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@ 1995 Kluwer Academic Publishers. Printed in the Netherlands.
R DAVIES and F. R A N N O U
Marine Materials Laboratory, IFREMER, Centre de Brest, BP 70, 29280 Plouzan~, France
Abstract. This paper investigates the use of coupon specimens to study the severity of defects
in filament wound tubes. Composites based on two types of resin are studied, an epoxy and a
vinylester. First, the properties of the unreinforced resins are measured. Next the properties of
fiat filament wound unidirectional glass fibre reinforced composite plates using these resins are
determined, and in particular their delamination resistance under mode I loading. These results
are then compared with those determined on specimens taken from filament wound tubes with
different winding angles (dz30°, ±45 ° and 4-60°) and diameters.
Key words: tubes, delamination, winding angle, epoxy, vinyl ester, glass fibres.
1. Introduction
Fibre reinforced polymeric composites are very widely used in the form of fil-
ament wound tubes. In different applications these may be thin or thick walled,
(often defined according to whether the diameter/thickness ratio is greater or
less than 10), loaded under either internal or external pressure. Well-established
examples using aramid and glass fibre reinforcement are rocket motor cases and
missiles [1]. For prototype deep sea submersibles carbon fibre composite cylin-
ders are being proposed to replace metallic pressure hulls [2]. Other recent exam-
ples in the marine industry, with glass fibres as the reinforcement, are cooling
water pipework in fishing boats [3], fire protection circuits on offshore plat-
forms [4], and containers for protecting deep sea instrumentation units [5]. For
all these applications appreciation of the influence of defects on the resistance of
the structure is essential, both for their design and in order to define quality con-
trol procedures. Since one type of defect frequently encountered is in the form
of delaminations, and as delamination propagation has been observed in test-
ing of thick and thin cylinders, the first part of this programme concentrated on
this type of defect. Other defects which may be found in tubes include porosity
and cracking due to handling or impact but these may also lead to delamination
failures.
The filament winding process provides uniform, high fibre volume fraction
composites ( V I of 0.65 or more). However, for the user who envisages a change
of resin, whether in order to reduce the sensitivity of the tube to defects or to
334 P. DAVIES AND E RANNOU
2. Materials
The materials tested were based on two types of resin, an epoxy and a vinyl
ester. The epoxy was of the type LY556 from Ciba Geigy, with hardener HY917,
which is a combination commonly used for filament winding. It requires curing
at elevated temperature so after winding tubes were rotated in an oven at 150°C
for 3 hours. The vinyl ester specification was 411-45 from Dow Chemical and
is based on an epoxy. This was cured at 100°C for 1 hour.
Unreinforced resin samples were cast, either between two plates to form 4 mm
thick flat sheets or into moulds to form flat dog-bone specimens. The dimensions
of the latter were such as to allow gauge length dimensions of 50 x 10 x 4 mm.
Samples were then cured following manufacturers recommendations.
The reinforcing fibres were of the E-glass type throughout. Both unidirectional-
ly-reinforced sheets and tubes reinforced at + 3 0 °, +45 ° and zk60 ° were filament
wound by SEPMA S.A., Mulhouse. The sheets were nominally 5 mm thick and
contained an aluminium film defect 15 microns thick, coated with release agent,
at mid-thickness. This film extended in from one edge in the 0 ° direction for
80 mm. Two plates of dimensions 300 x 300 mm were made for each resin. The
tubes also contained defects, of the same aluminium film, oriented as shown in
Figure 1. The film thicknesses in plate and tube after moulding were verified
in the scanning electron microscope. Two internal tube diameters were studied,
160 mm for all three winding angles and 60 mm for tubes at 4-45 °, and the
wall thickness was nominally 5 mm for both diameters. Tubes were wound such
that the wall thickness consisted of 12 layers. As successive layers were wound
at angles of + / - 0 the tubes were not mirror symmetric about their mid-plane.
The film defects were placed between the 6th and 7th layers, between layers
at + / - 0.
3. Experimental Methods
The elastic properties of the resins were determined by tensile tests on cast dog-
bone specimens. Klc values were measured following the ESIS protocol [18]
on single edge notch bend specimens (SENB), Figure 1, which had been pre-
cracked by tapping a new razor blade into a sawcut at mid-length. The fragile
nature of the resins made pre-cracking difficult and up to 30 specimens of each
resin were required to ensure 8 acceptably pre-cracked specimens (pre-cracks
perpendicular to the specimen edge and of length between 0.4 and 0.6 times the
specimen width). Pressing the razor blade into the specimens using the crosshead
of a universal test machine produced more reproducible pre-cracks but blunted
the crack tip (as had been found by previous work within the ESIS group) and
resulted in Kic values up to 100% higher than those obtained by tapping.
Fibre volume fractions and void contents of the composites were determined
by density measurements, bum-off at 500°C and weighing the residue.
336 p. DAVIES AND E R A N N O U
6
I 12
a) Unreinforced resin
Fibre direction
50
200
Three point flexural tests were performed on specimens taken from unidirec-
tional plates, following the standard test method EN-64, with a span length of
16 times the thickness and a specimen width of 15 mm.
Composite delamination resistance tests were all performed on 20 mrn wide
specimens at a loading rate between 1 and 5 mm min -1. The ESIS test protocols
were used [8] and specimens are shown in Figure 1. Mode I tests were performed
on specimens cut from both flat plates and tubes of both materials and all three
angles. At least five specimens were tested for each specimen type.
T h e mode I test involved a double cantilever beam (DCB) specimen with
aluminium end blocks for load introduction. Data was analysed using an exper-
imental compliance calibration obtained by testing a series of specimens with
different initial crack lengths, and for the values presented here large displace-
ment corrections were not necessary. Initiation values correspond to the point of
non-linearity on the load-displacement recording, and specimens were not pre-
cracked (i.e., values were determined for initiation directly from the aluminium
foil). The equation used to determine Gic was:
GIc = n P 6 / 2 B a
4. Results
Values of density, fibre volume fraction and estimated void content are presented
in Table I, to show that the constituents of plates and tubes were present in very
similar proportions. The only panel with slightly higher fibre content is that of
unidirectional vinyl ester. The void contents are quite low in all the materials
but it should be noted that these values are very sensitive to the densities of the
constituents used in the calculations. Here the fibre density was taken to be 2.55
and the resin densities were measured on cast epoxy and vinyl ester sheets to
be 1.20 and 1.13 respectively.
Three point flexure tests were performed on specimens from the unidirectional
plates. The results obtained are presented in Table II. The values obtained are
higher for the vinyl ester plate but this is a result of its higher fibre content.
Moduli agree quite closely with values calculated by laminate theory using fibre
volume fractions.
338 P. DAVIESAND E RANNOU
TABLE I. Densities, fibre volume fractions, and estimated void
contents (means of five samples for each)
Tubes
30 ° Vinylester 1890 55.7 3.0
45 ° Vinylester 1910 55.5 0.8
60 ° Vinylester 1890 55.0 1.9
30° Epoxy 1880 52.3 1.6
45 ° Epoxy 1885 53.2 2.0
60 ° Epoxy 1920 55:0 1.6
45 ° Vinylester a 1945 57.9 0.6
45 ~ Epoxya 1951 56.9 0.9
%0 mm diameter.
TABLE 1I. Flexural tests, measured (means from six specimens) and pre-
dicted values for unidirectional plates. Standard deviations in brackets
a) Unreinforced Resins
The elastic properties o f the two resins together with the KI~ values are shown
in Table III. F r o m the latter it is possible to obtain a value for Gc of the resin
using the expression for plane strain:
G =/('2(t --/22)/E.
Values o f Ge are also given in Table III. It should be noted that this is not the best
method o f determining Go, as it relies on the correct value of E being available,
i.e., that m e a s u r e d at the s a m e strain rote. A preferred method uses the area under
the load d i s p l a c e m e n t plot and specimens o f different notch length [18].
T h e results s h o w that the moduli and Gc values o f the two resins are very sim-
ilar, the values for vinyl ester being slightly higher. The moduli measured here are
a little lower than those quoted by the manufacturers, which are around 3.2 GPa
THE EFFECT OF DEFECTS IN TUBES 339
TABLE IV. Results from all mode I tests on fiat and tube
specimens. Mean values at initiation (standard deviations
in brackets)
Tubes, 60 mm diameter
45 ° Vinyl ester 230 (14)
45 ° Epoxy 288 (85)
[19, 20]. Post curing increases the modulus and reduces Gc for the vinyl ester
resin. T h e s e values were measured on resins which had been cured at tempera-
tures similar to those e m p l o y e d for the tubes. The e p o x y was cured at 140°C for
three hours. The vinyl esters were cured at 80°C for 3 hours rather than 100°C
for 1 hour, but as the crosslinking of this resin is virtually complete even after
r o o m temperature curing it is not expected that this difference would c h a n g e the
values of Kic greatly.
b) UD Composites
S p e c i m e n s cut f r o m the flat plates were tested under m o d e I loading. The initia-
tion (non-linear) delamination results are shown in Table IV for both materials.
It is apparent that initiation values are extremely similar for the composites with
340 P. DAVIES AND E RANNOU
Gc (J/m z)
250
200
150
100
50
0
Epoxy Epoxy Vinyl Vinyl
resin UD ester ester
resin UD
Fig. 2. Mode I initiation GIc results for unidirectional plate specimens, epoxy and vinyl
ester composites, and Gc results from resins.
both resins, Figure 2. Indeed, within experimental scatter they are identical. This
is not unexpected given the similar values of Gc measured on the resins.
Values of Gc increased as the crack progressed, resulting in R-curves such as
those shown in Figure 3. Propagation values are at least five times as high as ini-
tiation values. This type o f increase has been described previously in numerous
publications, e.g. [21-23] and was one of the principal reasons for the emphasis
on initiation values in the ASTM mode I standard. Here it is interesting to note
that the R curves for the two unidirectional materials are quite different. Plateau
values for the vinyl ester are some 25% lower than those for the epoxy, although
both appear to reach their plateau values after about 25 to 30 mm of crack prop-
agation. It should be remembered that the fibre volume fractions are not identical
in the two materials (Table I). The fibre volume content will affect the stiffness of
the DCB specimen and influence the development of the bridging zone. Here the
vinyl ester composite is around 15% stiffer than the epoxy but in published work
increasing the stiffness of specimens tends to increase propagation values [24,
25], so the delamination propagation resistance of the unidirectional vinyl ester
is probably genuinely lower than that of the epoxy composite. Other parameters
such as the strength of fibre-matrix adhesion will also affect the energy dissipation
in the bridging zone. Thus while the steepness of the rise in the Gicv crack length
plot may contain valuable information on the material its dependence on specimen
stiffness makes such information difficult to exploit quantitatively at present.
Mode I tests were then performed on samples cut from tubes, as shown in Fig-
ure 1. In each case tests were performed on both epoxy and vinyl ester compos-
T H E E F F E C T O F D E F E C T S IN T U B E S 341
Glc
2000 -
1800 -
1600
1400
1200
1000
800
600
400
0
(a) 50 55 60 65 70 75 80 85 90 95 100
2000
{Jim ~)
1800
1600
1400
1200
1000
800
600
400
200
a (ram)
0 t I I 1 -'-q-----~ I b- I r
ite specimens, taken from tubes with three different winding angles, + / - 30 °,
+ / - 45 ° and + / - 60 °.
The DCB specimens were treated as if they were flat. This assumption needs
to be justified as it is clear that opening a curved specimen will result in a
contribution from other modes. Indeed, in the extreme case of a semi-circular
specimen the outside edges of the specimen will be loaded in predominantly
mode III (out of plane) shear, and this may be one way of obtaining the elusive
Glllc values for composites. This is illustrated in Figure 4. Ripling et al. have
342 a DAVIESAND E RANNOU
~ 1P(T°tal)
3 i
)
III
used DCB specimens with inclined bondlines to obtain mixed mode (I/III) data
on adhesives [26], and a simple analysis shows that the mode I and mode II
contributions are:
For the specimens tested here, of width 20 mm taken from a tube of internal
diameter 160 ram, the angle 0 is so small that even at the specimen edge the
mode I component is over 99% of the total G. The assumption that the specimens
were flat appears justified but to check this a series of tests was performed on
narrower specimens from the 30 ° epoxy tube (B = 10 mm, for which at the
specimen edges Gt = 99.9% of GTot~). These results are shown in Table V.
The mean value obtained on narrow specimens is about 15% lower than that
measured on the specimens of recommended width but as the standard deviation
of the latter is around 15% the difference is probably not significant.
The second assumption to be justified is that lack of mirror symmetry between
the two arms of the DCB specimens taken from tubes did not introduce other
loading modes. As described earlier the tube wall consisted of 12 plies wound
successively at + 0 and then - 0 . Laksimi et at. have discussed the implications
of non-symmetry on the bending moments in DCB specimen arms [13], and it is
THE EFFECT OF DEFECTS IN TUBES 343
5. Discussion
5.1. RESIN-COMPOSITE COMPARISON
The transfer of toughness from resins to composites has attracted much atten-
tion in the past [27], but resin initiation values have frequently been compared
with propagation values for composites. This has led to the conclusion that the
presence of fibres increases delamination resistance in brittle matrix composites.
Here the resin and composite initiation values of Glc are similar, while compos-
344 E DAVIES AND F. RANNOU
GIc
2000
1500
1000
500
a (ram)
0 I J I I t ~ I-- r ~ I --~ I
(a) 35 40 45 50 55 60 65 70 75 80 85 90 95
3000
(b) TUBE 30 ° Glass/Vinyl ester
( J i m 2)
2500
2000
1500
1000
500
n (ram)
0
(b) 35 40 45 50 55 60 65 70 75 80 85 90 95
Fig. 6. Mode I propagation delamination resistance G1c for specimens from tubes wound
at + / - 30 °, (a) Glass/Epoxy, (b) Glass/Vinyl ester.
ite propagation values are over five times higher. Both initiation and propagation
values for the composites are relevant to material selection. The initiation values
offer a lower bound for static delamination resistance while to determine the
subsequent safety margin for propagation it is necessary to relate these values to
multidirectional lay-ups and this is examined below.
V a l u e s o f G i c at i n i t i a t i o n f o r s p e c i m e n s c u t f r o m t u b e s are c o m p a r e d w i t h v a l u e s
m e a s u r e d o n flat p l a t e s in F i g u r e 7 a n d T a b l e IV. T h e s p e c i m e n s c u t w i t h the
346 E DAVIES AND E RANNOU
GIc (J/m 2)
400 7-
300
200
100
I I t
~ °
fibres at 30 ° give values very similar to those measured on the flat specimens,
with lower scatter. As the angle is increased to 45 ° the scatter in values increases
but values are still quite similar to those from the unidirectional composite. It
appears that for mode I loading the initiation values of Glc are independent of
fibre angle to a first approximation. This has considerable importance as it would
simplify considerably the screening of matrix materials to be used in filament
wound structures. However other modes of loading must also be examined in
order to extend this hypothesis and these will be the subject of a subsequent
paper.
The mode I resistance curves of specimens taken from the + / - 30 ° fila-
ment wound tubes are similar to those of flat unidirectional specimens for the
epoxy composite, but higher than the flat vinyl ester composite specimen values.
Propagation resistance will be closely linked to fibre-resin interface strength. In
the case of defects in tubes it is apparent that once the crack has initiated at a
defect its orientation and the loading direction with respect to the fibre wind-
ing angle will determine whether it propagates further or not, so the R-curves
THE EFFECT OF DEFECTS IN TUBES 347
are also necessary for a complete characterization. However, overall the results
appear to justify the decision to concentrate standard tests on initiation values
when a specimen-independent fracture resistance value is needed to characterise
a matrix-fibre combination.
The two resins tested here show very similar initiation behaviour. The values
of Gc measured on the unreinforced resins were similar, 175 and 195 J m -2 for
the epoxy and vinyl ester. Initiation values for unidirectional and tube specimens
are also similar. Propagation values are higher for the unidirectional and tube
epoxy composite specimens and the fracture surfaces in Figure 5 suggest that the
fibre-matrix interface may be weaker for the glass-vinyl ester composites.
Based purely on a damage tolerance criterion it may not appear to be worth-
while to change from an epoxy to a vinyl ester matrix. However, it should be
noted that manufacturing parameters also play an important role in such a choice,
and in particular the lower temperature and shorter cure conditions required by
the vinyl ester may prove attractive. Relative costs will of course also play a part
in final material selection.
6. Conclusions
This paper has presented the results from the first part of a programme to study the
influence of defects on the properties of filament wound tubes. The delamination
resistance of plates and tubes has been determined. This has revealed that:
Mode I delamination resistance initiation measurements on filament wound
tubes correlate quite closely with the fracture toughnesses of the unreinforced
resins, and with the Gic initiation values measured on flat unidirectional speci-
mens. Initiation values are independent of reinforcement angle to a first approx-
imation so unidirectional values can be used predict mode I delamination resis-
tance of tubes. Propagation values of unidirectional epoxy and vinyl ester com-
posites correlate reasonably well with values measured on specimens taken from
tubes in which the crack is propagated at the + / - 30 ° interface.
Epoxy and vinyl ester matrix composites show very similar resistance to
delamination initiation but the propagation resistance of the epoxy composites is
higher.
In the second part of the study the mode II and mixed mode behaviour of these
materials in flat unidirectional and multidirectional tube form will be described.
Further studies are examining the influence of water on fracture and the nocivity
of defects in tubes under service conditions.
348 V. DAVIES AND E RANNOU
References
26. Ripling, E. J., Santner, J. S. and Crosley, E B., 'Fracture Toughness of Composite Adherend
Adhesive Joints under Mixed Mode I and III Loading', J. Materials Science 18, 1983, 2274-
2282.
27. Hunston, D. L., 'Composite Interlaminar Fracture: Effect of Matrix Fracture Energy', Com-
posite Tech. Review 6(4), 1984, 176-180.