Materials Science & Engineering A 613 (2014) 259–263

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Materials Science & Engineering A

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

High-temperature small punch test for mechanical characterization

of a nickel-base super alloy
S. Soltysiak a,n, M. Selent a, S. Roth a, M. Abendroth a, M. Hoffmann b, H. Biermann b,
M. Kuna a
a
Institute of Mechanics and Fluid Dynamics, TU Bergakademie Freiberg, Lampadiusstraße 4, 09599 Freiberg, Germany
b
Institute of Materials Engineering, TU Bergakademie Freiberg, Gustav-Zeuner-Straße 5, 09599 Freiberg, Germany

art ic l e i nf o a b s t r a c t

Article history: A testing device is presented, which allows the mechanical testing of miniaturized specimens at
Received 16 June 2014 temperatures up to 1273 K. Small punch specimens made from a thermally sprayed nickel-base super
Received in revised form alloy are tested at different temperatures and under different atmospheres. The tests are accompanied by
26 June 2014
finite element simulations. The sequential programming algorithm is used to determine the constitutive
Accepted 27 June 2014
Available online 5 July 2014
material parameters by minimizing the difference between simulated and experimentally obtained
small punch force–displacement curves. These findings are compared to results received by high-
Keywords: temperature tensile tests on standard-sized samples.
Small punch test & 2014 Elsevier B.V. All rights reserved.
High temperature
Thermally sprayed nickel-base super alloy
Sequential programming algorithm

1. Introduction
The small punch test (SPT) is used for decades now, and has
proven to be a reliable tool for the mechanical characterization of
materials. The procedure of testing as well as the geometrical
dimensions of the set-up are specified in a European Code of
Practice [1]. The SPT has been used for the evaluation of creep
properties by Dymáček and Milička [2], Chen et al. [3], and for the
determination of properties of brittle materials by Okuda et al. [4].
The brittle–ductile transition region of steels has been investigated
by Linse et al. [5]. Consequently, the SPT has been performed in a
wide temperature range. Abendroth et al. [6] and Milička et al. [7]
investigated creep properties of steels at 873 K, and Linse et al. [5]
performed experiments from room temperature down to 100 K.
Fracture mechanical parameters of steels have been determined by
Wang et al. [8] and by Abendroth and Kuna [9]. More special studies
like the inspection of irradiation effects were also performed [10].
The range of methods for the evaluation of SPT is as wide as the
range of its application. Baik et al. [11] identified empirical
correlations between the ductile–brittle transition temperature
obtained from experiments with Charpy V-notch specimens and
the SPT. Statistical material properties of brittle materials are
evaluated by means of the WEIBULL distribution [12,13]. The SPT is
nowadays often accompanied by a parameter identification with
the help of the finite element method (FEM). Kuna et al. [14]
presented the identification of parameters for the GURSON–T VER-
GAARD–NEEDLEMAN-model (GTN-model) and the BEREMIN-model by
means of neural networks (NN) or the response surface method
(RSM) from SPT data.
In this study a thermally sprayed nickel-base super alloy
(modified IN625) is investigated via the high-temperature small
punch test (HT-SPT). This alloy is used as a corrosion protection
coating on steel (1.5415) for heat exchanging devices. The material
is tested at three different temperatures (773 K, 973 K, and 1173 K).
At 1173 K two specimens are tested. One with a protective argon
atmosphere, and the other at air. The plastic stress–strain curves are
determined from the force–punch displacement curves (FD-curves)
by means of the sequential quadratic programming algorithm.
Furthermore, high-temperature tensile tests (HTT) are per-
formed with round bar tensile specimens. The specimens for both
tests are prepared from the thermally sprayed coating. The tensile
tests are carried out also at 773 K, 973 K, and 1173 K. The results of
the tensile tests are compared to those obtained from HT-SPT.
2. Experimental procedure
2.1. Testing set-up

n
Corresponding author. Tel.: þ 49 3731 39 3371. Fig. 1.(a) shows an overview of the entire test set-up, whereas
E-mail address: stefan.soltysiak@imfd.tu-freiberg.de (S. Soltysiak). Fig. 1.(b) depicts details of the SP-apparatus.

http://dx.doi.org/10.1016/j.msea.2014.06.105
0921-5093/& 2014 Elsevier B.V. All rights reserved.
260 S. Soltysiak et al. / Materials Science & Engineering A 613 (2014) 259–263

Fig. 1. (a) Scheme of the test set-up and (b) the details of the SP-apparatus.

0.5 mm

15 mm

Fig. 2. Pictures of the specimen preparations of (a) SPT specimens and (b) the HTT specimens, and the later loading directions (black arrows).

The load is applied via an universal testing machine (1) inspect
table 10 from HEGEWALD and PESCHKE with a maximum load capacity
of 10 kN. The universal testing machine provides the possibility to
perform either displacement or force controlled tests. The SPT is
performed at a constant displacement rate (SPT-CDR) of 0.5 mm/
min. The upper push-rod (2) is fixed at a 100 N load cell (3). The
SP-housing (4) is located inside an electrical furnace (5). This
electrical furnace has a maximum operating temperature of
1473 K. The furnace has three heating zones each controlled by a
PtRh10%  Pt=S thermocouple (6). A fourth thermocouple (TC) is
placed inside the SP-housing close to the specimen to ensure that
the specimen has the same temperature as the housing. The inert
gas (argon) is supplied through the pin (7) flowing through the
lower push-rod (8) in order to be pre-heated before reaching the
specimen.
The housing (a) for the SPT set-up and the fastener (b) are
made of a high-temperature alloy. The fastener seals the upper
part of the housing to retain the inert atmosphere, and guides the
punch (c). The specimen (d) having a radius R ¼ 4 mm and a
thickness of t ¼ 0:3 mm is placed onto the bearing (e). The centring
ring (f) aligns the specimen with respect to the punch and the
bearing. Two types of centring rings are available. The first one is
thicker than the specimens in order to perform tests without
clamping the specimen. The second one is thinner than the
specimens. The later one is used if a down-holding force should
be applied. In this case the guide-way (g) for the loading-ball (h) is
pressed onto the specimen by the fastener. The bearing as well as
centring ring, guide-way, loading-ball, and punch are made of
high-density alumina.
The high temperature tensile (HTT) tests are done using a
electro mechanical testing machine (Zwick Z020). Standard sized
specimens are mounted through two cone seats to assure a
moment-free application of tensile force. The displacement rate
for all hot tensile tests is 1  10  3 mm=s, and the force is
 S. Soltysiak et al. / Materials Science & Engineering A 613 (2014) 259–263
measured with a 2 kN load cell. The specimens are heated using an
electrical furnace with three heating zones. The specimen tem-
perature is measured in the middle of the gauge length directly at
the specimen surface.
2.2. Material and specimen preparation
A nickel-base super alloy (modified IN625) is investigated. This
material is used as a corrosion protection coating for 16Mo3 steel
at high temperatures. The application areas are for example heat
exchanging devices or waste incinerating plants. The corrosion
protection coating is applied on the substrate by a industrial high
velocity oxygen fuel (HVOF) spraying process. The particle size of
the spheroidal spray powder was about 45–90 μm.
For producing the SPT-specimens cylindrical rods (d ¼ 8 mm)
are cut from a plate, which has a corrosion protection coating (see
Fig. 2a). A core drill bit is used for the sampling. The protection
coating is separated from the substrate using an ACCUTOM 50 from
Struers. The specimens are grinded to remove residual parts of the
substrate. The final specimen thickness is t ¼ 300 μm.
For producing the HTT-specimens a plate of substrate material
16Mo3 is coated on one side with the modified IN625 alloy by
HVOF. The layer thickness is about 15 mm (see Fig. 2b). The coating
is separated from the substrate by wire cutting. Afterwards, the
final sample contour is machined by CNC precision turning. The
gauge length of the specimens is 50 mm and the gauge diameter is
5 mm.
3. Parameter identification
3.1. HT-SPT
The stress for either the initiation of the first crack or the
deviation from the linear elastic regime can be calculated by Eq.
(1), see [15]


F 3 Ra F t
σ¼ 2 1 þ ð1 þ νÞln ¼ 2 k; b 4 ð1Þ
t 2π b t 2 men tested under Argon atmosphere (Fig. 4b) does not present
In the equation above the parameters of the set-up are Ra , t,
and b, which are the inner radius of the bearing, specimen
thickness, and the contact radius between punch and specimen,
respectively. The POISSON's ratio ν is the only material parameter
that enters the equation. The parameters Ra , b, ν do not change for
one particular test series with the same set-up and the same
material. Therefore, they can be integrated into the set-up con-
stant k. The thickness of the specimen t is not incorporated into
the set-up constant because small thickness variations between
different specimens are acceptable.
A constant distribution of the force is assumed in the contact
area between loading-ball and specimen in Eq. (1). Since, the
correct determination of the contact radius b is nearly impossible
from experimental values, thus it is calculated using finite element
analysis.
The total work applied for a test can be calculated by Eq. (2).
This SP work is transformed into the elastic bending energy, the
plastic work of deformation, and the work of fracture (work to
create the surfaces of the cracks)
Z uf
W SP ¼ F du ð2Þ
u0
For the parameter identification a two-dimensional axisym-
metric finite element model of the SPT is used to calculate the
force–punch displacement curve (FD-curve) [16]. The non-linear
minimization problem
ΦðpÞ ¼ J F ðx; pÞ  y J -min
261
is solved using the sequential quadratic programming algorithm
(SQP) [17].
In Eq. (3) the vector p ¼ ½p1 ; …pn T contains the unknown
material parameters of the material law. The quantity ΦðpÞ is the
error norm between the calculated FD-curve F ðx; pÞ and the
experimentally obtained FD-curve y


1 N F sim ðuk ; pÞ  F exp ðuk Þ 2
ΦðpÞ ¼ ∑ -min ð4Þ
Nk¼1 F exp ðuk Þ
The FD-curves are discretized into N  1 regions (Eq. (4)), and
the sum of squares of differences is computed by each discretiza-
tion point inside the interval ½umin ; umax .
3.2. HTT
The stress–strain curves are calculated from the force-
elongation curves recorded during testing. The stresses are com-
puted with the measured force F HTT and the initial area of the cross
section S0 of the specimen.
F HTT
σ¼ ð5Þ
S0
4. Results and discussion
In Fig. 3 the specimens tested at 773 K and 973 K are presented.
The specimen tested at 773 K does not present macroscopic plastic
deformations. The five crack paths start from the center of the
specimen and extend on nearly straight lines symmetrically out-
wards. The specimen tested at 973 K does not break into fragments
but also shows five radial main cracks emanating from the speci-
men center and exhibits strong macroscopic plastic deformation.
The reverse sides of the two specimens tested at 1173 K are
shown in Fig. 4. The specimen presented in Fig. 4a is tested at air.
The green color, at the parts where the specimen is not supported
by the bearing, indicates high temperature oxidation. The speci-
such oxidation. A macroscopic change of the failure pattern, due to
the oxidation, cannot be observed. Compared to the sample tested
at 973 K the plastic deformation is concentrated in a smaller area
and the fracture surface is more rugged. The higher test tempera-
ture leads to a rise of ductility. The main plastic deformations are
shifted towards the specimen centre. As a result the five radial
main cracks do not reach the inner radius of the bearing. The
white areas in the middle of the specimens are the ceramic
loading-balls.
The FD-curves of the tested modified IN625 are shown in Fig. 5.
The material failure behavior changes from brittle fracture at
T ¼ 773 K to elastic–plastic damage above T ¼ 973 K. The max-
imum force is decreasing with increasing temperature. The punch
displacement, where the maximum force is reached, also increases
with higher temperatures. The change in the material behavior
leads to a higher total punch displacement for higher tempera-
tures. At a force of F drop ¼ 33:5 N the load drops by 13% for the
specimen tested at T¼ 773 K. This load drop indicates the initiation
of the first large crack [13]. The corresponding stress
σ drop ¼ 725:2 N mm  2 is calculated by Eq. (1).
Table 1 summarizes the SP results as there are maximum force,
punch displacement at maximum force, and SP-work for all tests.
The maximum force for the tests at T ¼ 1173 K is nearly equal,
which suggests that the observed oxidation on the specimen
tested at air is only facile, and has no significant influence on the
mechanical properties.
The change of the deformation behavior leads to an increasing
ð3Þ SP-work. The total work applied for the deformation of the
262 S. Soltysiak et al. / Materials Science & Engineering A 613 (2014) 259–263

Fig. 3. Specimens after the test at 773 K (a) and 973 K (b).

Fig. 4. Specimens after the test at 1173 K at air (a) and 1173 K under Ar-atmosphere (b). (For interpretation of the references to color in this figure caption, the reader is
referred to the web version of this paper.)

Fig. 5. FD-curves of the modified IN625 dependent on the testing temperature. Fig. 6. Stress–strain diagram obtained by means of HTT.

specimens at T ¼ 973 K and T ¼ 1173 K is about six times higher

Table 1 than the total work for the specimen tested at T ¼ 773 K. This
Maximum force F max , punch displacement at maximum force uðF max Þ, and defor-
strong increase can be explained by the additional plastic defor-
mation work W SP of the modified IN625 dependent on the testing temperature.
mation of the specimens tested at T ¼ 973 K and T ¼ 1173 K. The
T (K) 773 973 1173 1173 (Ar) differences of the SP-work for the tests at T ¼ 973 K and
T ¼ 1173 K are not significant.
F max ðNÞ 33.5 30.0 20.6 19.6 The stress–strain curves obtained by means of the HTT are
uðF max Þ ðmmÞ 0.11 0.33 0.64 0.65
W SP ðmJÞ 2.9 17.5 19.7 17.6
shown in Fig. 6. The change in the material behavior is evident.
The total strain is increasing, while the ultimate tensile strength is
 S. Soltysiak et al. / Materials Science & Engineering A 613 (2014) 259–263
Fig. 7. Comparison of experimentally obtained FD-curves with FD-curves from
parameter determination.
Table 2
0.2% offset yield strength σ y0:2 , and tensile strength Rm of the modified IN625
dependent on the testing temperature.
HT-SPT HTT
T (K) 773 973 1173 773 973
σ y0:2 ½N mm  2  – 192 11 – 163
Rm ½N mm  2  725 – – (565) 169
decreasing with increasing temperature. The fracture behavior
changes from brittle failure of the specimen tested at 773 K to
macroscopic plastic failure for the specimens tested at higher
temperatures.
The numerical identification of the stress–strain curves is
performed for the tests at 973 K and at 1173 K without argon
atmosphere. The experimentally obtained and the simulated FD-
curves are presented in Fig. 7. In both cases the mean quadratic
error between the curves is less than 1%.
The results of the HT-SPT and the HTT are summarized in
Table 2. The tensile strength, calculated from the tests at 773 K, is
significantly higher for the HT-SPT than for the HTT. Brittle fracture
of a specimen in the HTT goes along with sudden breakage of the
whole sample because of the homogeneous distribution of the
tensile stress within the gauge length of the specimen. Whereas in
the SPT specimen the failure process is a sequence of crack growth
events. Therefore, the SP tensile strength for brittle materials
corresponds to the initiation of the first crack.
The initial yield stress is higher for the test at 973 K obtained by
means of the HT-SPT, whereas σ y0 is significantly lower in the HT-
SPT at 1173 K. This may result from the different initial thicknesses
of the coating layers. The coating for the preparation of the tensile
test specimens is 30 times thicker than the coating for the SPT
specimens, and the coating is applied in several layers. This means
that the coating undergoes several thermal cycles accompanied by
melting and solidification of the material.
5. Conclusions
A testing apparatus for a miniaturized plate bending experiment
at high temperatures (HT-SPT) has been introduced. The test can be
263
performed with or without an inert atmosphere. The exact specimen
temperature is measured and controlled using an additional thermo-
couple inside the housing of the SP apparatus.
A HVOF deposited modified IN625 is tested at three different
temperatures using the HT-SPT. The transition from brittle to
ductile failure can be clearly observed. To identify the offset yield
stress and the tensile strength accompanied finite element ana-
lyses are necessary together with an optimization procedure. The
presented method gives comparable results as high temperature
tensile tests. But, the specimen thickness used for HT-SPT is more
representative for a thin layer coating than standard sized tensile
specimens. Care has to be taken if material particles reach a critical
size in comparison to SPT specimen thickness.
Acknowledgments
The financial support for S. Soltysiak by the German Research
Foundation (DFG) in the collaborative research center SFB920 is
gratefully acknowledged. M. Abendroth, S. Roth, M. Selent, and M.
Hoffmann are funded by EFRE of the European Union and by the
Ministry of Science and Art of Saxony (SMWK) within the Cluster
1173
of Excellence “Structure Design of Novel High-Performance Mate-
rials via Atomic Design and Defect Engineering (ADDE)”. The
37 authors appreciate the help of D. Schmidt with the specimen
43 preparation, and T. Behm with the LSM investigations.
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