Lab Oriented Project (BITS C313) Final Report

on
Experiments on Resin Transfer Molding

Under the supervision of Prof. B.J.C.Babu

K.V.Ravi Krishna 2006A4PS336G

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 INDEX
1. Composite materials 3
2. Resin systems 3
3. Fiber Reinforcement 4
4. Fiber Glass 4
5. Composite manufacturing 5
5.1 Hand Lay up 5
5.2 Spray Lay up 5
5.3 Resin Transfer Molding 6
5.4 Prepeg process 7
5.5 Resin Infusion process 7
5.6 Pultrusion 7
5.7 Filament Winding 8
6.1 Advantages of RTM 8
6.2 Disadvantages of RTM 9

7. Experiments conducted on polyester resin 10

7.1 Experiment 1 11

7.2 Experiment 2 12

7.3 Experiment 3 13

8. Experiment on an RTM 14

9. Double Cylinder Resin Injection System 14

9.1 Manufacture of Double cylinder Resin Injection System 14

a. Cylinders (hollow) 14

b. Flange 16
c. Solid cylinder 16
d. Pipes 16
10. Machining Process 17
11. Procedure for RTM 30
12. Some typical RTM products 30
13. Precautions while using RTM 32
14. Conclusion 34

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Introduction

1. Composite materials:
Composite materials by definition are made from combining two or more different
materials. These materials can be as simple as straw and clay or as complex as carbon fiber and
epoxy resin. A typical composite material consists of strong light fibers held in place by a
polymeric matrix material. The fibers serve as the primary load bearing material in the
composite. The role of matrix is to hold the composite together. It also protects the fibers from
the environment and helps distribute the load between fibers. Generally the composite with
higher volume fraction of glass fibers will be stronger if all the other things are equal. Also the
strength of composite is highly dependent on the orientation of fibers to the direction of load.
The composites are much stronger in the fiber direction. This allows designers to optimize the
weight of a structure by reinforcing it in the directions of anticipated load.

The physical properties of composite materials are generally not isotropic (independent of
direction of applied force) in nature, but rather are typically orthotropic (different depending on
the direction of the applied force or load). For instance, the stiffness of a composite panel will
often depend upon the orientation of the applied forces and/or moments. Panel stiffness is also
dependent on the design of the panel. For instance, the fiber reinforcement and matrix used, the
method of panel build, thermoset versus thermoplastic, type of weave, and orientation of fiber
axis to the primary force.

In contrast, isotropic materials (for example, aluminium or steel), in standard wrought forms,
typically have the same stiffness regardless of the directional orientation of the applied forces
and/or moments.

The relationship between forces/moments and strains/curvatures for an isotropic material can be
described with the following material properties: Young's Modulus, the Shear Modulus and the
Poisson's ratio, in relatively simple mathematical relationships. For the anisotropic material, it
requires the mathematics of a second order tensor and up to 21 material property constants. For
the special case of orthogonal isotropy, there are three different material property constants for
each of Young's Modulus, Shear Modulus and Poisson's ratio--a total of 9 constants to describe
the relationship between forces/moments and strains/curvatures.

2. Resin systems:
Common resin systems used in advance composites include polyester, vinyl-esters,
epoxies and thermoplastics. Polyester and vinyl ester resins have low viscosities and are more
benign environmentally than epoxies and tend to be less expensive. Epoxy resin systems tend to
be more versatile but are expensive and have environmental concerns associated with them.
Thermoplastic resin systems are the toughest of the resin systems but are highly viscous and are
not suited to process either by hand lay-up or RTM. Generally resin systems are processed as

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liquids. Resin systems cure by either forming cross-linked polymer chains, thermo sets or by
making vary long, entangled polymer chains. The cure time of a resin system is very important to
both RTM and hand lay-up. Resin systems have to remain liquid long enough to fill the mould
and properly wet out the fibers. The working time of a resin is referred to as gel time.

3. Fiber reinforcement:
Fibers bear the majority of load in a composite. Fibers used for RTM and hand lay-up
generally come in a textile form. First group of fibers are bundled together commonly called
fiber tows. Then bundles are stitched or woven to make a fabric. Fabrics may consist of
randomly oriented fibers, uni-directional fibers or several differently oriented fiber layers
stitched together.

4. Fiberglass:

Glass fiber is formed when thin strands of silica-based or other formulation glass is
extruded into many fibers with small diameters suitable for textile processing. Glass, even as a
fiber, has little crystalline structure (see amorphous solid). The properties of the structure of glass
in its softened stage are very much like its properties when spun into fiber. One definition of
glass is "an inorganic substance in a condition which is continuous with, and analogous to the
liquid state of that substance, but which, as a result of a reversible change in viscosity during
cooling, has attained so high a degree of viscosity as to be, for all practical purposes, rigid."

Glass fibers are useful because of their high ratio of surface area to weight. However, the
increased surface area makes them much more susceptible to chemical attack.

By trapping air within them, blocks of glass fiber make good thermal insulation, with a thermal
conductivity on the order of 0.05 W/(mK).

Glass strengths are usually tested and reported for "virgin" fibers: those which have just been
manufactured. The freshest, thinnest fibers are the strongest because the thinner fibers are more
ductile. The more the surface is scratched, the less the resulting tenacity. Because glass has an
amorphous structure, its properties are the same along the fiber and across the fiber. Humidity is
an important factor in the tensile strength. Moisture is easily adsorbed, and can worsen
microscopic cracks and surface defects, and lessen tenacity.

In contrast to carbon fiber, glass can undergo more elongation before it breaks. There is a
correlation between bending diameter of the filament and the filament diameter. The viscosity of
the molten glass is very important for manufacturing success. During drawing (pulling of the
glass to reduce fiber circumference), the viscosity should be relatively low. If it is too high, the

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fiber will break during drawing. However, if it is too low, the glass will form droplets rather than
drawing out into fiber.

5. Composite manufacturing:
In order to make a composite material the resin system need to be combined with the
fiber reinforcement. Since the orientation of the fibers is critical to the properties, it is essential
that the manufacturing process properly align the fibers. In addition, a good process will leave
parts with a high, uniform fiber volume fraction, allow rapid production of a large volume of
parts economically and have repeatable dimensional tolerances. The most common processes for
manufacturing composites are Hand lay-up and RTM.

5.1 Hand Lay-up:

Hand lay-up is an open mould process. Fabric layers are laid one at a time onto a one
sided mould. Resin is applied to each layer by pouring or spraying and pressed through the
thickness with a roller. A squeegee is used to remove excess resin and then another layer is
added. This process is repeated until all reinforcement layers have been placed. Because hand
lay-up requires simple tools and one mould surface, it is inexpensive to start up. Unfortunately, it
also requires a large amount of labor and high cycle time to produce parts. Since hand lay-up is
an open mould process, a considerable amount of volatiles are released from resin during
processing.

5.2 Spray Layup

Fibre is chopped in a hand-held gun and fed into a spray of catalysed resin directed at the mould.
The deposited materials are left to cure under standard atmospheric conditions.

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5.3 Resin Transfer Molding
Resin transfer molding (RTM) is a closed mould process for making composite
materials. It has the potential to produce parts more cost effectively than hand lay up or other
methods. However fluid flow tends to be unpredictable and is difficult to engineer without some
predictive method for resin flow. First, dry reinforcing fibers are placed in a two sided mould.
The mould is then sealed and at this time it is common to pull a vacuum. A vacuum helps
eliminate void formation during injection since the resin does not need to push air out of the
mould. The resin is then mixed to initiate curing and is injected under pressure. Resin viscosity is
critical to the RTM process. Injection times are limited and the fiber mats have a very low
permeability. If pressures get too high, the fibers will be moved by the resin, commonly called
fiber wash. Low viscosities decrease injection times and lower the risk of fiber wash.

The closed mould of RTM offers several advantages over hand lay-up. Parts have better
tolerances, they are finished on both sides and higher fiber volume fractions are possible. In
addition the closed mould prevents volatiles from escaping during processing. The principle
drawback of RTM is the start up cost. RTM requires expensive injecting equipment and RTM
moulds are expensive to produce. Accurate predictions of resin flow are necessary in order to
properly locate injection and vent ports.

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5.4Prepeg Moulding:
Fabrics and fibres are pre-impregnated by the materials manufacturer, under heat and
pressure or with solvent, with a pre-catalysed resin. The catalyst is largely latent at
ambient temperatures giving the materials several weeks, or sometimes months, of
useful life when defrosted. However to prolong storage life the materials are stored
frozen. The resin is usually a near-solid at ambient temperatures, and so the pre-
impregnated materials (prepregs) have a light sticky feel to them, such as that of
adhesive tape. Unidirectional materials take fibre direct from a creel, and are held
together by the resin alone. The prepregs are laid up by hand or machine onto a mould
surface, vacuum bagged and then heated to typically 120-180°C. This allows the resin to
initially reflow and eventually to cure. Additional pressure for the moulding is usually
provided by an autoclave (effectively a pressurised oven) which can apply up to 5
atmospheres to the laminate.

5.5Resin Infusion Process:

Dry fabrics are laid up interleaved with layers of semi-solid resin film supplied on a
release paper. The lay-up is vacuum bagged to remove air through the dry fabrics, and
then heated to allow the resin to first melt and flow into the air-free fabrics, and then
after a certain time, to cure.

5.6Pultrusion
Fibres are pulled from a creel through a resin bath and then on through a heated die. The
die completes the impregnation of the fiber, controls the resin content and cures the
material into its final shape as it passes through the die. This cured profile is then
automatically cut to length. Fabrics may also be introduced into the die to provide fibre
direction other than at 0°. Although pultrusion is a continuous process, producing a
profile of constant cross-section, a variant known as 'pulforming' allows for some
variation to be introduced into the cross-section. The process pulls the materials through

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 the die for impregnation, and then clamps them in a mould for curing. This makes the
process non-continuous, but accommodating of small changes in cross-section.

5.7Filament Winding
This process is primarily used for hollow, generally circular or oval sectioned
components, such as pipes and tanks. Fibre tows are passed through a resin bath before
being wound onto a mandrel in a variety of orientations, controlled by the fibre feeding
mechanism, and rate of rotation of the mandrel.

6.1 Advantages of RTM :

1. Net shape parts can be produced, eliminating some finishing operations.

2. Many reinforcements such as thick or 3-D wovens, stitched assemblies and braids, are
difficult to mold by conventional means, all of these forms can be handled via RTM and
no problems have been reported with any specific fibre types.

3. A wide variety of resin systems can be utilized. Much epoxy resin for formulaton for
prepeg is related to flow control during consolidation, this is not required for RTM resins

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 although the need for a low viscosity can be difficult to reconcile with toughness
requirements. Resins that cure by condensation reactions or contain volatiles are not
ideal. Even so good results have been reported with acid catalysed phenolics.

4. As noted above, the prepreg process stages relating to flow control and consolidation in
autoclaves are not required in RTM. This can lead to simplicity in cure scheduling, faster
heat-up rates for tools that are not injected at the cure temperature and generally leads to
shorter overall cure cycles.

5. Because prepreg is not used the shelf-life and refrigerated storage costs associated with
the use of prepreg are avoided.

6. For fixed cavity tooling, fibre volume fractions can be very well controlled, leading to
very consistent mechanical properties.

7. The factors leading to porosity and voidage in RTM are somewhat different to those in
prepreg molding. With correct mold design and good process control very low or zero
voidage levels are routinely achieved.

8. Experience with operating production lines has shown that defect rates in RTM
production of aerospace parts can be lower than those experienced in autoclave molding
production lines. While positioning of quality control inspection points may be different
for RTM and autoclave work, good control can be imposed on RTM-based production
lines.

9. Very complex parts can be produced in RTM. Many components have shown high levels
of parts integration, leading directly to cost savings. Some of the usual geometric
limitations, such as the use of bend radii several times the laminate thickness, can be
eliminated through the use of RTM.

10. Low pressure operations, molded-in inserts, fittings, ribs are possible.

11. Considerable design flexibility, class-A surface finish, short cycle times, requires low
labor intensity and skill levels.

6.2 Disadvantages:
1. Mold and tool design critical to part quality.

2. Tooling costs can be high for large production runs.

3. Preform and reinforcement alignment in the mold is critical.

4. Production quantities range from 100-5000 parts.

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 5. Requires matched, leakproof moulds.

7. Experiments Conducted on Polyester resin:

Study of kinetics of polymerization reaction of an orthotropic polyester resin (using MEKP and
Cobalt Octate as initiator and accelerator respectively):

Theory:
Polyester resin cures by an exothermic reaction created by the activator Methyl Ethyl
Ketone Peroxide (MEKP). The reaction of polyester will occur at the thickest cross section
sending out a wave of heat which cures resin to a hard glass like hardness. Temperature and
moisture content can affect the rate of cure and drying of part’s surface. The ratio is dependent
on air temperature, resin thickness, temperature of resin and mould. Resins that create
uncontrolled peak exotherm can exhibit wrinkles or alligator skin like surface deviation. In wet
weather conditions, tacky surfaces may be exhibited by resin due to high humidity. Working in a
controlled, heated area should help resin to cure properly.

In the reaction, the free radicals formed when the peroxide bond
breaks, attack the unsaturated bond in styrene. The Cobalt Octate MEKP

accelerates the reaction enabling the formation of a polymer.

Polyester

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Experiment 1:
Chemicals used:

Orthotropic polyester resin: 100gm

MEKP: 3.2 ml

Cobalt octate: 3.2 ml

The above chemicals were mixed thoroughly in a polypropylene beaker and temperatures
were observed.

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Experiment 2:
Orthotropic polyester resin: 100gm

Calcium Carbonate: 20gm

MEKP: 1.8 ml

Cobalt Octate: 1.8 ml

The above chemicals were mixed thoroughly in a polypropylene beaker and temperatures were
observed.

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Experiment 3:
Orthotropic polyester resin: 50gm

Calcium Carbonate : 5gm

MEKP: 1.6ml

Cobalt Octate: 1.6ml

The above chemicals were mixed thoroughly in a polypropylene beaker and temperatures
were observed.

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8. Experiment on an RTM:
A Resin Transfer Molding process was conducted on a small sized RTM machine (non-
vacuum). The primary difficulties faced were fast gel times and low resin flow rates in the fiber.
Possible solutions would be to use multiple injection points instead of a single one. The viability
of using multiple injection points depends on the regulation of pressure at the different points.

9. Double Cylinder Resin Injection System:

Using a double cylinder assembly for separate injection of Cobalt Octate and MEKP was
determined as the most viable solution. In a double cylinder RTM, since MEKP and Cobalt
octate get mixed in the pipe the previous problems encountered due to clogging of resin in the
cylinder can be avoided. Furthermore, since the gel time of the resin is very low, with
appropriate piping, flow of the resin into the mould can be increased contrary to the previous
case. In a double cylinder assembly, MEKP and Cobalt octate are mixed in the pipe. For this the
injection pressure in both the cylinders is to be maintained the same.

Double Cylinder Resin Injection system consists of:

Two hollow cylinders

Flanges

Solid Cylinder

Nylon Pipes

Air Compression system

Mould

9.1 Manufacturing of Double Cylinder Resin Injection System:

a. Cylinders:

A hollow steel cylinder of length 80cm, thickness 5mm and outer diameter 8.7cm was cut into
two halves using mechanical cutter. Resin and MEKP mixture is poured into one of the cylinders
and Resin and Cobalt Octate is poured into second cylinder so that they’ll mix in the common
outlet pipe to the mould.

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b. Flange:

Since we can’t carve the inside of the cylinder to get the taper, two flanges per cylinder
have been used to serve the purpose, one with the hollow cylinder and the other with the solid
cylinder welded to it.

There are three flanges, all the three with same width and thickness and two of them with
length 15cm and the third one 35cm. Upper flange is common to both the cylinders and the two
shorter flanges are welded to solid cylinders.

The edges of the cut flanges were made perpendicular using grinding machine.

For good weld, we need to grind one of the surfaces to get surface finish. First it was
ground roughly using hand grinder and for better surface finish, we grind using universal tool
machine.

c. Solid Cylinder:

Two Solid mild steel cylinders of length 6cm, diameter 5cm are welded to each of the
smaller flanges.

A hole of diameter 1.7cm is drilled in this assembly and is tapered 45 degrees as shown.

A groove of diameter 8.8cm, width 6mm and depth 8mm is made on the each of the
upper surfaces of smaller flanges.

d. Pipes:

Nylon pipes of diameter(outer) 2cm and thickness 1.5mm are used.

Air pressure of 2bar is used for this experiment.

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10. Machining Process:
10.1 Flange: Three flanges of thickness 1.2cm and lengths 15cm, 15cm, 35cm taken.

Two circular holes of diameter 80cm are bored on the larger flange in order to fit the cylinders
without any interference. This is done by center-punching method where we need to drill 6mm
holes on the circumference of the 80cm bore, the material is removed and further finishing is
done for smoothening of the inner surfaces of the bores.

Larger flange with 2 bores

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 The two smaller flanges are welded to the two solid cylinders of length 6cm and
diameter 5cm. For good weld, we need to grind one of the surfaces to get surface finish. First it
was ground roughly using hand grinder and for better surface finish, we grind using universal
tool machine. Then the cylindrical rods are welded to each of the flanges so that the centers of
the two coincide. This setup is shown in the following figures.

Welded solid cylinder and flange

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10.2 Drilling:

A through hole of radius 17mm is drilled in each of the cylinder flange assembly. This drilling is
done on the Lathe machine using 6mm, 9mm, 12mm, 15mm, 17mm drill-bits for effective
through holes, since directly using larger diameter drill bits may result in tool damage and
irregular removal of material. While working, speed(rpm) of the machine should be noticed,
since one cannot use the same speed for all sizes of drill-bits. Small diameter drill bits require
greater speed for machining and larger tools need lesser speed.

Drilled hole in the flange-solid cylinder

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10.3 Taper-turning:

After drilling, the next machining process to be done is the taper-turning of the drilled
product. For this we use single-point cutting tool made of High Speed Steel and the taper angle is
maintained 60degrees. For effective taper-turning, the tool with notched tip is used. The feed is
given in the direction of the notched surface of the tool. This tapering starts at the free surface of
the flange at 80mm diameter and ends in the solid cylinder with 10mm diameter. A groove of
inner diameter 7.8cm, depth 6mm and thickness 7mm is made around the tapered surface of the
flange

Tapering dimensions

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 Groove on the Tapered face of the flange

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 Tapered from bottom side

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 One end of the cylinders is closed with a welded lid. A hole is drilled on the lid and socket of
length 4cm and diameter 1.3cm is fixed on the hole of each cylinder as shown.

Cylinder with socket fixed to the lid.

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 A hole of diameter 17mm is drilled at lid end on the curved surface of the cylinder and a
socket of similar size is welded to it. The Air pressure pipe is fitted into this side socket and resin
is poured from the top socket. The top socket is closed after pouring the resin with air-tight cap.

Side socket

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Now the two large cylinders are fitted exactly into the two bores of the larger flange and are
welded as shown.

Cylinders-Flange Weld

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Next two Mild Steel sockets of length 4cm and diameter 1.3cm are welded at center of the
bottom end of the cylinder-flange assembly. The 1/2 inch- 1/4 inch brass nipple is fitted into the
sockets and the nylon pipe is fitted at the other end of the nipple. The other end of the pipe is
connected to the corresponding mould.

Bottom Socket

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The two smaller flanges and the larger flange are connected with the help of 8 bolts. Annular
gaskets of thickness 6mm are first fixed in the each groove of the smaller cylinders. This is done
so as to ensure that resin don’t leak out while working in high pressure conditions.

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 Fixing of two flanges with cylinders

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 Final view (without pipes) of Double Cylinder RTM

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 11.Procedure:
 The polyester resin + MEKP mixture is poured in one of the cylinders and resin + Cobalt
Octate is poured in the other cylinder and the lids are closed tightly.

 The two bottom pipes are connected to a single pipe and this single pipe is fixed to the
mould of desires shape.

 The mould may contain fibers for more reliable and harder composite.

 Each of the side-socket is connected to Air supply and is maintained at 2bar.

 Due to the air pressure the resin flows to the bottom pipe and the two mixtures results in
the solidification of the resin.

 The resin should flow into the mould before solidification.

 Since the two mixtures come in contact in the common pipe, the gel time is enough for
good amount of resin to settle in the mould.

 Valves of the air supply should be operated carefully since continuous higher pressure
leads to the damage of pipes and lower pressure results in the solidification of the resin in
pipes itself.

 With different shapes of the mould, different shapes of the composite can be obtained.

12.Some typical composite products:

Sporting: Skateboards, snow boards, skis, hockey sticks, race cars, bicycle frames, fishing rods,
tennis rackets, boat hulls.

Aerospace: Solar panel substrates, antenna reflectors, payload adapters, yokes of spacecrafts,
inter stage structures, heat shields of launch vehicles, helicopter blades, nozzles, radomes, rocket
motor casings, fuselage, wings, control surfaces, canisters.

Automobiles: hardtop roofs, dent-resistant door panels, bumper beams, tailgates, spoilers,
“survival cells” in racecars.

Electrical and Electronics Industry: electrical equipment boxes, circuit breakers, electric meter
boxes, power transmission poles and satellite dishes.

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Construction Industry: large complex forms (monobloc bathrooms), girders and framework
paths, decorative panels, roof components, rehabilitation buildings.

Industrial Engineering: chemical product tanks, pipelines and pressurized machines.

Composites In India:
Components used in Indian Railways : window frames, shutters, wall protector in toilets, trays
for battery boxes, snacks tables, air grill (for ac coach), FRP toilet modules, FRP- common mode
adopter, axle box covers, luggage bin, floor, ceiling and roof panels, double deck flooring,
internal side wall panels, external structural panels etc.

Aerospace:

1. Radomes or radar domes are casings for antenna use thermoplastics such as polyether
ether ketones.

2. Rocket motor casing: The composites generally used include carbon and aramid fibres.
Advanced carbon fiber composite RMCs for large rocket motors, such as for AGNI class
systems have been fabricated with indigenous technology.

3. LCA had gone supersonic with several components such as central fuselage, duct skins,
fins, rudder, wings, landing gear, forward and rear fuselage all made from composites
amounting to 45% of weight.

4. The Reinforced Plastics Centre is now in the process of making next generation
composites for use in recoverable missions.

13.Precautions while performing RTM:

1. Always work in well-ventilated areas.

2. Safety goggles, gloves and respirators should always be worn while handling resins,
hardeners and solvents.

3. Never use or store resins, solvents or hardeners near open flame.

4. Uncured resin spills should be absorbed material. The surface can then be cleaned
immediately with hot water and detergent.

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SOME OF THE RTM PRODUCTS :-

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 14.Conclusion:
The manufacture of the double cylinder injection system for the Resin Transfer Molding
machine is complete. Better results can be expected from using a double cylinder machine
instead of a single cylinder one.