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Crystals 13 00540

This study investigates the local microstructure and texture development of AA5182 aluminum alloy during friction stir spot welding (FSSW). The analysis reveals distinct zones with varying mechanical properties and microstructural features, including the stir zone, thermomechanically affected zone, and heat-affected zone, with microhardness decreasing from the keyhole. The findings contribute to understanding the microstructural evolution and mechanical properties of FSSW in aluminum alloys, emphasizing the importance of controlling texture and grain size.

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0% found this document useful (0 votes)
5 views25 pages

Crystals 13 00540

This study investigates the local microstructure and texture development of AA5182 aluminum alloy during friction stir spot welding (FSSW). The analysis reveals distinct zones with varying mechanical properties and microstructural features, including the stir zone, thermomechanically affected zone, and heat-affected zone, with microhardness decreasing from the keyhole. The findings contribute to understanding the microstructural evolution and mechanical properties of FSSW in aluminum alloys, emphasizing the importance of controlling texture and grain size.

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yudha
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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crystals

Article
Local Microstructure and Texture Development during Friction
Stir Spot of 5182 Aluminum Alloy
Thierry Baudin 1 , Sandrine Bozzi 2 , François Brisset 1 and Hiba Azzeddine 3, *

1 CNRS, Institut de Chimie Moléculaire et des Matériaux d’Orsay, Université Paris-Saclay, 91405 Orsay, France;
[email protected] (T.B.)
2 Aubert & Duval, Rue du Villa, 63770 Les Ancizes, France; [email protected]
3 Laboratory of Materials and Renewable Energy, Faculty of Sciences, Mohamed Boudiaf University,
M’sila 28000, Algeria
* Correspondence: [email protected]

Abstract: The local microstructure, texture gradient and mechanical properties through the shoulder
dimension (10 mm) of upper and lower AA5182 aluminum sheets were investigated using electron
backscatter diffraction (EBSD) and Vickers microhardness after friction stir spot welding (FSSW).
Based on the microstructural features (mean grain size, grain boundary type and dynamic recrys-
tallization (DRX)), the upper sheet was found to be mainly composed of the stir zone (SZ) and
thermomechanically affected zone (TMAZ) due to the high deformation induced simultaneously by
the tool rotation and the shoulder download force, while the SZ, TMAZ, heat-affected zone (HAZ)
and base metal (BM) were detected in the lower sheet due to the limited effect of the shoulder
on the lower sheet. The texture changes, due to the nature of the deformation, demonstrated a
shear-type texture at the SZ to a plane strain compression deformation type texture at the TMAZ
and then a recrystallization texture at the HAZ and BM. The microhardness gradually decreased
with the increasing distance from the keyhole along the SZ, TMAZ and HAZ regions. Eventually, the
microstructure and microhardness evolutions were correlated based on the Hall–Petch relationship.

Keywords: aluminum; EBSD; friction stir spot welding; microstructure; texture

Citation: Baudin, T.; Bozzi, S.; Brisset,


F.; Azzeddine, H. Local
Microstructure and Texture
Development during Friction Stir
1. Introduction
Spot of 5182 Aluminum Alloy. Aluminum (Al)-based alloys are widely used in transportation industries owing
Crystals 2023, 13, 540. https:// to their attractive properties such as high strength-to-weight ratio, high electrical and
doi.org/10.3390/cryst13030540 thermal conductivities and good corrosion resistance [1–3]. Today, friction stir welding
(FSW) and friction stir spot welding (FSSW) techniques are frequently used in automotive
Academic Editors: Bolv Xiao and
Yi Huang
and aerospace structural applications, especially in materials with poor weldability by
conventional fusion welding such as aluminum or titanium alloys [3–11].
Received: 7 March 2023 During FSW, a non-consumable tool formed of a shoulder and a pin is rotated and
Revised: 17 March 2023 plunged into two sheets and then translated in one direction. The combination of plastic
Accepted: 19 March 2023 deformation and frictional heat induced by the rotating tool guarantees the bonding
Published: 21 March 2023
between the two sheets by the formation of a solid-state weld [4,5,12]. The processing of
FSSW is similar to FSW but without the tool turning [13]. Therefore, FSSW involves three
steps: plunging, bonding and drawing out, which result in the formation of a keyhole in the
Copyright: © 2023 by the authors.
middle of the joint [14]. Consequently, FSW and FSSW produce a complex microstructure
Licensee MDPI, Basel, Switzerland. in the welded material that can be divided into four distinct regions: (1) the base metal
This article is an open access article (BM), (2) the heat-affected zone (HAZ), (3) the thermomechanically affected zone (TMAZ)
distributed under the terms and and (4) the stir zone (SZ) [10,15,16]. The material in the SZ undergoes both severe plastic
conditions of the Creative Commons deformation and high temperature after the friction stir, which results in excellent grain
Attribution (CC BY) license (https:// refinement due to the occurrence of dynamic recrystallization (DRX). In the TMAZ, the
creativecommons.org/licenses/by/ material suffers from plastic deformation and heating but it is insufficient for DRX; hence,
4.0/). this zone is usually characterized by a highly deformed microstructure. In the HAZ,

Crystals 2023, 13, 540. https://doi.org/10.3390/cryst13030540 https://www.mdpi.com/journal/crystals


Crystals 2023, 13, 540 2 of 25

the material is only affected by heat generated during welding and the microstructure,
especially the grain size, is similar to that of the BM. Finally, the BM is far away from the
weld and it is not affected by deformation or heating [10,16,17]. The crystallographic texture
can change through the weld joint, depending on the nature of the deformation processing.
Numerous papers can be found focusing only on the characterization of the texture in the
SZ that developed a shear texture type [18–23]. However, reports on the characterization of
the texture in the TMAZ and HAZ are very limited [9,21,24]. It is expected that the HAZ
has a similar texture to the BM and the texture of the TMAZ is more complicated due to the
heterogeneous plastic flow [9,21,24].
The heterogeneity of the microstructure and grain orientation (crystallographic texture)
along these zones directly affects the mechanical properties of the welded material and
therefore its performance [23]. Moreover, the final material will strongly depend on the
initial state in terms of grain size, grain morphology, the distribution and fraction of the
second phases [25–27]. Hence, in recent decades, various research and experimentation
has been conducted to elucidate the mechanisms responsible for the microstructural and
textural evolution [18–23,28–33], fractures [13,15,34] and material flow [14,21,35] during
processing and much of it has focused on the optimization of FSW parameters such as tool
rotation speed, downward force and tool geometry to improve the mechanical properties
and decrease the anisotropy in the welded materials [12,13,17,36–44].
For example, it was observed that the shear strength of the FSSW Al 5182 alloy is
significantly improved by increasing the rotational speed up to 1300 rpm [13]. In this case,
the high heat generated from the rotational speed causes the enlargement of the SZ and
assures good bonding [13]. Despite the various investigations, much work is still needed
for a full understanding of the microstructural and especially textural evolution of FSSW
and its associated mechanisms, notably in the TMAZ and HAZ.
Hence, the aim of the present study is the evaluation of the local textural and mi-
crostructural evolution of the SZ, TMAZ, HAZ and BM through the shoulder dimension
of the upper and lower Al5182 sheets after FSSW. In addition, the mechanical properties
obtained through the distribution of Vickers microhardness along the distance from the
keyhole center of the upper and lower sheets were correlated to these metallurgical evolu-
tions. Finally, the contribution of grain size strengthening to the local mechanical properties
was estimated by the Hall–Petch relationship [45,46]. It is believed that the present re-
sults can promote microstructure and texture control during the FSSW of non-treatable
Al-based alloys.

2. Materials and Methods


The chemical composition of the AA5182-O alloy is summarized in Table 1.

Table 1. Chemical composition in weight percentage of AA5182-O alloy.

Mg Fe Mn Zn Si Cu Cr Ti Al
4.5 0.35 0.35 0.25 0.2 0.15 0.1 0.1 balance

The FSSW was conducted using an AA5182 upper sheet 1.2 mm thick and an AA 5182
lower sheet 2 mm thick. Note that the sheet reference frame is defined as rolling direction
(RD), transverse direction (TD) and normal direction (ND). A cylindrical threaded pin
(3.5 mm diameter and 1.8 mm height) and flat shoulder (diameter 10 mm) fabricated of
steel Z38CDV5 treated at 50HRC was used for the welding.
The welding was realized with clamping force of 6 kN, rotation speed of 1300 rpm
and plunge time of 2.5 s. These parameters were selected based on a previous study in
which the AA5182 joint weld exhibited good mechanical properties [13].
The local microstructure and texture analysis through the FSSW joints were carried out
by EBSD measurements on the longitudinal cross-section (RD-ND plane), which is normal
to the welding direction (WD), i.e., the vertical axis in Figure 1. Figure 1 shows the scanning
Crystals 2023, 13, x FOR PEER REVIEW 3 of 25

Crystals 2023, 13, 540 3 of 25

scanning electron microscope (SEM) micrograph of the longitudinal cross-section of AA


5182 after FSSW
electron and the
microscope (SEM)EBSD scanning
micrograph of positions at the cross-section
the longitudinal upper (y = 1ofmm)
AA and
5182 lower
after (y =
FSSW
0 mm) and the
sheet, EBSD scanning
respectively. positionsinatthe
As indicated theFigure
upper 2,
(ythe
= 1measurements
mm) and lowerwere
(y = 0performed
mm)
sheet, respectively. As indicated in the Figure 2, the measurements were performed
at the right (x = 2, 2.5, 3, 3.5, 4 and 5 mm) and left (x = −2, −2.5, −3, −3.5, −4 and −5 at mm)
the right (x = 2, 2.5, 3, 3.5, 4 and 5 mm) and left (x = −2, −2.5, −3, −3.5, −4 and −5 mm)
sides on both sheets from the keyhole centre (x = 0 mm), respectively. The scale value was
sides on both sheets from the keyhole centre (x = 0 mm), respectively. The scale value was
positive on the right side and negative on the left side.
positive on the right side and negative on the left side.

Figure 1. The
Figure SEM
1. The SEMmicrograph of the
micrograph of thelongitudinal
longitudinal cross-section
cross-section of5182
of Al Al 5182
alloyalloy
after after
FSSWFSSW and the
and the
EBSD scanning
EBSD scanningpositions.
positions.

After
After theFSSW,
the FSSW, aa keyhole
keyhole is is formed
formedatatthe thecentre
centreof the FSSW
of the FSSWjointjoint
due toduethetopinthe pin
morphology. In addition, an amount of flash can be seen at
morphology. In addition, an amount of flash can be seen at the upper sheet (see arrow) the upper sheet (see arrow)
resulting from the penetration of the shoulder, which is expected during the FSSW [41]. The
resulting from the penetration of the shoulder, which is expected during the FSSW [41].
SEM micrograph also shows the formation of a hook (see Figure 2), which is the interface
The SEM micrograph also shows the formation of a hook (see Figure 2), which is the in-
between the upper and lower sheets near the SZ and is bent upwards towards the upper
terface
sheetbetween
owing to the upper and lower
the combination sheetsand
of plunging near the SZeffects
stirring and is bent welding
during upwards[44]. towards
The the
upper sheet
bonding at owing to theofcombination
the interfaces the upper andoflower plunging
sheets and
seemsstirring
better on effects
the leftduring
side. welding
[44]. The Thebonding
EBSD sampleat thepreparation
interfacesconsists
of the upper and lower
of mechanical sheets
polishing seems by
followed better on the left
electrolyt-
ical polishing at 20 ◦ C with a Struers A2 solution adapted to Al-based alloys with a voltage
side.
of The
45 VEBSD
over 12 s. The preparation
sample EBSD measurementsconsistswere performedpolishing
of mechanical using a TSL-EDAX-Hikari sys-
followed by electrolytical
tem mounted on a scanning electron microscope FEG-SEM ZEISS
polishing at 20 °C with a Struers A2 solution adapted to Al-based alloys2 with a voltage Supra 55 VP operating at of 45
20 kV. The acquisition and analysis of the scan areas of about 200 × 200 µm with a step size
V over 12 s. The EBSD measurements were performed using a TSL-EDAX-Hikari system
of 0.5 and/or 0.6 µm were processed by Orientation Imaging Microscopy, OIMTM software.
mounted on a scanning electron microscope FEG-SEM ZEISS Supra 55 VP operating at 20 kV.
The grain size data were obtained using a grain tolerance angle of 5◦ and a minimum
Thegrain
acquisition
size of 5and analysis
pixels. of the scan
All datum points areas
withofa about 200 ×index
confidence 200 µm(CI)with
2
lower a step
than size
0.05 of 0.5
and/or 0.6 µm were processed by Orientation Imaging Microscopy,
were excluded from the quantitative analyses, where CI quantifies the reliability of the OIM TM software.

The grain
indexed size[47].
pattern dataThewere meanobtained
grain sizeusingwasameasured
grain tolerance angle
using the of 5° and
equivalent a minimum
diameter
grain size of Grain
approach. 5 pixels. All datum
boundaries withpoints with a confidence
misorientation ◦ were(CI)
angles θ < 2index lowerfrom
excluded thanEBSD0.05 were
excluded from the quantitative analyses, where CI quantifies the reliability of the the
maps to avoid spurious boundaries caused by orientation noise [48]. Based on that, indexed
grain [47].
pattern boundary types grain
The mean were divided
size wasinto sub-grain
measured boundaries
using or very low
the equivalent angle grain
diameter approach.
boundaries
Grain (VLAGBs)
boundaries withwith misorientation
misorientation 2◦ < θ <
angles
◦ low angle grain boundaries (LAGBs)
θ 5< ,2° were excluded from EBSD maps to
with 5 < θ < 15 and high angle grain boundaries (HAGBs) with θ > 15◦ , respectively.
◦ ◦
avoid spurious boundaries caused by orientation noise [48]. Based on that, the grain
The grain orientation spread (GOS) and the kernel average misorientation (KAM)
boundary
approachestypes were divided
implemented into sub-grain
in OIM™ software boundaries
were used toorestimatevery low theangle grain bounda-
distribution of
riesplastic
(VLAGBs) with misorientation 2°< θ < 5°, low angle grain
deformation of a grain by measuring its local misorientation. Grain orientation boundaries (LAGBs) with
5°<spread
θ < 15°is and highasangle
defined grain boundaries
the average deviation between (HAGBs) the with θ > 15°,
orientation of respectively.
each point in the
Theand
grain grain
theorientation spread (GOS)
average orientation of theand thewhere
grain, kernelgrains
averagewithmisorientation
GOS lower than (KAM)1◦ ap-
are considered
proaches strain-free
implemented grains software
in OIM™ (undeformed wereorused fully to
recrystallized
estimate thegrains) [49]. Grain
distribution of plastic
orientationof
deformation spread
a grainvalue increases due
by measuring its to the misorientation.
local development ofGrain misorientation
orientation within
spreadthe is de-
grain resulting from the accumulation of dislocations. In the present
fined as the average deviation between the orientation of each point in the grain and the aver-case, the grains were
separated into three groups: (1) undeformed or recrystallized grains having GOS value
age orientation of the grain, where grains with GOS lower than 1° are considered strain-free
grains (undeformed or fully recrystallized grains) [49]. Grain orientation spread value in-
creases due to the development of misorientation within the grain resulting from the accumu-
lation of dislocations. In the present case, the grains were separated into three groups: (1) un-
deformed or recrystallized grains having GOS value in the range of 0–1°, (2) partially
by calculating the orientation distribution function (ODF) using the harmonic method (L
= 22) and a gaussian function with a half-width of 5° to model each orientation [51].
The measured texture in the TMAZ, HAZ and BM regions is presented in the ob-
served RD-ND plane. For the SZ, it is well documented that the shear texture reference
Crystals 2023, 13, 540 frame is not constant and changes with the rotation of the tool [9,11,19]. Accordingly, 4 of in
25
the transverse cross-section of the weld material (TD-ND plane), the shear direction (SD)
is tangential to the tool surface, the shear plane normal (SPN) is perpendicular to the tool
surface and rotation
in the range of 0–1◦ , direction axisdeformed
(2) partially (RA) is aligned with thegrains
or recovered inclined vertical
having GOSsurface
value of
in the
the
tool [9,11,19].◦ Usually, rotations are performed
range of 1–2 and (3) deformed grains having GOS > 2 . around ◦ the reference directions (RD, TD,
or ND) of the
Kernel EBSD measurement
average misorientationtoismatch
knownthe as shear texturemisorientation
the average developed in angle
the SZofwith the
a given
ideal reference frame SPN-SD plane.
point with all its neighbors belonging to the same grain [50]. Here, the θ KAM value was
In thefrom
calculated present
the case,
meanthe textures of the
misorientation SZ regions
angle betweenare presented
a given point in
andRD-ND
its 3th plane and
neighbors
the identification
excluding of the different
misorientations greatershear
than texture components
5◦ . Hence, of the density
the dislocation obtained {111}
can pole fig-
be obtained
ure and ODF
following theisequation
simply performed
[50]: by a direct comparison with the ideal shear component
positions in the different RA-SD, SPN-SD and αθ RA-SPN planes [52] as shown in Figure 2.
ρ = KAM (1)
The positions of ideal shear texture components ndb for face-centered cubic (FCC) materials
projected
where α = in RA-SD,
3 for mixtureSPN-SD and twist
of tilt and RA-SPN planestypes,
boundary are summarized
b = 0.28 nm is inthe
Table 2 [52].
Burgers The
vector,
shear texture
n = 3 for in FCC
the third materials
neighbor andisd is
formed
the scantypically from A-fiber ({111}//SP) composed of
step size.
A, 𝐴̅ ,MTEX
𝐴∗ and 𝐴∗ components
software was used to and B-fiber
analyze the(<110>//SD)
evolution ofcomprised of A,
texture in the 𝐴̅ , B, 𝐵
different and C
locations
components [52]. It is believed that the presentation of the SZ texture
by calculating the orientation distribution function (ODF) using the harmonic method in the RD-ND plane
(EBSD measurement plane) can be used to track the ◦
material flow within
(L = 22) and a gaussian function with a half-width of 5 to model each orientation [51]. the weld.

Figure 2. {111} pole figures and ODF sections at ϕ2 = 0 and 45◦ displaying the positions of the ideal
shear texture components on: (a) RA-SD, (b) SPN-SD and (c) RA-SPN planes for materials with FCC
structure [52].

The measured texture in the TMAZ, HAZ and BM regions is presented in the observed
RD-ND plane. For the SZ, it is well documented that the shear texture reference frame is not
constant and changes with the rotation of the tool [9,11,19]. Accordingly, in the transverse
cross-section of the weld material (TD-ND plane), the shear direction (SD) is tangential
to the tool surface, the shear plane normal (SPN) is perpendicular to the tool surface and
rotation direction axis (RA) is aligned with the inclined vertical surface of the tool [9,11,19].
Usually, rotations are performed around the reference directions (RD, TD, or ND) of the
EBSD measurement to match the shear texture developed in the SZ with the ideal reference
frame SPN-SD plane.
In the present case, the textures of the SZ regions are presented in RD-ND plane and
the identification of the different shear texture components of the obtained {111} pole figure
and ODF is simply performed by a direct comparison with the ideal shear component
positions in the different RA-SD, SPN-SD and RA-SPN planes [52] as shown in Figure 2.
The positions of ideal shear texture components for face-centered cubic (FCC) materials
projected in RA-SD, SPN-SD and RA-SPN planes are summarized in Table 2 [52]. The
shear texture in FCC materials is formed typically from A-fiber ({111}//SP) composed
Crystals 2023, 13, 540 5 of 25

− − −
of A, A, A1∗ and A2∗ components and B-fiber (<110>//SD) comprised of A, A, B, B and C
components [52]. It is believed that the presentation of the SZ texture in the RD-ND plane
(EBSD measurement plane) can be used to track the material flow within the weld.

Table 2. Position of ideal shear texture components for FCC materials projected in RA-SD, SPN-SD
and RA-SPN planes [52].

Notation RA-SD Plane SPN-SD Plane RA-SPN Plane


Miller index Euler angles (◦ ) Miller index Euler angles (◦ ) Miller index Euler angles (◦ )
{hkl}<uvw> (ϕ1 , Φ, ϕ2 ) {hkl}<uvw> (ϕ1 , Φ, ϕ2 ) {hkl}<uvw> (ϕ1 , Φ, ϕ2 )
− − −
A {1 11}<110> (60, 54.7, 45) {112}<1 10> (0, 35.2, 45) {110}<1 12> (54.7, 90, 45)
− − − −− − −−
A { 11 1 }< 1 10> (120, 54.7, 45) {211}<0 11> (50.7, 65.9, 63.4) {101}< 1 21> (35.26, 45, 90)
− −− −
A1∗ {11 1}<112> (90, 54.7, 45) {101}< 1 21> (35.26, 45, 90) {121}< 101> (129.23, 65.9, 26.5)
− − −− −
A2∗ {11 1 }<2 11> (30, 54.7, 45) {011}< 2 11> (144.7, 45, 0) {211}<0 11> (50.7, 65.9, 63.4)
− − −
B {1 12}<110> (50.7, 65.9, 63.4) {111}<1 10> (0, 54.7, 45) {110}<1 11> (35.26, 90, 45)
− − − −− − −−
B { 11 2 }< 1 10> (0, 35.26, 45) {111}<0 11> (60, 54.7, 45) {101}< 1 11> (54.7, 45, 90)
− −
C {001}<110> (45, 0, 0) {110}<1 10> (0, 90, 45) {011}<0 11> (90, 45, 0)

The microhardness distributions on the longitudinal cross-section of each sheet were


obtained using a Vickers microhardness tester (LECO M400H) with a 50 g load for 20 s and
a spacing of 0.5 mm along the y = 0 (lower sheet) and 1 mm (upper sheet) lines (Figure 1),
respectively.

3. Results
3.1. Microstructure and Texture of BM
Figure 3 presents the orientation imaging micrography (OIM) in inverse pole figure
(TD-IPF) and GOS maps of the BM of the upper and lower sheets, respectively. The HAGBs
are indicated by black lines. The mean grain size and fraction of recrystallized grains are
shown in the upper part of the TD-IPF and GOS maps. Both sheets exhibit a typical static
recrystallization microstructure formed of equiaxed and recrystallized grains (about 91 and
96%) with mean grain size of 19.5 µm in the upper sheet and 16.6 µm in the lower sheet.
These differences are obviously due to the thermomechanical forming processes. The initial
textures of both sheets are presented in Figure 3 via {111} pole figure and ODF sections at
ϕ2 = 0 and 45◦ , respectively. The ideal deformation and recrystallization textures of the
rolled FCC alloys are also shown in Figure 3 and their descriptions in the RD-ND plane are
given in Table 3. The texture of the upper sheet is dominated by the Cube component while
the texture of the lower sheet exhibits the presence of static recrystallization components
(Cube, Goss (G1 ) and rotated Goss (G2 )) and the retained deformation Brass (Bs) component.
The presence of retained deformation texture components such as Brass or Copper is often
reported in hot-rolled Al-based alloys [53–56].
Crystals 2023,13,
Crystals2023, 13,540
x FOR PEER REVIEW 66 of 25
25

Figure 3. The TD-IPF, GOS maps, {111} pole figure and ODF sections at φ2 = 0 and 45° of BM: (a)
Figure 3. The TD-IPF, GOS maps, {111} pole figure and ODF sections at ϕ2 = 0 and 45◦ of BM:
upper sheet and (b) lower sheet. Ideal texture component positions are shown for comparison.
(a) upper sheet and (b) lower sheet. Ideal texture component positions are shown for comparison.
3.2. Microstructure and Texture Evolution after FSSW
Table 3. Position of ideal deformation and recrystallization texture components for rolled FCC
3.2.1. Microstructure
materials Evolution
projected in RD-ND plane.after FSSW
Figures 4 and 5 present the evolution of the microstructure via TD-IPF and GOS maps
of the upper Notation
and lower sheets as a function of distance RD-ND Plane
from the keyhole center of the
welded Al 5182 alloy. In both sheets Miller
and index
both sides, the TD-IPF Eulershow
maps (◦ ) the mi-
anglesthat
Rolling component
crostructure is significantly heterogeneous {hkl}<uvw> * shoulder diameter.
along the Φ, ϕ2 )
(ϕ1 ,Basically, the mi-
crostructure is formed − − −
from fine grains near the keyhole corresponding to the SZ
Brass (Bs) {111}< 1 12>/{111}<11 2> (90, 55, 45)/(270, 55, and
45) the
grain size increases with increasing distance from − the keyhole center. A significant texture
Copper (Co) {110}<1center
11> is also noticed. The (30, 90, 45)
gradient along the distance from the keyhole evolution of tex-
Goss 1 (G ) {011}<100> (0, 45, 0)
ture is presented in1 the next section. The GOS maps indicate that the fine grains are mostly
Goss 2 (G2 ) {001}<110> (45, 0, 0)
fully recrystallized (having GOS 0–1°) and deformed − grains (having GOS > 2°) appear
Cube (Cu) {001}<0 10> (90, 0, 0)
with increasing distance typically belonging to the TMAZ, followed by large grains
*mostly
{hkl}//(RD, ND) plane
recovered and <uvw>//RD.
(green grains, having GOS 1–2°) belonging to the HAZ, and finally the
microstructure in some places, such as at x = −5 mm (left side) and x = 5 mm (right side)
3.2. Microstructure and Texture Evolution after FSSW
of the lower sheet, is fully recrystallized, which corresponds to the BM. It is interesting to
3.2.1. Microstructure
note that the BM is not Evolution
reachedafter FSSW
in the upper sheet through the entire distance (up to x =
Figures
−5 and 5 mm). 4 and 5 present the evolution of the microstructure via TD-IPF and GOS
maps of the upper and lower sheets as a function of distance from the keyhole center of
the welded Al 5182 alloy. In both sheets and both sides, the TD-IPF maps show that the
microstructure is significantly heterogeneous along the shoulder diameter. Basically, the
microstructure is formed from fine grains near the keyhole corresponding to the SZ and
the grain size increases with increasing distance from the keyhole center. A significant
texture gradient along the distance from the keyhole center is also noticed. The evolution
of texture is presented in the next section. The GOS maps indicate that the fine grains are
mostly fully recrystallized (having GOS 0–1◦ ) and deformed grains (having GOS > 2◦ )
appear with increasing distance typically belonging to the TMAZ, followed by large grains
mostly recovered (green grains, having GOS 1–2◦ ) belonging to the HAZ, and finally the
microstructure in some places, such as at x = −5 mm (left side) and x = 5 mm (right side)
of the lower sheet, is fully recrystallized, which corresponds to the BM. It is interesting
Crystals 2023, 13, 540 7 of 25

Crystals 2023, 13, x FOR PEER REVIEW


to note 7 of
that the BM is not reached in the upper sheet through the entire distance 25 to
(up
x = −5 and 5 mm).

Figure 4. The TD-IPF and GOS maps showing the evolution of the microstructure as a function of
Figure 4. The TD-IPF and GOS maps showing the evolution of the microstructure as a function
distance from the center of the keyhole (left side) at upper sheet (y = 1 mm) and lower sheet (y = 0
ofmm),
distance from the center of the keyhole (left side) at upper sheet (y = 1 mm) and lower sheet
respectively.
(y = 0 mm), respectively.
For more details, the evolution of mean grain size, DRX (GOS 0–1°), recovered or
◦ ), recovered or
partiallymore
For details,
deformed the1–2°)
(GOS evolution of mean(GOS
and deformed grain> 2°)
size, DRX
grain (GOS 0–1
fractions, VLAGBs, LAGBs
partially deformed (GOS 1–2 ◦ ) and deformed ◦
and HAGBs at different locations are shown(GOS > 2 )6.grain
in Figure Based fractions, VLAGBs, LAGBs
on the microstructural
and HAGBsthe
variations, at different locations
different joint zones are shown
in the upperinand Figure
lower6.sheets
Based areon the microstructural
identified and high-
variations, the different joint zones
lighted in the plots shown in Figure 6. in the upper and lower sheets are identified and
highlighted in the
Globally, theplots
uppershown
sheet in Figure
along the6.shoulder diameter is formed of 50% SZ, 41.6%
Globally, the upper sheet along
TMAZ and 8.4% HAZ, while the lower sheet the shoulder diameter
is composed is formed
of 16.7% SZ, 25%ofTMAZ,
50% SZ, 41.6%
41.6%
TMAZ
HAZ and 16.7% BM. Two main differences can be noticed in the weld joints. First, 41.6%
and 8.4% HAZ, while the lower sheet is composed of 16.7% SZ, 25% TMAZ, the
HAZ and 16.7%
deformation BM. Two
is more main differences
pronounced in the uppercan be noticed
sheet in the
than in the weld
lower joints.
sheet First, the
and second
deformation is more evolution
the microstructure pronounced in symmetrical
is not the upper sheet than
at the in the
right andlower sheet
left sides of and second the
the weld.
microstructure evolution can
The first difference is not
be symmetrical
evidenced byat thethe right and
evolution of left sides of the parameters
microstructural weld.
shown in Figure 6. Indeed, the right side of the lower sheet contains the four typical joint
zones: SZ, TMAZ, HAZ and BM. In this area, the mean grain size increases with increasing
distance from the keyhole (SZ and TMAZ) and then saturates when it reaches the HAZ
and BM. The fraction of DRX (GOS 0–1°) decreases with increasing distance from the key-
hole between the SZ and TMAZ and then increases in the HAZ region to reach a high
fraction of about 94% at the BM. It is interesting to note that the HAZ region is character-
ized by a high fraction of partially deformed grains (green grains, GOS 1–2°). The HAGB
fraction decreases with increasing distance and then rapidly increases when it reaches the
Crystals 2023, 13, x FOR PEER REVIEW 8 of 25

Crystals 2023, 13, 540 HAZ and continues to increase at the BM. Consequently, the fractions of VLAGBs and 8 of 25
LAGBs increase between the SZ and TMAZ due to the generation of dislocations and their
rearrangement and then decrease when reaching the HAZ and BM.

Figure 5. The TD-IPF and GOS maps showing the evolution of the microstructure as a function of
Figure 5. The TD-IPF and GOS maps showing the evolution of the microstructure as a function
distance from the center of the keyhole (right side) at upper sheet (y = 1 mm) and lower sheet (y = 0
ofmm),
distance from the center of the keyhole (right side) at upper sheet (y = 1 mm) and lower sheet
respectively.
(y = 0 mm), respectively.
Meanwhile, the evolution of the microstructural features at the right side of the upper
The
sheet, firstasdifference
such can be
the continuous evidenced
decrease in DRXby the
andevolution of microstructural
HAGB fractions parameters
up x = 5 mm, indicates
shown
the presence of only the SZ and TMAZ regions. It seems that the SZ and TMAZ width joint
in Figure 6. Indeed, the right side of the lower sheet contains the four typical is
zones:
largerSZ, TMAZ,
in the upperHAZsheetand
dueBM.to theInextra
this area,
severethe meandeformation
plastic grain size increases
induced by with
theincreasing
down-
distance from
load force of the
the keyhole
shoulder(SZ and TMAZ)
(compression and then saturates when it reaches the HAZ and
deformation).
BM. The fraction of DRX (GOS 0–1 ◦ ) decreases with increasing distance from the keyhole
Concerning the second noted difference, for example, the SZ is not detected at x = −2
between
mm of the thelower
SZ and TMAZ
sheet (Figureand 4)then
sinceincreases in thegrain
the large mean HAZsizeregion
(d = to
11.7reach
µm)aandhighthefraction
low
offraction
about 94% of DRXat the BM. Itrecorded
(15.4%) is interesting
in thistoposition
note that the HAZ
indicate thatregion is characterized
this area belongs to the by a
high fraction ◦ ). The HAGB fraction
TMAZ ratherofthan
partially
the SZ.deformed
Moreover,grainson the(green grains,
left side of theGOS
upper 1–2
sheet, the width of the
decreases
TMAZ (1with mm)increasing distance
is smaller than and
for the thenside
right rapidly
(about increases
2 mm). Thewhen it reaches
change of thethe HAZ
joint weldand
continues to increase
on both sides at the BM.
may indicate thatConsequently,
the right side the fractionsmore
undergoes of VLAGBs and LAGBs
deformation than the increase
left
between
side. Suchthedifferences
SZ and TMAZ coulddue to the generation
be created due to the of dislocations
nature and their
of the stirring rearrangement
process and the
and
toolthen decrease
movement onwhen
both reaching
sides. This theis HAZ
similarand
to BM.
the heterogeneity observed between the
Meanwhile,
advancing the evolution
and retreating sidesof inthe
themicrostructural
conventional FSW features at the
technique right side of the upper
[57].
sheet, such as the continuous decrease in DRX and HAGB fractions up x = 5 mm, indicates
the presence of only the SZ and TMAZ regions. It seems that the SZ and TMAZ width
is larger in the upper sheet due to the extra severe plastic deformation induced by the
download force of the shoulder (compression deformation).
Crystals 2023, 13, x FOR PEER REVIEW 9 of 25
Crystals 2023, 13, 540 9 of 25

Figure
Figure6.6.Evolution
Evolutionof
of (a,d)
(a,d) mean grain size,
mean grain size,(b,e)
(b,e)DRX
DRX(GOS
(GOS0–1
0–1°), partially
◦ ), partially deformed
deformed (GOS
(GOS 1–21–2°)
◦)
and
and deformed (GOS > 2 ) grain fractions and (c,f) grain boundary types (VLAGBs, LAGBs andand
deformed (GOS > 2°)
◦ grain fractions and (c,f) grain boundary types (VLAGBs, LAGBs
HAGBs) as a function of distance from the keyhole center at the upper and lower sheet, respectively.
HAGBs) as a function of distance from the keyhole center at the upper and lower sheet, respectively.

3.2.2. Texture Evolution


Concerning after FSSW
the second noted difference, for example, the SZ is not detected at
−2 mm of
x = Figures 7 and 8 present the(Figure
the lower sheet texture4)evolution
since the via
large mean
{111} thegrain
pole size (d and
figure = 11.7
ODFµm)
sec-
and the
tions at φlow fraction of DRX (15.4%) recorded in this position indicate that this area belongs
2 = 0 and 45° as a function of distance from the center of the keyhole at the upper
to the TMAZ
sheet (y = 1 mm) rather
andthan
lower thesheet
SZ. Moreover,
(y = 0 mm),onrespectively.
the left side ofThe
thepositions
upper sheet, the width
of ideal shearofand
the TMAZ (1 mm) is smaller than for the right side (about 2 mm). The change of the joint
rolling texture components in {111} the pole figure and ODF sections at φ2 = 0 and 45° of
weld on both sides may indicate that the right side undergoes more deformation than the
FCC materials are shown in Figures 2 and 3 and their descriptions are given in Tables 2
left side. Such differences could be created due to the nature of the stirring process and the
and 3, respectively.
tool movement on both sides. This is similar to the heterogeneity observed between the
There isand
advancing theretreating
obvious development of a pronounced
sides in the conventional texture gradient
FSW technique [57]. in the upper and
lower sheets through the distance from the keyhole center. It is clear from Figures 7 and 8
that theTexture
3.2.2. textural characteristics
Evolution after FSSWnear the keyhole (SZ) are typical of simple shear defor-
mation. Then, the texture gradually
Figures 7 and 8 present the texture transforms from
evolution via shear
{111} texture
the pole to typical
figure and ODF plane strain
sections
compression ◦
at ϕ2 = 0 and 45 as a function of distance from the center of the keyhole at the upperand
texture with increasing distance from the keyhole center (TMAZ, HAZ
BM).
sheet (y = 1 mm) and lower sheet (y = 0 mm), respectively. The positions of ideal shear
andBased
rollingontexture
Figurecomponents in {111}
2, the positions theshear
of the pole figure
textureand ODF sections
components at SZ
of the = 0 the
ϕ2 for andleft
45◦ (at
side of FCC
x = −2materials
and −2.5are mm) shown
of theinupper
Figures 2 and
sheet 3 and
show their
that the descriptions
RD-ND plane areisgiven in to
parallel
Tables 2 and 3, respectively.
the SPN-SD plane, while their positions at the right side (at x = 2, 2.5 and 3 mm) change to
the RA-SD plane (RD-ND//RA-SD). For the lower sheet, the shear texture is located only
at the right side (at x = 2 and 2.5 mm) and their positions indicate that the RD-ND plane
is aligned with the RA-SPN plane. The identification of different texture components
through the joints and the positions is complicated; hence, Table 4 summarizes the major
texture components developed in the SZ, TMAZ, HAZ and BM.
Crystals 2023, 13, 540 10 of 25
Crystals 2023, 13, x FOR PEER REVIEW 10 of 25

Crystals 2023, 13, x FOR PEER REVIEW 10 of 25

Figure 7. {111} pole figure and ODF sections at φ2 = 0 and 45° showing the texture evolution as a
7. {111} pole figure andcenter
ODFofsections at ϕ(left ◦ showing the texture evolution as a
Figure
function of distance from the the keyhole 2 =0 andat45upper
side) sheet (y = 1 mm) and lower
Figure 7. {111} pole figure and ODF sections at φ2 = 0 and 45° showing the texture evolution as a
function
sheet (yof=of
distance
0 distancefrom the center of the keyhole (left side) at upper sheet (y = 1 mm) and lower
mm), respectively.
function from the center of the keyhole (left side) at upper sheet (y = 1 mm) and lower
sheet (y (y
sheet = 0= mm),
0 mm),respectively.
respectively.

Figure 8. {111} pole figure and ODF sections at φ2 = 0 and 45° showing the texture evolution as a
function of distance from the center of the keyhole (right side) at upper sheet (y = 1 mm) and lower
Figure 8. {111} pole figure and ODF sections at φ2 = 0 and 45° showing the texture evolution as a
sheet8.(y{111}
=of0 distance
mm),
polerespectively.
figure and ODFofsections at ϕ(right ◦ showing the texture evolution as a
Figure
function from the center the keyhole 2 = 0side)
and at
45upper sheet (y = 1 mm) and lower
function of=distance
sheet (y from the center of the keyhole (right side) at upper sheet (y = 1 mm) and lower
0 mm), respectively.
sheet (y = 0 mm), respectively.
Crystals 2023, 13, 540 11 of 25

There is the obvious development of a pronounced texture gradient in the upper and
lower sheets through the distance from the keyhole center. It is clear from Figures 7 and 8
that the textural characteristics near the keyhole (SZ) are typical of simple shear deformation.
Then, the texture gradually transforms from shear texture to typical plane strain compres-
sion texture with increasing distance from the keyhole center (TMAZ, HAZ and BM).
Based on Figure 2, the positions of the shear texture components of the SZ for the left
side (at x = −2 and −2.5 mm) of the upper sheet show that the RD-ND plane is parallel to
the SPN-SD plane, while their positions at the right side (at x = 2, 2.5 and 3 mm) change to
the RA-SD plane (RD-ND//RA-SD). For the lower sheet, the shear texture is located only
at the right side (at x = 2 and 2.5 mm) and their positions indicate that the RD-ND plane is
aligned with the RA-SPN plane. The identification of different texture components through
the joints and the positions is complicated; hence, Table 4 summarizes the major texture
components developed in the SZ, TMAZ, HAZ and BM.

Table 4. The main texture components developed in different areas of the welded Al 5182 alloy.

SZ TMAZ HAZ BM
Upper sheet
C, B, A, A2∗ , Cu and G1 Co and G1 Cu and G1
Left side —
(at 2–3 mm) (at 3.5–4 mm) (at 5 mm)
C, B, A and G1 Cu, G1 and Bs
Right side — —
(at 2–3 mm) (at 3.5–5 mm)
Lower sheet
Cu, Co and G1 Cu, G1 and Bs Cu and Bs
Left side —
(at 2 mm) (at 2.5–4 mm) (at 5 mm)
A, B, A2∗ and G1 Cu and Bs Cu, G1 and Bs Cu
Right side
(at 2–2.5 mm) (at 3 mm) (at 3.5–4 mm) (at 5 mm)

The texture of the SZ at the upper sheet exhibits the presence of C, A, B, A2∗ , shear
components and recrystallization texture components such as Cube and Goss components.
The SZ of the lower sheet seems to show similar texture evolution except for the absence of
C and Cube components. Local texture inhomogeneity is detected in the SZ. For example,
the texture is gradually rotated about the TD at x = 2 mm (about 10◦ ) and at x = 3 mm (about
30◦ ) from the keyhole center as shown on the right side of the upper sheet (see Figure 8).
The instability of the shear texture of the SZ through the distance is widely reported in
various welded materials and it is explained by the complexity of deformation and strain
heterogeneity induced by the tool geometry [9,18,20–23,32,33,43].
The typical shear texture disappears at the TMAZ regions and is replaced by a typical
texture for plane strain compression with the development of Copper and Brass compo-
nents. It is interesting to note that the recrystallization texture components (Cube and Goss)
are still present in the TMAZ regions. The texture of the HAZ regions is characterized by
the presence of Cube, Goss and Brass (only in the lower sheet) components that are very
similar to the texture of both BMs (Figure 3). The texture differences between the upper
and lower sheets can also be related to the initial texture of both BM sheets (Figure 3).

3.3. Microhardness Evolution


Figure 9 displays the evolution of microhardness as a function of distance from the
keyhole center for the upper and lower sheets, respectively. The SZ, TMAZ, HAZ and BM
regions are highlighted in the microhardness plots. The microhardness of the BM is about
80 HV.
Crystals 2023,
Crystals 13,13,
2023, x FOR
540 PEER REVIEW 12 of 25 12 of 25

Figure 9.Microhardness
Figure 9. Microhardness evolution as aasfunction
evolution of distance
a function from the
of distance fromkeyhole center for:
the keyhole (a) upper
center for: (a) upper
and (b) lower sheet.
and (b) lower sheet.
The highest value of microhardness of about 95 HV is detected in the SZ (at x = 2 mm
4. Discussion
from the keyhole center) of both sheets due to the development of grain refinement. Then,
The evolutiongradually
the microhardness of the microstructure
decreases withand texturedistance
increasing along the shoulder
from dimension
the keyhole along of the
the TMAZ and HAZ regions. The high values of the TMAZ in comparison with
upper and lower sheets of the welded Al 5182 alloy was found to be very heterogeneous those
due to the development of different zones (SZ, TMAZ, HAZ and MB). Below,the
for the HAZ regions can be explained by the increase in dislocation density due to each joint
plastic deformation during the FSSW. The microhardness of the HAZ is similar to the BM
zone of the weld alloy is discussed separately.
in the lower sheet, reaching a value of 80 HV. The range of microhardness variation of
several Al-based alloys is found around 67–110 HV through the SZ, TMAZ, HAZ and BM
4.1. Microstructure and Texture Evolution in Different Joint Zones
regions [58–61].
4.1.1. The SZ Region
4. Discussion
The width of the SZ in the upper sheet coincides with the region where the upper
The evolution of the microstructure and texture along the shoulder dimension of the
and lower sheets are bonded (as can be seen in Figure 1). The grain refinement is very
upper and lower sheets of the welded Al 5182 alloy was found to be very heterogeneous
rapid due to the severe plastic deformation and heating, which makes the identification
due to the development of different zones (SZ, TMAZ, HAZ and MB). Below, each joint
of DRX
zone mechanisms
of the weld alloy isimpossible. However, many investigations demonstrated that, for
discussed separately.
materials with high stacking fault energy such as Al, the continuous DRX (CDRX) mech-
4.1. Microstructure
anism and Texture
is responsible Evolution
for grain in Different
refinement [30].Joint
TheZones
grain size recorded in the SZ of the
4.1.1. The
upper SZ Region
sheet (4.8 µm at x = −2 mm and 5.5 µm at x = 2 mm from the keyhole center) was
Thetowidth
similar that of
forthe
theSZSZin in
thethe
upper sheet
lower coincides
sheet (5.0 µmwith
atthe
x =region
2 mm), where
whichthe may
upperindicate
and that
lower
the sheets are
shoulder bonded
contact on(as
thecan be seen
upper in Figure
sheet does not1). affect
The grain
the refinement is very
grain structure ofrapid
the SZ.
due to themicrostructure
The severe plastic deformation
of the SZand heating,
in the upper which makes
sheet the identification
is characterized by of
anDRX
onion ring
structure resulting from the periodical deposition of material layers. The presence of an
onion ring structure in the SZ is the most characteristic feature of friction stir welds. In
general, the formation of such a specific structure is caused by the rotation of the tool and
the forward movement extrudes the metal around to the retreating side of the tool [40,62–
Crystals 2023, 13, 540 13 of 25

mechanisms impossible. However, many investigations demonstrated that, for materials


with high stacking fault energy such as Al, the continuous DRX (CDRX) mechanism is
responsible for grain refinement [30]. The grain size recorded in the SZ of the upper sheet
(4.8 µm at x = −2 mm and 5.5 µm at x = 2 mm from the keyhole center) was similar to that
for the SZ in the lower sheet (5.0 µm at x = 2 mm), which may indicate that the shoulder
contact on the upper sheet does not affect the grain structure of the SZ.
The microstructure of the SZ in the upper sheet is characterized by an onion ring
structure resulting from the periodical deposition of material layers. The presence of an
onion ring structure in the SZ is the most characteristic feature of friction stir welds. In
general, the formation of such a specific structure is caused by the rotation of the tool and the
forward movement extrudes the metal around to the retreating side of the tool [40,62–66].
It was proposed in the case of the FSW technique that the onion ring structure starts
on the retreating side of the weld and competes with tunnel defects originating at the
advancing side of the weld [63]. Consequently, the formation of a noticeable onion ring
structure indicates fewer tunnel defects [63]. Some investigations showed that the onion
ring structure is more noticeable on the advancing side than on the retreating side of the
weld [63,65]. Principally, the rotation and translation of the tool have the same direction
in the advancing side, which causes an increase in strain and heat, while the rotation
and translation directions are the opposite on the retreating side, which leads to a lower
strain [57]. However, other investigations observed that the onion ring structure was more
located on the retreating side of the weld [40]. The definition of advancing and retreating
sides cannot be used in FSSW since the translation movement is absent. However, it is
obvious that in the present case the onion ring structure is more pronounced on the right
side than on the left side of the upper sheet. The location of the onion ring seems to depend
on the tool geometry and its interaction with the material [40,63].
Figure 10 shows more detailed microstructural and textural examinations of the onion
ring structure formed in the SZ region of the upper sheet located at x = 2 mm (right side)
from the keyhole center. Figure 10 shows the onion ring structure in which the two materials
of the upper and lower sheets are well mixed. However, there is the obvious formation of
large and small bands with a thickness approximately equal to 12.1 and 4.5 µm, respectively.
In addition, the small bands contain fine grains with a mean grain size lower than 4.5 µm,
while the mean grain size of the large bands is higher than 4.5 µm.
The GOS map of the zoomed area shown by the black frame displays that the grains
of the small bands are fully recrystallized, while the majority of the grains belonging to
the large bands are partially or completely deformed. The texture evolution shown by
the ODF sections at ϕ2 = 0 and 45◦ in both bands is slightly different. Moreover, with the
domination of C and Goss components in both bands, grains in the small bands develop a
rotated Cube component (R-Cube {110}<1–10>, (0◦ , 90◦ , 45◦ ). The rotated Cube component
is known as a typical recrystallization texture component often developed in FCC materials,
while the SZ of the lower sheet shows no evidence of an onion ring structure. In addition,
the SZ on the left side of the lower sheet is not detected at 2 mm from the keyhole center,
indicating that the material in this region was not reached by the rotation of the tool.
Crystals 2023,2023,
Crystals 13, x13,
FOR540PEER REVIEW 14 of 25
14 of 25

Figure 10. The TD-IPF maps, GOS map of the zoomed area and ODF sections at φ2 = 0 and 45°
Figure 10. The TD-IPF maps, GOS map of the zoomed area and ODF sections at ϕ2 = 0 and 45◦
showing the microstructure and texture of large and small bands belonging to the onion ring struc-
showing the microstructure and texture of large and small bands belonging to the onion ring structure
ture of SZ region at 2 mm from the center of the keyhole (right side) of the upper sheet, respectively.
of SZ region at 2 mm from the center of the keyhole (right side) of the upper sheet, respectively.

It The
is noteworthy
SZ of the upperthat sheet
the Goss componentbyisthe
is characterized also present in of
development allC,ofBthe
andSZ. The Cube
A com-
component is also detected in the SZ left side of the upper ∗
sheet. In
ponents. In addition, the left side shows the presence of the A2 component. Concerning addition, the R-Cube

is the
detected
lower in the small
sheet, bands (Figure
the shear-type 10).
texture, The presence
formed of A, B andof these texture components
A2 components, is located in the
only on the right side, which is in good agreement with the evolution
SZ has rarely been reported in FSW Al-based alloys [28]. It is well known that the devel-of microstructural
parameters
opment (Figures
of these 5 and
texture 6). In addition,
components the C component
is characteristic seems
of the absent in of
occurrence thestatic
SZ of recrystal-
the
lower sheet compared with the upper sheet. This difference could be related to the local
lization. It seems that the heat generated from tool rotation is high enough to cause static
shear strain. For example, it was reported that the B component transformed into the C
recrystallization. The temperature cycle during the FSSW of AA 5182 recorded at the pe-
component under shoulder rotation [22]. This is seemingly in accordance with the present
riphery
results,ofsince
the the
toolshoulder
(keyhole is border) is shown
not in direct contactinwith
Figure 11. Assheet.
the lower can be
Theseen, the temperature
presence of the
increases
C and A1 /A2 components may indicate that the material has undergone a small value
∗rapidly
∗ up to 320 °C then slowly increases to reach a maximum amount ofof418 °C.
The peak temperature reached is in the range of the recrystallization temperature of the
AA 5xxx series [67–69]. Hence, it is expected that static recrystallization will occur during
the FSSW in which typical recrystallization texture components such as Cube, R-Cube,
Goss and R-Goss can be generated.
Crystals 2023, 13, 540 15 of 25


shear strain, while the development of the B/ B components means that the material has
experienced a high magnitude of shear strain [18,21]. Accordingly, the AA 5182 present
has been subjected to medium shear strain in the SZ.
It is noteworthy that the Goss component is also present in all of the SZ. The Cube
component is also detected in the SZ left side of the upper sheet. In addition, the R-Cube
is detected in the small bands (Figure 10). The presence of these texture components
in the SZ has rarely been reported in FSW Al-based alloys [28]. It is well known that
the development of these texture components is characteristic of the occurrence of static
recrystallization. It seems that the heat generated from tool rotation is high enough to
cause static recrystallization. The temperature cycle during the FSSW of AA 5182 recorded
at the periphery of the tool (keyhole border) is shown in Figure 11. As can be seen, the
temperature increases rapidly up to 320 ◦ C then slowly increases to reach a maximum
value of 418 ◦ C. The peak temperature reached is in the range of the recrystallization
temperature of the AA 5xxx series [67–69]. Hence, it is expected that static recrystallization
Crystals 2023, 13, x FOR PEER REVIEW 15 of 25
will occur during the FSSW in which typical recrystallization texture components such as
Cube, R-Cube, Goss and R-Goss can be generated.

Figure11.
Figure 11. Temperature
Temperature cycle
cycle during
during the
the FSSW
FSSW of
ofAA
AA5182
5182 recorded
recordedat
atthe
theperiphery
periphery of
ofthe
thetool
tool
(keyholeborder)
(keyhole [38].
border)[38].

4.1.2.
4.1.2.The
TheTMAZ
TMAZRegion
Region
The
The width ofthe
width of theTMAZ
TMAZwas wasnot
notthe
thesame
samein inthe
theupper
upperand andlower
lowersheets
sheetsororon
onthe
the
left
left and right sides. The larger width of 1.5 mm (from 3.5 to 5 mm) was located onthe
and right sides. The larger width of 1.5 mm (from 3.5 to 5 mm) was located on the
right
right side
side of
of the upper sheet,
the upper sheet, while
whilethe
thethin
thinwidths
widthsofof0.50.5mmmmand and 1 mm
1 mm were
were located
located on
on the right side (from 2.5 to 3 mm) and left side (from 1.5 to 2.5 mm) of the
the right side (from 2.5 to 3 mm) and left side (from 1.5 to 2.5 mm) of the lower sheet, lower sheet,
respectively.
respectively.This
Thiscould
couldbebeattributed
attributedtotothe
thedownload
downloadforceforceimposed
imposedmainly
mainlyon onthe
theupper
upper
sheet
sheet by the shoulder. The fractions of VLAGBs and HAGBs are higher in this regionin
by the shoulder. The fractions of VLAGBs and HAGBs are higher in this region in
comparison with the SZ and HAZ (Figure 6). The microstructure of the TMAZ near the
comparison with the SZ and HAZ (Figure 6). The microstructure of the TMAZ near the
SZ is mainly characterized by elongated deformed grains (having GOS > 2◦ ) and some
SZ is mainly characterized by elongated deformed grains (having GOS > 2°) and some
small, recrystallized grains (having GOS 0–1◦ ) located at the grain boundaries. This is
small, recrystallized grains (having GOS 0–1°) located at the grain boundaries. This is
characteristic of discontinuous DRX (DDRX) [70]. Examples are shown in the zoomed area
characteristic of discontinuous DRX (DDRX) [70]. Examples are shown in the zoomed area
of regions at −3.5 mm in the upper sheet and −2.0 mm in the lower sheet as indicated
of regions at −3.5 mm in the upper sheet and −2.0 mm in the lower sheet as indicated in
in Figure 12. Most of the grain boundaries (GBs) are serrated due to the difference in
Figure 12. Most of the grain boundaries (GBs) are serrated due to the difference in dislo-
dislocation density between the two sides of the grain boundaries. The misorientation
cation density between the two sides of the grain boundaries. The misorientation between
between the serrated GB and deformed grains increases, leading to the development of
the serrated GB and deformed grains increases, leading to the development of sub-grain
sub-grain boundaries (VLAGBs) that transform into LAGBs and then into small grains
boundaries (VLAGBs) that transform into LAGBs and then into small grains with HAGBs
with HAGBs as indicated by the white arrows in Figure 12. The corresponding {111} pole
as indicated by the white arrows in Figure 12. The corresponding {111} pole figures of
figures of deformed and DRX grains shown in Figure 12 indicate that DRX grains globally
deformed
develop and DRX
a similar grains
texture to shown in Figure
the deformed 12 indicate that DRX grains globally develop
grains.
a similar texture to the deformed grains.
The DRX is very weak in these regions and the deformed grain fraction (GOS > 2°) in
the TMAZ (Figure 6) increases with increasing distance from the keyhole center, demon-
strating that the effect of the heat generated from the tool rotation decreases with increas-
ing distance and hence prevents the occurrence of DRX. The elongated deformed grains
Crystals 2023, 13, x FOR PEER REVIEW 16 of 25

Crystals 2023, 13, 540 16 of 25


(mostly deviated from their ideal positions) observed in the TMAZ region, especially
along the upper sheet (Figure 8).

Figure
Figure 12.12.
TheTheTD-IPF,
TD-IPF,GOS
GOS maps
maps and
andthe
thecorresponding
corresponding {111} polepole
{111} figures of deformed
figures and DRX
of deformed and DRX
grains of TMAZ regions at −3.5 mm (left side) of the upper sheet and at −2 mm (left side) of the
grains of TMAZ regions at −3.5 mm (left side) of the upper sheet and at −2 mm (left side) of the
lower sheet, respectively.
lower sheet, respectively.
4.1.3. The HAZ Region
The DRX is very weak in these regions and the deformed grain fraction (GOS > 2◦ ) in
Details characteristic of the evolution of the microstructure and texture in the HAZ
the TMAZ (Figure 6) increases with increasing distance from the keyhole center, demon-
are not well documented in the literature. The HAZ is defined as a region from the weld
strating that the effect of the heat generated from the tool rotation decreases with increasing
joint in which the microstructure is only affected by the heat generated by the tool; hence,
distance and hence
it is expected prevents
that the the occurrence
microstructure of DRX.
and the texture The
will be elongated
quite similar deformed
to the BMgrains
but are
mostly
with afragmented anddue
larger grain size contain
to theagrain
relatively
growthhigh fraction
process. of VLAGBs
This may explain theand LAGBs
decrease ininside
them (see grains
dislocation 1–5ininthe
density Figure
HAZ12). This istoathe
compared characteristic
BM of naturally of CDRX
aged AA through theNev-
6063 [32]. sub-grain
development (SGD) mechanism
ertheless, experimental [70]. It is evident
results demonstrated that the that
grainthesizestored energy
of the HAZ wasdepends
found toon the
grain orientation.
be lower ForBM
than for the example,
in weldedthealuminum_steel
fraction of LAGBs is higher
joints and this was inexplained
grains 4by andthe5 than
use of 2.
in grain lowSeveral
weldinginvestigations
temperatures [31].
demonstrated the dependency of stored energy on the
In the present
crystallographic case, in
texture theconventional
mean grain size andof the HAZ was
severely very similar
deformed FCCtomaterials
the BM (Figure
[52,71–74].
6) It
butiswith a significant increase in the GOS value; i.e., the majority
worth noting that the SGD mechanism can maintain the orientation of of the HAZ grains arethe de-
partially deformed (green grain, GOS 1–2°), which means the presence of dislocation ac-
formed grains (see grains 2 and 3) or can gradually change the orientation of the subsequent
tivity in the HAZ region compared to the BM.
segments from the original orientation, as can be noticed in grains 1, 4 and 5 in Figure 12.
To quantify the amount of strain (dislocation density) in the HAZ region, the KAM
This explains the persistence of orientations such as Cube and Goss, while the presence of
maps of regions located at x = −3.5 and x = −4 mm from the keyhole center of the lower
thesheet
texture(leftgradient
side) are explains
shown in the development
Figure 13. The KAM of map
complexof BMrolling
(at x = textures
−5 mm) is(mostly deviated
also calcu-
from
lated for comparison and shown in Figure 13. It is obvious that the microstructure of the sheet
their ideal positions) observed in the TMAZ region, especially along the upper
(Figure 8).
Crystals 2023, 13, 540 17 of 25

4.1.3. The HAZ Region


Details characteristic of the evolution of the microstructure and texture in the HAZ
are not well documented in the literature. The HAZ is defined as a region from the weld
joint in which the microstructure is only affected by the heat generated by the tool; hence,
it is expected that the microstructure and the texture will be quite similar to the BM but
with a larger grain size due to the grain growth process. This may explain the decrease
in dislocation density in the HAZ compared to the BM of naturally aged AA 6063 [32].
Nevertheless, experimental results demonstrated that the grain size of the HAZ was found
to be lower than for the BM in welded aluminum_steel joints and this was explained by the
use of low welding temperatures [31].
In the present case, the mean grain size of the HAZ was very similar to the BM
(Figure 6) but with a significant increase in the GOS value; i.e., the majority of the HAZ
grains are partially deformed (green grain, GOS 1–2◦ ), which means the presence of
dislocation activity in the HAZ region compared to the BM.
To quantify the amount of strain (dislocation density) in the HAZ region, the KAM
maps of regions located at x = −3.5 and x = −4 mm from the keyhole center of the lower
sheet (left side) are shown in Figure 13. The KAM map of BM (at x = −5 mm) is also
calculated for comparison and shown in Figure 13. It is obvious that the microstructure
of the HAZ is more deformed than the BM and the deformation increases with increasing
distance from the BM. It seems that the distortion in the HAZ at x = −4 mm started at the
triple junction where sub-grain boundaries with misorientation of 2–5◦ start to accumulate
as indicated by arrows in the grain boundary type map of the zoomed area (red box). Then,
the number of sub-grain boundaries increases and propagates along the entire grain of the
HAZ at x = −3.5 mm as indicated in the zoomed area (yellow box). The dislocation density
was calculated based on Equation (1) and the results are shown in Figure 13. The dislocation
density of the BM is about 6.7 × 1013 m−2 and it increases to 9.3 and 12 × 1013 m−2 at
x = −4 and −3.5 mm, respectively. Such results demonstrate that the HAZ suffers from
some amount of deformation. Further investigations are needed to explore the source of
the strain distribution near the HAZ regions.
In contrast, the texture evolution of the HAZ and BM seems very similar and shows
principally the presence of the Cube, Goss and Brass components (Table 4). The evolution
of the volume fractions of these components is shown in Figure 14. The volume fractions
of the texture components were calculated with an orientation tolerance of 15◦ from their
ideal position. The fraction of the Brass component is similar in the three positions. The
Cube component first increases at x = −4 mm and then decreases at x = −3.5 mm, while
the fraction of the Goss component increases in both HAZ regions.
To identify the orientation of the different grains in both HAZ regions (at x = −3.5
and −4 mm of the lower sheet), their microstructures are partitioned as grains having GOS
values of 0–1◦ , 1–2◦ and >2◦ and their corresponding textures are shown in Figure 15. The
number of grains with GOS 0–1◦ (DRX grains) and GOS >2◦ (deformed grains) were very
low in the region at x = −3.5 and −4 mm, respectively; hence, they were not implemented in
Figure 15. As can be observed, the grains with GOS = 0–1◦ , considered fully recrystallized,
have Cube and rotated Goss (G2 ) orientations. This result explains the decrease in the
Cube texture component in the HAZ at x = −3.5 mm since the DRX is restricted, while
the orientations of grains with GOS = 1–2◦ for both regions change to near Goss and
Brass orientations. The Brass and Goss components are still present in grains with higher
deformation (GOS > 2◦ ). In addition, grains with a new orientation located near the Copper
one, as indicated by its ideal position in the ODF sections, are developed by crystal lattice
rotation induced by slip processing [75]. The Copper orientation is known as a deformation
texture component in FCC materials. In addition, the Copper texture component was
observed in the TMAZ region.
Then, the number of sub-grain boundaries increases and propagates along the entire grain
of the HAZ at x = −3.5 mm as indicated in the zoomed area (yellow box). The dislocation
density was calculated based on Equation (1) and the results are shown in Figure 13. The
dislocation density of the BM is about 6.7 × 1013 m−2 and it increases to 9.3 and 12 × 1013 m−2
at x = −4 and −3.5 mm, respectively. Such results demonstrate that the HAZ suffers from
Crystals 2023, 13, 540 18 of 25
some amount of deformation. Further investigations are needed to explore the source of
the strain distribution near the HAZ regions.

Crystals 2023, 13, x FOR PEER REVIEW


Figure 13. The KAM maps of HAZ regions at −3.5 and −4 mm and BM (at −5 mm) of the lower sheet 18 of 2
Figure 13. The
(left side) KAM
and the maps ofofHAZ
evolution dislocation at −3.5inand
regionsdensity −4regions.
these mm and BM (at −5 mm) of the lower
sheet (left side) and the evolution of dislocation density in these regions.
In contrast, the texture evolution of the HAZ and BM seems very similar and shows
principally the presence of the Cube, Goss and Brass components (Table 4). The evolution
of the volume fractions of these components is shown in Figure 14. The volume fractions
of the texture components were calculated with an orientation tolerance of 15° from their
ideal position. The fraction of the Brass component is similar in the three positions. The
Cube component first increases at x = −4 mm and then decreases at x = −3.5 mm, while the
fraction of the Goss component increases in both HAZ regions.

Figure14.
Figure 14.Evolution
Evolutionof of volume
volume fraction
fraction of Cube,
of Cube, Brass
Brass and and
GossGoss components
components in HAZin at
HAZ at3.5
x=− x = −3.5 an
−4 mm and BM at −5 mm from the keyhole center of the lower sheet (left
and −4 mm and BM at −5 mm from the keyhole center of the lower sheet (left side).side).

To identify the orientation of the different grains in both HAZ regions (at x = −3.5 and
−4 mm of the lower sheet), their microstructures are partitioned as grains having GO
values of 0–1°, 1–2° and >2° and their corresponding textures are shown in Figure 15. Th
number of grains with GOS 0–1° (DRX grains) and GOS >2° (deformed grains) were ver
low in the region at x = −3.5 and −4 mm, respectively; hence, they were not implemented
in Figure 15. As can be observed, the grains with GOS = 0–1°, considered fully recrystal
Crystals2023,
Crystals 2023,13,
13,540
x FOR PEER REVIEW 19 of
of 25
25

Figure 15. The TD-IPF maps and ODF sections at φ2 = 0 and 45° showing the microstructure and
Figure 15. The TD-IPF maps and ODF sections at ϕ2 = 0 and 45◦ showing the microstructure
texture of DRX (GOS 0–1°), partially deformed (GOS −1–2°) and deformed grains (GOS > 2°) of HAZ
and texture of DRX (GOS 0–1◦ ), partially deformed (GOS −1–2◦ ) and deformed grains (GOS > 2◦ )
regions at x = −3.5 and −4 mm from the center of the keyhole (left side) of the lower sheet, respec-
of HAZ regions at x = −3.5 and −4 mm from the center of the keyhole (left side) of the lower
tively.
sheet, respectively.
4.1.4. The BM Region
It is worth noting that the HAZ width of the lower sheet is quite similar on the left
(fromThex = evolution
−2.5 to −of the microstructure
4 mm) and right sides and texture
(from x = revealed
3 to 4 mm)thatand
thethe
BMmicrostructural
was not reached
along
and the shoulder
textural dimension
characteristics (10 mm)
are very in the
similar, upper
which sheet, while
indicates the BM in the
a homogeneous lower
heat sheet
coupled
was the
with detected
sameat x = −5 and
amount 5 mm (the extremity
of deformation of shoulder
input during dimension)
the welding. due to the
Meanwhile, absence
the HAZ
ofthe
in theupper
download
sheetforce of theonly
is located shoulder.
at x = To
−5localize
mm from thethe
BMkeyhole
in the upper
centersheet, additional
(left side). The
EBSD measurements were performed at x = 5.5 and 6 mm (on the left and right
microstructure and texture of this zone are slightly different from those of the lower sheet. sides) from
the example,
For keyhole center, andcomponent
the Brass the corresponding
is absent microstructures
in comparison(TD-IPF
with theandHAZGOSof maps) and
the lower
textures
sheet. This(ODF sectionssince
is expected, at φ2 the
= 0 microstructures
and 45°) are shown of theinBM
Figure 16.upper
of the As can be lower
and seen, the mi-
sheets
crostructures
are and textures
slightly different, at xshown
as already = −5.5 in
and 5.5 mm
Figure 3. still exhibit the characteristics of the
HAZ region and then the BM is attained at x = −6 and 6 mm from the keyhole center.
4.1.4. The BM Region
The evolution of the microstructure and texture revealed that the BM was not reached
along the shoulder dimension (10 mm) in the upper sheet, while the BM in the lower sheet
was detected at x = −5 and 5 mm (the extremity of shoulder dimension) due to the absence
Crystals 2023, 13, 540 20 of 25

of the download force of the shoulder. To localize the BM in the upper sheet, additional
EBSD measurements were performed at x = 5.5 and 6 mm (on the left and right sides) from
the keyhole center, and the corresponding microstructures (TD-IPF and GOS maps) and
textures (ODF sections at ϕ2 = 0 and 45◦ ) are shown in Figure 16. As can be seen, the
Crystals 2023, 13, x FOR PEER REVIEW
microstructures and textures at x = −5.5 and 5.5 mm still exhibit the characteristics20ofofthe
25

HAZ region and then the BM is attained at x = −6 and 6 mm from the keyhole center.

Figure 16. The TD-IFP, GOS maps and ODF sections at φ2 = 0 and 45° showing the evolution of
Figure 16. The TD-IFP, GOS maps and ODF sections at ϕ2 = 0 and 45◦ showing the evolution of
microstructure and texture of regions at 5.5 and 6 mm (left and right sides) from the keyhole center
microstructure and texture of regions at 5.5 and 6 mm (left and right sides) from the keyhole center of
of the upper sheet.
the upper sheet.
4.2. Relationship between Microstructure and Mechanical Properties of the Joint
It is interesting to note that the microhardness difference between the different zones
(SZ, TMAZ and HAZ and BM) is not sharp, which may assure good deformation compat-
ibility between the joint and the BM.
The hardening induced by the deformation processing of materials is generally at-
tributed to the concomitant occurrence of dislocation hardening and grain size hardening
[76]. Based on the microstructural evolution discussed earlier, it can be concluded that the
Crystals 2023, 13, 540 21 of 25

4.2. Relationship between Microstructure and Mechanical Properties of the Joint


It is interesting to note that the microhardness difference between the different zones
(SZ, TMAZ and HAZ and BM) is not sharp, which may assure good deformation compati-
bility between the joint and the BM.
Crystals 2023, 13, x FOR PEER REVIEW The hardening induced by the deformation processing of materials is generally 21 ofat-
25
tributed to the concomitant occurrence of dislocation hardening and grain size harden-
ing [76]. Based on the microstructural evolution discussed earlier, it can be concluded that
the grain size hardening is more important through the joint (BM, HAZ, TMAZ and SZ)
For further analysis, the microhardness values were plotted as a function of the re-
than dislocation hardening.
ciprocal of the square root of the mean grain size for the different (BM, HAZ, TMAZ and
For further analysis, the microhardness values were plotted as a function of the
SZ) welded zones following the Hall–Petch equation [45,46] and the result is shown in
reciprocal of the square root of the mean grain size for the different (BM, HAZ, TMAZ
Figure 17:
and SZ) welded zones following the Hall–Petch equation [45,46] and the result is shown in
Figure 17: 𝑘
𝐻 = 𝐻 k+H (2)
Hv = Hv0 + √ √𝑑 (2)
d
where Hv0 is the friction hardness associated with the resistance of the crystal lattice to the
where Hv0 is the friction hardness associated with the resistance of the crystal lattice to the
movement of dislocations and kH is a Hall–Petch constant, which indicates the contribu-
movement of dislocations and kH is a Hall–Petch constant, which indicates the contribution
tion
of theofgrain
the grain boundaries
boundaries to thetohardening.
the hardening.

Figure17.
Figure 17.Evolution
Evolutionof ofmicrohardness
microhardnessfor fordifferent
differentjoint
jointregions
regions(BM,
(BM,HAZ,
HAZ,TMAZ
TMAZand andSZ)
SZ)of
ofthe
the
AA5182
AA 5182FSSW
FSSWasasa function
a function
of of
thethe inverse
inverse of the
of the square
square rootroot of the
of the mean
mean grain
grain size size representing
representing the
the Hall–Petch
Hall–Petch relationship.
relationship.

Ascan
As canbebenoticed,
noticed,Figure
Figure1717 demonstrates
demonstrates thethe validation
validation of the
of the Hall–Petch
Hall–Petch relation-
relationship.
ship.
The The extrapolated
extrapolated value
value for thefor the friction
friction hardness
hardness and slopeandofslope of the Hall–Petch
the Hall–Petch equation
equation gives
gives values
values of Hv0 of Hv0 =HV
= 63.8 63.8 HV
and kHand kH =HV
= 68.1 68.1µm
HV1/2µm 1/2, respectively.
, respectively.
Indeed, the
Indeed, theSZSZisishighly
highlydeformed
deformedbut butgrain
grainrefinement
refinementoccurs
occursby byDRX
DRXwhere
wherethe the
dislocations gradually transform into HAGB. The evolution of the
dislocations gradually transform into HAGB. The evolution of the microstructure of themicrostructure of the
HAZand
HAZ andBMBMregions
regionsshows
showsalready
alreadyweakweakdislocation
dislocationdensity.
density.Nevertheless,
Nevertheless,ititseems
seemsthatthat
thevalues
the valuesforforthe
theTMAZ
TMAZslightly
slightlydeviate
deviatecompared
comparedto tothose
thosefor
forthe
theHAZ
HAZandandSZSZdueduetoto
the
thepresence
presenceof ofdeformation
deformationfeatures
featuresas asdiscussed
discussedin inSection
Section4.1.2.
4.1.2.In
Inthis
thiszone,
zone,ititcan
canbebe
assumed
assumedthatthatgrain
grainsize
sizeand
anddislocation
dislocation density
density simultaneously
simultaneously participate in the
participate hardening
in the harden-
of theofTMAZ
ing region.
the TMAZ region.

5. Conclusions
• Local microstructure and texture were evidenced in the upper and lower sheets
through the shoulder dimension (10 mm) during the FSSW of the AA 5182 alloy.
• The upper sheet was mainly composed of the SZ and TMAZ due to the high defor-
mation induced simultaneously by the tool rotation (shear deformation) and the
shoulder download force (compression deformation), while the lower sheet was
formed of the SZ, TMAZ, HAZ and BM due to the limited effect of the shoulder on
the lower sheet.
Crystals 2023, 13, 540 22 of 25

5. Conclusions
• Local microstructure and texture were evidenced in the upper and lower sheets
through the shoulder dimension (10 mm) during the FSSW of the AA 5182 alloy.
• The upper sheet was mainly composed of the SZ and TMAZ due to the high deforma-
tion induced simultaneously by the tool rotation (shear deformation) and the shoulder
download force (compression deformation), while the lower sheet was formed of the
SZ, TMAZ, HAZ and BM due to the limited effect of the shoulder on the lower sheet.
• The change of the joint weld indicated that the right side undergoes more deformation
than the left side.
• The formation of texture gradients is observed through the distance from the keyhole
center, from shear-type texture at the SZ to plane strain compression deformation type
texture at the TMAZ and then recrystallization texture at the HAZ and BM.
• The high temperature produced during FSSW seemed the origin of the development
of recrystallization texture components such as Cube, Rotated-Cube, Goss and Rotated
Goss in the SZ.
• Grain fragmentation and DDRX were evidenced in the TMAZ regions.
• The KAM approach demonstrated that the HAZ regions exhibit higher dislocation
density than BM.
• The microhardness gradually decreases with increasing distance from the keyhole
along the SZ, TMAZ and HAZ regions. However, the microhardness difference
between the different zones is rather small, which may assure good deformation
compatibility between the joint and the BM.
• The Hall–Petch constant was found valid through the weld zones with the fitting
parameters Hv0 = 63.8 HV and kH = 68.1 HV µm1/2 .

Author Contributions: T.B.: conceptualization, methodology, validation, writing—original draft


preparation, S.B.: conceptualization, investigation, F.B.: methodology, software, H.A.: conceptual-
ization, validation, writing—original draft preparation writing—reviewing and editing. All authors
have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Data Availability Statement: The data presented in this study are available on request from the
corresponding author.
Conflicts of Interest: The authors declare no conflict of interest.

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