Damage of Optical Fibers Under Wet Environments

R. El Abdi & A.D. Rujinski & M. Poulain & I. Severin

Received: 26 July 2009 / Accepted: 19 October 2009 / Published online: 6 November 2009
# Society for Experimental Mechanics 2009
Abstract Besides signal transmission for telecommunica-
tions, fibers are used in an increasing number of devices. A
number of applications relate to devices exposed to severe
wet environment (hot water, chemical attacks). It is the
case for the sensors used in nuclear plants, high energy
physics or plasmas devices. However, reliability issues
must be addressed for optical fiber sensors operating under
severe conditions such as harsh chemical solutions. The
purpose of this work is to study the mechanical behavior
and aging of fibers exposed to hot water action, to
hydrofluoric acid vapours (HF) and to tetramethoxysilane
(TMOS) for different durations. Dynamic fatigue tests were
implemented using a two-point bending testing device or
tensile test set-up. Standard fibers tested immediately after
exposure show a broader distribution of fiber strength
accompanied by the drastic decrease of the failure stress. In
some particular cases, the gain compared to as received
fibers can be positive. Polymer reacts with different wet
environments, which induces viscosity changes. This is
consistent with SEM observations.
Keywords Optical fibers
.
Aging
.
Epoxyacrylate coating
.
Severe environments
.
Fiber strength
Introduction
The availability of silica fibers enlarges the field of the
possible applications [1]. Passive and active applications
were foreseen at the early stage of development of fiber
optics [2]. A large group of applications encompasses
optical fiber sensors, remote chemical analysis, thermal
measurements and thermal imaging, reflectometry, optical
instrumentation and also laser power delivery. Most
medical applications of fibers, with their specific require-
ments, are related to this group. They could expand very
significantly when technologic progress will lead to
disposable fibers at reduced cost.
Active fibers are doped fibers from which laser effect
or amplification may be obtained. The large interaction
length of the fiber and the high energy density which may
be used for optical pumping are the main features
supporting the development of the active fiber devices.
Another attractive point is the possibility of generating
short wavelength signals using IR laser diodes as pump
sources. Powerful laser fibers may be built in this way
with a very good beam quality, which is more difficult to
achieve in semiconducting lasers. Cost aspects and
reliability still limit the practical applications, but signif-
icant changes are likely to occur in coming years. All
solid state and compact fiber lasers could replace the large
and noisy gas lasers.
Choosing the optimum optical fiber for a specific use
may be an obvious task or a subtle exercise of balance
between various parameters: attenuation, reliability, toxic-
ity, availability and cost. Fibers from different materials can
be used depending on choice criteria.
Silica fibers offer a set of unique advantages: lowest
attenuations, good mechanical and chemical resistance,
transparency range extending from 300 nm to 2 m. Silica
fibers for telecommunications are inexpensive but price
R. El Abdi (*)
:
A.D. Rujinski
:
I. Severin
Laboratoire Larmaur, University of Rennes1, Campus de Beaulieu,
CS 74205-35042 Rennes, France
e-mail: relabdi@univ-rennes1.fr
A.D. Rujinski
:
I. Severin
Politehnica University of Bucharest, Fac. IMST,
313 Splaiul Independentei,
cod 06042 Bucharest, Romania
M. Poulain
Lab. Matriaux Photoniques,
University of Rennes1, Campus de Beaulieu,
CS 74205-35042 Rennes, France
Experimental Mechanics (2010) 50:12251234
DOI 10.1007/s11340-009-9310-1
increases when special size and NA (sinus of the
maximum angle of total reflection at the core/cladding
interface) are needed, requiring to manufacture special
preforms. Special silica fibers have been developed for
UV transmission, either doped with OH or made from
fused quartz.
As a general rule, the life time of the fiber depends mainly
on chemical durability and applied stress. Failure corre-
sponds to breaking which is known to happen as crack
propagation from a surface flaw. Real fibers have surface
flaws resulting from the processing. The initial intrinsic
strength of a fiber is related to chemical composition, and
ultimately to the chemical bond energy. Current values are
4 GPa for silica fibers and less than 1 GPa for fluoride and
sulfide fibers. Initial strength decreases versus time when the
fiber is subject to stress corrosion, or more simply, under a
permanent stress in humid environment. This phenomenon
has been extensively studied in silica fibers [3].
An external polymeric coating is applied to protect fiber
from scratches, to limit chemical attack of water and to
increase mechanical strength. Usual coatings are epoxya-
crylate resins, but other polymers such as silicones and
polyimide may be used. In spite of their hydrophobic
properties, fluorinated polymersPTFE, FEPdo not
make an efficient barrier against hydrolysis and are less
favorable for mechanical properties.
As the main interest of fibers lies in their flexibility, they
will be moved and bent during operation. The minimum
bending radius must be defined. It depends on fiber
material and diameter: It is smalla few millimetersfor
silica fibers, but is larger for fluoride, chalcogenide and
polycrystalline fibers.
The aging of the fibers used for laser transmission also
depends on the evolution of the internal and ends defects
under laser irradiation. Finally this aging effect is mini-
mized if defect density is low enough, and if water
concentration and residual stress are controlled.
Apart from the worsening of the surface flaws, water
has little influence on oxide glasses which are insoluble
and remain transparent. Things are different for some
glasses such as phosphate and halide glasses. The
chemical action of water can weaken the fiber and reduce
transmission if fiber ends and outer surface are corroded.
Direct contact with liquid water has to be avoided and
various solutions have been successfully experienced for
harsh environments.
In practice, optical fiber aging depends on various
factors that may decrease effective fiber strength: applied
stress, temperature, water or chemical solutions. Several
optical fiber manufacturers want to obtain the fiber
behavior submitted to severe wet environment to analyse
the coating reliability and the evolution of the fiber strength
during the fiber life.
The aim of this work is to study the silica optical fibers
behavior when these fibers are in contact with severe
environments such as hot water, exposure to acid vapours
or in tetramethoxysilane solution and to analyze the
strength evolution and the life duration.
Tested Fiber
In this study, the monomode silica optical fibers are used,
and the fiber diameter is equal to 250 m. A fiber silica
core has 125 m in diameter. Two epoxy-acrylate polymer
coatings (0.2 NA Acrylate coupler fibers) with a thick of
62.5 m are used. The epoxy-acrylate coating is the most
used in standard optical fibers. It protects the fiber but it
remains permeable to water. The internal layer is soft with a
low glass transition temperature and is applied onto the
glass fiber surface. It ensures protection against micro-
bending and damping of the external stresses. The external
layer has a higher T
g
and protects the fiber against physical
aggression. To comply with process requirements, the UV-
polymerisation of the acrylate resins is rapidly performed,
in line, and offers an excellent adhesion and a large range of
elasticity (Young modulus).
Hot Water Effects
Aging Testing
Fibers subjected to aging were plunged into large tanks
containing deionised hot-water at 65C and 85C for
different durations ranging between 3 to 70 days. Eighteen
to 20 samples per series, each fiber of 1 meter in length,
were carefully arranged floating into the hot water tanks,
so as to subject no stress and the temperature along them
to be constant all over the aging treatment. After the
envisaged aging duration, the series of aged fibers were
removed from hot water and simply laid to dry into the
laboratory environment on absorbent paper for at least
3 days.
Static Bending Test
The static fatigue parameters were measured by a static
bending test which was implemented accordingly to the
international standard IEC 793 [4]. The aged and subse-
quently dried one meter in length sample fibers were
subjected to bending stresses by winding around an
alumina mandrel with calibrated size in diameter. The
constant level of applied stress can be varied by the proper
choice of the mandrel size. The failure time is measured,
this being the time required for the intrinsic strength of the
1226 Exp Mech (2010) 50:12251234
fiber to degrade until it equals the applied stress through the
proper mandrel diameter. The technique to monitor the time
to failure is the optical detection of the ceramic mandrel
presence in a special holder. Thus, the energy delivered
through fiber breaking pushed out the holder the mandrel,
initially in a vertical stable position, the time to failure
being directly recorded with an accuracy of 1 s. the testing
setup consists of a large number of vats containing 16
holders each.
The testing environmental conditions during static fatigue
measurements have slightly ranged between 18.5 and 20.5C,
in temperature and to 30 to 45% in a relative humidity.
Static Fatigue Testing Results
Optical fiber was wound on alumina mandrel. The applied
stress on the fiber depends on the mandrel diameter accord-
ingly to the Mallinder and Proctor relation [5, 6], as follows:
s E
0
:" 1
a
0
:"
2
_ _
1
where : applied stress (GPa); E
0
: Young modulus (=72 GPa
for the silica); : relative deformation of the fiber; =0.75 ;
with : non-linearity elastic parameter (=6).
The relative deformation of the fiber depends on the
mandrel calibrated diameter, as follows:
"
d
glass
f d
fiber
2
with f the mandrel diameter (in m); d
glace
= d
silica core
=
125 m, the fiber diameter; d
fiber
= 250 m, the fiber
diameter, including the double layer polymer coating.
Fibers were subjected to aging in hot water at 65 and
85C for long durations and then winded on 2.4 mm
diameter mandrel in order to be tested. The use of equations
(1) and (2) leads, in the case of usual telecommunication
fiber, to the corresponding stresses of 3.76 GPa. An
oscillating behaviour for the aging temperature of 65and
85C was noticed (Fig. 1). For the aging temperature of
65C, maximum values exceeding just a few the non aged
failure time (39.22 h for 4 days in hot water as compared to
33.40 h) are noted. For higher aging temperature (85C),
seeming to damage the polymer coating more and more
severely with the aging duration exposure, a drastic
decrease of the failure time may be observed immediately,
with some oscillations around very low failure durations
and very severe decrease when exceeding 50 days of aging.
Structural RelaxationDiscussion
The cyclic evolution of the fiber failure time subjected to
static fatigue was normally unexpected taking into account
the fiber strength decrease induced in time by water
chemical action. This behaviour in static fatigue conditions
may present some practical consequences suggesting that in
a wet environments, in some particular cases (temperature
and exposure duration), the as aged fiber lifetime has
exceeded the expected one, respectively the non aged fiber
failure time.
As already know, the microcracks smoothing due to the
curing effect of water molecules on silica resulted in a
stress intensity factor decrease and thus in a fiber failure
strength increase. But the smoothing effect might not be the
only responsible for an oscillatory process of the fiber
failure time while increasing the aging duration.
Failure time versus aging duration
0
10
20
30
40
0 10 20 30 40 50 60 70
Aging duration (days)
F
a
i
l
u
r
e

t
i
m
e

(
h
o
u
r
s
)
Aged at
65C
Aged at
85C
Fig. 1 Failure time versus aging duration at 65 and 85C
Faceplates
Control
block
Fiber
Piezo
electric
sensor
Stepper
motor

Faceplates
Fiber
d
g
d
f
d
c

d
Fiber
Fig. 2 Two point testing bench
Exp Mech (2010) 50:12251234 1227
The cyclic evolution of failure time versus aging duration in
static fatigue should be explained through the cyclic changes
at the fibers polymer interface due to the structural relaxation.
As previously reported [7], the cyclic evolution was noticed
for longer aging duration, with the first maximum after
3 months of exposure. Our series of experiments have
showed that the oscillatory process appeared for all the tested
fibers inside the as previously reported period too.
The structural relaxation is responsible for the oscillatory
evolution off the fiber failure time versus the aging duration
that means that a hydrated silica layer is formed on the
glass polymer interface, when the fiber is aged in water.
This layer inhibited in some extends, the micro-surface
flaws. In a first phase, this layer retards the water diffusion
towards the glass surface. As the layer grows, the fiber is
reinforced when subjected to static stress, but as containing
water, when the layer reaches a critical thickness, diffusion
through polymer coating tends to decrease the layer
thickness to a minimum value, accelerating the structural
relaxation accompanied by the fiber effective stress de-
crease. So, once the cyclic finishes, a new process initiation
allows the water attack of the glass-polymer interface.
Exposure to Hydrofluoric Acid Vapours
Silica exhibits a remarkable high chemical durability, as
exemplified by an extensive use in chemistry laboratories
for beakers, crucibles and reaction tubes. However it has
been demonstrated that silica is sensitive to environmental
action, including water, but also methanol and other
reagents, through the classical stress corrosion phenome-
non. Considering the numerous application fields of the
optical fibers, one may wonder to what extent more
aggressive chemical reagents may influence mechanical
reliability.
This is the case for very alkaline and fluorinating media
[8]. Silica is quite stable in most acids and, as an example
immersion into hot sulphuric acid is used for polymer
coating stripping [913]. While surface flaws may be easily
induced on the pristine fiber once the polymer coating is
removed, fiber strength is not much affected by this acid
etching if fiber is handled properly [10]. On the contrary,
fluorinating reagents severely attack silica [14], the intense
reaction between silica and hydrofluoric acid being largely
used in electronics.
The merged effects of stress corrosion and chemical
damage are studied hereafter. For this purpose, fibers have
been exposed to fluorinating reagents, and their mechanical
strength has been compared to that of untreated fibers.
Experimental Procedure
Chemical attack by hydrofluoric acid vapours (HF)
Series of 30 samples of 20 cm in length were carefully
arranged on a rigid bar and their upper extremity pasted
with adhesive tape. This bar was exposed to hydrogen
HF exposure, testing immediately
0
20
40
60
80
100
7 7.5 8 8.5
ln (F, MPa)
F
a
i
l
u
r
e

c
u
m
u
l
a
t
i
v
e

p
r
o
b
a
b
i
l
i
t
y

(
%
)
15 min
45 min
90 min
60 min
120 min
150 min
non-aged
Fig. 3 Weibull plots recorded from fibers exposed to HF vapours for
different times (in min) and tested immediately
HF exposure, dried 3... 5 days
0
20
40
60
80
100
7.8 8 8.2 8.4 8.6 8.8
ln (F, MPa)
F
a
i
l
u
r
e

c
u
m
u
l
a
t
i
v
e
p
r
o
b
a
b
i
l
i
t
y
(
%
)
15 min
45 min
90 min
60 min
120 min
150 min
Fig. 4 Weibull plots of fibers exposed to HF vapours for different
times (in min) and dried in ambient environment prior to test
Table 1 Physical properties of tetramethoxysilane used product
Chemical name Tetramethoxysilane
Formula C
4
H
12
O
4
Si
Molecular weight 152.22
Boiling point 122C (760 mm Hg)
Flash point 26C
Color and appearance Colorless transparent liquid
Density (25/25C) 1.032
Refractive index 1.3688 (20C)
Min. purity 98.5% by GC
Package 180 kg/drum
1228 Exp Mech (2010) 50:12251234
fluoride vapours produced through the interaction between
40% aqueous hydrofluoric acid (HF) and concentrated
sulphuric (H
2
SO
4
) acid. Sulphuric acid absorbs water and
HF molecules that are less soluble in H
2
SO
4
than in water
go to the vapour phase. The fiber was subjected to gaseous
HF into a transparent hermetic disposal for durations
ranging from 15 to 150 min.
A first series of treated fiber packages was tested
immediately; the second one was dried in air in the
laboratory environment (20C, 3040% RH) for 35 days
prior to testing. Each series consisted in multiple packages
of 30 samples; each package was exposed to HF for
different durations, as previously mentioned. For safety
reasons, the chemical container was put into an extractor
hood.
Dynamic fatigue measurement using a two-point bending
testing apparatus
While bending method does not replace tensile testing as a
fiber strength measurement technique, it presents attractive
features and advantages, providing valuable information
about flaw size distribution [15]. In our case, the ease and
the duration of the testing manipulations and the small
effective length of the fiber sample made the bending test
the most appropriate choice for investigation.
The as-received fibers and those exposed to fluorinated
vapours for different durations (15, 45, 60, 90, 120,
150 min) were put subsequently through dynamic tests
using a two-point bending testing device [16, 17] (Fig. 2).
The fiber package was cut into two parts, leading to
samples of 10 cm in length that were carefully bent and
placed between the grooved faceplates of the apparatus.
Special care was required to avoid the fiber slipping during
the faceplates displacement and to maintain the fibers ends
in the same vertical plan. The faceplates are brought
together by a computer-controller stepper motor which is
halted when the fiber fracture is detected by an acoustic
sensor (Fig. 2). A series of 30 samples were tested for a
faceplate constant velocity of 400 m/s that is a convenient
value for our investigation. The measurements were
performed in the ambient environment (20C, 3040%
RH), temperature and relative humidity being recorded for
each measurement series.
The stress to fracture was calculated from the distance
separating the faceplates. The failure stress was measured
for each fiber, and then the results were treated through a
statistical approach using the Weibull theory.
During the two point bending tests and at breaking time,
the stress applied to the fiber was deduced using the
distance value d between the two faceplates and the relation
defined by Griffioen [18] i.e.:
s E
0
:" 1
a
00
:"
2
_ _
3
The parameter is not equal to of equation (1), but
defined by:
a
00

3
4
a
1
4
4
where E
0
is the silica Young modulus, is the applied
stress (GPa), is a non linearity elastic parameter (=6) and
is the strain in the fiber:
" 1:198
d
f
d d
c
2d
g
_ _
5
0
20
40
60
80
100
1.6 1.62 1.64 1.66 1.68 1.7 1.72 1.74 1.76
Ln (F) (GPa)
F
a
i
l
u
r
e

c
u
m
u
l
a
t
i
v
e

p
r
o
b
a
b
i
l
i
t
y
(
%
)
.
50mm/min AR
50mm/min 4h
150mm/min AR
150mm/mn 4h
300mm/min AR
300mm/mn 4h
500mm/min AR
500mm/min 4h
50mm/min 4d
150mm/min 4d
300mm/min 4d
500mm/min 4d
Fig. 5 Aged fibers during 4 h
(4 h) and during 4 days (4 d) in
TMOS solution (17C) for
different tensile test velocities
(in mm/min)AR means As
Received fibers
Table 2 Median fiber strength for aging in cold TMOS solution (17C) during 4 h for different tensile test velocities
50 mm/min 150 mm/min 300 mm/min 500 mm/min
As received 4 h As received 4 h As received 4 h As received 4 h
Median strength (GPa) 5.038 5.086 5.274 5.368 5.401 5.418 5.442 5.454
Gain
a
(%) 0.95 1.76 0.30 0.21
a
The gain is calculated as the percentage of the improvement of the strength of aged fibers compared to that of non aged fibers
Exp Mech (2010) 50:12251234 1229
where d
f
is the polymer coating diameter, d
c
is the fiber
diameter, 2d
g
is the total depth of the 2 grooves and d is the
distance between the two faceplates (Fig. 2).
The statistical Weibull law gives a relationship between
the probability F of fiber rupture with a length L and the
applied stress :
Ln
1
L
Ln
1
1 F
_ _ _ _ _ _
m Ln s Ln s
o
6
where m is a size parameter and

is a scale parameter.
The evolution of Ln
1
L
Ln
1
1F
_ _ _ _ _ _
(Failure cumulative
probability in (%)) according to Ln(
F
) is called Weibull
diagram (
F
is the failure stress).
Results and Discussions
Fibers in harsh conditions
In previous experiments, the fiber was exposed to a
different fluorinated atmosphere consisting in the vapour
phase originating from heated ammonium hydrogenofluor-
ide NH
4
HF
2
[19]. From the observations gained in this
study, the duration treatment was adjusted to 19 h. The
amount of acids was chosen taking into consideration the
container volume of 2 litres: approximately 5 g of 40%
aqueous HF and 5 ml of 9597% H
2
SO
4
.
After 19 h exposure, fibers appeared extremely damaged
and the colour of the coating turned to brown. Moreover,
treated fibers had lost elasticity and could be bended
permanently, making mechanical tests impossible as no
fracture could be registered.
Further examination showed that glass fiber was largely
or even entirely destroyed, so that the fiber diameter was
close to zero while the polymeric coating remained as an
empty shield.
As this 19 h duration was obviously excessive, shorter
exposure times were applied for the following experiments.
Influence of exposure into hydrofluoric acid vapours
Less severe chemical attack was implemented reducing
exposure time, typically from 15 to 150 min. The dynamic
testing using the two-point bending apparatus (Fig. 2) were
performed (faceplate velocity of 400 m/s).
Various series of fibers were subject to HF attack. After
exposure, some series were immediately tested and some
other series of samples were dried at room atmosphere for
35 days then tested. The resulting Weibull plots (Failure
cumulative probability according to the failure stress
F
)
are shown in Figs. 3 and 4.
As already noticed during previous manipulations and
tests, the fibers exposed to HF vapours were much more
brittle then the non aged fibers (Figs. 3, 4). In spite of great
handling care, more than half of the prepared samples were
lost because they broke. In many cases, just touching the
bench faceplates or trying to bend the fiber to put it in the
bench lead to fiber fracture.
In the case of the standard fibers tested immediately after
exposure (Fig. 3), fiber strength showed a broader distribu-
tion and mean failure stress decreased drastically, reaching
only 50 to 75% of the origin strength. In some case the
distribution was bimodal, meaning that more than one single
type of defects is present on the fiber surface (Fig. 3). Taking
into account fiber position during vapours exposure into the
disposal and the use of one single package for two different
testing, no difference was observed according to the sample
position (upper or lower) along the fiber package. However
the colour change of the polymer coating turning to brown
was more evident for the lower extremity of the package.
During measurements, some handling difficulties due to the
HF absorption into the polymer coating were encountered:
Table 3 Median fiber strength for aging in cold TMOS solution (17C) during 4 days for different tensile test velocities
50 mm/min 150 mm/min 300 mm/min 500 mm/min
As received 4 d As received 4 d As received 4 d As received 4 d
Median strength (GPa) 5.038 5.157 5.274 5.376 5.401 5.479 5.442 5.565
Gain* (%) 2.36 1.91 1.44 2.25
Two
polymer
coatings
Fig. 6 Fracture morphology of as received silica optical fiber (tensile
test velocity of 50 mm/min)
1230 Exp Mech (2010) 50:12251234
apart from acidic smell, fibers left some kind of paste on
apparatus faceplates that had to be cleaned frequently, while
set-up had to be recalibrated. This observation is consistent
with the assumed change of polymer Tg.
It seems that the failure stress
F
increases according to
the exposure time. For a small exposure time (15 min) the
obtained results are not far away from the one of non aged
fibers (Fig. 3). On the other hand, this failure stress rapidly
decreases for 45 min of exposure time, then increases with
exposure time. One has noted many deposits at external
surface of fiber aged during 150 min, and these deposits are
likely to have grown from the vapour phase that contained a
mixture of inorganic species (SiF
4
, HF, H
2
O) and organic
from polymer coating. The involved chemical processes
may be complex and these deposits lead to the increasing of
failure stress in bending test.
Drying prior to test has also led to a broader distribution
of the experimental values of the exposed standard fibers
(Fig. 4) by comparison to the as-received fibers (Fig. 3).
But it was steeper than that of the fibers exposed to HF and
tested immediately. These dried fibers also show a decrease
of failure stress, down to 25 to 50% of the origin strength.
The most obvious bimodal distribution appeared for the
exposure duration of 15 min, while distribution appeared
roughly mono-modal, although broader, for the other
treatment durations.
Fiber in Tetramethoxysilane Solution (TMOS)
The tetramethoxysilane solution TMOS is used in room
temperature vulcanizing silicon rubber as a cross-linking
agent, and also used as reagent for ketal synthesis,
deposition frosting of glass, co catalyst with CsF for
Michael additions. It is used in manufacturing chemical
resistant coating and heat resistant coating. In some cases,
Tetramethoxysilane solution, used as sol-gel material is
often employed to improve the use of optical fibers in
spectroscopic detection [20, 21].
On the other hand, water is the major factor limiting
fiber strength through the well known stress corrosion
mechanism. Incorporating colloidal silica in the external
coating could be one way to reduce this effect. This may be
achieved using tetramethoxysilane (TMOS) that forms
silica by hydrolysis.
The aim of this paragraph is to study the evolution of the
silica optical fibers strength when these fibers have been
exposed to TMOS in various conditions. The results will
also give information about the influence of similar
chemical reagents.
Table 1 gives the typical physical properties of the used
product.
Fibers are put in containers filled with TMOS solution
the aged during several durations. Others fibers are put in
containers TMOS solution which are then posed on hot
water in thermal enclosures maintained at constant temper-
ature during different aging durations. After aging in hot
TMOS solution, the fibers are then dried during one day at
ambient environment (17C, 3040% RH) then subjected to
the dynamic tensile test. The obtained results are then
compared with those of as received fibers (reference fibers).
The strength of aged fibers during 4 hours in cold TMOS
solution (17C) appreciably increases (Fig. 5). The maxi-
mum gain is about 1.76% (the gain is calculated as the
percentage of the improvement of the strength of aged
fibers compared to that of non aged fibers) (Table 2).
Table 3 shows the maximum gain become 2.36% when the
aging duration in cold TMOS solution is equal to 4 days.
(a) (b)
Fig. 8 (a) Fiber aged in cold
TMOS solution during 4 days
(17C) (tensile test velocity of
50 mm/min) and (b) polymer
deterioration with external
microcraks
Fig. 7 Fiber aged in cold TMOS solution during 4 h (17C) (tensile
test velocity of 50 mm/min)
Exp Mech (2010) 50:12251234 1231
Table 5 Median fiber strength for aging in hot TMOS solution (40C) during 16 h for different tensile test velocities
50 mm/min 150 mm/min 300 mm/min 500 mm/min
As received 16 h As received 16 h As received 16 h As received 16 h
40C 40C 40C 40C
Median strength (GPa) 5.038 4.931 5.274 5.078 5.401 5.133 5.442 5.188
Gain* (%) 2.12 3.73 4.96 4.67
0
20
40
60
80
100
1.58 1.6 1.62 1.64 1.66 1.68 1.7 1.72
Ln (F) (GPa)
F
a
i
l
u
r
e

c
u
m
u
l
a
t
i
v
e
p
r
o
b
a
b
i
l
i
t
y
(
%
)
.
50mm/min AR
50mm/min 16h/40C
150mm/min AR
150mm/min 16h/40C
300mm/min AR
300mm/min 16h/40C
500mm/min AR
500mm/min 16h/40C
Fig. 10 Aged fibers during 16
hours in TMOS solution at 40C
(16 h/40C) for different tensile
test velocities (in mm/min)AR
means As Received fibers
Table 4 Median fiber strength for aging in hot TMOS solution (65C) during 4 h for different tensile test velocities
50 mm/min 150 mm/min 300 mm/min 500 mm/min
As received 4 h As received 4 h As received 4 h As received 4 h
65C 65C 65C 65C
Median strength (GPa) 5.038 4.644 5.274 4.760 5.401 4.822 5.442 4.912
Gain* (%) 7.83 9.76 10.73 9.75
0
20
40
60
80
100
1.45 1.5 1.55 1.6 1.65 1.7 1.75
Ln (F) (GPa)
F
a
i
l
u
r
e

c
u
m
u
l
a
t
i
v
e
p
r
o
b
a
b
i
l
i
t
y
(
%
)
.
50mm/min AR
150mm/min AR
300mm/min AR
500mm/min AR
50mm/min 4h/65C
150mm/min 4h/65C
300mm/min 4h/65C
500mm/min 4h/65C
Fig. 9 Aged fibers during 4 h in
TMOS solution at 65C (4 h/65
C) for different tensile test ve-
locities (in mm/min)AR
means As Received fibers
1232 Exp Mech (2010) 50:12251234
Figure 5 shows that the increase in the aging duration (from
4 h to 4 days) led to an increase in the average fiber
resistance.
As fiber surface has determined fracture to a large extent,
external coating appears critical. This coating is polymeric
in most cases, and modern optical fibers are coated by two
different layers, a soft coating at glass surface and a hard
coating at external surface (Fig. 6). The coating first makes a
protection against scratches that occur in normal handling; it
also fills the surface flaws gluing in some a way the two sides
of the micro cracks and finally, it reduces water activity at
glass surface. A non aged broken fiber is given in Fig. 6. The
crack propagation is not perpendicular to the fiber axis but
the microcrack is propagated with an angle of 45 and this
indicates a brittle fracture of the fiber core.
When the fiber is aged in cold TMOS solution during
4 h (17C) (Fig.7), small epoxy chips are present on the end
of the broken fiber.
No microscopic crack is present on the external surface
of the fiber after the dynamic tensile test. For a higher
exposure time (4 days), [Fig. 8(a)] a large circular crack
between the fiber core and the coating can lead to the core
pull out. Polymer deterioration is observed and external
microcraks appear [Fig. 8(b)].
On the other hand, one observes a decreasing of the fiber
strength as soon as the TMOS temperature increases
(Fig. 9) and the gain loss can reach10.73% (Table 4). If
the TMOS temperature decreases from 65C to 40C even
if the aging duration increases (from 4 h to16 h), the
strength decrease is lower than the one obtained when the
aging temperature was of 65C (Fig. 10 and Table 5).
When the TMOS solution is heated at 40C, a high
damage of the fiber core is observed [Fig. 11(a)]. The fiber
core is broken and the two polymer coatings are separate.
This shows severe attack of the warm TMOS solution. On
the polymer external surface [Fig. 11(b)], the dense and
continuous network of microscopic cracks appears and
quickly weakens the fiber resistance.
When the aging temperature of TMOS solution increases
(from 40 to 65C) core and polymer damage is accentuated
(Fig. 12). The fiber core is much deteriorated (several
pieces are removed), the polymer is torn with large cracks:
the fiber is very damaged.
Conclusion
Monomode optical fibers, aged in hot water at different
temperatures and durations were tested in static conditions.
All static fatigue testing showed an oscillatory evolution of
the fiber failure time versus aging duration.
The cyclic evolution may be explained by the structural
relaxation phenomenon at the glass polymer coating
interface. So, water has presented, in the same time, opposite
effects on the fiber interface. Faced to water, the polymer
coating is permeable, having a sponge type behaviour that has
favoured exchanges during aging. On one hand, water has a
corrosive action on the glass interface, tending to promote the
surface micro-cracks and on the other hand, it accelerates the
structural relaxation phenomenon.
On the other hand, the chemical attack by hydrofluoric acid
vapours (HF) has evidenced the merged effects of the
chemical damage in fluorinated environment on mechanical
reliability of monomode optical fiber. While standard fiber
was more severely damaged by hydrofluoric acid vapour
exposure, the epoxy-acrylate coating appeared not efficient to
protect from severe chemical damage. Consequently, it does
not ensure the mechanical stability in extreme conditions.
Fig. 12 Fiber aged in cold TMOS solution during 4 h at 65C (tensile
test velocity of 50 mm/min)
(a) (b)
Fig. 11 Fiber aged in cold
TMOS solution during 16 h at
40C (tensile test velocity of
50 mm/min)
Exp Mech (2010) 50:12251234 1233
Drying into laboratory environment the processed
standard fibers has lead to the failure stress decrease, down
to 25 to 50% of the origin strength.
Lastly, TMOS solution effect on epoxy-acrylate fiber is
disastrous when this solution is warm. SEM observations
are consistent with the mechanical measurements. Fiber
core is broken and multiple cracks are generated on external
polymer coating which reduces the mechanical fiber
resistance. For this environment the use of hermetic optical
fibers is advised. Such fibers are designed to improve aging
behaviour and to avoid diffusion through glass surface.
Fabrication process includes in-line deposition of a thin
layer of diamond like carbon, a few hundred in thickness
and firm polymer coatings.
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