97

6
Single-Fiber Tensile Testing and
Matrix Characterization Tests
6.1 Introduction
Fiber tests are used extensively for quality control purposes and evalua-
tion of the effect of potentially detrimental fber surface treatments. They
are also used to evaluate environmental degradation of fbers and to deter-
mine mechanical properties required for input in micromechanical analysis
(Chapter 2). Most fber test methods are designed to determine the modulus
and strength of the fber in uniaxial tension, although compression tests such
as the recoil test have been approached (see Allen 1987 and Kozey et al. 1995).
6.2 Single-Filament Test
The single-flament test of ASTM (American Society for Testing and
Materials) D3379 (1989) (withdrawn in 1998) provides methods to determine
fber tensile modulus and strength. For the test, a single flament is separated
from a dry tow of fbers and mounted on a slotted cardboard tab as shown
in Figure6.1. The tabbed specimen is then inserted in a testing machine; the
supporting tab carefully cut on both sides of the fber or burned away using
a hot wire, a soldering iron, or something similar; and the unsupported sin-
gle flament tested to failure. The test requires a very low force load cell, such
as a 5- to 20-N (0.5- to 2-kg) capacity load cell. Typically, there is large scatter
in fber modulus and strength data (Van der Zwaag 1989). Hence, a large
number of specimens must be tested to obtain statistically signifcant results.
One source of variability in the test data is the fber cross-sectional area
used to determine modulus and strength. The fber cross-sectional area is
determined on the dry tow from which the fbers are selected for specimen
mounting. This means that an average cross-sectional area is used, not the
one specifc for each fber.
98 Experimental Characterization of Advanced Composite Materials
6.2.1 Single-Filament Test Procedure
Choose a suitable single flament from a strand bundle. Care must be exer-
cised to ensure that coalesced fbers are not chosen. Each fber should be
inspected under an optical microscope prior to specimen preparation. Center
the flament over the tab opening with one end taped to the tab. Lightly
stretch the flament and fx the free end to the tab using tape. Carefully place
small dots of adhesive on the flament at the slot edges to bond the flament
to the tab (Figure 6.1). The specimen gage length is defned by the length
of the open slot in the end tab, nominally 25 mm as shown in Figure 6.1.
Determine the gage length to within 0.1 mm.
Mount the specimen in the grips of a properly calibrated testing machine.
Visually check for alignment of the test specimen between the grips. Cut
both sides of the mounting tab or burn the tab away at the midgage length.
Use care not to damage the flament. Set the crosshead speed to achieve fail-
ure in about 1 min. Ramirez (2008) used a crosshead speed of 0.5 mm/min.
Apply load to the specimen while recording load and crosshead displace-
ment until the flament fails. Fibers used as reinforcements of composites
typically display linearly elastic behavior up to failure; examples of stress
strain curves for carbon and glass fbers are shown in Figure6.2.
6.2.2 Data Reduction for Modulus and Strength
The fber elastic modulus is defned as follows

E =

(6.1)
12 mm
Cement or wax dot
Paper tab
Filament
2
5

m
m
6
0

m
m
A A
FIGURE 6.1
Single-flament test specimen.
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99 Single-Fiber Tensile Testing and Matrix Characterization Tests
where is the fber stress defned by

P
A
f
=
(6.2)
where P is the load applied, and A
f
is the fber cross-sectional area. The
strain is defned as the crosshead displacement () divided by the gage
length L:

L
=

(6.3)
Notice that Hookes law, Equation (6.1), demands strain in the linear
region of material response, that is, << 1. For determining A
f
, ASTM D3379
suggests planiometering a representative number (10) of fbers using pho-
tomicrographs of the fbers to determine the average cross-sectional area.
Ramirez (2008) determined the cross-sectional area based on measure-
ments of the fber diameter with a scanning electron microscope. If the
cross-sectional area of a tested fber needs to be determined, photomicro-
graphs of the broken ends may be prepared and examined.
The strain determined from the crosshead displacement, Equation (6.3),
includes contributions from the load cell and gripping system. To accurately
determine the strain of the specimen, it is necessary to subtract the system
compliance from the apparent specimen compliance:

C C C
a s
=
(6.4)
5000
4000
3000
2000
1000
0
6 5 4 3 2 1 0
Strain, %
S
t
r
e
s
s
,

M
P
a
E-glass
S-glass
Carbon
FIGURE 6.2
Typical stressstrain curves for carbon and glass fbers loaded in tension.
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100 Experimental Characterization of Advanced Composite Materials
where C, C
a
, and C
s
are the true specimen compliance, the apparent speci-
men compliance, and the system compliance, respectively. The true speci-
men compliance is given by

C
L
EA
f
= (6.5)
where L is the gage length. ASTM D3379 suggests conducting tension testing
(as described previously) on a material similar to the flament (or the actual
flament) over a range of gage lengths at small loads to determine the appar-
ent compliance C
a
. Plotting C
a
versus gage length should result in a graph
similar to the sketch shown in Figure6.3.
The system compliance C
s
, defned as the intercept of the best-ft straight
line at L = 0 is obtained by extrapolation. The fber axial modulus E may be
determined from the slope m of the line in Figure6.3 as

1
E
mA
f
= (6.6)
where it is assumed that the fber cross-sectional area is known.
The ultimate tensile strength of the fber
f
is defned as the maximum
stress before failure [Equation (6.2)].
6.3 Matrix Test Methods
Mechanical properties of matrix materials are mostly determined for perfor-
mance evaluation and specifcation of matrix properties for product data sheets.
Such properties can be used in micromechanics models that predict composite
0
0
Gage Length, L
C
o
m
p
l
i
a
n
c
e
,

C
a
m
C
s
FIGURE 6.3
Typical graph of compliance versus gage length for a single flament.
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101 Single-Fiber Tensile Testing and Matrix Characterization Tests
properties. It should always be remembered that neat resin properties are not
necessarily equivalent to those that will be achieved by the resin in a composite.
The fber/matrix interface region in particular may differ from the bulk matrix.
The mechanical properties of the matrix material are normally measured
in tension, compression, and shear. Since the materials are usually very brit-
tle, extreme care should be exercised in preparation of specimens and in car-
rying out the test.
As described in Chapter 4, neat resin test specimens are often prepared by
molding the resin. Some resins can be cast into void-free thick bars or dog-
bone test specimens. Others are best cast into sheets. The presence of voids
in casting will cause problems with premature failures of the test specimen.
The quality of specimens is important. To the extent possible, specimen design
should follow the standards or guidelines specifed for the test procedure
used.
Strain measurement should be accomplished through the use of extensom-
eters or strain gages. If an extensometer is used, care must be taken so that
the sharp knife edges of the extensometer do not promote failure. Typically,
the specimen surfaces are smooth and glossy, and the knife edges of the
extensometer may slip. A dot of White-Out correcting fuid has been found
to enhance friction. If strain gages are used, they should be 350- resistance
(or greater) gages. Polymers do not dissipate heat very fast, and gage heating
can be a problem. Excitation voltages should therefore be kept as low as pos-
sible. Strain gages may not perform properly for high-elongation polymers
because the gage/gages tend to debond at moderate-to-large strains. This is,
however, not a problem for most thermoset matrices used in advanced com-
posites since they tend to be relatively brittle.
Polymers are often hydrophilic and sensitive to temperature changes.
Specimen conditioning and the laboratory environment should be carefully
controlled and monitored both prior to and during testing.
ASTM D638 (2010) specifes conditioning of the specimens at 23 2C and
50 5% relative humidity for at least 40 h unless otherwise specifed. Testing
should be conducted under the same conditions. Because polymers are vis-
coelastic materials and strain rate sensitive, testing speeds must be well
defned and controlled for valid comparison of data.
6.3.1 Matrix Tensile Testing
The standard tension test is described by ASTM D638 (2010). Several types of
dog-bone specimen geometries are specifed by this standard, depending on
sheet thickness and polymer rigidity. Figure6.4 shows a typical type I (rigid
or semirigid polymer 7 mm or less thick) neat resin tensile specimen geom-
etry and dimension. For modulus determination, a longitudinal strain gage
or extensometer is required. Measurement of Poissons ratio requires the use
of two strain gages, a biaxial strain gage (0/90 rosette), or a biaxial exten-
someter to measure longitudinal and transverse strains simultaneously.
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102 Experimental Characterization of Advanced Composite Materials
All specimens should be inspected to ensure that voids and surface faws
are not present. ASTM D638 specifes tolerance of thickness and gage section
dimensions of 0.4 and 0.1 mm, respectively.
ASTM D638 stipulates a crosshead speed of 5 mm/min. To conform to
most composite tests described in this text, however, a crosshead rate of
12 mm/min is recommended. Test at least fve replicate specimens.
Figure 6.5 shows a typical stressstrain curve recorded for a vinylester
matrix in tension. The specimen fails after displaying a short nonlinear
165
99.3
57
19
R76
13
FIGURE 6.4
Tensile test specimen geometry (type I). All dimensions are in millimeters.
75
50
8084 Tensile
25
0
0 1 2
Strain (%)
3 4
S
t
r
e
s
s

(
M
P
a
)
FIGURE 6.5
Stressstrain curve in tension for vinylester 8084 resin. (After Figliolini, A.M., 2011, Degradation
of Mechanical Properties of Vinylester and Carbon Fiber/Vinylester Composites Due to Environmental
Exposure, master thesis, Florida Atlantic University.)
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103 Single-Fiber Tensile Testing and Matrix Characterization Tests
response region at a strain of 3.78%. From this curve, it is possible to deter-
mine Youngs modulus E, the yield stress (
ys
), defned by a 0.2% offset strain
(see Gere and Timoshenko 1997), and the ultimate tensile strength
t
. For
this particular specimen, E = 3.01 GPa,
ys
= 52.9 MPa, and
t
= 66.1 MPa.
6.3.2 Matrix Compressive Testing
Compression testing of the matrix material is conducted for purposes of
research and development and quality control. Compressive properties
include modulus of elasticity, yield stress, and compressive strength. The
ASTM D695 (2010) standard describes test specimens of various forms, such
as sheet and solid cylindrical rod. Although ASTM D695 includes testing of
thin sheet-like materials of thickness under 3.2 mm, testing of such requires
special support fxtures, and it is recommended here to test relatively short,
solid, cylindrical rod specimens to avoid instability failures.
The standard specimen is 12.7 mm in diameter and 25.4 mm long. Such
specimens may be prepared by molding longer cylinders (see Chapter 4)
and machining the specimen in a lathe to achieve smooth and parallel end
surfaces. At least fve replicate specimens should be prepared and tested.
Figure6.6 shows a photo of an actual test specimen.
FIGURE 6.6
Compression test specimen. (After Figliolini, A.M., 2011, Degradation of Mechanical Properties of
Vinylester and Carbon Fiber/Vinylester Composites Due to Environmental Exposure, master thesis,
Florida Atlantic University.)
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104 Experimental Characterization of Advanced Composite Materials
Prior to testing, the diameter and length of the specimen are to be mea-
sured to the nearest 0.01 mm at several points. Make sure the end surfaces
are fat and parallel. Place the specimen between the parallel platens of
the testing machine, centering the specimen to avoid introduction of load-
ing eccentricities. Since the specimen is quite short, it may not be feasible
to record strain using an extensometer or a strain gage. Hence, in many
cases strain is defned as crosshead displacement divided by the original
specimen length, which does not produce reliable results. As for the single-
flament testing described in Section 6.2, improved modulus determina-
tion is obtained if the system (machine) compliance is subtracted from the
apparent specimen compliance. The machine compliance for the compres-
sion test may be determined in a way similar to the procedure suggested for
the single-flament test.
Before the actual test, the position of the crosshead of the test frame
should be adjusted until it just contacts the specimen top surface. Set the
crosshead speed at 12 mm/min and start the test while recording load and
crosshead displacement. If the specimen does not fail catastrophically but
continues to yield, the test may be interrupted.
Figure6.7 shows a typical compressive stressstrain curve for a vinylester
resin. Based on this curve, it is possible to determine an apparent elastic modu-
lus E
a
, yield stress
ys
, and compressive strength
c
.
The apparent elastic modulus E
a
, is calculated based on an apparent strain
measure (crosshead displacement/specimen length). From the stressstrain
120
90
60
S
t
r
e
s
s

(
M
P
a
)
510A Compression
30
0
0 2 4
Strain (%)
6 8
FIGURE 6.7
Compressive stressstrain curve for a 510 vinylester specimen. (After Figliolini, A.M., 2011,
Degradation of Mechanical Properties of Vinylester and Carbon Fiber/Vinylester Composites Due to
Environmental Exposure, master thesis, Florida Atlantic University.)
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105 Single-Fiber Tensile Testing and Matrix Characterization Tests
curve in Figure6.7, the following data were reduced: E
a
= 4.00 GPa,
ys
= 95.2
MPa,
c
= 115 MPa.
6.3.3 Matrix Shear Testing
One of the most important functions of the matrix in a composite is to transfer
load into the stiff and strong reinforcing fbers. Such load transfer, discussed
in more detail in Chapter 7, occurs through shear stresses at the fber/matrix
interface. Analyses of several loading situations of structural parts made
from composite materials reveal transfer of load by shear. Consequently, the
shear response of the matrix is of prime importance.
Although there is no ASTM standard for the determination of the shear
stressstrain response of matrix materials, it is widely recognized (Adams
1990, Sullivan et al. 1984) that the most promising shear test of the matrix is the
Iosipescu shear test method (ASTM D5379 2005). This standard, developed
for composite materials (Chapter 10), is schematically illustrated in Figure6.8.
As shown in Figure6.8, the V-notched test specimen is held in the fxture,
which is loaded in compression to produce a fairly uniform state of shear
stress in the center region of the specimen, between the two notches.
A detail of the test specimen is shown in Figure 6.9. The specimen may
be molded or machined from a fat plate. The top and bottom edges must
be carefully machined to be fat and parallel to each other to avoid bend-
ing and twisting deformations when load is applied. The standard fxture
allows specimens up to 12.7 mm thick, although neat resin plates typi-
cally are about 3 to 5 mm in thickness. Details of specimen preparation are
provided in Chapter 4. The specimen is instrumented in the same way as
the composite specimen (Chapter 10), typically with a two-element strain
gage rosette confgured to measure strain in the 45 and 45 directions
(Figure6.9).
P
Fixture base
Adjustable
wedge
Specimen
Fixture attached
to guide rod by
linear roller bearing
Fixture
guide rod
Wedge
adjusting
screw
Specimen
adjusting
pin
FIGURE 6.8
Schematic of Iosipescu shear test.
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106 Experimental Characterization of Advanced Composite Materials
Prior to testing, the specimen dimensions are measured at several locations
to the nearest 0.01 mm. Insert the specimen in the test fxture. Apply load at a
crosshead rate of 12 mm/min while recording load and strain until the speci-
men fails. Failure of brittle-matrix specimens tends to initiate at the notches and
propagate in the 45 plane, where the principal stress is maximum.
For reduction of the load and strain gage readings, it is recognized that the
shear stress is given by

P
A
= (6.7)
where P is the load applied, and A is the cross-sectional area of the specimen
between the notches. The shear strain is given by

= + | (45 )| | ( 45 )|
(6.8)
50
40
30
S
h
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a
r

S
t
r
e
s
s

(
M
P
a
)
20
10
0
0 2 4
Shear Strain (%)
8084 Shear
6
FIGURE 6.10
Shear stressstrain curve for vinylester 8084. (After Figliolini, A.M., 2011, Degradation of
Mechanical Properties of Vinylester and Carbon Fiber/Vinylester Composites Due to Environmental
Exposure, master thesis, Florida Atlantic University.)
76.2
11.5 19.1
R1.3
38.1
90.0
FIGURE 6.9
Details of matrix Iosipescu specimen. All dimensions are in millimeters.
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107 Single-Fiber Tensile Testing and Matrix Characterization Tests
This formula assumes that a 45 strain gage rosette, or two 45 gages, is
used. If a single gage oriented at 45 or 45 is used,

= 2| (45 )|
(6.9)
Figure 6.10 shows a representative shear stressstrain curve for a vinyl-
ester Iosipescu specimen. Data reduction allows determination of the shear
modulus G, shear yield stress
ys
, and shear strength
u
. Based on the curve
shown in Figure6.10, the following properties were reduced: G = 0.93 GPa,

ys
= 33.3 MPa, and
u
= 42.2 MPa.
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