Engineering Failure Analysis 17 (2010) 777–786

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Engineering Failure Analysis

journal homepage: www.elsevier.com/locate/engfailanal

Hydrogen-induced intergranular stress corrosion cracking (HI-IGSCC)

of 0.35C–3.5Ni–1.5Cr–0.5Mo steel fastener
Abhay K. Jha *, Sushant Manwatkar, K. Sreekumar
Materials Characterization Division, Materials and Metallurgy Group, Vikram Sarabhai Space Centre, Indian Space Research Organisation,
Trivandrum 695 022, India

a r t i c l e i n f o a b s t r a c t

Article history: This paper brings a failure case study of high strength 0.35C–3.5Ni–1.5Cr–0.5Mo steel fas-
Received 18 June 2009 tener, which failed due to hydrogen-induced intergranular stress corrosion cracking (HI-
Accepted 8 October 2009 IGSCC). 0.35C–3.5Ni–1.5Cr–0.5Mo steel in hardened and tempered condition, meeting
Available online 10 November 2009
the specified axial tensile stress rating of 1250 MPa is widely used as fasteners in space
programmes.
Keywords: In the course of assembly of the structural parts of a satellite launch vehicle, 10 nos of fas-
0.35C–3.5Ni–1.5Cr–0.5Mo steel
teners developed cracks on tightening using a torque wrench set to 6 N m torque surprisingly.
Hydrogen-induced stress corrosion cracking
Also some fasteners, which were under assembly load of more than 6 months in the same
vehicle assembly, were found to be cracked.
The failure was attributed to hydrogen-induced intergranular stress corrosion cracking
(HI-IGSCC). The details of the analysis and mechanism involved in the HI-IGSCC are presented
in detail.
Detailed metallurgical analyses of the cracked fasteners support the successive steps of the
corrosion enhanced plasticity model, which is based on a local softening in the SCC crack
region. The mechanism of a dislocation pileup ahead of a crack under corrosion and stress
due to diffusing hydrogen promotes stress concentration against micro-obstacle and caused
failure.
Ó 2009 Elsevier Ltd. All rights reserved.

1. Introduction

The 0.35C–3.5Ni–1.5Cr–0.5Mo steel in hardened and tempered condition, meeting the specified axial tensile stress rating
of 1250 MPa is used as fasteners in space programmes.
In the course of assembly of the structural parts of a satellite launch vehicle, 10 nos of M 6X1X20 – grade 12.9 Hex. Socket
Head cap bolt fasteners developed cracks on tightening using a torque wrench set to 6 N m torque surprisingly.
Some more fasteners from the same batch of supply, which were already in use, failed under assembly load. These fas-
teners were under assembly load of more than 6 months. All the fasteners were supplied in a single lot in March 2004.
The failed fasteners were subjected to detailed metallurgical investigation to determine the cause of the failure. An at-
tempt is made in this paper to correlate the metallurgical features collected with the failure mode of the fastener.

2. Material

The 0.35C–3.5Ni–1.5Cr–0.5Mo steel, used for making the fasteners was primary melted in an electric arc furnace and re-
fined under vacuum prior to casting into ingot. The chemical composition of the failed fastener is given in Table 1. The ingot

* Corresponding author. Tel.: +91 471 2563628; fax: +91 471 2705048.
E-mail address: [email protected] (A.K. Jha).

1350-6307/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.engfailanal.2009.10.007
778 A.K. Jha et al. / Engineering Failure Analysis 17 (2010) 777–786

Table 1
Chemical composition of the material.

C Mn P S Si Ni Cr Mo Fe
Specification 0.30–0.40 0.30–0.60 <0.02 <0.02 0.15–0.40 3.50–4.20 1.60–2.0 0.35–0.60 Balance
Actual 0.37 0.42 0.017 0.017 0.31 3.88 1.92 0.49 Balance

was homogenized, forged to breakdown the cast structure and subsequently rolled to rods. The threads were formed by
thread rolling. Subsequently, the thread rolled fasteners were hardened and tempered to achieve the specified mechanical
properties. Cadmium was electro deposited on the fasteners to provide corrosion protection during storage or in service and
also to act as a lubricant [1].

3. Observations

The failed bolts were classified into two categories, one that failed during application of torque and the other failed under
sustained assembly load. The fasteners belonging to the first category had bright fracture surface. The fracture surface of the
second category of failed bolt had relatively dark and dull appearance.

Fig. 1. Corroded thread roots of failed fasteners.

Fig. 2. The corroded thread roots of unused fasteners from the same lot.
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Fig. 3. Dimple mode of failure and presence of oxide at thread root.

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3.1. Case study: I

3.1.1. Fasteners failed during application of torque

The failed fasteners had bright fracture surface. The failure occurred at the threaded shank portion of the fasteners. Fea-
tures of corrosive attack were noticed on almost all the thread roots and the fracture was found to initiate at the region of
such corroded region (Fig. 1). Unused bolts from the same batch of supply, also revealed similar features at thread root
(Fig. 2).
Fracture surface under SEM revealed predominantly fine dimples, typical of tensile overload failure (Figs. 3 and 4). The
slant surface of the thread had deposits, verified to be oxide deposit (Fig. 3d) by energy dispersive spectroscopy (EDS).

Fig. 4. SEM fractographs showing dimple mode of failure.

Fig. 5. Damage at thread root, absence of sharp tip of crack and its branching (a) unetched and (b) etched specimen.
 A.K. Jha et al. / Engineering Failure Analysis 17 (2010) 777–786 781

The shank portion of the failed fasteners were sliced off along the shank axis and prepared for conventional metallogra-
phy. The polished specimens under a light optical microscope revealed cracks of depth up to 100 lm. The crack tip was blunt
and showed no secondary cracks or branching (Fig. 5). Microstructure consisted of the tempered martensite typical of hard-
ened and tempered steel (Fig. 6).

Fig. 6. Tempered martensite.

Fig. 7. Failed fasteners with cracked head–shank junction.

Fig. 8. Fracture surface, after opening at head–shank junction (black dull appearance).
782 A.K. Jha et al. / Engineering Failure Analysis 17 (2010) 777–786

3.2. Case study: II

3.2.1. Fasteners failed under sustained assembly load

These fasteners also failed at threaded regions and had a dull surface appearance with relatively darker fracture surface.
The fracture surface had brown oxide deposit at certain location. There was a distinct crack at head–shank junction (Fig. 7),
which was able to be opened up with application of minor force. The opened fracture surface (flat) had dark color region
throughout the fracture surface except for a small near circular region with diameter of 600 lm. This was located nearly
at centre of fracture surface and had bright appearance (Fig. 8). Scanning electron microscopy (SEM) of the fracture surface
showed predominantly intergranular mode of fracture with deposits of corrosion products (Fig. 9). At certain locations sec-
ondary cracks was also seen, which opened in intergranular mode (Fig. 9c). Certain other locations showed micro fractures
along slip plane due to dislocation pileup ahead of SCC crack leaving features of ductile tearing was seen (Fig. 10). The failed
fasteners sliced along the shank axis were observed under optical microscope (OM) after preparing the specimens. There
were multiple cracks, near fracture edge, which propagated into sub-surface of material along the grain boundaries
(Fig. 11). Microstructure consisted of typical tempered martensite. Presence of secondary cracks propagating along grain
boundaries and forming tree root branching was clearly visible (Fig. 12). Ion chromatography revealed the deposit contained
chloride ion up to 63 ppm.

4. Discussion

It is to be noted here that the fasteners failed were from the same batch of supply and hence observations can be clubbed
together to infer the cause of failure. The possible source for the corrosion at thread root is attributed to improper storage of
the fasteners. The depth of such defects was estimated to 100 lm. The fasteners with such defects failed under overload
mode as evidenced by dimple mode of failure. Such damage at thread root, caused breaking of the protective cadmium layer
and hence exposed the bare alloy to environmental corrosive attack. The presence of oxide on the slant surface of thread was
seen, indicating breaking of cadmium layer and oxidation of base alloy system.
The fasteners, which failed under sustained assembly load had dull color and deposit on fracture surface was rich in chlo-
ride ions. Once the protective layer was broken, the alloy was exposed to marine environment. The intergranular mode of
fracture indicated role of corrosion under stress. Presence of corrosion deposits on the facets of grain confirmed this.

Fig. 9. SEM fractographs showing (a–c) intergranular mode of fracture with presence of secondary cracks and (a, c) corrosion deposits on fracture surface.
 A.K. Jha et al. / Engineering Failure Analysis 17 (2010) 777–786 783

Fig. 10. SEM fractographs showing (a) predominantly intergranular mode of fracture and (b) ductile tearing and fracture along slip plane.

Instances of secondary cracks opening in intergranular mode were also seen. The intergranular mode of failure was also
confirmed by the ‘‘tree root branching” of cracks, resulted from crack propagation towards the sub-surface of the fracture
edge along the grain boundaries [2].
Fractographic features appeared on the failed components help in diagnosing the mode of failure. At many occasions, dif-
ferent modes of failure reveal similar features with minor variation. For example stress corrosion cracking (SCC), hydrogen
embrittlement (HE) in high strength steels usually exhibit intergranular fractures along the prior-austenite grain boundaries.
The minor variation between the two, which an analyst must look for is SCC fracture surfaces are often covered by a black
Fe3O4 (magnetite) film, whereas HE fractures are usually clean-unless they are exposed to moisture after fracture so that
brown deposit of Fe2O3:H2O film (rust) are formed. Magnetite films can, however form in cracks produced by HE if it initiates
internally and then cracks intersect surfaces that are exposed to aqueous environments [3].
The fasteners were electrodeposited with cadmium, and hence hydrogen entry and their entrapment also could not be
ruled out. In such cases hydrogen entry into alloy system are: (a) electrochemical steps, where hydrogen is produced due
to hydrogen partial cathodic reaction and (b) chemisorption step, where chemisorptive forces causes atomic hydrogen to
784 A.K. Jha et al. / Engineering Failure Analysis 17 (2010) 777–786

Fig. 11. Presence of multiple cracks propagating along the grain boundaries (a) at fracture edge and (b) into sub-surface of the material.

get attracted to the metal surface and finally allow it to migrate into metals [4]. The fasteners were electrodeposited with
cadmium, which was followed by hydrogen de-embrittlement (through baking) process. However time gap between the
two processes was not logged in. ASTM [5] advocates embrittlement relief treatment should commence preferably within
1 h but not later than 3 h after plating. Considering the probable delay in executing embrittlement relief treatment through
baking and entry of hydrogen in monoatomic form to discontinuities of material causing its embrittlement could not be ru-
led out.
The applicable hydrogen embrittlement mechanism are summarized as hereunder.
Hydrogen-induced local plasticity (HELP) [6] believes that hydrogen causes an increase in plasticity on microscopic scale.
Louthan et al. [7] and Beachem [8] suggested that hydrogen accumulation ahead of crack tip usually modify the process of
plastic deformation and fracture. The increased plasticity due to hydrogen-dislocation motion at the crack tip, caused local
softening of material and often results in ductile tearing on a localized scale. Jha et al. [9] reported evidence of such ductile
tearing on intergranular facets of similar cadmium electrodeposited fasteners made of 0.35C–3.5Ni–1.5Cr–0.5Mo steel,
which failed due to hydrogen embrittlement. In the present case study, intergranular facets were predominantly smooth,
however features of ductile tearing and separation along slip plane were evidenced due to local softening of material.
Hydrogen-enhanced de-cohesion (HEDE) mechanism believes that monoatomic hydrogen travels to a region of high tri-
axial stress site. Sufficient high concentration of hydrogen ahead of the crack tip lowers the cohesive forces of metallic bond
such that the local tensile stress (residual/assembly stress) perpendicular to plane of crack becomes greater than the cohe-
sive force. This results in crack advancement along the metallurgical discontinuities, preferably along grain boundaries and
hence intergranular facets. In such case, failure mode is usually characterized by failure along grain boundaries and at
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Fig. 12. Intergranular crack propagation within the material.

dislocation slip band intersection which otherwise will have features characteristic of microvoid formation and coalescence
[10–13]. In the present case, failure was intergranular and hence possibility of HEDE mechanism exists.
Above evidence indicated that fasteners failed due to SCC assisted by hydrogen which was consequence of presence of
hydrogen and stress under sustained load in steel fasteners [10].

5. Conclusions

1. Fracture surface revealed intergranular mode of fracture with presence of corrosion product on grain facets.
2. Presence of chloride ions was detected through ion chromatography and metallurgical investigation confirmed crack
propagation in intergranular mode towards sub-surface of the fasteners.
3. The fasteners failed due to hydrogen assisted stress corrosion cracking.

Acknowledgements

The authors are thankful to Dr. P.P. Sinha, Deputy Director, VSSC (MME) for his technical support during the investigation.
They are indebted to Dr. K. Radakrishnanan, Director, VSSC for permission to publish this work.

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