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CHAPTER - 3

FABRICATION OF COMPOSITES

S. No. Name of the Sub-title Page No.

3.0 Introduction 69

3.1 Materials 71

3.2 Polymers 72

3.2.1 Polyester Resin 73

3.2.2 Mixing of Resin 75

3.3 Fiber Preparation and Hybridization 76

3.4 Composite Specimen Preparation 77

3.5 Summary 82
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3. FABRICATION OF COMPOSITES

3.0 INTRODUCTION

Continuous advancements in the manufacturing methodologies and

performance of fiber reinforced polymer (FRP) have led to a significant

growth in its market acceptance. The fabrication of composites is a

complex process and it requires the simultaneous consideration of

various parameters, such as component geometry, layering sequence,

production volume, reinforcement & matrix types, tooling requirements,

and process economics. The availability of choices makes it imperative

that the factors of economics, design and manufacturing be integrated

during the development process itself. For composites to become

competitive with metals, cost reduction is a necessity, besides durability,

maintainability and reliability.

The multitude of tasks involved in the manufacturing of composite

laminates can be divided into two stages: (1) Fabrication/manufacturing

techniques and (2) Processing methodologies. The fiber and matrix may

be in a pre-impregnated form, or the fiber and matrix material may be

combined for the first time, during this step of developing the structural

form. Fabrication techniques for composites are not dependent on the

type of matrix material. In fact, some metal forming techniques have

been adapted to composites fabrication, whereas, the processing

conditions are entirely dependent on the type of matrix material used.

For instance, thermosets require long processing times, whereas

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thermoplastics require relatively high pressures and temperatures. In the

present experimental study, a brief introduction to the manufacture of

composites by using the hand lay-up process, and the issues related to

manufacturing are presented and discussed in detail.

From the general perspective, manufacturing begins with the

manufacture of structural components from layers or plies of pre-

impregnated material called prepreg. Specifically, layers of a material

with the fibers in each layer aligned in a specific direction are used to

form a laminate. The hand fabricated laminate will be processed in an

autoclave, which is a pressurized oven that provides the proper levels of

heat and pressure. In the early years of the development of fiber-

reinforced materials, structural components were fabricated by hand.

Even today, in prototype development hand fabrication is common, and

this is also the case for specialty manufacturing and in many university

laboratories. However, as labor costs and the need for consistency have

increased, engineers have been entrusted with the task of designing low

cost automated manufacturing techniques. Now, automated techniques

like robotic tow and tape placement methods, injection molding and

pultrusion have dramatically reduced the cost of manufacturing

composite structures.

In all manufacturing methods, the use of tools like the die, mold and

mandrel is common, and they provide the structural shape to the

composite material. These tools are usually an inverse, of the desired

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structural shape, and the design of the tool is a critical and expensive

process. The cost of the tool often far exceeds the material and labor

costs to produce a composite structure. Also common to all

manufacturing methods, is the need to apply temperature and pressure

to the structural component, after the fiber and matrix are brought

together to the desired structural form. The pressure takes two forms:

actual pressure, ideally hydrostatic, to consolidate the tows and layers; a

vacuum to remove the air entrapped between the layers, and to reduce

the amount of unwanted gases given off by the resin as it cures. The

application of pressure can be in the form of closing both halves of the

tool, or as with a flat structural component pressing the laminate in a

hot press. Finally, the vacuum requirement is met by enclosing the

structural component in a vacuum-tight bag and drawing a vacuum.

3.1 MATERIALS

In this investigation Sisal (Agave sisalana), Jute (Corchorus oliotorus)

and glass fibers are used for fabricating the composite specimen. The

sisal and jute fibers were obtained from Dharmapuri District, Tamil

Nadu, India. Polyester resin and the catalyst Methyl Ethyl Ketone

Peroxide (MEKP) were purchased from M/s. Sakthi fiber glass Ltd.,

Chennai, India. The accelerator used for the investigation is Cobalt

Napthanate, and 1% of it is added with the resin and the catalyst. The

fibers used for the composite fabrication are presented in Fig. 3.1. The
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resin, accelerator, catalyst, and thinner used for processing of

composites are given in Fig. 3.2.

(a) Jute fiber (b) Sisal fiber (c) Glass fiber

Fig. 3.1: Fibers used for composite fabrication

(a) Polyester (b) Cobalt (c) Methyl Ethyl (d) Acetone

resin Napthanate Ketone Peroxide thinner
(MEKP)
Fig. 3.2: Materials used for composite fabrication

3.2 POLYMERS

Polymers can be classified on the basis of their origin, that is,

naturally occurring, or synthetic as given in Fig.3.3. Natural polymers

are available in large quantities from renewable sources, while synthetic

polymers are produced from non-renewable petroleum based resources.

Nowadays, degradable polymers are used in various forms including

films, moulded articles, sheets, etc.

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Cellulose
Plant Polysaccharides Starch
Alginate

Chitin (Chitosan)
Polysaccharides
Hyaluronate
Animal
Natural
origin
Collagen (Gelation)
Proteins
Albumin
Poly (3- hydroxyalkanoate)
Polyesters Poly (hydroxybutyrate)
Microbe
Poly (hydroxybutyrate-co-hydroxyvalerate)
origin
Polysaccharides Hyaluronate

Starch
Polylactides
Alginate
PolyglycolidePGA

Bio- Aliphatic Polycaprolactone

degradable Poly (butylenes succinate)
Polyesters
polymers Poly (alkenedicarboxylates) Poly (ethylene succinate)
Poly (butylene succinate
Poly (p-dioxanone)
-co-adipate)
Poly (ethylene adipate) Poly (trimethylene carbonate)
Polycarbonate Poly (propylene carbonate)
Copolyester carbonate

Poly (butylenes adipate

Aliphatic- Aromatic Polyesters
Synthetic -co-terephalate)
Polyurethanes
Poly (tetramethylene adipate
Poly amides and poly ester amide
/terephthalate)
Polyanhydrides
Poly (ortho esters)
Poly (propylene fumarate)
Polyphosphazenes
Polyphosphoster

Fig. 3.3: Classification of bio-degradable polymers [143]

3.2.1 Polyester Resin

Polyester, also known as thermoplastic polymer, is used in a wide

variety of applications, including packaging and labelling, textiles (e.g.,

ropes, thermal underwear and carpets), stationery, plastic parts and

reusable containers of various types, laboratory equipment,

loudspeakers, automotive components, and polymer banknotes.

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Durable goods such as motor vehicles, appliances and carpets

account for about 50% of polyester end uses in the industrialized areas

of the world. Consumption in these markets is mostly dependent on

economic cycles and consumer spending on hard goods. Packaging,

another major market for polyester, is often considered recession-proof

in comparison with other polyester end users, with regard to pull-

through demand. However, inventory swings along packaging's

substantial supply chain can play havoc with the production demand,

particularly during long down-market swings, such as those experienced

in 2000–2003 and again in 2008–2010. The packaging market has

suffered the impact of legislation mandating an increasing use of

recycled plastics, source reduction, and the reduction of disposables.

Compared with other large-volume thermoplastics, the polyester

business continues to exhibit excellent growth. Over the past ten years,

the world demand has grown annually by 4.8%. Since 2007–2008,

massive capacity additions have forced older units to be rationalized,

while the steep crude oil price increase has created some fundamental

shifts in the light olefin markets, creating a long-term increase in the

propylene-to-ethylene price ratio. Accordingly, polyester has become

more expensive relative to polyethylene, promoting shifts from polyester

to alternative products like HDPE (high density polyethylene), wherever

possible.
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While new applications continue to be developed for polyester, it is

still largely a commodity thermoplastic subject to economic fluctuations,

especially in the area of durable goods. Producers continue to struggle

with sustaining profitability, where cost volatility often undercuts the

ability to recover pricing in tightly supplied markets. Competitors have

consolidated, formed joint ventures and alliances in order to secure

feedstock, and have pursued broader commercial positions and/or

technologies to streamline and hopefully reduce the profit volatility of

their businesses. The properties of polyester resin are presented in

Table3.1.

Table 3.1 Properties of polyester resin [144]

Property Range Property Range
Tensile strength (MPa) 15-20 Density (g/cm3) 1-1.3
Tensile modulus (GPa) 0.8-1.2 Poisson’s ratio 0.45
Compressive strength (MPa) 80-220 Specific gravity 1-1.5
Flexural strength (MPa) 25-32 Shrinkage (%) 0.005-0.009
Flexural modulus (GPa) 1.1-1.6 Young’s modulus (GPa) 4-6

3.2.2 Mixing of Resin

The process of resin preparation is presented in Fig. 3.4. The

accelerator and catalyst are mixed with resin and stirred, using a stirrer

as shown in Fig. 3.4(a). After mixing, the quantity of resin to be used for

each layer is measured, and given in Fig. 3.4(b).

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(a)Mixing of resin (b) Resin ready to use

Fig. 3.4: Preparation of resin

3.3 FIBER PREPARATION AND HYBRIDIZATION

Most natural fibers have low processing temperatures; they cannot be

processed over 150ºC due to their biological nature and hence, fiber

preparation below 80ºC gives better properties. The raw sisal and jute

fibers are cut into equal lengths of 32±0.5cm, and the glass fiber of

unidirectional mat with 300gsm is also cut into the same length, and

used for the specimen preparation. The hybridization of fibers refers to

the combination of conventional fibers with natural fibers, by using

either synthetic or biopolymer matrix for improving the properties. In this

experiment, sisal and jute fibers are hybridized with glass fibers by using

polyester resin, with two different fiber orientations of 0º and 45º, and

three different fiber ratios of sisal-jute-glass fiber in the order of 40:0:60,

0:40:60 and 20:20:60 respectively. The main reason for hybridization is

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to reduce the weight, cost and environmental effects. The physical

properties of fibers used for composites fabrication are given in Table 3.2.

Table 3.2 Physical properties of the fibers [10]

Physical property Glass fiber Sisal fiber Jute fiber

Density (g/cm3) 2.5-2.7 1.3-1.6 1.3-1.5
Tensile strength (kN/mm2) 1700-2500 540-720 610-780
Stiffness (kN/mm) 70-75 30-40 15-35
Elongation at break (%) 3-5 2.2-3.3 1.0-1.9
Max. elongation (mm) 20-30 5-10 10-14
Tensile modulus (GPa) 68-75 10-40 12-60
Specific modulus (approx.) 29 18 32
Young’s modulus (GPa) - 13 15-30
Cellulose content (%) - 65-75 59-70
Hemicellulose content (%) - 10-15 15-20
Lignin content (%) - 7-13 11-15
Lumen size (mm) - 11 13
Fiber length (mm) - 10-150 120-900
Microfibrillar angle (deg) - 11-20 8-9
Moisture absorption (%) - 11 12

3.4 COMPOSITE SPECIMEN PREPARATION

The hand lay-up is one of the oldest, simplest and most commonly

used methods for composite parts’ construction. The specimen is

fabricated in layer stacking, and each layer is oriented to achieve the

maximum utilization of its properties. Layers of different materials can be

combined to further enhance the overall performance of the laminated

composite samples. Resins are impregnated by hand into fibers, which

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are in the form of woven, knitted, stitched or bonded fabrics. This is

usually accomplished by rollers or brushes, with an increasing use of

nip-roller type impregnators for forcing the resin into the fabrics, by

means of rotating rollers. Then the composite laminates are allowed to

cure under normal atmospheric conditions and dried under the hot sun

for over 24 hours.

The composite samples used for the present investigation consist of

five layers, and fabricated by the hand layup method. In the five layers,

the glass fiber layers are mounted on the top, middle and bottom of the

specimen. The second and fourth layers of the specimen are filled by

natural fibers, and the resin has to be poured on every layer. The layer

sequence of the different composite samples is presented in Table 3.3.

The fiber orientation, reinforcement arrangement and fiber content in

volume percentage of the fibers used for the fabrication of composites are

tabulated in Table 3.4.

Table 3.3 The layer sequence of the composite samples

Layer/Sample S1 and S4 S2 and S5 S3 and S6

Layer 1 Glass fiber Glass fiber Glass fiber
Layer 2 Sisal fiber Jute fiber Sisal fiber
Layer 3 Glass fiber Glass fiber Glass fiber
Layer 4 Sisal fiber Jute fiber Jute fiber
Layer 5 Glass fiber Glass fiber Glass fiber
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Table 3.4 Fiber orientation, reinforcement arrangement and fiber

content of the composite samples

Reinforcement
Fiber content
Fiber arrangement
Sample (Volume %)
orientation (Number of layers)
(Deg.) Sisal Jute Glass Sisal Jute Glass
fiber fiber fiber fiber fiber fiber
S1 0 2 0 3 40 0 60
S2 0 0 2 3 0 40 60
S3 0 1 1 3 20 20 60
S4 45 2 0 3 40 0 60
S5 45 0 2 3 0 40 60
S6 45 1 1 3 20 20 60

Add 1% catalyst and 1–1.5% accelerator by weight with resin for

quick setting, immediate mixing, and reduce the heat generated due to

exothermic reaction. Before fabricating the composite specimen the sisal

and jute fibers are dried in the hot air oven at 80ºC for 8 hours to remove

the moisture completely. Initially, the releasing agent is coated over the

plain horizontal table for easy removal of the specimen, and the first

layer of the specimen, i.e., the glass fiber mat is placed over the coated

surface after the releasing agent gets dried. Then the resin is applied over

the glass fiber mat and the resin is evenly distributed on the entire

surface by using a roller. The resin is allowed 10-20 minutes for getting

completely mixed; after that, the second layer of the specimen, i.e., the

natural fiber is placed over the glass fiber. The process is repeated for all
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five layers of the sample as well as for all the samples. The air gaps

formed between the layers during processing are gently squeezed out.

Then these samples are taken to the hydraulic press to remove the air

gap between the layers, and any excess air present in the resin, by

applying a force of about 70 to 100N for 48 hours, to get perfect samples.

After the samples get hardened completely, they are taken out from the

hydraulic press, and the rough edges are neatly cut as per the required

dimensions.

(a) Glass fiber layer (b) Resin distribution

(c) Natural fiber layer (d) Fabricated composite laminates

Fig. 3.5: Processing of the composite samples

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The process involved in fabricating the composite specimen is

explained in Fig. 3.5. In this experiment, the sisal, jute and glass fiber

reinforced hybrid composites are prepared at 32±2ºC, and an average

relative humidity of 65%.

(a) Tensile test (ASTM D638) (b) Flexural test (ASTM D790)

(c) Impact test (ASTM A370)

Fig. 3.6: Test specimen as per ASTM standards

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After fabrication, the composite samples are prepared for various

mechanical tests, such as tensile, flexural and impact tests as per ASTM

standards. The standard followed for the tensile test is ASTM D 638

[145], for flexural test ASTM D 790 [146], and the charpy impact strength

was conducted as per ASTM D 6110 [147]. Then the tests are conducted

for three samples in each case, and the average values are used for

discussion. The tensile, flexural and impact test samples according to

ASTM standards, are presented in Fig. 3.6.

3.5 SUMMARY

This chapter presents the details of the materials, and methodology

for fabricating composite samples, polyester resin and its properties,

resin preparation, fiber preparation and hybridization, reinforcement

arrangement, layer sequence, fiber content, processing of composite

samples by the hand lay-up method, and specimen preparation

according to ASTM standards.