPN11.
Figure
respectively.show the presumed orientations of shear direction and shear plane normal, respectively.

Considering the formation of textural bands after 12 FSP passes (Figure 7f), the
crystallographic orientations of the bands were also examined. To a first approximation,
two different types of textural bands could be defined in Figure 7f: (i) the green and (ii)
the blue-to-pink colored ones. The crystallographic orientations of the bands are shown
in Figure 11.

Figure11.
Figure 11.Images
Imagesofof111
111and
and110
110 pole
pole figures
figures showing
showing crystallographic
crystallographic orientationsofof
orientations textural
textural bands
bands in the material condition produced after 12 FSP passes (Figure 7f): (a) green-colored bands;
in the material condition produced after 12 FSP passes (Figure 7f): (a) green-colored bands; and
and (b) blue-to-pink colored bands. SD and SPN shows the presumed orientations of shear direc-
(b) blue-to-pink
tion colored
and shear plane bands.
normal, SD and SPN shows the presumed orientations of shear direction and
respectively.
shear plane normal, respectively.
In both cases, those were close to the B / B{112}  110  texture components.
In both cases, those were close to the B/B{112} < 110 > texture components. How-
However,
Figure 11. in the green-colored
Images of 111 and 110 bands,
pole the showing
figures 110  crystallographic
axis was precisely aligned ofwith
orientations the
ever, in the green-colored bands, the < 110 > axis was precisely aligned with the textural
transverse
transverse
bands in thedirection (i.e., the produced
material condition local shear direction)
after (Figure
12 FSP passes 11a),7f):
(Figure as (a)
is normally expected
green-colored bands;
direction (i.e., the local shear direction) (Figure 11a), as is normally expected for FSP-
for
andFSP-induced
(b) blue-to-pink texture.
colored In the SD
bands. blue-to-pink colored
and SPN shows bands, the
the presumed  110  ofaxis
orientations signifi-
shear direc-
induced
tion and
texture.
shear plane
In normal,
the blue-to-pink
respectively.
colored bands, the < 110 > axis significantly deviated
cantly deviated from this direction (Figure 11b). One of the possible explanations for this
from this direction (Figure 11b). One of the possible explanations for this observation may
observation may be the wobbling of the FSP tool.
be theIn wobbling
both cases,of the FSP tool.
those were close to the B / B{112}  110  texture components.
4. Conclusions
However, in the green-colored bands, the  110  axis was precisely aligned with the
4. Conclusions
transverse
This workdirection (i.e., the to
was initiated local shearnew
provide direction)
insight(Figure 11a), as is normally
into microstructural expected
evolution dur-
for This work
FSP-induced was initiated
texture. In to
theprovide new
blue-to-pink insight
colored into microstructural
bands,
ing the fabrication of aluminum-matrix composites by FSP. Considering the fact that the  110 evolution
axis during
signifi-
the
the
reinforcing particles during FSP are usually introduced through the grooves, which are the
fabrication
cantly deviated of
fromaluminum-matrix
this direction composites
(Figure 11b). One byof FSP.
the Considering
possible the
explanations factfor that
this
reinforcing
observation
placed along particles
may
the beFSPtheduring
wobbling
path, FSP
the are usually
of the introduced
FSP tool.
microstructural examinations through
in the the grooves,
current studywhichwere are
placed
focused on the longitudinal section of the produced composite. The main conclusionswere
along the FSP path, the microstructural examinations in the current study
focused on
4. Conclusions
derived from the
thislongitudinal
work are as sectionfollows. of the produced composite. The main conclusions
derived from
This work this work
wasFSP are
initiated as follows.
(1) Three or four passes,towhich
provide arenew insight
often appliedintoinmicrostructural
practice, are not evolution
sufficient dur-
to
(1)ing the
Three orafour
fabrication
provide FSP
of
homogeneous passes,
aluminum-matrix which are
dispersion often
composites
of the applied
by FSP.in
reinforcing practice,
Considering
particles are
thenot
throughout factsufficient
thatma-
the the to
reinforcing
provide particles
a homogeneous
trix material. during
It was found FSP arethe
usually
dispersion
that introduced
of the
particles reinforcing
rapidly through the
particles
rearranged intogrooves,
throughout whichthe are
the “onion-ring” matrix
placed along the
material. FSP path,
It was foundthe microstructural
that the particles examinations
rapidly rearrangedin the current
into the study were
“onion-ring”
focused on thewhich
structure, longitudinal
was very section of the
stable produced
against composite. The
the subsequent FSP main conclusions
passes. In fact, the
derived from this work are as follows.
remnants of the “onion-ring” structure as well as the comparatively coarse-scale
(1) particle
Three oragglomerations
four FSP passes,inwhich
the bottom partapplied
are often of the processed
in practice,material have survived
are not sufficient to
provide
even aftera 12
homogeneous
FSP passes.dispersion of the reinforcing particles throughout the ma-
(2) Thetrix gradual
material.dispersion
It was found
ofthat
the the particles particles
reinforcing rapidly rearranged
throughout into thealuminum
the “onion-ring”
matrix
promoted a subtle reduction in grain size and HAB fraction. These observations
were suggested to originate from the combined effects of the particle-stimulated
Materials 2023, 16, 2898 12 of 14

recrystallization as well as the retardation of grain-boundary migration and LAB-to-

HAB transformation during FSP.

Author Contributions: Conceptualization, S.S.M.; methodology, S.S.M.; software, S.S.M., I.S.Z. and
S.Y.M.; validation, S.S.M., I.S.Z., S.Y.M. and R.O.K.; formal analysis, S.S.M.; investigation, S.S.M. and
I.S.Z.; resources, S.S.M. and R.O.K.; data curation, S.S.M., I.S.Z. and S.Y.M.; writing—original draft
preparation, S.S.M. and S.Y.M.; writing—review and editing, S.Y.M. and R.O.K.; visualization, S.S.M.,
I.S.Z. and S.Y.M.; supervision, R.O.K.; project administration, S.S.M.; funding acquisition, S.S.M. and
I.S.Z. All authors have read and agreed to the published version of the manuscript.
Funding: The study was supported by a grant from the Russian Science Foundation No. 21-79-10088
(https://rscf.ru/en/project/21-79-10088/; accessed on 3 April 2023).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: The data presented in this study are available on request from the
corresponding author.
Acknowledgments: The experimental works were conducted using equipment of the Joint Research
Center of Belgorod State National Research University «Technology and Materials» the activity of
which was supported by the Ministry of Science and Higher Education of the Russian Federation
within the framework of agreement No. 075-15-2021-690 (the unique identifier for the project is
RF—2296.61321X0030).
Conflicts of Interest: The authors declare no conflict of interest.

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