Nuclear Engineering and Design 320 (2017) 298–308

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Nuclear Engineering and Design

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

Sub-size tensile specimen design for in-reactor irradiation and

post-irradiation testing
Maxim N. Gussev ⇑, Richard H. Howard, Kurt A. Terrani, Kevin G. Field
Oak Ridge National Laboratory, Oak Ridge, TN 37831, USA

h i g h l i g h t s

 New specimen geometry for post-irradiation testing (PIE) was designed.

 The new geometry performance was evaluated for several commercial and model alloys.
 Scale factor role was discussed in detail.

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

Article history: The present work aims to provide a complete engineering solution, an appropriate experimental data-
Received 12 October 2016 base, and a brief physical background on designing a miniature specimen geometry suitable for irradia-
Received in revised form 30 May 2017 tion in materials test reactors such as the High Flux Isotope Reactor and post-irradiation out-of-hot cell
Accepted 3 June 2017
testing. The physical limits of specimen miniaturization and a background of the scale factor effect are
discussed, and principal limitations are defined. The advantages of modern test methods like digital
image correlation, as well as some limitations connected to small specimen size, are analyzed. A sub-
Keywords:
sized specimen geometry, ‘‘SS-Mini,” is designed; the geometry employs existing irradiation capsules
Scale factor
Sub-size specimen geometry
leading to the reduced cost of any irradiation campaign. The new geometry performance is evaluated
Post-irradiation investigation using a commercial 304 L stainless steel, an aluminum alloy including advanced 3D-printed material, a
In-situ testing high nickel 718-alloy, tungsten, and an advanced fuel cladding FeCrAl alloy. Mechanical tests are con-
Flexible design for neutron irradiation ducted to compare the engineering mechanical properties (yield and ultimate tensile stress, uniform
capsules and total elongation values) and plastic behavior of the proposed miniature specimen with common
specimen types for irradiation testing.
Ó 2017 Elsevier B.V. All rights reserved.

1. Introduction mechanical properties or at a minimum yield coherent scaling

There is a constant and growing interest in the mechanical test-
ing of small specimens and analyzing material behavior at small
scales. In general materials science, this interest is driven by intro-
ducing smaller devices and exploring the micro- and nano-
mechanics areas (Connolley et al., 2005; Jaya and Alam, 2013).
The goal is to analyze the properties and performance of micro-
parts and components in detail while understanding materials
behavior at lower length scales.
At the same time, the nuclear industry often has a different goal
(Klueh, 1985; Kohno et al., 2000; Hindley et al., 2015; Viehrig et al.,
2015): testing of miniature samples taken from nuclear installa-
tions should provide information that is applicable to bulk
⇑ Corresponding author at: PO Box 2008, Oak Ridge, TN 37831, USA.
E-mail address: gussevmn@ornl.gov (M.N. Gussev).
parameters from small scale testing. The motivation for small-
scale mechanical testing in the nuclear industry is to best take
advantage of the limited experimental space in materials test reac-
tors and minimize the radiological dose produced from activated
materials that directly scales with their volume.
Additionally, recent progress in different in-situ test methods,
where small scale testing is routinely needed, is impressive
(Dehm et al., 2006), and the next decade is likely to see a consider-
able rise in the in-situ test techniques for general materials science
and nuclear engineering. For instance, micro-pillar testing (Dehm
et al., 2006; Shin et al., 2015), high-resolution EBSD (Jiang et al.,
2013), advanced tools for 3D structure reconstruction, and other
techniques are quickly providing new, unique, and—most impor-
tantly—insightful data. Employing these methods is an attractive
idea for the investigation of radiation effects in materials, including
plastic strain at small scales (Greer and De Hosson, 2011).

http://dx.doi.org/10.1016/j.nucengdes.2017.06.008
0029-5493/Ó 2017 Elsevier B.V. All rights reserved.
 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308
Moreover, the development of innovative nuclear systems con-
stantly requires new materials, which, in turn, means increasing
needs for advanced comprehensive testing methods (Fazio et al.,
2011; Yvon et al., 2015), like in-situ corrosion testing (Klecka
et al., 2015), while simultaneously reducing the time to achieve
such data and analysis.
The deployment of the advanced in-situ techniques on neutron
irradiated materials is of special importance. Although significant
progress was made to use light ion and heavy ion irradiations to
simulate neutron irradiation while producing samples with little
or no radioactivity [e.g., see (Was et al., 2002)], the discrepancies
in the observed microstructure and mechanical properties still
exist. Hence, data for neutron irradiated materials are still essential
to fully develop a nuclear-grade alloy ripe for commercial
deployment.
Irradiation may stimulate specific processes not observed with-
out irradiation, including swelling, increased diffusion and creep,
radiation-induced segregation (RIS), and irradiation-assisted stress
corrosion cracking (IASCC), just to name a few. Advanced in-situ
tools may bring new insights into well-known processes. For
instance, a preliminary, not-on-purpose analysis of the deforma-
tion localization in neutron irradiated austenitic steels revealed
specific phase transformation at the irradiated specimen’s surface
(Gussev et al., 2014b) along with areas of localized deformation
and high dislocation density spots (Field et al. 2014a) in addition
to the expected and well-known defect-free channels. It is impor-
tant to be able to test the irradiated specimen in-situ, registering,
for example, the evolution of dislocation density and the evolution
of local misorientation (Jiang et al., 2013) with direct measure-
ments of acting stress or observations of stress corrosion crack
appearance and propagation. These data, coupled with modern
modeling tools, allow for complex analysis of material behavior,
including constitutive crystal plasticity approaches. However, to
reach these goals, one has to at least have direct access to the spec-
imen for preparing the appropriate quality surface.
Miniature sub-size specimens for post-radiation testing have a
long history and are widely used for investigating mechanical
properties and deformation-hardening behavior of irradiated and
non-irradiated metals and alloys (Klueh, 1985; Panayotou et al.,
1986; Kohyama et al., 1991; Kohno et al., 2000; Gussev et al.,
2014a), weldments (Field et al., 2014b), nanostructured materials,
and different composites. A variety of different sizes and geome-
tries are used in nuclear materials science (Klueh, 1985; Pierron
et al., 2003; Wakai et al., 2011), with new geometries and testing
methods being constantly developed (Rickerby and Fenici, 1986;
Džugan et al., 2014; Hurst and Matocha, 2015; Rund et al., 2015).
Specimen miniaturization often involved other methods, not only
tensile testing. Thus, Jung et al., (1996) offered a miniature tensile
specimen with gauge section of 5  1  0.4 mm; additionally, a
number of testing methods for miniature specimens (tensile, fac-
ture toughness, punching, impact testing) were discussed in detail
(Jung et al., 1996) focusing on the detailed correlation between
miniature and bulk behavior. The offered tensile specimen geome-
try was intensively used in a number of projects (see for instance,
(Dai and Bauer, 2001)).
Through the past few decades, there has been a tendency to
decrease the overall specimen size and volume (Klueh, 1985). Prior
to this work, two miniature tensile specimen geometries were
commonly used for irradiations in the High Flux Isotope Reactor
(HFIR): the SS-3 and the SS-J type specimens (Klueh, 1985;
Gussev et al., 2014a). These two geometries provide acceptable
mechanical properties compared to standard-scale specimens
(Gussev et al., 2014a). However, the post-irradiation activity level
is usually too high for nuclear reactor metals after discharge, and
this limits the post-irradiation analysis to testing within a hot cell
facility only, especially when moderate to high damage dose (dpa)
299
samples are of interest. Reaching the acceptable level of radioactiv-
ity may require unacceptable waiting times that exceed the life-
time of the funding program or project interested in such data.
Thus, there is a need for a specimen geometry capable of sup-
porting the modern in-situ testing methods on moderate to highly
neutron irradiated materials, while still providing repeatable bulk-
scale mechanical properties. It is important for the new geometry
to provide appropriate mechanical test results and keep a continu-
ity and comparability with the existing databases in the literature.
If suitable, these small-scale mechanical testing specimens impact
scientific productivity in the nuclear materials area in two impor-
tant ways. First, by avoiding in-cell testing, a whole host of new
characterization techniques too costly or simply inviable for in-
cell deployment—where high radiation fields detrimentally inter-
act with electronic components—suddenly become available for
utilization. Second, the costs associated with in-cell testing are
often very high (e.g., at least a factor of 2–3x higher at ORNL)
and would, in turn, limit the depth and breadth of the R&D project.
The circumstances discussed above motivated the development
of a new specimen geometry allowing for: (1) in-HFIR irradiation
within the existing ‘‘rabbit capsule” geometry and specifications,
(2) out-of-hot cell testing with short ‘‘cool-down” (reduction in
radioactivity by decay) time, and (3) the capability to perform in-
situ measurements using advanced techniques. The present work
discusses the design, geometry, and implementation of a miniature
sub-size specimen that meets these requirements.
2. The background of scale and size effects
The scale factor and size effects usually become apparent when
the specimen size approaches the characteristic length scale of the
material microstructure (Connolley et al., 2005). For common
steels and alloys, this tends to be the grain size. Another size effect,
often observed in brittle materials (Bažant, 1999), occurs when the
size of the specimen becomes small compared to the spatial distri-
bution and density of critical defects. Additionally, size effects may
appear due to physical, chemical, or corrosion processes that are
negligible for relatively large objects but become critical when
the size of the test specimen decreases. Most of these processes,
like oxidation, usually do not appear in common mechanical tests;
however, some important physical phenomena sensitive to the
scale factor are briefly analyzed below.
Considering the scale factor role, researchers most often focus
on the uniform strain area, where the uniaxial stress state exists,
and on the necking behavior, where the complex stress state and
the stress triaxiality play an important role.
In the first case, under uniaxial stress, the specimen is often pre-
sented as a ‘‘multilayer” object with a layer of near-surface grains.
The ratio of the ‘‘near-surface grains” to the ‘‘bulk grains” impacts
the specimen deformation behavior and strain hardening rate
(Wang et al., 2013; Shin et al., 2015). The near-surface grains (or
the near-surface layer if a single crystal specimen is considered)
have smaller dislocation density and internal back stress level
compared to the bulk grains (Keller et al., 2010; Shin et al., 2015)
because of the dislocation escape through the free surface. Also,
the surface plays a key role in crack initiation during fatigue
(Signor et al., 2016) and stress corrosion cracking (SCC). To handle
very thin specimens (10–20 lm sheets), some special test method
(s) may be needed. For instance, Hoffman and Hong (Hoffmann and
Hong, 2006) offered an aero-bulging test method for testing thin
foils of different materials.
It is worth noting that the near-surface layer is not necessarily
‘‘weak;” that is to say, it does not necessarily have a decreased
strength. Often, specimens are produced by electric discharge
machining (EDM) followed by mechanical grinding or polishing
300 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308

to fit the dimensional requirements. EDM leads to the formation of However, the total elongation value demonstrated a more com-
a recast surface layer, often referred to as the ‘‘white layer” (Bleys plex behavior, as shown in Fig. 1, where saturation in the total
et al., 2006), which may be hard and brittle depending on the elongation values was reached at 2 mm thickness (T/W ratio of
material system. The subsequent mechanical grinding removes 0.67 in Fig. 1). Necking angle, the angle between the loading axis
the EDM layer but introduces cold-work related artifacts or even and the fracture plane, was also affected by thickness. The param-
results in the formation of fine grains (Kaneda et al., 2011). Elec- eter controlling these processes was found to be the T/W ratio that
tropolishing or controlled chemical etching may eliminate the influences the stress state in the neck (Byun et al., 1998). A similar
modified layer, but these techniques are both costly and time- result—post-necking elongation increased with thickness—was
consuming or produce specimens with thickness and edge shape obtained by (Yuan et al., 2012). In the context of the present work,
variations that can significantly skew results. this means that the T/W value of the conventional small-scale
Strictly speaking, it is impossible to avoid the free surface influ- specimens, like SS-3 [T/W  0.5, (Klueh, 1985)], and new miniature
ence. Instead, the question is how thick should the specimen be to geometries discussed later should be close, if not identical.
provide acceptable data? Usually, in mechanical test practice, the If the material behavior under the complex stress state is of
smallest specimen dimension should exceed 5–6 grains to mini- interest, a proper specimen geometry may be employed to analyze
mize the scale factor influence (Kohno et al., 2000). This rule may the stress triaxiality role on plastic behavior and fracture, as dis-
not be fully valid in some specific cases (e.g., in nano-structured cussed recently in (Algarni et al., 2015). If necessary, the stress
materials with high defect density). If defect spacing is much smal- state may be directly addressed via neck geometry measurements
ler than grain size, the bulk mechanical properties may be mea- [e.g., by multi-camera 3D DIC, (Kamaya and Kawakubo, 2014)] or
sured by using smaller specimens that contain as little as 2–4 by a finite element modeling (FEA) approach (Kim and Byun, 2010).
grains across the smallest dimension (Howard et al., 2016). A number of additional phenomena exist beyond the few dis-
Sometimes, there are additional limitations if the material being cussed above (Jaya and Alam, 2013); however, a detailed analysis
tested exhibits phenomena sensitive to the active volume or sur- is out of the present scope of work. In summary, it appears that
face conditions. For instance, plastic deformation generates energy geometrical (specimen thickness and presence of natural internal
release in the form of heat and leads to a temperature increase boundaries, like grain boundaries), technological (surface and
(Ayres, 1985), but this process is usually ignored. However, the near-surface layer conditions), and physical (potential scale-
temperature at the specimen gauge may rise by 10 °C or more even sensitive phenomena) limitations should be analyzed for the par-
at a moderate strain rate (10 3 s 1) (Ayres, 1985). In the case of ticular material before designing a specimen geometry for nuclear
fracture, a large amount of energy is being released in a small vol- materials development applications.
ume resulting in a temperature jump that can reach 100 °C. For
example, a temperature rise of 300 °C was observed in the shear
3. Materials and test methods
bands in metallic glass specimens (Yang et al., 2006). As an ulti-
mate case, melting of a metallic glass specimen during fracture
As discussed above, the scale-factor limiting criteria can vary
was observed in-situ (Yang et al., 2004). In the tensile test, the heat
from material to material and can be significant or insignificant
generation is proportional to the specimen volume (d3) in the
depending on the data of interest from a mechanical test. Thus, it
uniform strain area, whereas the heat losses rely on the specimen
is important to cover a wide range of strength and ductility values
surface or cross-sectional area (d2). Thus, the heating intensity is
and different types of strain hardening behavior by using a vast
proportional to the specimen size (d), being less pronounced in
array of different material systems. The present work included
small specimens compared to larger ones. If the material of interest
both well-known and advanced modern materials, as shown in
experiences strain-induced phase instability (Chen et al., 2013;
Table 1. Aluminum 6061 alloy is employed to cover the low
Shirdel et al., 2015), such as the transformation induced plasticity
strength/low ductility range; also, after annealing, this material
(TRIP) effect, deformation twinning, or dynamic deformation aging,
demonstrates specific deformation behavior with propagating
the effects of strain-induced heating should not be ignored.
deformation bands. Austenitic AISI 304L stainless steel is selected
Additionally, some materials, like carbon steels and Al-Mg
as a representative commercial, widely used nuclear material.
alloys, often exhibit Luders band propagation. In this case, a defor-
mation plateau is observed in the tensile curves (Mazière and
Forest, 2015). It appears that Luders deformation may also be
scale-sensitive. For instance, the plateau disappeared in a ferritic
A533B steel when a thin specimen geometry such as an SS-2 type
tensile specimen (T = 0.25 mm) is used (Gussev et al., 2014a). Also,
the material of interest may be sensitive to texturing; orientation
effects may appear in the specimens produced from rolled or
extruded material (Zhang et al., 2014).
The scale factor’s role during deformation localization and neck-
ing may be more complex compared to the uniform strain area. In
addition to the free surface effects and the different behavior of the
near-surface grains, the neck also experiences a complex stress
state. The neck shape and principal strain ratio may depend on
specimen thickness and thickness-to-width ratio (T/W). Byun
et al. (Byun et al., 1998) investigated the effect of specimen thick-
ness on the mechanical properties of miniature specimens with a
particular focus on deformation localization and necking. Regard-
ing the yield and ultimate stress and uniform ductility for ferritic
Fig. 1. The effect of the T/W ratio on the uniform (UE) and total (TE) elongation
steels, Byun et al. concluded (Byun et al., 1998) that these values
values. The plot includes the data from (Byun et al., 1998) on an RPV steel and the
will be close to the bulk material data of the specimen if thickness present work’s results on the advanced FeCrAl alloy (see below). The positions of
exceeds  0.3–0.4 mm (or  7–10  grain size). the designed small specimens on the T/W scale are shown by vertical, dashed lines.
 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308
Table 1
Element composition of the investigated materials.
Material Composition, wt% (or ppm wt. for tungsten).
6061 Al- Al: bal., Mg: 0.86, Si: 0.66, Fe: 0.35, Cu: 0.23, Cr: 0.13, Ti: 0.08,
alloy Mn: 0.08, Zn: 0.08, Ni: 0.02
304 L Fe: bal., C: 0.02, Mn: 1.3, Si: 0.45, Cr: 18.3, Ni: 8.02, Mo: 0.074
FeCrAl- Fe: 79.4, Cr: 13.1, Al: 5.3, Y: 0.05, Mo: 2.0, Si: 0.13, Nb: <0.01
alloy
718-alloy Ni: bal., Cr: 18.5, Fe: 18.7, Mn: 0.23, Mo: 3.03, Al: 0.48, Co: 0.29.
Tungsten (ppm wt.) W: bal., Al: 0.23, Si: 0.55, P: 0.68, V: 0.82, Cr: 1.7, Fe: 3,
Ni: 0.75, As: 0.39, Sn: 0.69, Ta < 5, other: <0.1 ppm wt.
Commercial 718-alloy is added as a high strength material.
Advanced FeCrAl alloy is selected to represent a system currently
undergoing alloy development efforts for accident tolerant clad-
ding and hence a material with a limited material database (Field
et al., 2014b; Yamamoto et al., 2015). Tungsten was selected as a
material to exhibit high strength, but low, if not zero, ductility.
To provide a baseline for comparison, Fig. 2 shows the geometry
and dimensions of the common specimen (the SS-J type with
0.75 mm thickness) used in the present work. The SS-J type sample
shown in Fig. 1 is typically used as the sheet type dog bone speci-
men. This geometry provides effective heat transfer across the
stacked faces during irradiation. Shoulder loading without pin-
holes provides sufficient material in the head of the tensile speci-
men for microhardness testing and electron microscopy sample
preparation.
Both SS-J and SS-Mini specimens discussed below are produced
from the bulk material using EDM. The specimens are also ground
down mechanically by a vendor to fit the dimensions. All speci-
mens are produced by the same vendor. Before the tensile test,
the thickness and width of each specimen are measured with an
accuracy of 10 lm or better; gauge length variations (±0.02 mm)
are too small to influence the plasticity results. For each geometry
and material, 4–5 specimens are tested per point. The strain rate is
close to 10 3 s 1 (with no more than a 5% difference) for all spec-
imen geometries.
Tensile tests are performed on an MTS Insight 2–52 one-column
tensile screw machine. All tensile specimens are shoulder loaded
and tested at room temperature. Before the tensile tests, a subset
of specimens are painted with a random speckle pattern. High-
resolution Allied Vision GT6600 and GX3300 cameras are used in
the experiments; the lenses used provide a resolution of 10–
15 lm per pixel for the GT6600 and 2–2.5 lm per pixel for the
GX3300 for both the SS-J type and miniature specimens. Strain
fields and true stress–true strain curves are calculated using VIC-
2D commercial software and a custom program utilizing common
digital image correlation (DIC) algorithms. DIC is a modern, con-
stantly developing experimental tool (Sutton et al., 2009) that
allows for non-contact strain measurements; the details, peculiar-
ities, and limitations of the DIC-based strain measurements are
Fig. 2. Geometry and dimensions of the common miniature specimen (SS-J type).
Dimensions are in mm; ‘‘T” designates thickness. Dimensional tolerances were as
follows: gauge length ±0.02 mm, gauge width ±0.02 mm, specimen thickness
±0.01 mm, and other dimensions ±0.04 mm. Grips used to test the specimen are
shown in (Gussev et al., 2014a).
301
widely discussed in the literature, see (Sutton et al., 2009) and
those cited within.
4. Miniature specimen design and properties
4.1. Design and geometry considerations
The following aspects based on the prior discussion were con-
sidered during the sub-size specimen design phase:
1. The miniature specimen geometry should reproduce a
polycrystalline-like behavior. To achieve this, the specimen
should contain at least 5–6 (or more) grains per the smallest
dimension. Generally, if the thinnest area has less than 5 grains,
the specimen will demonstrate reduced strength. The most
common grain size for ferrous and non-ferrous alloys is near
40–50 lm, resulting in 300–400 lm being the limiting mini-
mal thickness for the specimen.
2. To accurately reproduce necking and strain localization behav-
ior (or, at an absolute minimum, close to the SS-J types), the
geometry should meet specific thickness/width and length/
cross-section requirements.
3. The specimen should have limited activity after irradiation.
Currently, at the ORNL’s LAMDA (Low-Activation Materials
Development and Analysis) (Parish et al., 2015) facility, the
limit is 100 mR/h at 30 cm per specimen to allow for the out-
of-hot cell research activity. This limit is generally within typi-
cal limits for many research facilities within the United States.
Thus, specimen volume should be significantly reduced, com-
pared to an SS-J, especially if high dose (>10 dpa) specimens
are of interest.
4. Sample geometry should be simple and avoid or minimize
rounded shapes to reduce the sample production cost. In the
future, it would be advantageous to allow for machining the
same samples from irradiated materials in a hot cell facility.
5. Additionally, the specimens should fit into existing irradiation
capsule designs, thereby eliminating the need for conducting
complex heat transfer calculations. The number of specimens
per capsule should be larger compared to the SS-J types, allow-
ing for larger statistics or distributing the specimens among the
collaborating groups. Additionally, each capsule should be able
to carry both new and old specimen types and optimize the
number of specimens of each type as necessary for a particular
project.
4.2. The geometries included in the preliminary analysis
After analyzing the criteria and limitations listed above, several
geometries were considered for the preliminary analysis, as shown
in Fig. 3. Two gauge lengths were chosen: 2.55 mm and 3.55 mm
(Types 1 and 2, respectively), and two head types were employed.
Small heads (S) were expected and allowed to deform during the
test; however, these heads were strong enough to carry the load.
For this geometry, the head shape stability was sacrificed to reduce
mass and radioactivity level after neutron irradiation. As will be
discussed below, DIC allows for retrieving correct true stress–true
strain curves for the gauge portion of the specimen, regardless of
the selected head geometry. Extended heads (E) were designed
to carry the load with minimal plastic strain in the head. Further
head size increase would eliminate the plastic strain in the heads
completely, but the price paid would be the extra sample mass
and extra radioactivity after neutron irradiation. For each small
specimen geometry (Types 1 and 2, S- and E-heads), two different
specimen thicknesses (0.4 mm and 0.6 mm) were considered. All
302 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308

Fig. 3. General view of the preliminary geometries (left) and the detailed geometry of the Type-2E (right).

Table 2
A number of specimens per irradiation capsule and mechanical properties of the investigated FeCrAl alloy.

Mechanical properties
Specimen geometry Specimens per standard Yield stress, Ultimate Uniform Total Grading
HFIR rabbit capsule MPa stress, MPa elongation,% elongation,% points
SS-J type 12  2* 710 ± 25** 767 ± 28 7.9 ± 2.5 14.8 ± 3.7
SS-Mini*** Short 1S-0.4 12  9 607 760 10.8 23.1 
(2.55 mm gauge)
1E-0.4 12  9 725 782 6.6 18.2 
1S-0.6 12  6 663 796 10 29 –
1E-0.6 12  6 761 826 9 28 
Long 2S-0.4 12  6 708 821 9 18 
(3.55 mm gauge)
2E-0.4 12  6 705 ± 50 761 ± 52 7±1 15 ± 2 
2S-0.6 12  4 702 822 11 25 
2E-0.6 12  4 753 821 9 22 
*
For specimen with 0.75-mm thickness, 123 if an SS-J (T = 0.5 mm) type specimen is used.
**
One standard deviation value is given for two geometries as an inaccuracy estimation.
***
Nomenclature example: the ‘‘1S-0.4” abbreviator means Type 1 (short gauge) with small (S) head and thickness of 0.4 mm.

miniature specimens, regardless of thickness and gauge length,
could be tested using the same grips.
Table 2 shows the number of different specimens allowable per
capsule using standard packing configurations for irradiation cap-
sules in the central flux position of the HFIR. As discussed later
in Section 5, each irradiation capsule (commonly referred to as
‘‘rabbits”) contains three small cylindrical holders with four stack
positions each. Thus, there may be 12 stacks total, with two SS-J
type 0.75 mm thickness specimens in each—or 24 SS-J type [Thick-
ness (T)=0.75 mm] specimens in total. Using miniature geometries,
each stack may contain a larger number of small specimens, from 9
(SS-Mini 1E-0.4) to 4 (SS-Mini 2E-0.6). Specimens of different types
may be combined without disturbing the capsule’s internal tem-
perature field and dose distribution; this aspect is discussed in
greater detail in Section 5.
Comparable specimens are constantly being developed and are
used by a number of authors. For instance, small specimen
geometry with a gauge of 2 mm  1 mm  0.2 mm was designed,
irradiated, and used to investigate the radiation tolerance of
ultra-fine grained steel (Alsabbagh et al., 2013). Additionally,
Džugan et al. (2014) offered a tensile specimen with a
3 mm  1.5 mm  0.5 mm gauge; the specimen may be produced
from an 8 mm diameter disk. It was shown that non-contact optic
measurements (e.g., DIC) may provide additional important infor-
mation and true stress–true strain curves; the offered geometry
(Džugan et al., 2014) provides good tensile test results in compar-
ison with standard geometries for some common materials
(aluminum alloy, 99.99% copper, 14% chromium–steel, etc.).
However, compared to the geometries proposed here, their
specimen requires fixed mechanical grips and has higher mass
and volume. In the present work, pneumatic grips were rejected
since they require much larger heads to fix the specimen in a
timely and reliable manner—a key factor when working with
highly radioactive samples. The grips geometry employed within
this work (Gussev et al., 2014a) provides some degrees of freedom
to allow for alignment of the specimen to the loading axis.
4.3. Geometry comparison and selection
The mechanical test results obtained for the SS-Mini geome-
tries are compared with the data obtained for the SS-J type geom-
etry. Table 2 demonstrates a typical dataset for the FeCrAl alloy.
Scattering (one standard deviation value) is shown for several
geometries.
Here, close matching (i.e., the known, repeatable deviation) in
the mechanical properties was deemed beneficial as it allows for
comparing the new data with an existing database of mechanical
properties. Thus, using the data in Table 2, the best geometry
was chosen among the analyzed set using the following logic:
1. The specimens with small heads (S) demonstrated, as a rule,
smaller yield stress and larger ductility (especially total elonga-
tion) compared to the SS-J type. The extended heads (E) pro-
vided much better matching of the yield stress with less than
10% difference compared to the SS-J type, Table 2. To grade
the different geometries, all E-headed specimens received one
point in the selected ranking system for the selection of the best
geometry.
 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308 303

Table 3
Mechanical properties of the tested materials (SS-J vs. SS-Mini 2E-0.4).

Material Geometry Yield stress, MPa Ultimate stress, MPa Uniform elongation,% Total elongation,%
SS-Mini feasible materials
6061-0 SS-J 72 122 18.1 27.3
SS-2E 73 119 16.9 26.5
6061-T6 SS-J 294 315 7.2 15.4
SS-2E 279 301 5.8 14.3
Annealed 304 L SS-J 274 ± 22* 789 ± 14 67 ± 3 76 ± 3
SS-2E 272 ± 23 781 ± 34 69 ± 3 80 ± 4
FeCrAl SS-J 710 767 7.9 14.8
SS-2E 705 761 7.0 15.0
718-alloy SS-J 1237 ± 13 1461 ± 25 16.3 ± 0.4 22.5 ± 0.9
SS-2E 1170 ± 33 1386 ± 36 15.4 ± 0.8 21.0 ± 1.5
Non-SS-mini feasible
Tungsten, W SS-J 820** – – –
SS-2E 603** – – –
*
One standard deviation is shown for several materials to illustrate the typical result scattering.
**
Fracture stress is given for tungsten.

2. The specimens with a short gauge (Type 1, 2.55 mm) demon-

strated slightly higher uniform elongation and higher total
elongation compared to the specimens with a long gauge (Type
2, 3.55 mm); this result agrees with (Pierron et al., 2003). Duc-
tility values for the Type 2, in general, were closer to the SS-J
type compared to the Type 1. This provided an additional selec-
tion point for the Type 2 specimen group.
3. The thick specimens (0.6 mm) always had larger total elonga-
tion compared to the thin ones (0.4 mm). Thin 0.4 mm speci-
mens were closer to the SS-J type, thus providing the third
selection point as shown in Table 3. The resulting grading indi-
cated the SS-Mini 2E-0.4 geometry (or shortened, the SS-2E,
Fig. 3) as the best SS-mini prototype for further analysis. The
same process that was applied to the FeCrAl alloys was then
applied to the 304 steel, with the same conclusion: SS-2E is
the best geometry to mimic the SS-J type while also meeting Fig. 4. Engineering tensile curves in ‘‘plastic strain–engineering stress” coordinates
for alloy 6061-0 for specimens of different geometry. To demonstrate the PLC-effect
the criterion provided in Section 4.1.
peculiarities, the tensile curves were approximated and subtracted by the
polynomic curve.

4.4. Mechanical properties of the tested materials

Table 3 demonstrates the average mechanical test results for
the SS-J type geometry compared to the SS-2E for the tested mate-
rials. As shown in the table, for many materials the miniature
geometry provided close matching of the data between the two
types of specimen geometries. The typical difference in the yield
and ultimate stress values did not exceed 5–8%, which is within
the typical margin of error of a single measurement using either
geometry. Ductility values had slightly higher scattering, but, nev-
ertheless, the matching was deemed reasonable for most alloy
development efforts and comparative studies.
Aluminum 6061 alloy is of special interest in research reactor
core structures to form the skeleton, cladding, or the fuel or absor-
ber matrix (Kim et al., 2008). Due to its good fabricability, excellent
corrosion performance (with appropriate pH control), high
strength in the low-temperature water coolant of these reactors
(60–80 °C), and low neutron absorption rate, this material is rou-
tinely used in the fuel and control components of these cores. Dur-
ing straining at room temperature with a conventional strain rate
(10 3 s 1), this alloy after annealing (6061-0) demonstrated a
specific phenomenon known as the Portevin-Le-Chatelier effect
(PLC). The PLC effect causes deformation localization and consecu-
tive formation of the localized shear bands. Numerous force drops
appeared in the tensile curves, as seen in Fig. 4.
The evolution of the shear bands and amplitude of the force
drops depend on the collective behavior of grains in the polycrys-
talline aggregate. Detailed analysis of this phenomena reveals a
complex, multi-scale background (Mazière and Forest, 2015). The
specimen geometry change and the strong decrease in the number
of grains involved in the process is expected to affect, at a mini-
mum, the kinetics of the serration flow and amplitude of the force
drops. However, the data shows not only good matching in the
mechanical properties (Table 3) but also excellent agreement in
the tensile behavior for SS-J and SS-Mini geometries (Fig. 4). The
magnitude and type of the serrations were nearly identical.
Most alloys analyzed above demonstrate some ductility and
fracture after demonstrating significant area reduction. In contrast,
tungsten usually has very limited, if any, ductility and shows a brit-
tle fracture at room temperature. Small inaccuracies in specimen
and grips geometry can lead to minor deviations in the loading
axis, which may become particularly problematic with specimen
miniaturization. As outlined in Table 3, the SS-Mini 2E-0.4 geome-
try provided smaller fracture stress values (up to 25%) for tung-
sten, compared to the SS-J type geometry. As believed, this issue
may appear for brittle materials in general, not for tungsten only.
If so, special attention should be paid on the small deviations in
the specimen geometry, surface quality, and other factors influenc-
ing the test results.
4.5. Geometry limitations due to non-traditional scale factors
As discussed earlier, the grain size is a natural scale and allows
for estimating specimen size in ‘‘dimension-less” or ‘‘natural”
304 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308
units. Such a ‘‘natural scale” may be found in some other cases, for
instance, in the materials produced by ultrasonic additive manu-
facturing (UAM) (Dehoff and Babu, 2010). The UAM technique
exploits ultrasonic vibrations to effect a solid-state bonding
between metal tapes of 100–150 mm thickness, yielding a
multi-layer structure with numerous welded interfaces. The
UAM-produced materials have strong property inhomogeneity
depending on the loading direction (relative to the welding inter-
faces) (Schick et al., 2010). The direction perpendicular to the
welding interfaces (often named ‘‘Z-direction”) is usually the
weakest one; Z-direction loading often leads to a quasi-brittle
crack propagation and fracture with zero uniform and total ductil-
ity values. The UAM-produced tensile bars studied here had 7
and 3 metal tape layers across the thickness of the SS-J and SS-
2E specimens, respectively.
To estimate the role of the welding interface on a scale factor,
mechanical tests are conducted with tensile specimens produced
from UAM blocks (Fabrisonic, Columbus, OH) made of aluminum
6061-H18 alloy. The details of the UAM fabrication, bulk part pro-
duction, structure, and role of direction (X, Y, Z) on mechanical
behavior are given elsewhere (Sridharan et al., 2016) and will not
be discussed here. Table 4 shows the mechanical properties of
the SS-J type geometry specimens compared to the SS-Mini 2E-0.4.
As shown in Table 3, the same bulk commercial aluminum alloy
is almost insensitive to the scale factor; the results for the SS-J type
and SS-Mini 2E-0.4 geometries are within reason. In contrast, the
UAM-produced specimens demonstrate strong sensitivity to the
specimen geometry. In the case of SS-Mini 2E-0.4, the yield stress
is much smaller, and total elongation is much higher for X and Y
directions compared to the SS-J type. SS-Mini 2E-0.4 Z-direction
specimens have higher yield (fracture) stress than the SS-J type.
Most likely, this is caused by the probability of finding a welding
flaw of a critical size capable of crack initiation and fracture.
This limited study on the UAM objects highlights the need for
close inspection on the different scale factors contributing to the
mechanical response of a specimen of interest. In the case of the
Table 4
The scale factor role on UAM-produced aluminum 6061 alloy.
Direction Specimen geometry
X – along the tape length SS-J type
SS-Mini (SS-2E)
Y – direction of straining during welding SS-J type
SS-Mini (SS-2E)
Z – perpendicular to the welding interfaces SS-J type
SS-Mini (SS-2E)
Fig. 5. Strain level (von Mises strain, Hencky’s strain tensor) in the head of the deformed specimens at a strain level of 0.4. Note the reduction in the local strain level in the
specimen head (from point A to point C for SS-J specimen geometry).
UAM material, the grain size is not the dominating factor, and
the observed properties of the 3D-printed material might be more
sensitive to the specimen geometry and thickness, compared to a
conventional bulk alloy.
4.6. Some methodological aspects of DIC tensile testing
If a set of images has been taken during the test and a reference
(non-deformed) image is available, strain field evolution may be
analyzed using DIC algorithms (Sutton et al., 2009). The most com-
mon goals of DIC use are the strain field measurement (Fonseca
et al., 2005; Sutton et al., 2009; Ambriz et al., 2013), analysis of
property gradients in weldments (Field et al., 2014b), investigation
of constitutive behavior and true stress–true strain curves (Džugan
et al., 2014; Kamaya and Kawakubo, 2014), dealing with phenom-
ena such as Luders bands (Zhu et al., 2015), and investigating
deformation localization and necking (Suzuki et al., 2010). Among
these, true curves and constitutive behavior parameters are espe-
cially important for designing nuclear reactor components
(Christopher et al., 2015).
In the mechanical test practice, plastic deformation in the spec-
imen heads is often ignored; however, it may be of concern if there
is a need to perform focused ion beam (FIB) lift-out or produce
transmission electron microscopy (TEM) disks using the head
material, which is a common practice for producing electron
microscopy samples from irradiated material. Fig. 5 shows plastic
strain distribution obtained by DIC analysis in 304L steel speci-
mens deformed at the overall strain level of 0.4. As shown in
the data, the strain level reaches about half of the overall strain
level (0.2) observed at the gauge-head transition location (point
A), and this value (eA) is close for all specimen geometries. At the
distance of 0.8 mm from this location (point B), the strain level
(eB) is still significant in the S-type specimen with reduced head
size, whereas it drops to 0.03 in the E-type and SS-J specimen.
Note that even the SS-J specimen, with relatively massive heads
(in relation to the miniature specimens under investigation), is
Yield stress, MPa Ultimate stress, MPa Uniform elongation,% Total elongation,%
202.9 206.9 0.5 6.8
176.9 216.7 0.7 8.5
211.3 212.0 0.3 6.0
109.1 226.2 1.8 9.6
61.7 – – –
80.0 – – –
 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308
Fig. 6. Typical true stress–true strain curves for specimens of annealed austenitic
steel. Some increase in strain hardening rate is caused by martensitic
transformation.
not large enough to completely eliminate plastic deformation in
the heads. As distance from the gauge increases, local strain
decreases quickly (see point C for SS-J specimen in Fig. 5). For
the widest head portion, E- and SS-J geometries can provide virtu-
ally non-deformed material. Note also that plastic strain in the
heads should reduce quickly with strength level increase.
Fig. 6 shows the true stress–true strain curves calculated using
DIC for the annealed 304L steel. The measurements are conducted
using a ‘‘virtual digital extensometer” for the middle portion of the
specimen gauge. Here, annealed austenitic 304L steel is selected
due to its relatively low yield stress and pronounced strain harden-
ing. The difference between yield stress and ultimate stress reaches
3  as shown in Table 3, leading to increased stress in the heads
during straining. Nevertheless, as shown in the results from Fig. 6,
the curves are practically identical for all specimen geometries.
Small specimen geometries, even the ones with the smallest heads,
provide close matching. This result was expected (Džugan et al.,
2014); DIC eliminates the inaccuracy caused by the plastic strain
in the heads.
In the context of the present work, annealed 304L steel with a
strong strain hardening rate represents the worst case scenario.
Most likely, as mentioned above, plastic deformation in the heads
and its impact on the overall specimen behavior will be less pro-
nounced in irradiated specimens and materials with smaller hard-
ening rates such as the FeCrAl or 718-alloys.
One methodological aspect worth noting here is that in the case
of miniature specimens, creating DIC patterns may become an
issue. Traditional spray paint cans usually do not work well and
only provide a moderate speckle pattern density (Berfield et al.,
2007). Much denser patterns with smaller speckles can be created
with commercially available airbrushes, as noted by (Berfield et al.,
2007). With airbrushes, the air pressure (and therefore the speckle
pattern density) can be adjusted to suit the video system resolu-
tion to get the optical pattern quality and data volume. Most often,
Fig. 7. The HFIR rabbit capsule design for SS-J and SS-Mini tensile specimens. SiC: irradiation temperature sensor for SiC-thermometry.
305
speckles of 3–7 pixels provide the best sensitivity and smallest
error (Sutton et al., 2009).
5. Test case for materials test reactor
It is unlikely that the effects of neutron irradiation experiments
could be fully simulated in the near future with tools like multiple
simultaneous ion-bombardment tests and advanced modeling and
simulation, even with substantial development activities ongoing
in both of these areas. If an irradiation project considers a new
specimen geometry, it may be advantageous to maintain compat-
ibility with existing infrastructure. To perform specimen irradia-
tion at HFIR, which is an 85 MWt beryllium-reflected,
pressurized, light-water-cooled and moderated flux-trap-type
reactor (Xoubi and Primm III, 2005), small cylindrical ‘‘rabbit” cap-
sules were developed over two decades ago to take advantage of
the very high neutron flux in this reactor (>1015 n/cm2 s in both
the thermal and fast regions of the spectrum). Each of these cap-
sules accommodated up to 24 SS-J type specimens. The general
internal capsule design remains the same from project to project,
with only the gas gap value being adjusted to meet project-
specific requirements for the irradiation temperature.
In the present work, the rabbit capsule design is tailored to con-
tain various tensile specimen styles, as shown in Fig. 7. This versa-
tile, modular configuration was developed to provide flexibility in
specimen loading and accommodates a useful range of irradiation
temperatures in support of nuclear materials research. Each unique
specimen configuration was designed to share the thermal equiva-
lency, allowing the SS-J2 and SS-2E specimen modules to be inter-
changeable with no impact on the design performance. This
equivalency was achieved by making the tensile specimens and
their supporting parts (chevrons, holders, liners, etc.) form a uni-
form ‘‘coupon” module with common mass, geometry, neutronic,
and thermal properties. The internal components for the assembly
configuration are shown in Fig. 8.
A key component of any irradiation program is to obtain the
desired irradiation dose (in dpa and/or neutron fluence) and irradi-
ation temperature. To address the newly developed SS-2E geome-
try impact on design temperatures, an ANSYS finite element
analysis (FEA) model is used. Given the modular nature of the
design, only a single tensile configuration layer located at the cap-
sule centerline is analyzed to determine thermal performance.
Scoping analyses are performed to show that all generic configura-
tions of SS-J2/SS-2E tensile specimens perform in the same fashion,
given the virtually identical heat loading and contact gaps seen in
the loading permutations. Table 5 outlines this thermal equiva-
lency for an irradiation running at a nominal temperature of
550 °C. There is a larger span of temperatures for the SS-J specimen
caused by the large temperature gradients observed in the grip sec-
tion of the specimens. However, the tensile gauge lengths for the
specimens are more analogous, as seen in Fig. 9. Hence, the SS-
2E specimen geometry and the pre-existing capsule design may
306 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308

Fig. 8. Specimens and modules prior to capsule assembly (left) and rabbit capsule internals (right). Also see Fig. 7.

Table 5
Design performance of the modular tensile design demonstrating thermal equivalence of the 550 °C temperature case.

Type Component Mass(g) Location Temperature (°C)

Avg. Min. Max
SS-2E module 6 SS-2E specimens 0.186 Inner 550 530 560
Middle 540 536 547
Outer 525 515 531
SS-J module 3 SS-J (T = 0.5 mm) 0.526 Inner 547 506 580
Middle 536 502 570
Outer 515 498 548

data—exists for the materials studied in Table 1. Given this, the

reduced mass of the miniaturized specimen geometry (nearly
7  less) should result in a significantly reduced radiological threat
on a per specimen basis. Clearly, follow-on work will address the
performance of the SS-2E geometry in the irradiated state, includ-
ing tensile performance, thermal performance, and radiological
threat performance.

6. Conclusions

The present work provides a complete engineering solution and

Fig. 9. Analyzed temperature comparison between SS-J2 and SS-2E specimens (°C).
be used in all flux trap positions available in the HFIR. Furthermore,
the modular subassemblies provide inherent specimen grouping
and simplify the post-irradiation disassembly. This feature pro-
vides valuable cost savings, given the relatively high cost of hot cell
facility usage.
As stated previously, the design of the miniature test specimen
should have reduced mass to limit the activated volume during
neutron irradiation. Because the SS-2E specimen geometry is
newly developed, no irradiation data—and hence no activation
experimental database on a small specimen geometry suitable for
irradiation in materials test reactors and post-irradiation out-of-
hot cell testing. A sub-sized specimen geometry, ‘‘SS-Mini,” was
designed; the new geometry leverages existing geometries, and
configurations for irradiation capsules lead to reduced cost for
deployment. The performance of the proposed geometry was eval-
uated using 304L stainless steel and several commercial alloys
with several different strength and ductility levels. Mechanical ten-
sile tests were carried out to compare the engineering mechanical
properties (yield stress, ultimate tensile stress, and uniform and
total elongation values) and plastic behavior of different miniature
specimens. It is shown that the proposed specimen geometry pro-
vides acceptable mechanical property results and meets the design
parameters for use in a materials test reactor.
Acknowledgements
This research was primarily funded by the U.S. Department of
Energy, Office of Nuclear Energy, for the Nuclear Energy Enabling
 M.N. Gussev et al. / Nuclear Engineering and Design 320 (2017) 298–308
Technologies (NEET) program for the Reactor Materials effort. Lab-
oratory Directed R&D funds at ORNL were used for testing of UAM
manufactured aluminum. The authors would like to thank Dr. L.M.
Garrison (ORNL) for providing tungsten tensile specimens for the
present work and D.P. Stevens and S. Crawford (ORNL) for help
with manuscript preparation.
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