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Rania M. El-Shorbagy
Mining, Petroleum and Metallurgy Department, Faculty of Engineering, Cairo University, Giza 12613, Egypt
Z. M. El-Baradie
Central Metallurgical Research and Development Institute (CMRDI), Helwan, Cairo, Egypt
Ahmed I. Abdel-Aziz
Mechanical Engineering Department, Faculty of Engineering, Fayoum University, Fayoum, Egypt
Abstract
Friction stir processing (FSP) is the most effective severe different conditions (homogenized and stir friction) were
plastic deformation process for creating materials with examined by optical and scan microscopes attached with
very fine grains and good properties. The target of the EDS and Map analyzer. At the same time, a tensile test was
present research is to investigate the influence of FSP on conducted to assess the mechanical properties. The find-
the microstructure and mechanical properties of homoge- ings indicated that the microstructures were significantly
nized 2024 aluminum alloy with and without rare-earth refined after adding RE (Ce ? La) or applying the TMT
(RE) and thermomechanically treated conditions (TMT). technique. Whereas, the microstructures were greatly
The rare-earth elements used were Ce and La in the form improved after applying FSP to both conditions. Ultra-fine
of a master alloy containing (50% Ce ? 50% La). The grains were observed for both TMT and RE-containing
casting of 2024 aluminum alloys, both with and without alloys after FSP. On the other hand, the results of
(Ce ? La), was carried out using the conventional stir cast mechanical properties were significantly increased after
technique. Part of the obtained alloys was homogenized, applying multiple passes of FSP. The optimum results were
whereas the other part was thermomechanically treated obtained when two passes of stir friction were applied to
(TMT). The homogenized 2024 material was exposed to the TMT alloy condition.
FSP with multiple passes (one, two, and three) to obtain
the suitable pass number. After that, the best pass number Keywords: friction stir processing, aluminum alloy,
was performed on the 2024 aluminum alloy refined with RE casting, microstructure, tensile properties
(Ce ? La) and TMT materials. The microstructures in
2024 alloy 4.28 1.5 0.59 0.27 0.4 0.09 0.04 – Bal.
Alloy refined with (Ce ? La) 4.19 1.52 0.57 0.23 0.3 0.11 0.02 1 Bal.
Standard 2024 3.8–4.9 1.2–1.8 0.3–0.9 0.5 0.5 0.1 0.15 Bal.
Max. Max. Max. Max.
alloys were subjected to homogenization treatment at 500 perpendicular to the traverse direction of the tool. The
°C for 4 hours and then, cooled in air. specimens were polished and ground according to stan-
dard metallographic procedures. Then, the samples in dif-
ferent conditions (homogenized, TMT, and stir friction)
Friction Stir Process were etched with Kroll’s reagent (192 ml H2O, 6 ml HNO3,
and 2 ml HF). The metallographic studies were executed
Part of the homogenized 2024 Al alloy was thermome- using optical and scan microscopes, and phase analyzer
chanically treated. At the same time, the other part was EDS spectroscopy. The average grain size of each sample
subjected to FSP in the air with different passes (one, two, was measured by the linear intercept method. X-ray
and three passes) to obtain a suitable pass number condi- diffraction analysis for 2024 alloys with and without RE
tion. After that, the obtained pass condition was performed elements was carried out using an ‘‘X, PERT PRO’’
on the 2024 aluminum alloy modified with (Ce and La) rare machine with a Cu Ka target.
earth elements and also on the TMT alloy condition. The
homogenized plates were sectioned into 150 mm x 100 mm
x 4 mm plates for FSP using a wire-cutting machine. The Tensile Testing
plates were processed using a vertical milling machine at a
fixed distance. The cylindrical pin profile of the H13 (52 Tensile samples were taken away from homogenized alloys
HRC) steel processing tool had a flat surface. The pin has with and without RE (Ce and La) addition and TMT alloy.
dimensions of 4 mm diameter, 5 mm height, and 18 mm The FSP tensile samples, however, were taken from the
diameter shoulder, Figure 2a. A shoulder with a zero-tilt processed zone parallel to its longitudinal axis. So, the
angle was used. 80 mm/min tool’s travel speed and 1000 specimen gauge length must be from the stir zone. Wire-
rpm rotational speed were used in this work. The headpin cutting machine was used to fabricate these specimens.
was inserted into the workpiece until the sheet’s top surface Figure 3a and b provides the tensile specimen’s dimensions
was in contact with the shoulder of the headpin. The and schematic of the longitudinal tensile test specimen.
rotation axis of the tool was perpendicular to the work- Figure 3c represents the position of a tensile sample on the
piece’s top surface. A linear path was followed by the tool. stir zone. The tensile tests were performed at room tem-
Each pass was carried out with 100% overlap. During FSP, perature. A testing apparatus with a 10 KN capacity and a
the multi-pass technique was employed to introduce uni- constant cross-head speed of 0.3 mm/min was used in this
form deformation to the stir zone. In the first pass, the pin work.
was rotated clockwise, and anticlockwise in return pass.
The linear path of the tool was carried out along the whole
length of the plate, and the second pass was subjected Results and Discussion
completely to all the stir zone area. Then, the plate was
cooled to room temperature in the air. Figure 2b revised the Microstructure Examination
schematic of the FSP used in this study, Figure 2c shows
the FSP equipment with a sample, and Figure 2d shows the Microstructure of Base Metal
sample prepared.
The surface of homogenized plates 2024 with and without
RE (Ce and La) was prepared for microstructure exami-
Microstructure Characterization nations. Optical and SEM micrographs of homogenized
plate surface 2024 aluminum alloy are shown in Figure 4.
For microstructural observations, specimens from homog- The microstructure mainly displays coarse grains of a-solid
enized plates 2024 with and without RE (Ce and La) ele- solution matrix (the bright contrast) along with inter-
ments and TMT were subjected to a metallographic metallic phases. These intermetallic phases are precipitated
procedure. Meanwhile, cutting was applied on FSP samples at grain boundaries (GB) and have different morphologies
(the dark contrast). Some of these intermetallic phases
(Al2Cu and Al2CuMg) have a coarse plate-like morphol- macrostructure of the cross section perpendicular to the
ogy. Meanwhile, Chinese script morphology is recognized tool traverse direction of the specimen. It was observed that
in the phase containing Fe. The average grain size is about the processed zone is clearly visible. A confined boundary
55 lm. A fine microstructure is observed by adding Ce and of the processed zone distinguishes it from other regions. It
La RE elements. Also, as shown in Figure 5, fine precipi- can be shown that the depth of the stir zone is approxi-
tates at GB are indicated. At the same time, the AlCuM- mately 1.5 mm.
gRE-containing phase is recognized in the shape of plates.
The typical grain size is approximately 30 lm. On the other The microstructure underwent a significant change during
hand, the microstructure of the TMT, Figure 6, appears as the FSP, as shown by Figures 9, 10, and 11. As seen in
elongated grains parallel to the direction of rolling. While Figure 9, the parent material’s coarse grains have been
the morphology of plate-like precipitates was completely replaced by nearly equiaxed fine grains after the first pass
changed to fine particles. The XRD analysis of this alloy of the FSP. The tool pin rotates at the material surface
indicates the presence of these intermetallic phases, during FSP. The mixture has to flow around the tool pin as
Figure 7. a result of the stirring action. During the action of the
traverse tool, the materials move to the back of the pin and
cause plastic deformation. As the tool moves across the
Macro- and Microstructure After FSP surface of the workpiece, the alloy is subjected to severe
breaking, and the precipitates are redistributed beneath the
Figure 8 shows the surface of the processed sample After tool.21 While, compared to the base metal, the
FSP passes. After processing, samples are extracted from microstructure after the second pass, Figure 10, reveals an
the surface of the stir-processed zone for microstructure increased number of small recrystallized grains and a sig-
examination (Figure 8a at location 1). Figure 8b shows the nificant amount of GB precipitations. These findings
Figure 5. Homogenized alloy with RE elements (Ce and La) (a) Optical, (b) SEM.
Figure 7. XRD pattern of the (a) 2024 homogenized sample and (b) Alloy refined with
Ce and La RE elements.
Figure 9. Homogenized alloy after one pass FSP, (a) Optical, (b) SEM.
Figure 10. Homogenized alloy after two passes FSP, (a) Optical, (b) SEM.
Figure 11. Homogenized alloy after three passes FSP, (a) Optical, (b) SEM.
Figure 12. Alloy with RE elements after two passes FSP, (a) Optical, (b) SEM.
After FSP, more homogeneity in the distribution of the value of UTS, YS and ductility for homogenized condition
alloying elements is clearly evident, especially in alloy were mainly a result of coarse grains and the grain
refined with (Ce ? La) after two passes. It can be con- boundary secondary phases. It was noted that multi-pass
cluded that the alloying elements dissolute during FSP and FSP improved mechanical characteristics. This enhance-
then re-precipitate as one phase with different composition. ment was credited to both homogeneous multi-pass pro-
cessed regions and uniformly fine precipitate distribution in
the matrix. It was demonstrated that the tool rotation speed
Tensile Properties significantly influences mechanical properties and
microstructure refinement as a result of higher heat input,
Figure 16 displays yield strength (YS) and ultimate tensile causing the rotating tool pin’s softening and intense stirring
strength (UTS) of homogenized and FSP alloys. The FSP action. This causes better grain refinement, leading to
tensile samples were taken from the stir processed zone in improved mechanical properties.27–30 According to Mishra
longitudinal direction (Figure 2b). The tensile test results et al.31, FSP increases strength and elongation by
are the average of three test specimens. For 2024 homog- decreasing the porosity content of the homogenized sam-
enized alloy, the YS and UTS were 92 and 147 MPa, ple. While GP-precipitates dissolution and coarse S-phase
respectively (Table 2). After FSP, the tensile properties formation are the causes of decreasing UTS, YS, and
significantly improved. After one-pass FSP, the YS and ductility in the three-pass sample compared to the two-pass
UTS increased with ratio up to 30 % and 72% more than FSP sample. It should be observed that the three-pass
the homogenized alloy, respectively. Meanwhile, after two sample exhibits greater effects of GP-precipitation disso-
passes of FSP, UTS experienced a twofold increase com- lution and coarsening of S-phase particles than two passes
pared to the homogenized material, whereas the YS specimen. This may be related to heat input resulting
increased by up to 53%. It was demonstrated that the through FSP in three passes sample. According to Bousqet
improvement was occurred due to grain refinement in the et al.32, the reduction in hardness during the FSP of Al
microstructure with increases the passes number. On the 2024 alloy is related to S-phase coarsening. Adding Ce and
other hand, after three passes of FSP, even though the La to the 2024 alloy resulted in increasing the tensile
tensile properties are significantly improved compared to properties. Compared with the conventional alloy, the
they were in the homogenized condition, the UTS UTS, YS and elongation increased by 6, 15 and 33%,
decreased by 13%, while YS decreased by 28% compared respectively. The grain refinement occurred due to addition
with the two passes condition. The elongation percent of of Ce and La additives can be attributed to the grain growth
homogenized and FSP alloys is shown in Figure 17. The restriction by RE additives in solid solution. The RE ele-
homogenized alloy has 4.5% elongation. The ductility ments act as nucleation sites leading to grain growth
significantly increased under the FSP conditions. After inhibiting. The fine precipitates not only affect the diffu-
one-pass FSP, the elongation increased to 8%. The elon- sion of the atom in the alloy but also restrict the movement
gation increased to 16% after two FSP passes, which was of the interfaces. Thus, it will act as an obstacle for the
threefold higher than that of homogenized one. On the grain to grow. Grain boundaries are effective delphinium to
other hand, after three passes of FSP, although there is a the dislocation motion, and therefore small grained mate-
significant improvement in the elongation value than the rials will have higher grain boundaries density per unit
homogenized alloy, the elongation decreased to 12% volume.20 Thus, the decreasing of grain size leads to
compared with the two-pass FSP condition. The reduced increasing the tensile strength. After the application of
Table 2. UTS, YS and % Elongation for Different Meanwhile, the UTS and YS increased by 46 and 58 %,
Specimens respectively, while ductility decreased compared with the
alloy before FSP. The presence of fine-sized particles in the
Specimen YS (MPa) UTS (MPa) % microstructure resulting from FSP is responsible for the
elongation
enhancement in tensile properties.
2024 alloy 92.33±5.86 147.37±8.85 4.53±0.96
Alloy after one 120.33±8.01 253.00±8.54 8.07±1.25
pass Conclusions
Alloy after two 141.00±6.00 329.33±9.50 16.12±0.85
pass
The current investigation carefully examines the multi-pass FSP
effect on microstructure and mechanical characteristics of 2024
Alloy after three 110.30±7.11 290.40±5.61 12.08±1.68
aluminum alloy with and without (Ce ? La) or applying TMT
pass
technique. The conclusions are outlined as follows:
Alloy with (Ce ? 106.00±7.55 156.17±6.39 6.18±1.09
La)
1. Incorporating RE (Ce ? La) elements into the
Alloy with (Ce ? 156.20±5.80 337.33±6.56 14.08±1.39 alloy or employing TMT leads to microstructure
La) after two
refinement and improved mechanical properties.
pass FSP
2. FSP significantly enhances the microstructure, pre-
TMT alloy 120.23±5.96 260.20±6.10 28.49±1.12 cipitate morphologies, and mechanical properties of
TMT alloy after 190.03±8.47 380.00±5.36 25.08±1.05 homogenized aluminum 2024 alloy, regardless of
two pass FSP whether RE addition or TMT alloy is utilized.
3. The microstructure refinement in the processed
zone is prominently observed with two passes of
FSP, a substantial enhancement in tensile properties was FSP, featuring a finer structure and a more even
achieved. YS increased by 47% while UTS and elongation distribution of alloying elements.
increased up to 2 times compared with the alloy before 4. The mechanical properties are improved by two
FSP. This enhancement in mechanical properties is due to passes of FSP. This improvement is a result of the
the maximum refining in microstructure and the modifi- uniform processed region achieved through mul-
cation of the morphological of the Chinese script and plate- ti-pass FSP and the even dispersion of ultra-fine
like phases. On the other hand, TMT condition reveals the precipitates within the matrix.
maximum tensile properties. The UTS and YS increased by 5. The optimum combination of microstructure and
76 and 30%, respectively, and increased more than 6 times mechanical properties is revealed for the TMT
for ductility compared with the conventional alloy. alloy after applying two passes FSP technique.
Acknowledgements use, you will need to obtain permission directly from the copyright
holder. To view a copy of this licence, visit http://creativecommons.
This research was financially supported by CMRDI org/licenses/by/4.0/.
Fund, Egypt, Project Grant No. ID: 1/2022-2023. The
authors thank everyone who contributed to conducting
the experiments for this research, Prof. Ahmed Ismail REFERENCES
Plastic Deformation dept., Eng. Ahmed Abdel-Meguid,
and technician Mahmoud Shehata Non-Ferrous dept 1. J. Joel, P. Jeyapandiarajan, A. Xavior, R. Harshitha, R.
CMRDI. Sreekumar, P. Raju, Surface modification of hBN
reinforced aluminum alloy Al 2024 through friction stir
Funding processing. J. Phys. Conf. Ser. 2198, 012047 (2022).
https://doi.org/10.1088/1742-6596/2198/1/012047
Open access funding provided by The Science, Technol- 2. M. Regev, S. Spigarelli, Study of mechanical,
ogy & Innovation Funding Authority (STDF) in microstructural and thermal stability properties of
cooperation with The Egyptian Knowledge Bank friction stir processed aluminum 2024-T3 alloy.
(EKB). Kovove Mater. 57, 229–236 (2019). https://doi.org/10.
4149/km-2019-4-229
Data Availability 3. N. Sun, D. Apelian, Friction stir processing of
aluminum alloy A206: part II- tensile and fatigue
On reasonable request, the corresponding author will properties. Int. J. Metalcast. 13(2), 244–254 (2019).
provide the information supporting the study’s conclu- https://doi.org/10.1007/s40962-018-0268-6
sions. 4. S. Caizhi, L. Hui, W. Feng et al., Study on the
microstructure and mechanical properties of ZrB2/
Conflict of interest There are no conflicts of interest, according to AA6111 particle-reinforced aluminum matrix com-
the authors.
posites by friction stir processing and heat treatment.
Ethical Approval None of the authors of this article conducted any Int. J. Metalcast. (2023). https://doi.org/10.1007/
studies on animals. Furthermore, none of the authors’ studies s40962-023-01029-2
involving human subjects are included. 5. I.G. Papantoniou, P. Karmiris-Obratański, B. Leszc-
zyńska-Madej, D.E. Manolakos, The effect of friction
Open Access This article is licensed under a Creative Commons stir processing on the hydrogen susceptibility of
Attribution 4.0 International License, which permits use, sharing,
adaptation, distribution and reproduction in any medium or format, as
AA5083 specimens after hydrogen cathodic charging.
long as you give appropriate credit to the original author(s) and the Int. J. Adv. Manuf. Technol. 125, 4399–4413 (2023).
source, provide a link to the Creative Commons licence, and indicate https://doi.org/10.1007/s00170-023-10971-8
if changes were made. The images or other third party material in this 6. N. Sun, D. Apelian, Friction stir processing of
article are included in the article’s Creative Commons licence, unless aluminum alloy A206: part I- microstructure evolu-
indicated otherwise in a credit line to the material. If material is not tion. Int. J. Metalcast. 13(2), 234–243 (2019). https://
included in the article’s Creative Commons licence and your intended
use is not permitted by statutory regulation or exceeds the permitted doi.org/10.1007/s40962-018-0263-y