BARC Newsletter Issue No.

249

CHARACTERIZATION OF MATERIAL
PROPERTIES BY ULTRASONICS
P.P. Nanekar and B. K. Shah
Atomic Fuels Division
Bhabha Atomic Research Centre

Abstract

Non-destructive testing techniques are most commonly employed for detection and characterization
of flaws in the component. Apart from flaw characteristics, another parameter which is equally
important to assess the structural integrity of engineering components is the material property. Non-
destructive testing techniques offer several advantages over the conventional coupon-based
techniques. Ultrasonic Testing is one of the widely used NDT techniques for material
characterization. In the past few decades, researchers all over the world have carried out extensive
study to characterize, both microstructural and mechanical properties of materials by ultrasonic
testing. This paper highlights the ultrasonic testing parameters useful for material characterization
studies and also investigations carried out in various laboratories including authors laboratory on
characterization of microstructural and mechanical properties of materials, qualification of
processing treatments during fabrication and assessment of damage during service due to various
degradation mechanisms.

Introduction these parameters can be measured very

accurately to correlate them with various

O
ne of the prime objectives of Non- material properties with a reasonable confidence
Destructive Testing (NDT) is to certify level. Some of the important metallurgical
that the component being examined is properties that have been correlated with
fit for the intended service. The most common ultrasonic testing parameters are grain size,
way of doing it is by examination of the inclusion content, elastic modulus, hardness,
component with one or combination of various fracture toughness, yield strength, tensile
Non-Destructive Testing Techniques to strength, etc. Ultrasonic material
determine the presence or absence of flaws in characterization has also been used to qualify
the component. If the flaw exists, then it is various processing treatments during fabrication
characterized with respect to location, size, and to assess the damage due to various
orientation, shape, nature, etc. to determine its degradation mechanisms like fatigue, creep,
acceptability under the operating conditions. corrosion, hydrogen damage, etc. The scope of
Apart from flaw characteristics, another material characterization by Ultrasonics is
parameter which is equally important to assess widened by development of Acoustic
the structural integrity of a component is the Microscopes, which produces images similar to
material property. Ultrasonic Testing is the most the one obtained by optical microscopes. This
preferred NDT technique for characterization of paper briefly describes the importance of
material properties. Ultrasonic testing material characterization by non-destructive
parameters are significantly affected by changes testing and the affect of material properties on
in microstructural or mechanical properties of various ultrasonic testing parameters. Ultrasonic
materials. With the advancement in electronics, characterization studies carried out in various

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laboratories including authors laboratory on the component during the design stage itself.
determination of microstructural and mechanical Moreover, it may not be possible to draw a
properties of materials, qualification of various coupon from a component to determine its health
processing treatments and assessment of damage for continued service. Non-destructive
during service due to various degradation characterization of material properties therefore
mechanisms are also discussed. assumes a great significance during fabrication
as well as service life of the component. Some of
Importance of Non-destructive
the non-destructive testing techniques that have
Characterization of Material been used to characterize material properties are
Properties ultrasonic testing, eddy current testing, magnetic
There are four metallurgical characteristics, methods, Barkhaussen noise, radiometry,
which controls all the material properties. These Mossabuer spectroscopy, positron annihilation,
are chemical composition, microstructure, etc. [1 11, 40]
crystal structure and dislocation density.
Material Characterization by
Material properties can broadly be classified as
microstructural properties and mechanical Ultrasonic Testing
properties. Conventionally, determination of Ultrasonic Testing is the most preferred NDT
microstructural properties is done by technique for characterization of material
metallography which involves cutting, polishing, properties. Being volumetric in nature,
grinding and etching, while mechanical ultrasonic examination can give an idea about
properties are determined by mechanical tests the bulk material properties. Moreover,
like tension tests, Charpy test, Drop weight test, ultrasonic testing parameters are significantly
etc. These tests being destructive in nature are affected by changes in microstructural or
done on coupons with an assumption that the mechanical properties of materials. With the
coupon is the true representative of the advancement in electronics, these parameters
component that will go into service. During can be measured very accurately to correlate
fabrication of any component, processes like them with various material properties with a
solidification, mechanical working and heat reasonable confidence level. Some of the
treatment governs the above four characteristics important metallurgical properties that have been
and thereby material properties. The correlated with ultrasonic testing parameters are
conventional coupon based approach of grain size, inclusion content, elastic modulus,
determining material properties may not be good hardness, fracture toughness, yield strength,
enough as there may be variation in the thermo- tensile strength, etc. Ultrasonic material
mechanical treatment seen by the coupon and the characterization has also been used to qualify
component itself. Hence the results of various processing treatments like precipitation
destructive tests on coupons may not truly apply hardening, case hardening, etc. and to assess the
to the component to be used in service. During damage due to various degradation mechanisms
service, there are many factors, which adversely like fatigue, creep, corrosion, hydrogen damage,
affect the designed life of a component leading etc. Following are some of the commonly
to its premature retirement. Such factors include measured ultrasonic testing parameters for
unanticipated stresses (residual and system), material characterization studies:
operation outside designed limits (excessive
temperature and load cycling), operation and Velocity
environmental effects, degradation of material
properties in service, etc. It is difficult to predict Ultrasonic velocity in longitudinal and shear
the affect of these factors on the service life of modes can be correlated to various material

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properties. The measurement involves [12]. Attenuation measurement technique is

determination of time of travel between the first widely used in material property characterization
and the second backsurface reflection and for determination of grain size, distribution of
dividing it by the distance traveled by second phase participles like inclusions and
ultrasound. The accuracy of these measurements porosity, distribution of diffuse discontinuities
depends on the accuracy with which time of like micro-cracks, etc.
travel and the thickness of the component are
Backscatter amplitude
measured. In cases, where there is access to only
surface of the component (in-situ applications), Backscattering signals (often referred to as
velocity ratio (longitudinal to shear) serves as a noise) from grain boundaries or second phase
useful parameter. Unlike velocity determination, particles create lots of problems during
which needs thickness of the component as ultrasonic examination for flaw detection.
input, velocity ratio can be found out from time However, the scatter signals carry information
of travel data alone for longitudinal and shear about the size and the nature of scatter.
waves. Some of the techniques used for velocity Techniques have been established to
determination are pulse echo overlap technique, quantitatively determine backscatter amplitude
pulse superposition method, sing around method for assessment of grain size and distribution of
and phase comparison method [40]. With the second phase particles [13]. Backscatter
advancement in electronics and digital measurement also finds applications in
technology, velocity can be measured with an determination of diffuse discontinuities like
accuracy of less than 1m/sec, making it a very micro-cracks that appear in components due to
reliable parameter for material property various degradation mechanisms.
characterization. Spectral analysis
Attenuation The ultrasonic wave traveling inside material
Attenuation refers to the loss of sound energy as consists of many frequency components. The
the ultrasonic beam passes through the material. energy distribution (amplitude) at different
Attenuation has two components, absorption and frequencies (frequency spectrum) can be
scattering. Energy loss due to absorption is a obtained by taking the Fast Fourier Transform of
result of mechanisms such as dislocation the back surface reflection. Two parameters that
damping, hysterisis losses, thermoelastic effects, can be useful from frequency spectrum for
etc. Loss due to scattering in polycrystalline material characterization studies are peak
materials depend on the ratio of grain size (D) frequency and the bandwidth. Due to changes in
and wavelength (). There are three distinct material properties some of the frequency
regimes of scattering, each having different components are preferentially attenuated as
attenuation coefficient depending on grain size compared to others. This causes change in the
(D), wavelength () and frequency (f). spectrum, which can be correlated with the
Attenuation co-efficient is measured by finding change in material properties.
the amplitude difference (dB) between the two Critical angles
backsurface signals and then dividing it by the
total path traveled. It is expressed in terms of When the longitudinal wave traveling in one
dB/mm. In more advanced techniques, the medium is incident at an angle on the interface
frequency spectrum (frequency vs. amplitude with the other medium, it undergoes refraction
plot) of two successive backsurface signals are and mode conversion. The refracted angle of
obtained. From these spectra, attenuation co- longitudinal and shear wave in other medium
efficient at different frequencies is found out depends on the incident angle as well as the ratio

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of sound velocities in the two media (Snells studies carried out in various laboratories for
Law). Increase in the incidence angle results in measurement of metallurgical properties:
increase in refracted angles of longitudinal and
Measurement of grain size
shear wave. At the first critical angle the
refracted longitudinal wave travels along the Grain size is one of the important
surface leaving only shear wave in the other microstructural properties, which controls
medium. At the second critical angle the mechanical properties like strength and fracture
refracted shear starts traveling along the surface. toughness. Measurement of grain size by
The values of these critical angles are very ultrasonic testing is based on measurement of
sensitive to the surface property of the material. scattering co-efficient [13-16]. Scattering co-
These can be measured very precisely by using efficient s is given by:
Goniometer for studying the surface property s = Cr. D 3.f 4 (1)
variation and case depth measurements in
components. Cr is the scattering parameter depending on the
type of wave used and the material anisotropy
Acoustic microscopy
D is the mean grain size.
Acoustic Microscopy refers to high resolution,
high frequency ultrasonic inspection techniques f is the frequency
that produce images of features beneath the The above equation is valid in Rayleigh
surface of the sample. Unlike optical Scattering range, where wavelength is greater
microscopy, where one can get information only than the grain size. This is the region in which
about the surface features, acoustic microscopes majority of ultrasonic examination is carried out.
give information about the bulk or volumetric The scattering co-efficient varies with the
features. In conventional ultrasonic testing the frequency as well as the grain size. To begin
frequency of examination varies from 1 to 10 with, calibration curves between the scattering
MHz. In Acoustic Microscopy, the frequencies co-efficient and known grain sizes at different
used are up to 1 GHz or even more. At these frequencies are obtained. Then scattering co-
frequencies the wavelength in most of the efficient for an unknown grain size is obtained at
engineering materials is of the order of few a particular frequency. From the calibration
microns. Hence, resolution of the order obtained curves the grain size is estimated.
with optical microscopes is achieved with
acoustic microscopes. Estimation of nom-metallic inclusions in steel
Characterization of Microstructural Non-metallic inclusions in steel can be in the
and Mechanical Properties by form of sulphides, alumina, silicates and oxides.
Ultrasonic Testing These inclusions adversely affect mechanical
properties like fatigue limit and often act as an
Studies have been carried out in various initiation site for pitting corrosion. They are also
laboratories to determine various microstructural responsible for poor surface finish, which cannot
properties like grain size, inclusion rating, etc. be tolerated for components used for sealing
and also mechanical properties like Youngs applications. Conventionally, metallographic
modulus, hardness, yield strength, tensile examination is carried out as per ASTM E 45 to
strength and fracture toughness. These properties rate the severity of these inclusions. These
have been determined by measurement of one or inclusions can be rated by ultrasonic
the combination of the above ultrasonic testing examination as well. There exists an ASTM
parameters. Following are the some of the standard E 588 titled Detection of large

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inclusions in bearing quality steel by ultrasonic crystallites form, which act as Rayleigh scatters,
method. The advantage of this technique is that yielding to higher value of N. With increase in
it can detect inclusions in the entire volume. temperature, more number of crystallites
However, this technique is not very sensitive to nucleates and few of them grow to a region of
all types and sizes of inclusions. Ultrasonic stochastic scattering. At this stage the value of N
examination involves immersion scanning of the drops. The onset, degree and the end of
component using 5 to 10 MHz transducer. recrystallization are monitored from the
Reflected signals from inclusions of various transition in the attenuation vs. temperature and
sizes and different depths are categorized into exponent of frequency vs. temperature plots.
different groups. The severity rating S is given
Determination of elastic modulus
by the following formula:
Elastic Modulus is related to the inter-atomic
S ={A (NL) + B (NM) + C (NH)} / V (2)
forces and hence indicates maximum attainable
A, B, C are weighting factors strength. There exists a direct mathematical
NL, NM & NH are number of low, medium & relationship between elastic modulus and
high level indications counted ultrasonic longitudinal and shear velocity. These
V is the volume of material tested relationships are as follows:
Measurement of degree of recrystallization Youngs Modulus E = . VT2. (3VL2 4VT2) /
(VL2 VT2) (4a)
In the Rayleigh scattering region, the attenuation
Shear Modulus G = . VT 2
(4b)
co-efficient is given by the Equation 1. In the
Bulk Modulus B = . (VL2 4. (VT2) / 3) (4c)
Stochastic scattering region, where the grain size
Poissons Ratio = (VL2 2. VT2) /
is of the order of wavelength, the attenuation
(2. VL2 2. VT2) (4d)
coefficient is given by
One of the major applications of modulus
s = Cs. D.f 2 (3)
determination by ultrasonic velocity
Cs is the scattering parameter measurements is for brittle materials since other
D is the mean grain size methods like tensile test produce poor results.
f is the frequency Youngs and Shear Modulus have been
determined in authors laboratory for several
Equation 1 & 3 indicate that with the increase in grades glass and resins. The values obtained are
grain size relative to the wavelength, there is the in good agreement with the ones reported in the
change in the exponent of ultrasonic frequency literature.
dependence on attenuation (from 4 to 2). This
factor has been found to be a key variable Estimation of hardness
relating ultrasonic attenuation to the thermal Hardness refers to the resistance of material to
kinetics of recrystallization process. Study was plastic deformation. It is measured in terms of
carried out on cold worked Nickel 200 rod to resistance to indentation by using Brinell,
correlate ultrasonic parameter with different Vickers and Rockwell hardness testers [18].
stages of recrystallization process [17]. The Ultrasonic hardness testers are also used in many
exponent of frequency dependence (N) is found applications, especially for in-situ measure-
out from the frequency vs. attenuation curves (s ments. In this technique a Vickers diamond is
= C.f N). At a constant frequency, the attenuation attached to one end of the magneto-strictive rod.
coefficient shows a non-monotonic behavior The diamond tipped rod is excited to its natural
with the increase in annealing temperature. frequency by a piezo-electric converter. The
When recrystallization starts, small nucleated resonant frequency of the rod changes as the free

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end of the rod is brought into contact with the Monitoring ductile to brittle transition
surface of a solid body. The change is frequency temperature
depends upon the area of contact between the
Ductile to brittle transition temperature (DBTT)
diamond tip and the test surface, which is
is related to the toughness of the material. It
inversely proportional to hardness of the test
represents the temperature below which the
specimen. Studies have also been carried out to
component is likely to fail by catastrophic brittle
measure velocity and attenuation for determining
fracture. In order to avoid this, it must always be
the hardness. It has been observed that the
ensured that the service temperature of a
velocity varies parabolicaly and attenuation
component is well above DBTT. Conventionally
varies linearly and inversely with the hardness.
DBTT is determined by Drop Weight Test
Estimation of strength (destructive) on coupons during the fabrication
stage. However during service, there can be
Strength of metals is estimated by subjecting the
factors like neutron irradiation, which increase
specimen to tension test. However, for non-
DBTT and may take it beyond the service
metallic materials like concrete and ceramics,
temperature. One of the important factors, which
tension test cannot be used. Ultrasonic velocity
control DBTT, is the grain size. For a fixed
measurement is an established and widely used
composition, DBTT increases with the grain
technique to estimate the strength of concrete
size. Since increase in grain size also results in
and ceramics. The following table gives the
increase in attenuation, attenuation measure-
relationship between velocity and the strength of
ments can be used to monitor DBTT. A study
concrete structure:
was carried out to monitor DBTT in Fe-C alloys
[20]. In these alloys DBTT increases with the
Table 1: Condition of concrete structure
increase in carbon content. For a fixed grain
vis--vis ultrasonic velocity
size, attenuation measurements were taken with
Velocity (m/sec) Structure Condition
varying carbon content. It was observed that
4575 and above Excellent
attenuation decreases with increase in carbon
3600 to 4575 Good
content (i.e. with increase in DBTT). The
3050 to 3600 Questionable reduction in attenuation is due to decrease in
2135 to 3150 Poor dislocation damping in high carbon steel, which
Below 2135 Very Poor is one of the predominant mechanisms of
absorption. For this alloy system it was observed
Ceramic materials are also characterized by
that although increase in grain size and carbon
ultrasonic velocity and attenuation
content increase DBTT, their influence on
measurements. Ultrasonic characterization of
attenuation variation is contradictory.
Alumina-Zirconia-Silica ceramic was carried out
in authors laboratory [19]. This ceramic Estimation of fracture toughness
material is used as refractory lining in glass Fracture toughness is an intrinsic property that
melting industry. The objective of this study was characterizes fracture behavior of a material. It
to correlate ultrasonic velocity and attenuation corresponds to the critical stress intensity factor
with the soundness of refractory. Ultrasonic at which crack propagates catastrophically.
measurements on the samples indicated that the Fracture toughness KC is given by:
velocity is found to be higher ((6800m/sec as
against 6400m/sec) and attenuation is found to KC = E. Gc (5)
be lower in the sound material as compared to E is the Youngs Modulus
the region where there exists a shrinkage cavity. Gc is the strain energy release factor

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E is related to ultrasonic velocity and KC is mechanical properties. Nodular cast irons are
related to the microstructure, which in turn superior in strength and toughness as compared
affects ultrasonic attenuation. Hence correlation to gray cast iron. Relationship between
exists between fracture toughness and ultrasonic ultrasonic velocity and strength is used to many
propagation properties via ultrasonic velocity industries to assure the strength of components
and attenuation. A Vary demonstrated the made of nodular cast iron. The increase in
feasibility of ultrasonic measurement of plane degree of nodularity increases the strength which
strain fracture toughness KIC for two grades of in turn results in increase in the ultrasonic
Maraging steels and a Titanium alloy [21]. The velocity [22, 23, 40].
following empirical correlation was found
Qualification of heat treatment of uranium
between ultrasonic attenuation slope and KIC:
rods
(KIC/Y)2 = M (Vl. / m) (6)
Uranium rods are used as fuel in nuclear
Vl is the longitudinal velocity research reactors. One of the critical steps in the
is d/df ( is attenuation coefficient and f is fabrication route of fuel elements is the heat
the frequency) evaluated at a particular treatment of uranium rods after hot rolling. The
frequency, which is based on mean grain size heat treatment randomizes the preferential
M is the empirical constant texture that gets developed during hot rolling
operation. The presence of texture leads to non-
Qualification of Processing Treatments uniform elongation during irradiation in the
During fabrication the components are subjected reactor. Conventionally, heat treatment of
to various processing treatments in order to uranium rods is qualified by thermal cycling test,
achieve required material properties. Studies during which the sample is subjected to 1000
have been carried out in various laboratories to thermal cycles from 0oC to 550oC and back. The
establish the feasibility of using ultrasonic acceptance criteria demands that the total
testing parameters to qualify these processing elongation after the test should not exceed 15%.
treatments. Some of these studies are discussed The thermal cycling test is very time consuming
below: and by the time the results are obtained the rod is
already loaded in the reactor. Hence, there was a
Nodularity of cast iron
need to develop an NDT technique by means of
Cast irons are classified based on the which heat treatment can be qualified quickly.
morphology of graphite. Carbon in cast iron can Ultrasonic testing technique based on velocity
be forced to agglomerate into spheroidal form or measurement was developed in authors
nodules during solidification of iron by the laboratory [24]. The following table gives the
addition of magnesium ferrosilicon to the melt. variation in axial and radial velocity in uranium
Lack of this treatment results in gray cast iron in rod for rolled and rolled & heat treated
which carbon is present in the form of flakes. conditions:
Graphite morphology in cast irons affects their

Table 2: Ultrasonic longitudinal velocity in uranium rods for different conditions

Condition Long. Velocity Long. Velocity
Radial (m/sec) Axial (m/sec)
Hot Rolled 3434 3242
Rolled, heat treated and water quenched 3365 3360

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This technique has now been incorporated as a measurement is carried out on coupon basis by
quality control step to qualify the heat cutting the sample at a particular location and
treatment of uranium rods. observing it under microscope. Weston
Bartholomew successfully carried out study to
Qualification of heat treatment of precipitation
measure case depth of carburized layer by
hardenable 17-4 PH stainless steel
ultrasonic testing. Measurement employed
17-4 PH Stainless Steel exhibits high strength surface waves and was based on finding the
and corrosion resistance. It is procured in critical angle at which Rayleigh waves are
solution annealed condition (Condition A), generated in the material. Rayleigh waves are
machined to desired shape and then subjected to confined to the surface (for a depth of one
low temperature heat treatment (900 -1000oF) to wavelength). The critical angle for generation of
achieve desired strength. Strength increases Rayleigh wave is given by:
during heat treatment due to precipitation of
copper. Ultrasonic testing technique based on R = Sin -1 (Cw/ Cr) (7)
velocity and attenuation measurement was
Cw is the velocity of longitudinal waves in water
developed in authors laboratory to qualify the
Cr is the velocity of Rayleigh waves in the
heat treatment of these steels [25]. The following
material
table shows the variation in velocity and
attenuation with heat treatment: Precise measurement of critical angle was
carried out by using a goniometer.
Table 3 : Variation in ultrasonic velocity and attenuation with It was observed that R increases
heat treatment for 17-4 PH SS with the case depth. A calibration
Heat treatment Hardness Longitudinal Attenuation curve was first obtained between
Condition Rc Velocity dB/mm case depth and R, by taking
m/s measurements on the samples of
Soln. Annealed 27 5776 0.120 known case depth at a particular
900oF/ 1hr 47 5878 0.159 frequency. Then the precise
1025oF / 4 hr 37 5839 0.160 critical angle for the unknown
1100oF / 4 hr 36 5877 0.173
case depth was found out by using
The table indicates that following the heat a goniometer. From the
treatment, the hardness increases and so does the calibration curve the case depth was estimated.
velocity as compared to the solution annealed This technique was able to measure the case
condition. There is also an increase in depth from 400 to 1200 micron with an accuracy
attenuation after heat treatment. of 50microns [26].
Measurement of case depth
Ultrasonic Characterization of
Many applications demand that the surface of Material Degradation during Service
component to be hard retaining its core in soft
and tough condition. In such cases, the Any engineering component when put in service,
components are subjected to surface hardening is designed to last for a definite amount of time,
treatments like carburizing, nitriding carbo- which is referred to as useful life or designed life
nitriding, flame hardening, etc. One of the of the component. There are many factors, which
important parameters that needs to be controlled adversely affect the designed life of the
in these processing treatments is the depth up to component and lead to its premature retirement
which hardening is carried out, referred to as from service. Such factors include, unanticipated
case depth Conventionally, case depth stresses (residual and system), operation outside

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designed limits (excessive temperature and load damage. Attenuation changes because of
cycling), operation and environmental effects, interaction of ultrasonic waves with physically
degradation of material properties in service, etc. deformed region or micro-crack that forms at an
Some of the most common types of degradation early stage of fatigue damage. Study was carried
mechanisms observed in engineering out by Joshi and Green [28] on aluminum and
components include fatigue, creep, uniform and steel samples by employing attenuation
localized corrosion, age hardening, hydrogen measurement as well as reflection based
damage, neutron irradiation, etc. It is difficult to technique. The results indicate that change in
predict the extent of their damage on the attenuation during the fatigue test is observed
serviceability of the component at the designed much earlier during the fatigue test than the
stage. It is also not possible to take out a coupon appearance of reflected signal in reflection based
from the component to assess its microstructural technique.
and mechanical properties for continued service
Early detection of creep damage
by destructive tests. Non-destructive evaluation
of material properties play a crucial role to Creep refers to the time dependent plastic
assess the damage caused by various degradation deformation at constant load at high temperature.
mechanisms in components during service. Creep damage is characterized by three stages
Ultrasonic testing is widely used in many viz. micro-pore formation at grain boundaries,
industries for this purpose. Following are some pore growth & pore coalescence and micro-
of the investigations carried out to characterize crack formation and crack growth. Density of
the material degradation during service by the material depends on pore concentration. The
ultrasonic testing: elastic and shear modulus is also affected by the
pore fraction. Since ultrasonic longitudinal and
Detection of fatigue damage
shear wave velocity is mathematically related to
Two techniques have been used for ultrasonic modulus of elasticity and density, their
detection of fatigue damage, one based on measurement forms the basis of detection of
reflection and the other on attenuation early creep damage. Dobmann observed that
measurement. Acoustic emission (AE) technique longitudinal, shear as well as Rayleigh wave
is also used, but the background noise during velocity decreases with increase in the pore
fatigue tests causes problems during AE. For fraction [29]. The measurements were sensitive
reflection based ultrasonic examination to detect the density change of the order of 0.8%
techniques, either using bulk waves or surface due to pore formation. Presence of pores also
waves, the fatigue crack has to be sufficiently affects the attenuation and very precise
deep to record a measurable signal. Hence, these measurement of this parameter gives useful
techniques are not suitable for detection of early information about the creep damage.
fatigue damage. However, these are best suited
Hydrogen attack in low alloy steel
for accurate sizing of cracks once they grow
deeper. Attenuation measurement has been Hydrogen attack in low alloy steel has been
observed to be very sensitive to detect early observed in components which are exposed to
stages of fatigue damage [27]. Since dislocation high pressure hydrogen at high temperatures.
motion is prerequisite to any kind of plastic The chemical reaction between hydrogen and
deformation and ultrasonic attenuation is steel produces methane gas, which bubbles at
sensitive to dislocation motion or dislocation grain boundaries, grow and interlink to form
damping, very precise attenuation measurement fissures and micro-cracks. These cracks are
during fatigue tests gives very useful responsible for lowering of fracture toughness of
information about the initiation of fatigue the material. It is important to detect this damage

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non-destructively in pressure vessel and piping (25-70ppm) to be measured reliably by

which are prone to such attack. Ultrasonic ultrasonic techniques. P.K. De, et. al. [32] used
testing parameters viz. velocity, attenuation and ultrasonic velocity, attenuation and electrical
backscattering have been observed to be very conductivity measurements to assess the
sensitive to detect hydrogen damage in low alloy hydrogen in the level of few hundred ppm. It is
steel [30, 31]. It is observed that the velocity in mandatory to carry out periodic in-service
the affected samples decreases (from 5800m/sec inspection of pressure tubes in the reactors to
to 5280 m/sec) due to overall decrease in bulk assure their structural integrity during operation.
modulus of elasticity caused by micro-cracks. While detection of DHC is based on
This parameter is useful to monitor extensive conventional ultrasonic flaw detection
damage. Attenuation, as expected is found to techniques, these are not useful for detection of
increase with the damage due to increase in hydride blisters. This is because the interface
scattering form the micro-cracks. Backscatter is between the zircaloy-2 pressure tube and the
found to increase in the affected sample due to zirconium hydride blister is a poor reflector of
impedance mismatch at the grain boundary. It is ultrasound. In order detect zirconium hydride
a useful parameter for monitoring low level of blister, two techniques were standardized in the
hydrogen attack. Its primary advantage is that authors laboratory [33-36]. Detection of
this parameter is unaffected by the condition of zirconium hydride blister is based on difference
inside surface of the component when the in longitudinal and shear wave velocity in
measurements are being made from the outside zircaloy 2 and zirconium hydride. It has been
surface. observed that the velocity ratio (longitudinal to
shear) for zircaloy-2 is 2.0 as against 2.8 for
Hydrogen damage in zircaloy 2
zirconium hydride. The velocity ratio at the
Zircaloy 2 (Zr-2.5%Sn. 0.1%Fe, 0.1%Cr and blister location is between these two limits
0.1%Ni) is used as pressure tube material in depending on the depth of blister. The change in
pressurized heavy water reactors. The corrosion time of travel at blister location due to difference
reaction during service between pressure tube in velocity was utilized to get the B-scan images.
and high temperature heavy water coolant results
Intergranular Corrosion attack in Austenitic
in evolution of hydrogen, a part of which is
Stainless Steel
absorbed in pressure tube material. In zircaloy
2 pressure tubes, damage due to hydrogen Intergranular Corrosion (IGC) attack refers to
manifests itself in two forms, delayed hydride localized corrosion along the grain boundary.
cracking and hydride blister formation. In the Sensitized steels (due to chromium depletion
former case, hydrogen migrates to a region of along grain boundaries) are prone to this attack
high localized stress like flaw tip, resulting in when exposed to corrosive environment.
precipitation of hydride platelets, their growth Conventionally, IGC tests are performed as per
and cracking. This cycle continues as the crack ASTM A262 Practice A to E. The severity of
initiates and grows in the pressure tube. In the IGC is expressed as depth of IGC attack.
case of blister, hydrogen migrates down the Ultrasonic velocity and attenuation are very
temperature gradient at a localized cold spot, useful parameters to monitor the depth of IGC
which can form if the pressure tube comes in attack [37]. Velocity is reduced in attacked
contact with the surrounding (cold) calandria region as the acoustic property of corrosion
tube during service. The hydride blister grows products filling IGC affected micro-cracks are
and cracks after attaining the critical size. There different than that of grain matrix. Attenuation
are threshold limits of hydrogen for initiation of increases in IGC affected region due to increased
DHC and blister, but these are too low scattering by micro-cracks at grain boundaries.

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Study carried in authors laboratory indicates 600oC) for 25,000, 50,000 and 1,00,000 hrs.
that with the depth of attack in excess of 200 Study indicated that in the service aged samples,
micron, there is a significant change in the both velocity and attenuation was higher as
velocity and attenuation. compared to virgin sample. No significant
difference was observed in these two parameters
Thermal Embitterment of Duplex Stainless
in samples exposed for different times. The
Steel
samples were then subjected to heat treatment
The microstructure of duplex stainless steel (700oC, 6 hrs.) in order to regain the mechanical
consists of austenite and ferrite. They offer high properties. Consequent to this heat treatment the
corrosion resistance, high strength & toughness velocity and attenuation reduces and approaches
and good weldability. They find extensive use in that of the virgin sample. The study established
chemical plants and marine construction. One of that the onset of age hardening in this alloy as
the degradation mechanism observed in duplex well as the recovery of its mechanical properties
stainless steel is the embrittlement during after heat treatment can be detected by
exposure to 600oC to 800oC, due to precipitation monitoring ultrasonic velocity and attenuation.
of sigma phase As a result the fracture toughness
comes down. E. Ikuta, et.al. carried out study on Conclusion
ultrasonic evaluation for thermal embrittlement
of duplex stainless steels. The test samples were Ultrasonic testing is traditionally used for flaw
annealed at 800oC for up to 10 hours to produce detection and characterization. The spectrum of
sigma phase. Ultrasonic measurements and ultrasonic testing applications is widened by its
destructive tests were performed on these use for material characterization. With the
samples. Ultrasonic evaluation involved advancement in electronics and digital
measurement of ultrasonic velocity, attenuation technology, ultrasonic testing parameters, which
and the central frequency of the received are affected by changes in material properties,
ultrasonic pulse. Destructive tests like Charpy can be measured with high accuracy to provide a
Impact Test and Vickers Test were carried out reasonable confidence level. Ultrasonic testing
to correlate ultrasonic parameters with the for material characterization can not play a vital
degree of embrittlement. It was observed that role in quality assurance during in-manufacture
while the attenuation decreases, the velocity and inspection but can serve as a powerful tool for
the central frequency increase with the life prediction technology during in-service
embrittlement [38]. inspection, residual life assessment and plant life
extension. There are however few difficulties
Ageing degradation in Alloy 625 which are encountered during ultrasonic testing
Alloy 625 (Ni based) is extensively used in for material characterization. There is no one to
chemical industry for its high temperature one mapping between ultrasonic parameters and
strength and corrosion resistance. Ageing microstructural / mechanical properties.
degradation during long term exposure at high Microstructural properties, which control the
temperature due to precipitation of Ni3Nb/ mechanical properties, affect the ultrasonic
Ni2Mo phase causes reduction in ductility and propagation factors differently. In order to
toughness. Study was carried out in authors establish any correlation between mechanical
laboratory to correlate ultrasonic testing properties and ultrasonic parameters the effects
parameters viz. velocity and attenuation with the of various microstructural properties on
degree of age hardening in Alloy 625 [39]. The ultrasonic testing parameters must be separated.
study was carried out on samples with high For quantitative material characterization,
temperature service exposures (approx. 500oC to empirical correlations and calibration must be

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BARC Newsletter Issue No. 249

established for each material. It is important to techniques An overview, ISNT Journal of

have a mechanistic understanding of relationship Non-Destructive Evaluation, Vol. 17, No. 1,
between ultrasonic testing parameters and 1997
individual microstructural properties for 10. G. Dobmann, et., al., Ageing material
effective non-destructive characterization of evaluation and studies by non-destructive
material properties and their performance. techniques (AMES-NDT), A European
Network Project, Nuclear Engineering and
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9. D.K. Bhattacharya, Characterization of structure, Testing and Quality Control,
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BARC Newsletter Issue No. 249

conducted by ASM India Section, May magnetic techniques) for strength and
2001, Mumbai. toughness prediction and the detection of
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38. E.Ikuta, et.al. Ultrasonic evaluation of 625, Proc. of 14th World Conference on
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of aging degradation during long term high 374
temperature exposure in Nickel base alloy

This paper received the Best Paper Award during the National Seminar
on Non-Destructive Evaluation, NDE 2003, conducted by Indian Society
for Non-Destructive Testing, held at Trivandrum during December 2003

About the authors ...

Mr P.P. Nanekar is a metallurgical engineer from VNIT, Nagpur. He joined BARC in the year
1992 (35th batch of BARC Training School) and is working in the field of Non-Destructive
Testing. He holds a Level III certificate in ultrasonic testing and Level II certificate in eddy
current testing and liquid penetrant testing. His field of work includes:
Development of techniques for in-service inspection of nuclear reactors
Quality assurance during fabrication of nuclear reactor components
Flaw characterization by advanced ultrasonic testing techniques
Material characterization studies on nuclear fuel, zirconium alloys and stainless steel
He has published over 30 technical papers in the field of NDT. Three of his papers, including the two presented
during 14th World Conference on NDT, received Best Paper Award.

Mr B.K. Shah did his B.Sc. Engg. (Metallurgy) from Regional Institute of Technology
(RIT), Jamshedpur and M.Tech. (Corrosion Science & Engg.) from Indian Institute of
Technology (IIT), Bombay. He joined BARC in 1973(17th batch of BARC Training
School). Presently, he is Head, NDT & Quality Evaluation Section, Atomic Fuels Division,
BARC. His field of work includes :
Quality assurance in the manufacture of nuclear fuel & reactor core components
Material characterization by NDT
Metallurgical failure analysis
In-service inspection
Corrosion studies on reactor materials
He has published more than 160 technical papers in various National & International journals and Conference
proceedings. He has received best paper awards for four technical papers, including the two presented during
14th World Conference on NDT. In recognition of his contributions to the Research & Development in the area of
Non-destructive Testing & Evaluation, he has been awarded NDT National Award 1998 and ISNT Mumbai
Chapter NDT Achievement Award 2001.
He is a Life Fellow of Indian Society for NDT and Regional Controller of Examination (Western Region),
National Certification Board on NDT. He is Life Member of IIM, INS, IVS, & NAARRI.

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