1. Introduction
Micro metal forming, particularly for austenitic stainless steel (ASS), is a promising approach in the biomedical, electronic, chemical, electrical power, food, and nuclear industries [
1], ASS has excellent corrosion resistance and processability [
1,
2]. In addition, the high demand for microparts has received significant attention in recent decades [
2,
3]. However, microforming technology has a number of challenges, such as the limitation of material applications and the high cost of mass production [
1,
2,
3]. When ASS is subjected to plastic deformation, martensitic-induced transformation occurs in the ASS [
1]. The transformed martensitic volume fraction increases with the increase in plastic deformation [
1,
2,
3]. Martensitic transformation reduces the toughness but increases the strength of ASS [
4,
5]. When subjected to plastic deformation, austenitic stainless steel, as a metastable phase, undergoes a transformation from Face Centered Cubic (FCC) austenite to Body Centered Tetragonal (BCT) martensite at room temperature [
1,
2,
3,
4]. The martensitic transformation enhances the strength of thin metal foils and results in elongation because an increasing work hardening rate can delay the occurrence of plastic instability in thin metal foils [
1,
2,
3,
4,
5]. Factors that may result in martensitic transformations are chemical composition, strain path, grain size, strain level, and strain rate [
6]. Xue et al. [
1] found that the martensitic-transformed volume fraction can be controlled by controlling the stainless strip steel deformation. Martensitic transformation on the surface is larger than that in the interior with the same strain [
1,
2,
3,
4]. When ASS is subjected to plastic deformation, in addition to martensitic phase transformation (MPT), dislocation interaction and twinning also occur [
1,
5]. Twinning is greater on the surface than in the interior of ASS [
1,
6]. Increasing martensitic transformation results in the increasing stacking fault energy (SFE) of martensite; hence, the martensitic transformation occurs more readily on the surface than in the interior [
1]. Furthermore, surface roughening also occurs more readily on the surface than in the interior of thin metal foils [
1,
2,
3]. It is necessary to investigate the dependency between surface roughening behavior and MPT in ASS thin metal foils. Peng et al. [
7] concluded that MPT is caused by an increasing strain rate, which results in an increase in the local temperature. A large increase in the strain rate suppresses MPT [
7,
8]. The Olson and Cohen model, called the OC model, is fundamental to the description of the kinetics of strain induced in martensite [
1,
7,
9,
10]. The shear band intersection, as a dominant nucleation site, is considered [
7,
11]. The transformation curve is constructed only as a function of the plastic strain and a constant environmental temperature in the OC model [
7,
10,
12]. Tomita et al. [
8] found that the number of shear band intersections, as the location of the nucleation site, increases as the strain rate increases, while the probability that a shear band intersection forms an embryo decreases. This conclusion was considered only for a constant temperature, and the increasing temperature caused by self-heating in the tensile test was ignored. Zandrahimi et al. [
9], concluded that transformation of austenite to martensite (MPT) in AISI 304 resulted in surface hardening, which led to deterioration of the wear resistance. It is necessary to investigate the surface roughness caused by MPT because surface roughening is caused by grain deformation on the surface and affects thin metal foil properties, particularly on the surface. Zihao et al. [
10] concluded that uniform elongation (UEL), ultimate tensile strength (UTS), and martensitic volume fraction decreased because of increasing strain rate and temperature. Jeom et al. [
11] concluded that, in duplex stainless steel, strain-induced martensitic transformation (SIMT) occurred after plastic deformation. The transformation from austenite to ε martensite occurred at a low strain level, and transformation from austenite to α′ martensite occurred at a high strain level [
10,
11].
In addition, in miniaturization and metal forming processes, with decreasing sheet thickness, the ratio of surface roughness to thickness increases in metal foils, and this is known as a non-uniform thickness [
12,
13,
14]. The surface roughening phenomena of the sheet material have a strong effect on necking and fracture behavior of materials [
12,
13]. The inhomogeneous deformation of each grain located near the free surface will cause surface roughening phenomena on the free surface of polycrystalline metals [
13,
14]. Thus, surface roughening is highly important in the field of microforming technology using sheet or thin metal foils [
12,
13,
14]. Surface roughening results in the size effect of thin metal foils [
15]. Furushima et al. [
3] concluded that fracture behavior at the microscale is the major factor causing surface roughening. The failure behavior and material flow of thin sheet metals are influenced by the size effect, which is mainly caused by the low number of grains in the straining zone [
16]. Meng et al. [
17] found that, when the surface non-uniformity increases to the same magnitude as the sample thickness, the effect of the free surface roughening on fracture strain and flow behavior is significant. Stoudt et al. [
18] found that a linear dependency exists between grain size and roughening rate, as well as demonstrated that the roughening rate was dependent on Mg-Al alloy grain size. Furushima et al. [
19] found that pure titanium and pure copper dramatically decrease the fracture strain for thicknesses from 0.3 to 0.1 mm. Fracture strain is significantly affected by material thickness [
18,
19]. The size effect is challenging for micro metal forming of ultra-thin metal foils [
17,
18,
19]. When plastic strain increases, the ratio of the surface roughness to the thickness for each material linearly increases [
16,
17,
18,
19]. Rabee et al. [
20] found that clarification is needed in respect of the relationship between deformation-induced surface roughness and the local microstructure. Furushima et al. [
21] concluded that fractures were caused by free surface roughening because dimpling did not occur for pure copper thin foil in the range of thicknesses from 0.05 to 0.1 mm. Surface roughness increased under uniaxial deformation because of decreased thickness in the same area [
19,
20,
21]. This indicates that, when the number of grains is decreased, the surface roughness increases, as shown by uniaxial tensile testing with the same strain level. The fracture strain was low and surface roughness significantly increased in a uniaxial tensile test with the same strain level due to the five-fold decrease in the quantity of grain size (Dg) [
20,
21]. Lei Zhang et al. [
22] found that investigation is limited regarding the quantitative description of the evolution of the surface roughness of FCC polycrystalline metals. Research and investigation of surface roughness, other than that of FCC structure polycrystalline metals, is, therefore, needed [
18,
19,
20,
21,
22]. Kengo Yoshida [
23] found that surface roughness is mainly governed by the Dg, and investigation is needed in respect of surface roughness behavior with Dg below 10 μm. Shimizu et al. [
24] concluded that the mutuality of grains affects the surface roughening behavior. Different individual deformations of grains affect the surface roughening behavior [
16,
17,
18,
19,
20,
21,
22,
23,
24]. It is necessary to investigate surface roughness behavior with different Dg, which may result in different mechanisms of surface roughness behavior. Linfa Peng et al. [
25] found that the individual grains, and particularly the surface grains, are less restricted due to the decrease in grain boundary density caused by the increasing Dg. As the grain orientation and the structures of individual grains are randomly distributed, the inhomogeneity of grains is more significant, which leads to a significant increase in surface roughness [
24,
25]. Thus, investigation and understanding are needed in respect of surface roughening behavior with various Dg.
Furushima et al. [
26] found that plastic deformation preferentially occurs in weak grains, which have lower flow stress in pure copper (C 10220-O) ultra-thin metal foil with a thickness of 0.05 mm. The roughening phenomena on the free surface of polycrystalline metals are affected by the inhomogeneous deformation in each grain located near the free surface [
14,
26]. P. Groche et al. [
27] found that, due to the Hall–Petch theory, the flattening of the surface asperities is hindered by the increase in yield stress. Cheng et al. [
28] found that the mechanical properties are affected by free surface roughening in thin metal foils, rather than the growth of the voids in the side materials, in thin sheet metal or thin metal foils. Thus, research and study of surface roughening is needed to understand the mechanisms of surface roughening, particularly for small Dg. Aziz et al. [
29] found that surface roughening increased proportionally without annealing in coarse grains of SUS 304. The increase in surface roughening was not proportional without annealing in fine grains in either SUS 304 or SUS 316 thin metal foils. Furushima et al. [
30] found that the grain strength variation is a representation parameter that determines material inhomogeneity. The decrease in the ratio of thickness to grain size, t/d, leads to inhomogeneous deformation, which affects the surface roughness behavior [
26,
27,
28,
29,
30]. As a result, the increase in Dg in the same thickness leads to inhomogeneity of the grain strength [
26,
27,
28,
29,
30,
31].
For stainless steel (SUS) 304, the grain has high volume fraction of MPT induced by plastic deformation, and the grain strength increases, and grain deformation becomes more difficult, compared to grains with lower MPT. Furthermore, the effect of MPT on the surface roughness could depend on the microstructure, which means that the effect of MPT depends on the grain size. However, the effect of the MPT for different grain size on the surface roughness is unclear yet. The aim of this study was to clarify how the MPT and GMO result in inhomogeneous grain strength which is shown by the surface roughening behavior of thin metal foils with various Dg. In this study, ASS SUS 304 and SUS 316 thin metal foils were subjected to five cycles of sequential uniaxial tensile stress state testing to measure surface roughening behavior, and the MPT, GMO, and grain deformation mechanisms were analyzed using SEM-EBSD.
3. Experimental Results of Tensile Test
Figure 3 shows the stress–strain curves of SUS 304 and SUS 316 thin metal foils with various Dg. In SUS 304 thin metal foils, fracture strain is influential factor in this study. In contrast, tensile strength decreases with increasing Dg in SUS 304 thin metal foils. The strength and ductility of SUS 304 are higher than those of SUS 316 thin metal foils, as shown in
Figure 3. According to the Hall–Petch theory, materials with fine grains exhibit higher strength than materials with coarse grains. The strength significantly improved when the grain size decreased from coarse to fine [
34]. The correlations between surface roughness behavior with strain level without annealing have been revealed in previous study, showing that surface roughness increases proportional in coarse grain and does not increase proportional in fine grain during uniaxial tensile test [
29].
Figure 4 indicates the relation between the surface roughness and true strain at a low strain level of 5% (1.0% at one stage of the tensile test) and at a high strain level of 25% (5.0% at one stage). The samples of both SUS 304 and SUS 316 thin metal foils were subjected to five stages of a tensile test at low strain and high strain levels. Thus, the accumulation of the strain level for low strain was 5.0%, and the accumulation of the strain level for high strain was 25.0%.
According to
Figure 3a,b, Dg 1.3 µm was SUS 316 thin foil without annealing, and Dg 0.5 µm, Dg 1.0 µm, Dg 1.5 µm, Dg 3.0 µm, Dg 9.0 µm were SUS 304 thin foil without annealing [
29]. The strength of thin foils between SUS 304 and SUS 316 as received and after annealing are similar, as shown in
Figure 3a,b.
The correlation between surface roughness and true strain is shown in
Figure 4a,b, in both low and high strain level. Surface roughness (Ra) increased proportional both in low and high strain level. Based on
Figure 4a, the surface roughness increased proportionally in the low strain level in both the fine and coarse grains. The tendency of surface roughness behavior is similar in fine and coarse grains at the low strain level. Based on
Figure 4B, the surface roughness increased proportionally at the high strain level in both fine and coarse grains. The increase in surface roughness was higher for coarse grain than fine grain, in both SUS 316 and SUS 304 thin metal foils.
Figure 5 indicates the relation between the increase in surface roughness (ΔRa) and the true strain instead of Ra. ΔRa means the difference between the initial surface roughness and the surface roughness after the five steps of the tensile test. At a high strain level, ΔRa was proportional to true strain in both fine and coarse grains, and ΔRa increased to a higher value in coarse grains than in fine grains. The greater increase in Ra in coarse grains under high strain conditions indicates that the mechanisms of fine and coarse grains are different at a high strain level.
Figure 6 indicates the ΔRa values for SUS 304 and SUS 316 thin metal foils at a high strain level with various grain sizes. The ΔRa increased proportional to Dg, but the gradient depends on the material.
Since the grain strength of fine grains is higher than that of coarse grains, the grain strength may have an effect on surface roughness increasing. The higher the strength in fine grains, the more difficult it is to deform them. According to the Hall–Petch effect, the higher strength in fine grains than coarse grains is also indicated by the higher tensile strength in fine grains compared to coarse grains, as shown in
Figure 3.
The surface roughness also depends on the inhomogeneity of the grains; higher inhomogeneity of grains will result in higher surface roughness after plastic deformation with the same strain level [
26].
The Δ
Ra of SUS 304 coarse grains is higher than the Δ
Ra of SUS 316 coarse grains because the grain strength in SUS 304 is higher than that of SUS 316, as indicated by the higher tensile strength in SUS 304 than SUS 316 thin metal foil fine grains, as shown in
Figure 3.
Based on previous studies [
30],
increases linearly to product of grain size (
Dg) and strain levels or true strain (ε), as shown in Equation (1),
where
is initial surface roughness, and
is the material constant. Since
, we could write the equation as:
The equation means that coefficient
only depends on the material but not on
Dg and ε. By substituting the results shown in
Figure 5 into Equation (2), the correlation between product of grain size (
Dg), true strain (ε), and
can be plotted as shown in
Figure 7. The
increase proportional with the increasing
. However, there are differences in the gradients. The difference of the gradients may depend on the homogeneous and inhomogeneous grain strength of thin metal foils due to the grain sizes. Different mechanisms may also result in different tendencies in surface roughness behavior in SUS 304 and SUS 316 s.
For investigation of the different in deformation mechanisms, microstructures of the material after the tensile test was analyzed by using SEM-EBSD, discussed in next section.
4. Results of SEM-EBSD and Discussion
In this research, SEM-EBSD was used to obtain a phase map, IPF map, and KAM map before and after the sequential uniaxial tensile test. The Phase map consists of austenite and martensite phases in the SEM-EBSD result. The inverse pole figure (IPF) map derived by EBSD reflects the locally discovered orientation. From the IPF map, we could obtain grain deformation behavior with the changing of a color in a grain. The kernel average misorientation (KAM) map is a map that shows grains orientation by changing collective color in the EBSD result. The KAM map comes from the calculation and averaged grain misorientation in the center with the surroundings.
The microstructures, consisting of MPT derived from phase map and GMO derived from KAM map, were obtained using SEM-EBSD analysis. The MPT and GMO were investigated in fine and coarse grains of SUS 304 and SUS 316 thin metal foils at both low and high strain levels and related to surface roughness behavior. In
Figure 8(A1–A4), the phase map is shown. The red color is the gamma (γ) or austenite phase, and the green color is martensite phase transformation (MPT), also known as alpha (α) iron;
Figure 8(B1–B4) show the IPF normal direction (ND) map. Grain deformation is more severe in coarse grains, as shown in
Figure 8(B3,B4), than fine grains, as shown in
Figure 8(B1,B2), in both SUS 304 and SUS 316 thin metal foils. There was no MPT in SUS 316 fine grain and coarse grain, as shown in
Figure 8(A1,A4), even after 25% total strain level. The grain deformation in coarse grain of SUS 316 was more severe, as shown in
Figure 8(B4), compared to fine grain, as shown in
Figure 8(B1). The MPT was very high and spread uniformly in fine grain of SUS 304, as shown in
Figure 8(A2). The MPT was low and not uniformly spread in coarse grain, as shown in
Figure 8(A3).
During the tensile test with the same strain level, the slip band intersection was higher in fine-grain SUS 304 thin metal foils than the coarse grains of SUS 304 thin metal foils [
8,
9,
10]. As a result, MPT in fine grains was greater than that in coarse grains of SUS 304 thin metal foils. The slip band intersection is the location of the martensitic embryo and nucleation [
10,
11,
35]. Fine grains have a higher probability of the slip band intersection than coarse grains [
10], thus, MPT is greater in fine grains than coarse grains with the same strain level. Therefore, fine grains have greater grain strength than coarse grains, and fine grains have lower inhomogeneous grain strength than coarse grains. As a result, coarse grains with lower MPT become inhomogeneous grains, and fine grains that consist of higher MPT become homogeneous grains, which indicates the higher surface roughening behavior in coarse grains than in fine grains of SUS 304 thin metal foils at the same strain level.
As shown in
Figure 9(A1–A4), it was known that the KAM map consists of three kinds of color, the blue one was 0° misorientation, the green one was 2° misorientation, and the red one was 5° misorientation [
29]. The effect on the grain strength of 5° misorientation was higher than 2° grain misorientation, and the effect on the grain strength of 2° misorientation was higher than 0° grain misorientation [
24,
27,
29]. There was no effect on 0° grain misorientation in grain strength [
24,
29]. According to the grain misorientation, the grain strength of SUS 316 thin foil was high, and the grain strength of SUS 304 fine grain was very high.
Figure 9(A1,A2) show that the amount of 5° grain misorientation was similar between SUS 304 and SUS 316 fine grain thin foils, but 2° green misorientation in SUS 316 thin metal foils was lower than the green misorientation in SUS 304 thin metal foils. This means that a grain of SUS 316 is weaker than a grain of SUS 304.
The type of grain deformation mechanism, in both SUS 304 and SUS 316 fine grain thin metal foils, was intergrain deformation [
24,
27]. Intergrain deformation results in a small change in the surface roughness in fine grain SUS 304 and SUS 316 thin metal foils because the intergrain deformation affects the low inclination of a grain from the normal direction that affects more homogeneous grain strength values [
22,
24,
25,
36]. The surface roughness in fine-grain SUS 304 thin metal foils was almost the same as that of fine grain SUS 316 thin metal foils because the grain inclinations were similar after plastic deformation, even though the grain strength of SUS 316 thin metal foil is weaker than that of SUS 304 thin metal foil.