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The effect of moisture on the mechanical properties and the failure behaviour of fibre-reinforced polymer
composites was investigated. Moisture was introduced into the specimens by immersion in distilled water.
Three materials were investigated, which were all reinforced with continuous carbon fibres. Two thermo-
setting matrices (unmodified and toughness-modified epoxy) and one thermoplastic matrix (polyether-
etherketone) were used. The results showed that the absorbed moisture decreases those properties of
both epoxy-based composites which were dominated by the matrix or the interface. The influence of
water on the fibre-dominated values, as well as on the properties of the thermoplastic material, was not
detectable. The distinct fall of the matrix- and interface-based values due to moisture can be ascribed to the
weakening of bonding between fibre and matrix and softening of the matrix material. 0 1997 Elsevier
Science Limited
595
Moisture and mechanical properties: R. Seizer and K. Friedrich
Name and supplier Type P (g cm-3 ) E (GPa) c (MPa) E (%) GIcResin (J mm2 1
Name and supplier Type Diameter (pm) P (g cmm3) E (GPa) 0 (MPa) E (%)
manufactured out of hybrid yarn. The polyetherether- to co01 for a short period of time before being weighed.
ketone used in this study had a crystallinity of -28%. In the case of specimens with moisture, the surfaces were
All panels made out of this material had the same carefully wiped before weighing. The weight gain process
crystallinity. This fact was very important for the was continued until saturation of the materials. The
mechanical tests, because the crystallinity of a material weight was measured with an analytical balance, and the
has a significant influence on the properties and cannot weight gain was calculated according to the following
be neglected4. equation:
Due to the fact that the properties of the fibres were Moisture content
rather similar (Table 2), the same term, CF, was used to
denote all fibre types in this paper. Information about weight of specimen - weight of dry specimen
=
fibre treatment for improved fibre-matrix adhesion was weight of dry specimen
not available. The average fibre volume fraction was xl00 [%] (1)
60% by volume, with a standard deviation of 1% for all
The weight gains, maximum moisture contents and
material systems studied. Both epoxy resins were rein-
diffusivities of such materials during immersion in dis-
forced with carbon fibre G30-500, and the thermoplastic
tilled water were reported and discussed in a previous
with AS4 fibre, respectively.
publication13.
All test specimens were cut from unidirectional
([0]16,[90]&, bidirectional ([0, 9014,) and/or multidirec-
tional ([0, f 45,90],,) panels which were manufactured Test procedures
out of 16 prepreg plies and cured in an autoclave
The tensile, compression, fatigue and compression-
according to the recommendations of the manufacturers.
after-impact tests were performed according to the
For the specimens used for investigation of the inter-
standards listed in Table 3. For the mode I and mode
laminar fracture properties, a foil was placed at the mid-
II tests the double cantilever beam (DCB) and the end-
thickness of the laminate. This foil prevented adhesion
notched flexure (ENF) test configurations were used. A
between the two prepreg layers and had the same effect as
detailed description of specimen geometry, test pro-
a delamination.
cedures and data reduction is given in ref. 14.
After various periods of time the specimens were
taken out of the baths and subjected to the mechanical
Conditioning
tests. The tests were performed at room temperature in a
Dry and moisturized specimens were used in this laboratory air environment. The amount of moisture
investigation. All specimens were preconditioned in an desorbed during the span of testing was found to be
oven at 77°C until their weight loss had stabilized, and negligible. The specimens were tested in three different
no further weight loss could be observed. This condition states: dry, half-saturated and fully saturated.
of the specimens was referred to as dry. After pre-
conditioning, the specimens labelled dry were stored in a
dessicator and those labelled as wet were placed in Table 3 Tests, standards and recorded properties
containers of distilled water at three different tempera-
Test Standard Value
tures: 23, 70 and 100°C. Immersing samples in water is
the worst possible moisture attack. Resting the speci- Tensile DIN 29971 Strength, modulus, elongation
mens in humid air results in a lower maximum moisture Compression DIN 65380 Strength, modulus
Fatigue DIN 50100 Fatigue strength
content’1Y12. Specimens were removed from the contain- Compression after DIN 65561 Damage resistance
ers at various time intervals for weight measurements. impact Damage tolerance
The effect of this removal on weight gain determination Mode I EGF Energy release rate, GI,
Mode II EGF Energy release rate, Gnc
had been shown to be negligible. Specimens were allowed
596
Moisture and mechanical properties: R. Selzer and K. Friedrich
Tensile tests
RESULTS
To characterize the material behaviour under tension
Glass transition temperature the strength, modulus and elongation were recorded
during testing. In the diagrams that follow the results are
The range of use of composite materials with a
shown versus the relative moisture content, which was
polymeric matrix is limited by their thermal and
defined as absolute moisture content Am [calculated
mechanical properties. Polymer composites used above
according to equation (l)] in relation to the maximum
their glass transition temperature Tg show a substantial
moisture content A mmax. So 0 means dry, 0.5, half-
loss in desired physical properties; therefore a material’s
saturation, and 1 stands for fully saturated.
glass transition temperature and its change with moisture
It appeared from Figure 1 that the tensile strength was
absorption must be investigated. In this case Tg was
not affected by the moisture for specimens with a fibre
measured as the maximum damping in the damping
orientation in the direction of the load. The variation of
versus temperature diagram. The results are presented in
the mean values was smaller than the scatter. So the
Table 4.
influence of moisture for this fibre orientation was
Due to moisture absorption the glass transition
negligible. Due to the fact that the properties of the
temperature of the resin became low, which in turn
carbon fibres were equal, the results for the 0” tensile
degraded the high temperature properties of the resins.
tests of the different composites were similar.
Nevertheless, Tg did not go below the maximum water
Specimens with a fibre orientation perpendicular to
temperature of 100°C. The glass transition temperature
of CFjPEEK was not affected by the absorbed water.
One reason for this behaviour could be the fact that CF/
3ooo
PEEK absorbed only 0.3 wt% moisture (cf. CF/EP,
1.6wt% and CF/EPmod, 2.5wt%). 2500
z
z
Testing problems 2000
S
In order to protect specimens from damage during F 1500
clamping in the testing jig and to obtain a symmetrical g
UJ
stress distribution in the samples without any stress Q)
.G 1000 I I
peaks, tabs were bonded on the specimen surface. One e - - q CF/EP
problem was that it was not possible to glue the tabs on c” 500 ---muo CFlEPmod -
to the specimens before immersing them, because the 1
I
I
I
I
I
)-A
I
CF/PEEK 1 1
1 I
quality of the glue interface between the tab and speci- 01 . 1 , 1 . I . I I
men decreased as a consequence of moisture attack; this 0.0 0.2 0.4 0.6 0.8 1.0
caused layer failure before the specimen maximum load Relative Moisture Content
was reached. Therefore, it was necessary to bond the tabs Figure 1 Tensile strength of 0” laminates
597
Moisture and mechanical properties: R. Seizer and K. Friedrich
0
0.0 0.2 0.4 0.6 0.0 1.0
0.0 0.2 0.4 0.6 0.8 1.0
Relative Moisture Content
Relative Moisture Content
Figure 3 Tensile modulus of 0” laminates Figure 5 Elongation of 0” laminates
290
1-5
10
z
‘=
6 l,o
CR
E
5 0
iii 0,5
01 J I . J 050
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Relative Moisture Content Relative Moisture Content
Figure 4 Tensile modulus of 90” laminates Figure 6 Elongation of 90” laminates
the load direction showed different behaviour (Figure 2). temperatures used on the mechanical properties. This is
The more the specimens took up moisture, the more the due to the fact that Tg did not go below the maximum
mean values of fracture strength decreased. The data water temperature of 100°C.
show a reduction of 52 and 66% in strength for the
saturated condition compared to the dry condition for
Compression tests
CF/EP and CF/EP,,d, respectively. It was indicated by
these results that the more the tensile strength values To examine the influence of the stacking sequence,
depend on the matrix and the interface, the stronger the tests were conducted for each material combination with
influence of moisture absorption was. unidirectional laminates loaded in the fibre direction [0]
Figures 3 and 4 showed that the curves of the tensile as well as in the direction transverse [90] to the fibres. The
moduli had the same trends as those of the tensile results of the compression tests are shown in Figures
strength. The decrease of the 90” tension modulus was a 7-10.
result of softening of the epoxy matrices due to moisture Figure 7 showed that the strength of 0” epoxy-based
absorption, because the modulus was calculated from a laminates was affected by the absorbed water. The
range of the strength-elongation curve where no fracture moisture reduced the compressive strength of the two
occurred. epoxy composites; -23 and 35% for CF/EP and CF/
The elongation values of the 90” laminates showed a respectively. For laminates with a [90] lay-up
decrease with increasing moisture content. The reason ~!$$L 8) the reduction was greater; 30% for CF/EP and
for this behaviour was not the softening of the epoxy 37% for CF/EP,,d. It was indicated by these results that
matrices, but weakening of the fibre-matrix interface. the more the compressive strength depends on the
Softening of the resins with increasing moisture content matrix, the stronger the influence of moisture absorption
would lead to higher elongations. was.
It was mentioned above that the specimens were It appeared from Figure 9 that the stiffness was not
conditioned at three different temperatures. Neverthe- affected by the moisture for specimens with a fibre orien-
less, it was not possible to detect an influence of the tation in the loading direction. As the variation of the
598
Moisture and mechanical properties: R. Seizer and K. Friedrich
_ ,CI CF/EP
500 H..... o CF/EPmod 1-1
j-A CF/PEEK
0 I ,
0.0 0.2 0.4 0.6 0.8 1.0
0.0 0.2 0.4 0.6 0.8 1.0
Relative Moisture Content Relative Moisture Content
Figure 7 Compression strength of 0” laminates Figure 10 Compression modulus of 90” laminates
. 1 . . . ]
0.0 0.2 0.4 0.6 0.0 1.0
Relative Moisture Content
Figure 11 Fatigue behaviour of dry materials, lay-up [0,+45,90]2s
Figure 8 Compression strength of 90” laminates
150
compression tests performed on carbon fibre-reinforced
polyetheretherketone, no moisture effects on stiffness
and strength of the laminates were detected. This could
100
be explained by the low maximum moisture content of
the PEEK matrix, and the excellent hot/wet properties of
this matrix material.
50
Fatigue tests
---mmo CF/EPmod The fatigue behaviour of the materials in dry and wet
-A CF/PEEK conditions were demonstrated in Wohler curves (Figures
0 I1 and 12). The fatigue tests were carried out on a
0.0 0.2 0.4 0.6 0.0 1.0
Relative Moisture Content
Schenck servohydraulic testing machine with a force
capacity in the range of l-250 kN. The ratio R between
Figure 9 Compression modulus of 0” laminates
minimum and maximum dynamic load was chosen as
R = 0.1, while the frequency was 10 Hz. The fatigue-
mean values was smaller than the scatter, the influence of tested specimens that did not fail within the maximum of
moisture for this fibre orientation was negligible. Speci- 2 x lo6 cycles are shown by arrows.
mens with a fibre orientation perpendicular to the load The courses of the Wijhler curves were very flat. This
direction and an epoxy matrix showed different behav- fact was a result of the good fatigue behaviour of carbon
iour (Figure ZO). The more the specimens took up fibres. Because this type of fibre does not fatigue, the
moisture, the more the stiffness decreased. The data effect of moisture on carbon fibre-reinforced polymers
showed a reduction of 42 and 36% in stiffness for the with high fibre contents is negligible15. Another result of
saturated condition when compared to the dry condition, this investigation was that the curves for polymer
for CF/EP and CF/EP,,d, respectively. Regarding the composites do not flatten out like the curves for steel,
599
Moisture and mechanical properties: R. Selzer and K. Friedrich
0 6
EP,,d and 7% for CF/EP was found. The influence of Impact Energy [J/mm]
moisture on CF/PEEK was negligible. Figure 14 Compression strength of CF/EP after impacts with varying
energies
600
Moisture and mechanical properties: R. Seizer and K. Friedrich
601
Moisture and mechanical properties: R. Seizer and K. Friedrich
DISCUSSION
Correlation between static andfatigue behaviour
602
Moisture and mechanical properties: R. Seizer and K. Friedrich
Failure maps
5 300. Defaminations
In general the tensile and the compression moduli
F
of a material are almost equal, because both values are
;
measured in the linear-elastic range of the material. v)
Comparing the results of this investigation it could be J
S
observed that for all materials the compression modulus z loo- Damage Free
LL
was lower than the tensile modulus. The reason for this
behaviour was that the high stiffness of the carbon fibres
was fully transferred to the composite when the specimen
was loaded in tension. In the compression tests the fibres Relative Moisture Content
tended to kink or bend under load, so that the com- Figure 25 Failure map for material CFIEP,,,
603
Moisture and mechanical properties: R. Seizer and K. Friedrich
604