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Institute for Polymer Product Engineering, Johannes Kepler University Linz, Austria
Institute for Polymeric Materials and Testing, Johannes Kepler University Linz, A, Former Institute of Materials Science and Testing of Plastics,
University of Leoben, Leoben, Austria
c
Polymer Competence Center Leoben GmbH, Leoben, Austria
b
a r t i c l e
i n f o
Article history:
Received 5 January 2009
Received in revised form 6 August 2009
Accepted 17 August 2009
Available online 21 August 2009
Keywords:
Rapid gas decompression failure
Crack initiation and propagation
Fracture toughness of rubber
Tearing energy
Continuous and discontinuous crack growth
a b s t r a c t
The monotonic fracture behaviour of two elastomer compounds (HNBR and FKM) was
characterized in this study. These elastomeric materials are frequently used in many oileld applications (e.g., seals and hoses) and are exposed to a complex combination of
mechanical, thermal and environmental loads. Furthermore, rapid gas decompression failure of these elastomeric materials was observed under real service conditions. A phenomenon termed rapid gas decompression (RGD) damage occurs when elastomer seals exposed
to high gas pressure fail in a brittle manner upon the sudden release of the gas pressure.
Hence, to support both material development and design efforts, it is of prime theoretical
and practical importance to characterize the fracture behaviour of these materials. Fracture
mechanics tests using a faint waist pure shear specimen (FWPS) conguration were performed over a wide loading rate range. First, global force and displacement values were
measured and single parameter fracture mechanics values in terms of peak tearing energy,
Tp values were calculated. Furthermore, the crack growth process and the local crack tip
deformation were characterized by non-contact optical devices. The digital image correlation technique used allows for the determination of displacement and full-eld strain up to
a high strain and crack growth rate. Based on above measurements, crack growth resistance curves in terms of tearing energy (T Dc) and crack tip opening angle (CTOA Dc)
functions were derived. While a continuous crack growth was observed for HNBR at all
loading rates, a discontinuous crack extension was observed for FKM. Finally a phenomenological model was deduced for describing the rapid monotonic crack extension process
for these elastomeric compounds.
2009 Elsevier Ltd. All rights reserved.
* Corresponding author. Address: Institute for Polymer Product Engineering, Johannes Kepler University Linz, Polymer Competence Center Leoben GmbH,
Altenberger STr 69, Linz, Austria. Tel.: +43 732 2468 1651.
E-mail addresses: zoltan.major@jku.at (Z. Major), reinhold.lang@jku.at (R.W. Lang).
1350-6307/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.engfailanal.2009.08.004
702
mal and non-isobar test conditions. The overall RGD process is described by Briscoe et al. [1], Derham and Thompson [2],
Stewenson and Morgan [3] and Seregely and Schunck [4] for elastomers and by Lorge et al. [5] for a thermoplastic polymer
with many different aspects. More specically, the gas permeability and diffusivity problems are described and discussed by
Klopfer et al. and Filus et al., [6,7] and the cavitation process analyzed along with a simple solution among others by Chao
and Gent [8]. Recently, a novel model was proposed by Volokh [9] and simulations were performed on cavities in hydrostatic
tension applying the softening hyperelasticity theory and a coupled approach for modeling thermo-mechanical loading in
gaseous environment was developed by Rambert and Grandidier [10]. Furthermore, a novel instrumented test was recently
developed by the authors group and several elastomer grades were characterized regarding to their rapid gas decompression
failure behavior [11,12]. Moreover, it was early recognized that fracture mechanics concepts and methods can provide an
effective tool for characterizing the rapid gas decompression failure process as described by Briscoe and Savvas [1], Derham
and Thompson [2], Lakes [13], and Medri and Strozzi [14]. In spite of these signicant efforts, hardly any accurate description
of the fast crack growth process was found and no material parameters in terms of fracture toughness (Gc, Jc or CTOD) are
available for both material development and for design efforts. Hence, the objective of this paper is to characterize the crack
initiation and crack growth behaviour of two selected RGD relevant elastomer grades over a wide deformation rate range
using pure shear fracture specimen and to derive appropriate fracture toughness parameters.
2. Experimental
2.1. Materials and test specimens
Two elastomer types, a hydrogenated nitrile rubber (HNBR) and a uorelastomer type (FKM) were selected for these
investigations. The compounds were produced with a nominal hardness of 85 5 SHA by the company partner (SKF Economos GmbH, Judenburg, Austria) and provided for the investigations as cylindrical specimens with a nominal diameter of
10 mm and height of 25 mm and as faint waist pure shear (FWPS) test specimens. Furthermore, the nominal stressstrain
diagrams of both materials both for an unloaded case and after pressurization are shown in Fig. 1a and b. Moreover, scanning
electron microscopy images of both materials are shown in Fig. 1c and d. It is clearly seen that in spite of the exactly same
nominal hardness values, both the microstructure and the macroscopic deformation behavior of these compounds are signicantly different. More controversially, both materials revealed a very similar rapid gas decompression failure performance in the rst experiments [11,12].
R smax
T Wh0
Fds
0
BW a
where W is the strain energy density, B is the specimen thickness and (W a) is the remaining ligament length. The critical
tearing energy, Tc was dened as the peak load tearing energy, Tp and it was determined at the peak load value. The loading
rate was dened as the velocity of the actuator and a nominal strain rate (far eld) was calculated using this loading rate
divided by the nominal gage length of the specimen (h0 = 16 mm).
In addition to the conventional global forcedisplacement measurement, optical, non-contact devices (Aramis, GOM,
Braunschweig, Germany) and an IR-thermography testing system (CEDIP Infrared Systems, Paris, France) were also applied
for characterizing the crack tip and the ligament deformation behaviour. The complete test system (testing machine, Aramis
703
40
H-ECORUBBER - HNBR
T=23 C
30
virgin O-ring
20
pressurized O-rings
10
40
O-ringTensile Test
ECORUBBER 2 - FKM
T=23 C
30
20
virgin O-ring
10
pressurized O-ring
0
0
0
50
100
150
200
250
300
350
nominal strain , %
50
100
150
200
250
300
350
nominal strain , %
Fig. 1. Structureproperty relationship for the two elastomer grades investigated; Nominal stressstrain curves of virgin (unloaded) and pressurized/
depressurized O-rings, (a) HNBR and (b) FKM; SEM images with a magnication of 5000; (c) HNBR and (d) FKM.
and thermo-camera system) is shown in Fig. 4. The Aramis system uses the digital image correlation technique and both the
local deformations can be measured and 2 or 3-dimensional full-eld strain analysis can also be performed. While an excellent overview of the image correlation technique is given by Sutton and co-workers [16] the details of the procedure used in
our experiments are described by Feichter et al. [17] and by Jerabek et al. [18]. As the digital image correlation system applied here has a maximal image acquisition rate of 8000 frames/s with reduced resolution (512 256) and about 500
frames/s with full (1024 1024) resolution, the rapid crack propagation can be followed and recorded with sufcient quality
for further analysis.
Furthermore, multiple parameter crack growth resistance curves (T Dc) for various elastomer types under monotonic
test conditions were determined over a wide loading rate range. The crack length, c was measured by the Aramis system
from the edge of the specimen to the crack tip in the crack plane and the actual crack growth rate, dc/dt was also calculated.
Due to the continuous measurement of the crack length the actual cross section can be calculated. Hence, the tearing energy
was calculated based on true (actual cross-section) stress values. Moreover, the crack tip opening angle; CTOA was dened at
1 mm distance from the actual crack tip to the specimen edge between two secant lines on the crack contour. The results of
the fracture experiments are also analysed based on the crack growth kinetics (dc/dt c curves) and crack tip opening angle
vs. crack extension (CTOA Dc) curves.
Finally, to gain more insight into the real local material behavior under complex loading conditions full-eld strain and
temperature measurements were performed both in the near crack tip and in the far eld in the specimen ligament and the
strain distribution is depicted in Fig. 5a. Although, the full-eld strain analysis did not always work perfectly on the contour
edge of the crack, the maximal crack tip strain, ect
max was realistically estimated. In addition to the tearing energy derived from
global forcedisplacement data, the knowledge of local strain makes the determination of local strain or local strain energy
based fracture parameters possible [17].
704
Fig. 2. Volume change of round bar test (RBT) specimen and the appearance of the crack in autoclave; (a) original state, (b) compression phase (saturated),
(c) decompression phase (maximal volume strain) and (d) crack appearance.
Fig. 3. Specimen conguration and test set-up for bulk elastomer fatigue tests; (a) test system, (b) xture and (c) FWPS test specimen with initial notch.
The temperature and temperature distribution across the specimen was measured by the thermo camera. The crack tip
temperature of FWPS specimen is shown at the moment of maximum load and at about 1 s1 nominal strain rate in Fig. 5b
for HNBR. As expected, high strain and temperature gradient was observed in the vicinity of the crack tip. These strain and
temperature gradients depend on the crack length and reveal also pronounced loading rate dependence. In addition to the
gradient a higher temperature crack layer was also observed. Further details to this phenomenon and about the possible
characterization methods can be found at Chudnovsky and Moet [19] and at Persson and Brener [20] and will also be described in a future work by the authors.
3. Results and discussion
The change of the test parameters (pressure, p and temperature, T) and the volumetric deformation, DV behaviour of a
cylindrical test specimen is shown in Fig. 6 during an instrumented RGD test. While the overall process is shown in
Fig. 6a, the pressurization process is shown in Fig. 6b and the depressurization in Fig. 6c in an enlarged time scale. In the
pressurization phase a moderate increase of the material volume was observed up to the saturation (up to about 40% volume
705
Fig. 4. Test set-up with full-eld strain and temperature analysis systems.
Fig. 5. Strain and temperature distribution of a FWPS specimen at the crack tip and in the ligament; (a) the vertical strain, y component and (b) the
temperature prole is depicted.
expansion) until 250300 min. After the pressure release a sudden increase of the specimen volume up to very high volumetric strain was observed in a short time (from 40% to 500% in 30 s, compare Figs. 1c and 6c). Furthermore, the due to
the crack initiation the volume increase was stop and a sudden decrease of the volume was detected (compare Figs. 1d
706
600
300
250
500
200
400
150
300
100
50
200
100
volume expansion V, %
pressure p bar
temperature T, C
0
0
200
400
600
800
1000
1200
1400
time t, min
90
compression
80
70
250
60
200
150
50
40
30
100
20
10
50
350
600
300
volume expansion V, %
500
explosion
250
200
150
decompression
50
100
150
time t, min
200
250
300
200
100
100
50
0
-10
300
400
volume expansion V, %
300
pressure p bar
temperature T, C
100
350
pressure p bar
temperature T, C
0
0
1359,0
1359,5
1360,0
1360,5
1361,0
time t, min
Fig. 6. The change of the test parameters and the size of the round bar test specimen during an instrumented RGD test; (a) the complete test sequence, (b)
pressurization phase and (c) decompression phase.
and 6c after 1360 min). Moreover, the chamber temperature was not constant but rst decreased with the pressure and than
increased after the crack initiation. This is associated with the adiabatic heating during the fast deformation process.
Based on these diagrams and images depicted above (see Fig. 1) the entire process can be analyzed in detail. Due to the
rapid pressure decrease the gas solved in rubber expands and tries to move from the bulk to the free surface of the rubber.
During this process a very high degree of volumetric deformation of the elastomer was observed and simultaneously
decreasing chamber temperature was recorded. The possible locations of the crack initiation are; (i) rubber matrix/ller
interface and (ii) the space between particles where the matrix is highly constrained. A detailed comparison of RGD behaviour of the elastomers along with scanning electron microscopy images of the fracture surfaces after RGD test is provided by
Schwarz et al. [12].
As the autoclave experiments are very time consuming and expensive, efforts were made to characterize the elastomers
by fracture mechanics methods on the laboratory specimen scale.
3.1. Determination of single fracture parameters using loaddisplacement data (global measurements)
Global loaddisplacement curves at two testing rates are shown in Fig. 7a for the HNBR compound. First, single parameter
fracture toughness values in terms of tearing energy were determined at the peak load, Tp. Both compounds revealed distinct
rate dependence, with increasing loading rate continuously increasing peak tearing energy values, Tp were observed for both
elastomer grades (see Fig. 7b) with moderate date scatter (about 15%). Furthermore, as it is seen in Fig. 7b no signicant difference between HNBR and FKM was obtained. This is may be due to the fact that at about 100% strain similar stress values
were observed in the nominal stressstrain diagrams for both compounds (compare Fig. 1a and b). Hence, further experiments were performed and local parameters related to the crack tip deformation and crack growth were derived and discussed below.
707
2500
HNBR
100 mm/s
2000
load F, N
1500
10 mm/s
1000
500
60
50
HNBR
FKM
40
30
20
10
0
-10
10
20
10-1
30
100
101
102
103
104
displacement s, mm
Fig. 7. Single parameter fracture tests; (a) loaddisplacement curves and (b) loading rate dependence of peak load tearing energy, Tp for HNBR and FKM.
200
b
ct ,
150
100
50
FKM
HNBR
0
10 -2
10 -1
10 0
10 1
10 2
10 3
50
45
40
35
30
25
20
10-2
FKM
HNBR
10-1
100
101
102
-1
Fig. 8. Nominal strain rate dependence of (a) the maximal strain at the crack tip, max ct and (b) the max crack tip temperature, Tp. ct.
103
708
observed at signicantly lower crack length values (from 5 to 15 mm) for FKM. This difference is assumed to be associated
with the different crack tip deformation and crack growth initiation process for the two elastomer grades.
Moreover, the kinetics of the crack growth was also analysed and the crack growth rate, dc/dt was calculated based on the
video sequences. The crack length and loading rate dependence of the crack growth rate is shown in Fig. 10a for HNBR and in
Fig. 10b for FKM. While a constant increase of the crack growth rate with increasing crack length with similar slope at all
loading rates was observed for HNBR, signicant changes are seen in the same curves for FKM. It is assumed that the crack
growth is continuous in the pure shear specimen for HNBR and contrary to this, it is discontinuous for FKM with crack deceleration and acceleration phases. Latter phenomenon (crack jumping) is associated with the crack tip blunting and sharpening process. Considering the real RGD loading situation where the gas expansion induces a stress controlled loading with
high loading rates, this could be a disadvantageous property for the FKM grade.
Furthermore, the crack tip blunting was also analyzed during the crack growth. A crack tip opening angle value, CTOA was
dened and CTOA values were determined for all test conditions. The loading rate dependence of CTOA values is shown in
Fig. 11a for HNBR and in Fig. 11b for FKM. While the CTOA value remains nearly constant during the crack growth process
and reveals only small rate dependence for HNBR, signicant and with increasing loading rate increasing changes of the CTOA
values were observed for FKM (see Fig. 11b). This higher strain rate dependence of FKM is in good agreement with the observation shown in Fig. 8a.
The nominal strain rate dependence of the CTOAmax values at the maximal crack length are plotted in Fig. 12 for both elastomer grades. While the CTOAmax values revealed a small decrease with increasing strain rate for HNBR (about 20%) a signicant decrease was observed for FKM (more than 100%). Furthermore, the rate dependence of CTOAmax is opposite as it
was observed for peak load tearing energy, Tp values (compare Fig. 12 with Fig. 7b). It was assumed, however, that this tendency corresponds to and describe more realistic the crack initiation process observed in the autoclave experiments.
60
50
40
30
20
HNBR, v= 1 mm/s
HNBR, v= 10 mm/s
HNBR, v= 100 mm/s
HNBR, v= 500 mm/s
10
peak load
Tearing Energy
0
0
10
20
30
40
50
60
40
30
20
FKM, v= 1 mm/s
FKM, v= 10 mm/s
FKM, v= 100 mm/s
FKM, v= 500 mm/s
10
peak load
Tearing Energy
0
0
50
10
crack extension c, mm
20
30
40
50
crack extension c, mm
Fig. 9. Loading rate dependence of crack growth resistance curves and the location of peak load tearing energy, Tp values for; (a) HNBR and (b) FKM.
10 6
10 5
10 4
10 3
10 2
10 1
10 0
106
FKM
FKM
FKM
FKM
105
(v=
(v=
(v=
(v=
1 mm/s)
10 mm/s)
100 mm/s)
500 mm/s)
104
103
102
101
100
10 -1
0.1
10
crack length c, mm
100
1000
0.1
10
crack length c, mm
Fig. 10. Crack length and loading rate dependence of crack growth rate, dc/dt for; (a) HNBR and (b) FKM.
100
1000
709
140
120
b
crack tip opening angle CTOA,
HNBR
100
80
60
40
v= 1 mm/s
v= 10 mm/s
v= 100 mm/s
v= 500 mm/s
20
0
0
10
20
30
40
140
FKM
120
100
CTOAmax
a
crack tip opening angle CTOA,
These crack tip deformation processes are schematically summarized in Fig. 13 for both elastomers investigated. The
crack tip blunting is uniform during the entire crack growth process and remains the same over the loading rate range inves-
80
60
40
20
v=
v=
v=
v=
50
10
20
30
40
1 mm/s
10 mm/s
100 mm/s
500 mm/s
50
crack length c, mm
crack length c, mm
Fig. 11. Loading rate dependence of the crack tip opening angle, CTOA for; (a) HNBR and (b) FKM.
140
120
100
80
60
40
20
FKM
HNBR
0
0.1
10
100
Fig. 13. Schematic representation of the crack tip deformation process with increasing crack length for both elastomer grades (FKM and HNBR)
investigated.
710
tigated for HNBR elastomer. This results in a continuous crack growth and in a uniform crack growth rate prole. In contrary
to this, the degree of the crack tip blunting changes during the crack growth process for FKM grade elastomer. The variation
of blunted and sharpened crack tip results in continuous and discontinuous crack growth for FKM. Finally, the kinetics of this
continuous and discontinuous process highly depends on the global loading rate of the specimen.
711
Acknowledgement
The research work for this paper was performed at the Polymer Competence Center Leoben GmbH (PCCL, Austria) within
the framework of the Kplus-programs of the Austrian Ministry of Trafc, Innovation and Technology with the contributions of
the University of Leoben as scientic partner and the SKF Economos (Judenburg, Austria) as company partner. The PCCL is
founded be the Austrian Government and the State Governments of Styria and Upper Austria. Special appreciation goes
to Mr. Klaus Lederer for performing the majority of these tests and data reduction in his M.Sc. Thesis and for efciently supporting us during the project work. The additional technical support from Dr. T. Schwarz, M. Moitzi and M. Mitterhuber (SKF
Economos) is also gratefully acknowledged.
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