Low-temperature mechanical properties of

glass/epoxy laminates
Cite as: AIP Conference Proceedings 1574, 109 (2014); https://doi.org/10.1063/1.4860612
Published Online: 17 February 2015

R. P. Reed, M. Madhukar, B. Thaicharoenporn, et al.

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 Low-Temperature Mechanical Properties of
Glass/Epoxy Laminates

R. P. Reeda, M. Madhukarb, B. Thaicharoenpornb, and N. N. Martovetskyc

a
Cryogenic Materials, Inc., Boulder, CO 80305
b
Magnet Development Laboratory, Knoxville, TN 37996
c
US-ITER Project, Oak Ridge National Laboratory, Oak Ridge, TN 37830

ABSTRACT. Selected mechanical properties of glass/epoxy laminate candidates for use in the electrical turn and ground
insulation of the ITER Central solenoid (CS) modules were measured. Short-beam shear and flexural tests have been
conducted on various E-glass cloth weaves/epoxy laminates at 295 and 77 K. Types of glass weave include 1581, 7500,
7781, and 38050, which represent both satin and plain weaves. The epoxy, planned for use for vacuum-pressure
impregnation of the CS module, consists of an anhydride-cured bisphenol F resin system. Inter-laminar shear strength,
flexural elastic modulus, and flexural strength have been measured. The data indicate that these properties are dependent on
the volume percent of glass. Short-beam shear strength was measured as a function of the span-to-thickness ratio for all
laminates at 77 K. Comprehensive fractography was conducted to obtain the failure mode of each short-beam shear test
sample.

KEYWORDS: Glass/epoxy laminates, short-beam shear test, flexural strength, interlaminar shear strength, flexural
modulus, E-glass fabrics, electrical insulation.

INTRODUCTION

Electrical protection for large superconducting coils consists of turn, possibly layer, and ground insulation. For the
Central Solenoid (CS) of ITER, the turn insulation is glass and Kapton tape wound around stainless steel conductors
that contain the superconductor. The ground insulation is glass cloth, Kapton (sheet) film, and G-10CR (high-
pressure laminate) panels. The types of glass cloth and tape in these insulation systems is selected based on their
thickness, density, pliability (for ease in winding), and type of weave.
In selection of appropriate electrical insulation for coils, the designer must consider available space, resin flow (if
a vacuum-pressure impregnation [VPI] resin transfer process is used), and mechanical and electrical design criteria
requirements. In the case of the horizontal ground insulation for the CS Modules, compressive loads (up to 91 x 10 3
kg, 100 tons) are applied on the lower sections. Previous resin permeability tests [1,2] have demonstrated that resin
flow through glass cloth under compressive loads is a function of the density (areal density/cloth thickness, where
the areal density is the planar density of the cloth, in units of g/cm2) of the glass cloth. Type 7500, which has a much
lower density that type 7781, a commonly used glass tape, was found to be a good candidate for use to increase resin
permeability in the horizontal ground insulation under large vertical compressive loads. This report compares some
of the important mechanical properties at 295 K and 77 K of composite laminates that contain selected types and
amounts of various glass-cloth weaves.
Three-point bend tests were conducted at room temperature and 77 K on epoxy-based, glass-reinforced laminates.
The glass cloths included types 7781 and 1581 (satin weaves with higher densities), 7500 (plain weave with lower
density), a 7781/7500 hybrid with a combination of both 7781 and 7500 cloth, and 38050 (a low density, plain
weave). Both short-beam shear (low span-to-sample thickness ratio) and flexural (high span to sample thickness
ratio) measurements wee conducted. Both sample fabrication (VPI process) and testing were conducted at the
Magnet Development Laboratory, Inc. in Knoxville, TN.

Advances in Cryogenic Engineering

AIP Conf. Proc. 1574, 109-116 (2014); doi: 10.1063/1.4860612
© 2014 AIP Publishing LLC 978-0-7354-1204-0/$30.00

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 MATERIALS AND TEST PROCEDURES

The resin used for all laminates had been used for the ITER-CS Model Coil [3] and is planned for use for the CS
Modules. It consists of 100 parts by weight (pbw) DGEBF epoxy (Aradite GY 282), 82 pbw MTHPA hardener
(Aradur 918), and 0.25 pbw accelerator (DY-073-1). Huntsman Corporation supplied all components.
All of the glass cloth in this program was E-glass. The types of glass cloth and the layups that were used for
reinforcement of the laminates are listed here:
7781 – satin weave, 0.23 mm thick, areal density = 0.0304g/cm2, density = 1.33g/cm3
laminate #1: thickness = 3.75 mm, 16 plies cloth, volume % glass = 51.0
laminate #2: thickness = 2.29 mm, 8 plies cloth, volume % glass = 44.5
7500 – plain weave, 0.36 mm thick, areal density = 0.0326g/cm2, density = 0.92g/cm3
laminate#3: thickness = 3.75 mm, 10 plies cloth, volume % glass = 34.0
7781/7500 hybrid –
laminate #4: 8 plies 7781 cloth, 5 plies 7500 cloth; thickness = 3.75 mm, volume % glass = 42.5
1581 – satin weave, 0.23 mm thick, areal density = 0.031g/cm2, density = 1.35g/cm3
laminate #5: thickness = 2.21 mm, 7 plies cloth, volume % glass = 38.7
38050 – plain weave, 0.100 mm thick, areal density = 0. 089g/cm2, density = 0.890g/cm3
laminate #6: thickness = 2.18 mm, 2 plies cloth, volume % glass = 32.1
The lay-up of glass plies in the hybrid laminate consisted of 8 layers of 7781 cloth and 5 layers of 7500 in the
following symmetric order: 7781/7781/7500/7781/7500/7781/7500/7781/7500/7781/7500/7781/ 7781.
All glass products had epoxy-compatible (Volane) finishes with the exception of type 38050, whose glass contained
no special finish. The glass densities listed above were computed using handbook values of the areal density/weave
thickness. There were no visible voids or porosity in the resin in laminates # 1-5; in laminate # 6, containing glass
cloth that contained no epoxy-compatible finish, there was evidence of resin porosity and lack of coherent
resin/glass fiber interfaces. The laminates were produced using the vacuum-pressure impregnation process [3] which
did not include the application of added pressure following initial resin fill and during the hold and gel stages of the
cure cycle.
Three-point bend tests were conducted with different span (S)-to-specimen thickness (t) ratios (S/t) to obtain both
short-beam shear (S/t = 2.8 – 9) and flexural measurements (S/t = 18 - 20) at 295 and 77 K. Each specimen width
was 6.2 mm. Other details about short-beam shear testing of composite laminates have been discussed previously [4]
and the ASTM D-2344 test standard was followed [5]. The two end supports for the bend tests were 6.3 mm radius
cylindrical pins and the center loading cylindrical bar (12.7 mm diameter) was machined to a radius of 2.3 mm for
contact with the specimens. All tests at 77 K were conducted in liquid nitrogen.
The shear stress (τ) was calculated using:

τ = 0.75 P/wt (1)

where P is the applied load, w is the specimen width, and t is the thickness of the specimen. The bending (flexural)
strength (σb) was calculated using:

σb = 1.5 PS/wt2 (2)

The bending (flexural) modulus (Eb) was calculated using:

Eb = PS3/4wt3δ (3)

where δ is the deflection increment at mid-span.

For accurate measurement of the interlaminar shear strength (ILSS), the span-to-sample thickness ratio (S/t)
must be varied for each laminate. The failure mode is examined after testing at various S/t ratios. The failure stress
that corresponds to the S/t ratio that results in interlaminar shear failure is taken as the ILSS. The procedure is
repeated for each type of material and each test temperature. In this series of tests, S/t ratios that varied from 2.8 to
9.0 were used. Various types of failure modes are illustrated in Figure 1 for different S/t ratios. Flexural tests, with
very large S/t ratios (18.4-20.4), result in tension failure modes. Interlaminar shear cracking occurs in the S/t ratios
that separate the compression and tension-controlled crack arrays. Cracks propagate through the resin system for

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interlaminar shear failures; but, for compressive, tensile, and diagonal shear failures, cracks also propagate through
layers of glass cloth. This latter failure mode requires the extensive fracture of glass strands.

FIGURE 1. Typical failure modes of short-beam shear samples as a function of the span-to-sample thickness ratio.
Flexural test samples fail under the tension failure mode.

RESULTS
The shear and flexural properties derived from the test data are summarized in Table 1. Volume percent glass of
each type of laminate is also included, calculated from the relation: volume % glass = (# glass plies x areal fabric
density)/ (laminate thickness x density of glass). Averages of all test data, including the laminate that did not contain
an epoxy-compatible finish on its glass fabric (laminate # 6), were included. Data spreads ranged from +/-5% to +/-
15% for 5-9 samples per test for each property (shear strength and flexural) at each temperature. In Table 1 for
laminates # 1, 3, and 4, the S/t for the ILSS data were taken at S/t ratios of 5, 7.5, and 7, respectively and the S/t for
the flexural tests was 18.4. The S/t for laminates 2, 5, and 6, was 20.4 for the flexural tests.
For comparison and for use in plotting, estimates of the epoxy shear and tensile strengths and modulus were
obtained from typical epoxy data contained in the report by Reed and McColskey [6]. The epoxy data included in
Table I, and in the subsequent figures, represent average-value estimates from data obtained for a range of epoxies.
Tensile modulus and strength data of flat dog-bone samples are included for comparison with the flexural test data
and shear data, obtained with torsion tests, are included for comparison with the interlaminar shear strength data.
The shear strengths at 77 K versus S/t ratios for laminates are shown in Figure 2. As described in earlier work [4],
there is a linear dependence of the shear strength at failure versus S/t ratio. For type 7781 laminates, interlaminar
shear failures occurred at an S/t ratio of 5. For the 7500/7781 type laminate a diagonal shear failure, combined with
occasional interlaminar cracking, was present for S/t ratios of 5 – 6 and interlaminar shear failure was observed at
the S/t ratio of 8. For type 7500 laminate, no interlaminar cracking was observed. However, multiple, diagonal
cracks (compression dominated) were present in the S/t range 4-6 and tension-dominated, diagonal cracks were
observed in the S/t range 8-9; therefore, interlaminar cracking was assumed to occur at the (untested) S/t ratio of 7.
The measured shear strength of composite laminates is dependent on the S/t ratio. In Figure 2 this dependence is
shown for the three laminates that were tested and all glass fabrics appeared to have the same dependence. In Figure
2 the open data points represent the occurrence of interlaminar-shear cracking.

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 TABLE 1. Average values of 295 K and 77 K test data
________________________________________________________________
Laminate # volume interlaminar shear flexural elastic flexural
Glass type % glass strength, MPa modulus, GPa strength, MPa
295K 77K 295K 77K 295K 77K
#1-7781 51.0 69 90 25 28 620 1030
#2-7781 44.5 --- --- 22 24 650 1010
#3-7500 34.0 67 49 18 20 420 740
#4-7781/7500 42.5 70 58 21 24 520 940
#5-1581 38.7 --- --- 20 21 560 850
#6-38050 32.1 --- --- 7.6 8.5 200 330
Epoxy 0 70 120 4 7 70 180

FIGURE 2. Shear strength at 77 K versus span-to-sample thickness (S/t) ratio. Each data point an average of 5-9 tests. Type
7500 interlaminar shear mode is estimated at S/t = 7. Open data points represent interlaminar- shear cracking in the samples.

The shear strength at room temperature is plotted as a function of the test span-to-specimen thickness ratio in
Figure 3. Note that there is also an apparent linear dependence of shear strength on S/t for these data. This
dependence is less than at 77 K (see Figure 2, also). Similarly, the shear strength of the data at 295 K is dependent
on the glass content of the laminate, with the 7781 laminate having higher shear strengths, per S/t ratio, than the
other laminates.
The dependence of the interlaminar shear strength and flexural strength and modulus on glass content are
illustrated in Figures 4 - 6. The ILSS is plotted versus volume % glass in Figure 4. Note that at room temperature,
the shear strength is independent of glass content and averages about 70 MPa, the same value as the average shear
strength of neat epoxy resins[6]. At 77 K, ILSS is dependent on glass content for the laminate specimens and
decreases with decreasing glass content. But, very surprisingly, the ILSS of the laminates are lower than the nominal
shear strength of epoxy neat resins at 77 K.

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Figure 3. Shear strength data at 295 K for three laminates with varying glass contents. Note less dependence on S/t ratio than at
77 K (Figure 2). All data at span-to-thickness ratios between 2.7 and 4 represented interlaminar shear failures.

The flexural strength and stiffness are dominated by the glass content of the composite laminate. In these tests
with long span-to-thickness ratios, the stresses on the laminate are primarily tensile (see Figure 1). In Figure 5 the
flexural strengths of all laminates and the nominal tensile strength of epoxy are shown as a function of glass content.
At 77 K the strengths are both larger and more dependent on glass content, compared to room temperature. The data
of the sample of the volume glass content of 32 % are inconsistent with the other data and reflect the poor quality of
this type 38050 glass laminate. As described earlier, these samples contained a glass fabric that did not have an
epoxy-compatible finish, thus the laminates contained areas of lack of resin/glass bonding and, also, considerable
resin porosity.
In Figure 6 the flexural modulus of all laminates and the tensile modulus of epoxy are plotted as a function of
glass content. The equivalent trend of the modulus as a function of the glass content at both temperatures indicates
the dominant role of glass content on the flexural modulus. The modulus increases about 10 % from 295 to 77 K.
Similar to the flexural strength, the data at 32 volume % glass are not compatible with other data. This again reflects
the relatively poor quality of the 38050 laminate.
In their order of strengths, the types of glass cloths/tapes are ranked as follows: 7781 (highest strength), 1581,
7500, and 38050 (lowest strength). This ranking is directly associated with the volume percent glass in each
laminate.

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 140

120
interlaminar shear strength, MPa

100

80 77 K

60
295 K

40

20

0
0 10 20 30 40 50 60
volume glass, %
FIGURE 4. Average interlaminar shear strength at 295 and 77 K as a function of volume % glass for laminates 1, 3, and 4 and
the shear strength of epoxy resin [6]. See Figure 2 for S/t ratios for each laminate.

FIGURE 5. Average flexural (in-plane) strength dependence on volume % glass at 295 and 77 K and tensile
strengths for epoxy resin [6]. S/t ratios of 18.4 and 20.4 for laminate samples, see text for sample identification.

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FIGURE 6. The dependence of the average flexural modulus on volume % glass at 295 and 77 K. The tensile moduli of epoxy
at these temperatures are also included [6]. See Table 1 for descriptions of each data point.

DISCUSSION AND SUMMARY

These tests demonstrate the following:

(1) The flexural strength and flexural elastic modulus of glass/epoxy laminates are linearly dependent on
the volume percent glass, both at 295 and 77 K, in the range from pure (neat) resin to over 50 volume
percent glass. In flexural and tensile tests the failure mode includes the fracture of glass fibers, thus the
dependency on the quantity of fibers. And, the elastic modulus of E-glass fiber is considerably larger
(~72.5 GPa at 295 K) than the epoxy modulus; this results in considerable stiffening of the laminate
with glass addition. The linear dependency of the elastic modulus (Figure 6) on glass content does not
extrapolate to the modulus of the fiber, owing to the effect of fiber curvature and orientation within the
glass cloths. The dependencies of the flexural modulus on glass content at 295 and 77 K are
equivalent; but the dependence of the flexural strength on glass content is higher for the 77 K data,
compared to the 295 K data.
(2) The shear strengths of these laminates are linearly dependent on the S/t ratio (Figures 2 and 3) and on
the volume percent glass (not plotted) at both test temperatures.
(3) The ILSS of composite laminates is marked by a failure path through the resin, between plies of glass
cloth. At 295 K, the ILSS is dependent on the strength of the resin, independent of the glass content. At
77 K, the ILSS is considerably lower than the neat resin shear strength, but is also dependent on glass
content. This dependency indicates that the fracture of some glass fibers plays a role in ILSS failures at
77 K. Since it has previously been demonstrated that the tensile strength of neat resins is dependent on
flaw size [6], we postulate that the 77 K ILSS is dependent on the fracture toughness of the resin
system since the failure mode must also continue to be within the resin and adjacent glass plies. Glass
content has also been shown to affect, secondarily, the magnitude of the ILSS at both temperatures.
This explanation, that the presence of small flaws in the resin system effects the low temperature ILSS
of laminates, is also supported by the reported ILSS of G-10CR [7} of about 150 MPa from short-
beam shear tests. This high-pressure laminate (cured at about 10 MPa [1500 psi] as opposed to 0.21
MPa [30 psi] for the laminates of this test series) is expected to contain much smaller and fewer defects
and lower porosity with about 53 volume percent glass.

115
 (4) In one composite laminate, type 38050, the glass cloth did not contain an epoxy-compatible surface
finish and this laminate contained excessive porosity and lack of fiber/epoxy adhesion The bend shear
and flexural properties of this laminate were substandard compared to the other laminates and did not
correlate well with their dependence on glass content.
Figures 5 and 6 demonstrate that the flexure modulus and strength laminate data as a function of volume percent
glass can be extrapolated to the resin tensile modulus and strength. The disparity between the ILSS at 77 K, and the
correlation of the ILSS at 295 K, with the corresponding neat resin shear strength have also been identified. The
disparity at 77 K between the ILSS of neat epoxy resin and epoxy /glass laminates has not been previously
discussed. This disparity demonstrates that interlaminar cracking of resin that separates laminate layers occurs
prematurely to the cracking of the resin in pure, neat resin samples. This must be initiated by flaws within the resin
system that have been influenced either by the glass cloth or, more likely, by the processing parameters.. It has
previously been demonstrated that the fracture of neat resins is dependent on its fracture toughness and on internal
flaw size [6]. The ILSS of G-10CR laminates has been reported [7] to be 140-150 MPa at 77 K This value is
equivalent to, or slightly larger than, the shear strength of the neat resin. The large difference between the ILSS of
G-10CR compared to the laminates in this project is likely due to the presence of added pressure during the resin
cure cyle of the G-10Cr (a high-pressure laminate). The laminates in this study were VPI-fabricated without the
addition of pressure during the hold and gel stages of the cure cycle, whereas about 10 MPa is applied during the
cure cyle of G-10CR. This argues for the application, during the VPI resin cure cycle, of as high a pressure that can
be managed, based on VPI mold design.
In selection of appropriate electrical insulation for coils, the designer must consider available space, resin flow (if
a VPI resin injection process is used), and mechanical and electrical property design criteria. In the case of the
horizontal ground insulation for the CS Modules, compressive loads (up to 90 x 10 3 kg) are applied on the lower
sections. Previous resin permeability tests have demonstrated that resin flow through glass cloth under compressive
loads is a function of the density (areal density/cloth thickness) of the glass cloth [2]. When type 7500 cloth was
substituted for type 7781 cloth, an increase of at least a factor of 8 can be achieved in resin flow during the VPI
process. Thus, there is a trade-off for selection of the type of glass for insulation systems. Higher glass cloth
densities result in higher laminate densities and improved properties, but also result in less resin permeable
conditions during the VPI process under compressive load. The reductions in strengths and elastic modulus at 77 K
for laminates reinforced with E-glass type 7500, compared to type 7781, are about 20 % for the flexural (in-plane
elastic) modulus, 30 % for the flexural (in-plane tensile) strength, and 45% for the ILSS.

REFERENCES

1. R. Reed, F. Roundy, and P. Biermann, “The Flow of Epoxy Resin under Compressive Load through Holey
Kapton Sheet and Glass Cloth”, Cryogenic Materials, Inc. (Boulder, CO) and S.A. Composites (Loveland, CO),
report to US-ITER project, Oak Ridge National Laboratory, Oak Ridge, TN (November 5, 2010).
2. R. P. Reed, N. N. Martovetsky, “Fabrication of an ITER CS Module Cross-Section”, To be published, Advances
in Cryogenic Engineering-Materials, vol 60 (2014).
3. R. P. Reed and P. Clark, “Vacuum-Pressure Impregnation of U.S. CS Model Coil”, Cryogenic
Materials, Inc., Boulder, CO, Radius Engineering, Inc., Salt Lake City, UT, U.S. ITER report to
Plasma Physics Center, M.I.T., Cambridge, MA (March, 1999).
4. R. P. Reed, J.B. Darr, and J. B. Schutz, “Short-Beam Shear Testing of Candidate Magnet Insulators”,
Cryogenics, vol. 32, ICMC Supplement (1992), pp, 9-13.
5. American Society for Test Standards, D-2344-04, Short-Beam Shear Test Standards, ASTM, Philadelphia, PA.
6. R. P. Reed and J. D. McColskey, “Composite Struts for SMES Plants”, NISTIR 5024, National Institute of
Standards and Technology, Boulder, CO (1994).
7. R. P. Reed, J.B. Darr, J. B. Schutz, “Short-Beam Shear Testing of Candidate Magnet Insulators”,
Cryogenics, ICMC Supplement, vol. 32 (1992), pp. 9-13.

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