Received: 31 August 2017 Accepted: 9 September 2017

DOI: 10.1002/er.3905

SPECIAL ISSUE PAPER

Effects of δ‐hydride precipitated at a crack tip on crack

instability in Zircaloy‐4

Siddharth Suman1 | Mohd Kaleem Khan1 | Manabendra Pathak1 | R.N. Singh2

1
Department of Mechanical Engineering,
Summary
Indian Institute of Technology Patna,
Patna 801 103, India A fraction of hydrogen produced due to the waterside corrosion of Zircaloy‐4
2
Mechanical Metallurgy Division, Bhabha nuclear fuel cladding diffuses into it. Diffused hydrogen migrates up a stress
Atomic Research Centre, Mumbai 400 085, gradient in the Zircaloy‐4 and accrues in the regions of higher stress like a crack
India
tip. When the concentration of hydrogen exceeds terminal solid solubility, it
Correspondence precipitates as brittle hydride phases. Hydride precipitated at the tip of a crack
Mohd Kaleem Khan, Department of
may induce crack instability, causing failure of the cladding. To understand the
Mechanical Engineering, Indian Institute
of Technology Patna, Patna 801 103, India. effects of hydride precipitated at the tip of a crack on crack instability in
Email: mkkhan@iitp.ac.in Zircaloy‐4, a numerical investigation is performed on single‐edge notched ten-

Funding information
Board of Research in Nuclear Sciences,
Grant/Award Number: 36(2)/14/30/2014‐
BRNS/1665
sion specimen by using the extended finite element method. The mechanical
properties of the Zircaloy‐4 cladding and hydride precipitated in it—used in this
numerical analysis—are evaluated by using nanoindentation technique. The
crack length is taken between 0.05 and 0.2 mm, while the length of the hydride
is varied in the range of 0.1 to 0.2 mm. The influence of hydride dimensions,
number of hydrides, orientation of hydrides, and distance of hydride from the
crack tip on crack instability is evaluated. The stability of the crack is assessed
in stress intensity factor and J‐integral for each case. Results reveal that stress
distribution around the crack tip is significantly altered by the precipitation of
hydride. The circumferential hydride is less detrimental compared with the
radial hydride. As the distance of hydride from the crack tip increases, there
is a decline in the stress intensity factors and J‐integrals, implicating that there
may exist a critical distance beyond which hydride precipitation has negligible
effect on crack instability.

KEYWORDS
crack, embrittlement, hydride, hydrogen, XFEM, zircaloy

1 | INTRODUCTION undergo waterside corrosion during service and hydrogen

Zircaloy‐4 is widely employed as the fuel cladding in
water cooled nuclear reactors. The fuel cladding encases
radioactive uranium fuel pellets undergoing fission, and
its outside surface is exposed to pressurized coolant water
or heavy water, which takes away the generated heat for
power generation.1,2 Zircaloy‐4 fuel cladding tubes
produced due to the corrosion diffuses into it.3
Zr þ 2H2 O→ ZrO2 þ 4 H
4 H þ 2 Zr→ 2 ZrH2
The hydrogen in solid solution form in the Zircaloy‐4
matrix is highly mobile at nuclear reactor operating

Int J Energy Res. 2017;1–9. wileyonlinelibrary.com/journal/er Copyright © 2017 John Wiley & Sons, Ltd. 1
2 SUMAN
conditions. It migrates down both the concentration and
the temperature gradients while migrates up a stress gra-
dient.4 When the concentration of hydrogen exceeds a
limiting level—maximum concentration of hydrogen,
which can be contained in the zircaloy metal matrix with-
out precipitation of secondary hydride phase—called ter-
minal solid solubility, it precipitates as brittle hydride
phase. Because the hydrogen migrates up the stress gradi-
ent, it will segregate toward a stressed crack tip, and when
the hydrogen concentration exceeds the terminal solid
solubility for the given conditions, it precipitates as brittle
hydride phase. Moreover, the crack tip itself may undergo
the corrosion reaction and the released hydrogen can be
absorbed in its vicinity, subsequently precipitating as
hydride. The brittle hydride phase assists the crack propa-
gation in both the cases; the former is associated with
delayed hydride cracking, and the latter is called corro-
sion hydrogen cracking. However, precipitation of brittle
hydride phases at crack tip or near crack tip is a common
characteristic of both types of cracking; it is the way
hydrogen is reaching near the crack tip distinguishing
these 2 phenomena. It is important to emphasize at this
juncture that hydride‐assisted cracking happens in a
repetitive way locally even when the bulk concentration
of hydrogen is below the terminal solid solubility. The
local hydrogen concentration at crack tip reaches termi-
nal solid solubility, brittle hydride phase is precipitated,
and crack growth occurs through hydride of critical size
and extends the preexisting crack; again, hydrogen starts
migrating toward it, and the phenomenon repeats.5
Given the complexities in experimental investigation
of interaction between crack and hydride in zircaloy,
there are several attempts6-13 made to analytically and
numerically investigate the various phenomena related
to it. Table 1 provides a summary of numerical studies
performed to understand the consequences of interaction
between hydride and preexiting flaws. Ellyin and others6,7
used analytical and finite element methods to analyze the
effect of hydride precipitation on the stress field near a
crack tip. They reported that hydride precipitation causes
removal of the peak stress and a shift of the peak stress to
the front end of the hydride. This may initiate cracking of
the hydride at this region. Varias and Massih8,9 evaluated
the role of hydrogen diffusion in zircaloy cracked plate
under tensile stress and temperature gradient. According
to their numerical results, the contribution of stress gradi-
ent on hydrogen flux becomes dominant near the crack
tip. Chao et al10 studied the failure of Zr‐2.5% Nb due to
delayed hydride cracking with the help of finite element
code of ANSYS used in conjunction with strain energy
density theory. Their work interpreted the effects of differ-
ent hydride orientations, the amount of zirconium
hydride, and various crack configurations on the crack
ET AL.
growth during delayed hydride cracking. They concluded
that crack propagation is more rapid if the orientation of
hydride is shifted from the circumferential to the radial
direction. Kubo and Kobayashi11 also used ANSYS to
investigate the effects of hydride precipitation on the
stress distribution around the crack tip in Zircaloy‐2 clad-
dings. Hydride precipitation is found to significantly alter
the stress distribution around the crack tip. Tseng et al13
employed finite element method to understand the effect
of hydride on crack stability in Zircaloy‐4 fuel cladding.
The analyses were performed to investigate the effects of
hydride dimensions, number of hydrides, the patterns of
split in the hydride, and the presence of a circumferential
hydride among radial hydrides on crack propagation.
Their study found that radial hydrides near the crack tip
had a significant effect on crack propagation and the lon-
ger hydride platelet has more pronounced influence.
All these studies were only limited to 2‐dimensional
model, and the effects of crack tip hydride precipitation
on the crack instability in Zircaloy‐4 have never been
investigated numerically. Two‐dimensional models can-
not provide an exact evaluation of crack instability in
the presence of different phases because the stress state
and hydrogen concentration are expected to be different
for the surface and the bulk of the material. At the sur-
face, plastic field around the crack tip is large under the
plain stress state, which would disperse the hydrogen
and decrease the hydrogen concentration at the crack
tip.14 Moreover, these studies used conventional finite ele-
ment method, which has high computational cost and
time. It is also observed during the literature survey that
a number of studies have assumed elastic properties of
hydride same as the zircaloy metal matrix given the non-
availability of experimental data, which is not the case.
This assumption may have significant influences on the
final outcome of the numerical studies. The determina-
tion of the mechanical properties of hydride precipitated
in the Zircaloy‐4 matrix and the numerical investigation
of 3‐dimensional model using advanced and crack specific
computational approach may lead to overcome these
issues. In the present investigation, mechanical properties
are evaluated for the both phases, namely, Zircaloy‐4
metal matrix and δ‐hydride using nanoindentation tech-
nique.15,16 The properties are then taken as input in the
numerical investigation to assess the influence of hydride
precipitation at a crack tip on the crack instability. Three‐
dimensional numerical investigation is performed on sin-
gle edge notched tension specimen by using extended
finite element method (XFEM) in Abaqus 6.12. The
effects of crack and hydride dimensions on crack stability
are presented in fracture parameters like stress intensity
factor and J‐integral. The difference between the effect
of radial and circumferential hydrides is also presented.
 SUMAN
ET AL.

TABLE 1 Numerical studies focused on interaction of hydride and crack in zircaloys

Range of Parameters
Hydride
Crack
Length Length Thickness Loading
Material mm μm μm Methodology Remarks
6
Zr‐2.5%Nb – 100 2.5 – Analytical ▪ Effect of a hydride precipitate forming in the plastic zone of the
crack is modeled.
▪ Occurrence of a compressive zone at the crack tip due to hydride
causing suppression of fracture
Zr‐2.5%Nb7 8.0 5‐20 0.1‐0.25 Tensile stress Finite element method ▪ Effect of a hydride precipitation on the stress, strain, and displacement
0‐80 MPa fields near crack tip was investigated.
Zr‐2 plate8 0.08 – – Tensile stress Finite element method ▪ Strong effect of crack tip stress intensification on hydrogen diffusion
0‐300 MPa and initial hydride precipitation
Zircaloy9 – 12 2.0 – Finite element method ▪ Stress intensity factor is estimated at various temperatures and under
various constraint conditions.
Zircaloy cladding10 0.11‐0.15 – – Internal pressure Finite element method [ANSYS] ▪ Strain energy density factor is maximum when hydride is oriented
68 MPa between 30° and 60° from crack face.
Zircaloy‐211 0.1 0‐10 1 Finite element method [ANSYS] ▪ Stress distribution around the crack tip is significantly altered by
precipitation of hydride.
Zr‐HCP unit cell12 – – – – Embedded atom method ▪ Crack propagation was found to depend on the specific position
of the H interstitials.
Zircaloy cladding13 0.1 100‐300 25.0 – Finite element method ▪ Longer hydride platelet resulted in a remarkable effect on crack propagation.
3
4 SUMAN
Moreover, the role of distance between the crack tip and
precipitated hydride is evaluated.
2 | FORMATION O F FOUNDATION
FOR NUMERICAL INVESTIGATION
This section describes the methodology in brief and high-
lights the necessary steps taken in background to execute
the present numerical investigation.
2.1 | Extended finite element method
The XFEM is a numerical technique that extends the clas-
sical finite element approach based on the concept of par-
tition of unity; that is, the sum of shape functions is equal
to 1. While other techniques require a mesh created in
close accordance with the crack geometry, XFEM does
not need to consider crack geometry when the mesh is
created. A priori known information about the solution
of a given problem is added to the finite element formula-
tion, which makes possible to represent discontinuities
and singularities independently of the mesh. Main con-
cepts of this approach are enriching technique by using
special function and adding extra degree of freedom.
These can be done by adding singular expressions and
adding discontinuous expressions that allow an element
to have 2 strain and stress fields. Let all nodes in the solu-
tion space be represented by the set S, the nodes that com-
prise the crack tips are the set Sc, and the other
comprising the physical discontinuity are the set Sh. Then,
the approximation is given as
2 3
N
6 4
7
u ðx; yÞ ¼ ∑ N i ðx; yÞ 4ui þ H ðx; yÞ ai þ ∑ ψi ðx; yÞ bi 5
i∈S i∈Sh i¼1
i∈Sc
where ui is the nodal displacement, ai represents the vec-
tor of enriched nodes with the discontinuity function, and
bi are the nodes enriched with the crack tip asymptotic
solutions. In other words, the first term is similar to finite
element method and applied to all the nodes of the model,
the second term is applied to the nodes whose shape func-
tion is cut by the crack interior, and the last or third term
is applied to the nodes whose shape function is cut by the
crack tip; for more details, refer to Mohammadi.17
2.2 | Numerical computation model
Single‐edge notched tension specimen is taken as the
computational model in the present study. It is a cuboidal
shape specimen with an edge crack in its longitudinal
symmetry axis (see Figure 1A). The choice of this
ET AL.
specimen for the numerical simulation is due to its popu-
larity in experimental studies of fracture mechanics. Due
to this fact, this specimen is likely to have an accurate
empirical solution for the stress intensity factor, and this
is very important for comparing the numerical results
with it before assessing the crack instability for unknown
cases like in the presence of hydride. The crack length is
varied in the range of 0.05 to 0.2 mm, while hydride
length is taken as 0.1 to 0.2 mm. The hydride width is
fixed as 0.030 mm. A tensile pressure of 25 MPa, typical
of stress developed in fuel cladding during service, is
applied at the top and the bottom faces as the boundary
conditions. The stress intensity factor for this specimen
for mentioned loading is given as17
 a  a 2  a 3  a 4  pffiffiffiffiffiffiffi
K I ¼ 1:12−0:23 þ 10:56 −21:74 þ 30:42 σ πa
W W W W
(1)
where W is the width of the specimen, a is the size of the
edge crack, and σ is the applied uniaxial tensile stress.
Hexahedron‐structured medial meshing option is used
to mesh the computational model. The element size
around the crack tip is kept small to achieve higher degree
of accuracy. It is achieved by partitioning the region hav-
ing the precrack and seeding with very small element size.
After consulting the literature and conducting an optimi-
zation for different ways of partitioning the single‐edge
notched tension specimen, finally, the most suitable
partitioning scheme that gives the best quality of mesh
near the crack is selected as shown in Figure 1B. Three‐
dimensional stress element—an 8‐node linear brick
C3D8R element—is selected with full integration.
Hydride is embedded in the model as inclusion, and its
mechanical properties are assigned separately. The time
step is taken as 1 with maximum increment of 0.01. Max-
imum principal stress criterion is used for damage
evolution.
2.3 | Determination of mechanical
properties
During the literature survey, it is realized that a number
of studies have either assumed mechanical properties of
hydride same as zircaloy or extrapolated in accordance
with bulk behavior of hydrided zircaloy, given the lack
of experimental data availability.18 These assumptions
may have substantial impact on the final outcome of
numerical studies. Even though recently, Weck et al19
has predicted the properties of δ‐hydride embedded in
Zircaloy‐4 matrix by using density functional perturbation
theory, experimental determination of the Young's modu-
lus, yield stress, and the hardness of the δ‐hydride
SUMAN ET AL.
FIGURE 1 (A) Schematic of single‐edge notched tension specimen used for numerical investigation. (B) Meshed single‐edge notched
tension specimen [Colour figure can be viewed at wileyonlinelibrary.com]
precipitated in Zircaloy‐4 metal matrix is not available in
the open literature. Thus, it is decided to evaluate the
mechanical properties of both the phases, namely,
Zircaloy‐4 metal matrix and hydride precipitated in it,
using nanoindentation technique. Nanoindentation
enables to apply indenting load on individual phases pres-
ent in any material and to evaluate their mechanical
responses. The cold‐worked stress‐relieved unirradiated
Zircaloy‐4 cladding tube (outer diameter of 13.08 mm
and thickness of 0.41 mm) is hydrided with concentra-
tions of 600 and 900 ppm by using gaseous hydrogen
charging method. Gaseous charging facility consists of a
cylindrical glass chamber placed inside the furnace. The
clad specimen is weighed and then placed inside the
chamber. The glass chamber is evacuated to create a vac-
uum of the order of 10−5 torr. Subsequently, the specimen
chamber is heated to the temperature of 363°C. Depend-
ing upon the weight of the sample, hydrogen is released
into the specimen chamber up to a precomputed pressure.
5
The amount of hydrogen picked up the sample is calcu-
lated from the difference between the initial and the final
pressure readings recorded at ambient temperature.
Hydrogen concentration in the cladding specimens is
determined by an inert gas fusion technique by using a
LECO RH IE hydrogen determinator. Mechanical proper-
ties of both δ‐hydride and Zircaloy‐4 metal matrix are
evaluated by using Hysitron TI 950 Triboindenter
equipped with in situ scanning probe microscopy. The
material properties evaluated in the present work as well
as used in the analyses are provided in Table 2.15,20-22
2.4 | Mesh sensitivity analysis
It is critical to make sure in any mesh‐based computation
like the present one that the mesh correctly resolves the
physics of the problem. There is a certain maximum size
an element can have to evaluate the local field value
within the permissible range. Taking smaller element size
6 SUMAN ET AL.

TABLE 2 Material properties of Zircaloy‐4 and hydride used in the simulation

Phase of the Material

Properties Zircaloy‐4 δ‐hydride Unit Source
Young's modulus 99.24 133.18 GPa
Yield stress 310 709 MPa Present work
Ultimate tensile stress 436 998 MPa
Poisson's ratio 0.296 0.320 – 20,21

15,22
Fracture toughness 40 3.3 MPa√m

arbitrarily is computationally expensive. Thus, a mesh
sensitivity analysis is performed to get optimized element
size and accurate result. Element size in the crack block
region is varied from 0.006 to 0.001, and the obtained
stress intensity factor is compared with analytical solution
given by Equation 1. It is observed, as shown in Figure 2
A, that solution is most accurate for the element size of
0.0015, and thus, this element size is fixed for all the sub-
sequent numerical simulation. A comparison between the
analytical stress intensity factor and those obtained from
XFEM for different crack lengths is plotted in Figure 2B.
The results match well, and the maximum error of
1.12% is observed for the crack length of 0.1 mm. This
comparison is crucial to establish the use of extended
finite element before investigating the cases of hydride
precipitation at the crack tip for which there is no stan-
dard analytical solution available.

3 | R ESULTS A ND DISCUSSION

The stress intensity factor quantifies the stress state or

FIGURE 2 (A) Mesh sensitivity analysis. (B) Comparison of
analytical stress intensity factor with extended finite element
solution [Colour figure can be viewed at wileyonlinelibrary.com]
intensity at a crack tip caused by a far‐field applied stress
and is used to establish failure criterion due to fracture. Its
magnitude is dependent on the specimen geometry, the
dimension and orientation of the crack, and the magni-
tude and the modal distribution of applied loads on the
material. J‐integral represents the rate of change of net
potential energy with respect to crack advance (per unit
thickness of crack front) for a nonlinear elastic solid. It
also can be thought of as the energy flow into the crack
tip. Thus, J‐integral is a measure of the singularity
strength at the crack tip for the case of elastic‐plastic
material response. Both stress intensity factor and J‐inte-
gral are determined to evaluate the crack stability in the
present work.
The precipitation of hydride at the tip of a crack signif-
icantly alters the von Mises stress distributions. The stress
distribution for different cases is presented in the Figure 3.
The stress singularity at the crack tip could be identified
from the stress contour; the highest stress is seen in the
case of 2 parallel radial hydrides near the crack tip. The
circumferential hydride is less detrimental in comparison
with the radial hydride; it is in accordance with many
other experimental observations.23,24 In case of the cir-
cumferential hydride, the higher stress region extended
from the crack tip toward the hydride, which implicates
the distribution of the load bearing capacity.
The stress intensity factor and the J‐integral are higher
for the crack with hydride presence at its tip or in vicinity.
Figure 4 shows the increase in stress intensity factors and
SUMAN ET AL. 7

FIGURE 3 von Mises stress distributions (A) 0.2 mm crack, (B) 0.2 mm crack with 0.1 mm radial hydride, (C) 0.2 mm crack with 0.1 mm
circumferential hydride, and (D) 0.2 mm crack with two 0.1 mm parallel radial hydrides [Colour figure can be viewed at wileyonlinelibrary.
com]

J‐integrals for different crack lengths due to precipitation
of hydride. Evidently, it would enhance the propagation
of crack in Zircaloy‐4.13,25-27 Another interesting observa-
tion is that severity induced due to the presence of a
hydride increases with increase in the crack length. The
change in stress intensity factor due to precipitation of
hydride is 39.27% for 0.05 mm crack, while it is 55.59%
for the crack length of 0.1 mm. The larger crack length
is more unstable after the hydride precipitation.
The distance between the crack tip and the hydride
also influences the crack stability. As the distance of the
hydride increases from the tip, there is a decline in the
stress intensity factor and J‐integral. However, after a cer-
tain distance, the stress intensity factor seems to stabilize,

FIGURE 4 Variation in stress intensity factors and J‐integrals FIGURE 5 Variation in stress intensity factors and J‐integrals
after the precipitation of hydride for different crack lengths with increase in the distance between hydride and crack tip
[Colour figure can be viewed at wileyonlinelibrary.com] [Colour figure can be viewed at wileyonlinelibrary.com]
8 SUMAN
TABLE 3 Comparison of stress intensity factor for different cases
Case
0.2 mm crack with no hydride
0.2 mm crack with 0.1 mm radial hydride at tip
0.2 mm crack with 0.2 mm circumferential hydride at tip
0.2 mm crack with two 0.1 mm parallel radial hydride near tip
thus indicating that there must exist a limiting or critical
distance between the crack tip and the hydride within
which hydride may make the crack unstable. Beyond that
critical distance, the precipitation of the hydride has little
role in the crack propagation. Figure 5 is plotted to under-
stand the role of distance between the crack tip and the
precipitated hydride.
With increase in the number of radial hydrides, the
stress intensity factor and J‐integral increase significantly.
The precipitation of circumferential hydride too has
degrading effect and enhances the stress intensity factor
drastically. Nevertheless, the increase in stress intensity
factor is less compared with radial hydride. Table 3 pro-
vides a comparison of stress intensity factor for these dif-
ferent cases of hydride precipitation. Two parallel radial
hydrides in the vicinity of crack tip are the most detrimen-
tal and may be observed from the Figure 3 too. It is worth
mentioning here that the hydride orientation near the
crack tip is governed by the stress field direction to which
the specimen is subjected, and it is not possible to have 2
different configurations of hydride near the same crack tip
for the same tensile loading direction as considered in the
present study. However, such computational model is
considered to have a comparison between the detrimental
effects of the 2 different orientations under identical
conditions.10,11,13
4 | CONCLUSIONS
The mechanical properties of the δ‐hydride precipitated in
the Zircaloy‐4 fuel cladding are determined by using
nanoindentation technique. The effects of hydride precip-
itation at the tip or in vicinity of a preexisting crack in
Zircaloy‐4 are numerically investigated by using XFEM.
Numerical investigation is performed on single‐edge
notched tension specimen, and crack length is varied
from 0.05 to 0.2 mm. The influence of hydride dimen-
sions, number of hydrides, orientation of hydrides, and
distance of hydride from the crack tip on crack instability
is evaluated in stress intensity factor and J‐integral. It is
seen that stress distribution around the crack tip is signif-
icantly altered by precipitation of hydride. The 2‐parallel
hydride configuration is the most detrimental. The cir-
cumferential hydride is less detrimental compared with
ET AL.
Stress Intensity Factor (MPa√mm)
41.73
60.32
54.96
69.38
the radial hydride, which is in accordance with the
established experimental findings. As the distance of
hydride from the crack tip increases, there is a decline
in the stress intensity factors and J‐integrals.
ACKNOWLEDGEMENT
We sincerely acknowledge the Board of Research in
Nuclear Sciences (BRNS), Government of India, grant
number 36(2)/14/30/2014‐BRNS/1665 for providing the
financial support needed to carry out the present work.
ORCID
Mohd Kaleem Khan http://orcid.org/0000-0003-3557-957X
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How to cite this article: Suman S, Khan MK,
Pathak M, Singh RN. Effects of δ‐hydride
precipitated at a crack tip on crack instability in
Zircaloy‐4. Int J Energy Res. 2017. https://doi.org/
10.1002/er.3905