Accepted Manuscript

On the determination of the ductile to brittle transition temperature from small punch
tests on Grade 91 ferritic-martensitic steel

M. Bruchhausen, S. Holmström, J.-M. Lapetite, S. Ripplinger

PII: S0308-0161(15)30116-2
DOI: 10.1016/j.ijpvp.2017.06.008
Reference: IPVP 3632

To appear in: International Journal of Pressure Vessels and Piping

Received Date: 9 November 2015

Revised Date: 17 January 2017
Accepted Date: 19 June 2017

Please cite this article as: Bruchhausen M, Holmström S, Lapetite J-M, Ripplinger S, On the
determination of the ductile to brittle transition temperature from small punch tests on Grade 91
ferritic-martensitic steel, International Journal of Pressure Vessels and Piping (2017), doi: 10.1016/
j.ijpvp.2017.06.008.

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 ACCEPTED MANUSCRIPT

On the determination of the Ductile to Brittle Transition Temperature from Small

Punch tests on Grade 91 ferritic-martensitic steel

M. Bruchhausena,∗, S. Holmströma , J.-M. Lapetitea , S. Ripplingera

a European Commission, Joint Research Centre (JRC), Institute for Energy and Transport (IET), Westerduinweg 3, 1755 LE Petten, The

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Netherlands

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Abstract
The exposure of structural materials to the environment in nuclear power plants leads to aging through thermal and/or

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irradiation effects. One of the consequences of this aging is the shift of the ductile to brittle transition temperature
(DBT T ) towards higher temperatures. Characterising the aging of structural materials is therefore a safety relevant
topic especially in the context of long term operation of nuclear plants.
For testing in service materials and to reduce the health risks and costs associated with handling of irradiated

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materials miniature testing techniques are being developed. The small punch (SP) technique is one of these methods.
In a tensile/fracture SP test, a punch with a hemispherical tip is pushed with a constant displacement rate through the
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center of a small cylindrical disk specimen.
A series of tensile SP tests on the ferritic/martensitic steel Gr. 91 at two different displacement rates show no impact
of the displacement rate on the DBT T . A new method using fracture energies normalised to the maximum force for
deriving the DBT T from force-deflection data is presented.
M

Post-test analysis by means of X-ray computed tomography is used for deriving the DBT T from fracture strains.
Both methods give consistent values for the transition temperature. However, the DBT T determined in this study is
higher than what can be found in the literature. Supplementary tests indicate that the punch diameter has an effect on
the SP defined DBT T .
D

Keywords: Small Punch Testing, Ductile to Brittle Transition Temperature (DBT T ), fracture strain, Grade 91,
Gr. 91, P 91, T 91, miniature testing techniques
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1. Introduction One of the possible areas of application of SP testing

in the energy sector is the characterization of structural
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Recently the small punch (SP) test technique [1]
has received much attention for characterising materi-
als with regard to their mechanical properties.
The multi-axial, time dependent stress state makes it
C
materials with regard to aging phenomena such as tem-
per embrittlement. In nuclear power plants the expo-
sure of structural components to neutron fluxes during
their lifetime also leads to irradiation induced embrit-

difficult to relate the mechanical properties determined tlement. Both embrittlement processes lead to the shift
by SP testing to the results from standard sized spec- of the ductile to brittle transition temperature (DBT T )
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imens [1–7]. The small specimen size nevertheless
makes SP testing a valuable tool for materials character-
ization, especially when only small amounts of material
are available (as for aged materials or experimental ma-
terials that are still being developed) or because safety
considerations require the use of small specimens (as
for irradiated materials) [2, 5, 8, 9].
∗ Correspondingauthor
Email address: matthias.bruchhausen@ec.europa.eu ( M.
Bruchhausen)
towards higher temperatures. The DBT T is usually de-
termined by means of Charpy tests which require quite
large standard specimens (10×10×55 mm3 ) [10]. Irradi-
ation embrittlement of the structural components of nu-
clear power plants is monitored using dedicated Charpy
specimens that were deposited in the reactor pressure
vessel and have been exposed to the same irradiation
history as the actual reactor components. Especially in
the context of lifetime extension projects for many nu-
clear power plants there is a strong interest in develop-
ing techniques for determining the DBT T with smaller

Preprint submitted to International Journal of Pressure Vessels and Piping June 20, 2017
 ACCEPTED MANUSCRIPT

specimens. Consequently, the SP test is also used in that

context [5, 6, 11].
We present SP results regarding the impact of the
punch displacement rate on the measured DBT T . Dif-
ferent approaches for deriving the DBT T from fracture
energies are discussed and compared to the DBT T esti-
mated from fracture strains.

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The material selected for the present work was the
ferritic/martensitic steel Grade 91 (Gr. 91). The me-
chanical properties of the alloy such as its tensile and
creep characteristics and its swelling resistance make it

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an interesting candidate material especially for nuclear
applications. Consequently, is has been in the focus of
European projects like MATTER [12] and MATISSE.

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2. Experimental Details

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2.1. Material and specimens Figure 1: Sketch of the SP setup. The main dimensions are listed in
Tab. 3
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The alloy used in the present study is the fer-
ritic/martensitic steel Gr. 91 (X10CrMoVNb9-1). It has
the same chemical composition as P91/T91 but is sup-
2.2. Test rig
plied in form of a plate rather than as pipe (P91) or tube
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(T91). The particular batch of Gr. 91 used in the present
work (S50460) as part of the FP7 project MATTER
[12] was originally produced for the FP6 project EURO-
TRANS (project domain 4: DEMETRA). Its chemical
D
In a tensile/fracture SP test, a hemispherical punch
is pushed with a constant displacement rate through the
disc shaped specimen along its axis of symmetry. Dur-

ing the test, the applied force is recorded as a function

composition is listed in Tab. 1. The material was deliv- of punch displacement.
ered as hot rolled and heat treated plate with a thickness The setup used in the current work is shown in
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of 15 mm by Industeel, Arcelor group. The steps of the
heat treatment are detailed in Tab. 2.
Disc shaped SP specimens as specified in the Euro-
pean Code of Practice [1] were used. Their diameter
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Fig. 1. The specimen holder consists of two dies be-
tween which the specimen is clamped. The punch
(2 mm diameter) is pushed from the top through the
specimen. The receiving hole in the lower die has a

was 8 mm and their thickness 0.5 mm. The surface
roughness was less than Ra = 0.15 µm on both sides as
specified by the workshop. One surface of every speci-
men was checked using a surface roughness tester (Mi-
C
diameter of 4 mm with a 45◦ chamfer to avoid shearing-
off of the specimen. The movement of the punch is
controlled by means of an Instron type 5586 universal
testing machine.

tutoyo SJ-201) and no surfaces out of specification were Below the specimen a ceramic rod is mounted. This
found. ceramic rod contains a thermocouple in direct contact
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All specimens were cut from the same block of mate-
rial but with two different orientations: TS and TL. The
letters L, T and S respectively refer to the longitudinal
(rolling), transverse and short transverse directions. The
designation of the groups follows the principle that the
letter missing in the designations indicates the axis per-
pendicular to the specimen plane.
Investigations within the MATTER project did not
show any anisotropy effect in SP tensile tests, so the dif-
ferent orientations in the two test groups are considered
having no impact on the test results [13].
2
with the lower specimen surface for controlling the test
temperature. The ceramic rod also transmits the defor-
mation of the specimen to a linear variable displacement
transducer (LVDT). This configuration avoids measure-
ment uncertainties from the test rig compliance. How-
ever, due to thinning of the specimen during the test, the
measured deflection is slightly smaller than the actual
punch tip displacement.
The specimen holder is placed in a thermal chamber
(Instron 3119-407 series) that can be cooled down to
−196 ◦ C by means of liquid nitrogen or heated up to
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Fe C Mn P S Si Cu Ni Cr Mo Al Nb V Ti N
bal. 0.097 0.386 0.020 0.0005 0.218 0.080 0.115 8.873 0.871 0.009 0.077 0.195 0.003 0.0440

Table 1: Chemical composition of the DEMETRA Gr. 91 heat [wt.%] according to supplier

step temperature duration cooling

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◦
normalization 1050 C 15 minutes water cooling to room temperature
tempering 770 ◦ C 45 minutes air cooling to room temperature

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Table 2: Heat treatment of the DEMETRA Gr. 91

300 ◦ C.

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2000

1800
For the present work tests were carried out at punch
1600
displacement rates of 0.5 mm/s and 0.005 mm/s as mea-
1400
sured from the cross-head displacement.
1200

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F [N]
1000

800
2.3. Post-test analysis
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600
TL17
400
Post-test determination of the fracture strains was car- du/dt = 0.005 mm/s
200 T = −100 °C
ried out by means of X-ray computed tomography (CT)
0
using a commercial Phoenix Nanotom S research edi- 0 0.5 1 1.5 2
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u [mm]
tion tomograph. In a CT analysis, the specimen is ro-
tated stepwise and X-ray images are taken under differ- Figure 2: Force-deflection curve for ductile failure.
ent angles. In a post processing step, all the scans taken
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at the different angles are used to reconstruct a full 3D

model of the specimen. The scans in the present study
3. Experimental results
were carried out with a voltage of 130 kV and a cur-
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rent of 120 µA. A 0.5 mm Sn filter was used to cut-off
the low-energetic radiation. The configuration lead to a
spatial resolution of 4.24 µm.
A commercial software package (VGStudio Max 2.2
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3.1. Fracture energy
One possibility for determining the DBT T is based
on the temperature dependence of the fracture energy
Efrac . In the transition region, a small reduction of tem-

from Volume Graphics) was used for visualizing and
analyzing the data. Specimen thicknesses were deter-
mined by means of the metrology module ”Wall Thick-
ness”. For this purpose, first the specimen surface was
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perature leads to a strong drop of Efrac .
Fig. 2 shows the force-deflection curve of a typical
ductile fracture. In order to determine Efrac , the force F
has to be integrated over the deflection u until specimen

determined from the 3D data. During the actual wall rupture occurs. The current Code of Practice suggests
thickness determination, a simulated beam is sent from using the force drop to 80% of its maximum [1] as rup-
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each point of the surface in the direction normal to the
surface through the specimen and bounced back from
the opposite surface. If the reflected beam hits the spot
from which the original beam was emitted, the distance
between the emission point and the point where the
beam was reflected is considered as the wall thickness
in that point of the specimen. For the surface normals
at the points where the beam is emitted and where it is
reflected tolerance angles of 20◦ were used.
More detailed information on the experimental pro-
cedures can be found in [14].
3
ture criterion. In the present work, however, the integra-
tion is carried out up the maximum force as seems to be
done by most authors [5, 15–17].
Fig. 3 shows the force-deflection curve for a typical
brittle case where failure does not occur in a single event
but progressively in several steps. In the example three
occasions (as indicated by the black arrows) can be seen
where the force drops before reaching its maximum.
This case of brittle failure is not covered by the cur-
rent Code of Practice. Three possibilities for defining
the fracture energy Efrac in the case of brittle failure are:
 ACCEPTED MANUSCRIPT

feature symbol size

punch diameter d 2 mm
diameter of receiving hole (lower die) d2 4 mm
chamfer length (lower die) l 0.2 mm
chamfer angle (lower die) α 45◦
specimen diameter d1 8 mm
specimen thickness h 0.5 mm

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Table 3: Principle dimensions of the SP specimen and setup

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1500
these cases the consecutive force drops added up to a
cumulative drop of 20% before the maximum force was

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reached. After reaching its maximum the value the force
1000 drops very quickly so that in the present case maximum
and the 20% cumulative drop criterion lead to virtually
F [N]

identical results. Therefore only the maximum and first

crack criteria are considered further.

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500
TL14
The fracture energies evaluated according to both def-
initions are plotted in Fig. 4 for the two cross-head dis-
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du/dt = 0.500 mm/s
T = −196 °C
placement rates. The data upon which these evaluations
0
0 0.5 1 1.5 2 are based can be found in Tab. 4 in the appendix. The
u [mm]
data sets themselves are identified by digital object iden-
tifiers (DOIs) [20]. They can be accessed through the
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Figure 3: Force-deflection curve for brittle failure in several steps

European Commission’s online data base MatDB via
the ODIN portal [21].
In both graphs the fracture energy Efrac starts at low
1. Maximum Force
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temperatures at a low level, rises quickly in a transition

In this case, Efrac is calculated exactly as in the region and then drops again slowly at higher tempera-
ductile case by integrating the force up to its max- tures. There is no discernible effect of the variation in
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imum. This procedure has been used by several
authors on different types of steels [5, 16, 17].
2. 20% cumulative drop
This is an extension of the 20% force drop criterion
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displacement rate. The scatter in the lower shelf i.e. at
temperatures below the transition temperature for brittle
fracture is much higher than for ductile failure for both
methods of evaluating the fracture energy Efrac . This re-

suggested in the current Code of Practice: consec-
utive force drops are added until a total cummu-
lative force drop of 20% has been reached. This
method has been applied on ferritic oxide disper-
C
flects the strong dependency especially of brittle crack
initiation on irregularities in the microstructure or mi-
croscopic scratches even on polished surfaces.

sion strengthened steel MA956 [18].

3.2. DBT T from fracture energy
3. First Crack
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Applying this method considers the first onset of
cracking indicated by the first measurable drop of
the force as upper limit for the integration. The
specimen has not yet failed at this point and is able
to support higher stresses as demonstrated by the
continued increase of the force after initial crack-
ing (Fig. 3). This method has been used e.g. for
the characterization of the ferritic-pearlitic steel
AE460 [19].
In the present study many cases of multi-step fracture
in the brittle regime were found, however in none of
4
For determining the DBT T the fracture energies are
often considered separately in the upper and the lower
shelf regions [5, 16]. We use the same approach as in [5]
where Efrac is considered separately in the lower and up-
per shelves and described as a function of temperature
T in the form:
ELS/US (T ) = ALS/US + BLS/US exp CLS/US T
 
(1)
where the fitting parameters ALS/US , BLS/US and CLS/US
are determined independently by least squares fits in the
lower (index LS) and upper (index US) shelves where
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the lower shelf includes the transition region. In this ap-

proach two distinctive energies can be defined: Emin , the
fracture energy at the zero-point of the absolute temper-
ature (i.e. T = −273.15 ◦ C), is determined by extrapo-
lating the fitted function for the lower shelf. Emax is the
fracture energy at the intersection point between the fits
for the lower and upper shelves. The transition tempera-

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ture DBT T 2fits is then defined as the temperature where:
Emin + Emax
(a) 2.5 Efrac (DBT T 2fits ) = (2)
0.5 mm/s 2

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0.005 mm/s
where the index ”2 fits” refers to the 2 functions fitting
2 procedure.
The curves in Fig. 4 show the fitted curves for both

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1.5 displacement rates and evaluation methods. The differ-
E frac [J]

ent symbols for the data points identify the points hav-
ing been assigned to the lower and upper shelf regions
1 respectively. In the case of the lower displacement rate
the data point at −130 ◦ C (specimen TS09) was consid-

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Method: maximum

0.5
E min = 0.7 J E min = 0.1 J ered being at the edge of the upper shelf and has there-
Emax = 1.7 J Emax = 1.6 J
fore been taken into account for fitting both functions
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DBTT2 fits = -120.9 °C DBTT2 fits = -171.7 °C
ELS (T ) and EUS (T ).
0 The calculated transition temperatures DBT T 2fits (as
-200 -150 -100 -50 0 50
T [°C] listed in Fig. 4) lie relatively close together with the ex-
ception of the case where the data for a cross-head dis-
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(b) 3
0.5 mm/s placement of 0.005 mm/s was evaluated with the maxi-
0.005 mm/s
2.5
mum method (red, dashed line in Fig. 4 (a)). A problem
with this two fits method is that the intersection point
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between the two separately fitted functions for the up-

2
per and lower shelves needs to be determined accurately
E frac [J]

since that defines Emax in eq. 2. In cases where there is

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1.5
no data point at the low edge of the upper shelf, this in-
tersection point needs to be determined by extrapolation
1 which can lead to relatively large uncertainties.
Method: first crack
E min = 0.4 J E min = 0.5 J An alternative approach is determining DBT T by fit-
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0.5 Emax = 1.7 J Emax = 1.7 J ting a tanh function as the one used in varying formula-
DBTT2 fits = -124.0 °C DBTT2 fits = -122.9 °C
tions for evaluating Charpy tests [11, 22–24]:
0
-200 -150 -100 -50 0 50 EUS + ELS EUS − ELS  T − DBT T 
Efrac = + tanh (3)
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T [°C]
2 2 2∆T
Figure 4: Fracture energy Efrac as function of temperature evaluated where T is the temperature, EUS and ELS are the upper
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using the maximum (a) and the first crack (b) method. and lower shelf energies, DBT T is the transition tem-
perature and ∆T is a fitting parameter characterizing the
slope in the transition region.
However, when looking at the data points in the upper
shelf it is clear that Efrac drops with rising temperature.
This trend has already been observed by several authors
for a variety of materials [17, 25–28]; although some
data indicate this behaviour might be material depen-
dent and not be a universal trend [11, 17]. In the case
of many materials, where the fracture energy Efrac in the
upper shelf drops with temperature the function in eq. 3
5
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×10 -3 In all cases, the normalization of Efrac with Fmax leads

(a) 1
0.5 mm/s to constant values in the upper shelf and the data points
0.005 mm/s
can be well described by a function as in eq. 3 where
0.8 the energies are replaced by normalized energies. For
the data in the present study, the transition temperatures
E frac / F max [m]

0.6
DBT T n determined by this procedure are 5−10 ◦ C lower
than DBT T 2fits determined above. However, there is one

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outlier, namely the DBT T n determined for a displace-
Method: maximum
0.4
DBTT n = -125 °C DBTT n = -135 °C
ment rate of 0.5 mm/s evaluated using the first crack
E/F LS = 0.470 mm E/F LS = 0.369 mm
method. The significantly lower DBT T results from the
data point at −196 ◦ C which is from a specimen that

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E/F US = 0.837 mm E/F US = 0.867 mm
0.2
∆T n = 2.72 °C ∆T n = 21.28 °C started cracking at a very low force level Fig. 5 (b)).
Using the tanh function (eq. 3) for calculating the
0 transition temperature from the fracture energies instead
-200 -150 -100 -50 0 50

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T [°C]
of the method based on two independent fits (eq. 1) has
×10 -3 the advantages that less fitting parameters are required,
(b) 1
0.5 mm/s
it potentially avoids extrapolation and does not require
0.005 mm/s a manual (and to some extend subjective) attribution of

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0.8 the data points to the lower or upper shelf.
Regarding the calculation of Efrac by either the max-
imum or the first crack method and respectively com-
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E frac / F max [m]

0.6
paring the data points plotted in Fig. 4 (a) and (b) and in
Fig. 5 (a) and (b), it is obvious that there is less scatter in
0.4
Method: first crack the plots (a) in both cases i.e. when Efrac was calculated
DBTT n = -149 °C DBTT n = -128 °C
using the maximum of the force also for brittle failure.
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E/F LS = 0.053 mm E/F LS = 0.361 mm

Hence, based on the data from the present study, the
E/F US = 0.867 mm E/F US = 0.853 mm
0.2 best method for calculating DBT T from the fracture
∆T n = 25.11 °C ∆T n = 8.80 °C
energies is using the maximum method for calculating
D

0
Efrac , normalizing it by the maximum force Fmax and
-200 -150 -100 -50 0 50 fitting a tanh function according to eq. 3. That corre-
T [°C]
sponds to the evaluation shown in Fig. 5 (a).
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Figure 5: Fracture energy Efrac normalized to the maximum force as

function of temperature evaluated using the maximum (a) and the first
3.3. DBT T from fracture strain
crack (b) method. Another possibility for determining the DBT T from
SP tests is by means of the fracture strain εf which is
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defined as [1]:
!
t0
is not suited to describe the data in the entire upper shelf εf = ln (4)
region. One possibility to overcome this problem would tf
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be to use only data on the low temperature side of the where t0 is the initial specimen thickness and tf the final
upper shelf for the fit. We propose a different approach: specimen thickness next to the area of failure. We have
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the drop of Efrac with rising temperature is likely caused
by the reduction of the ultimate tensile strength σUTS
with rising temperature. The maximum force in a small
punch test Fmax is correlated to σUTS [4, 5, 29]. We
therefore propose normalizing Efrac with Fmax , the max-
imum force reached in the test. When the maximum
method is applied for calculating Efrac , Fmax is simply
the maximum force during the entire test; when the first
crack method is applied, Fmax is the first (local) maxi-
mum of the force signal. The results are plotted in Fig. 5
for both evaluation methods.
6
used X-ray computed tomography (CT) for determining
εf for a number of SP specimens. Since the CT scans are
quite time consuming, only the specimens tested with a
displacement rate of 0.5 mm/s have been investigated.
Fig. 6 shows the reconstructed 3D model of a SP
specimen tested at −196 ◦ C. The color coding refers
to the specimen thickness which determined as laid out
in section 2.3 . The thickness has not changed signif-
icantly in the outer part of the specimen where it was
clamped during the test. In the central part of the speci-
men, however, significant thinning can be observed with
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1.5
0.5 mm/s

ǫf

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0.5
ǫ min = 0.14
ǫ max = 1.06

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DBTTǫ = -123.0 °C
Figure 6: Full view of a CT image of specimen TL14 (tested at
∆ Tǫ = 13.1 °C
−196 ◦ C) with automatic thickness determination. In the gray areas
no thickness could be calculated. 0
-200 -150 -100 -50 0 50

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T [°C]

Figure 8: Fracture strain εf as function of temperature T for specimens

tested with a displacement rate of 0.5 mm/s.

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εUS + εLS εUS − εLS  T − DBT T 
ε
εf = + tanh (5)
2 2 2∆T
The transition temperature DBT T ε determined from
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the fracture strain is −123 ◦ C which coincides very well

with the DBT T of −125 ◦ C determined from the same
Figure 7: Profile taken from the specimen in Fig. 6. specimens’ normalized fracture energies using the max-
D

ium method (solid black curve in Fig. 5 (a)). In an

earlier study on the micro-alloyed ferritic-pearlitic steel
AE460, the DBT T from fracture strain was found to be
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the thinnest area being in a ring around the specimen 15 ◦ C higher than the DBT T from the fracture energies
center. [19].
The current CWA recommends cutting the specimen
through the centre on a line perpendicular to the crack
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and measure its thickness ”adjacent to the area of fail- 4. Discussion

ure”. The CT data allows building on that procedure and
analysing the thickness along two perpendicular diamet- Based on a number of SP tests and specimens two
ric cuts. Fig. 7 shows one of these cuts with the colors completely independent evaluations have resulted in
C

again referring to the wall thickness. The thinnest part close estimates for the DBT T . One evaluation was
along the profile has been used to calculate the fracture based on the force and deflection data registered during
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strain according to eq. 4. For determining the thinnest
part of the specimen the areas in violet at the edges
of the crack have been discarded. E.g. in the case of
the specimen in Figs. 6 and 7 tf was determined to be
407 µm.
In Fig. 8 εf is plotted as a function of temperature
T . The transition from brittle failure at lower temper-
atures to ductile behaviour at higher temperatures is
clearly visible. The corresponding transition tempera-
ture DBT T ε was determined by a least squares fit of a
tanh function of the same form as for the determination
7
the test (DBT T 2fits , DBT T n ) whereas the other method
used post-test analysis of the specimens (DBT T ε ). The
good agreement between the transition temperatures
gives a strong confidence in their accuracy. Neverthe-
less, previous studies using SP tests for determining the
DBT T of Gr. 91 came to significantly lower transition
temperatures around −164 ◦ C [11] and −167 – −178 ◦ C
in an inter-laboratory comparison [5]. Since the latter
study used material from the same block of Gr. 91 as
the present work, material variations can be ruled out as
a possible reason for this discrepancy.
 ACCEPTED MANUSCRIPT

An explanation might be found in the test setup itself: 3000

while all tests were carried out using 0.5 mm thick spec- 2.0 mm punch
2.5 mm punch
imens with 8 mm diameter and the diameter of the lower 2500

die was 4 mm, the two studies cited above used punches
2000
with a tip diameter of 2.5 mm whereas the punch used

F [N]
in this study had a tip diameter of 2 mm. It seems likely 1500
that the smaller punch could have lead to the higher tran-

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1000
sition temperatures. In fact in [5] smaller TEM-type SP
specimens were compared to the ususal SP specimens. 500
The TEM-type specimens had a diameter of 3 mm and
a thickness of 0.25 mm. The punch tip diameter was 0

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0 0.5 1 1.5
1 mm. The DBT T determined from the smaller speci- u [mm]
mens showed a larger spread but were generally lower
than the values from classical SP specimens (−170 – Figure 9: Force deflection curves for Gr. 91 specimens at −140 ◦ C
with two different punch diameters.

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−193 ◦ C). This supports the hypothesis that the test
setup has an impact on the DBT T .
To confirm or refute this hypothesis a number of addi-
tional small punch tests were performed with two punch were based on the maximum force and the first
diameters (2 mm and 2.5 mm) at −140 ◦ C, a tempera-

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ture lying between the DBT T from the literature and
the DBT T determined in the present study. The tests
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have been carried out at a cross-head displacement rate
of 0.005 mm/s on a different melt of Gr. 91 (60 mm
thick plate 20057 (M1) from ArcelorMittal delivered for
the MATTER project). In two cases the hemispherical
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crack, respectivly, the former method proved to be
the better choice because it led to less scatter in the
data.
2. The method proposed in this work for calculating
the DBT T based on fracture energies normalized
with the maximum force has significant advantages
compared to the method frequently used in the lit-

punch was replaced by a ceramic ball bearing ball with erature which directly uses the fracture energies. It
the same diameter (see Tab. 5). This change is not ex- allows using a single fitting function over the entire
pected to have an effect on the test. The advantage of us- temperature region, requires less fitting parameters
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ing balls is that these can easily be changed after every and avoids a manual attribution of data points to
test which eleminates potential issues related to wear of the lower or upper shelf region.
the punch tip caused by repeated testing with the same
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3. X-ray computed tomography is a reliable, non de-

punch. structive means for determining fracture strains.
A criterion for distinguishing between brittle and
4. Fracture strains can be used for calculating the
ductile failure could be whether the force-deflection
DBT T . The DBT T determined independently
curve reaches the ”force reversal point” i.e. the point
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from normalised fracture energies and fracture

where dF/du = 0. Applying this criterion to the force-
strains of the same specimens are consistent.
deflection curves from the additional tests (Fig. 9) show
5. Depending on the punch diameter SP tests under
that all three specimens tested with the 2 mm punch in-
otherwise identical conditions can lead to brittle or
curred brittle failure. In the tests with a 2.5 mm punch
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ductile fracture with a smaller punch diameter fa-

only the single early failure was brittle whereas the three
voring brittle fracture. This explains the difference
other specimens failed in a ductile way. This observa-
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between the DBT T determined in the present study

tion confirms the impact of the punch diameter on the
and data from the literature.
DBT T determined by small punch testing.

5. Conclusions 6. Appendix: Test Data

A series of tensile SP tests were carried out on Gr. 91
specimens with two displacement rates and the ductile
to brittle transition temperatures have been determined.
The following main conclusions can be drawn:
1. From the two methods used for determining the
fracture energy from force-deflection curves which
8
7. Acknowledgment
The materials were made available through the MAT-
TER project within the European Union Seventh Frame-
work Programme (FP7/2007-2013) under grant agree-
ment number 269706. The reasearch was carried out
 ACCEPTED MANUSCRIPT

maximum first crack

Displacement
Specimen T [◦ C] Efrac [J] Efrac
Fmax [m] Efrac [J] Efrac
Fmax [m] εf
rate [mm/s]
TS08 0.005 -196 0.633 0.000420 0.633 0.000420 -

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TS15 0.005 -196 0.378 0.000365 0.273 0.000266 -
TS11 0.005 -170 0.681 0.000444 0.681 0.000444 -
TL08 0.005 -150 1.045 0.000582 0.370 0.000338 -
TL23 0.005 -132 1.109 0.000580 1.110 0.000580 -

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TS09 0.005 -120 1.407 0.000703 1.399 0.000699 -
TL17 0.005 -100 1.624 0.000816 1.624 0.000816 -
TL22 0.005 -60 1.530 0.000859 1.529 0.000859 -

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TS05 0.005 -20 1.482 0.000920 1.482 0.000920 -
TL24 0.005 23 1.287 0.000854 1.287 0.000854 -
TL14 0.5 -196 0.709 0.000517 0.019 0.000053 0.206
TL10 0.5 -196 - - - - 0.142

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TL16 0.5 -170 0.825 0.000477 0.825 0.000477 0.223
TS13 0.5 -170 0.528 0.000379 0.528 0.000379 0.272
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TL12 0.5 -150 0.760 0.000506 0.261 0.000254 0.243
TL20 0.5 -130 0.895 0.000522 0.895 0.000522 0.307
TS07 0.5 -120 1.705 0.000788 1.705 0.000788 0.835
TL26 0.5 -100 1.703 0.000809 1.703 0.000809 0.853
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TL18 0.5 -60 1.614 0.000861 1.614 0.000861 1.039

TS10 0.5 -20 1.458 0.000839 1.458 0.000839 1.121
TL25 0.5 23 1.332 0.000840 1.332 0.000840 1.027
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Table 4: Test data for Gr. 91 from the INTEGRITY project. The fracture strain has only been determined for the tests at a cross head displacement
rate of 0.5 mm/s. For specimen TL10 no curve data is available because of a problem with the data acquisition. The full data sets are identified
through digital object identifiers (DOIs) [20]. The data can be accessed through the European Commission’s online data base MatDB via the ODIN
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portal [21]. Additional information on the experimental procedures is available in [14].

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Specimen T [◦C] Punch diameter [mm] Punch type Failure mode Fmax [N]
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AW023 -142 2 hemispherical brittle 1946

AW024 -135 2 hemispherical brittle 1824
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AW028 -142 2 hemispherical brittle 1833

AW025 -142 2.5 ball ductile 2797
AW033 -141 2.5 hemispherical ductile 2720
AW034 -142 2.5 hemispherical brittle 1684
AW036 -141 2.5 ball ductile 2657

Table 5: Tests on specimens from the 60 mm plate of Gr. 91 from the MATTER project. The full data sets are identified through digital object
identifiers (DOIs) [30]. The data can be accessed through the European Commission’s online data base MatDB via the ODIN portal [21].

9
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 ACCEPTED MANUSCRIPT
 Small punch testing was used to determine the DBTT of Gr. 91 steel.
 Evaluation methods based on fracture energy and fracture strain are compared.
 A single type fitting function is proposed for the determination of the DBTT.
 DBTT derived from fracture energy and fracture strain was very similar.
 The data are openly available.

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