54

CHAPTER- 4

EXPERIMENTAL METHODOLOGY
1.1 Materials & Methods 55
1.1.1 Factors Influencing the Materials Selection 55
1.1.1.1 Availability of Materials 55
1.1.1.2 Mechanical Properties 55
1.1.1.3 Environmental Stability 56
1.1.1.4 Ease of Manufacturing 56
1.1.1.5 Cost 56
1.2 Selection of Material for Preparation of Specimen 57
1.3 Fabrication of Laminates 58
1.3.1 Hand layup & Vacuum Bagging Technique for Preparation of the
Laminate 58
1.4 Preparation of Specimen as per ASTM Standards 64
1.5 Tension Test ASTM-3039 70
1.6 Flexural Test ASTM-D790 71
1.6.1 Three-Point Flexural Test 71
1.6.2 Flexural Test Specimen Details 73
1.7 Inter laminar Shear Test / Short Beam Shear Test ASTM-D2344 76
1.8 Failure Modes 78
1.9 Finite Element Analysis 79
BIBLIOGRAPHY 81
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CHAPTER 4

EXPERIMENTAL METHODOLOGY

4.1 MATERIALS & METHODS

This section deals with the selection of materials and its importance, further a

detailed methodology adopted to manufacture the specimen is illustrated here.

4.1.1 Factors influencing the Material Selection

 Availability.

 Mechanical properties.

 Environmental Stability.

 Ease of Manufacturing.

 Cost.

4.1.1.1 Availability of material:

The selection of material is done based on the availability of the material in

the market the ease with which the material is available the commercial accessibility

of the material in the open market were the parameters that were taken into

consideration. The plain bi-woven fibres of glass, graphite and carbon were chosen as

the reinforcing material and epoxy resin was selected as the base matrix material, as

these materials were easily accessible in commercial market and were able to be

procured with a very short lead time.

4.1.1.2 Mechanical properties:

The selection of material is done by emphasizing on the various mechanical

aspects of the material from the literature and also from the manufacturers guide. The

materials selected were having the required mechanical strength, stiffness, stability.
 56

4.1.1.3 Environmental Stability:

The materials are selected considering their environmental stability. The

material fabricated should not respond/react with the environmental conditions and

should not degrade and loose its mechanical properties as the materials are exposed to

the severe environmental conditions. The materials should have sufficient resistance

to combat with the environmental conditions and with stand its mechanical stability.

The material selected should have properties which have anti rusting and anti

chemical reacting properties, should have whether resisting properties. The material

selected should have resistance to UV radiations and should have resistance to

moisture absorption. Finally the material selected should be environmentally stable

and provide best performance with varying environments.

4.1.1.4 Ease of Manufacturing:

The materials selected should have the capabilities to be easily manufactured.

The manufacturing process that is going to be adopted should be simple and general

in its nature in the present application for manufacturing the laminates hand lay up

technique followed by vacuum bagging is adopted .The time period required to

manufacture the composites should be minimum.

4.1.1.5 Cost:

The cost of material plays a significant role in the selection of the material the

composites manufactured should be economical so that it can be wide used for

various applications. If the cost of the material it self becomes too costly it will make

the over all cost of the finished product much costly. Hence while selecting the

material for the preparation of the composites much of the emphasise has to be laid

on the selection of material which is economical in the market.

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4.2 SELECTION OF MATERIAL FOR PREPARATION OF SPECIMEN:

1. Reinforcement Material

 Plain weave Bi-Woven Glass Fabre

 Plain weave Bi-woven Graphite Fiber

 Plain weave Bi- Woven Carbon Fabre

2. Epoxy Resin

 LY556

3. Hardener

 HY 951

The polymer laminates used in the present experimental investigation are plain

weave bi-woven Epoxy / Glass fibre cloth, plain weave bi-woven Epoxy/Graphite

fibre cloth and plain weave bi-woven Epoxy/ carbon fibre cloth with epoxy resin

(LY556 and HY 951) as adhesive with 0/90 fibre orientation and 0 0/450 fibre

orientation. Each layer of cloth is measuring 0.28-0.3 mm thick. Two different

thicknesses of specimens were prepared and the average thicknesses of the laminates

were maintained at 2mm and 4mm.

The laminated composite specimens are fabricated and tested as per ASTM

standards. The laminate was cut to the required size and bonded to the fibre cloth by

using an adhesive made from a mixture of LY556 resin & HY 951 hardener in

proportions of 10:1 by weight. The surfaces were thoroughly cleaned in order to

ensure that they are free from various dusts, oil, dirt, moisture and other chemicals.

etc, before curing of the specimens and bonding at room temperature and pressure.

The models were allowed to cure for about 24 hours and the thorough bonding of the

laminates with the resin is ensured by allowing the laminate to cure for the required

period of time.
 58

4.3 FABRICATION OF LAMINATES

Details of the composite models fabricated are as shown in Fig. 4.1 – 4.9.

1. Hand layup & Vacuum Bagging Technique.

2. Preparation of specimens as per ASTM standards.

4.3.1. Hand layup & Vacuum Bagging Technique for the preparation of the

laminates

 Simple method for production of laminated composites.

 A mold is used for hand lay-up parts.

 The mold can be a plane surface or a flat sheet can be considered and

used as mold.

 Before lay-up, the mold is applied with a release agent to insure that

the part will not adhere to the mold.

 Reinforcement fibres are cut and laid in the mold.

 fibres are aligned in the required direction of the design.

 Resin must then be catalyzed and added to the fibres.

 A brush, roller or squeeze can be used to impregnate the fibres with

the resin.

Vacuum bagging follows similar steps to the hand lay-up process. When the

resin is adequately impregnated into the fibres with excess, the part is sealed with

vacuum bagging materials.

 A layer of peel ply is laid down on the part because the resin will not

stick to peel ply.

 Then a layer of breather cloth is laid down to soak up excess resin and

insure an adequate path for the vacuum pressure.

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 Then a layer of plastic sheeting is laid down and sealed around the part

to isolate the part from the atmosphere.

 A hose pipe is connected to a vacuum pump is attached to the sealed

part.

 A vacuum is then applied using the vacuum pump to the enclosed part.

The part will be compacted by the vacuum and the breather cloth will

collect the excess resin.

The hand lay up process is a simple method which is adopted for the

manufacture of the laminated composites, a mould can be used for this hand lay up

process the mould can be as simple as a flat sheet or a flat surface before the layup is

done the surface is thoroughly cleaned by applying some chemical agents such as

acetone and to this surface a release agent like wax or oil or petroleum jelly is applied

to insure the laminated pert does not adhere to the mould part. The reinforcing

material such as plain weave bi-woven glass fibres, plain weave bi-woven graphite

fibres and plain weave bi-woven carbon fibres are cut into required size and are laid

on the flat surface of the mould. The fibres of the required size are laid along the

required direction as per the design requirements. The resin that is LY556 and

hardener HY 951 are mixed in the proportions as recommended by the manufacturer

in the required proportions that is in the proportions of 10:1 as suggested by the

manufacturer is mixed thoroughly and is applied on the laminated surface to be

laminated. The resin is spread evenly on the reinforcing fibres, the resin is squeezed

evenly on the surface using a roller and compressed thoroughly with the roller it self.

The reinforcing fibres are stacked one above the other and the above mentioned

procedure is repeated repeatedly. The laminated composite material is enclosed in a

bagging and a recommended vacuum pressure is applied on the laminate to remove

 60

the entrapped air bubbles in the layers of the laminated composites. The laminated

composites are allowed to cure for 24 hours. These laminated composites are post

cured at a temperature of 1200c for 2 hours to ensure the even distribution of the resin

and to ensure the proper percolation of the matrix into the reinforcing material. The

laminate is ready and this laminate is cut into required size as per ASTM standard and

subjected to various tests.

The following are the pictures which show the complete process of the

manufacturing process adopted to manufacture the laminates and the specimens as

followed and recommended by ASTM standards. Pictures show the manufacturing

process of the laminates in the sequence of its operation.

The entire manufacturing process is carried as per the standards procedure

followed in the polymer composite industries. The manufacturing methodology

adopted is simple, easy, and takes less time to manufacture the required composite

laminates.

Table 4.1: Details of Composite Prepared

Fibre Laminate
No. of
Sl. No. Laminate Orientation Thickness
Layers Used
In Deg. In mm
1. 2 7
Glass/Epoxy 0/900
2. 4 14
3. 2 7
Glass/Epoxy 0/450
4. 4 14
5. 2 7
Carbon/Epoxy 0/900
6. 4 14
7. 2 7
Carbon/Epoxy 0/450
8. 4 14
9. 2 7
Graphite/Epoxy 0/900
10. 4 14
11. 2 7
Graphite/Epoxy 0/450
12. 4 14
 61

Following figures illustrates the sequential process of manufacturing of the

laminated composites.

Fig.4.1: Picture of plain bi-woven Glass fibre and plain bi-woven graphite fibre rolls

Fig.4.2: Picture of plain bi-woven Glass fibre cut into the required size

Fig 4.3: Picture of plain bi-woven Glass fibre and resin being mixed in a container
 62

Fig.4.4: Picture showing the Resin being applied on the Glass fibres

Fig.4.5: Picture showing the Resin being applied on the Glass fibres

Fig.4.6: Picture showing the Resin being applied on the Glass and Graphite
fibre fibres
 63

Fig.4.7: Picture showing the Resin being applied on the Glass fibre

Fig.4.8: Picture showing the carbon fibre laminate being manufactured

Fig.4.9: Picture showing vacuum bagging process performed

 64

4.4 PREPARATION OF SPECIMEN AS PER ASTM STANDARDS

After the preparation of the laminates the specimens were cut as per the

ASTM standard and the standard specimens are as shown in the pictures below.

Fig.4.10: Picture showing the glass fibre laminated specimen.

Fig.4.11: Picture showing the graphite laminated specimen

Fig.4.12: Picture showing the Carbon laminated specimen

 65

Fig.4.13: Picture showing glass fibre reinforced

laminates

Fig.4.14: Picture showing Graphite fibre reinforced

laminates
 66

Fig.4.15: Picture showing Carbon fibre reinforced laminates –ASTM Standards

Fig.4.16: Picture showing Carbon & Glass fibre reinforced laminates

 67

Fig.4.17: Picture showing the Tensile Test Specimens

Fig.4.18: Picture showing the Glass Fibre Reinforced ILSS Test Specimen

Fig.4.19: Picture showing the Graphite Fibre Reinforced ILSS Test Specimen
 68

Fig.4.20: Picture showing the Graphite Fibre Reinforced ILSS Test

Specimen

Fig.4.21: Picture showing the Glass Fibre Reinforced ILSS Test

Specimen
 69

Fig.4.22: Picture showing the Glass Fibre Reinforced ILSS Test

Specimen

Fig.4.23: Picture showing the Glass Fibre Reinforced ILSS Test

Specimen
 70

4.5 TENSION TEST ASTM -3039

The following types of specimens were prepared as recommended by the ASTM

3039 standards.

Type A: Plain bi-woven glass fibre reinforced laminates [00/90 0] n.

Type B: Plain bi-woven graphite fibre reinforced laminates [00/900] n.

Type C: Plain bi-woven Carbon fibre reinforced laminates [0 0/900] n.

The specimen is prepared as per the specifications shown below.

Fig.4.24: Specifications of the Tensile Test Specimens

Figure 4.25 shows the specimen being mounted

on the tension test rig. The tension test is

conducted as per ASTM 3039 standard. The

specimen is loaded gradually the loading was

done at a controlled rate, the load at yield point

is noted down. Further the specimen was loaded

till the specimen fails. The load at yield point

was recorded. This is repeated for different

specimens. Fig.4.25: Specimen being

subjected to Tension Test.
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4.6 FLEXURAL TEST- ASTM D-790

Fig.4.26: Schematic of 3 point flexural

test

The primary objective of this test is to investigate experimentally the

mechanical behaviour of composite materials subjected to flexural loadings. The use

of flexural tests to determine the mechanical properties of resins and laminated fibre

composite materials is widespread throughout industry owing to the relative

simplicity of the test method, instrumentation and equipment required. It is also

possible to use flexure tests to determine the inter laminar shear strength. By careful

design of the laminated composite beam it is possible to asses not only the flexural

and shear stiffness, but also flexural modulus and flexural strength. Flexural test may

also be used to evaluate the inter laminar fracture toughness of laminates. In general,

flexure type tests are applicable to quality control and material selection where

comparative rather than absolute values are required. As such, these types of test

continue to be used widely because their relative simplicity allows a rapid assessment

to be made with a minimum of technical expertise.

4.6.1 Three-point flexure test: For flexure tests there is no involvement with end-

tabs, or (normally) changes in the specimen shape, tests being conducted on simply

supported beams of constant cross-section area. This method most usually used for
 72

the determination of flexural properties of laminates illustrated in Figure below. A flat

rectangular specimen is simply supported close to its ends and either centrally loaded

in three-point bending. The specimen will be mounted on two supports of the bottom

fixture, perpendicular to the loading nose, and then the upper anvil will be manually

adjusted just barely touching the composite specimen. After the initial preparation, the

test will be conducted and automatically stopped at rupture of the specimen. The

results from the series of flexural tests indicate the relative consistent flexure stress

and strain of the composite specimens. Three point bend fixture proved to be suitable

with adjustable span as recommended by the ASTM specifications.

Load Cell capacity 5 kN

Load Cell accuracy +/- 1% of
indicated load
LVDT for Range 10 mm
displacement
Maximum cross 700 mm with
head travel load cell &
Grips
Flexural specimen Adjustable span
support span
Fixtures 3 and 4 Point
fixtures
Motor details AC Induction
Motor
Control Panel Micro- Processor
based

Table-4.2: Specification of Test Fig.4.27: Specimen mounted on

Rig Flexural Test Rig

The specification of the test rig is provided and the test rig is shown by the

side of it. The specification plays an important role in the conduction of the

experiments the accuracy of the experimental values depends on the specification of

the test rig & the speed at which the cross head traverse.
 73

4.6.2 Flexural Test Specimen Details:

FIBRE
SPECIMEN TYPE THICKNESS
ORIENTATION

2mm
0 0
0 /45
4mm
Bi-Woven Glass Fibre
Reinforced Polymer 2mm
0 0
0 /90
4mm

2mm
0 0
0 /45
Bi-Woven Graphite Fibre 4mm
Reinforced Polymer 2mm
0 0
0 /90
4mm

2mm
0 0/450
4mm
Bi-Woven Carbon Fibre
Reinforced Polymer 2mm
0 0
0 /90
4mm

Table-4.3: Details of the Specimens prepared for Flexural Test

The various specimens prepared for the flexural tests are as listed above from

the table it can to understood that there are basically three fibre types used they are

plain bi-woven Glass fibre, graphite, and carbon fibre reinforced polymer laminates

with two different fibre orientations that is 00/900 and 00/450, further the laminates are

manufactured for two different thickness 2mm and 4mm. These specimens are

subjected to 3-point bending test and the flexural test is conducted as per the ASTM

D790 standards. The test is carried by gradually loading the specimen and the various

flexural properties are determined.

 74

Fig.4.28: Specimen being loaded on the Test Rig

Fig.4.29: Specimen under flexural loading

 75

Fig.4.30: Load displacement curve on the monitor & Specimen Being loaded
on the Test Rig.

Fig.4.31: Load & displacement values recorded on the digital indicator & the
specimen being loaded on the Test Rig.

The figures above show the various sequential procedures that are followed in

conducting the flexural test. The specimen is mounted on the flexural test rig the load

is applied gradually on the specimen at a controlled rate. The load is recorded at the

yield point the load is applied further till the specimen fails it was observed that the

laminate fails gradually the maximum load is recorded at the yield point after that the

there was a decrease in the load applied specimens were loaded till the specimen fails.
 76

4.7 INTERLAMINAR SHEAR TEST / SHORT BEAM SHEAR TEST

ASTM D-2344

Laminated Fibre reinforced polymer–matrix composite materials have been

used successfully in many industries such as aerospace, automobile, marine, military,

etc., their inter laminar shear strength (ILSS) is usually a limiting design

characteristic. This is because conventional manufacturing techniques do not produce

reinforcing Fibres oriented in the thickness direction to sustain transverse load [1].

Inter laminar shear properties are important data required for the analysis of polymer

matrix composite structures. These properties of a variety of polymer matrix

composites under quasi-static loading conditions are well documented. Currently, the

most widely practiced ILS strength standard is the three-point bend test ASTM

D2344, also known as short beam shear (SBS). Improving ILSS has long been an

important goal in the Fibre reinforced composites field, and to this end, different

approaches have been tried. Some of the more effective attempts have been weaving

Fibres in the thickness direction or using Z-pins to connect the laminae [2–7].

TYPE ORIENTATION THICKNESS

0 0 2mm
GLASS FIBRE 0 / 90
4mm
0 0 2mm
GRAPHITE 0 / 90
4mm
0 0 2mm
CARBON 0 / 90 4mm

Table-4.4: Details of specimen for Short Beam

Shear Test
 77

Fig.4.32: Picture showing the Inter laminar shear and specimen loaded for the test

Fig.4.33: Picture showing the Inter laminar shear and specimen loaded for the test

Fig.4.34: Picture showing Short Beam Shear Test Being Performed

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4.8 FAILURE MODES

The steadily increasing utilization of polymer based composites in high

performance structural applications demands that reliable quality control techniques

be developed. In view of the need to characterize a variety as wide as possible of

fracture mechanisms testing was carried out in flexure. This is more versatile loading

configuration whereby three major failure modes may be induced namely, tensile,

compressive and de lamination, each comprising a sequence of fracture events.

Previous investigations [8-10] also reported that the ultimate strength of

composites might be higher or lower than the polymer matrix material. In view of Fu

et al [11] the ultimate strength of a composite depends on the weakest fracture path

throughout the material. Hard particles affect the strength in two ways. One is the

weakening effect due to the stress concentration they cause, and another is the

reinforcing effect since they may serve as barriers to crack growth. In some cases, the

weakening effect is predominant and thus the composite strength is lower than the

matrix; and in other cases, the reinforcing effect is more significant and then the

composites will have strengths higher than the matrix. Prediction of the strength of

composites is difficult. The difficulty arises because the strength of composites is

determined by the fracture behaviours which are associated with the extreme values of

such parameters as interface adhesion, stress concentration and defect size/spatial

distributions. Thus, the load-bearing capacity of a particulate composite depends on

the strength of the weakest path throughout the microstructure, rather than the

statistically averaged values of the microstructure parameters.

Sreekanth et al [9] attribute the reduction of failure strain with the increase of

filler content to the interference of filler in the mobility or deformability of the matrix.

This interference is created through the physical interaction and immobilization of the
 79

polymer matrix by the presence of mechanical restraints, thereby reducing the

elongation at break. As for failure strain, it was found that all composites have lower

failure strain than the matrix material, and that the failure strain is inversely

proportional to the filler volume fraction and filler stiffness. Similar results were

reported by several investigators [12].

4.9 FINITE ELEMENT ANALYSIS

During this period effort has been successfully made to investigate the flexural

strength and stiffness of Polymer Matrix Composite using Finite Element Analysis.

The understanding of the mechanical and physical property determination and damage

evaluation of PMC experimentally is very complex and cumbersome. Alternatively,

FEA tool has been applied as a part of this work to carry out the investigations on

Polymer Matrix Composites subjected to flexural load. In this work, properties of

epoxy/ glass, epoxy carbon and epoxy/graphite Fibres (Continuous) and epoxy resin

system has been used and commercially available FE package ANSYS has been used

for conducting static analysis. The element chosen was SHELL 99 shown in fig below

which is compatible for laminated composite structures. The modelling was

performed with four layers at different orientation (00/900/00/90 0) and the total

thickness of the specimen was maintained at 2 & 4 mm throughout the analysis. With

the new approach of reinforcing glass as well as graphite and carbon as Fibres the

influence of these Fibres on the flexural strength, stiffness and structural efficiency

were evaluated without sacrificing to the weight and the results are discussed &

presented.
 80

Fig.4.35: Showing the Shell 99 geometry

 81

BIBLIOGRAPHY
[1] Rosselli F, Santare MH. Comparison of the short beam shear (SBS) and

interlaminar shear device (ISD) tests. Compos Pt A: Appl Sci Manuf 1997;

28(6), pp. 587–94.

[2] Byrd LW, Birman V. Effectiveness of z-pins in preventing delamination of co-

cured composite joints on the example of a double cantilever test. Compos Pt

B: Eng 2006; 37 (4–5), pp. 365–78.

[3] Jain LK, Mai YW. In the effect of stitching on mode-I delamination toughness

of laminated composites. Compos Sci Technol 1994;51(3), pp 331–45.

[4] Partridge IK, Cartie DDR. Delamination resistant laminates by Zfiber (R)

pinning: part I – manufacture and fracture performance. Compos Pt A: Appl

Sci Manuf 2005; 36(1), pp. 55–64.

[5] Sharma SK, Sankar BV. Effect of stitching on impact and interlaminar

properties of graphite/epoxy laminates. J Thermoplast Compos Mater

1997;10(3):241–53.

[6] Zhang X, Hounslow L, Grassi M. Improvement of low-velocity impact and

compression-after-impact performance by z-fibre pinning.Compos Sci Technol

2006; 66(15), pp. 2785–94.

[7] Mouritz AP, Leong KH, Herszberg I. A review of the effect of stitching on the

in-plane mechanical properties of fibre-reinforced polymer composites.

Compos Pt A: Appl Sci Manuf 1997;28(12), pp. 979–91.

[8] Sapuan, S.M .; Harimi, M. and Maleque M. A. Mechanical properties of epoxy/

coconut shell filler particle composites. The Arabian Journal for Science and

Engineering, 28, (2B), 2003.

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[9] Sreekanth, M .S.; Bambole, V.A.; M haske, S.T. and Mahanwar, P.A. Effect of

Particle Size and Concentration of Flyash on Properties of Polyester

Thermoplastic Elastomer Composites. Journal of Minerals & M aterials

Characterization & Engineering, 8(3), 2009, pp. 237-248.

[10] Sideridis, E.; Ky topoulos, V.N.; Prassianakis, J.N. and Sakellaris, I. Ap ril .

Acoustic and Mechanical properties of particulate composites. 3rd International

Non Destructive Testing Symposium and Exhibition, Istanbul Turkey, 2008.

[11] Fu, Shao-Yun; Feng, Xi-Qiao; Lauke, Bernd and Mai, Yiu-Wing. Effects of

particle size, particle/matrix interface adhesion and particle loading on

mechanical properties of particulate–polymer composites. Composites: Part B

39 2008, pp 933–961.

[12] Akinci, A.,Mechanical and morphological properties of basalt filled polymer

matrix composites. Archives of materials science and engineering 35 issue 1,

2009, pp 29-32.