Contents lists available at ScienceDirect Materials Science & Engineering A ELSEVIER journal homepage: www.clsevier.com/locateimsea Effect of torsional pre-strain on low cycle fatigue performance of 304 stainless steel “oe e Shengyuan Ji, Caiming Liu, Yajing Li, Shouwen SI tak of Chen gern an ed, Ynj Undery, yn 20073, cna » Xu Chen® Keyns Unloxal tensile tests and low cycle fatigue tests were performed on 304 stainles steal treated with diferent torsional prestrains. The slatinship between torsional prestrain and mechanical propers is established. Furthermore, de changes inthe amount of martensite phase anions are measured during ow eyee fatigue tests and after specimen fracture are observed. This is mainly Because martensitic transformation is roquent phenomenon during plsti deformation, which is clsly related othe mechaneal properties. In this tu, ti found that torsional prestrain inereasts yield strength and reduces elongation. The ductility of 304 stains, soa decreases wih the increase of torsional presta, while its flgue life doesnot AS the amplitude of torsional prestrain increases, the fatigue fe of the materi changes in ype. Impact, the fatigue fe increses when the torsional prestrain between M+ and #8. From the analy ofthe microcoame ditebation ‘ofthe martensite itis ound that the fatigue lifes afeted by the combined actin of martensite transformation fad ductility. The test resus rggest that it should skip the relatively dangerous sr ‘train aren when im proving mechanical properties of 208 stainless sel by way of changing shen pe-srn, 1, Introduction 304 stainless stel ($5304) is a kindof austenitic stainless steel with ‘excellent mechanical properties, corrosion resistance, and low-tem- erature resistance, making it widely used in food, medical chemical and power industries (1,2]- One sueh circumstance is the mobile ‘eryogenic tanks used fo store liquid natural gas (LNG) due to its low: temperature resistance [3]. The eryogenic tank consists of an inner container and a shell connected by a supporting piece. The annular ‘clearance between the inner container and the outer shell filed with multilayer aluminum foils or pearlescent sand as vacuum insulation materials. However, due tothe low yield strength of $8304, the wall thickness ofthe inner container Is thick, and the relatively larger ma- terial cost and economic cost are not negligible. Meanwhile, $8304 also has a characteristic that it has a relatively low yield/tensle ratio, which is actually waste of material mechanical properties to some extent. The inner container made of $S304 i traditionally prestrained to enhance the yield strength for igntweight design purpose, aiming to reduce ‘weight and be more economical efficient. The utmost significant aspect ‘of ING storing systems is steuetural safety, as LNG Is kept ata tem perature below ~ 168". Therefore, the design of eryogenic tanks is proposed to be lightweight and safety. Pre-strain of the material before ‘manufacture or after formation ean be processed to achieve the goal of Corsepondingsuthrs mal odds: syshiai.educn (8 Shi, xchen jeden OC Chen) upd or/10.1016/}.nsea 2019.01.17 Received 9 November 2018; Aceped 4 January 2019 ‘Available online Os nary 2019 (0921-5083/ © 2019 Elsevier BY. Al ights reserved. reinforcement, and the mechanical properties of the material can be strengthened. One way to improve mechanical properties is clled col work hardening (4-7). To ensure the structural integrity of the eryo- genic tank, the mechanical properties after pre-strained should be evaluated. ‘The effects of prestrain on mechanical properties of materials have been explored with a focus on tensile prestrain, For stainless stels and various alloys, the yield strength of materials ean be improved by tensile prestrain at the cost of reducing ductility and consequently decreased service life [8-14]. For $8304 which is a metastable aust- nite tales stet, martensite transformation also ceurs in addition to plastie deformation. The martensite phase will interact with plastic Aeformation and produce different phenomena (15-171. Both the hardness and strength of martensite are larger than those ofthe aus tenite, so the martensite transformation process will increase the overall strength and hardness of $5304. Meanwhile, the formation of ‘martensite due to plastic deformation also affects the fatigue properties fof material, The existence of martensite gave nses to sigmncant re sistance to crack growth due to itshigh strength and hardness (18) 16 found thatthe whole material show brite failure features and reduced life with increasing amount of martensite [19]. This indicates that martensitic transformation plays an important role in influencing me- ‘chanical properties of $5308However, the traltional pressure expansion treatment cannot ‘guarantee that the equipment deformation is uniform during the pre strain process, and the equipment size ater prestrain is not con twolable. The advent of new technology makes it possible to control the prestrain of the cold rolling process in addition to the traditional Pressure expansion treatment on lov temperatire storage tank after ‘manufacture. The difference between the above two proces is in the fact that the former one uses shear force while the latter one applies axial tension. The stress state of torsional prestrain treatment is the same as cold rolled coil. The effects of torsional prestrain on me ‘chanical properties of materials such as Cu-Zn brass (20) and pure ti- tanium (21) are also investigated. tis found that the torsional pre strain will improve yield strength, decrease elongation and lie ofthe ‘material, but the mechanical and fatigue performance of $8304 has not been systematically studied. And in previous studies, the amplitude of torsional prestrain is generally large and not quantified, which is of ltl significance for application in engineering practice. n this study, the small torsional prestrain (=15%) treatment of SS304 was per formed, followed by fatigue and tensile tests. The martensite phase transition was also investigated to show how it influence the fatigue performance of $S204, The findings inthis paper are beneficial fr the design and manufacture of cryogenic storage tanks. 2. Materials and methods The material used in this experiment Is $8304 and its chemical ‘composition isshown in Table 1. ln order to obtain a more accurate and ‘uniform shear stress-strain state, the thin-walled tubular specimen was used according tothe standards (22). The gauge length is 35mm, and the outer diameter and wall thickness of the gatge are 12.5mm and 1.25mm, respectively. The dimension specification of the specimen is shown in Fig. 1. Asreceived specimen is denoted as origin, wile that after torsional is denoted as “pretor”. Pre-train treatment, uniaxial tension test and low cycle fatigue (cr) test were caried out using strain control mode. As recommenced by the test method (28), the strain-rate of uniaxial tensile test and LCE test are 0,001 5 and 0.005", respectively. The strain amplitude of the LCF est is 0.4% Al test conditions are summarized in Table 2. To ‘ensure the accuracy and reproducibility of test results, each test was repeated at last 3 times. Al tests were conducted at room temperature. ‘The torsional pre-ain was firstly applied using the MIS tenson- torsional test machine and the uniaxial tensile test and UGE test were then carried out ona LETRY test machine (Xian LETRY testing machine Co, Ltd, China. Prior to test the gauge segment ofthe specimen is careful grinded, ‘mechanical polished and electri polished for microscopic observation ‘The Keyence VHX-900F 3-D digital microscope (Keyence, Japan) was used to observe slip formation after pre-stain treatment and experiment. Te feritescope (FERIISCOPE* FMP30) was used to measure the amount of martensite phase during experiment. However, we cannot ‘promise that the specimen is free of residual stress during the mea- surement so that there may be negative magnetosriction or the Villar ‘effect, which makes the measurement reslt less than actual e-mar- tensitic content. The actual volume fraction of martensite was, therefore, obtained by multiplying @ factor of 1.7 based on the frri- tescope readings according tothe literature [24]. The principle ofa martensitic phase being measured by ferstescope is that feritescope ‘ean measure magnetic phases, and only a’ martensitic phase is mag neti in 304 stainless steel [25] ‘Table 1 Chemteal omposition Mai one aging A 453019) 0-57 a d | 8] [30 a 110.4 EBSD (Cectron Back Seater Diffraction) was used identify the distribution density and the exact postion of martensite phase. The [EBSD images were captured under the condition of 23m and 0:5 step for microstructure analysis. Atleast three images were taken foreach specimen. EBSD specimens were water-abraded with #400- to #2400- gut SiC papers, and then elecro-polished in 95% acetic acid and 5% perchloric acid solution to relieve residual sess. 2, Revults 3.1, Bfeet of torsional pre-soain on uniaval tensile properties Pig, 2@) shows the effect of torsional prestrain on uniaxial stress strain behaviors of $S304. After 5% pre-torsion strain treatment, the stress-strain shifts upwards. Further increasing pre-torsin strain from 5% to 10% does not bring about significant changes. As can be seen from Fig. 2(be), the yield strength of the material increases with the Increase of torsional prestrain, while the elongation shows the opposite {rend and lite change is observed forthe ultimate strength, The eason {is that the plastic deformation inthe prestrain prevents the generation of new paste strain in subsequent tests and the yield strength is im- proved (12). From the analysis above, i is feasible to increase yield strength by torsional prestrain to realize light weight of low tem- perature storage tank. However, the safety problems caused by the ‘eduction of toughness should be evaluated through fatigue tes. 5.2, Yet of trstonalpre-sain on eye faigu propery “The prestrain treatment will sult in strength improvement but at the risk of reducing fatigue life. Therefore, inthis paper, he eyelic tests of torsional prestrain treated 304 stainless stel are carried out o study the relationship between fatigue properties and torsional pre-stain Fig. 3 shows the stress amplitude response under diferent torsional pre strain conditions where the stress amplitude response of 304 stainless steel can be divided into three stages wit increasing numberof cycles: hardening, softening and secondary hardening, The fist hardening ‘occurs in te frst 10 cycles because of the rapid emergence of a large numberof dislocation structures [26]. Then the subsequent softening ‘occurs and lasts for about 1000 cycles. Finally, secondary hardening ‘ceurs and lat ill the end ofthe test due to martensiie transformationMah Sie gem A 4 (2019) 5057 ()1200: & = © 000 3 e004 = 5 i a i” 2 ao E 5 ° | 0 20 40 60 80 100 True strain(s) origin 5%pre-tor 10%pre-tor (b)500 (100 oO. & = Exo Bo 5 3 B20 & 404 3 a * 1004 20-4 . 0 origin 5%pre-tor 10%pre-tor Fig. 2. Uniawal tensile propertion of $504 under diferent osional prestrain coiions a) Stree-stran curves (b) Viel strengt (Ul logation 500 Fs00 4 3 = a0 5 3 erin 8 00 | oe Spree a™ Sieroter peer ea epee Sa epee 100-4 + 10 100 1000 10000100000 Number of cycles ig. 3. Curves of seas ample es snberof eles nde diferent trional prestrain conions. origin S9%pre-tor 10%pre-tor ate tensile trong L171, Moreover, the stress amplitude increases with the increase of torsional prestrain, and all of them present similar evolution trends. It Indicates thatthe stress response mode ofthe material doesnot change ith te inerease of torsional prestrain. Only the stress level affected, fand the material shows stress enhancement with the increase of tor sonal peestrain until the end of lif. In order to analyze the effect of torsional prestrain on LCF perfor mance, the cyclic stress-strain responses are analyzed. In particular, the firstcyele hysteresis leop and mic life hysteresis loop ae compared, 38 shown in Fig. 4. Itean be seen from Fig (a) that the stress amplitude of the first circle increases with the increase of torsional prestrain. It proves that the difference in stress amplitude during the whole cycle in ig. 8 is mainly caused by the Increase in yield strength due to the plastie strain after torsional prestrain, The midlife hysteresis loop in Fig. (0) i primarily wed to analyze the mechanical response during the material service. The mid-life hysteresis loop becomes slender with the increase of torsional prestrain. Moreover, the frst-cyele hysteresis Joop and mid-life hysteresis loop are symmetrical, indicating that the torsional prestrain can elevate both tensile yield strength and com- pressive yield strength throughout the service life ofthe material. “Table 3 shows the fatigue life of test specimens. Fig. 5 shows the relationship between the torsional prestrain and the life of $8304 at (0.4% strain amplitude, It ean be seen from Fig. 2(€) that the elongation ‘of $8304 decreases with the increase of torsional prestrain. GenerallyMai one aging A 453019) 0-57 (600 se0 an ai } so] “RES 1 m eS 4 7004 ae 8 quo] “ere i 5 . e o é 3 : zo Sel i f 5 20 -200 = soo 00 | ca on Prestain®) ‘Strain(%) Fig. 5. Fatigue life under different torsional pre-strain conditions. wen decom ith acon rina exc dh Men stg ‘cen nr We Sage om esti opie fm, a SS ena ih nce of resin spe: a ‘nomenon indicates that the material ductility is not the only factor Siang he i a SSO oe wrol esainemenyet tah oral tunfornatn Saal an ema 320 g 3.3. Effect of torsional pre-strain on microscopic morphology | Fig. 6 shows the metallographic of S04 with original, 586 and 10% = torsional prestrain, respectively. The outer surface of $8304 tubular ® 2004 ‘specimen after sanding with sandpaper and mechanical polishing is Sorin ts) ean be ent ne aro he Spee 00 | ie hn al mnt f apt wer ee ne a the Sn en sete! sin ene eng ‘rl presi anne 0 toe unt sip 200: T T T ‘bands and a certain number of slip band intersections on the surface of a oa spcnc ig se), neon tector pea ines, ont) dey esp nd pty cease ane fom gc Fig. 4 Midi hysteresis oops under diferent torsional prestrain condtions {) lst je hysteresis loops (b) Mid life hysteresis lop ‘Table lLaweeyce fatigue properties of torsional prestraned 8304 specimen, speaking, decreased ductility of the material results in reduced life. However, withthe increase of prestrain, the life of $8304 does not ‘show a monotonic decrease but a change ofS” type. When the torsional prestrain is less than 5% (stage 1 or lrger than 89% (stage I, the life transforms from a single slip band to slip band intersections. The ie parable deformation is mainly manifested in the formation of disloce tion, which forms a slip that can be observed under an optical micro Scope (27). The number of slip bands indicates the degree of plastic strain and the region where the stess concentration fs prominent. ‘$8304 is a metastable austenitic steel that ean be ansformed into martensite under certain conditions. The main factor: influencing martensite transformation in $5304 are plastic strain and working temperature [28,29] In this experiments, the temperature is constant, and the plastic strain is the main factor influencing martensite trans formation, The martensite wansformation process manifexs Ise martensite appearing atthe slip band intersections and their growth {erminated at grain boundaries (17). The change in the amount of martensite phase is “S" type with the inerease of plastic strain. The content of martensite grows slowly at the initial stage, then enters the second stage of rapid growth, and finally returns to the slow growth state and eventually develops stably [17]. When the growth rate ie low, the specimen fil to reach the third stage because of its breaking, leading toa linear growth phenomena. It can be sen from Fg. 7 that the martensite content shows linear growth pattern with the inerease ‘ofeycle, which isthe same as the trend of secondary hardening, but the martensite growth rate is different for different torsional presrains. ‘The growth rate of small torsional prestrain is faster than that of large torsional pre-strain. This is mainly due tothe fact that the plastic strainFig. 6. Opsical micrograph of tesionl peestained 8304 (a) origin () 5% tosioal prestrain (€) 10% tosinal presto ‘of $3304 with larger torsional prestrain is relatively lower due to its larger strength in the LCF experiments under the same strain amplitude, Fig. 8 shows the cumulative plastic strain of $8304 under diferent torsional prestrans, Iti found that the plastic strain decreases gra- ‘dually with the increase ofthe torsional prestrain. In addition, itcan be ‘seen from Fig, 6 thatthe larger torsional prestrain will induce more slip. The formation of martensite indicates thatthe more slip bands are more likely to lead to the martensite phase transitions, and the slip band intersections is prone to occur (30]. Under the synchronously action of plastic strain and slip band, the martensite transformation rate ‘gradually decreases with the increase of prestrain This indicates that the plastic strain isthe main factor influencing martensite transforma- tion rate during martensite transformation, 4. Discussion Prom the above results it can be found that the plastic deformation formed by torsional prestrain is the decisive factor to enhance the yield strength of the material. In addition, due to the increase of yield strength, the stress response in LCF test also increased, which affected Mah Sie gem A 4 (2019) 5057 2 ai @ Bis 3 $310 2 Boat oxo 2 < Ripetor 4, i Speco rer 2 rose 15% pre-tor 0 4000 Number of cycles ig. 7. Martensite content during fe under diferent torsional prestrain eon 8000 12000-16000 160 ‘S120 : 80 = angi = ys Se Siprtr 5 40 py Brpretr 6 peor a O8ipretor + 1spretr ° © 4000-000 12000-16000 Number of cycle Fig. 8, Accumolted paste srain af 8904 under diferent torsional prestrain. the martensite transformation rate, This indicates thatthe torsion pre strain treatment is feasible to meet the equipment lightweight re ‘urements and its performance is stable during the service. However, the cause ofthe variation of fatigue life of SS304 under different tr sonal prestrain cannot be analyzed only from the change of ductility Therefore, the fracture surface ofthe specimen is analyzed by EBSD at the end of the eyli teat for diferent torsional pre-straina to scarch the relationship between martensite transformation and life span. The EBSD measurement can capture grain boundaries, phase boundaries and the distribution of sip bands, which is beneficial forthe under standing of martensite phase evolutions. It is convenient to reveal the distribution density of martensite and austenite to analyze the re- lationship between martensite phase transition and slip band. Two {types of martensitic phases have been reported hexagonal close-packed femartensite and cubie martensite (31. This paper focuses on a ‘martensite rather than e-martenste as emartensit are rarely produced during phase transformation process and canbe neglected, as shown in Fig 9 Fig. 9 shows the phase map and boundary map ofthe material In boundary map, the grey base isthe grain ofthe material, the blue base Js large angle grain boundary from 15° to 180° and the red region isMai one aging A 453019) 0-57 Fig. 9. Micratrcturs of SS204 unde diferent torsional p= strain (2) Boundary map without torional prestrained (b) ‘se map without torsional prestraine (¢) Boundary map wth torsional pre strained up to 3% () phase map with tr sional prestraned upto 3% (€) boundary map with torsional restrained upto 5% (phase map with torsional prestrained Sp to 5s (0) boundary map with Yoronal prestrain’ wp to ‘8h; (h) phase map wth torsional prestrsined wp to BG) ‘ondary map wih sional prestraned up © 10%; () phase ‘map with torsional presraned! upto 10% (k) boundary map ‘with torsional prestraned upto 158%; () phase map with tr Sonal presrained wp 10 15%small angle grain boundary ftom 2° to 15° Inthe phase map, the red region is austenite and the green region is martensite, The region of martensite phase transformation is the slip band and the grain boundary. It can be seen from Fig. 9 that most martensite distribute in the grain interior, while the martesite in specimens with 8%, 10% and 1596 torsional prestrain distribute on grain boundaries. With the in- ‘rease of torsional prestrain, the distribution of martensite gradually ‘changes from a concentrated mass to a zonal distribution. Such changes ‘of martensite are reated to prefabricated slip band induced by torsional prestrain. The martensite phase transition process is periodic. Firstly, nucleation of martensite occurs at nucleation points due to stress con” ‘centration a these ste, Then the martensite grow into intrcrystaline ‘oF intererystaline martensite with the accumulation of plate strain ‘according, fo the nucleation location [17,30]. From Fig. 9(@-), the martensite presents a massive concentrated distribution on the basis of ‘grain for original and small torsional prestrain, With the increase of torsional pre-srain, the martensites start to appear within gains and tend to disperse as shown in Fig. 91). Meanwhile, the strength im- provement leads to the reduction of plastie strain per eyele and the ‘decrease of martensite growth rate. In summary, the martensite region ‘gradually presents the dispersion change. team be seen from Pig. 5 that the ductility deereases with the in- ‘crease of the torsional prestrain, but the life does not decrease mano tonieally. The LCF life of the material is divided into three stages. ‘Combining with. 9, it an be found that the material in stage 1 only has intraerystal martensite. While stage Ills composed of intergranular martensite and intracrystal martensite. The main reason for the two diferent martensite is the formation of different nucleation points ‘Three nucleation of martensite are reported, including slip band in- tersection, grain boundary triple point and isolated slip band (301. From the shape of formed martensite as shown ini. 9, when the value ‘of torsional prestrain ie less than Sh, martensite mainly starts phase transformation from the slip band intersection and isolated slip band ‘and eventually forms intergranular martensite, The dislcation density In the maceral is more easily increased under the combined action of shear strain and axial strain (238). So with the increase of torsional prestrain, the dislocation density between grains gradually increased under the combined action of shear plastic deformation and cyl plastic accumulation until the martensite phase transition could occur to form intererystalline martensite. Seen from results ofthe identical ‘stage with the same mirostructure, the if ofthe material dereases with the decrease of dutty. However, the LCF lif ofthe material has an upward trend in the tage I, which is mainly due tothe formation of intererystalline martensite that greatly influence the erack growth. ‘Crack grows includes two stages: eack initiation and erack propaga tion [34]. Crack initiation stats from the location of stress concentra- tion. Normally, it starts from grain boundary [35] and loation of sip band (6). After erack initiation, erack grows gradually during the continuous loading. Both crack initiation and crack propagation in ‘small size (=1 mm) play an important role in the LCF life ofthe ma- terial n $8304, miere-racks wil form at the interface of austenite and ‘martensite and inside martensite phase after cyclic loading because of ‘rest concentration at these microstructural points {2°), The crack then propagates through the grain in the direction of the vertical slip band. Martensite is a phase with higher strength and hardness than ‘austenite, When martensite forms inside austenite, the stress state ofthe whole austenite grain will not be significantly fected. Moreover, a large number of martensite can make the whole austenite grain appear brittle and reduce the fatigue property of the material [19]. When martensite formed atthe grain boundary, i slike «hard martensite shell is placed onthe austenite grain. That will largely prevent the crack ‘occurrence from spreading with the increase of materia’ LCF lf, This result is of great significance for improving the safety of exyogenie storage tank. However, with the increase of torsional prestrain, the ‘cause of intercrystalline martensite gradually appeared in $S304 isnot clear, which requires further study. Mai one aging A 453019) 0-57 5. Conclusions In the present study, uniaxial tensile test and LCF test were per formed on $8304 treated by diferent torsional prestrain. The micro structure was observed by optical microscope and EBSD to establish the relationship between microstructure and mechanical properties of the material. The yield strength, elongation and LCF life of $8304 are analyzed, the conclusions are summarized as follows: 1. The torsional prestrain can enhance the tensile and compressive yield strength of $S304 and reduce the elongation. This resul means that torsional pre-strain ean be used to achieve lightweight, Inthe LCF test, the stress response of $8304 was divided into three stages: hardening, softening and secondary hardening caused by ‘martensite transformation. With the increase of torsional prestrain, the stress response amplitude gradually increases, while the stress response mode 1s not affected Plastie strain is always produced during LCF est, which leads tothe transformation of austenite phase into martensite phase. With the Increase of torsional prestrain, the martensite transformation ve- locity decreases. Inthe LCF tests under the same strain amplitude, the plastic strain in the material with higher yield strength occupies less proportion in the total strain, Slow plastle stain accumulation «auses lower martensite transformation. 4. The ductility of $5904 decreased gradually with the increase ofthe torsional prestrain. However, its life was not monotonically de creasing with the decease of detilty. With the increase of torsional prestrain, the fatigue life of $8904 is divided into thre stages: the stage land stage Il are menotonically decreasing, while the stage Il |s monotonically increasing. This isthe result of a combination effect of ductility and martensite transformation, Intererystalline marten site coats the austenite grains, which increases the resistance of «rack initiation and propagation, and eventually leads to increase of fatigue te “The rewearch results above prove that itis feasible to control the pre strain by rolling coil in the manufacture of low temperature storage tank. However, the small shear prestrain will greatly shorten the m- terial life under the condition of sight strength increase, so it is im- portant to note thatthe smal strain area should be skipped during the pre-stain processing. 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