art ic l e i nf o a b s t r a c t
Article history: The effect of surface grinding on the stress corrosion cracking (SCC) behavior of 304L austenitic stainless
Received 21 December 2015 steel in boiling magnesium chloride has been investigated. SCC tests were conducted both without ex-
Accepted 25 January 2016 ternal loading and with varied levels of four-point bend loading for as-delivered material and for spe-
Available online 29 January 2016
cimens which had been ground parallel or perpendicular to the loading direction. Residual stresses due
Keywords: to the grinding operation were measured using the X-ray diffraction technique. In addition, surface stress
Stress corrosion cracking measurements under applied load were performed before exposure to evaluate the deviation between
Residual stress actual applied loading and calculated values according to ASTM G39. Micro-cracks initiated by a high
Austenitic stainless steel 304L level of tensile residual stress in the surface layer were observed for all the ground specimens but not
Grinding
those in the as-delivered condition. Grinding along the loading direction increased the susceptibility to
chloride induced SCC; while grinding perpendicular to the loading direction improved SCC resistance.
Surface tensile residual stresses were largely relieved after the initiation of cracks.
& 2016 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2016.01.078
0921-5093/& 2016 Elsevier B.V. All rights reserved.
N. Zhou et al. / Materials Science & Engineering A 658 (2016) 5059 51
Fig. 1. Cross-section microstructure and grain orientation of 304L austenitic stainless steel as-delivered.
Fig. 4. In-depth residual stresses and full width at half maximum proles of (a) as-delivered material, (b) ground specimen. Positive values denote tensile stresses and
negative compressive stresses.
Fig. 5. Measured surface stresses in the loading direction for four-point bending of (a) as-delivered material, (b) ground specimens.
54 N. Zhou et al. / Materials Science & Engineering A 658 (2016) 5059
Fig. 7. Surface morphology after exposure without external loading: (a) as-delivered specimen, (b) ground-RD specimen.
deformed surface layer comprised of fragmented grains and dis- 3.3. Corrosion behavior with four-point bend loading
location sub-cells only a few microns in thickness. Below this layer,
densely populated slip bands with multiple orientations were 3.3.1. Macro-crack examination
observed. Both the ground-RD and ground-TD specimens show Macro-cracks developed in some specimens exposed with ex-
similar features from the cross-section investigations. As illu- ternal loading and could result in sample fracture. Macro-cracks
strated in Fig. 8(a), micro-cracks in the absence of external loading are dened in this study as those that can be observed by stereo
appeared mainly perpendicular to the grinding marks i.e. per- microscopy with highest magnication 63. Table 3 gives a
pendicular to the direction of highest residual tensile stress. The summary of the macro-crack examination from the corrosion test
cracks initiated from the ground surface and ranged in length from under different four-point bend loading values as well as without
less than 1 mm up to more than 10 mm. The micro-cracks were thus external loading. No macro-cracking occurred during exposure
largely within the highly deformed surface layer. On the other without external loading regardless of surface conditions. How-
hand, in the section parallel to the grinding marks (Fig. 8(b)), only ever for specimens under four-point bending, one out of three as-
small rather blunt points of attack were seen; these had not de- delivered specimens loaded to 50 MPa was cracked through
veloped into cracks. The results agree well with the surface mor- thickness after exposure in boiling MgCl2 for 24 h. With increasing
phology investigation. Detailed microstructural characterization at the applied loading up to 110, 200 and 300 MPa respectively, all
higher magnication revealed that both intergranular micro- the exposed as-delivered specimens cracked. For the ground-RD
cracks (Fig. 8(c)) and transgranular micro-cracks (Fig. 8(d)) were specimens, large cracks were observed on both specimens with
present. Some branching occurred (Fig. 8(d)) and cracks could run 50 MPa or 300 MPa loading. In the case of ground-TD specimens
parallel to and across deformation slip bands. no macro-cracks were seen at applied load levels of 50 MPa or
110 MPa.
Fig. 8. Cross-section microstructures after exposure without external loading: (a) ground-RD specimen sectioned parallel to the rolling/grinding direction, (b) ground-RD
specimen sectioned perpendicular to rolling/grinding, (c) ground-RD specimen showing intergranular micro-crack, (d) ground-RD specimen showing transgranular micro-
crack and multi-branched micro-crack.
N. Zhou et al. / Materials Science & Engineering A 658 (2016) 5059 55
Table 3
Extent of micro- and macroscopic cracking after exposure with four-point bend loading. The measured surface stresses from Figs. 4 to 5 are also included for comparison.
Specimen Applied four-point bend Measured (or interpolated) sur- Exposure time No. of specimens No. of specimens with Presence of micro-
loading (MPa) face stress (MPa) tested macro-cracks cracks
3.3.2. Surface morphology after exposure marks. This applied even for the ground-TD specimens, which
Initial examination of the cracked surfaces was performed by means that the residual stress effect outweighed the effect of the
stereo microscopy. When cracking occurred, there were usually applied load and the possible notch effect from the grinding
multiple cracks, with one major crack extending nearly through marks.
the specimen. The cracks tended to run parallel to each other, and
were all perpendicular to the loading direction. 3.3.3. Cross-section investigation after exposure
Detailed characterization of all the three types of specimens Cross-sections parallel to the loading direction were examined
after testing at 50 MPa four-point bend loading is shown by the for all the cracked specimens after exposure. Fig. 10 presents SEM
SEM micrographs in Fig. 9. The macro-cracks were wide and ex- images of two specimens as examples: the AD and ground-RD
hibited multiple branching (Fig. 9(a) and (c)). Pitting was observed specimens with 50 MPa applied load. These show that the macro-
in varying degrees for all specimens. Even in the absence of macro- crack path was mainly branched transgranular, in good agreement
cracks, large pits were found, as exemplied by the as-delivered with the fracture surface investigation (see below). Pits were
specimen shown in Fig. 9(b). Pits were also seen on the ground evident on the surface and macro-cracks were always associated
surfaces and showed some tendency to follow the micro-cracks. with such pits, i.e. always initiated and propagated from the pits.
Cracks were sometimes seen to extend from pits, indicating that Micro-cracks were also observed to initiate from the surface and
pits may be precursors to cracks. Similar to the corrosion tests have penetration depths of up to 10 mm, but these were not nor-
without external loading, micro-cracks with extensive branching mally associated with pits (Fig. 10(b)). No micro-cracking was
were also found on the exposed surfaces of all ground specimens observed in AD cross-section (Fig. 10(a)).
regardless of loading or the occurrence of macro-cracks. Micro- Cross-sections both parallel and perpendicular to the loading
cracks were primarily oriented perpendicular to the grinding directions of all the ground specimens after exposure under
Fig. 9. Surface morphology after exposure with 50 MPa four-point bend loading: (a) as-delivered cracked specimen, (b) as-delivered uncracked specimen, (c) ground-RD
cracked specimen, (d) ground-TD uncracked specimen. The loading direction is horizontal in all cases.
56 N. Zhou et al. / Materials Science & Engineering A 658 (2016) 5059
Fig. 10. Cross-section microstructures showing stress corrosion cracking after exposure with 50 MPa four-point bend loading: (a) as-delivered specimen sectioned in the
longitudinal direction, (b) ground-RD specimen sectioned in the longitudinal direction.
Fig. 11. Cross-section microstructures after exposure with 50 MPa four-point bend loading showing: (a) ground-RD specimen parallel to rolling/grinding direction,
(b) ground-TD specimen perpendicular to rolling/grinding direction, (c) surface pit and micro-cracks in ground-RD specimen, (d) surface pit and micro-cracks in ground-TD
specimen.
Fig. 12. Fracture surfaces after exposure: (a) as-delivered specimen under 50 MPa loading, (b) ground-RD specimen under 50 MPa loading.
different applied loads were examined by ECCI. Images of two agreement with the surface morphology results. For the ground-
specimens are illustrated in Fig. 11 as examples. A high density of RD specimens, 50 MPa four-point bend loading signicantly in-
pits and micro-cracks was observed for all the specimens, in creased the density and size of the pits. The penetration depth of
N. Zhou et al. / Materials Science & Engineering A 658 (2016) 5059 57
micro-cracks also obviously increased, especially for cracks per- may be recalled that this specimen exhibited no macro-cracking.
pendicular to the loading/grinding direction (Fig. 11a), when In-depth residual stress prole of a ground-RD specimen before
comparing with the same specimen exposed without external and after exposure in the absence of external loading is presented
loading. For the ground-TD specimen, the same load also sig- in Fig. 14. Residual stresses were measured both parallel and
nicantly increased the penetration depth and density of micro- perpendicular to rolling/grinding directions of the specimen. As
cracks perpendicular to the loading direction i.e. parallel to the shown in the gure, the tensile component reduced dramatically
grinding direction (Fig. 11(b)). However the change was small for after exposure from surface to sub-surface until reaching zero at
micro-cracks parallel to the loading direction. Higher magnica- the depth where nearly all the micro-cracks stopped. The change
tion characterization revealed that multiple cracks often origi- of compressive component showed small, in-depth residual
nated from a single pit (Fig. 11 (c) and (d)), which also agrees with stresses showed similar values before and after exposure.
the exposed surface observation. Both transgranular and inter- In-depth surface morphology (Fig. 14) was also characterized of
granular micro-cracks were observed to be associated with pits this specimen with different distances from the original surface.
(Fig. 11 (c)) and these could run parallel to or across the de- The penetration depths of micro-cracks were very uneven. Some
formation slip bands (Fig. 11(d)). of them disappeared after 2 mm of surface has been polished away,
while some penetrated to a depth more than 10 mm from surface.
3.3.4. Fracture surface investigation Very few micro-cracks can be observed at 13 mm electrolytic pol-
Fig. 12 presents SEM images showing fracture surfaces of both ishing depth. The results agree with the cross-section observation.
as-delivered and ground-RD specimens which cracked at 50 MPa
applied stress. The fracture appearance of both specimens shows
typical cleavage fracture which is predominantly transgranular, 4. Discussion
although there are also some local indications of intergranular
cracking. Some indications of crack branching are seen for both of 4.1. Residual stress distribution
the specimens.
Residual stresses for the as-delivered material are close to zero,
3.4. Stress relaxation after exposure while grinding operations generated massive residual stresses in
the surface and sub-surface layers of the steel. During grinding,
Surface stresses of ground specimens before and after exposure thermally and mechanically induced residual stresses may be
under different loading conditions were measured to correlate the produced simultaneously; the relative signicance varies from one
SCC behavior and residual stresses; the results are presented in process to another [25]. Heat is generated from the interaction
Fig. 13. The grinding operations generated tensile residual stresses between the abrasive grit and the workpiece material during
up to more than 350 MPa parallel to the grinding direction and grinding operations. Due to the low thermal conductivity of 304L
compressive residual stresses in the perpendicular direction. For stainless steel, a temperature gradient is formed from surface to
the ground-RD specimen (Fig. 13(a)), after 40 h exposure without the bulk. During the cooling period, contraction of the surface
applying any external loading, surface tensile stresses parallel to layer is hindered by the bulk thus resulting in surface tension and
the grinding marks signicantly reduced to below 100 MPa; while subsurface compression [25,26]. However, in the present case
perpendicular to the grinding marks, compressive stresses in- tensile residual stresses parallel to the grinding direction and
creased slightly. These effects can be directly related to the for- compressive residual stresses perpendicular to the grinding di-
mation of micro-cracks which relax the surface tensile stress. After rection were observed. This measured anisotropic surface residual
exposure at 50 MPa applied load, surface tensile residual stresses stress can be attributed to the anisotropic plastic deformation of
reduced even more, to below 50 MPa, this is attributable to the the ground surface layer, and indicates that residual stresses in-
formation of both micro- and macro-cracks. The change in the duced by mechanical effects dominate over thermal effects in this
perpendicular direction was again small. For 300 MPa loading, study. The surface layer experienced compressive plastic de-
surface stress reduced to zero in the loading direction. In the case formation in the grinding direction and tensile deformation in the
of ground-TD specimen (Fig. 13(b), the surface stress relaxation transverse direction. After the grinding zone moved away, the
due to exposure without external loading was similar to the constraint by the material beneath surface resulted in tensile but
ground-RD specimen. The inuence of applied loading up to compressive in the surface layer [20,27]. Such anisotropic re-
110 MPa on surface stress relaxation was relatively small, and it sidual stress distributions have also been observed in previous
Fig. 13. Measured surface residual stress of ground specimens parallel and perpendicular to rolling and grinding directions before and after exposure: (a) ground-RD
specimen, (b) ground-TD specimen.
58 N. Zhou et al. / Materials Science & Engineering A 658 (2016) 5059
stress is dominant here. In contrast, the improvement of SCC re- Duplex stainless steel world conference, Beaune, 2010.
sistance of ground-TD specimens was also clear; although the in- [2] D.A. Jones, Principles and Prevention of Corrosion, Pearson Education, US,
1996.
duced compressive residual stresses were entirely released during [3] S. Ghosh, V. Kain, Effect of surface machining and cold working on the ambient
loading and were then converted into a state of tension, much temperature chloride stress corrosion cracking susceptibility of AISI 304L
higher level of compressive residual stresses beneath the ground stainless steel, Mater. Sci. Eng. A 527 (2010) 679683.
surface compensated for the surface tension and effectively re- [4] W. Jin, S. Yang, H. Kokawa, Z. Wang, Y.S. Sato, Improvement of intergranular
stress corrosion crack susceptibility of austenite stainless steel through grain
tarded the appearance of macro-cracks. The results suggest the boundary engineering, J. Mater. Sci. Technol. 23 (2007) 785789.
idea that grinding transverse to the main stress direction in a [5] S. Ghosh, V.P.S. Rana, V. Kain, V. Mittal, S. Baveja, Role of residual stresses
construction could possibly be used to decrease the cracking risk. induced by industrial fabrication on stress corrosion cracking susceptibility of
austenitic stainless steel, Mater. Des. 32 (2011) 38233831.
[6] A. Turnbull, K. Mingard, J. Lord, B. Roebuck, D. Tice, K. Mottershead,
N. Fairweather, A. Bradbury, Sensitivity of stress corrosion cracking of stainless
5. Conclusions steel to surface machining and grinding procedure, Corros. Sci. 53 (2011)
33983415.
[7] S. Ghosh, V. Kain, Microstructural changes in AISI 304L stainless steel due to
The effect of surface grinding on chloride induced stress cor-
surface machining: effect on its susceptibility to chloride stress corrosion
rosion cracking of austenitic stainless steel 304L has been in- cracking, J. Nucl. Mater. 403 (2010) 6267.
vestigated. The following conclusions can be drawn: [8] K. Lyon, T. Marrow, S. Lyon, Inuence of milling on the development of stress
corrosion cracks in austenitic stainless steel, J. Mater. Process. Technol. 218
Grinding generated tensile residual stresses parallel to the (2015) 3237.
[9] W. Karlsen, G. Diego, B. Devrient, Localized deformation as a key precursor to
grinding direction ( ) but compressive residual stresses per- initiate of intergranular stress corrosion cracking of austenitic stainless steels
pendicular to the grinding direction ( ) in the surface layer. employed in nuclear power plants, J. Nucl. Mater. 406 (2010) 138151.
Beneath the ground surface, a layer of compressive stresses in [10] J. Lu, K. Luo, X. Cheng, J. Hu, F. Dai, H. Qi, L. Zhang, J. Zhong, Q. Wang, Y. Zhang,
Effects of laser peening on stress corrosion cracking (SCC) of ANSI 304 aus-
both directions was formed with much higher values in the
tenitic stainless steel, Corrosion Science 60 (2012) 145152.
perpendicular direction. The residual stress distribution ob- [11] B. Kumar, R. Singh, B. Mahato, P. De, N. Bandyopadhyay, D. Bhattacharya, Effect
served in this study indicated that anisotropic mechanical ef- of texture on corrosion behavior of AISI 304L stainless steel, Mater. Charact. 54
fects dominated over isotropic thermal effects from grinding. (2005) 141147.
Stress measurements on four-point bend loaded specimens
[12] M. Meisnar, A. Vilalta-Clemente, A. Gholinia, M. Moody, A.J. Wilkinson,
N. Huin, S. Lozano-Perez, Using transmission Kikuchi diffraction to study in-
demonstrated that the actual loading may deviate appreciably tergranular stress corrosion cracking in type 316 stainless steels, Micron 75
from that calculated according to the formula in ASTM G39. For (2015) 110.
annealed material with low residual stresses the formula gave a [13] S.-l Baik, M. Olszta, S. Bruemmer, D.N. Seidman, Grain-boundary structure and
segregation behavior in a nickel-base stainless ally, Scr. Mater. 66 (10) (2012)
reasonable estimate of the applied stress up to the proof stress.
809812.
For surface ground material there was a linear relationship up to [14] S.M. Bruemmer, M.J. Olszta, M.B. Toloczko, L.E. Thomas, Linking grain bound-
much higher loads but the absolute value was strongly affected ary microstructure to stress corrosion cracking of cold rolled alloy 690 in
by residual stresses from grinding. PWRprimary water, Corrosion (2012) 95129527.
Surface tensile residual stresses were found to be the main
[15] E. Johansson, T. Prosek, Stress corrosion cracking properties of UNS S32101- a
new duplex stainless steel with low nickel content, in: Proceedings of the
factor causing the initiation of micro-cracks on ground surfaces Corrosin 2007 Conference & Expo, 2007.
during exposure with or without an externally applied load. [16] ASTM, G39-99, Standard Practice for Preparation and Use of Bent-beam Stress-
Crack arrest occurred when micro-cracks grew into a region 10 corrosion Test Specimens, 2011.
[17] ISO, 7539, Corrosion of Metals and Alloys Stress Corrosion Testing, 1995.
15 mm below the surface with low or no tensile residual stresses. [18] U. Kiviskk, G. Chai, Inuence of test method and relaxation on the result from
Macroscopic cracking leading to nal failure only occurred un- stress corrosion cracking tests of stainless steels in dilute neutral chlorides,
der an applied load and there appeared to be a threshold at load Corrosion 59 (2003) 828835.
[19] N. Zhou, R.L. Peng, R. Pettersson, Surface characterization of austenitic stain-
of around 50 MPa. A residual tensile stress in the grinding di-
less steel 304L after different grinding operations, J. Mater. Process. Technol.
rection increased the susceptibility to chloride-induced SCC (2015), under review.
while grinding perpendicular to the applied loading direction [20] I. Noyan, J. Cohen, Residual Stress Measurement by Diffraction and Inter-
retarded cracking. It is therefore suggested that grinding pretation, Springer-Verlag New York Inc, New York City, United States, 1987.
[21] N. Zhou, R. Lin Peng, R. Pettersson, Surface integrity of 2304 duplex stainless
transverse to the main stress direction in a construction could
steel after different grinding operations, J. Mater. Process. Technol. 229 (2016)
possibly be used to decrease the cracking risk. 294304.
Pits tended to initiate at micro-cracks on the surface, and [22] ASTM, G36-94, Standard Practice for Evaluating Stress-Corrosion-Cracking
macro-cracks were always associated with pits. This indicates Resistance of Metals Aned Alloys in a Boiling Magnesium Chloride Solution,
Reapproved 2006.
that pits formed before macro-cracks and acted as precursors to [23] V. Roy, B. Nahak, M.Z.K. Yusufzai, M. Vashista, Assessment of plastic de-
macroscopic crack development. formation upon grinding using X-ray diffraction proles, Int. J. Eng. Res. 2 (2)
(2013) 119124.
[24] S. Johansson, J. Moverare, R. Peng, Recent applications of scanning electron
microscopy, Pract. Metallogr. 50 (2013) 810820.
Acknowledgment [25] J.P. Davim, Surface Intergrity in Machining, Springer London Ltd, London,
2010.
This work was performed within the Swedish Steel Industry [26] N.B. Fredj, H. Sidhom, C. Braham, Ground surface improvement of the auste-
nitic stainless steel AISI 304 using cryogenic cooling, Surf. Coat. Technol. 200
Graduate School with nancial support from Outokumpu Stainless
(2006) 48464860.
Research Foundation, Region Dalarna, Region Gvleborg, Lns- [27] G. Guo, Z. Liu, X. Cai, Q. An, M. Chen, Investigation of surface integrity in
styrelsen Gvleborg, Jernkontoret, Sandviken Kummun and conventional grinding of Ti6Al4V, Adv. Mater. Res. 126128 (2010) 899904.
Hgskolan Dalarna. The assistance with part of the sample pre- [28] P. Marcus, Corrosion Mechanisms in Theory and Practice, CRC Press Inc, Boca
Raton, 2012.
paration work by Ulf Modin at Hgskolan Dalarna is also appre- [29] R. Lin Peng, J. Gibmeier, G. Chai, S. Johansson, Load Partitioning in a Duplex
ciated. The authors are grateful to Timo Pittulainen at Outokumpu Stainless Steel With Surface Strength Gradient and Residual Stresses, in:
Stainless AB for providing the test materials and the material data. JCPDS-International centre for diffraction data, 2009.
[30] G. Hinds, L. Wickstrm, K. Mingard, A. Turnbull, Impact of surface condition on
References sulphide stress corrosion cracking of 316L stainless steel, Corros. Sci. 71 (2013)
4352.