1. Introduction
Al-Mg alloys are well-known structural materials that are widely used in various applications including those where welding is a single option joining method. Improving the Al-Mg alloy strength characteristics is achieved by alloying the metals with scandium and zirconium [
1,
2,
3,
4], which makes them hereditary fine-grained alloys while retaining their corrosion resistance [
2,
5].
The alloy fine-grained microstructure is stabilized by the precipitation of nanosized Al
6Mn, Al
3Sc, and Al
3(Sc,Zr) matrix coherent particles, which first precipitate from a solid solution and then have a pinning effect on the grain boundaries so that even annealing at 723 K for 16 h does not increase the grain size [
6]. The Al
3Sc precipitates are the most effective precipitates for pinning the grain boundaries [
7]. It is known also [
8] that the nanosized Al
3Sc precipitates are stable against coalescence so that that their mean diameter increased only from 13.5 to 15.4 nm for 7 days at 350 °C.
Friction stir welding (FSW) is a method used for joining metals in a solid state and is, therefore, often used on metals and alloys that cannot be welded using any fusion welding technique. An Al-Mg-Sc-Zr alloy is an example of such a hardly weldable alloy that and is, therefore, a candidate for joining with friction stir welding. It is common knowledge that this solid state joining method usually forms a fine-grained microstructure in the stirring zone. The presence of the nanosized growth inhibitors in Al-Mg-Sc-Zr is an extra factor that helps retaining the fine-grained structure of the welded metal and thus improving its mechanical characteristics [
9]. For example, it was reported [
10] that FSW increased the ultimate and yield stresses of the Sc + Zr-alloyed aluminum alloy by 23.8 and 11.9%, respectively. Practically a 100% tensile strength was achieved on the Al-5.4Mg-0.2Sc-0.1Zr alloy FSW seam even after annealing [
11]. The mechanical strength advantage of the FSW joint compared to that of the TIG on the Al-Mg-Sc-Zr alloy was thus demonstrated [
10].
Another positive factor of the FSW-generated fine-grained structure is its potential to take advantage of superplasticity characteristics [
12,
13,
14,
15,
16] that allow up to 2000% elongation while retaining microstructural thermal stability at 450 °C [
12].
The effect of Al
3Sc and Al
3(Sc,Zr) nanosized precipitates on pinning the fatigue crack tip was also reported [
17]. It was shown [
18] that friction stir processing improves the corrosion resistance of Al-Mg alloys in a NaCl aqueous solution.
An important problem in FSW is obtaining a flawless and reliable seam when joining thick sheets. The inhomogeneity and efficiency of metal stirring, enhanced adhesion of metal to the FSW tool, diffusion-controlled FSW tool wear, fast heat removal, and high mechanical loads are factors that aggravate the problems commonly encountered with FSW on aluminum alloy sheets up to 10 mm thickness. Some technologies require welding heavy gauge sheets or pipes, which then are then machined to obtain the final structure. This requirement makes it necessary to study FSW seams on heavy gauge workpieces.
It may be concluded, therefore, that Al-Mg-Sc and Al-Mg-Sc-Zr alloys not only possess high mechanical characteristics and are weldable using FSW but also that their characteristics can be further improved using FSW, which is a promising research field from both practical and scientific points of view.
The severe thermomechanical impact of FSW on the plasticized aluminum alloy in the stirring zone creates the conditions for the strain-induced dissolution of particles, thereby enriching the solid solution with the alloying elements and facilitating the fast precipitation of particles. This is an element of FSW aspect that has not received much attention in the literature, especially when taking into account the dynamic character of dissolution/precipitation, as well as recrystallization, during the process. This issue becomes even more intriguing when applying FSW to an Al-Mg-Sc-Zr alloy, whose microstructure is known to have high temperature stability. The FSW joint structure formation is determined by the specificity of metal transfer and the role played by the adhesion of plasticized metal to the FSW tool.
The objective of this paper is to study the microstructures and mechanical characteristics of the FSW joint zones obtained on heavy gauge Al-Mg-Sc-Zr alloy sheets.
2. Materials and Methods
Hot-rolled 30 and 35 mm thick 300 mm × 300 mm sheets of AA1570 and HSS M2 steel FSW tools were used to carry out friction stir welding using an FSP machine PowerStir 345C (Holroyd Precision Ltd., Milnrow, UK) at the facilities of S.P. Korolev RSC Energia Experimental Machine-building Plant ZEM. The shape and parameters of the tools used for the welding are shown in
Figure 1. The process parameters were adjusted experimentally to obtain the FSW joints, as shown in
Figure 1. The FSW tool rotation rate, traverse speed, and plunging force were 600 RPM, 10 mm/min, and 40 kN, respectively. The FSW seam can be divided into three zones as shown in
Figure 1a, where zones B, S, and H denote the FSW tool plunging zone characterized by insufficient heating plasticization, steady welding, and the FSW tool exit zone, respectively.
The stop-action technique [
19] was applied to study the mechanical behavior of the metal in the thermomechanically affected zones (TMAZs) when the FSW tool exit hole was sectioned and then marked as shown in
Figure 2. Another series of metallographic views was obtained by EDM cutting the seam by planes normal to the sheet surface and both perpendicular and parallel to the FSW joint line. An EDM cutting machine DK7745 (Suzhou Simos CNC Technology Co., Ltd. Suzhou, China) was used to cut off the samples, which were then ground, polished, and etched to prepare the metallographic section views.
The joint strength was tested using a test machine BISS UT-04-0100 (BISS (P) Ltd. Bangalore, India) on samples cut off the seam by a plane perpendicular to the tool travel direction at different distances below the top surface so that the stir zone was located in the middle of the sample’s gauge length part (
Figure 1). The loading speed was 100 mm/s.
A microstructural examination was performed using optical microscopes Altami MET 1T(Altami Ltd., Saint-Petersburg, Russia), Olympus OLK41102 (Olympus Corp, Tokio, Japan), SEM and TEM instruments Tescan VEGA 3 (TESCAN ORSAY HOLDING, BRNO, Czech Republic), Zeiss LEO EVO 50 (Carl Zeiss AG, Oberkochen Germany), and JEOL JEM-2100 (JEOL Ltd., Akishima, Japan).
Thin foils for TEM were prepared using EDM cutting, mechanical polishing, and ion thinning to represent the stir zone metal in two perpendicular sections with respect to the joint line. A microhardness tester Duramin-5 (Struers A/S, Ballerup, Danemark) was used to obtain microhardness profiles across the FSW seam zones at a 490 mN load.
4. Discussion
The stir zone formation in high thickness materials may occur in a very complex multiflow manner so that a number of vortex structures with different configurations forms there, partially due to the low pressure in the welding zone. As a result, a welded joint has, in addition to structural irregularities, significant differences in its mechanical properties with respect to the distance below the top surface. Despite the presence of structural irregularities, it is possible to accurately characterize the process of the welded joint formation in the tool pin stir zone (excluding the area of shoulders influence). As described above, the direct material transfer by the tool is predefined by the primary subdivision of the base metal grains through severe plastic deformation with the formation of a wide thermomechanically affected zone (
Figure 5). The grain size is expected to increase with distance from the stir zone to the heat-affected zone (
Figure 8). The different widths of the TMAZ at different levels of the weld indicates that the process of grain subdivision and, consequently, the formation of the material transfer layer (
Figure 14 and
Figure 15) occurs with a different intensity depending on the distance below the top surface. This ensures that the stir zone consists of several nuggets and makes the material transfer frequency potentially differ from level to level. This irregularity in the adhesive interaction also likely affects the mechanical characteristics. However, the peculiarities of the formation of structures at each of the studied weld levels demonstrate that the welded joint formation in the tool pin stir zone occurs via the same mechanism.
The results obtained in this work, as well as those obtained earlier, suggest that FSW seam formation occurs according to the scheme shown in
Figure 16.
After plunging the FSW tool into a metal, the tool starts travelling along the joint line. The plasticized and grain refined metal layer is transferred by the rotating tool to the trailing zone where it is detached from the tool and sticks back to the hot metal deposited. This cycle is repeated again and again to form the welded seam. The transferred layer thickness is determined by the temperature and shear stress/strain gradients exerted from the tool into the base metal. This model was inferred from numerous experiments on unlubricated and adhesion controlled sliding friction when direct and reversed metal transfer occurs between the contacting bodies [
20,
21,
22].
This discontinuous transfer mechanism is responsible for the formation of inhomogeneous grain structures, SZ nuggets, and the TMAZ. An overly strong adhesion of the plasticized metal to the FSW tool may have detrimental effects on the stirring and metal flow efficiency. The transferred portion of metal may not detach from the tool surface and thus be involved in the next cycle, thus breaking the regularity of transfer and forming additional metal flows, which can then provide the final multi-nugget pattern shown in this work in
Figure 3c,d. This is especially likely in FSW on thick metal sheets with high pressure and tool travel resistance.
On the other hand, overly weak adhesion would not allow the metal to form a welded joint at all. Therefore, the adhesion of the metal to the tool is an important factor in metal transfer, which has never been considered in modeling. It is known, for example, that it is possible to obtain an FSW seam using an absolutely smooth FSW pin surface [
23,
24] and that it is the adhesion that works here to help transfer the metal.
Our results show that the SZ metal precipitates are not coherent with the Al-Mg matrix; thus, grain structure recrystallization is not stopped and continues by means of grain boundary migration and diffusion-controlled dissolution of the incoherent precipitates, leading to numerous dislocation loops forming in the metal. It is known that the dislocation loops can appear by a vacancy condensation mechanism in diffusion on the grain boundaries. It seems that the coarse precipitates almost have no pinning effect of the grain boundaries so that grains may grow as large as several micrometers. Severe deformation and heating during FSW facilitates strain dissolution of the initial precipitates that, consequently, have to precipitate again. Intense stirring in the SZ dissolves them again and again until stirring is stopped and the metal comes to rest. This is where precipitation overtakes dissolution, and precipitates grow very quickly on the defective structure. That is why the coarsest precipitates are found in the TMAZ (
Figure 3), where the strain is low and some particles are hiding there and thus avoid the strain dissolution. In addition,
Figure 8a shows that some grain growth can occur in the vicinity of the SZ/TMAZ boundary. This finding can be explained by the same reason, i.e., that the coarse incoherent precipitates are formed in the TMAZ and allow the grains to grow. Nevertheless, even if the precipitates are semicoherent, they may still retain some pinning effects on the grain boundaries.
The TMAZ zone is characterized by kinked grains (
Figure 4d), which are the results of deformation under the pressure exerted by the FSW tool. A similar effect was observed under compression deformation of the Al-Mg-Sc alloy (AA5024) at 523 K [
25]. TEM mages show that these kinked grains are composed of even smaller subgrains with high-angle boundaries (
Figure 13) that are plausibly formed by microshears in the band-like grains, according to the scheme proposed by Belyakov et al. [
26]. Another possible mechanism could be geometrical recrystallization [
27], which is considered to be a type of continuous recrystallization. It was reported [
28] that continuous recrystallization is inherent with the Al-Mg-Sc-Zr alloys.
Author Contributions
Conceptualization, writing—original draft preparation, methodology, investigation, visualization, T.K. and A.C.; formal analysis, writing—review and editing K.K.; investigation, S.F.; project administration, supervision, E.K.; conceptualization, S.T. All authors have read and agreed to the published version of the manuscript.
Funding
The work was performed according to the government research assignment for ISPMS SB RAS, project No. III.23.2.4.
Conflicts of Interest
The authors declare no conflict of interest.
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Figure 1.
The friction stir welding (FSW) seam zones on a 35 mm thick AA1570 sheet (a), the FSW tool used for the 35 mm thick sheet after welding (b), the FSW tool used for the 30 mm thick sheet after welding (c), and the FSW tool used for the 35 mm thick sheet before welding (d). 1–tensile specimens; 2–metallographic section views, dmax–the larger pin diameter, h–the pin height, α–the taper angle.
Figure 2.
A diagram showing the sample cut-off scheme: (a) the leading edge of the exit hole on the retreating side (LE-RS), (b) the leading edge of the exit hole on the advancing side (LE-AS), (c) the trailing edge of the exit hole on the retreating side (TE-RS), (d) the trailing edge of the exit hole on the advancing side (TE-AS).
Figure 3.
The macrostructures of the FSW joint on 35 mm thickness alloy sheet in section parallel to the joint line: (a) the cross section of zone B (b); the cross section of zone S (c); the multi-nugget macrostructure of the stir zone (d); and a cross section view of the joint on the 30 mm thickness metal (e).
Figure 4.
Macrostructures in the FSW tool exit zone as viewed from the plane parallel to the welding direction and perpendicular to the sheet’s surface: (a) trailing part of the exit hole, sample 4.2; (b) the exit hole on the advancing side of the weld under different magnifications (c,e); kinked TMAZ grains in the top (f) and bottom (d) parts, respectively.
Figure 5.
The microstructural evolution on stir zone (SZ), thermomechanically-affected zone (TMAZ), heat-affected zone (HAZ) and base metal (BM)microstructures near the exit hole leading edge on the advancing side (AS), as seen in plane sections 2.2 (
a), 2.3 (
b), 2.4 (
c), 2.5 (
d), and 2.6 (
e) (
Figure 2).
Figure 6.
The alloy structures in the exit hole leading edge on the AS side, as viewed in sections 3.2 (
a), 3.3 (
b), 3.4 (
c), 3.5 (
d) and 3.6 (
e) (
Figure 2).
Figure 7.
The TMAZ grain structures in planar sections 3.2 (a), 3.3 (b), 3.4 (c), 3.5 (d) and 3.6 (e), as viewed normal to the sheet plane.
Figure 8.
The TMAZ grain size distributions as measured along lines 3 (
a), 2 (
b), and 1 (
c) (in
Figure 5 and
Figure 6 (
a,
c)) and the dependence of the TMAZ size on the height of the 30 mm thick sample (
d). The diagram labels are in accordance with those of the diagram in
Figure 3.
Figure 9.
TEM images of the stir zone coarse precipitates, grains, and dislocation loops in 35 mm (a,c) and 30 mm (b,d) welds.
Figure 10.
TEM images of the TMAZ structures in the 35 mm (a) and 30 mm (b) thickness seams.
Figure 11.
Mechanical properties of specimens cut across the weld at different distances from the weld root for 35 mm-thick (
a,
b) and 30 mm-thick (
c,
d) plates, the dependence of the mechanical properties on the distance from the weld root for 35 mm-thick (
e) and 30 mm-thick (
f) plates in zones “B” and “S” (see
Figure 1), and the test diagrams of the base metal tested along and across the rolling direction (
g).
Figure 12.
The microhardness profile across the FSW joint at 5 mm below the surface on 35 mm thickness metal.
Figure 13.
Optical images of the microstructures formed in the FSW tool exit hole metal leading edge metal (section 2.2 in
Figure 2). Blue dotted line contour denotes the transfer layer area.
Figure 14.
Optical images of the microstructures formed in the FSW tool exit hole metal trailing edge metal (section 3.2 in
Figure 2). The blue dotted line contour denotes the transfer layer area.
Figure 15.
SEM BSE composite image of the metal and precipitates in the FSW tool exit hole leading edge metal (section 2.2 in
Figure 2).
Figure 16.
Schematic diagram to illustrate the adhesion-assisted transfer of metal with the FSW pin. 1—tool, 2—rotation direction, 3—primary grain subdivision, 4—formation of transfer layer, 5—reverse transfer (deposition), 6—successive layer-by-layer metal transfer and deposition.
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