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Analysis of Free Edge Delamination in [0m, 90„]s Composite

Structures: Experimental Approach

F. A. Netto 1 and S.F. Estefen 2

1
Institute) de Pesquisas da Marinha - Rua Ipiru n" 2 - Jardim Guanabara
llha do Governador - Rio de Janeiro - RJ - Brasil
CEP: 21931-090
2
Coordenagäo dos Programas em Pos -Graduagäo em Engenharia (COPPE)
Programa de Engenharia Oceänica - Universidade Federal do Rio de Janeiro
Rio de Janeiro - RJ - Brasil

ABSTRACT bigger than the transversal one (ET), so 0° laminae will


contract more than 90° ones in this direction. However,
Layer debonding (delamination) is one of the most considering a perfect gluing in laminate, the laminae are
frequent cracking modes in laminated composite forced to contract the same amount, causing the
materials. In this paper, quasi-static and fatigue appearing of tension and compression stresses between
experiments are accomplished in order to observe the 0° and 90° layers. At free edge, these stresses reach their
damage in terms of initiation and growth of free edge maximum values, causing delamination problem.
delamination. Considering laminated glass fiber/ In this paper, the damage mechanism described
polyester resin structures [0m, 90 n ] s (m, η —> 2, 4, 6), the above is analyzed through quasi-static and fatigue tests,
experimental approach shows that different laminate observing edge delamination process in glass
constructions induce particular conditions for the fiber/polyester resin structures [0m, 90„]s (m, η 2, 4,
appearance of edge delamination. 6). Damage characterization includes microscopic
analyses of delamination initiation and growth, in order
to study the effects of laminate stacking sequence on the
INTRODUCTION damage process.

Depending on the fiber filament orientation,


different laminate responses are observed in terms of EXPERIMENTAL PROCEDURE
mechanical strength as well as delamination
Material
characterization. Considering a simple cross-ply
laminate [0/90]s subjected to a tension load in its Four panels 305 mm square of glass fiber/polyester
longitudinal direction (the 0° layers are aligned in resin, each one for [02, 90 4 ] s , [04, 90 2 ] s , [02) 906]S) [06,
positive χ axis), the difference between the values of the 90 2 ] s lay-ups, were manufactured in an autoclave at the
Poisson ratios in the two directions (v LT >v TL ) causes Brazilian Navy Shipyard (AMRJ). 1% of Cobalt and 2%
different contractions for 0° and 90° layers in transversal of MEK. were used as accelerating and catalytic agents,
direction (y axis). This effect occurs because of the fact respectively. Table 1 illustrates the main physics and
that longitudinal modulus of elasticity (EL) is much chemistry properties of the resin.

' To whom all correspondence should be addressed,


e-mail: antoun@ipqm.mar.mil.br

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Vol. 10, No. 1, 2002 Free Edge Delamination

Specimen size followed O ' B r i e n ' s standard 12,21. In According to A S T M - D - 3 0 3 9 / 7 6 , the results must
this way, the specimens were carefully cut from each have a statistical treatment. Therefore, for each series of
panel using a high-speed diamond disk. They were 127 tests, the average value, standard deviation and
m m long by 25 m m wide and thickness dependent on coefficient of variation were calculated for each variable
laminate lay-up. considered. Tables 2 to 5 list the results obtained in
terms of the tensile stress for matrix cracking initiation
Table 1 ( a j ) and the number of cracks observed in the gage
Resin physics and chemistry properties section (NF).
Polystyrene 44.5 %
Acidity 15 m g K O H / g Table 2
Density 1.15 g/cm 3 Average values for σ, and NF - [0 2 , 90 6 ] s configuration

T i m e for Gel 13 minutes Average Deviation Variation (%)

Temperature of Gel 31°C Oj ( M P a ) 41,939 4,8956 11,68

Color Yellow NF 1,0 0,0 0,0

Cure cycle Standard A S T M - D - 2 4 7 1 / 7 1


Table 3

As regards the laminate fabrication process, each Average values for σ, and NF - [0 6 , 90 2 ] s configuration

layer had a nominal thickness of 0.250 m m and a fiber Average Deviation Variation (%)
volume of 39.37%. Environmental moisture and ο-, ( M P a ) 82,582 4,0560 6,481
temperature were controlled and maintained, NF 1,0 0,0 0,0
respectively, at 24° C and 6 3 % during all manufacturing
processes. Table 4
Average values for σ, and NF - [0 2 , 90 4 ] s configuration
Average Deviation Variation (%)
Oi ( M P a ) 43,780 8,1100 18,52
Quasi-Static Tests NF 1,2 0,4 0,3

Tensile tests were performed in order to verify the


Table 5
stress level associated with the beginning of the damage
Average values for and NF - [0 4 , 90 2 ] s configuration
for different laminate configurations. In this way,
Average Deviation Variation (%)
specimens were loaded until the first indication of
θ\ ( M P a ) 77,537 9,4006 12,12
cracking.
NF 1,6 0,8 0,5
T h e n five specimens of each lay-up were placed
separately in the hydraulic load frame such that each
specimen had a gage length between grips of
approximately 76 m m . All variables related to the ramp
tests (displacement, load and strain) were monitored. T h e correct choice of laminate s t a c k i n g s e q u e n c e is
Specimens were loaded in tension at a rate of 2 mm/min m a n d a t o r y in order to avoid f r e e e d g e delamination.
until the first audible indication of cracking was heard. This effect can be noticed through the results presented
All tests had linear versus nominal strain plots up to the in Tables 2 to 5. Comparing the obtained tensile stress
point when the loading was stopped. After that, the levels for cracking initiation a m o n g laminates with the
specimens were r e m o v e d from the load frame and the same number of layers, it can be observed that the quan-
their edges were polished by a grinding machine tity of 0° laminae influences directly laminate response.
producing an excellent finishing. Photographs of the Otherwise, Oj magnitude for [0 6 , 90 2 ] s configuration is
polished edges were taken through optical microscope about twice the [0 2 , 90 6 ] s one and for [0 4 , 90 2 ] s and [0 2 ,
in order to examine the damage. 90 4 ] s configurations, the maximum tensile stress is

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F.Α. Netto and S.F. Estefen Science and Engineering of Composite Materials

about 1,8 times the [0 4 , 90 2 ] s lay-up. Even considering


the results f r o m laminates with different number of
layers, for instance [0 4 , 90 2 ] s and [0 2 , 90 6 ] s
configurations, it can be seen that the addition of 0°
plies in the laminate retards d a m a g e onset.
Damage extension occurs in different sizes,
considering each kind of construction tested. For
example, taking into account [0 6 , 90 2 ] s specimens, crack
length varies between 10 to 15mm. On the other hand,
observing [0 2 , 90 6 ] s laminates, matrix crack extends
along the specimen width (25 mm). For both cases,
damage has been developed in the 90° plies. Figure 1
shows the comparison between matrix crack lengths for Fig. 2: Typical d a m a g e characterization of [0 2 , 90 6 ] s
[0 2 , 90 6 ] s and [0 6 , 90 2 ] s specimens. configuration - Magnification 50 X

Fig. 1: Crack lengths for [0 2 , 90 6 ] s (specimen 3) and


Fig. 3: Typical damage characterization of [0 2 , 90 6 ] s
[0 6 , 90 2 ] s (specimen 4)
configuration - Magnification 100 X

Figures 2 to 5 illustrate edge micrographs at 0°/90° I · Wi .1


«Ο'®"«!""*!!11*·
interface, considering the different laminate con-
figurations tested. For [0 6 , 90 2 ] s configurations, it is .Vtacgocrmck
verified that the presence of matrix cracks does not
cause delamination. T h e same is observed for [0 4 , 90 2 ] s
configuration. However, for [0 2 , 90 6 ] s and [0 2 , 90 4 ] s
constructions, matrix cracks have several branches and
delamination onset is noticed. For all configurations, it
has been observed that there is an increase in crack
thickness when it goes through matrix regions with a
high concentration o f 90° oriented fibers. It happens
because fiber boundaries are regions of stress
concentration. Fiber interaction, during loading, Fig. 4: Typical d a m a g e characterization of [0 4 , 90 2 ] s
contributes to damage propagation. configuration - Magnification 50 X

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Vol. 10, No. 1, 2002 Free Edge Delamination

the end of the tests. It was also observed that cracks


originated at the free edge and propagated to the
laminate interior in the loading transversal, through 90°
plies. The cracks usually formed secondary branches in
the matrix region and some of them caused edge
delamination. As a consequence, one of the specimens
fractured completely at 660 cycles (Figure 6).

Fig. 5: Matrix microcracks in 90° laminae - [0 2 , 90 4 ] s


configuration - Magnification 50 X

FATIGUE TESTS

For each lay-up, five specimens were tested Fig. 6: [02, 90 6 ] s fractured specimen
separately. Gage length between the grips was again
fixed at 76 mm and an oscilloscope monitored the
parameters related to cycling loading (amplitude, Figures 7 and 8 show free edge micrographs that

frequency and period). The specimens were loaded at a illustrate the fragility of [02, 90 6 ] s configurations. On the

frequency of 5 Hz and a ratio (r) of 0.1. The number of other hand, [06, 90 2 ] s constructions had 11 to 14 cracks

load cycles varied with the test. with lengths varying between 5 and 12 mm. After

For [0 2 , 90 6 ] s and [0 6 , 90 2 ] s configurations, two damage characterization, delaminations and crack

fatigue analyses were performed: endurance and branches were not observed.

damage characterization. Considering [0 2 , 90 4 ] s , [0 4 , Comparing laminate responses, some characteristics


90 2 ] s constructions, a conventional fatigue test was should be mentioned. Firstly, it must be pointed out that
applied in order to verify the declination of Oj as a [06, 90 2 ] 5 specimens were subjected to loads up to twice
function of the number of load cycles (N). the [02, 90 6 ] s ones. Even so, no delaminations have been

[0 2 , 90 6 ] 5 a n d [0 6 , 90 2 ] s c o n f i g u r a t i o n s

Endurance Test
The objective of the test is to observe the occurrence
of delaminations when laminates are subjected to
extreme cyclic loads. In this way, loads up to 90% of
the laminate tensile strength for matrix cracking
initiation in quasi-static tests (Tables 2 and 3) were
considered as a maximum value for the cyclic load. The
number of cycles was fixed at 1000. At the end, it was
possible to verify the presence of delaminations and to
count the number of cracks in the gage section.
Considering [02, 90 6 ] s configurations, the occurrence Fig. 7: Typical damage characterization of [0 2 , 90 6 ] s
of 1 to 2 cracks was noticed (with 25 mm of length) at configuration - Magnification 200 X

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F.Α. Netto andS.F. Estefen Science and Engineering of Composite Materials

produce significant d a m a g e in [0 6 , 90 2 ] s specimens.


Therefore, their results were not relevant in terms of
damage characterization. Figure 9 shows the beginning
of the microcrack formation in a specimen submitted to
10 6 cycles.

Fig. 8: Typical d a m a g e characterization o f [0 2 , 90 6 ] s


configuration - Magnification 50 X

formed in [0 6 , 90 2 ] s laminates. On the other hand, the


difference between crack lengths can be attributed to the
number of 0° plies in each type of configuration tested.
Fig. 9: Microcracking onset in [0 6 , 90 2 ] s configuration
The addition of 0° plies in laminate restrains crack
- Magnification 2 0 0 X
propagation, causing the appearance of several small
cracks in [0 6 , 90 2 ] s laminates. Therefore, it can be
concluded that laminate fragility increases with the
addition of 90° laminae. Even though a small quantity of For [0 2 , 90 6 ] s configurations, the d a m a g e process can
cracks have been noticed in [0 2 , 90 6 ] s specimens, they be observed in its plenitude. Figure 10 shows the
have caused prejudicial effects in laminate mechanical damage sequence in a [0 2 , 90 6 ] s laminate. It can be seen
strength by forming delamination at 0°/90° interface. that damage development occurs in 90° laminae. Figure
10(a) shows matrix microcracking onset at 0°/90°
Damage Characterization interface. From 0° layers, microcracks begin to be
The purpose of the test is to observe damage localized in the loading transversal direction, Figure
mechanism, considering both matrix crack process and 10(b). Figure 10(c) illustrates the following phase, when
delamination onset. In this way, tests were interrupted at a significant increase of microcracks is noticed,
3 4 5 6
10 , ΙΟ , 10 and 10 cycles, when the specimens were denoting region saturation. This means the threshold
removed from the grips and the edges were polished and between microscopic and macroscopic damages. In the
examined in the microscope. For each set of cycles, next stage, matrix saturation reaches its maximum level,
photographs of the edge were taken in order to causing the appearance o f macrocracks, Figure 10(d).
document the d a m a g e mechanism. Then, it was possible The occurrence of secondary macrocracks denotes the
to determine the presence of local delaminations fragility of the region due to the high density of
associated with matrix crack near the free edge. For all microcracks. The presence of delaminations can also be
tests, maximum load values were considered 2 0 % of the noticed, which appears after matrix macrocracking as a
laminate tensile strength for matrix cracking initiation consequence of continuous loading. Delaminations
obtained from quasi-static test o f [0 2 , 90 6 ] s constructions mean microcracking extension, usually in the same
(Table 2). direction of the loading. However, delamination effects
As expected, there have been different responses for are very prejudicial to the laminate integrity. Being
[0 2 , 90 f) ] s and [0 6 , 90 2 ] s configurations. Firstly, the placed at 0°/90° interface, delaminations produce layer
maximum number of cycles considered was unable to debonding, which may cause structural collapse.

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Vol. 10, No. 1, 2002 Free Edge Delamination

»WPP

(c) (d)
Fig. 10: Damage development process in [02, 90 6 ] s configurations: (a) 103 cycles; (b) 104 cycles; (c) 105 cycles and (d)
106 cycles - Magnification 200 X

h.T,.

As described previously, independently of the 5). For each specimen, the loading was maintained until
configuration type, the specimens were subjected to the the First indication of cracking.
same number of loading cycles. Therefore, the results Figures 11 and 12 describe σ versus Ν plots and the
indicate that [0 2 , 90 6 ] s configurations are more sensitive equations (1) and (2) show their mathematical
to damage than [0 6 , 90 2 ] s ones, as already pointed out in representation, a straight line adjusted from the
previous section. experimental results, considering [0 4 , 90 2 ] s and [0 2 , 90 4 ] s
configurations, respectively.

[0 2 , 90 4 ] s a n d [0 4 , 90 2 ] s c o n f i g u r a t i o n s
σ =-12,30 Log(N) + 7 8 , 3 8 (1)
Fatigue tests were conducted for [0 2 , 90 4 ] s and [0 4 ,
90 2 ] s configurations in order to observe the decrease of σ = -5,59 Log(N) + 44,86 (2)
laminate strength through the cyclic loading. Fourteen
specimens were tested for different load levels, As expected, the results indicate that [0 2 , 90 4 ] s
corresponding to 90%, 80%, 70%, 60%, 50%, 40% and configurations are more sensitive to damage than [0 4 ,
30% of the laminate'tensile strength for matrix cracking 90 2 ] s ones and, as previously explained, this behavior is
initiation obtained from quasi-static tests (Tables 4 and related to the quantity of 0° and 90° plies in the

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F A. Netto andS.F. Estefen Science and Engineering of Composite Materials

Table 6
Number of macrocracks ( N F ) and length variation (LF)
for [04, 90 2 ]s configurations
σ (MPa) Specime NF LF (mm)
η
1 6
69,54 2 8 10 to 15
3 3
61,82 1 4 10 to 12
2 5
1 2
Fig. 11: Fatigue behavior - [04, 90 2 ] s configuration 54,09 2 1 5 to 8
3 2
46,36 1 2 3 to 5
1 1
38,63 2 1 3 to 5
3 1
23,18 1 1 2 to 4
2 1

Table 7
Number of macrocracks ( N F ) and length variation (LF)
liagM
for [02, 90 4 ] s configurations
σ (MPa) Specimen NF LF (mm)
Fig. 12: Fatigue behavior - [02, 90 4 ] s configuration 1 1
39,39 2 1 25
3 1
35,02 1 1 15 to 20
2 1
laminate. Tables 6 and 7 list the number of macrocracks
1 1
(NF) and their length variation (LF), taking into account
30,64 2 1 10 to 20
the different number of loading cycles.
3 2
It can be seen that larger crack lengths are observed
1 2
when the specimens are subjected to higher loading
21,89 2 1 5 to 10
levels as well as damage extension reduces if the
3 1
loading value decreases. This behavior can be easily
explained: if laminate is subjected to a lower level of
loading, damage occurs little by little, from matrix
microcracking till delamination onset at 0790° interface. value of the loading applied. On the other hand, if
Damage appears as macrocracks with small lengths, as a smaller values of loads are applied, damage
consequence of the gradual cyclic loading process. development occurs as previously described.
It was also noticed that [04, 90 2 ] s laminates have a Comparing LF results, it is observed that even when
peculiar failure mode when subjected to extreme loads: subjected to lower loading [02, 90 4 ] s specimens
cracks appear simultaneously in different places at the presented larger crack lengths than [04, 90 2 ] s ones. At
laminate edge. As a typical example, in Table 6 the the same time, a larger quantity of macrocracks was
occurrence of 8 macrocracks can be seen for the highest noticed in [04, 90 2 ] s configurations. This behavior is in

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Vol. 10, No. 1, 2002 Free Edge Delamination

agreement with the conclusions of the Endurance Tests,


where it has been seen that the addition of 0° plies in
laminate makes crack propagation difficult.
Independently of the laminate type, the damage
aspect was similar. Figures 13 to 16 show that, even
considering different levels of loading, the damage
process was characterized by the occurrence of
macrocracks, secondary microcracks, and sometimes,
delamination onset. This behavior was expected because
all tests were interrupted when the first indication of
damage was noticed.

Fig. 15: [0 2 , 90 4 ] s specimen failed at 70 cycles with σ


= 35,02 MPa - Magnification 200 X

Fig. 13: [0 4 , 90 2 ] s failed specimen at 05 cycles with σ


= 69,54 MPa - Magnification 100 X

Fig. 16: [0 2 , 90 4 ] s specimen failed at 5704 cycles with


σ = 21,89 MPa - Magnification 500 X

CONCLUSIONS

Quasi-static tests showed that [0 m , 90 2 ] s (m—>4, 6)


specimens withstand higher loads levels than [0 2 , 90 n ] s
(n-»4, 6) ones. Considering fatigue tests, it has been
performed endurance and characterization analyses in
[0 2 , 90 6 ] s and [0 6 , 9CL2]S. ponfigurations. In Endurance
Tests, the occurrence wa$ noticed of delaminations at
0790° interface in [0 2 ,i90 6 ] s specimens, denoting the
fragility of this laminate configuration. On the other
Fig. 14: [0 4 , 90 2 ] s failed specimen at 1280 cycles with hand, taking into account damage characterization
σ = 46,36 MPa - Magnification 200 X analysis, quite different behavior has been noticed for

42
F.A. Netto and S.F. Estefen Science and Engineering of Composite Materials

each configuration type: no damage was observed in [06, Onset and Growth in a Composite Laminate".
90 2 ] s specimens although failure process was noticed in Damage in Composite Materials. ASTM STP 775,
its plenitude for [02, 90 6 ] s configurations. Considering pp. 140-167, 1982.
[02, 904]s and [04, 90 2 ] s specimens, the results allowed to 5. T.K. O'Brien, "Analysis of Local Delaminations
plot the laminate fatigue behavior for each configuration and their Influence on Composite Laminate
type. As expected, the results indicated that [02, 90 4 ] s Behavior", Delamination and Debonding of
configurations are more sensitive to damage than [04, Materials. ASTM STP 876, pp. 282-297, 1985.
90 2 ] s ones. Therefore, the results showed that the 6. T.K. O'Brien; G.B. Murri and S.A. Salpekar,
addition of 90° plies in laminate causes beneficial "Interlaminar Shear Fracture Toughness and
conditions for damage appearance. Fatigue Thresholds for Composite Materials".
Composite Materials: Fatigue and Fracture,
ASTM STP 1012, pp. 222-250, 1989.
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"Tension Fatigue Analysis and Life Prediction for
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Composite Materials Structures", D.Sc. Thesis (in Fatigue, 11 (6), 379-393 (1989).
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Federal University of Rio de Janeiro, Rio de Delamination Onset in Fatigue". In: Proceedings
Janeiro, Brazil, 1999. of International Conference on Advanced
2. T.K. O'Brien, "Local Delamination in Laminates Composite Materials, Wollengeng, Australia,
with Angle Ply Matrix Cracks, Part I: Tension 1993.
Tests and Stress Analysis", Composite Materials: 9. R.A. Shenoi and J.F. Wellicome, "Composite
Fatigue and Fracture, ASTM STP 1156, v. 4, pp. Materials in Maritime Structures - Volume 1:
491 - 506, 1993. Fundamental Aspects", Cambridge University
3. T.K. O'Brien, "Local Delamination in Laminates Press Editor, 1993.
with Angle Ply Matrix Cracks, Part II: 10. F.A. Netto and S.F. Estefen, "Application of Strain
Delamination Fracture Analysis and Fatigue Energy Release Rate Concept in the Study of Edge
Characterization", Composite Materials: Fatigue Delamination Growth for Composite Structures",
and Fracture, ASTM STP 1156, v. 4, pp. 507 - 537, Proceedings of Sixth International Conference of
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