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Fatigue Fract. Engng Mater. Struct. Vol. 20, No.4, pp. 565-571, 1997 Printed i Great Britain.

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8756-758X/97 $6.00+0.00 Copyright Q 1997 Fatigue & Fracture of Engineering Materials & Structures Ltd

THE BRITTLE FRACTURE OF 475°C EMBRITTLED CAST DUPLEX STAINLESS STEEL
T. J. MARROW N. BURY and
Manchester Materials Science Centre, University of Manchester and UMIST, Grosvenor Street, Manchester, M1 7HS, UK Received in finalform 20 December 1996 Abstract-The fracture behaviour of cast duplex stainless steels, heat treated to different ferrite contents and hardness was investigated using tensile and notched bend tests. The purpose was to identify the microstructural features which controlled the ductile-to-brittle fracture transition of 475°C ernbrittled duplex stainless steel. The results indicate that twin nucleated cleavage has a tensile stress fracture criteria and the brittle-to-ductile transition temperature depends on ferrite microhardness, ferrite grain size and constraint. Keywords-Duplex stainless steel; 475°C ernbrittlement; Deformation twinning; Brittle-to-ductile transition; Age hardening.

NOMENCLATURE
b = Burger’s length. D = slip band length G = shear modulus y = fracture energy ( T = tensile fracture stress ~ tf= critical resolved shear fracture stress ti = dislocation friction shear stress t = critical resolved shear stress to nucleate a crack , v = Poisson’s ratio

INTRODUCTION

It has been previously shown that brittle fracture of duplex stainless steel is nucleated by deformation twinning [l]. Brittle fracture is encouraged by the increase in ferrite yield stress at low temperatures and with age-hardening (475°C embrittlement). The previous study used a finite element model of the deformation around a notch to demonstrate that brittle fracture initiation in notched samples required a critical shear stress acting over a critical distance. This critical shear stress was comparable to the shear stress at fracture in smooth tensile specimens that failed in a brittle manner. Although providing a quantitative insight into the problem of 475°C embrittlement in duplex stainless steels, the model had some flaws. First; the finite element analysis treated the duplex microstructure as a homogeneous continuum. Second, and more importantly; although the critical shear fracture stress was consistent with twin nucleated cleavage, it did not account for the observed effect of tensile stress which caused ferrite cleavage in the centre of necked tensile specimens [ 11. A nucleation-controlled twin-nucleated cleavage model also did not provide a satisfactory explanation for the occurrence of a brittle-to-ductile transition, nor for the observations that yielding in age-hardened duplex stainless steels occurred with profuse twinning, yet fracture occurred above the yield stress after some plastic strain.
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annealed at 1 3 0 ° C for 1 h and water quenched.%): Steel A (25. A similar finite element analysis has been used to determine the effects of the notch.4 Cr.l at room temperature (20°C) using steel A.5 Si). Audible clicking (acoustic emission) was heard well below the yield stress in all samples. J. The ferrite subgrains were revealed by an electrolytic oxalic acid etch. Test specimens were then machined and aged at 475°C for up to 640 h.7 Mn. ferrite microhardness. The light element content was not determined. 6.3 Ni.01 s . Duplex stainless steel microstructures: (a) steel A. 0. The ferrite contents were determined using image analysis of metallographic samples electrolytically etched in 30% KOH solution. 5. 3. ferrite content.8 Mo.8 Mn). with the Vickers hardness (30 kg diamond pyramid indenter) after ageing for approximately one week at 475°C. increasing in Fig. The results are given in Table 1. EXPERIMENTAL DETAILS AND RESULTS Materials Two cast duplex stainless steels were used. Both steels were annealed as blanks at 1100°C and 1300°C for 1 h and water quenched. 0. Steel and Annealing temperature SteelA 1l00"C SteelA 10' 30C 723 1000+200 Steel3 1looOC SteelB 1300°C 83*5 Ferrite Content (%) Ferrite Grain size (pm) Ferrite subgrain size (pm) Vickers Hardness (30kg) (aged one w k a 45C t 7') 47*2 90M150 5 1*2 40W60 16i4 327k7 75WlOO 12. (b) steel A. annealed at 1100°C for 1 h and water quenched.566 T. 2. MARROW N. 0. BURY and This paper addresses some of these concerns and attempts to identify the important microstructural parameters which control the ductile-to-brittle transition.0 Mo.6 Ni. Tensile tests (steel A) Tensile tests (diameter 5 mm) were performed at a strain rate of 0.i4 14 % 408i22 16a4 346f6 32&8 . and the ferrite grain size was inferred from the distribution of the austenite (Fig 1). Energy dispersive X-ray analysis gave the following compositions (in wt. The proof stress at 1% plastic strain was taken as the yield stress.5 Cr. 1. ferrite subgrain size and ferrite grain size in heat treated cast duplex stainless steels. and steel B (25.

Brittle fracture generally occurred after yielding with plastic strains of the order of 3-10%. 3(b)). annealed at 1100°C and 1300°C and aged at 475°C Ageing time (hours) Fracture mode Vickers hardness (30 kg) . (b) Brittle fracture (aged for 640 h). Table 2. The fracture surface was either completely ductile (Fig. (b) yield stress (1% proof stress). A transition from ductile to brittle fracture was observed with increasing hardness. The Vickers hardness and ferrite microhardness on either side of the brittle-to-ductile transition in steel A. 2. Only the material annealed at 1300°C and aged for 640 h failed without yielding. 3(a)) or completely brittle with ferrite cleavage and ductile shearing of the austenite (Fig. except for the 1300°C annealed steel aged for 640 h (hardness 447 & 20). The tensile fracture stress for tests which failed without yielding. Both steels showed the same linear dependence of yield stress and hardness. (a) Ductile fracture (aged for 48 h). Effect of annealing temperature (1100°C and 1300°C) on the relationship between Vickers hardness (30 kg): (a) ageing time. frequency at yield with very little emission after yield. This material failed below the expected yield stress. hardness and fracture behaviour was determined. 2. The effect of ageing time on yield stress. Fig.Brittle fracture of duplex stainless steels 567 5Wr -0 0 0 Fracture stress 4W 450 500 s'i AGEING TIME (hours) MCKERS HARDNESS Fig. 3. Ageing had a greater effect on the hardness of the 1300°C annealed steel. annealed at 1100°C. The effect of ageing time on the fracture of steel A. and the critical hardness for the brittle-to-ductile transitions (BDT) are also shown. The results are shown in Fig. No samples failed with both cleavage and ductile failure of the ferrite.

There is no significant difference between the results for the two microstructures. These results are in Table 2.10°C and -60°C.30°C was sectioned along its axis for metallographic examination. 7 mm) were performed at a strain rate of 0. All tests showed nonreversible plastic strain. and no agreement of the tensile stress. The behaviour close to the notch surface may be an artefact of the mesh used in the model. Tensile tests (dia.1 was used. A strain hardening exponent of 0.568 T. They did not appear to be influenced by either the Fe subgrain boundaries or the austenite within the Fe grains (Fig. annealed at 11Oo"C. A model of the elasticplastic deformation at the notch root was constructed using LUSAS finite element software. The details of the analysis were similar to those previously published [ 1. which had previously been found to be insensitive to age-hardening in a wrought duplex stainless steel [ 11. at a displacement rate of 1 mm/minute with a loading span of 80 m. mm. The tensile stress increased by approximately 10% over the same distances. J. The ferrite (Fe) microhardness (50 g) after ageing for both annealing temperatures was 380 & 30. which was calculated using the tensile specimen fracture surface area. 4. The results are shown in Fig. There is good agreement between the shear stress at fracture in the smooth and notched tests. The stresses at failure were calculated using the failure load. aged for 168 h at 475°C and tested at . The shear stress was taken as half the maximum true tensile stress. with occasional load drops before brittle fracture. A tensile specimen of the steel which had been annealed at 1100°C and tested at . Linear features in the gauge length of a tensile specimen of steel B. The hardness values are given in Table 1. The finite element model calculated that the shear stress ahead of the notch root decreased rapidly with increasing distance up to 140pm and then decreased by less than 20% between 140 pm and 1. 5. compared with the shear and tensile stresses at failure in the tensile tests. A clip strain gauge at the notch was used to monitor the specimen deflection.10°C. annealed at 1100°C and 1300"C.2]. were aged at 475°C for 168 h. The shear stress and tensile stress at the distance of 200 pm were taken to represent the average stress state operating over a distance of the order of the ferrite grain size. Fig. The stresses increased with strain hardening. The yield stress and failure load were used to determine the maximum shear and tensile stresses at the notch at failure. . Tensile and bend tests (steel B) Test specimens from steel B. 4). BURY and The Vickers hardness (30 kg diamond pyramid indenter) with ferrite Vickers microhardness (50 g diamond pyramid indenter) were measured for tests on either side of the brittle-to-ductile transition. MARROW N.01 s . Linear features were observed which spanned the Fe grains. All the samples failed in a brittle manner after yielding with plastic strains of up to 20%.1. Bend specimens with a 60" notch (notch root radius 250 pm) were tested in 3 point bending at the same temperatures.l at temperatures between .

It is important to determine whether twin nucleated cleavage is nucleation controlled (difficult crack nucleation. If cleavage is nucleated by the nucleation controlled Stroh mechanism [S]. The shear fracture stress (notched) and tensile fracture stress (notched) were calculated for the notched end specimens. If the twin length is large then the friction stress due to age-hardening is the most significant component of the fracture shear stress. The maximum shear stress at fracture is of the order of 400 MPa (Fig. Twin nucleated cleavage is generally considered to be nucleation controlled [3.v) G E where T~is the friction stress. b is the Burger’s length and D is the length of a dislocation pile-up equivalent to the arrested twin. then the critical shear fracture stress. For example. 5) are both consistent with deformation twinning. of 200 pm.28 and shear modulus of 81 GPa. 5). difficult crack propagation). with a pile-up length. z. The shear fracture stress (smooth) and tensile fracture stress (smooth) were measured in tensile specimens. easy crack propagation) or propagation controlled (easy crack nucleation. zf. A comparison of the shear and tensile stresses in notched and smooth specimens at the failure load in steel B. v is Poisson’s ratio. G is the shear modulus.4]. is 40 MPa. is zf = Ti + 7.25 nm.aged for 168 h at 475°C and tested between . This simplified the identification of the brittle-to-ductile transition.Brittle fracture of duplex stainless steels 569 2000 x 1 100°C : Sbear Fracture Stress (smooth) rm a a o 1100°C : Shear Fracture Stress (notched) + 1300°C : Shear Fracture Stress (smooth) A A Pm 500 0 A t A 13OO0C: Shear Fracture Stress (notched) 1 100°C : Tensile Fracturo Stress (smooth) 13OOOC : Tensile Fracture Stress (smooth) o 1100°C : Tensile Fracture Stress (notched) A i i -20 0 rn 13OO0C: Tmsile Fracture Stress (notched) -60 -40 TEMPERATURE(“C) Fig. producing brittle fracture within a shorter time in the 1300°C annealed steel. The acoustic emission during loading and the linear features in the ferrite (Fig. = 274 1 . Annealing steel A at 1100°C and 1300°C produced microstructures with different ferrite contents. D. 5. annealed at 1100°C and 1300”C. The change in ferrite chemical composition with increasing ferrite content increased the rate of age-hardening. It is proposed that ferrite cleavage in cast duplex stainless steels is deformation twin nucleated. Burger’s length of 0. Brittle fracture in a wrought duplex stainless steel was caused by deformation twinning [ 11. but with a comparable ferrite subgrain size and a small difference in ferrite grain size (Table 1). then z.10°C and -60°C. DISCUSSION The brittle-to-ductile transition The coarse ferrite grain size ensured that the brittle fracture propagating in one grain was sufficient to cause failure. The friction stress would therefore account for . Poisson’s ratio of 0.

There is no conclusive evidence that the brittle-to-ductile transition in ferritic and duplex stainless steels is mechanism controlled [ 1. The results for steel A indicate that brittle fracture occurs above a critical ferrite microhardness of between approximately 550 and 590 in the steel annealed at 1100°C and between 490 and 540 in the 1300°C annealed steel. The critical microhardness may or may not be affected by microstructure. The length of the arrested twin would therefore have no effect on the brittle-to-ductile transition. and the brittle-to-ductile transition may therefore depend on plastic relaxation of the elastic strain at the tip of an arrested twin. microstructure and ferrite microhardness on the brittle-to-ductile transition is expected. The maximum tensile stress in the ferrite would then depend on the ferrite yield strength and the level of constraint. The finite element model. both mechanisms predict that the brittle-to-ductile fracture transition depends on the ferrite microhardness. Duplex stainless steels are clean steels and no evidence has been found suggesting that cleavage is nucleated at large brittle inclusions. acting over a distance of the order of the grain size. which would be determined by the ferrite yield strength. The low failure stress observed in steel A.2]. Alternatively.570 T. An effect of constraint. The fracture energy is y. The notch effect. The decrease in the critical ferrite microhardness of the brittle-to-ductile transition with increasing twin length is not consistent with a nucleation controlled cleavage mechanism and supports propagation controlled cleavage. the brittle-to-ductiletransition will depend on both the crack nucleus size and the maximum tensile stress in the ferrite. In smooth tensile specimens. This is supported by the observation of cleavage in the centre of the fracture surface of necked tensile specimens [l]. shows that brittle fracture required a critical shear stress. Fracture occurred after yielding. The nucleated crack length therefore increases with the length of the twin. The critical shear stress to nucleate cleavage is therefore expected to be very insensitive to the ferrite content and ferrite grain size. but higher than the yield stress. and the critical shear stress was similar to. annealed at 1300°C . measurable as the ferrite microhardness. afnb = 2y (3) where n and b are the number and the Burgers length of the dislocations in a dislocation pile-up equivalent to the arrested twin. Annealing at the higher temperature increased the average ferrite grain size. The strain hardening rate in duplex stainless steels is low [ 11 and consequently the calculated critical shear stress for brittle fracture is close to the shear stress at yield. strain hardening is necessary to achieve a sufficient tensile stress for the propagation of cracks nucleated at yield. This fracture criterion is equivalent to a critical shear stress acting over a critical distance. BURY and approximately 90" of the fracture stress. which was similar in both notched and smooth specimens. It is suggested that the tensile stress near the notch tip generally exceeds the critical tensile stress for cleavage propagation. This would be controlled by the effects of agehardening and temperature on the mobility and ease to cross-slip of dislocations [S]. and brittle fracture requires crack nucleation within a critical volume ahead of the notch tip. This volume may reasonably be assumed to depend on the microstructure and to be related to the probability of forming a favourably oriented crack nucleus. Hence. J. MARROW N. According to the Cottrell mechanism of crack nucleation at intersecting twins and dislocations [81. decreasing the critical tensile fracture stress. if there is a mechanism of easy crack nucleation by deformation twinning [7]. however. The preceding discussion concluded that brittle fracture required a critical tensile stress. the brittle-to-ductile transition occurs at a critical tensile stress. with no change in the ferrite subgrain size (Table 2). of. depending on the crack nucleation mechanism.

T. The tensile stress at the tip of a sharp crack is higher than that ahead of a blunt notch. similar to that observed in the two heat treatments of steel A. W. Vol. T. Stroh (1955) The formation of cracks in plastic flow 11. 215-230. ferrite hardness and temperature on the fracture toughness of duplex stainless steels. Ghosh (1987) On the microstructural theories of stress-induced cleavage microcracking in crystalline solids. AIME. since the twin length is the ferrite grain size. Marrow (1996) The fracture mechanism in 475°C embrittled ferritic stainless steels. as observed in steel A (Fig. Fatigue Fract.232A. D. K. Both microstructures of steel B were tested below their brittle-to-ductile transition temperature. Lagneborg (1967) Yielding and fracture of Fe-30%Cr alloys subjected to 475°C-embrittlement. Harris (1996) The fracture mechanism of 475°C embrittlement in a duplex stainless steel. there is no experimental evidence positively identifying this mechanism. The yield stress of an age-hardened duplex stainless steel is dominated by the ferrite yield stress and depends on the ferrite content.Brittle fracture of duplex stainless steels 571 and aged for 640h implies that the ferrite microhardness was sufficiently high to propagate microcracks nucleated by the small number of twins formed below the yield stress. New York. SOC. Engng Muter. Taylor for the provision of facilities at the Manchester Materials Science Centre. although a difference in the brittleto-ductile transition temperature or hardness is expected. H. 935-947. Hull (1960) Twinning and fracture in single crystals of 3% silicon iron. 11-18. A. 192-203. SOC. J. 6. 62. McMahon (1967) The microstructural aspects of tensile fracture. However. Mech. 2). 919-933. Acta Polytech. pp. Acknowledgements-The authors would like to thank Professors G. Lorimer and R. Scand. The brittle-to-ductile transition temperature depends on the stress state. is considered to have counteracted the effect of ferrite content. 548-560. N. J. Trans Metall. 7. the yield stress of the 1300°C annealed steel B was not significantly higher than the 1100°C annealed steel B. 19. which is analogous to a critical shear stress acting over a critical distance. Plenum. Sarfarazi and S. I. Fatigue Fruct. Roy. A. Struct. 247-284. The fracture toughness of fatigue cracked age-hardened duplex stainless steels should therefore be determined by the development of a critical yielded volume. 212. Proc. Struct. Both heat treatments of steel B therefore had similar fracture behaviour. J. 27. 5. despite the significant increase in ferrite content. Acta Metall. Propagation controlled cleavage requires an easy crack nucleation mechanism. the ferrite microhardness and the ferrite grain size. Both steels has similar ferrite microhardness and yield occurred by twinning. Engng Fract. 3. Fundamental Phenomena in the Material Sciences. Engng Muter. REFERENCES 1. Work is in progress to develop a model for the effects of microstructure. Ch. Fracture occurred in the notched samples when the grains around the notch root yielded and after some strain hardening of the smooth tensile specimens. . Cottrell (1958) Theory of brittle fracture in steel and similar metals. R. CONCLUSIONS Brittle fracture in age-hardened (475°C embrittled) duplex stainless steels is twin nucleated and propagates at a critical tensile stress. At present. Marrow and C. C. 8. 8. 19. The increase in grain size and consequent decrease in the critical shear stress for yield by twinning. M. 4. 2. 4.