TP 2443

Transactions of The Indian Institute of Metals

Vol. 64, Issues 1 & 2, February-April 2011, pp. 67-70

Anisotropy in impact behavior of Zr-2.5Nb pressure tube alloy

Priti Kotak Shah, P.M. Satheesh, R.N. Singh1, J.S. Dubey, R.S. Shriwastaw, K.S. Balakrishnan,
A.P. Kulkarni, Prerna Mishra, V.P. Jathar, S. Majumdar, V.D. Alur, S. Anantharaman and
J.K. Chakravartty1
Post Irradiation Examination Division, 1 MMS, Materials Group, Bhabha Atomic Research Centre, Trombay, Mumbai

E-mail: pritik@barc.gov.in

Received 01 November 2010

Revised 17 February 2011 Keywords:
Accepted 01 March 2011 anisotropy; impact behavior; Zr-2.5Nb; Zr-hydrides; axial and
Online at www.springerlink.com transverse orientation
© 2011 TIIM, India

Abstract
Zr-2.5Nb alloy tubes in cold worked and stress relieved (CWSR) condition serve as pressure boundary for hot coolant in Indian Pressurized
Heavy Water Reactor (IPHWR). Due to both microstructural and crystallographic anisotropy, the mechanical properties in general and fracture
behavior in particular are anisotropic for this material/component. In this work impact behavior of the pressure tube material was characterized
over a range of temperature by impact test using specimens with crack growth direction along axial and transverse directions of the tubes.
It has been found that both temperature and orientation have strong influence on the absorbed impact energy.

1. Introduction by impact test using specimens with crack growth direction

Zr-2.5Nb alloy is being increasingly used in several
nuclear reactor systems such as IPHWR, CANDU and RBMK
reactors [1] because of its low neutron absorption cross
section, adequate mechanical properties and good resistance
to aqueous corrosion at reactor operating temperatures.
These tubes are manufactured following a fabrication route
that involves extrusion, cold working imparted by pilgering,
annealing and stress relieving. These steps of fabrication
result in a microstructure and texture that decide performance
of these tubes in service. The microstructure of the CWSR
Zr-2.5Nb pressure tube material consists of heavily elongated
and textured D-Zr phase with thin grain-boundary network of
E-Zr phase. Due to both microstructural and crystallographic
anisotropy, the mechanical properties in general and fracture
behavior in particular are anisotropic for this material. During
service the pressure tubes are subjected to aqueous
corrosion resulting in release of nascent hydrogen or
deuterium. A part of the hydrogen or its isotope deuterium
thus released is picked up by these components. Once solid
solubility is exceeded, brittle hydride plates form and thereby
making these components susceptible to gross hydride
embrittlement. The hydride formation results in lowering of
fracture toughness. In order to assess structure integrity and
ensure safety, evaluation of fracture toughness under quasi-
static and dynamic loading is necessary. In an earlier work
influence of hydrogen on fracture toughness of Zr-2.5Nb
pressure tube material over a range of temperature was
reported [2].
Directional dependence of the impact energy is required
for safety assessment of the pressure tubes under accidental
condition. Very little information is available in literature on
the impact behavior of Indian Pressure Tube material [3-5].
In this work impact behavior of this material was characterized
along axial and transverse directions of the tubes. Both as-
received and hydrogen charged materials were used for this
investigation. The objective of this investigation is to study
the effect of notch orientation and hydrogen on the impact
property of Zr-2.5Nb pressure tube over a range of
temperature. Impact test data was analysed to delineate the
effect of crack growth direction, test temperature and
hydrogen content. Fracture appearances for specimens with
axial notch and with notch in transverse directions were also
significantly different. An attempt has been made in this
work to rationalize the observation in terms of microstructure,
influence of sample holding device, sample geometry,
hydrogen content and test temperature.
2. Experimental
2.1 Material
Zr-2.5Nb tube piece used in this investigation is from a
pressure tube of 82.5 mm average internal diameter and 3.5 mm
thickness. The fabrication route of the pressure tube, that
imparted about 20% cold work in the finished product,
included vacuum arc melting, extrusion and two stages of
cold pilgering with an intermediate annealing. One Spool of
150 mm length were cut from the tube and the inner and outer
surfaces of the spools were polished using 1200 grit abrasive
paper to obtain a fresh and oxide free surface. The polished
spools were gaseously charged at 363oC to the desired level
with controlled amount of hydrogen in a modified Sievert’s
apparatus [6]. The spools after hydrogen charging were
furnace cooled to room temperature. The actual hydrogen
content in the samples was estimated by inert gas fusion
technique.
68 Priti Kotak Shah et al. : Trans. IIM Vol. 64, Issues 1 & 2, February-April 2011

Fig. 1 : Schematic diagram of (a) Dimension of Charpy sample (b) sample orientation in the tube and (c) fixture for holding the axial
notched sample during test.

2.2 Charpy V-notch specimens and drop tower impact test

The impact tests were carried out on as-received and

hydrided Zr-2.5Nb pressure tube material. Impact samples of
dimension 55x10xt were machined from the pressure tube
spools where t is the thickness of the pressure tube which
is 3.5 in IPHWRs. The orientations of the notch was such
that it facilitated crack growth either along axial or along
circumferential directions of the pressure tube. These samples
will be referred to respectively as axial and transverse samples
throughout this manuscript. Dimensions of the Charpy
specimens used in the present study and their orientations
with respect to the pressure tube are schematically shown in
Fig. 1(a) and (b), respectively.
Drop tower impact testing machine, with an environment
chamber for thermal conditioning of the specimens, was used
for testing. A specially designed anvil was fitted in place of
standard Charpy anvil, located in the environment chamber.
The anvil for holding the specimen and the exploded view of
the specimen are schematically shown in Fig. 1(c). It is
ensured that the specimen sits freely in the slot of the anvil
at all temperatures of testing. Velocity of testing was 3.5 m/
s (corresponding to a drop height of 0.625 m). Impact tests
were carried out from room temperature to up to 300oC. The
basic data generated during the test is the load–displacement
plot. The area under the load–displacement plot provides the
total energy to fracture.

2.3 Metallography and fractography Fig. 2 : Hydride distribution along transverse-radial and axial-
radial plane of the tube
Specimens from the undeformed end of the impact-tested
samples were sectioned along axial–radial (longitudinal
direction of the tube) and radial–circumferential (transverse
direction of the tube) planes of the pressure tube. Standard
metallographic techniques were used to prepare the samples.
Hydrides were revealed after swabbing for few seconds with
an etchant of 10%HF, 45% HNO3 and 45% lactic acid. Fracture
surfaces of broken Charpy specimens were examined under
scanning electron microscope (SEM).

3. Results and discussion

Hydrogen content (by weight) in the as received material
was 10 ppm and in the hydride pressure tube it was 84 ppm.
Hydrogen charging was fairly uniform in the spools. Fig. 2
shows the micrograph of the Zr-2.5Nb pressure tube material
charged with 84 wppm of hydrogen along transverse-radial Fig. 3 : Absorbed energy versus temperature plots for as-received
and axial-radial plane of the tube. Dark lines in these and hydrided samples for axial and transverse notched
micrographs are the traces of hydride platelets. As is evident samples
from this figure hydride plates are uniformly distributed
 Priti Kotak Shah et al. : Trans. IIM Vol. 64, Issues 1 & 2, February-April 2011
across the thickness of the tube. The traces of hydrides
along axial direction are straighter and longer as compared to
that along transverse direction, which has been rationalized
by Singh et al [6] in terms of microstructural features.
Figure 3 shows the variation in impact energy as a
function of temperature for axial and transverse samples for
both the as-received as well as hydrided specimens. In case
of as-received material, impact energy of the axial samples
was observed to increase with increase in temperature linearly
up to about 180°C after which it appeared to have reached
saturation value. Such a behavior has been reported [7] for
Zircaloy-2 pressure tube material and has been attributed to
enhanced ductility of matrix with increase in temperature.
However, the impact energy values for the samples facilitating
crack growth along transverse direction were showing much
Fig. 4 : Room temperature J versus del a plot in axial and
transverse direction of hydrided pressure tube
Fig. 5 : SEM fractography of hydride specimen with axial notch tested at 300 oC
Fig. 6 : SEM fractography of hydride specimen with transverse notch tested at 300oC
69
weaker temperature dependence and its values were much
lower as compared to those for axial notched samples. Such
a drastic reduction in impact energy of the transverse
specimens as compared to the axial specimens could be
revealed due to the combined effect of microstructural and
crystallographic anisotropy, specimen geometry.
The variation in the impact energy value of the hydrided
samples is also shown in fig. 3 and was observed to be lower
than as-received material for both types of sample orientation.
For the samples facilitating crack growth along axial direction
the hydrided samples showed a remarkable change (as
compared to as-received material) in its temperature
dependence by exhibiting distinct lower and upper shelf
regimes. The temperature dependence of impact energy
values for samples facilitating crack growth along transverse
direction showed weak temperature dependence similar to
the as-received material.
It may be noted that in the case of the samples which
have notch in the transverse direction (that facilitate crack
growth circumferentially), the hydride platelets depicted in
the axial- radial plane would become perpendicular to the
notch. These hydride platelets are much longer than those
in the transverse - radial plane. If hydride plates can be
assumed to be akin to cracks, such long hydrides oriented
perpendicular to that of the notch would bring about a
substantial reduction in the ductility/toughness of the
component which might experience crack growth in the
circumferential direction as is shown in the present
experiment. However, it needs more detailed study involving
fractographic analysis, numerical simulation, modification of
the test fixture etc to understand the exact reasons of this
difference between impact behavior of axial and transverse
specimens.
Figure 3 reveals that there is considerable difference in
impact property between axial and transverse notched
specimens. There is marginal effect of hydrogen for
transverse notched specimens. As far as axial notched
specimens are concerned the hydride effect is pronounced at
70 Priti Kotak Shah et al. : Trans. IIM Vol. 64, Issues 1 & 2, February-April 2011
and below 200oC. The hydride specimens with axial notch
showed typical S-curve nature as is obtained in ferritic steels.
For hydride specimens the impact toughness is independent
of notch orientation below about 180oC which is not the case
for as-received specimens.
In order to delineate the role of microstructural and
crystallographic anisotropy and rate of loading J-R curves
were obtained for hydride pressure tube using 17 mm curves
compact tension samples by loading under quasi-static
condition. The J-R curves for both the types of samples are
shown in Fig. 4 which reveals that the J-R curves for both
types of samples are nearly identical.
Figure 5 shows the fractograph of the hydride axial
samples tested at 300oC and were observed to be marked by
axial splits. However hydride transverse specimens did not
show any splits oriented normal to crack plane and the
fracture surface is shown in Fig. 6. Fracture surface of both
axial and transverse specimens tested at 300°C exhibited
fibrous features suggesting ductile failure.
4. Conclusion
The following conclusions could be drawn from this
work:
z Ductile-to-brittle-transition behavior was exhibited by
as-received and hydride Zr-2.5Nb for axial notched
specimens. Hydrided material showed a sharp
transitional behavior.
z There is marginal effect of hydrogen for transverse
notched specimens.
z At all temperatures of testing, transverse notched
samples showed lower toughness than the axial notched
samples.
Acknowledgement
Constant encouragement and invaluable support
provided by Dr. U.K. Viswanathan is acknowledged.
Hydriding and specimen preparation help provided by
Shri K.C. Mazumdar, Shri K. B. Gaonkar, Shri H. N. Tripathy
and Shri S.B. Deherkar is also greatly acknowledged.
References
1. Lemaignan C and Motta A T, Zirconium alloys in nuclear
applications, Materials Science & Techno. A Comprehensive
treatment, eds. Cahn R W, Haasen P and Kramer E J, 10B
chapter 7, (1994) 1.
2. Dubey J S, Chakravartty J K and Banerjee S, Fracture Behaviour
of Dilute Zirconium Alloys: Role of Hydrogen and Trace
Impurities, Paper no. 50483, Proceedings of 13th. International
Conference on Nuclear Engineering (ICONE-13, ASME) Bejing,
China, May 16-20, (2005).
3. Singh R N, Mukherjee S, Anuja Gupta and Banerjee S, Terminal
Solid Solubility of Hydrogen in Zr-alloy Pressure Tube Materials,
Journal of Alloys and Compounds, 389 (2005) 102.
4. Singh R N, Lala Mikin R, Dey G K, Sah D N, Batra I S and
Ståhle P, Influence of temperature on threshold stress for
reorientation of hydrides and residual stress variation across
thickness of Zr-2.5Nb alloy pressure tube, Journal of Nuclear
Materials, 359 (2006) 208.
5. Singh R N, Kishore R, Singh S S, Sinha T K and Kashyap B P,
Stress-reorientation of hydrides and hydride embrittlement of
Zr-2.5 wt. % Nb pressure tube alloy, Journal of Nuclear Materials
325 (2004) 26.
6. Singh R N, PhD Thesis, Indian Institute of Technology, Mumbai,
India, 2002
7. Viswanathan U K, Singh R N, Basak C N, Anantharaman S and
Sahoo K C, Evaluation of effect of hydrogen on toughness of
Zircaloy-2 by instrumented drop weight impact testing, Journal
of Nuclear Materials, 350 (2006) 310.