FEATURE

A study of the factors that

affect extrusion resistance
of elastomers
Peter Warren, Stephen Winterbottom and Andrew Douglas, James Walker &
Co Ltd, Cockermouth, UK

This article describes a simple method for evaluating extrusion resistance, and The “Rizla effect” is normally associated with
studies fluorocarbon and hydrogenated nitrile rubber compounds at differ- a continuous application of pressure and most
ent temperatures and extrusion gaps. It also considers any correlation between often occurs with O-rings (or other designs that
standard laboratory test data and failure conditions. Having benchmarked those may rotate in a housing). Here the seal is forced
elastomers which use ‘‘conventional’’ compounding technology, modifications into a clearance and with time literally unwinds
are made to improve their performance using a number of techniques. Finally, into that clearance (hence the “Rizla effect”).
an assessment of the maximum extrusion resistance that may be expected from
an elastomer at elevated temperatures, while maintaining a balance of elasto-
meric properties, concludes this article. Test equipment
Although there are numerous test methods which
have been used over the years, we decided to
The extrusion of elastomeric seal mate- itself in various forms and is normally evident concentrate on testing O-rings in a jig designed to
rial occurs through creep and/or by fracture. on the low-pressure side unless, for example, emulate the type of failure found in the field.
Materials with poor set characteristics tend to chemical swelling or thermal expansion has While this is based on earlier work at James
initially creep into the gaps while those with occurred. Classic extrusion into a small clear- Walker, our test-rig design (Figure 2) for testing
good set properties are more likely to suffer ini- ance occurs over medium-to-long periods and this extrusion resistance is similar in principle to
tial damage from the edge of the gap. results in lace-like debris (Figure 1). that used by Halliburton for its evaluations.[2]
The forces applied in application can be Extrusion may also happen catastrophically This arrangement has narrow lands and large
considerable. Hertz[1] states: ‘for viscoelastic over a localised portion of the seal, through spill areas in order to exaggerate the process
materials such as rubber, there is a stress ampli- sudden failure of portions of any anti-extrusion and do not allow extruded material to hinder
fication factor that causes local concentrations device, or because of housing dilation at high further extrusion.
well in excess of the mean applied stress’. pressures, causing the clearance to increase. As this work was primarily initiated to
Although back-up rings and other elements Nibbling damage is normally observed when understand materials it was felt that this par-
are often used to reduce extrusion to a mini- pressure cycling occurs. When system pressure ticular design would enable us to readily distin-
mum, it is preferable to use a material with is applied the housing “lifts” or “dilates” caus- guish between compounds. For this reason the
good resistance to extrusion damage whether or ing the clearance to increase. A nub of rubber pressure values quoted will not be fully repre-
not back-up rings are used. extrudes into this clearance and is subsequently sentative of application.
Extrusion damage occurs when housing clear- “nibbled” off when the pressure is dropped and The extrusion testing can be controlled man-
ances are too large or when a seal, which has the clearance is reduced. ually or by a computer. This is a modified ver-
either no or inadequate anti-extrusion elements, sion of one of our existing test rigs – the only
is forced into or through a clearance. This may change being the test block that is used.
be observed around the whole circumference of For ease of use the test block employed
a seal or may be limited to a portion of a seal a bobbin Figure 3 with two ports in the
where housing offset has occurred. It manifests housing for the oil. This bobbin enables

Figure 2. A cutaway view of the test rig

Figure 1. A classic case of ‘lace’ extrusion. showing the extraction device. Figure 3. The test bobbin containing a failed seal.

7
July 2012 Sealing Technology
 FEATURE
O-rings (50-329) with an inside diameter of
50.17 mm and a section diameter of 5.33 mm
to be used. Furthermore, a simple screw meth-
od was employed to enable easy fitment and
extraction of the bobbin.
The control system enables us to ramp up to
a specific pressure, hold that pressure for a fixed
time and then repeat at a selected pressure incre-
ment, or to continuously ramp at a set rate. The
system also enables a fixed pressure to be applied
with or without ramping. The pressure within
the test block is monitored and can be plotted
against time to produce charts that show pres-
sure, and any drop in pressure, during testing.
The extrusion gaps employed were 0.4 mm and
0.8 mm (0.2 mm and 0.4 mm radial clearances).
Although these gaps may be considered large by
industry standards, they were chosen to demon-
strate the material characteristics rather than give
application values. Two temperatures – 100°C
and 150°C – were initially chosen, although later
work will examine lower and higher temperatures.
Figure 4. Chart of extrusion failure pressures at 100°C.
Figure 5. Chart of extrusion failure pressures at 150°C.
8
Sealing Technology
Fluoroelastomers (FKMs) and hydrogenated
nitrile rubbers (HNBRs) were evaluated – com-
pared with each other and within each family.
Test method
The rings were fitted to the bobbin and the out-
side of the seals was lightly lubricated with the
test oil (Shell Heat Transfer Oil S2). The bobbin
was loaded into the block, sealed and oil intro-
duced at minimal pressure. After ensuring there
was no air trapped within the system, the block
(seated on a heated platen) was allowed to stabi-
lise at the test temperature for an hour.
For our material evaluations it was decided to
gradually ramp the pressure at a rate of 40 bar
per minute. This was a large screening exercise
and it is likely that a hold time at incremental
pressures will be used for future evaluations
when time is less restrictive.
The pressure was increased until a significant
pressure drop occurred. At this point the rig
was cooled, dismantled and the seals examined.
Although this drop may be the end of the test-
ing, the charts may indicate when the failure
begins – by showing a series of small pressure
drops earlier.
An initial test run was normally followed by
two replicates to give three data points under
each set of conditions.
Extrusion resistance
of FKMs
Bisphenol cures
Initially we tested a bisphenol-cured 90 hard
material which has a long history of use in appli-
cation. This had median failure values of 588 bar
(0.4 mm gap) and 369 bar (0.8 mm gap) at
100°C. At 150°C the results were 290 bar and
202 bar, respectively. This gave us our initial
points of reference for further developments.
Readers will notice the high level of consist-
ency in failure pressure between test runs. A
similar level of consistency prevailed through-
out the remainder of the test programme.
In order to establish the effect of filler, the
level was increased dramatically in this com-
pound and this was then tested in comparison.
The cure rate was similar to that of the stand-
ard product and sample rings were moulded
under the same conditions and given the same
post bake. The material was made stiffer, by
the addition of filler, and harder, with 50%
modulus increase, from 4.30 MPa to 6.10 MPa.
Tensile strength, however, was reduced and
elongation at break dropped to less than 100%.
As can be seen from the charts in Figure 4 and
Figure 5 the addition of filler increased extrusion
resistance, but this was especially evident at the
lowest temperature and narrowest gap.
The improvement was in the order of 64%
for the 0.4-mm gap at 100°C, but only 33% at
0.8 mm. The physical properties are dramati-
cally reduced when such a high level of filler is
used. However, a moderate increase in filler level
may increase stiffness and reduce creep without
compromising processing or final properties.
Improvement in extrusion resistance may be less
evident with smaller increases, but this improve-
ment still may be significant at perhaps 20%.
Peroxide cures
Our next task was to look at the comparative
values for peroxide-cured polymers. These were
more extrusion resistant than the bisphenol-
cured compound at both gaps and both temper-
atures. The results (Figure 6) for these materials
were similar despite using different polymers and
quite different formulations. However, the results
July 2012
 FEATURE

are significantly better than those obtained from

the bisphenol-cured compound.
To complete the picture, a batch of low-
temperature peroxide-cured FKM (Figure 7)
was made using the terpolymer formulation
and substituting the polymer. Using the same
polymer with minor changes to cure and filler
gave a slight improvement in extrusion resist-
ance over the standard formulation.
There are a variety of peroxide-cured poly-
mers available and compounds were mixed
using both high fluorine and high fluorine,
low-temperature grades. These gave similar
results to the previous polymers although no
effort had been made to optimise the formula-
tions for extrusion resistance.
All the compounds included in the chart in
Figure 8 are 90 IRHD nominal. Actual values
range from 87 to 92. The extrusion resistance, Figure 6. Chart of extrusion failure pressures at 150°C.
however, does not directly relate to specific
hardness in this evaluation. Tear strengths for
bisphenol and peroxide grades both at 23°C
and 100°C were similar.
Elongation of 50% and 100% reveal that
while modulus values for varying formulations
within a polymer type do show a trend in line
with extrusion resistance, for different polymers
this does not apply.
As mentioned by Halliburton,[2] Aflas FKM is
a classic example of a material with high modu-
lus, but poor extrusion resistance (Figure 9, on
page 10). We confirmed its findings as part of
our evaluations.

Extrusion resistance
of HNBRs
Although not as good as peroxide-cured FKMs
at a lower temperature the resistance of HNBRs Figure 7. Chart of extrusion failure pressures at 150°C
does not decay as much at a higher temperature
(Figures 10 & 11, on page 10).
Again the resistance seems to be polymer
dependent. The modulus does not coincide
with resistance.
As with the FKMs, an increase in the filler
level will increase extrusion resistance. As
increasing the filler level further would not give
satisfactory dispersion in the HNBR, the com-
parison used involved a reduction in black level.
As expected, the 90 hard material was sig-
nificantly better than the 75 hard material, but
again this was most evident at the smallest gap
and lowest temperature.

Cross-link density
It is well known that shear modulus increases
as the distance between cross-links is reduced.
This is obviously both polymer-related and
Figure 8. Chart of extrusion failure pressures at 150°C
cure-related.

9
July 2012 Sealing Technology
 FEATURE

Increasing cross-link density has a significant

effect on physical properties, but the optimal
density for one property may be very different
to the optimal density for another.
A balancing act rather than compromise is
required. The ultimate aim is to produce mate-
rials that will resist extrusion in application, but
there is no single physical test which will show
this ability. The evaluation has shown that it is
dependent on the choice of polymer first and
then the optimisation of both cure and fillers to
“toughen” the material. But what is toughness?
It has been defined in various ways such as
“resistance to crack initiation plus resistance to
crack propagation” and “the ability of a mate-
rial to absorb energy and plastically deform
without fracturing”.
Gordon[10] states: “The worst sin in an
engineering material is not lack of strength or
Figure 9. Chart of extrusion failure pressures at 100°C plotted against modulus values at 23°C.
lack of stiffness, as desirable as these properties
are, but lack of toughness, that is to say, lack of
resistance to the propagation of cracks”.
When considering extrusion resistance, key
factors for consideration are hydrostatic com-
pression and shear, therefore conventional wis-
dom does not apply.[4,5] For the highest tear
resistance it is accepted that cross-link density
should be as low as illustrated in Figure 12.
This, however, does not apply for tear resist-
ance in compression.
A material that has been optimised for tough-
ness may be improved further by cure and post-
cure conditions. However, this improvement
has limitations and can only make marginal
improvements to a well compounded material.
Selecting an HNBR compound that is usu-
ally post cured and testing it with and without
post cure does show a reduction in extrusion
resistance for the latter of about 17% at 100°C
Figure 10. Chart of extrusion failure pressures at 100°C. and 23% at 150°C. It should be noted, how-
ever, that this decrease is of the same order at
both temperatures and both extrusion gaps in
contrast to increasing filler levels. A formula-
tion which is specifically compounded so that it
does not need a post cure would not, however,
improve significantly if it were to be given one.
Just simply increasing cross-link density does
not result in a significant improvement. While
some properties increase others decrease. Taken
too far, the increase in cross-link density will
tend towards brittleness, especially at elevated
temperatures, and in some cases results in a
dramatic drop in resilience.
It is known, however, that increasing cross-
link density does reduce the creep of rubbers
and it is likely that part of the extrusion resist-
ance is enhanced.[7]
This work also concluded that creep was
not directly related to stiffness, hardness or
resilience, but was most closely related to
Figure 11. Chart of extrusion failure pressures at 150°C.
compression set.

10
Sealing Technology July 2012

Figure 12. Graphical representation showing the influence of cross-link density on given
properties (A.Y. Coran[6]).
From an extrusion resistance principle, our
evaluations suggest that a poor set is likely to give
poor extrusion resistance. However, it does not
mean that an outstanding compression set result
will lead to outstanding extrusion resistance.
Other reinforcements
In order to understand the effects of using other
reinforcements, an HNBR compound was mixed
in three versions in the laboratory. These were
a standard version, one with multi-wall carbon
nano-tubes and another using an Aramid powder.
The addition of these materials was at 10 phr
(5%), and dispersion was satisfactory at this level.
The use of these reinforcing materials
increased the modulus, but also severely reduced
elongation. We believe that using a higher level
would have compromised use in application.
In effect, there was no improvement in resist-
ance to extrusion and a small decrease was
observed. This may be related to a tendency
towards brittle failure or orientation.
Summary
UÊ ÝÌÀÕȜ˜ÊÀiÈÃÌ>˜ViʈÃʘœÌÊi>ÃÞÊ̜ÊiÃ̈“>ÌiÊ
using conventional laboratory tests. However,
it may be possible to discount certain materials
based on such tests. Our test and others like it
give a better understanding and do enable pre-
dictions with some confidence to be made.
UÊ / iÊ«œÞ“iÀÊ>««i>ÀÃÊ̜ÊLiÊÌ iʓ>ˆ˜ÊVœ˜Ãˆ`-
eration in obtaining good performance. The
reason why particular polymers are better or
worse than others has not been fully inves-
tigated, but it would appear that it is not
related simply to molecular weight.
UÊ ˜VÀi>Ș}ÊvˆiÀʏiÛiÃÊ܈Êˆ“«ÀœÛiÊÀiÈÃÌ>˜ViÊ
with narrow gaps and lower temperatures,
but it is not sufficient as severity increases.
UÊ / iÊVÀœÃǏˆ˜ŽÊ`i˜ÃˆÌÞÊ>}>ˆ˜ÊV>˜ÊLiÊÕÃi`Ê̜ʓ>ŽiÊ
moderate improvements, but there are limita-
July 2012
tions because of other physical requirements.
UÊ / iÊLiÃÌÊÀiÃՏÌÃÊ>ÀiʜLÌ>ˆ˜i`ÊLÞÊV>ÀivՏÊ
optimisation of the individual ingredients to
maximise their effects.
We had hoped to give an indication of the limits
of a well compounded material under constant
pressure, though will need to quantify this using
a rig which relates more closely to application.
Applying full pressure without ramping
tended to encourage rotation of samples. Such
rotation was not noticeable during the ramped
tests used for this study. We will modify our rig
to avoid this problem before re-evaluating con-
stant pressure effects.
Using ‘‘exotic’’ reinforcements may give bet-
ter results with smaller extrusion gaps, or differ-
ing techniques, although the polymer is still the
main consideration and, therefore, always may
be the limiting factor.
The values obtained from this study are purely
comparative, and operating limits for a given
elastomer will vary according to the conditions
prevailing in a specific application. However,
simple test methods, such as those described,
do enable materials to be selected that will offer
improved performance when assessed under con-
ditions replicating field operation.
Acknowledgements
The authors would like to extend their thanks
to Paul Bowman, Duncan Smith and James
Wilkinson for the design of the test rig, and
provision of extrusion test data.
References
1. Hertz Jr, D.L., Mechanics of Elastomers at
High Temperatures, presented at the High
Temperature Electronics and Instrumentation
Seminar, Houston, Texas, USA, 3–4
December 1979.
FEATURE
2. Slay, B., (Halliburton), Seal System Testing
for High Performance Completions, Oilfield
Engineering with Polymers Conference 2008.
3. Gordon, J.E. ‘The New Science of Strong
Materials – or Why You Don’t Fall Through
the Floor”, Penguin Books, 1968.
4. Bridgman, P.W., ‘The Physics of High Pressure’,
G. Bell and Sons Ltd, London, UK, 1949 and
‘Studies in Large Plastic Flaw and Fracture’,
McGraw-Hill, New York, USA. 1952.
5. Lindsey, G.H., ‘Hydrostatic Tensile Fracture
of Polyurethane Elastomer’, California
Institute of Technology, USA. 1966.
6. Coran, A.Y., chapter entitled Vulcanisation,
in ‘Science & Technology of Rubber’,
Academic Press, New York, USA. 1978.
7. Creep Phenomena (chapter 6), ‘The Services
Rubber Investigations: Users Memoranda’,
1954.
Contact:
Peter Warren, James Walker & Co Ltd, Cockermouth,
Cumbria CA13 0NH, UK. Tel: +44 1900 898277,
Email peter.warren@jameswalker.biz,
Web: www.jameswalker.biz
(Peter Warren has been in the sealing industry
for over 33 years. As well as being a Fellow of the
Institute of Materials, Minerals and Mining he is
also a chartered scientist. His current role is head
of Materials Engineering at James Walker & Co
Ltd where he leads a team of 12 highly qualified
scientists, technologists and technicians.)
This feature – by Peter Warren, Stephen
Winterbottom and Andrew Douglas – is
based on a paper entitled ‘Extrusion resist-
ance of elastomers: a study of factors that
affect performance’, which was presented in
Aberdeen, Scotland, UK, on 17–18 April at
this year’s High Performance Elastomers and
Polymers for Oil & Gas Applications confer-
ence that was organised by iSmithers, part of
Smithers Rapra Technology Ltd.
Contact:
Helen Charlesworth, Conferences, Smithers Rapra
Technology Ltd, Shawbury, Shropshire SY4 4NR, UK.
Tel: +44 1939 250383, Fax: +44 1939 1118,
Email: hcharlesworth@ismithers.net,
Web: http://info.smithersrapra.com
Editor’s comment: Also see the interview with
James Walker’s Peter Warren and the feature
entitled ‘Achieving RGD resistance to meet
current oilfield needs’ which appear in Sealing
Technology March 2012, pages 8–9 and
October 2011, pages 9–12, respectively.
11
Sealing Technology