J Fail. Anal. and Preven.
(2009) 9:420–428
DOI 10.1007/s11668-009-9277-3
CASE HISTORY—PEER-REVIEWED
Hydrogen-Induced Cracking (HIC) of Hardened and Tempered
Steel Fastener Used in Space Application
Abhay K. Jha Æ K. Sreekumar
Submitted: 21 June 2009 / in revised form: 14 July 2009 / Published online: 29 July 2009
Ó ASM International 2009
Abstract Cadmium-plated 0.35C–3.5Ni–1.5Cr–0.5Mo
steel threaded fasteners of 1230 MPa properties class are
used for aerospace applications. These fasteners were tor-
qued to 13 N
m. Few fasteners parted into two pieces while
in use under sustained assembly load for a period of
50 days. The fracture surface of the failed fasteners had
two distinct regions when viewed under microscope at
higher magnification. Fractography revealed that the larger
region consisted of predominantly intergranular features,
whereas the smaller region had features of microvoid
coalescence. From the metallography evidences it was
concluded that the fastener failure was due to hydrogen
embrittlement. Electro-deposit of cadmium was identified
to be the main source for hydrogen entrapment, which
could not be compelled completely by post-plating baking
treatment.
Keywords 0.35C–3.5Ni-1.5Cr–0.5Mo steel

Hydrogen embrittlement
Introduction
The steel, 0.35C–3.5Ni–1.5Cr–0.5Mo, in the hardened and
tempered condition, meeting the specified axial tensile
stress rating of 1230 MPa, is widely used as fasteners in
space programs. These fasteners were applied a torque of
13 N
m in a launch vehicle assembly and three fasteners
were parted in two pieces after experiencing sustained
A. K. Jha (&)
K. Sreekumar
Materials Characterization Division, Materials and Metallurgy
Group, Vikram Sarabhai Space Centre, Indian Space Research
Organisation, Trivandrum 695 022, India
e-mail: ak_jha@vssc.gov.in
123
assembly load for a period of 50 days. Out of three fas-
teners failed, two had failure at thread region, while the
third one failed at the smooth surface of shank portion.
The failed fasteners were removed from the assembly
and subjected to detailed metallurgical investigation to
determine the cause of the failure. An attempt is made here
to correlate the metallurgical features seen in the failed
fasteners with their failure mode.
Material
The steel used for making the fasteners was melted in
primary electric arc furnace and further refined under
vacuum prior to casting into ingot. The chemical compo-
sition of the failed fastener is given in Table 1. The cast
ingot was forged to breakdown the cast structure and rolled
to 10-mm-diameter rods. The threads were made by thread
rolling. The thread-rolled fasteners were hardened and
tempered to achieve the specified mechanical property.
Cadmium plating was provided to the fasteners not only for
corrosion protection during storage or in service, but also to
serve as a lubricant.
Observations
The failure occurred at the thread portion of the two fas-
teners, hereafter will be referred as ‘1’ and ‘2’, while it was
at smooth region of shank portion of third failed fastener,
hereafter referred as ‘3’. There were cracks due to damaged
cadmium layer and subsequent corrosion was noticed on
almost all the thread roots (Fig. 1). The fracture initiated
from such damage at the thread root (Fig. 2). The third
fastener failure occurred at the unthreaded region of shank
J Fail. Anal. and Preven. (2009) 9:420–428 421

Table 1 Chemical composition of the material

C Mn P S Si Ni Cr Mo Fe

Spec 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 0.38 0.52 0.017 0.012 0.27 3.83 1.87 0.47 Balance

Fig. 1 Corrosive attack at thread roots of failed fasteners ‘1’ and ‘2’

The bolt was cut along its axis and prepared by

Fig. 2 Fracture initiated at thread root of failed fasteners ‘1’ and ‘2’
portion of the bolt. Surface was corroded and a crack of
approximately 1.2 mm length was seen at the region,
adjacent to the fracture edge of failed fasteners (Fig. 3).
conventional metallographic technique to study the met-
allurgical features. The slices were taken in such a way that
the plane parallel to the bolt axis could be viewed for
metallographic features. The polished specimens were
evaluated for inclusion content by comparison method
using JK chart as per ASTM E45. The globular oxide
inclusions were rated as high as ‘‘2 thin’’. All other
inclusions were less than ‘‘1 heavy’’ as per the chart. The
thread roots of the failed bolt when examined under optical
microscope confirmed the depth of corroded region was up
to 100 lm. These defect regions at the thread root had
blunt tips. The absence of branching of a crack at its tip
indicated that the corrosion was general in nature.
The specimens etched with 5% Nital solution revealed a
microstructure consisting of tempered martensite, typical
of hardened and tempered steel (Fig. 4). No predominant
secondary cracks at the subsurface of the material could be
observed.
Observations of fracture surface under optical micro-
scope with stereographic facility revealed the presence of

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Fig. 3 (a) Failed fastener ‘3’, (b) surface corrosion and (c) crack
adjacent to the fracture edge
two distinct regions in all the three failed fasteners. The
first and larger region, hereafter will be referred as ‘LR,’
had grainy features while the smaller region, hereafter
referred as ‘SR,’ had fibrous features (Fig. 5). The two
distinct regions when viewed under scanning electron
microscope (SEM) revealed different morphology of crack
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J Fail. Anal. and Preven. (2009) 9:420–428
Fig. 4 Optical photomicrograph showing fracture edge of failed
fastener. Microstructure consisted of tempered martensite
propagation. The region ‘LR’ had intergranular mode of
fracture (Fig. 6b–d, 7b–d and 8b–d). Separation of polyg-
onal faces of grain was clearly seen (Fig. 6d, 7d and 8d).
Secondary cracks were also present on the fracture surface,
as shown in Fig. 6(c) and 7(d). Evidence of ductile tearing
in the form of fine dimples was seen at many locations on
intergranular facets (Fig. 6c, d and 9).
The smaller region referred as ‘SR’ had fibrous features
(Fig. 6f, 7g and 8g). These fibrous regions consisted of fine
dimples (Fig. 6h, 7f and 8h) were typical of tensile over-
load failure of steel. Transition of fracture mode from
intergranular mode to dimple mode was clearly seen at the
interface between the two regions namely ‘LR’ and ‘SR’
(Fig. 7g and 8g). Figure 9 shows the fractographs con-
sisting of features belonging to the regions ‘LR’ and ‘SR’,
i.e. intergranular at ‘LR’ and dimple mode at ‘SR’. Fea-
tures of ductile tearing as an indication of plasticity ahead
of crack tip were seen at intergranular facets at many
locations (shown by arrows in Fig. 9). The fracture surface
was free from any corrosion products.
Discussion
The fasteners failed under sustained assembly load for a
cumulative period of 50 days. Totally three fasteners were
found to be broken. Cracks were found to initiate at the
thread region of two failed fasteners, while it was at the
unthreaded region of shank for third failed fastener.
There was corrosion attack caused by local damage of
protective cadmium layer to almost all the thread roots,
which were fracture initiation sites. Fracture surface of
failed fasteners, when viewed under optical microscope
with stereographic facility, revealed the presence of two
distinct regions. Observations of fracture surface of all the
three failed fasteners under SEM revealed intergranular
mode of failure within the ‘LR’ region while the region
‘SR’ had dimple mode of failure.
The difference in morphology of the fracture features
between the two distinct regions was conclusive evidence
for the two different mechanisms that operated during
fracture.
J Fail. Anal. and Preven. (2009) 9:420–428
Fig. 5 Fracture surface (a, b)
fastener ‘1’, (c, d) fastener ‘2’
and (e, f) fastener ‘3’ showing
two distinct regions ‘LR’ and
‘SR’ of fracture surface
The presence of the two distinct regions, LR with
intergranular features and SR with dimple mode of failure,
indicated that cracks propagated inward to certain distance
under some embrittling mechanism, while the remaining
material at that time experienced overload under sustained
assembly load and thus had dimple features.
Transition of fracture mode from the intergranular to the
dimple type was clearly seen at the interface between the
two regions.
The fasteners were made from low alloy tempered
martensitic steel and were provided with protective cad-
mium plating. Furthermore, though the steels of this class
are amenable to hardening on transforming the austenite to
martensite by simple air cooling, drastic cooling rates were
used in the present case by oil quenching, thus inducing
stresses within the material.
The fasteners were electrodeposited with cadmium, and
hence hydrogen entry and entrapment also could not be
ruled out. In such cases, hydrogen entry into alloy system
are (a) electrochemical steps, where hydrogen is produced
423
due to hydrogen partial cathodic reaction, and (b) chemi-
sorption step, where chemisorptive forces cause atomic
hydrogen to get attracted to the metal surface and finally
allow it to migrate into metals [1]. The fasteners were
electrodeposited with cadmium, which was followed by
hydrogen de-embrittlement (through baking) process.
However, the time gap between the two processes was not
logged in. ASTM [2] 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 discontinu-
ities of material causing, its embrittlement could not be
ruled out.
There are various mechanisms that lead to intergranular
mode of failure, such as stress corrosion cracking, hydrogen
embrittlement, temper embrittlement, high-temperature
embrittlement, etc. Except for the first two, all remaining
mechanisms affect the bulk of the material. In the present
case, the intergranular feature was found in the larger region
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Fig. 6 Fractographs of fastener

‘1’ showing (a) larger region
‘LR’, (b, c) intergranular (IG)
mode, (d) ductile tearing at IG
facets, (e) smaller region ‘SR’,
(f) fibrous feature, (g, h) dimple
mode

of the fracture surface only. Overload fracture of remaining
ligaments of smaller portion of the failed bolt were dimpled
and hence any mechanism affecting the bulk of the material
was ruled out conclusively. Furthermore, the possibility that
SCC occurred was discounted because corrosion product
was not seen on the fracture surface near the origin or even
away from the origin. Failure in intergranular mode with
features of plasticity ahead of the crack tip was typical of
hydrogen embrittlement. The failure was concluded to be
due to hydrogen embrittlement.
Evidences observed in the present case study can be
explained in a supportive manner through various mecha-
nisms as mentioned next.
The hydrogen embrittlement (HE) process mainly
depends on three factors: (a) origin of the hydrogen, (b)
transport process to carry hydrogen from its source to the

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J Fail. Anal. and Preven. (2009) 9:420–428 425

Fig. 7 Fractographs of fastener

‘2’ showing (a) larger region
‘LR’, (b, c, d) intergranular
mode, (e) smaller region ‘SR’,
(f) dimple mode, (g, h)
transition of IG mode to dimple
mode

locations where it causes embrittlement and (c) the
embrittling mechanism itself. Out of the various embrit-
tling mechanisms discussed, the most convincing are the
adsorption mechanism (where hydrogen lowers the surface
energy), decohesion mechanism (where hydrogen reduces
the lattice cohesive force) and the hydrogen-induced local
plasticity (where hydrogen–dislocation interaction provides
softening of material at the crack tip) [3].
Monoatomic hydrogen is a small interstitial atom that
diffuses very rapidly even at room temperature and even-
tually accumulates at voids/defects and other metallurgical
discontinuities. The accumulation of hydrogen also occurs

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426 J Fail. Anal. and Preven. (2009) 9:420–428

Fig. 8 Fractographs of fastener

‘3’ showing (a) larger region
‘LR’, (b, c, d) intergranular
mode, (e) smaller region ‘SR’,
(f, g) transition from IG mode to
dimple mode, (h) dimple mode

at lattice dilations in high-stressed regions and hydrogen
embrittlement takes place when the accumulations reach a
certain level.
The intergranular features as noticed in the larger region
of the failed bolt can be explained by the decohesion theory
of hydrogen damage. The hydrogen-enhanced decohesion
(HEDE) mechanism was first proposed by Troiano in 1960
[4], further reinforced by Oriani [5] and Gerberich et al.
[6]. HEDE provides the hypothesis that interstitial hydro-
gen lowers the cohesive strength by dilation of the atomic
lattice and hence lowers the fracture energy [7]. This
results in crack advancement along the metallurgical dis-
continuities, preferable along grain boundaries and hence
intergranular facets [8–11].

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J Fail. Anal. and Preven. (2009) 9:420–428
Fig. 9 Fractograph showing transition of intergranular mode to
dimple mode of failure. Features of ductile tearing on intergranular
facets are shown by arrow
The hydrogen-enhanced localized plasticity (HELP)
mechanism of hydrogen embrittlement was first proposed
by Beachem [12] in 1972. This was further reinforced by
Birnbaun and Sofronis [13] in 1980. According to the
HELP mechanism, adsorption-induced dislocation emis-
sion (AIDE) model supports the evidence of localized
plasticity ahead of crack tip due to hydrogen–dislocation
interaction [14].
At certain locations, the presence of ductile tearing at
intergranular facets is explained due to enhance plastic
flow caused by hydrogen dislocation interaction at crack
tip, which resulted in local softening of material on a
localized scale. This resulted in ductile tearing on a
localized scale. Birnbaun and Sofronis [13] found that in
non-hydride forming system, the evidence for failure by
HELP is strong. Woodtli and Kieselbach [15] and Jha et al.
[16] found similar characteristics of hydrogen embrittle-
ment in the form of a partially intergranular fracture with
ductile marking on the grain boundaries.
The hydrogen diffusion took place under the influence
of stress (residual stress introduced in the material during
thermal quenching treatment and/or assembly stress)
reached to certain distance inward, tailing behind features
of HEDE and HELP, leaving remaining material within
smaller region ‘SR’ to bear the assembly load. Under these
circumstances, the assembly load exceeded the yield
strength of material leading to ductile mode of failure for
the remaining material.
The mechanism of failure was hydrogen embrittlement,
which occurred as
1. hydrogen pickup during electro-deposition of cadmium,
2. residual stresses due to oil quenching and/or assembly
stresses, and
427
3. hydrogen pickup in the fastener having internal
residual stresses during cadmium plating and its partial
retention in the component due to insufficient baking
operation.
Conclusion
Based on the facts and findings it can be concluded that the
fasteners failed due to hydrogen embrittlement.
Recommendations
1. High-strength fasteners should be given preferably
vacuum deposition of cadmium rather than electro-
deposition.
2. Proper baking after electro-deposition and within
stipulated time is recommended.
3. Locked-in stresses within the material should be kept
as low as possible.
Acknowledgments The authors thank Dr. P.P. Sinha, Deputy
Director, VSSC (MME), for his technical support during the inves-
tigation. They are indebted to Dr. K. Radakrishnanan, Director,
VSSC, for permission to publish this work.
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