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Mode- I Interlaminar Fracture Toughness of Carbon Fiber Composites

Brad J. Tribley
Junior, Department of Aerospace Engineering
Texas A&M University

ABSTRACT: Composites are one of the main focuses of current materials science. Given their unique properties,
characterizing these materials holds great value for future material development. Through experimental Double
Cantilever Beam testing, this paper characterizes the interlaminar fracture toughness of EPON 862 woven Carbon
fiber composites. The objective of this research is to quantify the strength characteristics of the composites as a
foundation for comparison with nano-reinforced composites. Preliminary results see an increase in fracture
toughness of the nanotube reinforced composite in comparison with the unmodified specimen.

INTRODUCTION
Composite materials are becoming
commonplace in the aerospace industry.
Nanotechnology has given promise to a
new, exciting dimension to materials
science. As these materials develop,
characterization is required for product
development. Testing is a vital ingredient in
determining the livelihood of nano-
reinforced composites [4]. In this light, the
fracture toughness provides a strong
quantitative investigation of composite
strength.

Fracture toughness may be described as the
critical energy a material may absorb before
failure. Independent of specimen geometry,
this property describes the general resistance
of a material to delaminate [5]. In
interlaminar fracture, there are three modes
of delamination: Mode I (figure 1), mode II,
and mixed mode [2].


Figure 1: Mode-I Delamination

The purpose of this paper is to study the
effect of nanotube reinforcement for the
mode-I interlaminar fracture toughness of
woven carbon fiber composites. By using a

Double Cantilever Beam (DCB) testing, one
can isolate fracture surface in a purely
Mode-I delamination. This paper reviews
the fracture toughness values for sample
with and without nanotube reinforcement in
the midplane.

EXPERIMENTAL SETUP
Specimen
All testing specimen are fabricated using a
high temperature vacuum resin transfer
molding process using EPON 862 with
curing agent W. The fabric composites are
composed of IM7 Carbon fiber woven in a
satin weave pattern.

The specimen without nanotube
reinforcement, provided by Texas A&M
Aerospace Engineering, is a 20 ply
specimen with a Teflon-coated polyethylene
film, for crack starting, inserted 2.5in
(63mm) in the midplane.

Additionally, the nanotube specimen is
composed of .05wt% single wall nanotubes
(SWNT) on the midplane. Provided by Rice
University, this 12ply specimen has
equivalent thickness to the unmodified
specimen.

For visual assistance of the crack path, the
specimen edges were coated with white
painting primer. Two piano-style hinges are
Formatted: Number of columns: 1,
Force equal column width
Deleted:
Deleted:
Section Break (Continuous)
Deleted: The quantitative value for the
interlaminar fracture toughness can be
calculated [1]:
ba
nP
G
c c
IC
2

= [J/m
2
], where
) P (
x
y
n
a
b
c
Pc
c c
log vs / log for
length on Delaminati
cimenwidth Averagespe
failure at nt Displaceme
failue at Load

=
=
=
=
=
2
bonded to the specimen end using 3M DP-
460 epoxy cured at 50C for a minimum of
three hours.


Figure 2: Image of Testing Specimen

Testing Apparatus
A 20kip Material Testing System (MTS)
machine is utilized for load application
during the DCB test. Standards call for a
crosshead speed or displacement rate of 1 to
three 5mm/min; however, a 3mm/min speed
is recommended [1]. A 300lb Transducer is
attached to the MTS machine for continuous
load and displacement data collection. To
minimize the amount of data, collection was
achieved at a rate of 5Hz.

For optical viewing of the crack
propagation, a Questar QM100 Long
Distance Microscope is positioned at a
working distance of about 13in. The
microscope is positioned on a Questar
microscope stage with three axis
maneuverability. For coarse adjustments,
the stage is attached to an industrial tripod.

To obtain crack length measurements during
testing, a dial indicator with a 5in travel
range is utilized. Attached to the
microscope stage, this analog indicator will
produce crack length measurements to an
accuracy of a thousandth of an inch (.001).

Control of the testing environment is
achieved by the Station Manager software
package for the MTS load frame.
Parameters such as crosshead speeds and
loading rates are manipulated by the
software.

PROCEDURE
Double cantilever beam testing is used as
the approach for calculating fracture
toughness values. Test parameters such as
cross head speeds, specimen geometry,
specimen tolerances are adopted from the
ASTM 5528 standards for the mode-I
interlaminar fracture toughness.

Specimens are attached to the MTS machine
for testing via a hinge system. The bonded
hinges are connected to the load frame by a
steel-fabricated hinge which is inserted in to
the machine grips. A steel pin connects the
bonded hinges to the grip hinges.

The testing schedule consists of loading the
specimen at a specific rate, as specified by
standards, until the crack is arrested. At this
point, delamination data is recorded. This is
accomplished by focusing the long distance
microscope over the crack tip and recording
the displacement of the dial indicator. The
specimen is then unloaded back to zero.
This entire process is controlled through the
Station Manager software which coordinates
with the MTS load frame, and it is repeated
multiple times for each specimen and their
crack measurements.

Upon completion of the test, post processing
is required to achieve fracture toughness
values. Standards call for three different
data reduction methods. For testing, the
compliance calibration method was chosen.
This method relates the fracture toughness
with a relationship between compliance and
delamination lengths. Load-displacement
and compliance-delamination length curves
are used to compile parameters that affect
the mode-I fracture toughness value.

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The quantitative value for the interlaminar
fracture toughness can be calculated [1]:
ba
nP
G
c c
IC
2

= [J/m
2
], where
(a) ) P (
x
y
n
a
b
c
Pc
c c
log vs / log for
length on Delaminati
cimenwidth Averagespe
failure at nt Displaceme
failue at Load

=
=
=
=
=


To achieve the value for n, a log-log plot of
delamination length versus compliance is
required. Using a least squares
approximation, the slope of the log(
c
/P
c
)
versus log(a) yields the value of n.

Both testing and post processing are
conducted similarly for each specimen.

RESULTS
Figures 3 and 4 (see additional page)
summarize the load-displacement curves for
the two specimen. It is to be noted that to
speed up the test, the unmodified specimen
was not unloaded completely. Table 1 gives
the initiation and average propagation
toughness values for the two specimen. The
resistance curve, or R-Curve, is shown in
Figure 5 (see additional page) and reflects
both specimen data. Since the modified
specimen is without a crack starting film, the
initiation toughness values cannot be
determined. Based on this data along with
compliance and delamination data, the
fracture toughness values are achieved and
expressed in Figure 5 (see additional page)
and Table 1.

Table 1: Initiation and propagation G
IC

Fracture Toughness: G
IC
(J/m
2
)

Specimen Initiation Propagation Avg.
Unmodified 218 364
Modified NA 772
Although the analysis is only preliminary,
there are numerous differences between the
two samples. For the unmodified specimen,
rapid crack propagation and sudden load
drops was noticed in the load-displacement
curve at the time of crack propagation. This
occurred at each interval of the test, and
indicates unstable crack propagation. This
characteristic may be a sign of rachetting
which states that a small, secondary crack
originates ahead of the arrested primary
crack [3]. In addition to the possibility of
rachetting, there are signs of ply bridging
in both specimens (more significantly in the
modified specimen).

As shown in Figure 6, the modified sample
experiences instances where the crack would
propagate around the weave pattern of the
specimen.


Figure 6: Ply bridging in the modified specimen

As the crack propagated through the
specimen, it would jump in certain places
between plies. One justification for this
occurrence is that nanotubes may exist at the
points of discontinuity. This could possibly
conclude that nanotubes are a strengthening
mechanism as it requires greater energy to
bridge plies before delamination occurs. Due
to the crack jumping plies, the toughness
values do not really represent the toughness
of the nano-reinforced mid-plane. Thus,
even though the data for the modified
sample is not strictly valid, it does show that
nanotubes hold a toughness effect. These
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values may represent only a starting point
for further investigation. In the case of the
modified sample with the nanotubes, the
yielded toughness values may represent the
lower bound for the fracture toughness.

A final remark in regards to specimen
parameters is that the unmodified specimen
has twice the number of plies than the
modified specimen. Noting that the
specimen had the same thickness, this leaves
the modified specimen with a higher resin
concentration. This increased resin
concentration may explain some of
delamination values and the associated
fracture toughness values.

The objective of this test is to investigate the
nanotube reinforcement and compare it to
the unmodified specimen.

CONCLUSION
The effect of nanotube reinforcement on the
mode-I fracture toughness of woven carbon
fiber composites was studied. Specimens
were tested using a double cantilever beam.
Preliminary testing and results have
concluded that nanotubes strengthen the
material; however, the data presented in the
paper represents only an initial study of
nanotube reinforcement. Through scatter in
data due to ply bridging, it can be assumed
the concluded toughness values signify the
lower bound of a woven carbon fiber
composite with nanotube reinforcement.

Much more research is required in the future
to supplement the data presented. First and
foremost, a nanotube reinforced specimen
with a midplane crack starter film must be
tested. This will provide a stronger
comparison between the unmodified and
modified specimens. Also, to expand the
scope of study, one must conduct tests that
would study mode-II and mixed mode
delamination. This might assist in removing
the issues of crack jumping. Additionally,
including tests of unidirectional samples will
provide a better comparison and range of
samples.

By expanding the scope of study through
different samples, sample preparation, and
testing modes, a more precise comparison
can be made. This enhanced test matrix can
provide a better justification for nanotube
reinforcement and ultimately influence the
development of future nano-materials. This
test has created a starting point for greater
investigation.




ACKNOWLEDGEMENT
This Research Experience for Undergraduates (REU) Site is sponsored the National Science
Foundation NSF Grant No. 0453578, Air Force Office of Scientific Research, U.S. Air Force,
Department of Defense, NASA Cooperative Agreement NCC1-02038, and Air Force Research
Laboratory.

I would like to thank my research advisor, Mr. Patrick Klein, for his continual efforts and
assistance throughout the entire project. I would like to further thank my faculty mentor, Dr.
Dimistris Lagoudas, for always guiding the project and keeping my objectives in sight.




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REFERENCES

[1] ASTM D5528-01: Standard Test Method for Mode I Interlaminar Fracture Toughness of
Unidirectional Fiber-Reinforced Polymer Matrix Composites

[2] Alif, N. Carlsson, L.A. and Gillespie, J.W. Mode I, Mode II, and Mixed Mode Interlaminar
Fracture of Woven Fabric Carbon/Epoxy, Composite Materials: Testing and Design,
Thirteenth Volume, ASTM STP, S.J. Hooper, Ed. American Society for Testing and
Materials, 1997.

[3] Paris, I., Minguet, P.J., and OBrien, T.K., Comparison of Delamination Characterization
for IM7/8552 Composite Woven and Tape Laminates, Composite Materials: Testing
and Design Fourteenth Volume, ASTM STP 1436, C.E. Bakis, Ed., ASTM Interational,
West Conshohocken, PA, 2003.

[4] Thosetenson, E.T., Ren, Z., and Chou, T., Advances in the science and technology of carbon
nanotubes and their composites: a review, www.elsevier.com.

[5] Whitney, J.M., Browning, C.E., and Hoogsteden, W., A Double Cantilever Beam Test for
Characterizing Mode I Delamination of Composite Materials, Reinforced Plastics and
Composites, Volume One, 1982. pp 297-313.
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ADDITIONAL FIGURES

EPON 862 Carbon Fiber (Non-Reinforced)
DCB Test
0
10
20
30
40
50
60
70
0 5 10 15 20
Displacement (mm)
L
o
a
d

(
N
)

Figure 3: Load-displacement for unmodified sample

Nano-Reinforced Carbon Fiber Composite
DCB Test
0
50
100
150
200
250
300
350
400
450
500
0 1 2 3 4 5 6
Displacement (mm)
L
o
a
d

(
N
)

Figure 4: Load-displacement for modified specimen

Specimen Comparison
Resistance Curve
0
100
200
300
400
500
600
700
800
900
1000
0.0 20.0 40.0 60.0 80.0 100.0 120.0
Delamination Length (mm)
G
I
C

(
J
/
m
^
2
)
SWNT
Without Nanotubes


Figure 5: Resistance Curves for both test specimen