Nuclear Engineering and Design 323 (2017) 345–358

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Nuclear Engineering and Design

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

Miniature test techniques for life management of operating equipment

Kundan Kumar a,⇑, K. Madhusoodanan a, R.N. Singh b
a
Reactor Engineering Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085, India
b
Mechanical Metallurgy Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085, India

h i g h l i g h t s

Methodology for scooping out small volume of material from any operating equipment.

Preparation of miniature test specimens from scooped volume of material.

Special test fixtures for conducting miniature tensile and fatigue tests.

Determination of miniature tensile specimen geometry.

Development of new UTS correlation based on necking zone of SPT disk specimens.

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

Article history: Life management of operating equipment is always a preferred way for maximising its operating life
Received 14 September 2016 effectively and safely. Many novel test techniques, based on hardness or indentation methods, are used
Received in revised form 2 March 2017 for assessing the material properties of the equipment to ensure its safe operation. The novel test tech-
Accepted 3 March 2017
niques are correlation based indirect test methods to provide tentative material properties, which help in
Available online 22 March 2017
determination of residual life of the equipment. In comparison to these indirect test techniques, residual
life estimate based on miniature test techniques are unique and precise as they give direct material data
Keywords:
from the equipment. This is achieved by conducting destructive test of miniature test specimens, which
Life management
Boat sample
are made from the material scooped out from the operating equipment. The critical issue is reliability and
Miniature specimens acceptability of these results from miniature test specimens in absence of any international standards.
Tensile test Considerable work is going on in this direction for making the miniature test techniques as standard test
SPT techniques, which will make it acceptable to all concerned enabling them to exploit many of its advan-
Fatigue test tages. Even though various applications of miniature test techniques are found in literature, this paper
discusses one of the important industrial applications of the technique which is in the field of life man-
agement of operating equipment. Due to lack of standardisation, there are many issues with the minia-
ture test techniques, which must be addressed prior to its application in any area. This paper discusses
the issues with some of the miniature test techniques, viz. tensile test, fatigue test and small punch test
techniques. These issues have been addressed using experimental, analytical and metallurgical methods
to make the techniques suitable for application in life management of equipment. At the end, scope of
application of miniature test techniques in development of a new material, named as functionally graded
materials (FGM), has been discussed.
Ó 2017 Elsevier B.V. All rights reserved.

1. Introduction component. In order to assess the available safe operating margin,

the equipment needs to be periodically inspected to know the
Degradation of material properties of equipment due to pro- existing material properties. Various inspection methods are used
longed operation in harsh operating conditions, like radiation, high in industries for estimating the existing material properties for
temperature and high pressure, is one of the primary concerns to ensuring continued operation of the equipment. In case of non-
be addressed for its continued safe operation. Material degradation replaceable equipment, the inspection becomes vital as in-situ
leads to reduction in safe operating margin of the equipment or inspection methods are required with enough reliability of the
inspection data, as erroneous data may lead to wrong assessment
of safe operating life and may result in failure and subsequent
⇑ Corresponding author.
major consequences. Evaluation of the existing material properties
E-mail address: [email protected] (K. Kumar).

http://dx.doi.org/10.1016/j.nucengdes.2017.03.007
0029-5493/Ó 2017 Elsevier B.V. All rights reserved.
346 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358

of such in-service equipment, precisely, is a major thrust area for 1991; Jung et al., 1996; Kohno et al., 2000; Byun et al., 1998;
long, which has resulted in the development of many invasive Sergueeva et al., 2009) in terms of material, gauge length, cross-
and non-invasive techniques. section, thickness, grain-size, number of grains in cross-section,
Hardness measurement based techniques, such as indentation fabrication method, load frame, test parameters etc. have been car-
and micro-hardness tests have been quite popular among other ried out in order to standardise the specimen’s geometry, fabrica-
non-invasive techniques. Several researchers have used the inden- tion and testing methods. This paper also is a part of this global
tation test and have suggested direct correlations of the measured effort towards standardisation of miniature specimen test tech-
hardness value with yield and tensile strengths (Tabor, 1951; nique for fruitful purposes. As an application of miniature test
Shabel and Young, 1987; Lai and Lim, 1991; Gasco and techniques for life assessment of equipment, this paper gives
Rosenberg, 2011) of the materials. The disadvantage of the sug- details of the scooping technique to obtain boat sample from the
gested correlations is that they are valid only for specific classes equipment, preparation of miniature test specimen from boat sam-
of materials and this makes the use of the hardness properties a ple, description of testing apparatus and testing methodologies for
procedure lacking in accuracy and not generally appropriate for miniature tensile, SPT and fatigue test specimens, and test results.
evaluating the main material strength parameters (Blagoeva It is likely that scooping device would be deployed at boiling water
et al., 2007) and these correlations are not universal (Dobi and reactors (BWRs) at Tarapur for health assessment of t he core
Junghans, 1999; Dedov and Klevtsov, 2012). shrouds. This paper discusses the preparedness for the operation
These days, miniature test techniques are increasingly being with full scale mockup trial and determination of mechanical prop-
used in getting direct material data in such cases. For this purpose, erties using miniature tensile and SPT specimens from mock boat
scooped out material is used for preparation of various types of sample. One of the potential application areas of miniature test
miniature test specimens, viz, tensile test, small punch test (SPT), techniques is development of new material. At the end of the
and fatigue test specimens etc. These miniature test specimens paper, future application of miniature test techniques is discussed
require very small volume of material, of the order of 1/500th of for development of functionally graded materials (FGMs).
that required for a standard tensile test specimen (Manahan
et al., 1986). These techniques are very attractive and have many
2. Development of scooping device
benefits (Panayotou et al., 1986; Rosinski et al., 1993; Xu et al.,
2000; Kohno et al., 2000; Jung et al., 1996; Klueh, 1985; Kumar
Scooping a physical sample from the service-exposed equip-
et al., 2014), however at the same time they have many chal-
ment/component is preferred, if margin is available in the material
lenges/issues. One of the issues is lack of standardised miniature
thickness. Sampling process is effectively non-invasive in the sense
specimen geometry for tensile test which could give data compara-
that scooping of material does not require post-sampling repair or
ble to that from standard tensile tests. Many efforts have been put
reduced operating functionality for subsequent service life of the
towards standardisation of specimen geometry of miniature ten-
component. In the process, a small volume of material is scooped
sile specimens, which has resulted in development of various
out from any in-service equipment, in a non-destructive manner
designs of tensile specimens (Klueh, 1985; Kohyama et al., 1986,
(Xu et al., 2000; Kumar et al., 2002; Klevtsov et al., 2009; Madia
1991; Jung et al., 1996; Byun et al., 1998, 2001; Dai et al., 2008;
et al., 2013). For the present case, Boat Sampling Technique (BST)
Dobi and Junghans, 1999; Kim et al., 2009; Klevtsov et al., 2009);
was developed and has been discussed elsewhere (Kumar et al.,
however, no consensus has been arrived on standardised specimen
2014, 2002). The technique, utilizes a scooping device, known as
geometries and still there is an ambiguity in this regard. One of the
‘Sampling Module’, shown in Fig. 1a, which operates under water
hurdles in standardisation of geometry is the determination of
filled condition and grinds out a boat-shaped sample. The sampling
thickness of tensile test specimens, which has been attempted by
operation is an internal grinding operation and the sample is
many (Kohyama et al., 1991; Byun et al., 1998; Kohno et al.,
obtained by spinning the cutter, Fig. 1b, about its axis of symmetry,
2000), however, no consensus has been arrived so far to define
Fig. 1c, while slowly advancing it about a perpendicular axis to feed
the minimum thickness requirement. Due to these geometrical
the cutter into the parent material. The overall process of scooping
issues there is non-conformity of strength and ductility data from
is remotely controlled and at the end of the sampling operation,
miniature tensile tests with standard tensile tests.
the boat sample falls in the cutter shell or in module housing by
Small punch test techniques use correlation based methodolo-
gravity, which is collected remotely. Fine mesh powder is gener-
gies for evaluation of mechanical properties from TEM-sized disk
ated due to grinding action during sampling which is lost in the
specimens. Yield strength (YS) and ultimate tensile strength
pool water.
(UTS) and other material properties are evaluated from the load-
The scooped material, known as ‘boat sample’, Fig. 2a, is used to
displacement plots from the SPT experiments. It may be noted that
carry out required mechanical & metallurgical tests. A typical boat
the correlations for evaluation of YS (Lucas et al., 1986; Mao and
sample is elliptical in shape and has approximate dimensions as
Takahashi, 1987; Kameda and Mao, 1992; Vorlicek et al., 1995;
40 mm long, 25 mm wide and 3 mm thick at centre. The thickness
Xu et al., 2000; Flueury and Ha, 1998; Wang et al., 2008;
of the boat sample can be controlled by the thickness of the control
Rodríguez et al., 2009; Garcia et al., 2014; Singh et al., 2014) using
device in the module.
Py (value of load corresponding to the transition from elastic bend-
The depth of the depression left in the base material is known as
ing to plastic bending in the SPT plot), are more or less in agree-
scooped region and is equivalent to the sample thickness plus the
ment with YS obtainable from conventional tensile tests, but
kerf width. The contour of scooped region, shown in Fig. 2b, merges
correlations for evaluation of UTS (Lucas et al., 1986; Mao and
smoothly with the parent material to avoid stress concentration
Takahashi, 1987; Vorlicek et al., 1995; Flueury and Ha, 1998; Xu
and there is no loss of integrity or reduction in service life of the
et al., 2000; Klevtsov et al., 2008, 2009; Wang et al., 2008; Garcia
equipment. The scooped region has approximate dimensions as
et al., 2014; Singh et al., 2014) using Pmax (max. value of load in
45 mm long, 30 mm wide and 4.5 mm depth at centre.
the SPT plot) are in disagreement.
Efforts are ongoing at world level for making miniature test
techniques as standard test techniques, which has resulted in 3. Preparation of miniature test specimens from boat sample
development of various correlations for SPT, fatigue tests and
miniature tensile tests. Parametric studies of miniature tensile A number of miniature size test specimens, viz. miniature ten-
specimen (Klueh, 1985; Panayotou et al., 1986; Kohyama et al., sile specimen of gauge length 3-5 mm, small punch test specimen
 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358 347

Fig. 1. Photographs of (a) sampling module and (b) cutter; and (c) schematic of scooping operation.

Fig. 2. Typical geometry of (a) boat sample (X = 25 mm, Y = 40 mm, T = 3 mm) and (b) scooped region (H = 45 mm, W = 30 mm, D = 4.5 mm).

of diameter 3 mm, miniature hour-glass shaped fatigue test speci- which leads to different material behaviour in the microscale com-
men of 3 mm diameter, and miniature Charpy impact test speci- pared to the mesoscale and macroscale (Sergueeva et al., 2009). In
men can be extracted from the boat sample, as shown in Fig. 3. mechanics, this effect is limited to the strength dependence on
The miniature test specimens have certain issues, due to which cross-sectional area, however in general it is much wider and
these are not accepted as standard test techniques. Following sec- may relate not only to specimen size and geometry, but also, to
tions discuss briefly about these issues, efforts towards addressing other factors, such as micro-structural constraints, viz. thickness,
these issues, and application of miniature test techniques, related grain size, anisotropy due to microstructure & crystallographic tex-
to tensile test, SPT and miniature fatigue test. Discussion on minia- ture, micro-structural and chemical inhomogeneity etc., surface
ture impact test specimen is not part of this paper. effect and residual stresses. These requirements have lead to a
number of parametric studies in terms of gauge length, cross-
section, thickness, grain-size, number of grains in cross-section,
4. Miniature tensile test fabrication method, load frame, test parameters etc. (Klueh,
1985; Panayotou et al., 1986; Kohyama et al., 1986, 1991; Kohno
The major issue of using miniature tensile specimen is the reli- et al., 2000; Byun et al., 1998, 2001; Sergueeva et al., 2009).
ability and acceptability of the test results, which need validation In order to have reliable data from miniature tensile specimens,
through standard tests and numerical analyses. Miniaturisation it was required to address some of the issues related to size-effect
of specimen causes the so-called ‘size effect’ or ‘scaling effect’, by way of optimising the geometry of miniature tensile test spec-

Fig. 3. Layout of miniature test specimens in a boat sample.

348 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358

Table 1
Chemical composition of materials taken for study(wt%).

Material C Cr Mo Mn Ni S P Si Cu Co N V
20MnNiMo55 0.18 0.078 0.49 1.24 0.58 0.007 0.014 0.23 0.067 0.0069 0.0068 –
CrMoV 0.17 2.51 0.63 0.38 0.8 0.009 0.015 0.28 0.054 0.013 0.065 0.17
SS304LN 0.022 18.60 0.24 1.73 9.32 0.004 0.018 0.46 0.28 0.11 0.071 –

Fig. 4. Microstructures of (a) 20MnMoNi55, (b) CrMoV Steel and (c) SS304LN materials.

Table 2
Mechanical properties of materials.

Temp 20MnMoNi55 CrMoV SS304LN

YS UTS Elongation, % YS UTS Elongation, % YS UTS Elongation, %
MPa MPa MPa MPa MPa MPa
Uniform Total Uniform Total Uniform Total
25 484 629 10.4 22.8 471 610 10.2 20.8 245 584 67.6 75.9
100 451 582 8.1 18.2 425 544 7.4 19.3 178 455 56.8 71.3
200 433 573 6.8 14.9 400 516 7 18.2 137 404 44.2 56.5
250 453 600 8.1 19.3 399 514 6.4 16.7 132 387 43.1 54.8
300 457 621 8.4 17.9 394 503 6.2 15.8 118 395 43.7 52.0

imen which can be prepared from the scooped volume of materi- jected to quenching and tempering treatment. Quenching of
als. This was done by way of experimentations on three different CrMoV steel was carried out from 950 °C followed by tempering
materials (given in next section), FEM analysis, analysing the fail- at 650 °C for 25 h. Chemical compositions of these materials are
ure behaviour of test specimens and fractography. given in Table 1 and the microstructures are shown in Fig. 4. The
mechanical properties of the materials are given in Table 2.
4.1. Materials used for experiments

Two pressure vessel materials, 20MnMoNi55 and CrMoV low 4.2. Testing apparatus and methodology
alloy steels and one piping material, austenitic stainless steel
304LN were selected for conducting the experiments. A 10kN screw driven universal testing machine, Fig. 5(a), was
20MnMoNi55 steel was cut from 130 mm thick plate, whereas used for conducting all the tensile tests. The miniature specimen,
CrMoV was cut from 60 mm thick plate. SS304LN was a cut section having very limited size and grip section, required development
of a pipe of inner diameter 275 mm and outer diameter of 325 mm. of special testing grips, which is shown in Fig. 5(b). The grips have
20MnMoNi55 and SS304LN materials were used for making test the provision for holding the specimens through their shoulders
specimens in as received condition, whereas CrMoV steel was sub- while conducting the tests.
 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358 349

4.3. Determination of thickness and other dimensions of miniature

tensile specimen

In order to determine the minimum thickness of miniature ten-

sile test specimens, tensile tests were conducted on miniature
specimens, having 1 mm width but with varying thicknesses,
0.15, 0.2, 0.25, 0.3, 0.35 and 0.4 mm. The stress-strain graphs of
all these experiments are as shown in Fig. 8. These graphs, shown
in the present work are presented with additional data besides the
ones published earlier (Kumar et al., 2016). It was observed that for
thinner specimens, yielding and failure took place early in compar-
ison to thicker specimens, resulting in lesser value of strength and
ductility data for the former. This behaviour was prominent in 0.15
Fig. 5. Photographs of (a) universal testing machine, 10 kN capacity and (b) special and 0.2 mm thick specimens among all the three materials. In
grips for miniature tensile test specimens. order to assess the reason for early failure of thinner specimens
and to understand the type of fracture taking place in various
thicknesses of specimens, further analyses were carried out on
the broken test specimen, using photographs, fractographs and
FEM analyses, which is described elsewhere (Kumar et al., 2016).
The images were analyzed to find out variations in geometries of
the broken neck regions; viz. diffused neck length, neck angle
and fracture angle. These three parameters were found to be useful
in determining the minimum thickness as these give information
about the ability of the specimens to resist necking and failure.
Lack of this resistance due to inadequate volume of material in
the gauge section results in early necking and failure of specimen,
which shows lesser strength and ductility values.
The lower values of the YS and UTS for thinner specimens, Fig. 8,
can be explained by the Ashby’s model (Dieter, 2013) as well. In a
standard tensile test, the grains of a polycrystalline material con-
strain each other to accommodate the misfit between them in
the form of geometrically necessary dislocations, Fig. 9, which
induce the long-range back stress fields. For yielding to take place,
Fig. 6. Photographs of (a) video extensometer (b) camera image from video the applied stress, rAPP, has to overcome the back stresses, r1B, r2B
extensometer with marked gauge length on the test specimen. and r3B in directions 1, 2 and 3, as shown in Fig. 10. At the same
time, the back stress components normal to the surface should
be relaxed to satisfy the plane stress condition. For specimen of
Due to non availability of sufficient space for mounting a sufficient thickness, the crystals within the specimen are able to
mechanical extensometer of the miniature tensile test specimen, resist the applied tensile stresses, as discussed above, by creating
a video extensometer based strain measurement system was used, back stresses; however, for thinner specimens there are less or
which is shown in Fig. 6(a). The video extensometer works on the relaxed induced back stresses in the thickness direction, r3B  0,
principle of pattern recognition technique. The test specimen is Fig. 10, to resist the yielding. Thus, the relaxed back stresses reduce
marked with contrast patterns prior to loading in the machine. the yield strength and UTS of thinner specimens.
The camera tracks the marked targets on the test specimen, Fig. 6 Lower value of r3B, which is approximately equal to zero in case
(b), and gives the displacement data. of thinner specimens, as explained above, is also responsible for
To ensure the usefulness of miniature test techniques it is low ductility values. Preferential straining in thickness direction
important to have comparable results of miniature tests and con- takes place due to maximum resolved shear stresses being higher
ventional tests with respect to the mechanical properties, viz. in thickness direction, i.e. s1–3  s1–2, as shown in Fig. 10 and given
UTS, YS and elongation. Validation of mechanical properties in Eq. (1) (Byun et al., 1998). The plastic deformation is localized in
obtained from miniature tensile specimen has been done by com- thickness direction even before the development of plastic instabil-
paring them with the results of sub-size tensile specimens, Fig. 7. ity. Necking takes place when strain in thickness direction
Sub-size and miniature specimens were made from same blocks becomes equal to the critical strain for plastic instability. After
of materials of 20MnMoNi55, CrMoV steel and SS304LN for the the initiation of plastic instability, the elongation increment (total
comparison purpose. In order to have comparable tensile data elongation-uniform elongation) reduces in thin specimens. This
the miniature test specimen needed to be geometrically similar causes lesser value of total strain
to the sub-size specimen (Dieter, 2013). This required optimisation
of the various geometric dimensions of the tensile specimens, such r1  r3 r1  r2
s13 ¼ P s12 ¼ ð1Þ
as gauge length (L), specimen thickness (t) or cross sectional area 2 2
pffiffiffi
(A), in order to have similar L= A ratio among miniature and These experimental results were corroborated with FEM analy-
sub-size test specimens. Among these geometrical parameters, sis (Kumar et al., 2016) to conclude that for the given three mate-
thickness of the test specimen needs serious consideration, as rials 20MnMoNi55, CrMoV steel and SS304LN, the required
other parameters are based on the availability of material, like size specimen thickness was 0.3 mm for getting tensile data compara-
of boat sample in present case; and can be based on geometric ble to standard specimens’ results. The optimized dimensions of
ratios. The thickness of the test specimen was determined based the miniature tensile specimens, obtainable from boat sample,
on a number of experimental and numerical analysis, as described are given as gauge length: 3 mm, width: 1 mm and thickness:
in Section 4.3. 0.3 mm, as shown in Fig. 7(b).
350 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358

Fig. 7. Dimensional details of (a) sub-size flat specimen and (b) miniature tensile test specimen and respective photographs in (c) and (d).

Fig. 8. The engineering stress – strain plots for varying thicknesses for (a) 20MnMoNi55 steel, (b) Cr-Mo-V steel and (c) SS304LN obtained using miniature test specimens.

5. Small punch test (SPT) lations till date has made the SPT rather more challenging and
attractive. Due to these reasons, with progress of time, many
Even though SPT does not give direct mechanical properties as researchers have joined the field and have put their efforts to
the universal tensile test does, its ability to evaluate these proper- establish the universal set of correlations for estimation of
ties, based on the correlations has made it attractive. It is also a fact mechanical properties.
that some of these correlations have established themselves, such One such correlation is for evaluation of UTS using SPT, which
as correlation for YS, but at the same time, some are yet to be has been an open issue since the development of the technique.
established. The inability to establish a universal set of such corre- Various correlations of UTS developed by different researchers
 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358 351

Fig. 9. Ashby’s model of deformation of polycrystalline material (a) Polycrystalline material deforms in macroscopic uniform way, produces overlap and voids at boundaries
(b) These can be corrected by introducing geometrically necessary dislocations at (c) and (d). Here statistical dislocations have not been shown (Dieter, 2013).

Fig. 10. Maximum resolved shear stress in tensile test specimen.

(discussed earlier), however, the most popular correlation has been 5.2. Testing apparatus and methodology
given by Mao and Takahashi (1987). They gave the following cor-
relation for evaluation of UTS using SPT: For conducting SPT experiments, a test setup was developed as
shown in Fig. 11. Internal arrangement of the test setup is also
Pmax shown as a cross-sectional view in Fig. 11. A typical load-
UTS ¼ 130  320 ð2Þ
t20 displacement curve of SPT experiment is shown in Fig. 12. The
SPT curve has in general four zones; namely (I) elastic bending,
where, t0 = specimen initial thickness, mm, UTS = ultimate tensile (II) plastic bending, (III) membrane stretching, and (IV) instability.
strength, MPa, Py = yield load, kN and Pmax = maximum load, kN As discussed above, various correlations have been given by vari-
UTS correlations based on Pmax, i.e. maximum value of load in ous researchers based on some points on this curve; for example
load-displacement curve, have also been used by others (discussed YS is given in terms of Py whereas the UTS is in terms of Pmax.
earlier), but these correlations, including the one from Mao and For the present work, SPT disks of 3 mm diameter were fabri-
Takahashi, have been in disagreement (Campitelli et al., 2004; cated using EDM process and were polished with 1000, 1200,
Garcia et al., 2014). Their argument is that the point corresponding 2400 and 4000 grit papers prior to final diamond polishing for
to Pmax does not represent a necking situation as in case of a uni- 0.25micron surface finish with a target thickness of 0.25 mm
axial tensile test and they suggested that the necking situation (±0.002 mm).
appears prior to Pmax (Campitelli et al., 2004; Garcia et al., 2014).
Based on this information, an UTS correlation was developed, by 5.3. Development of correlation for UTS
locating necking zone, through experiments and FEM analyses
and has been discussed elsewhere (Kumar et al., 2015). It was SPT disk specimens from the three materials, 20MnMoNi55,
found that for the necking of disk specimens for the given test CrMoV steel and SS304LN, were used for conducting the experi-
parameters was near 0.48 mm of punch displacement and load ments at a displacement rate of 0.2 mm/min. Tests were conducted
corresponding to this displacement value was used for develop- at 25 °C, 100 °C, 200 °C, 250 °C and 300 °C for each material and the
ment of UTS correlation. For present work also, since same test load-displacement plots of these are shown in Fig. 13. Load corre-
set-up is being used, P0.48 value would be utilised for development sponding to 0.48 mm punch displacement was found out for each
of UTS correlation. load-displacement plot and value of P0.48/t20 were evaluated. Plot of
P0.48/t20 vs. UTS was used to evaluate the UTS correlation, as shown
in Fig. 14. The UTS correlation, obtained, is given as
5.1. Materials used for experiments UTS = 130*P0.48/t20 + 19. However, in our previous work (Kumar
et al., 2015) the UTS correlation obtained was UTS = 130*P0.48/
Same materials, as discussed in Section 4.1, i.e. 20MnMoNi55, t20 + 6. One of the reasons for the different offset values in these
CrMoV ferritic steel and SS304LN, were used for the experiments two correlations may be the number of SPT experiments carried
for small punch tests also. out in each case. While in present case only 15 numbers of exper-
352 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358

ricate the standard size test specimen. With a knowledge that fati-
gue strength evaluated by the axial loading test is independent of
specimen size while that evaluated by bend test and torsion test is
dependent on the specimen size, (Nunomura et al., 1993), it was
preferred to develop a TEM size test specimen, with special align-
ment and gripping fixture. A tension-tension test method was
adopted by Nunomura with a stress amplitude and with a stress
ratio of 0.1 and cyclic frequency of 25 Hz, however he didn’t prefer
fatigue test due to complicated gripping system. Hong and Weil
(Connolley et al., 2005) performed stress-controlled LCF on
0.25 mm electro deposited copper foils and 0.33 mm thick wrought
foils. The stress-life data fitted the Basquin equation

re ¼ r0f ð2Nf Þp ð4Þ

where re is endurance limit, r0f is fatigue strength coefficient, Nf is

cycle to failure and p is a constant
Volak et al. conducted tension-tension fatigue tests on seven
different steels and an Al-alloy on conventional as well as on
miniature specimen of hour-glass shaped and concluded that S-N
Fig. 11. Small punch test (SPT) setup. curve of miniature test specimens have a steeper course in com-
parison to the conventional ones for all the tested materials. How-
ever, he failed to establish any valid correlation between the
fatigue results of the two types of specimens.
In the present work an hour-glass shaped miniature test speci-
men of 0.25 mm thickness and 3 mm diameter was used, as shown
in Fig. 15, with a specially developed gripping and alignment fix-
ture, as shown in Fig. 16. The results from miniature specimen
were compared with those from sub-size specimen, Fig. 17, in
tension-tension test. It may be noted that, even though the beha-
viour is same, there is a scaling effect when the specimen size is
reduced. Based on further experiments on other materials, an
attempt for development of correlations between standard and
miniature test results would be made. It is expected that the
miniature disk specimen could be used as a screening test to
quickly assess the fatigue behaviour of irradiated materials.

7. Application of miniature test technique for evaluation of

mechanical properties of core shrouds of Indian BWRs at
Tarapur

Fig. 12. Typical load vs. displacement curve with different zones in SPT. It is proposed to deploy the BST at Tarapur BWR for health
assessment of core shroud of the unit-1 and unit-2 of the reactors,
iments were carried out, in previous work this number was more
in the light of available information world over regarding core
than 70. Based on these it can be argued that if adequate numbers
shroud cracking at H4A and other weld locations. For the purpose,
of experiments are carried out, we may get a correlation without
a full scale mock up facility, as shown in Fig. 18(a), was created at
any offset values, as given in Eq. (3), below:
Tarapur, simulating top and bottom grid plates and the H4A weld
P0:48 location of the core shroud. The sampling module was attached to
UTS ¼ 130 ð3Þ a specially developed handling manipulator, Fig. 18(b), for opera-
t20
tion in the core shroud. The mock-up facility was placed at bottom
of a water pool having 12 m depth. The sampling module was low-
6. Miniature fatigue test ered in the water pool and positioned between simulated top and
bottom grid plates of the mock-up facility. Sampling operation was
Component failure due to cyclic loading is one of the major done on the parent material near the simulated H4A weld. Boat
areas of concern which requires evaluation of the fatigue life of sample, Fig. 18(c) was collected in the sampling module. The sim-
the component before and after some time of service (Volak ulated shroud plate was left with an impression of scooped region,
et al., 2012). Fatigue test methods and specimens of different sizes Fig. 18(d). The sampling operation was monitored through camera
have been developed for evaluation of fatigue life, however for any apart from the features available in the sampling module. The full
operating component; the residual fatigue life estimation is never scale mock-up trials reaffirmed the capability of BST for actual core
so easy, especially due to non-availability of sufficient material for shroud sampling operation.
making the test specimen of conventional size.
Despite the well-known fact that a material may fail at a stress 7.1. Experimental results of miniature tensile and small punch test
considerably lower than the normal breaking stress if the load is specimens prepared from mock boat sample
applied in a cyclic manner, the fatigue properties of highly irradi-
ated wall materials have not been studied in detail (Nunomura A mock boat sample, as shown in Fig. 18(c), was subjected to
et al., 1993), mainly due to the unavailability of the material to fab- electro-discharge machining (EDM) process for extracting a num-
 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358 353

Fig. 13. Experimental load-displacement graphs from SPT for materials (a) 20MnMoNi55 steel, (b) CrMoV ferritic steel and (c) SS304LN.

7.2. Comparison and validation of tensile test data from miniature

tensile specimen from mock boat sample

Tensile tests were conducted at room temperature at a strain

rate of 103 per sec on miniature size test specimens, prepared
from the mock boat sample of SS304 materials, as shown in
Fig. 20. The composition of the SS304 material used is shown in
Table 3. The tests were conducted on a screw driven machine.
The strain values were measured using single camera video exten-
someter. The sub-size specimens from the same block were also
tested under similar conditions. The results are summarized in
Table 4 and Fig. 20. For miniature specimen the UTS and YS values
are in the range of 725–751 MPa and 423–471 MPa in comparison
to respective sub-size values as 727–741 MPa and 438–455 MPa.
The minimum UTS values for both the cases are very close to each
other while the minimum YS values are within 3.5% range. The per-
centage uniform elongation and total elongation values for minia-
ture specimen are 46.2–59.6 and 58.6–74.3 in comparison to
respective sub-size values as 46.6–62.7 and 64.5–75.
The minimum uniform percentage elongation for both the cases
are very close to each other, however the minimum total percent-
Fig. 14. Development of correlation for UTS using SPT. age elongations are within 10% range. Due to high ductility of
SS304 material, during testing, there is overall stretching in the
ber of miniature test specimens, Fig. 19. These test specimens were parallel section of the specimen and there is continuous strain
subjected to polishing using SiC papers having various grit sizes hardening till the failure and there is not much deformation after
1000, 1200, 2400 and 4000, for removing the disturbed and recast necking. Therefore uniform elongation values are very close to
layer on the both sides of the surfaces of the test specimens. Small total elongation values. Overall it can be concluded that the results
punch test specimen needed final polishing by diamond paste of obtained by miniature test specimens are comparable with those
0.25 mm prior to conducting the test. obtained by conventional sub-size test specimens within a very
354 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358

Fig. 15. Dimensional details of a) sub-size and b) miniature fatigue test specimens & photographs showing c) miniature and d) sub-size fatigue specimens.

as mentioned in Table 4. As per this table, the average UTS value for
the material is 735 MPa. It is found that the UTS values obtained
using the new correlation has error of 8.54%, whereas the UTS
obtained using Mao’s correlation has error of 12.24%.

8. Future applications of miniature test techniques

Apart from life assessment of in-service equipment, many

applications of the miniature test techniques are found in litera-
ture. One of the important applications of the technique is seen
in development of functionally graded materials (FGM). FGMs are
Fig. 16. a) Miniature fatigue testing machine and b) special grips for hour-glass non-homogeneous composites having discrete or continuous vari-
shaped miniature test specimen. ation of material composition involving two or more material sys-
tems over a definable geometrical length. This variation in
composition along the gradient direction can result in gradually
varying physical, mechanical or thermal behaviour of such mate-
rial systems. The principal concept behind the design of FGMs is
their ability to utilize multiple functionalities in an integrated
material system which can provide a balanced performance in sev-
eral applications (Koohbor et al., 2015). The progressive spatial
variation of material properties in FGMs is their key difference
compared with common homogeneous materials or traditional
laminated composites. Research work on FGM started in Japan in
1984 for development of materials for high temperature applica-
tions (Miyamoto et al., 1996). In order to create FGMs, the architec-
ture of design, processing, and evaluation needs to be developed.
The concept of integrating incompatible functions such as the
refractories of ceramics and the toughness of metals with relax-
ation of thermal stress, led to research project for the development
of FGM architecture in 1987 (Miyamoto et al., 1996), with the fol-
lowing research areas:

i) Establishment of mathematical definitions and theories for

Fig. 17. Comparison of conventional and miniature fatigue test results. graded structures and properties
ii) Development of a computer aided design and modeling
close error band. With the precise control of surface finish of test
system
specimen, dimensional deviations, alignment of test fixtures, bet-
iii) Development of cost effective processes
ter strain measurement, and the error band can be further mini-
iv) Evaluation of graded properties
mized. It can be emphasized that the method has the potential
v) Establishment of a data base for FGM architecture.
for successful implementation for mechanical properties evalua-
tion of any other pressure vessel which needs an urgent attention
FGM are classified according to different application criteria
of its life management issues.
(Udupa et al., 2014). There are many ongoing studies towards
establishment of mathematical definitions and theories for FGM
7.3. SPT experiments on specimens from boat sample and validation and other activities as discussed above. Tounsi et al. (2013, 2016)
discussed a refined trigonometric shear deformation theory
Small punch tests were also conducted on specimens made out (RTSDT) taking into account transverse shear deformation effects
from dummy boat sample. The load-displacement plots for six for the thermoelastic bending analysis of functionally graded sand-
specimens are shown in Fig. 21. The UTS values were obtained wich plates. It was concluded that the RTSDT was accurate and
using newly developed correlation as per Eq. (3), mentioned in Sec- simple in solving the thermoelastic bending behaviour of function-
tion 5.3. The UTS values were also obtained using Mao’s correla- ally graded plates. Bourada et al. (2015) discussed development of
tion, as per Eq. (2) in Section 5. All these data are summarised in a simple and refined trigonometric higher-order beam theory for
Table 5. The UTS values, obtained from both the correlations are bending and vibration of functionally graded beams. The theory
compared with the average of tensile data from sub-size specimen, considers the thickness stretching effect (ez – 0) in addition to
 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358 355

Fig. 18. A full scale mock up trials were conducted at TAPS (a) The mock-up test set-up, having simulated upper & lower grids structures and simulated core shroud, being
lowered in a water pool of 12metre depth, (b) Integrated assembly of sampling module and handling manipulator, (c) boat sample from simulated core shroud and (d)
scooped region created in the simulated core shroud.

Fig. 19. Preparation of miniature test specimens by EDM from the mock boat sample.

modeling the displacement field with only three unknowns as in displacement into bending, shear and thickness stretching parts,
Timoshenko beam theory. Results showed that this theory was the number of unknowns and governing equations reduced, signif-
able to include the thickness stretching effect and provide accurate icantly facilitating engineering analysis. Indeed, the number of
results in comparison to other existing higher order beam theories. unknown functions involved in the theory was only five, as
Other researchers also presented an efficient and simple higher opposed to six or even greater numbers in the case of other shear
order shear and normal deformation theory for FGM plates and normal deformation theories. This theory accounted for both
(Belabed et al., 2014; Mahi et al., 2015). By dividing the transverse shear deformation and thickness stretching effects by a hyperbolic
356 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358

Fig. 20. (a) the engineering stress – strain curve for sub-size and miniature specimens from mock boat sample (b) scatter in YS and UTS, uniform and total elongation data of
miniature specimens in comparison to sub-size specimens.

Table 3
Chemical composition of material used for experiment.

Material C Cr Ni Mo S P Co Si Mn Cu N
SS304 0.061 18.02 8.17 0.26 0.012 0.026 0.13 0.40 1.72 0.35 0.041

Table 4
Tensile test results of sub-size and miniature test specimens.

Specimen No. Sub-size specimens Miniature specimens

1 2 3 1 2 3 4 5 6
YS, MPa 438.3 449.1 454.6 423.3 438.5 435.0 424.6 435.0 471.0
UTS, MPa 741.4 736.3 727.2 750.9 728.1 727.3 726.6 745.1 724.9
Uniform elongation, % 54.5 62.7 46.6 52.6 49.5 46.5 52.0 59.6 46.2
Total elongation, % 75.0 68.1 64.5 69.0 58.6 59.2 66.9 74.3 59.3

In case of FGM preparation, the main objective is focused on the

appropriate means to achieve the composition of FGM. It can be
divided into powder densification method, coating method,
electro-deposition method, vapour deposition method with physi-
cal deposition method and chemical deposition method (Kieback
et al., 2003; Udupa et al., 2014). As part of material development,
testing methods were also developed. Saito et al. has discussed
about the use of SPT to evaluate the fracture energy of a thin
FGM disk (Miyamoto et al., 1996). Mechanical Testing of various
types of FGMs has been done by use of miniature or small size ten-
sile tests (Saito et al., 1991; Shen et al., 2006; Kapil et al., 2014).

9. Conclusions

Miniature test techniques show an excellent potential towards

life estimation of in-service equipment and development of new
material. It is understood that there are various other types of
industrial needs for the development of miniature test techniques.
This paper is focused on the use of miniature tensile test, small
Fig. 21. Load-displacement plots obtained using SPT specimens from mock boat
sample from SS304 plate. punch test and miniature fatigues test techniques to meet specific
data requirements for life assessment of operating equipment.
From the literature, it is also clear that many designs of miniature
variation of all displacements across the thickness, and satisfied tensile specimens have user driven requirements and there is no
the stress-free boundary conditions on the upper and lower sur- ‘‘perfect” or ‘‘universally agreed‘‘ design finalized yet. This paper
faces of the plate without requiring any shear correction factor. It is an attempt towards standardisation of miniature tensile test
was conveyed that the proposed theory was accurate and simple techniques. To make it acceptable worldwide more international
in predicting the bending and free vibration responses of function- efforts are required for standardisation of tensile test specimen
ally graded plates. sizes and test methods. For small punch test techniques, it is found
 K. Kumar et al. / Nuclear Engineering and Design 323 (2017) 345–358 357

Table 5
Small punch test results on specimens from boat sample.

Specimen No. Thickness (mm) P0.48 Pmax UTS (as per Eq. (3) UTS (as per Eq. (2)
kN kN MPa MPa
1 0.2528 0.4113 0.542 836.6 782.6
2 0.25 0.3993 0.5634 830.5 851.7
3 0.2524 0.3955 0.5567 807.1 816.0
4 0.2526 0.3808 0.5444 775.8 789.1
5 0.2512 0.3749 0.5707 772.4 855.7
6 0.2506 0.3691 0.5676 764.1 854.9
Average value 797.8 825
Error in the UTS values 8.54% 12.24%

that there is no consensus on UTS correlations, which are based on thankfully acknowledge these contributions. Authors are also
Pmax value in load-displacement plot. The present work aimed grateful for encouragement and support received from Dr. P.K.
towards development of a new UTS correlation, based on the neck- Vijayan, ex-Director, RD&DG and Shri A. Rama Rao, Associate
ing zone of the SPT disk. For experiments, two pressure vessel Director, RD&DG and Head, RED. Authors gratefully acknowledge
materials, 20MnMoNi55 and CrMoV steel; and one piping materi- the technical support received from Mr. T. V. Shyam, RED, BARC;
als SS304LN; were used and following are the conclusions: Mr. S. P. Prabhakar, DRHR, BARC; Mr. A. P. Kulkarni, TAPS; Mr. J.
Akhtar, TAPS; senior officials from TAPS and BARC; and other team

Boat sampling technique was developed for scooping of boat members from TAPS and BARC for their efforts & contributions
sample from any in-service component in a non-destructive towards full-scale qualificaton of boat sampling technique at TAPS
manner. Boat samples can be used for fabrication of miniature site.
specimens for various tests, such as tensile test, small punch
test, fatigue test and Charpy impact test.
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