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3
Specimen preparation
F L M ATTHEWS

3.1

Introduction

There are a number of subsidiary, but vital, issues that are complementary
to the main activity of mechanical testing. These issues, taken together, constitute the preparatory work required to produce test specimens of adequate quality. If insufficient attention is given to any of these activities, the
results from a particular test could be invalidated. The following remarks
relate to the use of specimens of high performance composites fabricated
from continuous preimpregnated fibres, the subject of this text. The four
stages considered are: laminate production; quality checking; specimen
manufacture; application of strain gauges. The final three stages would, of
course, apply to any material.

3.2

Laminate production

Thin sheets, known as laminates, usually 1 or 2 mm thick for coupon specimens, are manufactured from layers of fibres preimpregnated with partially
cured (if epoxy-based) resin prepreg. The matrix is usually an epoxy, but
BMI (bismaleimide) and thermoplastic prepregs are also used. It should be
noted that the following discourse relates mainly to epoxy prepregs (owing
mainly to their popularity). It should, however, be pointed out that the
preparation of laminates with thermoplastic matrices is in many ways
a similar but more straightforward process, because the plastic resin is
not required to cure, but simply melts at a suitably high temperature and
resolidifies when cooled.
A single prepreg layer is usually 0.125 or 0.25 mm thick and the fibres are
either continuous and parallel (unidirectional), or in the form of a woven
fabric. The prepreg is supplied as tape, normally 0.3 m wide (but suppliers
having width preferences, woven materials being generally wider than unidirectional products), sandwiched between protective layers of paper or
plastic and wound on a reel. If epoxy, the prepreg should be kept in a freezer
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until it is required; if thermoplastic, low temperature is not a requirement

but it is advisable to store the material in a clean, light-free environment.
Shelf-life (for epoxies) is normally around 18 months and will be clearly
stated by the supplier; thermoplastics, on the other hand, generally degrade
very slowly at ambient temperatures. If the prepreg has exceeded its lifetime it can probably still be used for a further six months, at least. However,
its suitability should be checked by moulding a test panel, or by checking
the cure state of the matrix resin using differential scanning calorimetry
(DSC).
Appropriate lengths are cut from the reel and placed on top of each other
with the fibres in each layer oriented relative to one another in a predetermined sequence. Hand tools, such as a Stanley knife drawn against a
hard edge, are usually satisfactory for cutting. Fabric prepreg can be cut
using shears or scissors. Where available, a rotary knife or water jet could
be used. The protective layers are removed before each layer is placed on
that previously laid down, and the layer carefully smoothed out to prevent
air entrapment. It is essential that the layers are aligned with reference to
a datum, since even a few degrees misalignment can cause a dramatic effect
on mechanical properties. With properly prepared prepreg the edge of the
protective backing sheets can be used as a reference. Care must be taken
to ensure that twisted or knotted fibre bundles, or prepreg areas containing gaps between bundles, are not included in the laminate.
Following completion of the layup, the stack of prepreg layers is prepared
for curing in the case of epoxies, or consolidation for thermoplastics. The
epoxy resin, which forms the matrix of the composite, is formulated for
autoclave curing; the whole curing process lasts several hours and involves
a combination of vacuum, raised temperature (to 120 or 175C for epoxies,
often higher for thermoplastics) and raised pressure. The prepreg layers are
contained within a sealed blanket as illustrated in Fig. 3.1.
To prevent the laminate sticking to the base and caul (pressure) plates,
the latter can be coated with release agent, or layers of release fabric or a
polymeric film are inserted between the plates and the prepreg. A disadvantage of the second approach is that an impression of the fabric is left
on the surface of the laminate, thus making it difficult to detect the fibre
orientation in the surface layers with the naked eye.
As an alternative to autoclave curing it is possible to use a heated press,
in which case it is necessary to monitor separately the state of resin gelation, or a press-clave. The latter device, illustrated in Fig. 3.2, is placed in a
heated press, in combination with a separate high pressure supply and a
vacuum source.A heated press, with facilities for rapid cooling of its platens,
would be used for processing advanced thermoplastic prepregs. Clearly the
size of the laminate that can be produced will be determined by the size of
press available.

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Mechanical testing of advanced fibre composites

Vacuum bagging material

Air breather cloth

Laminated composite plate

Peel ply

Pressure plate

Vacuum connection
Melinex
Sealing
tape

3.1 Arrangement for producing laminates by autoclaving.

Top plate
Melinex
Bleed cloth
Peel ply
Laminate
Peel ply
Perforated PTFE
Peel ply
Frame

Baseplate
Vacuum connection

Pressure vessel

Baseplate

Pressure connection
Diaphragm
Top plate
Laminate, etc.
Frame
Vacuum connection

3.2 Layout of a press-clave.

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3.3

39

Quality checking

The manufacturing process, if not properly controlled, can introduce defects

into the laminate. Typical defects are voids (small cavities in the resin),
delaminations (unbonded areas between layers) or, unusually, longitudinal
cracks (lack of bonding between fibre and matrix).
Voids can be caused if the prepreg is not allowed to warm to room temperature before laying-up, thus introducing moisture into the prepreg stack.
Delaminations can be caused by entrapped air or the inclusion of pieces of
backing sheet. Longitudinal splitting and delamination can occur in multidirectional laminates as a result of thermal stresses induced during cooldown from the curing temperature.
All the above defects will degrade mechanical properties, particularly
in compression, shear and flexure. It is, therefore, important that their
presence is detected so that faulty laminates can be discarded.
The standard method of detection is to use ultrasonic C-scan, which is
good at detecting inclusions, porosity and delaminations, or, possibly, X-ray
techniques, which can detect through-thickness cracks.

3.4

Specimen manufacture

Specimens, as defined by the relevant standard, or test to be carried out,

are cut from the laminates using a diamond-tipped saw. The normal blade
has 600 grit, but a cleaner cut, with less damage to the laminate, is obtained
with 800 grit. In the latter case the blade can become clogged with debris
and frequent cleaning may be required. Laminates produced by autoclaving will have a feathered edge which must be removed.
It is clearly vital that edges produced after trimming, which effectively
act as a datum for subsequent specimen cutting, are correctly aligned with
the fibres in the layers. A commonly used method for establishing the 0
direction of a cured laminate prior to cutting is to split off a narrow strip
of material along this direction (in multidirectional laminates this can be
done if the 0 layer is made slightly wider), but it has been shown that this
approach may not be sufficiently accurate, and a preferred method1 is to
mark the outermost ply by scoring across in the 90 direction in a nonstressed region.
High temperatures are generated during dry cutting, which can cause
local degradation and damage at the machined edge. This can be largely
prevented by the use of a coolant (water), but subsequent drying-out steps
must be taken to remove any absorbed liquid from the specimen. Generally, specimen blanks are machined oversize, final dimensions being
achieved by grinding.
Drilling is readily achieved with tungsten carbide or diamond tipped bits,

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Mechanical testing of advanced fibre composites

the laminate being supported by a (sacrificial) backing plate. It is advisable

to use a drill bit tip angle of 5560 for thin laminates and 90100 for thick
sections, rather than the usual 120. Other operations are best achieved by
grinding. Clearly, appropriate support is needed for thin laminates if
through-thickness shaping is to be carried out. Kevlar fibre-reinforced
materials need special attention. Owing to the nature of the fibre it is
difficult to avoid a furry edge. Specially adapted impregnated wheels can
be obtained for cutting. Another alternative is to use a high pressure water
jet.
For many tests, for example tension and compression, it is often necessary to bond end-tabs to the specimen; this is done to diffuse the gripping
loads and prevent failure at the specimen ends. According to the particular requirements, the tabs may be of aluminium alloy, GFRP (glass-fibre
reinforced plastic) or CFRP (carbon-fibre reinforced plastic). When the
tabs are of composite, the preferred method is to stick strips to the trimmed
laminate before cutting into specimens. This approach is not only quicker,
but it also ensures alignment of tabs and specimen. When the tabs are metal
this approach cannot be adopted and the tabs must be bonded to individual specimens, using a jig to give accurate positioning. Surfaces where
end-tabs are to be bonded should be abraded in order to remove surface
contamination, whilst taking care not to damage the outermost fibres. This
is done most easily, particularly if the laminate surface is rough, by grit blasting, the only objection to this method being that the surface may itself
become contaminated, either by grease carried by the grit or embedment
of the grit. Surfaces not needing to be abraded can be protected by masking
with self-adhesive tape. The grade of grit used, typically 80120 grade, does
not appear to be critical if care is taken to avoid excessive abrasion
and damage to the composite. The dust left behind on the material
after grit blasting is most easily removed by flushing under running water.
If the water lies on the surface in an unbroken film, a good standard
of surface cleanliness is indicated. The amount of water absorbed by the
laminate will be small, particularly if the material is dried immediately after
washing.
After drying, the surfaces are solvent wiped and bonded. Commercial
two-tube epoxy resin has been found to be suitable for bonding end-tabs
to be used for tests at room temperature and should be applied sparingly
to both bonding surfaces. The joint, when assembled, can be contained in
a simple vacuum bag which will apply an adequate clamping force and
remove entrapped air. The tab material can be located by using small pegs
inserted in notches cut through the tab and test materials. An alternative
to low temperature curing adhesive is to use bonding film which is cured
under elevated temperature and pressure, although in some cases this can
cause thermal stresses sufficient to split a 0 laminate. Whatever adhesive

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is used it should be tough, with a greater failure strain than that of the material under test. CRAG2 specifies that it should have a shear strength greater
than 30 MPa. Special adhesives would be preferred for fatigue testing or
high temperature work. An incidental advantage in using GFRP end-tabs
is that the material is translucent and any gaps in the glue film can be seen
by visual examination. Even if the joint is strong enough to withstand specimen failure loads, gaps in the glue line can result in uneven stresses in the
underlying composite and cause premature failure.1
The crucial issue when bonding is to ensure that both the specimen and
the tabs are properly prepared. Composites need to be degreased and
abraded to remove all traces of release agent transferred during moulding.
This procedure should be followed by wiping with a solvent. Similar procedures should be followed when making bonded joints. In addition to
degreasing, aluminium alloy tabs need to be etched in chromic acid or
phosphoric acid.

3.5

Strain gauging

All mechanical tests will involve the measurement of displacements or

strains, as defined by the appropriate standard. When strain gauges are
called for, it is important to follow the recommended procedures.The length
of the gauge may be specified by the relevant standards, but should always
be significantly shorter than the gauge length of the specimen. Composites
can cause particular difficulties not encountered with metals.3
The issues that must be addressed are as follows:
1

High gauge resistances are desirable because high voltages (24 V) with
low current can then be used; this improves hysteresis effects and zero
load stability.
If possible, use gauges with lead wires attached, or solder wires to the
gauge before installation; this should avoid soldering damage to the
composite.
Ideally the pattern of the autoclave scrim cloth should be removed
before gauge installation; this is particularly important if contact adhesives are used.
Corrections may be necessary to gauge transverse sensitivity effects;
errors of over 100% between actual and measured strains can be
obtained.
Gauges must be precisely aligned; errors of 15% can result from a 2
misalignment. There is no universally acceptable way of ensuring alignment. The scrim cloth pattern can be misleading. Sometimes C-scan
after installation can be useful, or checking with failure surfaces after
fracture.

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6

Mechanical testing of advanced fibre composites

Dummy gauges are the preferred method for temperature compensation but, again, precise alignment is needed. It is necessary to mount the
dummy gauges on an identical piece of laminate, with the same orientation relative to the fibres as used for the active gauges.

3.6

Summary

In summary, it is essential that careful and consistent procedures are followed at every stage of specimen production. Failure to do so will throw
doubt on the validity of any data generated.

References
1. P W Manders and I M Kowalski, The effect of small angular fiber misalignments
and tabbing techniques on the tensile strength of carbon fiber composites, 32nd
International SAMPE Symposium, Anaheim, CA, USA, eds R Carson, M Burg
and K J Kjoller, Society for the Advancement of Material and Process
Engineering, Covina, CA, USA, 1987.
2. P T Curtis (Ed), CRAG Test Methods for the Measurement of the Engineering
Properties of Fibre Reinforced Plastics, Royal Aircraft Establishment, Farnborough, UK, Technical Report 88012, 1988.
3. M E Tuttle and H F Brinson, Resistance Foil Gauge Technology as Applied to
Composite Materials, Report No. VPI-E-83-19, Department of Engineering
Science and Mechanics, Virginia Polytechnic Institute and State University,
Blacksburg, VA 24061, USA, June 1983.

2000,Woodhead Publishing Ltd, except chapters 6, 8, 11 and 15, Crown copyright.