Received: 9 February 2024 Revised: 3 April 2024 Accepted: 10 April 2024

DOI: 10.1002/pls2.10132

RESEARCH ARTICLE

Statistical analysis to examine the influence of thermal

aging on hybrid glass epoxy polymer composites
with fillers of multi-walled carbon nanotubes

K. Sravanthi 1 | V. Mahesh 2 | B. Nageswara Rao 3 | S. P. Jani 1

1
Department of Mechanical Engineering,
Marri Laxman Reddy Institute of Abstract
Technology and Management (MLRITM), E-glass fibers are widely preferred due to ease of processing and its low cost,
Hyderabad, India
which has substantial scope in the fields of electronics and electrical insula-
2
Department of Mechanical Engineering,
tion applications. Because of its low strength and corrosion resistance, use
SR Engineering College, Warangal, India
3
Department of Mechanical Engineering,
of E-glass fibers is limited in aerospace and automotive applications. There
Koneru Lakshmaiah Education is a need for enhancing the properties of the composite to overcome such
Foundation, K L Deemed to be University, limitations. Therefore, an attempt is made to introduce multi-walled carbon
Guntur, India
nanotubes (MWCNT) as fillers into E-glass fibers to meet the industry
Correspondence needs. In the current study, woven glass fiber of 5 layers and multi-walled
S. P. Jani, Department of Mechanical
nano carbon fillers of 2, 4 and 6 by wt%, LY556 epoxy resin, and HY951
Engineering, Marri Laxman Reddy
Institute of Technology and Management hardener were used to prepare 4 different type of composites along with the
(MLRITM), Dundigal, Hyderabad 500 043, neat epoxy glass fiber reinforced polymer composites (GFRP). The hand-
India.
layup route was used in the composite preparation due to its low cost, tech-
Email: [email protected]
nological feasibility, and simple process setup. The developed samples were
characterized for mechanical properties via tensile, flexural and impact
tests. Tribological characteristics were performed by air jet erosion test.
Chauvenet's criterion is applied for identifying the outliers (if any) from the
data of repeated test properties. Taguchi's L9 OA (orthogonal array) is
selected for obtaining optimal hybrid composite, which yield better mechanical
properties. Empirical relations are developed for the material properties in
terms of process variables. The sample (4 wt% MWCNT) exhibited enhance-
ment of 17.27% in tensile strength, 6% of impact strength and 7.3% of flexural
strength when compared with neat epoxy GFRP. This hybrid composite is con-
sidered for thermal aging and observed at 60
C, 8% increase in tensile, 7%
increase of impact and 15% in flexural strength due to the precipitation on car-
bon nano tubes along the gain boundaries. The present study recommends 4%
MWCNT fillers in developing hybrid glass epoxy polymer composites for use
in aerospace, automotive and civil construction industries due to economic
and technological feasibility.

This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided
the original work is properly cited.
© 2024 The Authors. SPE Polymers published by Wiley Periodicals LLC on behalf of Society of Plastics Engineers.

SPE Polymers. 2024;1–17. wileyonlinelibrary.com/journal/pls2 1

2 SRAVANTHI ET AL.

Highlights
• Utilize low-cost E-glass fibers in electronics and electrical insulation
applications.
• Improve composite properties for aerospace and automotive industries.
• Develop hybrid glass epoxy composites with 2 to 6 wt% MWCNT fillers.
• Examine wear characteristics under air jet erosion and study the impact of
thermal aging on mechanical properties.
• Apply Chauvenet's criterion for outlier identification in measured properties
datasets.

KEYWORDS
Chauvenet's criterion, erosion rate, flexural strength, GFRP, impact strength, MWCNTs,
optimization, Taguchi method, tensile strength

1 | INTRODUCTION directional strength, and stiffness, thermal and electrical

conductivity and allows tailored material properties to
Composite materials have many properties including meet specific application requirements.11–13 Incorpora-
high strength and stiffness, light-weight, superior fatigue tion of micro-carbon and nano-carbon, such as carbon
life and resistance to wear, corrosion and impact. Proper- nanotubes and graphene, into polymer matrix compos-
ties can be tailored during manufacturing according to ites can significantly improve mechanical properties,
specific application requirements. They find various appli- thermal and electrical conductivity, and barrier proper-
cations in different industries: process improvement in the ties.14,15 However, nano-sized carbon fillers provide a
automotive industry1,2; Addressing structural integrity and more significant improvement in polymer properties
maintenance challenges in the oil and gas industry2,3; due to their much higher aspect ratios and surface areas
Aerospace industry due to their desirable properties such compared to micro-fillers.
as mechanical resistance and lightness2,4; Construction The properties of composite materials depend on the
and building industry due to improved properties com- characteristics of their constituent materials (matrix and
pared to constituent materials2; high chemical and reinforcement), their individual volume fractions, and
mechanical durability for medical technology applica- the manner in which the reinforcement is embedded in
tions5; and various engineering fields including telecom- the matrix material.16–20 Interesting investigations were
munications, furniture and marine industries, due to their carried out on: woven E-glass/polyester-reinforced com-
superior properties and performance advantages.2 posites21 and plain woven kenaf/kevlar hybrid compos-
The selection of fillers for composites involves careful ites22; Dimensional stability of Bamboo/Kenaf/nanoclay
consideration of their purpose, types, particle size, material reinforced epoxy hybrid nanocomposites23; and the influ-
and cost implications, impact on properties, and dispersion ence of hydrothermal aging on the durability and perfor-
within the matrix. These factors are essential in determining mance of the adhesive bonded joints.24 The pyrolyzed oil
the overall performance and characteristics of the composite rubber (from waste tires)-epoxy polymer blend composite
material. Adding fillers (whether natural or synthetic) to developed for coating applications.25,26
composites improves performance characteristics (such as
tensile, flexural and impact properties)6,7; and reduces costs.8
Understanding and optimizing the interface between filler 1.1 | Addition of CNTs to composites
and polymer matrix is essential to improve the properties of
filled polymers.9 Different types of fillers (such as particulate, Carbon nanotubes (CNTs) offer many advantages in
plate, and fiber fillers) offer a wide range of properties the construction of new materials.27,28 They have
including reinforcement, thermal and electrical conductivity, unique and interesting properties such as mechanical,
flame retardancy, and esthetics.10 electrical, optical, and magnetic properties, which can
The fiber strength of E-glass is 16% lower than that be tuned to some extent. CNTs can improve the
of carbon. The addition of synthetic fibers such as car- mechanical and electrical properties of materials, mak-
bon and glass to polymer composites significantly ing them suitable for applications in strength-
increases their mechanical properties, fatigue resistance, enhanced structural materials, wearable thermoelectric
SRAVANTHI ET AL. 3

devices, smart textiles, and flat panel displays. Addi- composites significantly enhances mechanical and tri-
tionally, CNTs can be used to enhance the antimicro- bological properties of the hybrid composites.41 Rein-
bial and antibiofilm activity of composites, making forcing large amounts of nano-fillers with matrix
them useful in biomedical, industrial, and environ- content indicate improvements in mechanical, electrical,
mental fields. However, there are also some disadvan- dielectric, and responses to other stimuli such as pH, ther-
tages associated with CNTs. When the concentration of mal, and magnetic fields.42 Introduction of carbon nano-
CNTs exceeds a certain limit, the mechanical proper- tubes (CNTs) enhances the properties in area of high
ties of the nanocomposite may deteriorate. In addition, strength and temperature applications.43–48 GFRP compos-
there are concerns regarding the solubility, biodegrad- ites have superior mechanical properties when compared
ability, dispersibility, and toxicity of CNTs, which need to that of Jute woven and jute/glass hybrid polyester com-
to be addressed for their clinical development. posites.49 Better interfacial bonding between the fiber and
Addition of multi-walled carbon nanotubes (MWCNTs) matrix is achieved introducing various organic/inorganic
to glass fiber reinforced polymer composites can enhance carbon particles.50–52 Epoxy hybrid fiber glass composites
their mechanical properties, energy absorption capacity and in presence of hard powders (such as tungsten carbide
dimensional stability. The behavior of these composites (WC) and tantalum niobium carbide (Ta/NbC)) are tested
under various loading conditions, such as tensile testing for improved abrasive wear properties.53 Addition of large
and thermal shock, has been investigated to understand quantities of CNTs can reduce the tensile strength due to
their performance in various applications.29 Modeling possible agglomerations and side wall interactions.54
techniques are used to predict the mechanical behavior Vasavi et al.55 reviewed on erosion wear characteristics of
of composites under various conditions.30 Thermal and polymer matrix composites.
thermo-mechanical characterization of MWCNTs inte-
grated E-glass/carbon fabric reinforced composites
revealed significant improvements in thermal stability 1.3 | Research gaps
and mechanical properties, highlighting their potential
for high-performance applications in various indus- Studies on micro-carbon powder based composites indi-
tries.31 Thermal and flammability properties indicate cate improved mechanical, thermal and wear resistance
the potential for improved fire resistance and mechani- properties, which may be sensitive to environmental
cal behavior through the incorporation of MWCNTs changes. Limited studies made on the influence of aging,
into laminates.32 The influence of various surfactants especially on hybrid glass epoxy polymer composites with
on carbon fiber dispersion and the mechanical perfor- micro and nanocarbon particulate fillers,56,57 which need
mance of smart piezoresistive cementitious composites to be filled for wider use in industries.
is an important area of investigation, focusing on
achieving high-quality dispersion and optimizing the
mechanical, electrical, and thermal behaviors of the 1.4 | Objectives of the current study
composites.33 There is a possibility to develop multi-
functional cementitious composites with MWCNTs that In lieu of the above-identified literature gap, the objec-
have enhanced mechanical performance and self- tives of the current study are to: (i) Develop hybrid glass
sensing capabilities.34,35 epoxy composite and examine the influence of multi-
walled carbon nano tube (MWCNT) fillers on the
mechanical and tribiological properties including thermal
1.2 | Hybrid glass/epoxy composites with aging; and (ii) Finalize optimal processing conditions.
fillers of MWCNT Chauvenet's criterion is adopted to verify the statistical
scatter in the 5 times repeated test data for elimination of
Hybrid composites are introduced by combining the the outliers (if any). Optimal processing conditions (such
synthetic fibers with carbon fillers in a common as jet angle, jet pressure and composite type) are specified
matrix. Reinforcements (fillers) (such as micro to achieve optimal wear characteristics under air jet ero-
carbon,36,37 Al2O338 and SiO239) and nano-carbons sion (viz., minimum erosion rate), while aging time and
(say, carbon nanotubes and grapheme40) are being aging temperature are the processing conditions for the
introduced into polymer matrix composites and identified hybrid composite to achieve the mechanical
achieved good mechanical and thermal properties. properties under thermal aging. The modified Taguchi
Addition of short fibers, continuous fibers and ceramic approach is followed to obtain the optimal solutions. This
particulates/fillers as a first and/or second reinforce- technique will be useful to solve industrial optimization
ment with the Epoxy/Polyester/Poly lactic Acid matrix problems with few tests.
4 SRAVANTHI ET AL.

2 | MATERIALS AND India Limited is used as matrix material. Adnano Tech-

CHARAC TERIZATION nologies Private Limited, India supplied powder of
MWCNT (5–15 nm dia.). The hand lay-up method (see
Development of hybrid glass/epoxy composites with Figure 1) is used to process E-glass fiber composite with
fillers of multi-walled carbon nanotubes (MWCNTs) and different filler percentages of MWCNT (2, 4, and 6 wt%)
characterization is briefly presented here. The GSM at a weight ratio of 40:60 fiber to matrix.
(grams per square meter) of E-glass fiber can vary Flat plywood is placed on the table to ensure that the
depending on the specific product and application. How- plywood is free from dirt. Mats are cut to the required
ever, E-glass fiber is commonly available in a wide variety size to create five layers by positioning the plastic sheet
of areal weights, ranging from 48 to 1300 gsm, providing on the plywood and incorporating the mold release spray
flexibility in material performance and economics. As for to the plastic sheet, in order to prevent sticking the matt
the directionality of glass fiber, E-glass fiber can be both to the plastic sheet. Resin and hardener are mixed with a
uni-directional and bi-directional. Uni-directional glass mechanical stirrer in a ratio of 10:1. When it comes to
fiber is oriented in a single direction, providing strength mixing multi-wall carbon nanotubes (MWCNT) with
and stiffness along that axis. On the other hand, bi- epoxy, mechanical stirring can be an efficient method to
directional glass fiber (such as twill weave fabrics) offer mix the epoxy, especially when working with large quan-
strength in both horizontal and vertical directions, with tities of epoxy. The process time for mechanical stirring
warp and fill yarns at 0
and 90
respectively. This pro- can vary depending on various factors such as the
vides excellent conformability, strength characteristics, amount of mixture and the desired level of dispersion.
and formability. However, it may still require careful monitoring to
ensure that all areas of the mix are evenly mixed. In the
present study with a little quantity of epoxy, MWCNT
2.1 | Making of hybrid glass/epoxy fillers are thoroughly mixed with a mechanical stirrer for
composites with fillers of MWCNTs 5 min. If the epoxy resin is applied to the plastic sheet
and the first woven mat is placed on the sheet and the
E-glass fiber (bi-directional-5 layers) having a density of epoxy resin is applied evenly to the bi-directional mat,
2.56 g/cc, is used as reinforcement material. Epoxy resin then the second glass fiber mat is placed on the first mat
(LY556) and hardener (HY951) supplied by Ciba Geigy and this process is repeated up to 5 layers. The mold is

(A) (B) (C)

(D) (E) (F)

F I G U R E 1 Hand lay-up technique for making hybrid glass epoxy polymer composites with fillers of MWCNTs: (A) Mold for composite
making; (B) Epoxy weighing; (C) Applying mold release spray; (D) Filler in epoxy; (E) Chopped glass fiber to mold size; (F) Casting hybrid GFRP.
SRAVANTHI ET AL. 5

FIGURE 2 INSTRON tensile tester and test specimen as per the ASTM D638 standards.

F I G U R E 3 Experimental set
up for flexural testing and test
specimen as per the ASTM D790
standards.

closed with a plastic sheet and finally load is applied to tester (with a cross head speed of 2 mm/min) for the tensile
the composite material for 24 h for curing. Specimens strength evaluation and modulus of elasticity of the compos-
were prepared as per the ASTM standards for tensile, ite. The flexural stress test is generally referred to as three-
flexural and impact testing. point bending test. A transverse load is applied at the center
of the span of the simply supported composite beam. Tests
are conducted to measure the failure loads for flexural
2.2 | Strength of the developed hybrid strength and flexural modulus evaluation. Impact testing
composites carried out on 4 mm thick rectangular composite plates of
length 63.5 ± 2 mm and width 12.7 ± 0.2 mm, which is
ASTM D638 standards followed for tensile testing fixed in the vice of the testing machine. The specimen is
(Figure 2), whereas ASTM D790 standards for flexural test- struck by the striking edge of the pendulum (upon releasing
ing (Figure 3) and ASTM D246 standards for impact testing operating lever).Recorded the energy absorbed in breaking
(Figure 4). Tests performed on INSTRON H10KS Tensile the specimen to assess the impact resistance.
6 SRAVANTHI ET AL.

F I G U R E 4 Impact testing
machine and test specimen as per
the ASTM D246 standard.

qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
P
For easy of reference, the developed hybrid compos- σ x ¼ n1 ni¼1 ðx i  x Þ2 . While analyzing the test data
ites are designated by C0 (Five layers of neat GFRP); fx 1 , x 2 ,::……, x n g, Chauvenet's criterion recommends find-
C1 (Five layers of glass epoxy with 2 wt% of MWCNT); ing the deviation ratio ðDRi Þ of each individual value
C2 (Five layers of glass epoxy with 4 wt% of MWCNT); ðx i , i ¼ 1 to nÞ from
and C3 (Five layers of glass epoxy with 6 wt% of
MWCNT). jx i  x j
DRi ¼ , ð1Þ
Flexural, tensile and impact testing performed on the σx
developed hybrid glass epoxy polymer composites with
fillers of MWCNTs and generated the strength properties. Compare the deviation ratio ðDRi Þ with the critical
Each test is repeated 5 times and applied the Chauvenet's deviation ratio ðDRc Þ of Chauvenet's criterion58 to declare
criterion to verify the statistical scatter in the test data for the data x i as outlier, if DRi > DRc . The acceptable range
elimination of the outliers (if any). of the dataset is58
Chauvenet's criterion58 is a statistical method used to
assess whether a particular data point in a set of observa- x i  ½x  DRc σ x , x þ DRc σ x  ð2Þ
tions may be an outlier and, thus, spurious. The criterion
provides a means to objectively and quantitatively iden- The criterion is applied to the measured 5 flexural
tify outliers in a dataset, assuming that the data follow a strength tests of the C0 composites. The critical deviation
normal distribution. Here is a detailed explanation of ratio ðDRc Þ in Equation (2) for the sample size ðn ¼ 5Þ is
Chauvenet's criterion and its application in testing statis- 1.645. Recorded data set {194.0, 183.2, 192.4, 191.7, and
tical scatter in test data. 184.2 MPa} for the flexural strength of 5 layers of neat
 test data: x 1 , x 2 ,::……, x n ,
Consider a set of n repeated GFRP is considered and followed the Chauvenet's crite-
P
whose mean, x ¼ n1 ni¼1 x i and standard deviation, rion to verify the scatter in data as acceptable.
SRAVANTHI ET AL. 7

T A B L E 1 Strength properties of the composites fabricated for neat epoxy GFRP (C0) and hybrid composites with fillers of MWCNTs
varying 2, 4, and 6 wt% (C1, C2, C3).

Flexural testing Tensile testing

Impact strength
Composite type Strength (MPa) Modulus (GPa) Strength (MPa) Modulus (GPa) (kJ/m2)
C0 189.1 12.276 112.4 2.804 83.6
C1 203.0 13.124 131.8 4.351 88.4
C2 216.7 13.313 142.4 3.222 92.4
C3 206.0 12.453 128.6 3.414 90.0

FIGURE 5 Microstructural observations on the tensile fracture of composite type, C2.

The sample mean, x ¼ 189:1MPa and the sample stan- and 6 wt%) of MWCNTs (C1, C2, C3). Tensile strength prop-
dard deviation, σ x ¼ 4:471MPa. The acceptable range of erties in Table 1 indicate degradation when the MCWNTs
the flexural strength data set, x i  ½181:7, 196:5. The added upon 4% due to possible agglomerations and side wall
recorded data of the flexural strength of C0 composite are interactions.54 The sample with 4% of MWCNT dispersion
within the acceptable range. Hence, mean value of the in the composite (C2) has maximum flexural strength of
acceptable recorded data set is considered while charac- 216.7 MPa, tensile strength of 142.4 MPa and impact
terizing the developed composites. strength of 92.4 kJ/m2. The dispersion of MWCNT in the
The flexural, tensile and impact strength properties matrix material increases the brittleness and reduces the
of the composites fabricated for neat epoxy GFRP strength. The observed reduction in strength properties
(C0) followed by the variation of weight percentages (2, 4, beyond 4 wt% composition of MWCNTs can be attributed to
8 SRAVANTHI ET AL.

F I G U R E 6 Microstructural observations on failed composite type C2 that failed in flexural testing show: (A) failure due to bending;
(B) fiber is stretched as a result of weak dispersion; (C) Epoxy stack (white part on fibers) causes deterioration in flexural properties, which is
attributed to (D) poor wettability.

F I G U R E 7 Microstructural
observations on composite type C2
after impact testing.

the adverse effects of higher MWCNT concentrations on the are crucial for optimizing the design, manufacturing, and
mechanical properties of the composite material. These performance of hybrid composite materials.
effects may include a decrease in compressive strength, Common procedures generally used in preparing sam-
impact resistance, and damage tolerance, indicating a non- ples for scanning electron microscopy (SEM) analysis are:
linear relationship between MWCNT concentration and the (i) fixation of the specimen to preserve its structure and pre-
mechanical properties of the composite material.59 vent degradation during subsequent processing; (ii). dehy-
Microstructural observations contribute to understanding dration to remove water from the sample through a series of
the failure mechanisms in hybrid composites by enabling alcohol or acetone washes of increasing concentration to
defect analysis, assessing interfacial bonding, localizing dam- gradually replace the water with a dehydrating agent;
age, analyzing fracture behavior, and correlating microstruc- (iii) drying (critical point drying, freeze-drying or air-drying)
tural features with macroscopic performance. These insights methods to remove residual solvent (if any) (iv) mounting
SRAVANTHI ET AL. 9

TABLE 2 Levels of input variables and the output response (viz., erosion rate per minute), ER as per the Taguchi's L9 orthogonal array.

Input variables Designation Level-1 Level-2 Level-3

Jet angle ( ) A 30 45 90
Jet pressure (bar) B 1 1.5 2
Composite type C C1 C2 C3
Fictitious D d1 d2 d3
Levels of input parameters Estimate Equation (4)
ER Estimated range of
Test run A B C D (g/kg)/min test np ¼ 3 R.E. (%) np ¼ 4 ER (g/kg)/min
1 1 1 1 1 0.698 0.7838 12.3 0.698 0.698–0.831
2 1 2 2 2 1.369 1.3221 3.4 1.369 1.236–1.369
3 1 3 3 3 2.245 2.2062 1.7 2.245 2.120–2.253
4 2 1 2 3 1.189 1.1501 3.3 1.189 1.064–1.197
5 2 2 3 1 2.374 2.4598 3.6 2.374 2.374–2.507
6 2 3 1 2 2.331 2.2841 2.0 2.331 2.198–2.331
7 3 1 3 2 1.288 1.2412 3.6 1.288 1.155–1.288
8 3 2 1 3 1.530 1.4911 2.5 1.530 1.405–1.538
9 3 3 2 1 1.518 1.6038 5.7 1.518 1.518–1.651

TABLE 3 Analysis of variance (ANOVA) for the output response (viz., erosion rate per minute), ER (g/kg)/min.

Input variables 1-Mean 2-Mean 3-Mean Mean Sum of squares %Contribution

A 1.4373 1.9647 1.4453 1.6158 0.5479 20.4
B 1.0583 1.7577 2.0313 1.6158 1.5107 56.1
C 1.5197 1.3587 1.9690 1.6158 0.6003 22.3
D 1.5300 1.6627 1.6547 1.6158 0.0332 1.2

on a suitable substrate or stub using an adhesive material; resulting in fiber pull-out. Also, the thread like CNT
(v) coating (materials include gold, gold/palladium or car- structures indicating the fiber resistance offered against
bon) to increase the conductivity of non-conductive samples the flexural strength. The white portion on fibers in
and reduce charging effects during imaging; and (vi) storage Figure 6C is epoxy stack cause deterioration of flexural
and handling to protect specimens from damage and con- properties. This deterioration attributes to poor wetta-
tamination. It should be noted that specific sample prepara- bility as in Figure 6D. It is evident from the microstruc-
tion techniques may vary depending on the nature of the tural observations in Figure 7 that the fibers have
sample and the desired analysis. shown excellent resistance to the impact loading and
Microstructural investigations are made on the failed the multiple cracks are due to non-uniformly distrib-
hybrid composites with fillers of 4 wt% MWCNTs, which uted MWCNTs.
yielded high strength. Observations in Figure 5A revealed
a strong adhesion between matrix and fibers. Surface
nomenclature in Figure 5B indicates non-uniform align- 3 | RESULTS A ND DISCUSSION
ment of MWCNTs due to the adopted hand-lay-up pro-
cess. Dimples in surface topography in Figure 5C are The developed hybrid composites with fillers of
indicative of ductile fracture. MWCNTs are subjected to erosion testing and thermal
Microstructural investigations made on the failed aging by following the Taguchi's L 9 OA (orthogonal
composites in flexural testing are as follows. The SEM array) for minimizing the tests and obtaining the opti-
micrograph in Figure 6A shows the failure due to bend- mal process parameters to yield improved material
ing. The holes in Figure 6B indicate weak dispersion properties.
10 SRAVANTHI ET AL.

F I G U R E 8 Comparison of
measured and estimated erosion
rate for the full factorial design of
experiments.

T A B L E 4 Minimum erosion rate,

Composite type Test Empirical relation (5) Expected range
ER (g/kg)/min for the developed 3 types
C1 0.698 0.784 0.698–0.831 of hybrid glass epoxy composite (Jet
C2 0.927 0.623 0.537–0.670 angle, A1 = 30
and Jet pressure,
C3 1.182 1.233 1.147–1.280 B1 = 1 bar).

3.1 | Erosion testing of the developed output response for optimization (see Table 2). ANOVA
hybrid composites (analysis of variance) is performed (see Table 3).
ANOVA analysis helps the designer to identify the opti-
The air jet abrasive particle erosion studies are made mal levels of the input variables from the mean values of
using hard silica particle to impinge at specific angles the output response, in addition to the %Contribution of
over the composites. Erosion tests are performed follow- each input variable on the output response. ANOVA
ing the ASTMG76 standard. Jet angle, jet pressure, and results also help the designer to establish relationship
composite type are the variable process parameters con- between the output response and input variables through
sidered to achieve optimal wear characteristics under air additive law, which is well explained in references 61–67
jet erosion (viz., minimum erosion rate). Jet angle (A), jet pressure (B), composite type
Air jet erosion process parameters are: Erodent parti- (C) and fictitious parameter (D)have 20.4%, 56.1%,
cle size = 50 μm; Particle velocity = 48 to 82 m/s; Ero- 22.3%, and 1.2% contribution on the output response
dent flow rate = 2 g/mm; Stand-of-distance = 10 mm; (erosion rate per minute). The significance of %Contri-
and Angle of impingement = 30 to 90
. bution of input variables is on the grand mean value of
The wear rate (or Erosion rate), ER is evaluated from: the output response, ER. The %Contribution of the ficti-
tious parameter (D) on ER indicates 1.2% error. From
Weight Loss of the Test Sample ðgÞ the ANOVA Table 3, the input variables for minimum
ER ¼ ð3Þ
Mass of the Erosion Particle ðgÞ ER is A1B1C2 in which subscripts denotes the levels of
the input variables. The optimal input variables are: Jet
The weight loss of the test sample (g) is determined from angle, A1 = 30
; Jet pressure, B1 = 1 bar; and Composite
the difference in weight of the samples before and after type, C2 = Five layers of glass epoxy with 4 wt% of
each test. The mass of the erosion particles (g) is hitting MWCNT.
of the target sample for the test time. Erosion rate, ER Using the additive law,58 the erosion rate can be esti-
(g/g) is evaluated by exposing the composites for 2, 4, mated from
6, 8, and 10 min. Steady state is observed by exposing the
composites for 10 minutes. Jet angle, jet pressure and X
np

fillers of 2 to 6 wt% MWCNTs are considered as input ERe ¼ ERmean þ ðERi  ERmean Þ ð4Þ
i¼1
variables. Taguchi method60 is utilized for solving engi-
neering optimization problems.61–67 Experiments are
conducted as per the Taguchi's L9 OA (orthogonal array) Here ERe is the estimated value of the surface roughness;
for the 3 input variables with 3 levels and reported the ERmean is the overall surface roughness mean value of
SRAVANTHI ET AL. 11

F I G U R E 9 Variation of
erosion rate with jet angle using
empirical relation (5) for the jet
pressure, B1 = 1 bar and composite
type, C2.

F I G U R E 1 0 Variation of
erosion rate with jet pressure using
empirical relation (5) for the jet
angle, A1 = 30
and composite
type, C2.

FIGURE 11 SEM micrographs of test specimen after erosion test (A) dimple (B, C) Carbon particle dispersed composite.

the total test runs; ERi is the mean value of the surface for the fictitious parameter (D), the range of estimates is
roughness corresponding to the cutting parameter at the arrived from Equation (4).Corrections to the ER esti-
specified level; and np is the number of input variables. mates at the specified levels of the cutting parameters (A,
Introducing the fictitious parameter (i.e., np ¼ 4), the esti- B, and C) are 0.0858 and 0.0469 (g/kg) per minute. The
mates of ER using the additive law (4) are matching with test data are within the estimated range (Table 2).
test data (Table 2). Considering only the levels of mini- Using the additive law (4), ER is evaluated for all
mum and maximum mean values of surface roughness 27 combinations of 3 input variables with 3 levels:
12 SRAVANTHI ET AL.

T A B L E 5 Flexural, tensile and

Aging parameters Designation Level-1 Level-2 Level-3
impact strength properties of the hybrid
Aging temperature (
C) T 60 120 180 glass epoxy composite with fillers of
Aging time (hours) t 2 4 6 4 wt% MWCNTs and levels of thermal
Fictitious-1 ε1 ε11 ε12 ε13 aging parameters as per Taguchi's
L9 OA (orthogonal array).
Fictitious-2 ε2 ε21 ε22 ε23
Levels of aging
Impact
parameters Flexural testing Tensile testing
strength,
Test Strength, Modulus, Strength, Modulus, σ3
run A B C D σ 1 (MPa) E1 (GPa) σ 2 (MPa) E 2 (GPa) (kJ/m2)
1 1 1 1 1 225.4 13.85 146.7 3.319 85.94
2 1 2 2 2 231.4 14.22 150.9 3.416 88.28
3 1 3 3 3 232.7 14.30 151.7 3.432 88.86
4 2 1 2 3 202.9 12.47 133.1 3.013 78.16
5 2 2 3 1 196.7 12.09 129.6 2.932 75.24
6 2 3 1 2 189.5 11.64 123.9 2.803 71.73
7 3 1 3 2 192.3 11.82 125.3 2.836 72.56
8 3 2 1 3 186.3 11.45 113.9 2.578 66.04
9 3 3 2 1 175.7 10.79 108.2 2.449 62.70

TABLE 6a Significance of aging parameters on flexural strength through ANOVA.

Aging parameters 1-Mean 2-Mean 3-Mean Sum of squares %Contribution

Flexural strength, σ 1 (MPa): grand mean = 203.65
T 229.83 196.37 184.75 3286.42 92.6
t 206.87 204.81 199.28 92.46 2.6
ε1 200.37 203.33 207.26 71.61 2.0
ε2 199.25 204.41 207.30 99.85 2.8
Flexural modulus, E1 (GPa): grand mean = 12.51
T 14.12 12.06 11.35 12.41 92.6
t 12.71 12.58 12.24 0.35 2.6
ε1 12.31 12.49 12.73 0.27 2.0
ε2 12.24 12.56 12.74 0.38 2.8

    
Ai , Bj , Ck , k ¼ 1 to 3 ,j ¼ 1 to 3 , i ¼ 1 to 3 . Corrections for composite type, C3. Corrections to the ER estimates
are applied to obtain the estimated range of ER. The from (5) for the input variables (A, B, and C) are 0.0858
lower and upper bound estimates of ER are made for the and 0.0469 (g/kg)/min.
full factorial design of experiments (Figure 8). Test data is From the ANOVA Table 3, the input variables for the
within/close-to the estimated range. 3 composite types (C1, C2, and C3) to achieve minimum
Empirical relation developed for the erosion rate erosion rate (ER) are: Jet angle, A1 = 30
and Jet pres-
(ER) in terms of input variables (viz., jet angle (A), jet sure, B1 = 1 bar. Table 4 presents minimum ER values
pressure (B), composite type (C)) is for the developed 3 types of hybrid glass epoxy composite.
Variation of erosion rate with jet angle and with jet pres-
ER ¼ 1:8494 þ 0:004ξ1  0:5233ξ21 þ 0:4865ξ2  0:2128ξ22 sure using empirical relation (5) is shown in Figures 9
þ 0:2247ξ3 þ 0:3857ξ23 and 10 for the composite type, C2. Both figures show
ð5Þ minimum at A1 = 30
and B1 = 1 bar.
Erosion testing outcomes provide essential information
ðA45Þ  
Here ξ1 ¼ 900 80  23 A ; ξ2 ¼ 2B  3; ξ3 ¼ 1 for com- for understanding the wear characteristics of composites,
posite type, C1; ξ3 ¼ 0 for composite type, C2, and ξ3 ¼ 1 enabling the assessment of erosion behavior, wear rate
SRAVANTHI ET AL. 13

TABLE 6b Significance of aging parameters on tensile strength through ANOVA.

Aging parameters 1-Mean 2-Mean 3-Mean Sum of squares %Contribution

Tensile strength, σ 2 (MPa): grand mean = 131.48
T 149.75 128.87 115.81 1758.20 89.3
t 135.04 131.48 127.92 76.04 3.9
ε1 128.15 130.77 135.51 83.60 4.2
ε2 128.15 133.38 132.90 50.04 2.5
Tensile modulus, E 2 (GPa): grand mean = 2.975
T 3.389 2.916 2.621 0.900 89.4
t 3.056 2.975 2.895 0.039 3.9
ε1 2.900 2.959 3.066 0.043 4.2
ε2 2.900 3.018 3.007 0.026 2.5

TABLE 6c Significance of aging parameters on impact strength through ANOVA.

Aging parameters 1-Mean 2-Mean 3-Mean Sum of squares %Contribution

Impact strength, σ 3 (kJ/m ): grand mean = 76.61
2

T 87.69 75.04 67.10 647.18 89.5

t 78.89 76.52 74.43 29.86 4.1
ε1 74.57 76.38 78.89 28.23 3.9
ε2 74.62 77.52 77.69 17.82 2.5

T A B L E 7 Mechanical properties of the developed hybrid glass epoxy composite with fillers of 4 wt% MWCNTs (C2) at optimal thermal
aging temperature, T1 = 60
C; and time, t1 = 2 h.

Testing Strength and modulus Achieved property Empirical relation Estimated range
Flexural σ 1 (MPa) 225.4 (216.7) a
233.0 225.3–240.3
E1 (GPa) 13.85 (13.313) 14.32 13.85–14.77
Tensile σ 2 (MPa) 146.7 (142.4) 153.3 146.7–159.3
E2 (GPa) 3.319 (3.222) 3.470 3.320–3.600
Impact σ 3 (kJ/m2) 85.94 (92.40) 89.97 85.94–93.32
a
Achieved properties at room temperature.

F I G U R E 1 2 Decreasing trend of flexural, tensile and impact strengths with aging temperature for the (A) optimal aging time, t1 = 2 h,
(B) optimal aging temperature, T1 = 60
C.
14 SRAVANTHI ET AL.

comparison, microstructural examination, performance opti- σ 3 ¼ 94:95  10:3η1 þ 2:355η21  2:229η2 þ 0:139η22
mization, and the development of application-specific ð8Þ
Expected range : ðσ 3  4:03, σ 3 þ 3:35Þ
solutions.
SEM micrograph of test specimen after erosion test
E 1 ¼ 12:136  1:385η1 þ 0:671η21  0:233η2  0:107η22
in Figure 11A visualizes smooth surface and thorough ð9Þ
Expected range : ðE 1  0:47, E 1 þ 0:45Þ
fibers dispersion. Figure 11B is indicative of fibers in
proper alignment and bridging of CNTs between fiber
and matrix. Micro-cracks on the surface topology in E 2 ¼ 2:916  0:384η1 þ 0:089η21  0:081η2
ð10Þ
Figure 11C indicate on fiber breakage resisted by CNTs Expected range : ðE 2  0:15, E 2 þ 0:13Þ
in the epoxy.
Here, η1 ¼ ðT120 Þ ðt4Þ
60 ; andη2 ¼ 2 .
From the ANOVA Tables 6a–6c, the input variables
3.2 | Thermal aging for maximum flexural, tensile and impact strengths is
T1t1 in which subscriptions denotes the levels of the input
The thermal aging process on hybrid glass epoxy variables. Since, the optimal set of input variables or parame-
composites with MWCNT fillers aims to assess the ters are found to be same for this case study, there is no need
stability of the composite material when exposed to to go for multi-objective optimization. The optimal input var-
elevated temperatures, as well as to understand the iables are: Aging temperature, T1 = 60
C; and aging time,
long-term effects of thermal stress on the material's t1 = 2 h. The achieved mechanical properties are within the
properties. This information is valuable for predicting expected range (Table 7). In case of different sets of optimal
the material's performance and lifespan in real-world input variables for the maximum flexural, tensile and
applications where thermal aging is a significant impact strengths, multi-objective optimization63–67 pro-
factor. vides a set of optimal input variables. For aging time,
The high strength hybrid glass epoxy composites with t1 = 2 h, empirical relations of flexural, tensile and impact
fillers of 4 wt% MWCNTs are subjected to thermal aging. In strengths show decreasing trend with aging temperature
a thermal aging woven, the developed composites are (Figure 12A). Similarly, for the aging temperature,
exposed to specific aging temperature and time duration. T1 = 60
C, empirical relations of flexural, tensile and
Samples are made as per ASTM standards and tested for impact strengths show slightly decreasing trend with aging
flexural, tensile, and impact strengths for each aging tem- time (Figure 12B).
perature and time. Experiments are conducted as per the Table 7 presents the mechanical properties of the
Taguchi's L9 OA (orthogonal array) for the 2 input variables developed hybrid glass epoxy composite with fillers of
with 3 levels and reported the output response for optimiza- 4 wt% MWCNTs (C2) at optimal thermal aging tempera-
tion (see Table 5).ANOVA (analysis of variance) analysis is ture, T1 = 60
C; and time, t1 = 2 h. The measured flex-
performed (see Tables 6a–6c).The significance of %Contribu- ural, tensile and impact strength values of C2 hybrid
tion of input variables is on the grand mean value of the composite are 216.7 MPa, 142.4 MPa and 92.4 kJ/m2,
output responses. The %Contribution of the fictitious-1 (ε1 ), which are with the developed empirical relation-
and fictitious-2 (ε2 ) on the output responses indicate % ships (6) to (8).
error. Aging temperature (T) indicates the highest %Con-
tribution ð ≈ 90%Þ on output responses, whereas aging
time (t) indicates %Contribution ð ≈ 4%Þ. Error% is the 4 | CONCLUDING REMARKS
remaining 6%.
Empirical relations developed for the flexural E-glass with low mechanical properties and good electri-
strength, σ 1 (MPa); flexural modulus, E 1 (GPa); tensile cal resistivity is preferred in electrical and electronic
strength, σ 2 (MPa); tensile modulus, E 2 (GPa); and based applications. Current research is towards improv-
impact strength, σ 3 (kJ/m2) in terms of input variables ing the properties by adding filler materials and making
(viz., aging temperature (T) and aging time (t)) are them wider applications. CNTs exhibit excellent proper-
ties either individually or when added to composites.
σ 1 ¼ 197:5  22:54η1 þ 10:92η21  3:795η2  1:738η22 Hence the use of MWCNTs has become the primary
ð6Þ
Expected range : ðσ 1  7:69, σ 1 þ 7:25Þ choice in the present study.
Hybrid glass/epoxy composites with MWCNT fillers
σ 2 ¼ 128:9  16:97η1 þ 3:915η21  3:56η2 have been developed by adopting a technically and eco-
ð7Þ nomically feasible hand lay-up technique. Mechanical
Expected range : ðσ 2  6:65, σ 2 þ 5:94Þ
and tribological properties are generated to investigate
SRAVANTHI ET AL. 15

the effect of nano-carbon fillers. A study is carried out C O N F L I C T O F I N T E R E S T S T A TE M E N T

on the wear characteristics of hybrid composites The authors declare that they have no known competing
under air jet erosion. Investigated the influence of ther- financial interests or personal relationships that could
mal aging and time duration on the mechanical have appeared to influence the work reported in this
properties of hybrid composites and drew the following paper.
conclusions.
DA TA AVAI LA BI LI TY S T ATE ME NT
• Strength to weight ratio of hybrid composites enhanced All data generated or analyzed during this study are
by the addition of MWCNTs. included in this published article.
• Material characterization (tensile, impact, flexural, ero-
sion, and thermal aging tests) is carried out to verify
the adequacy of the developed hybrid composites. ORCID
• Significant enhancement in tensile strength, impact S. P. Jani https://orcid.org/0000-0002-8491-6117
strength, and flexural strength is achieved for fillers of
2 and 4 wt% MWCNTs. RE FER EN CES
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