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Mechanical Properties of Polyester Resin Formed by Resin Transfer Moulding

(RTM)

Article · January 2004

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Mechanical Properties of Polyester Resin
Formed by Resin Transfer Moulding
(RTM)

M. Davallo*, A. N. Wilkinsona, P. Ziaratib

*
Dept. of Chemistry, Islamic Azad University (North Branch), 9th Iranian Chemical Engineering Congress
P.O.Box 19136, Tehran, Iran
a
Dept of Chemistry and Materials, Manchester Metropolitan Iran University of Science and
University, Manchester, England Technology
b
Dept of Pharmaceutical Sciences, Islamic Azad University, Tehran 23-25 November, 2004
19419, Iran
m_davallo@yahoo.com

Abstract
Mechanical behaviour of polyester matrix formed by resin transfer moulding (RTM) has
been studied to determine several important parameters, such as tensile and
compressive/strain responses, single edge-notch tensile (SENT) fracture toughness,
fracture energy and flexural properties. Fracture toughness, KIC, and fracture energy,
GIC, obtained for the polyester matrix lie between the typical values for epoxy resins and
polystyrene.
From experimental strain failure of the polymer matrix, theoretical mode-I delamination
fracture energy of a composite was found to give a value of GIC of ≈ 600 J m-2, which agrees
well with experimental values of propagation GIC for bidirectional composites.

Keyword: Polyester Resin, Flexural Test, Resin Transfer Moulding, Onset of Damage
Part9: Polymer Engineering 4057

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Introduction
The matrix forms a significant volume fraction of a polymer composite and it has a number of
critical functions; it binds the reinforcements together, maintains the shape of a component and
transfers the applied load to the reinforcing fibres. it protects the reinforcing fibres from
degradation, due to abrasion or environmental attack.
it contributes significantly to the mechanical properties of structural polymer composites,
acting to resist delamination between plies of reinforcements and to inhibit fibre buckling
during compression. Thermoplastics are used in certain applications but constitute a relatively
small sector of the structural composites market. Matrices used for structural composites are
mainly thermosetting plastics, such as polyester resins, epoxy resins, phenolic resins and vinyl-
ester resins. Polyester resins are the most widely used resin systems, particularly in the marine
industry. By far the majority of dinghies, yachts and work-boats built in composites make use
of this resin system. Thermosetting plastic systems generally consist of liquid mixtures of
relatively low molar mass reactants, such as monomers and/or prepolymers, which polymerise
upon heating to form highly-crosslinked, network polymers [1-9].

Experimental
Materials. The polymer matrix used for moulding sheets of resin based on Synolite 1077-N-3
(ex. DSM Resins), a low-viscosity unsaturated polyester resin of the orthophthalic type. It is
especially suitable for resin transfer moulding (RTM) due to its low viscosity and non-
thixotropic nature.
Curing System. The curing agent used was a cobalt naphthenate accelerator/methyl-ethyl-
ketone peroxide (MEKP) initiator system of 0.40/1.0 weight ratio, respectively (ex. Glasplies
Ltd). The cobalt accelerator was a solution of cobalt salts diluted in styrene and white spirit of
6% (w/w) cobalt content, which was mixed into the resin first, before the MEKP initiator. The
initiator was a solution of MEKP diluted in dibutyl phthalate of 50% (w/w) MEKP content.
This cure system was chosen to allow cure to occur in a reasonable time, in order to allow
sheets of resin to be moulded before gelation occurs. To determine reactivity a pre-mixed resin
(0.2 g accelerator/ 0.5 g MEKP and 50 g resin) was poured upon an in-mould dielectric
sensor (AGC sensor, ex. Plastech Thermoset Tectonics) and allowed to react from an initial
mould temperature of 40 0C. The sensor output is the voltage generated from the electrolytic
chemical activity of the resin system during its transition from liquid to a solid form. Hence, a
signature of the sensor output versus time was obtained (gelation time, tg of ≈ 17 minutes,
induction time, ti of 6 minutes).
Moulding. A Plastech Thermoset Tectonics Hypaject-3 resin transfer moulding (RTM)
machine was used to mould sheets of various thicknesses. All sheets were moulded using an
injection pressure of 0.20 MPa and a mould temperature of 40 0C.
Mechanical Testing. Tensile data for the polymer matrix were obtained at 20±2 0C using a
Hounsfield, HTE10K universal tensometer. Tests were conducted on at least five specimens
(dumb-bell specimens), according to BS 2782 Part 3 Method 320C [10], at a cross-head rate
of 5 mm min-1. The fracture properties of the matrix were measured in a single edge-notch
tensile (SENT) geometry using rectangular specimens of length (L) 150 mm, width (w) 25 mm
and thickness (b) 6.49 mm. Tests were conducted at 20±2 0C, using a J.J. Lloyd M30K screw-

9th Iranian Chemical Engineering Congress (IChEC9), Iran University of Science and Technology (IUST), 23-25 Nov., 2004
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driven tensometer at a cross-head rate of 5 mm min-1. At least ten specimens were tested and
the nominal notch depth of the specimens, a, was varied to give a/b ratios in the range 0.30 ≤
a/b ≤ 1.80. The actual notch depths, a, were measured, after fracture, to within 0.01 mm using
a travelling microscope. A linear-elastic fracture mechanics analysis was used to determine
fracture toughness, KIC, according to;

K2IC = σ2f Y2 a (1)

where σf is the stress at fracture and Y is a calibration factor that depends on the crack length
and specimen dimensions. For specimens with a single-edge crack, Y, is given as [11];

Y =[1.99 - 0.41 (a/w) + 18.70 (a/w)2 - 38.48 (a/w)3 + 53.85 (a/w)4] (2)

Plots of σ2f Y2 versus a-1 were linear with slope equal to K2IC. Fracture energy, GIC was
determined according to;

GIC = K2IC / E (3)

where E is the elastic modulus of the polymer matrix. However, this expression is only valid if
the thickness, b, of the specimen satisfies the criterion;

b ≥ 2.5 (KIC / σy)2 (4)

where σy is the yield stress of the polymer matrix. The yield stress of this brittle matrix was
determined by compression testing, using at least five specimens of 20 mm x 20 mm and
thickness 6.49 mm. The tests were conducted at 20±2 0C, using a J.J. Lloyd M30K screw-
driven tensometer at a cross-head rate of 5 mm min-1.
Flexural Testing of Polymer matrix. The flexural properties were determined in three-point
bending. At least five rectangular beam specimens were tested at a support span-to-depth ratio
of 16:1 according to ASTM, D790M [12]. Tests were conducted at 20±2 0C, using a J.J.
Lloyd M30K screw-driven tensometer. Specimens were centre loaded in 3-point bending as a
simply supported beam, using 3 mm diameter supports and loading bar. The maximum tensile
stress in the outer fibres was calculated according to [12];

σm = 3PL / 2bd2 (5)

where P is the load at a given point on the load-deflection curve, L is the support span and b
and d are the width and depth of the beam, respectively. The modulus of elasticity was
calculated according to;

E = L3m / 4 bd3 (6)

where m is the slope of the tangent to the initial straight-line portion of the load-deflection curve.

9th Iranian Chemical Engineering Congress (IChEC9), Iran University of Science and Technology (IUST), 23-25 Nov., 2004
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The maximum tensile strain in the outer fibres was calculated according to;

ε = 6Dd / L2 (7)

where D is the deflection of the beam at a given point on the load-deflection curve.

Results and Discussion

Tensile data for the polyester matrix were obtained according to BS 2782, Part 3 [10]. A
typical stress-strain plot for the matrix is shown in Figure 1. The curve shows linear
deformation behaviour with the force rising to a maximum value (Fm) where fracture occurred.
The Young's modulus, E, of the polyester matrix was calculated from the slope of the curve.
Fracture toughness is a measure of a material's resistance to crack propagation, but in a
composite this can be hard to measure accurately. However, the stress/strain curve of the resin
system on its own provides some indication of the material's toughness. Generally the more
deformation the resin will accept before failure the tougher and more crack-resistance the
material will be. It should also be noted that when a composite is loaded in tension, for the full
mechanical properties of the fibre component to be achieved, the resin must be able to deform
to at least the same extent as the fibre. The fracture properties of the polyester matrix were
measured in a single edge-notch tensile (SENT) geometry using rectangular specimens (length
150 mm, width 25 mm and thickness 6.49 mm). Figure 2 shows a plot of (σfY)2 versus a-1 data
obtained from SENT tests, from which the fracture toughness KIC can be calculated according
to equations 1 and 2 presented earlier [11]. The plot of (σfY)2 versus a-1 is linear with a slope
equal to K2IC. A linear regression fit to this data through the origin gave a value of fracture
toughness, KIC of 0.33 MPa m1/2 with a correlation coefficient of R=0.91. The fracture energy,
GIC, was determined according to equation 3 [11]. However, plane strain fracture parameters
are only obtained if the thickness, b, of the specimen satisfies the criterion in equation 4 [11].
In tension fracture occurred at 52±2.54 (MPa) and there was no sign of yielding before
fracture. Thus, the yield stress in tension was determined using [1];

σyC / σy ≈ 1.3 (8)

where, σyC is the yield stress of the polyester matrix determined in compression (Figure 2).
During compression testing, large scale yielding occurred at a yield stress of 135±3 (MPa).
Thus, the critical value of b calculated using equation 4 was 0.025 mm and the specimens
(b = 6.49 mm) easily satisfy the criterion. From the yield stress, σy, and the stress intensity
factor, KIC, plastic deformation/damage zone size, 2rp of the polyester matrix was estimated
according to [11];

2rp = (KIC/σy)2 / 3π (9)

which gave the length of the damage zone size ahead of the crack ≈ 1.1 µm.

9th Iranian Chemical Engineering Congress (IChEC9), Iran University of Science and Technology (IUST), 23-25 Nov., 2004
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200

180

160

140

120

Stress (MPa)
100

80

60

40

20
Tension
Compression
0
0 2 4 6 8 10 12 14
Strain (%)

Figure 1: Typical stress versus strain curves for the polyester matrix

60

50

40
2
(ofY) (MPa)

30
2

20

10

0
0 100 200 300 400 500

1/a (m-1)

Figure 2: A plot of (σfY)2 versus a-1/m-1 curve for the polyester matrix

The flexural properties of the polymer matrix were determined according to ASTM D790M
[12]. The maximum stress in the specimen, σm, the modulus of elasticity, E, and the strain in
the outer fibres, εC, were calculated according to equations 5 to 7. The tensile, flexural and
fracture parameters obtained for the polyester matrix are shown in Table 1 and Table 2,
respectively.

Table 1: Tensile properties of the polyester matrix (± 95% confidence limits)

Tensile
Stress Modulus Strain
at Fracture at Fracture
σm (MPa) E (GPa) εC (%)

52±2.54 1.05±0.20 4.6±0.1

9th Iranian Chemical Engineering Congress (IChEC9), Iran University of Science and Technology (IUST), 23-25 Nov., 2004
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Table 2: Flexural and fracture properties of the polyester matrix (± 95% confidence limits)
Fracture Fracture
Flexural
Toughness Energy
Stress Modulus Strain
at Fracture at Fracture KIC GIC
σm (MPa) E (GPa) εC (%)
(MPa m1/2) (J m-2)

71.1±1.2 4.3±0.45 2.0±0.40 0.33 105

In 3-point flexure, the specimen is subjected to a combination of tensile and compressive

stresses. As the compressive moduli of polymers are relatively high, flexural testing results in
higher values of modulus and ultimate stress but lower values of ultimate strain compared to
tensile tests. The flexural values determined for the bidirectional composites [13] were
significantly higher than that for the neat polyester resin (see table of 2), indicating that fracture
resistance was not solely due to resin. Polyester resins, without reinforcement, are relatively
brittle polymers and the fracture toughness, KIC, and fracture energy, GIC, obtained for the
polyester matrix lie between the typical values of KIC and GIC reported [11] for epoxy resins
(0.5 MPa m1/2, 100 J m-2) and polystyrene (1.1 MPa m1/2 , 400 J m-2). The matrix toughness
plays an important role in the interlaminar fracture behaviour of composites. It is reported by
Bradley [14] and Jordan et al [15] that decreasing the yield strength of the matrix increases
delamination fracture energy by increasing the size of the plastic deformation or non-linear
viscoelastic zone ahead of the crack tip, resulting in greater load redistribution away from the
crack tip and hence more crack-tip blunting. However, there is a relatively low efficiency of
translation of a high matrix GmIC value into the delamination fracture energy of a composite,
due mainly to constraint provided by the fibres in the confined spaces between the reinforcing
plies which restricts the size of the plastic deformation zone [14-17]. Thus, a decrease in fibre
Vf can result in a smaller degree of crack tip constraint, giving larger deformation/damage zone
sizes and, consequently, higher composite GC values in either mode-I and mode-II. In contrast,
very efficient translation of GmIC into delamination fracture energy is observed in composites
made with brittle matrices, due to the full development of the small plastic deformation zones
which occur in these matrices.
Bradley [14] reported that increasing matrix GmIC above an initial value of 70 J m-2 resulted in
significant increases in composite GIC, but that further increases in matrix GmIC ( > 400 J m-2)
resulted in a poor translation of GmIC values into composite GIC. Similar results were reported
by Russell and Street [16], in that the incremental increase in composite GIC that resulted from
increasing GmIC above 400 J m-2 was much smaller than the incremental increases observed as
GmIC was increased from 100 to 400 J m-2. Jordan et al [15] proposed that the tensile elongation
can be related to mode-I delamination fracture energy for a composite material, expressed by;
log10 GIC = 2.14 + 1.16 log10 (el) - 0.31 {log10 (el)}2
where (el) is the tensile elongation (strain at failure) of polymer matrix in percent. Using equation
above with the experimental strain at failure of the polyester matrix (4.6%, see Table 1) gave a

9th Iranian Chemical Engineering Congress (IChEC9), Iran University of Science and Technology (IUST), 23-25 Nov., 2004
Part9: Polymer Engineering 4062

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value of GIC of ≈ 600 J m-2, which agrees well with experimental values of propagation GIC for the
bidirectional composites [18].
Conclusions
1. Polyester matrix formed by resin transfer moulding (RTM) was studied to determine several
important mechanical parameters.
2. Tensile stress and strain at failure of the neat resin was found 52 MPa and 4.6%
respectively.
3. Fracture toughness, KIC, and fracture energy, GIC, obtained for the polyester matrix lie
between the typical values for epoxy resins and polystyrene, which was found 0.33 MPa m1/2
and 105 J/m2 respectively.
4. Using experimental tensile elongation of polymer matrix, theoretical delamination fracture energy
of a composite was found to give a value of GIC of ≈ 600 J m-2 (almost 6x higher than neat polyester
resin), which agrees well with experimental values of propagation GIC for bidirectional composites.
5. The flexural values determined for the neat polyester resin (without reinforcement) are
relatively brittle than reinforced polyester composites by a factor of 1.5x to 4.5x.

9th Iranian Chemical Engineering Congress (IChEC9), Iran University of Science and Technology (IUST), 23-25 Nov., 2004
 Part9: Polymer Engineering 4063

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9th Iranian Chemical Engineering Congress (IChEC9), Iran University of Science and Technology (IUST), 23-25 Nov., 2004

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