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Mechanical testing and microstructure characterization of glass fiber


reinforced isophthalic polyester composites

Article  in  Journal of Materials Research and Technology · June 2019


DOI: 10.1016/j.jmrt.2019.06.003

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Original Article

Mechanical testing and microstructure


characterization of glass fiber reinforced
isophthalic polyester composites

Ritesh Bhat, Nanjangud Mohan ∗ , Sathyashankara Sharma, Ashu Pratap,


Agastya Prasad Keni, Dev Sodani
Mechanical Engineering, Manipal Institute of Technology, Manipal Academy of Higher Education, Manipal 576104, Karnataka, India

a r t i c l e i n f o a b s t r a c t

Article history: The present work investigates the effect of material geometry in terms of material thickness
Received 25 May 2019 on the mechanical properties of glass fiber reinforced isophthalic polyesters. The tensile
Accepted 1 June 2019 strength, flexural strength, and Barcol hardness quantify the mechanical properties in this
Available online xxx article. The experimental tests as per the ASTM standards show that the tensile strength
and hardness increase with the increase in the thickness of laminates. The flexural strength
Keywords: is determined to decrease with the increasing thickness of laminates. The statistical anal-
Glass fiber ysis through ANOVA test shows that material thickness is a significant factor affecting the
Isophthalic polyesters mechanical properties with 83.88, 70.37, 97.63 and 62.19% contribution toward the vari-
Mechanical testing ance in the tensile strength, Young’s modulus, flexural strength, and hardness respectively
Microstructure characterization within the selected range of values for glass fiber reinforced isophthalic polyesters. The ten-
Tensile failure modes sile failure mode analysis indicates that the increase in the thickness of laminates increases
ANOVA delamination failure. It is also found that the anisotropic behavior of the composites leads
to an angular failure of the specimen in the tensile test. The random orientation of fibers
leading to anisotropic behavior and increasing voids/decreasing interfacial bonding with
the increasing laminate thickness is visualized in the microstructural studies through SEM
images.
© 2019 The Authors. Published by Elsevier B.V. This is an open access article under the
CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

application in hull casing, sonar dome, and masts of the sub-


1. Introduction marine. Other non-transportation application of FRP includes
deck gates, low-pressure underwater pipes, storage tanks, and
Composite materials, particularly fiber reinforced polymer civil infrastructures [1].
(FRP) are most often used in marine crafts such as canoes, The excellent functional properties compared to con-
fishing trawlers, patrol boats, and naval ships. It also finds the ventional metals, good resistance to fatigue, and corrosion

Abbreviations: FRP, fiber reinforced polymer; GFRP, glass fiber reinforced polymer; SEM, scanning electron microscope; ANOVA, analysis
of variance.

Corresponding author.
E-mail: ns.mohan@manipal.edu (N. Mohan).
https://doi.org/10.1016/j.jmrt.2019.06.003
2238-7854/© 2019 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).

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emphasizes the use of FRP composites in the marine industry


Table 1 – Thickness and the corresponding number of
[2]. Though there exists a good number of choices of rein- layers for the manufactured composite sheets.
forcement, for its economic advantage, the emphasis for bulk
S. No. Thickness (mm) Number of layers (N)
use is firmly on the glass fiber compared to the carbon and
aramid fiber for the marine applications. There do exist high- 1. 6 8
performance crafts which employ the combination of carbon 2. 8 11
and aramid fibers, but the glass fiber still accounts for over 3. 10 14

95% of the utilization in the maritime applications [3].


Polyester resins are one amongst the most popular and the popularity of the hand lay-up process, the same has been
widely used matrix material in the glass fiber reinforced poly- employed in the current work to make the required glass fiber
mer (GFRP) composites used for the maritime applications reinforced polymer composites.
[4–6]. Polyester resins are categorized broadly into two types The chopped stranded mat of E-glass fiber of 450 GSM with
viz., orthophthalic polyester resins, also known as standard randomly oriented fibers is used as the reinforcing material
economic polyester resins, being widely used in several indus- and the marine grade isophthalic polyester resin is used as
trial applications and isophthalic polyester resins, which is the matrix or the binding material. The methyl-ethyl-ketone
trending to be the preferred matrix material in the marine peroxide (MEKP) is used as the hardener and mixed in the ratio
industry for its superior water resistance properties [7]. The of 0.012:1 (hardener to resin). The resins, fiber mats, and the
prior is prepared using phthalic anhydride, maleic anhydride hardener are procured from Shri Mookambika poly products,
or fumaric acid and glycols, whereas; the latter is prepared by Udupi, Karnataka, India. The standard 2:1 ratio (glass fiber t0
replacing phthalic anhydride by isophthalic acid [8]. the polyester matrix) is followed for making the composite
Evaluating the mechanical property of materials is of the laminates. Composites of dimensions 300 mm × 300 mm are
utmost importance in any application. Various researchers made each for three different thickness values of 6, 8, and
have dedicated their time in investigating the mechanical 10 mm. The number of layers required for fabricating each of
property of fiber reinforced polymer matrix composites in the three variants is calculated using Eqs. (1)–(3), where is the
aged as well as unaged conditions concerning the marine thickness of constituent, Tc1 and Tc2 are the thickness of rein-
applications. Awaja et al. [9] in their comprehensive review, forcement and matrix materials respectively, Ta is the total
emphasized the prevention of crack propagation in the marine thickness of one layer of composite laminate and T is the total
application-based glass fiber reinforced polymers. Jang et al. desired thickness. Table 1 details the number of layers calcu-
[10] in their research work investigated the effect of gel-coats lated for each of the three variants of manufactured composite
used in the fiber reinforced polymer composites used in the sheets. m and d in Eq. (1) represents the mass and density
marine industry on the tensile strength and hardness. Tran values.
et al. [11] investigated the pyrolysis effect on marine-based
GFRP composites and proposed a possible solution to impro- m
Tc = (1)
vise it. Jesthi and Nayak [12] proposed a way of hybridizing d
the glass and carbon fibers to improve the mechanical prop- Ta = Tc1 + Tc2 (2)
erties of marine application-based fiber reinforced composite
materials. T
N= (3)
Though isophthalic polyesters are the trending replace- Ta
ment to the general purpose orthophthalic polyester resins,
only a few have focused on investigating the mechanical prop- 2.2. Experimental method
erty of it concerning the marine application. Also, there has
been no much focus of the researchers in investigating the 2.2.1. Tensile test
effect of variation in thickness on the mechanical property. The mechanical properties in terms of the ultimate tensile
Considering the research gaps, the present work focuses on strength, tensile strain, and Young’s modulus are determined
investigating the mechanical properties in terms of tensile, by employing ASTM D3039 standard for determining the ten-
flexural strength, and Barcol hardness of glass fiber reinforced sile properties of a polymer matrix composite [16]. Five flat
isophthalic polyesters used in marine applications. The work strips specimens with rectangular cross-section are cut from
also discusses in detail regarding the modes of tensile failure each of three thick composites. The strips are mounted in the
as per the ASTM standards. grips of Unitek 9450 computerized universal testing machine,
as shown in Fig. 1, which is monotonically loaded in tension
while recording the applied load. The ultimate strength of the
2. Materials and methods specimen is determined for the maximum load carried before
failure. The stress–strain responses are recorded to determine
2.1. Material preparation Young’s modulus for each specimen. The mode of failure also
is noted, concerning the ASTM D 3039 standards, as shown in
Hand lay-up method is one of the simplest and oldest Fig. 2.
techniques of manufacturing the fiber reinforced polymer
composites [13–15]. It is also the most economical process 2.2.2. Flexural test
compared to its counterparts like resin transfer molding and The mechanical property in terms of the flexural stiffness or
vacuum process. Considering the economic advantage and strength is determined by employing ASTM D7264 standard

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Fig. 3 – Flexural strength testing using Instron 3366 UTM.

Table 2 – Details of specimens for the flexural test.


S. No. Thickness (mm) Length (mm) Width (mm)

1. 6 36 12
2. 8 48 16
3. 10 60 20

for determining the flexural properties of a polymer matrix


composite [17]. The specimens are supported as a beam and
deflected at a constant rate. The point load is applied at the
midpoint from the supporting end. The force thus applied
Fig. 1 – Tensile strength test using Unitek 9450 to the specimen and the resulting specimen deflection at
computerized universal testing machine. the mid-portion is measured and recorded until the failure
occurs on either of the two surfaces. The Instron 3366 UTM
is employed for accomplishing the discussed test and shown
in Fig. 3. The details of specimens for flexural or three-point
bending test are given in Table 2.

2.2.3. Hardness test


The mechanical property in terms of hardness is determined
by employing ASTM D2583 standard for determining the
Barcol hardness of a polymer matrix composite [18]. Five spec-
imens with 30 mm × 30 mm dimension are cut from each of
three thick composites. The specimens are dry conditioned at
room temperature for 48 h before testing as per the require-
ment of ASTM 2583 standard. The hardness test is then
conducted in the laboratory at ambient atmospheric condi-
tions. The indentations created on each of the specimens are
at least 3 mm away from the edge of the specimen and each
other. The indentation is done only on the smooth surface,
which is coated by the polyester resin. On each specimen, five
readings are recorded. The specimens prepared and tested for
hardness is shown in Fig. 4.

3. Results and discussion

3.1. Tensile test experimental and statistical results

The results obtained for the conducted tensile test as per


Fig. 2 – Modes of failure during the tensile test in a polymer
the ASTM D3039 standard are given in Tables 3 and 4. The
matrix composite specimen [16].
stress–strain graph representing the maximum recorded

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Fig. 4 – Prepared and tested specimens for Barcol hardness


test.

Table 3 – Tensile test results concerning the ultimate


tensile strength for 6, 8, and 10 mm thick GFRP
specimens.
Sample No. Ultimate tensile strength (MPa) Fig. 6 – Analysis of tensile strength for the tested specimen.
6 mm 8 mm 10 mm

1 120.89 127.63 145.03


2 121.65 138.45 150.68 Table 5 – ANOVA results for tensile strength.
3 110.10 134.74 149.70 Source DF Adj SS Adj MS F-value P-value
4 115.89 128.44 144.80
5 119.03 128.07 139.72 Factor 2 2027.1 1013.54 46.63 0.000
Average 117.51 131.46 145.99 Error 12 260.8 21.74
Total 14 2287.9

Table 4 – Tensile test results concerning Young’s


modulus for 6, 8, and 10 mm thick GFRP specimens. Table 6 – ANOVA results for Young’s modulus.
Sample No. Young’s modulus (MPa) Source DF Adj SS Adj MS F-value P-value

6 mm 8 mm 10 mm Factor 2 1593207 796604 14.25 0.001


Error 12 670786 55899
1 3231.35 2587.14 2394.80 Total 14 2263993
2 3368.81 2858.18 2359.10
3 2575.98 2844.73 2224.43
4 3563.56 2587.43 2387.06 11.86 and 11.06% when the material thickness is increased
5 3058.90 2835.81 2443.07 from 6 to 8 mm and 8 to 10 mm, respectively. Young’s modulus
Average 3159.72 2742.66 2361.69 decreased by 13.12 and 13.89% when for material thickness
increased from 6 to 8 mm and 8 to 10 mm, respectively. The
results indicate that the thickness has a significant effect on
the tensile strength and Young’s modulus in case of glass fiber
reinforced isophthalic polyesters.
The one-way analysis of variance (ANOVA) test results
for tensile strength and Young’s modulus are given in
Tables 5 and 6. The ANOVA result for tensile strength at 95%
confidence interval validates the obtained experimental result
and proves that there is a significant effect of thickness on the
tensile strength, as the obtained ‘P-value’ is less than the ˛
value of 0.05.
The high range of ‘F-value’ of 46.63, being greater than the
Fcrit = 3.7, proves the fact that the variance within the group
is lesser than the variance between the group. Thickness is
Fig. 5 – Comparison of stress–strain curves for the proved to contribute 88.6% toward the variance in the tensile
maximum tensile strength values. strength corresponding to a very high degree of correlation
(94.12%).
values concerning the three different thickness is shown in The ANOVA result for Young’s modulus at 95% confidence
Fig. 5. The obtained stress–strain graph indicates the brittle interval validates the obtained experimental result and proves
nature resulting in the catastrophic failure of the prepared that there is a significant effect of thickness on Young’s mod-
composite as there exist no yield points before the fracture ulus, as the obtained ‘P-value’ is less than the ˛ value of
mechanism. The bar chart of tensile strength versus thick- 0.05. The high range of ‘F-value’ of 14.25, being greater than
ness is shown in Fig. 6. The tensile strength increased by the Fcrit = 3.7, proves the fact that the variance within the

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Fig. 9 – Fractured specimen of 10 mm thickness after the


tensile test.

Fig. 7 – Fractured specimen of 6 mm thickness after the of the specimen [19]. Table 7 also indicates that three out of
tensile test. five specimens had an angular type of failure instead of lateral
failure. The reason for the angular failure is the anisotropic
characteristic of the composites [20]. The orientation of the
fibers has a significant influence on the mechanical property
[21]. The anisotropic behavior is highly induced in the com-
posites having randomly oriented fibers [22] as is the case
of the composite specimens prepared for the current study.
Specimens 3 and 4 faced delamination type of failure, wherein
the damage primarily occurred due to the separation of layers
from each other [23]. The delamination failure is developed
generally due to excessive inter-laminar stresses generated at
the interfaced between adjacent piles. The delamination fail-
ure in the specimen during mechanical testing can also be
known as premature failure.
The same is evident from Table 3, wherein specimens 3 and
4 demonstrate a lower tensile strength compared to the other
three for the 6 mm thick laminate. Table 8 indicates that all the
specimens bearing 8 mm thickness demonstrate the angular
type of failure at the top end. As discussed earlier, the angular
failure indicates the anisotropic behavior due to randomly ori-
Fig. 8 – Fractured specimen of 8 mm thickness after the ented fibers, and the top end failure represents the formation
tensile test. of the main chap at the top location [19–21]. Also, it is observed
from Table 8 that the majority of specimens failed at the grip.
group is lesser than the variance between the group. Thick- The reason for this being the local damage caused resulting in
ness is proved to contribute 70.37% toward the variance in excessive stress concentration due to a high clamping force
Young’s modulus, corresponding to a high degree of correla- and the absence of tabs, the presence of which provides a
tion (83.88%). cushion effect to the applied grip force [24]. Table 9 indicates
that four out of five specimens bearing 10 mm thickness fails
3.2. Tensile failure mode analysis at the top, which is an indication of high-stress concentra-
tion resulting from the high clamping force and absence of
Figs. 7–9 represent the pictures of the fractured specimens of the tab [24]. It also indicates that the majority of failures are of
6, 8, and 10 mm thickness respectively after the tensile test. delamination type because of the combined effect of increased
From Fig. 7, it is evident that the mode of fracture varies in the thickness of laminates and the high clamping force at the grips
6 mm thick laminates. The variety of fracture modes observed [25,26].
in comparison to the standard codes as per the ASTM stan-
dards is given in Table 7 for 6 mm thick samples. Table 7 shows 3.3. Flexural test experimental and statistical results
that all the specimen fail at the top location. The reason being
the formation of the main chap causing the stress concentra- The results obtained for the conducted flexural strength test
tion at the top end portion. Though multiple chap formation is as per the ASTM D7264 standard is given in Table 10. The
the actual phenomenon, the formed main chap at the top por- results indicate that the thickness has a significant effect
tion inhibits the further development of chaps at other portion on the flexural strength in case of glass fiber reinforced

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Table 7 – Mode of failures in 6 mm thick specimen as per the ASTM D3039 standards.
Specimen number (left to Mode of failure as per the First character (Failure type) Second character Third character
right in Fig. 6) ASTM standards (Failure area) (Failure location)

1 AGT Angular Gage Top


2 AAT Angular At the grip Top
3 DGT Delamination Gage Top
4 DGM Delamination Gage Middle
5 AAT Angular At the grip Top

Table 8 – Mode of failures in 8 mm thick specimen as per the ASTM D3039 standards.
Specimen number (left to Mode of failure as per the First character (Failure type) Second character Third character
right in Fig. 6) ASTM standards (Failure area) (Failure location)

1 AGT Angular Gage Top


2 AAT Angular At the grip Top
3 AAT Angular At the grip Top
4 AAT Angular At the grip Top
5 AAT Angular At the grip Top

Table 9 – Mode of failures in 10 mm thick specimen as per the ASTM D3039 standards.
Specimen number (left to Mode of failure as per the First character (Failure type) Second character Third character
right in Fig. 6) ASTM standards (Failure area) (Failure location)

1 LGT Lateral Gage Top


2 DAT Delamination At the grip Top
3 DAT Delamination At the grip Top
4 DMV Delamination Multiple areas Various
5 DAT Delamination At the grip Top

Table 10 – Flexural test results for the 6, 8, and 10 mm


thick laminate specimens.
Sample No. Flexural strength (MPa)

6 mm 8 mm 10 mm

1 329.36 310.43 213.60


2 323.71 284.06 212.16
3 317.91 295.61 225.26
4 322.38 294.00 229.98
5 325.28 291.38 212.79
Average 323.73 295.10 218.76

Table 11 – ANOVA results for flexural strength.


Source DF Adj SS Adj MS F-value P-value

Factor 2 29443.3 14721.7 246.75 0.000


Error 12 716.0 59.7
Total 14 30159.3
Fig. 10 – Analysis of flexural strength for the tested
specimen.
isophthalic polyesters and is found to reduce with the increase
in the thickness of laminates. Fig. 10 represents the reduc-
tion observed in the flexural strength with the increase in the
thickness of the composite laminates. The flexural strength variance within the group is lesser than the variance between
decreased by 8.84 and 25.87% when the material thickness the group. Thickness is proved to contribute 97.63% toward the
increased from 6 to 8 mm and 8 to 10 mm, respectively. variance in the flexural strength corresponding to a very high
The same has been validated statistically using the one-way degree of correlation (98.81%).
ANOVA test given in Table 11. The ANOVA result for flexu- The increase in the thickness of laminates increases the
ral strength at 95% confidence interval validates the obtained fiber volume or content in the composites. Though researchers
experimental result and proves that there is a significant effect state that the increase in the fiber content in the compos-
of thickness on the flexural strength, as the obtained ‘P-value’ ites solely causes a reduction in the flexural strength of
is less than the ˛ value of 0.05. The high range of ‘F-value’ of the laminates [27], the stated reason stands hypothetical as
246.75, being greater than the Fcrit = 3.7, proves the fact that the there is a constant ratio of glass fiber to matrix maintained

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Table 12 – Barcol hardness test results for the 6, 8, and


10 mm thick laminate specimens.
Sample Barcol hardness number (HB) (average of
No. 5 points on a specimen)

6 mm 8 mm 10 mm

1 43.40 46.60 45.40


2 45.80 49.20 52.40
3 42.40 48.40 49.40
4 42.20 45.40 48.80
5 42.60 43.80 52.60
Average 43.28 46.68 49.72

Table 13 – ANOVA results for Barcol hardness.


Source DF Adj SS Adj MS F-value P-value

Factor 2 103.79 51.896 9.87 0.003 Fig. 11 – SEM image for the 6 mm thick glass fiber
Error 12 63.10 5.259 reinforced polyester composites.
Total 14 166.90

inconsiderate to the thickness of the material. The actual rea-


son for the tremendous decrease in the flexural strength is the
decrease in the compression strength [28] of the upper surface
of the fiber, which is less supported by the matrix [29].

3.4. Hardness test experimental and statistical results

The results obtained for the conducted Barcol hardness test as


per the ASTM D2583 standard is given in Table 12. The results
indicate that the thickness has a significant effect on the hard-
ness in case of glass fiber reinforced isophthalic polyesters
and is found to increase with the increase in the thickness
of laminates. The Barcol hardness increased by 7.86 and 6.51%
when the material thickness increased from 6 to 8 mm and 8 to
10 mm, respectively. The same has been validated statistically
using the one-way ANOVA test given in Table 13.
The ANOVA result for flexural strength at 95% confidence Fig. 12 – SEM image for the 8 mm thick glass fiber
interval validates the obtained experimental result and proves reinforced polyester composites.
that there is a significant effect of thickness on the hardness,
as the obtained ‘P-value’ is less than the ˛ value of 0.05. The
high range of ‘F-value’ of 9.87, being greater than the Fcrit = 3.7,
proves the fact that the variance within the group is lesser
than the variance between the group. Thickness is proved to
contribute 62.19% toward the variance in the hardness corre-
sponding to a nearly high degree of correlation (78.86%). The
hardness is defined as the resistance to permanent indenta-
tion or penetration. In simple words, it is the resistance to
the plastic deformation [30]. The increase in thickness implies
the increase in fiber layers. The increase in the fiber contents
increases the hardness of the composites [31,32]. The same
effect is seen in the experimental test results.

3.5. Microstructural studies

The microstructure of the fabricated glass fiber reinforced


isophthalic polyester composites is investigated using the
scanning electron microscopic (SEM) analysis. The SEM Fig. 13 – SEM image for the 10 mm thick glass fiber
images of 6, 8, and 10 mm specimen are shown in Figs. 11–13, reinforced polyester composites.
respectively. From the obtained SEM images, it is evident that
the compact interfacial bonding between the glass fiber and

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the isophthalic polyester resins decreases with the increase in


the thickness. The compact bonding between the reinforcing
Competing interest
fiber and binding matrix is high in 6 mm specimen and least
in 10 mm specimen. The authors declare that there is no competing interest.
The voids increase with the increase in thickness, which
validates the previously obtained results of decrease in the
flexural strength and occurrence of the delamination during Funding
the tensile test with the increase in the thickness. The ran-
dom orientation of glass fibers is also observed, which leads The present work did not receive any funding from private,
to anisotropic behavior, leading to angular failure of the spec- government, and non-government organization.
imen during the tensile testing.

Availability of data
4. Conclusions
All the data are available with the authors and can be provided
In the present work, the contingency of mechanical prop- on request.
erty over the material thickness is investigated on the glass
fiber reinforced isophthalic polyester composite material. The
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