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 475C 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 475C 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; 475C ernbrittlement; Deformation twinning; Brittle-to-ductile transition; Age hardening.

NOMENCLATURE
b = Burgers 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 = Poissons 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 (475C 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 475C 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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T. J. MARROW N. BURY and

This paper addresses some of these concerns and attempts to identify the important microstructural parameters which control the ductile-to-brittle transition. A similar finite element analysis has been used to determine the effects of the notch, ferrite content, ferrite microhardness, ferrite subgrain size and ferrite grain size in heat treated cast duplex stainless steels.
EXPERIMENTAL DETAILS AND RESULTS

Materials Two cast duplex stainless steels were used. Energy dispersive X-ray analysis gave the following compositions (in wt.%): Steel A (25.5 Cr, 6.3 Ni, 3.8 Mo, 0.8 Mn), and steel B (25.4 Cr, 5.6 Ni, 2.0 Mo, 0.7 Mn, 0.5 Si). The light element content was not determined. Both steels were annealed as blanks at 1100C and 1300C for 1 h and water quenched. Test specimens were then machined and aged at 475C for up to 640 h. The ferrite contents were determined using image analysis of metallographic samples electrolytically etched in 30% KOH solution. The ferrite subgrains were revealed by an electrolytic oxalic acid etch, and the ferrite grain size was inferred from the distribution of the austenite (Fig 1). The results are given in Table 1, with the Vickers hardness (30 kg diamond pyramid indenter) after ageing for approximately one week at 475C. Tensile tests (steel A) Tensile tests (diameter 5 mm) were performed at a strain rate of 0.01 s - l at room temperature (20C) using steel A. The proof stress at 1% plastic strain was taken as the yield stress. Audible clicking (acoustic emission) was heard well below the yield stress in all samples, increasing in

Fig. 1. Duplex stainless steel microstructures: (a) steel A, annealed at 1100C for 1 h and water quenched, (b) steel A, annealed at 1 3 0 C for 1 h and water quenched.

Steel and Annealing temperature

SteelA 1l00"C

SteelA 10' 30C 723

1000+200

Steel3
1looOC

SteelB 1300C
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.i4

14 % 408i22

16a4 346f6

32&8

Brittle fracture of duplex stainless steels

567

5Wr
-0 0 0

Fracture stress
4W
450 500

s'i

AGEING TIME (hours)

MCKERS HARDNESS

Fig. 2. Effect of annealing temperature (1100C and 1300C) on the relationship between Vickers hardness (30 kg): (a) ageing time, (b) yield stress (1% proof stress). The tensile fracture stress for tests which failed without yielding, and the critical hardness for the brittle-to-ductile transitions (BDT) are also shown.

frequency at yield with very little emission after yield. The effect of ageing time on yield stress, hardness and fracture behaviour was determined. The results are shown in Fig. 2. Ageing had a greater effect on the hardness of the 1300C annealed steel. Both steels showed the same linear dependence of yield stress and hardness, except for the 1300C annealed steel aged for 640 h (hardness 447 & 20). This material failed below the expected yield stress. A transition from ductile to brittle fracture was observed with increasing hardness. The fracture surface was either completely ductile (Fig. 3(a)) or completely brittle with ferrite cleavage and ductile shearing of the austenite (Fig. 3(b)). No samples failed with both cleavage and ductile failure of the ferrite. Brittle fracture generally occurred after yielding with plastic strains of the order of 3-10%. Only the material annealed at 1300C and aged for 640 h failed without yielding.

Fig. 3. The effect of ageing time on the fracture of steel A, annealed at 1100C. (a) Ductile fracture (aged for 48 h). (b) Brittle fracture (aged for 640 h).

Table 2. The Vickers hardness and ferrite microhardness on either side of the brittle-to-ductile transition in steel A, annealed at 1100C and 1300C and aged at 475C Ageing time (hours) Fracture mode Vickers hardness (30 kg)

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T. J. MARROW N. 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. These results are in Table 2.
Tensile and bend tests (steel B) Test specimens from steel B, annealed at 1100C and 1300"C, were aged at 475C for 168 h. The hardness values are given in Table 1. The ferrite (Fe) microhardness (50 g) after ageing for both annealing temperatures was 380 & 30. Tensile tests (dia. 7 mm) were performed at a strain rate of 0.01 s - l at temperatures between - 10C and -60C. All the samples failed in a brittle manner after yielding with plastic strains of up to 20%. A tensile specimen of the steel which had been annealed at 1100C and tested at - 30C was sectioned along its axis for metallographic examination. Linear features were observed which spanned the Fe grains. They did not appear to be influenced by either the Fe subgrain boundaries or the austenite within the Fe grains (Fig. 4). Bend specimens with a 60" notch (notch root radius 250 pm) were tested in 3 point bending at the same temperatures, at a displacement rate of 1 mm/minute with a loading span of 80 m. A clip strain gauge at the notch was used to monitor the specimen deflection. All tests showed nonreversible plastic strain, with occasional load drops before brittle fracture. 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 [ 1,2]. The yield stress and failure load were used to determine the maximum shear and tensile stresses at the notch at failure. A strain hardening exponent of 0.1 was used, which had previously been found to be insensitive to age-hardening in a wrought duplex stainless steel [ 11. 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 1.1. mm. The tensile stress increased by approximately 10% over the same distances. The stresses increased with strain hardening. The behaviour close to the notch surface may be an artefact of the mesh used in the model. 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. The stresses at failure were calculated using the failure load. The results are shown in Fig. 5, compared with the shear and tensile stresses at failure in the tensile tests. The shear stress was taken as half the maximum true tensile stress, which was calculated using the tensile specimen fracture surface area. There is good agreement between the shear stress at fracture in the smooth and notched tests, and no agreement of the tensile stress. There is no significant difference between the results for the two microstructures.

Fig. 4. Linear features in the gauge length of a tensile specimen of steel B, annealed at 11Oo"C, aged for 168 h at 475C and tested at - 10C.

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2000

x 1 100C : Sbear Fracture Stress (smooth)

rm
a
a

o 1100C : Shear Fracture Stress (notched)

+ 1300C : Shear Fracture Stress (smooth)

A A

Pm
500
0

t
A

13OO0C: Shear Fracture Stress (notched) 1 100C : Tensile Fracturo Stress (smooth) 13OOOC : Tensile Fracture Stress (smooth)
o 1100C : Tensile Fracture Stress (notched)
A

i
-20
0

rn 13OO0C: Tmsile Fracture Stress (notched)

-60
-40

TEMPERATURE(C)

Fig. 5. A comparison of the shear and tensile stresses in notched and smooth specimens at the failure load in steel B, annealed at 1100C and 1300C,aged for 168 h at 475C and tested between - 10C and -60C. The shear fracture stress (smooth) and tensile fracture stress (smooth) were measured in tensile specimens. The shear fracture stress (notched) and tensile fracture stress (notched) were calculated for the notched end specimens.

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. This simplified the identification of the brittle-to-ductile transition. Annealing steel A at 1100C and 1300C produced microstructures with different ferrite contents, but with a comparable ferrite subgrain size and a small difference in ferrite grain size (Table 1). The change in ferrite chemical composition with increasing ferrite content increased the rate of age-hardening, producing brittle fracture within a shorter time in the 1300C annealed steel. Brittle fracture in a wrought duplex stainless steel was caused by deformation twinning [ 11. The acoustic emission during loading and the linear features in the ferrite (Fig. 5) are both consistent with deformation twinning. It is proposed that ferrite cleavage in cast duplex stainless steels is deformation twin nucleated. It is important to determine whether twin nucleated cleavage is nucleation controlled (difficult crack nucleation, easy crack propagation) or propagation controlled (easy crack nucleation, difficult crack propagation). Twin nucleated cleavage is generally considered to be nucleation controlled [3,4]. If cleavage is nucleated by the nucleation controlled Stroh mechanism [S], then the critical shear fracture stress, zf, is

zf = Ti + 7,
z, = 274 1 - v)

G E

where T~is the friction stress, G is the shear modulus, v is Poissons ratio, b is the Burgers length and D is the length of a dislocation pile-up equivalent to the arrested twin. If the twin length is large then the friction stress due to age-hardening is the most significant component of the fracture shear stress. For example, with a pile-up length, D, of 200 pm, Burgers length of 0.25 nm, Poissons ratio of 0.28 and shear modulus of 81 GPa, then z, is 40 MPa. The maximum shear stress at fracture is of the order of 400 MPa (Fig. 5). The friction stress would therefore account for

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T. J. MARROW N. BURY and

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

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. Both microstructures of steel B were tested below their brittle-to-ductile transition temperature. Fracture occurred in the notched samples when the grains around the notch root yielded and after some strain hardening of the smooth tensile specimens. The yield stress of an age-hardened duplex stainless steel is dominated by the ferrite yield stress and depends on the ferrite content, as observed in steel A (Fig. 2). However, the yield stress of the 1300C annealed steel B was not significantly higher than the 1100C annealed steel B, despite the significant increase in ferrite content. Both steels has similar ferrite microhardness and yield occurred by twinning. The increase in grain size and consequent decrease in the critical shear stress for yield by twinning, since the twin length is the ferrite grain size, is considered to have counteracted the effect of ferrite content. Both heat treatments of steel B therefore had similar fracture behaviour, although a difference in the brittleto-ductile transition temperature or hardness is expected, similar to that observed in the two heat treatments of steel A. The tensile stress at the tip of a sharp crack is higher than that ahead of a blunt notch. The fracture toughness of fatigue cracked age-hardened duplex stainless steels should therefore be determined by the development of a critical yielded volume, which is analogous to a critical shear stress acting over a critical distance. Work is in progress to develop a model for the effects of microstructure, ferrite hardness and temperature on the fracture toughness of duplex stainless steels. Propagation controlled cleavage requires an easy crack nucleation mechanism. At present, there is no experimental evidence positively identifying this mechanism.
CONCLUSIONS

Brittle fracture in age-hardened (475C embrittled) duplex stainless steels is twin nucleated and propagates at a critical tensile stress. The brittle-to-ductile transition temperature depends on the stress state, the ferrite microhardness and the ferrite grain size.
Acknowledgements-The authors would like to thank Professors G. W. Lorimer and R. I. Taylor for the provision of facilities at the Manchester Materials Science Centre.

REFERENCES
1. T. J. Marrow and C. Harris (1996) The fracture mechanism of 475C embrittlement in a duplex stainless steel. Fatigue Fract. Engng Muter. Struct. 19, 935-947. 2. T. J. Marrow (1996) The fracture mechanism in 475C embrittled ferritic stainless steels. Fatigue Fruct. Engng Muter. Struct. 19, 919-933. 3. D. Hull (1960) Twinning and fracture in single crystals of 3% silicon iron. Acta Metall. 8, 11-18. 4. M. Sarfarazi and S. K. Ghosh (1987) On the microstructural theories of stress-induced cleavage microcracking in crystalline solids. Engng Fract. Mech. 27, 215-230. 5. A. N. Stroh (1955) The formation of cracks in plastic flow 11. Proc. Roy. SOC.232A, 548-560. 6. C. J. McMahon (1967) The microstructural aspects of tensile fracture, Fundamental Phenomena in the Material Sciences, Vol. 4, pp. 247-284. Plenum, New York. 7. R. Lagneborg (1967) Yielding and fracture of Fe-30%Cr alloys subjected to 475C-embrittlement. Acta Polytech. Scand. Ch. 62. 8. A. H. Cottrell (1958) Theory of brittle fracture in steel and similar metals. Trans Metall. SOC. AIME. 212, 192-203.