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A R T I C LE I N FO A B S T R A C T
Keywords: In the present research, the AISI 321 austenitic stainless steel was subjected to cold rolling with different amount
AISI 321 austenitic stainless steel of reductions. The 80% cold rolled samples were then annealed in the temperature range of 700–900 °C with
Cold rolling different durations. The microstructural evolutions during cold rolling and subsequent annealing were in-
Bimodal grain structure vestigated by XRD analysis, optical and scanning electron microscopy, and feritscope analysis. The mechanical
Mechanical properties
properties were evaluated by room temperature tensile testing. Results showed that the amount of strain induced
martensite is increased with increasing the rolling reduction. Annealing at 700 °C for 2 min resulted in the
simultaneous increase of tensile strength and elongation due to the formation of ultrafine grain austenite. By
annealing at 900 °C for 5, 10, and 15 min the bimodal grain structure was obtained as a result of the occurrence
of static recrystallization and martensite to austenite reverse transformation simultaneously. Results of tensile
testing showed that the good combination of strength and elongation is obtained by the formation of bimodal
grain structure.
⁎
Corresponding author.
E-mail address: eghbali@sut.ac.ir (B. Eghbali).
https://doi.org/10.1016/j.msea.2018.09.012
Received 10 June 2018; Received in revised form 5 August 2018; Accepted 5 September 2018
Available online 06 September 2018
0921-5093/ © 2018 Elsevier B.V. All rights reserved.
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
Fig. 2. Optical micrographs of AISI 321 steel before etching (a), and after etching (b), and X-ray diffraction pattern (c) after annealing at 1200 °C for 15 min.
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
Fig. 4. X-ray diffraction patterns of AISI 321 austenitic steel at different conditions: a) As annealed, b) 30% cold worked, c) 60% cold worked, d) 80% cold worked
state.
distinguished using the x-ray diffraction pattern due to their very small steel after annealing at 700 C for different durations are shown in Fig. 7.
volume fraction. Fig. 6 represents the SEM micrograph along with EDS In all microstructures, the dark regions indicate the martensite phase or
analysis from the scattered inclusions in the austenite matrix. As it is the ultra-fine grained austenite transformed from strain induced mar-
clear, these inclusions contain titanium and nitrogen elements that tensite during annealing, and the bright regions are the elongated
match with the composition of TiN intermetallic phase. The optical austenite grains exist in the microstructure of samples after cold rolling.
micrographs from the microstructure of AISI 321 austenitic stainless It is worth noting that static recovery is occurred inside these elongated
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
900 °C, it is seen that the fraction and the size of recrystallized grains
inside primary austenite grains (cold worked grains) is increased
compared with the microstructure of annealed sample for 5 min. It is
also apparent that the mean grain size of the ultrafine austenite grains
developed as a result of the martensite to austenite inverse transfor-
mation is increased with increasing the annealing time to 10 min. As
seen in Fig. 8(c), the bimodal grain structure is developed after an-
nealing at 900 °C for 10 min which is consisted of the intermittent layers
of recrystallized grains and finer grains developed as a result of the
martensite to austenite reversion. Increasing annealing time to 15 min
(Fig. 8(d)) results in the growth of the two types of austenite grains but
the traces of the elongated primary austenite grains are remained due to
the limited growth of the recrystallized and reversion transformed
austenite grains. Whereas, the uniform microstructure with equiaxed
austenite grains are developed after annealing for 25 min at 900 °C and
Fig. 5. Variations of the martensite phase fraction with cold rolling reduction. the traces of the primary elongated austenite grains are disappeared
(Fig. 8(e)). As can be seen, the bimodal grain structure is replaced with
grains during annealing. Some shear bands are also observed in Fig. 7 as uniform grain structure after prolonged annealing due to the higher
indicated by arrows. In addition, the dark regions in Fig. 7 are heavily growth rate of the ultrafine austenite grains compared with statically
deformed austenite which was transformed to ά martensite during de- recrystallized grains. Therefore, the difference between the grain sizes
formation, and the ultrafine grained austenite formed from martensite of these two types of austenite grains is decreased with increasing the
phase during annealing. Therefore, some regions with ultrafine grained annealing duration and finally the uniform grain structure is obtained.
austenite phase are formed in the microstructure after annealing at It is worth to note that the high amounts of Ti is added to AISI 321
700̊C. Also, it is seen that the volume fraction of ultrafine grained austenitic stainless steel to prevent grain boundary sensitization at high
austenite is increased with increasing annealing time from 2 to 25 min. temperatures. This amounts of Ti (for example 0.32% wt. in the in-
It is observed that after annealing for 25 min at 700 °C, near the 70% of vestigated steel) is high enough to form different types of precipitates
microstructure is transformed to ultrafine grained austenite. Also, shear and inclusions. It is well stablished that the TiN inclusions are formed
bands inside the elongated austenite grains were disappeared due to the during solidification process and remain stable upon cooling to ambient
annealing effect (see Fig. 7(d)). It is worth noting that the annealing temperature [29]. This type of inclusions are in the size of several
temperature of 700̊ °C is not higher enough to trigger static re- micrometer and distributed uniformly in the austenite matrix. Also, it
crystallization inside cold rolled austenite (bright regions in Fig. 7) has been demonstrated that the nanometer sized TiC and Ti(C, N)
during annealing so that the elongated austenite grains are observed in precipitates are formed in the matrix of Ti modified steels [30].
all of the annealed microstructures. Therefore, the interaction of nanometer sized precipitates with auste-
Fig. 8 represents the optical microstructures of AISI 321 austenitic nite grain boundaries decreases the boundary mobility and hinder the
stainless steel after cold rolling and annealing at 900̊C for different growth of austenite grains. Also, the coarse TiN inclusions provides
durations. As can be seen, after annealing for 2 min at 900 °C (Fig. 8(a)), preferred nucleation sites for static recrystallization during annealing
the microstructure is composed of austenite grains elongated in the which is called particle stimulated nucleation (PSN) [31]. Accordingly,
rolling directions with shear bands aligned parallel to each other and the both mentioned mechanisms result in higher levels of grain re-
ultrafine austenite grains developed in some regions between two finement in AISI 321 steel compared with other grades of austenitic
neighboring elongated grains. After 5 min annealing (Fig. 8(b)), some stainless steels.
equiaxed grains are observed inside elongated austenite grains in con- Fig. 9 shows the optical microstructures of cold rolled AISI 321
junction with the ultrafine grains developed as a consequence of the austenitic stainless steel after annealing for 25 min at different tem-
reversion of strain induced martensite to austenite phase. It is also peratures. As mentioned, at annealing temperature of 700 °C the com-
worth to note that the static recrystallization of cold worked austenite bination of ultrafine and primary elongated austenite grains are ob-
grains is not complete after annealing for 5 min and the boundaries served after 25 min annealing (Fig. 9(a)). Increasing annealing
between elongated grains are observable indicating the cold worked temperature to 750 °C, results in the growth of reverted austenite
features. In Fig. 8(c), the microstructure after 10 min annealing at grains. Careful inspection of Fig. 9(b) reveals that the shear bands are
Fig. 6. SEM micrograph from TiN inclusion (a), and related EDS analysis (b).
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
Fig. 7. Optical microstructures of cold rolled AISI 321 austenitic stainless steel annealed at 700 °C for different durations: a) 2 min, b) 5 min, c) 10 min, d) 15 min, and
e) 25 min.
observable inside some elongated grains. It is concluded that the static 3.4. Mechanical properties
recrystallization is not initiated at this temperature. At annealing
temperature of 800 °C (Fig. 9(c)) the size of the reverted austenite Fig. 10 represents the engineering stress - engineering strain curves
grains is increased and shear bands are disappeared which is the in- of initial annealed (d~ 200 µm) and cold rolled steel. As can be seen,
dication of the occurrence of recrystallization. After annealing at 850 °C the AISI 321 steel in the annealed condition has lower strength and
(Fig. 9(d)) the bimodal grain structure is obtained as a result of the higher elongation to failure compared with cold worked condition.
martensite to austenite reversion and static recrystallization in elon- Elongation to failure of annealed steel is around 125% which decreases
gated grains. Finally, the uniform grain structure is obtained as a result to 14.7% after 80% cold rolling reduction. Also, the tensile strength is
of the austenite grain growth (Fig. 9(e)). increased from 440 MPa to 1270 MPa by cold rolling. The increase in
the tensile strength value and the reduction of the elongation to failure
of austenitic stainless steels with cold rolling can be attributed to the
increased dislocation density, formation of substructures and the
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
Fig. 8. Optical microstructures of cold rolled AISI 321 austenitic stainless steel annealed at 900 °C for different durations: a) 2 min, b) 5 min, c) 10 min, d) 15 min, and
e) 25 min.
presence of deformation induced martensite. In the present investiga- important microstructural phenomena. The first one is the occurrence
tion, the effect of post annealing treatment on mechanical properties of of recovery inside the deformed austenite grains and the second is the
the AISI 321 austenitic stainless steel were evaluated using a series of formations of reverted ultrafine grained austenite from strain induce
tensile testing at room temperature. Fig. 11 shows the engineering martensie in the area of primary austenite grain boundaries. In the
stress-strain curves of material after annealing at 700 °C and 900 °C for initial stages of annealing the degree of the increase in strength due to
different durations. Also the effect of annealing duration on tensile the formation of ultrafine grain (UFG) austenite is higher than the
strength and elongation of cold rolled steel is represented in Fig. 12. As amount of softening due to the recovery inside the primary austenite
it is evident, both of tensile strength and elongation to failure of sam- grains. Therefore, the tensile strength is increased with annealing.
ples annealed for 2 min at 700 °C is higher than the cold rolled sample. Further annealing results in the higher degree of recovery with the
The increase in the tensile strength with annealing can be described annihilation and rearrangement of dislocations inside the elongated
according to the microstructural evolutions. It must be mentioned that grains and also the growth of UFG austenite grains developed at the
during annealing for 2 min the strength of material is affected with two early stages of annealing. Therefore it is observed that the tensile
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
Fig. 9. Optical microstructures of col rolled AISI 321 austenitic stainless steel annealed for 25 min at different temperatures: a) 700 °C, b) 750 °C, c) 800 °C, d) 850 °C,
and e) 900 °C.
strength is decreased with increasing annealing time. Also, it is ap- and elongation of cold rolled AISI 321 steel is shown in Fig. 12 (b). As it
parent that the elongation is almost constant at annealed samples. The is seen, the tensile strength is decreased with annealing duration and
insignificant variations of elongation with annealing time are a con- the elongation to failure is increase and reaches to the steady state
sequence of the microstructural evolutions. The occurrence of static value. The variations in the mechanical properties can be explained
recovery inside deformed austenite increases the amount of elongation considering the microstructural evolutions during annealing at 900 °C.
to failure but its effect is compensated by the decrease in elongation due As it is obvious in Fig. 8, the static recrystallization is occurred inside
to the formation of ultrafine grained austenite. As can be seen in Fig. 7 primary cold worked austenite grains and the reverted austenite grains
the volume fraction of reverted austenite is increased with annealing formed from strain induced martensite grow during annealing. As it is
time and its inverse effect on elongation is compensated by the progress seen, the difference between the grain size of recrystallized and re-
of recovery in primary elongated austenite grains. Fig. 11 (b) shows the verted austenite grain is decreased with increasing annealing time and
stress-strain curves of cold rolled steel after annealing at 900 °C for the bimodal structure formed in the initial stages of annealing changes
different durations. Also, the effect of annealing time on tensile strength into uniform microstructure after annealing for 25 min (Fig. 8(e)).
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
Fig. 11. Engineering stress-strain curves of cold rolled AISI 321 austenitic stainless steel after annealing at a) 700 °C, and b) 900 °C for different durations.
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H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
References
373
Downloaded from https://iranpaper.ir
https://www.tarjomano.com https://www.tarjomano.com
H.A. Rezaei et al. Materials Science & Engineering A 736 (2018) 364–374
[24] A.D. Schino, I. Salvatori, J. Kenny, Effects of martensite formation and austenite [28] A. Hedayati, A. Najafizadeh, A. Kermanpur, F. Forouzan, The effect of cold rolling
reversion on grain refining of AISI 304 stainless steel, J. Mater. Sci. 37 (21) (2002) regime on microstructure and mechanical properties of AISI 304L stainless steel, J.
4561–4565. Mater. Process. Technol. 210 (8) (2010) 1017–1022.
[25] L. Vitos, J.O. Nilsson, B. Johansson, Alloying effects on the stacking fault energy in [29] S.K. Michelic, D. Loder, T. Reip, A.A. Barani, C. Bernhard, Characterization of TiN,
austenitic stainless steels from first-principles theory, Acta Mater. 54 (14) (2006) TiC and Ti(C,N) in titanium-alloyed ferritic chromium steel focusing on the sig-
3821–3826. nificance of different particle morphologies, Mater. Charact. 100 (2015) 61–67.
[26] M.S. Ghazani, B. Eghbali, G.R. Ebrahimi, Kinetics and critical conditions for in- [30] Y.L. Kang, Q.H. Han, X.M. Zhao, M.H. Cai, Influence of nanoparticle reinforcements
itiation of dynamic recrystallization during hot compression deformation of AISI on the strengthening mechanisms of an ultrafine-grained dual phase steel con-
321 austenitic stainless steel, Met. Mater. Int. 23 (5) (2017) 964–973. taining titanium, Mater. Des. 44 (2013) 331–339.
[27] M. Milad, N. Zreiba, F. Elhalouani, C. Baradai, The effect of cold work on structure [31] J.D. Robson, D.T. Henry, B. Davis, Particle effects on recrystallization in magne-
and properties of AISI 304 stainless steel, J. Mater. Process. Technol. 203 (1–3) sium–manganese alloys: particle-stimulated nucleation, Acta Mater. 57 (9) (2009)
(2008) 80–85. 2739–2747.
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