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Received: 21 December 2022 Revised: 13 April 2023 Accepted: 25 April 2023

DOI: 10.1002/fam.3163

RESEARCH ARTICLE

Effect of fibre orientation and thermal exposure on the


post-fire mechanical behaviour of carbon fibre reinforced
polymer material

Tim J. Aspinall 1 | Emmajane L. Erskine 2 | Derek C. Taylor 2 | Rory M. Hadden 1

1
Centre for Fire Safety Engineering, The
University of Edinburgh, Edinburgh, UK Abstract
2
Defence Science and Technology Laboratory, This study investigates the influence of fibre orientation and heat flux on the post-fire
Dstl Porton Down, Salisbury, UK
(residual) load-bearing properties of carbon fibre-reinforced polymer (CFRP) laminates.
Correspondence As a result, a deep insight into the post-fire load-bearing response is gained, which is
Tim J. Aspinall, Centre for Fire Safety
Engineering, The University of Edinburgh, necessary to fully understand and assess the advantages of CFRP laminates containing
Edinburgh EH9 3JL, UK. different fibre orientations for use in load-bearing structures. Specimens were pro-
Email: timothy.aspinall@ed.ac.uk
duced from three CFRP laminates containing different fibre orientations, exposed to
Funding information varying heat fluxes up to 40 kW=m2 and then loaded in either tension or three-point
Defence Science and Technology Laboratory
bending at ambient room temperature. The study's results have shown that the post-
fire behaviour of CFRP specimens is sensitive to changes in fibre orientation and heat
flux. For example, specimens with an anisotropic fibre orientation in tension had the
highest tensile load-bearing capacity, whereas those with bidirectional and multi-
directional fibre orientations demonstrated lower tensile load-bearing capacities. In
bending, however, specimens containing bidirectional and multidirectional fibre ori-
entations had higher load-bearing capacities than specimens with an anisotropic fibre
orientation. Furthermore, the data also shows that exposure to a heat flux reduces
the load-bearing capacity in both the bending and tensile specimens.

KEYWORDS
carbon fibre reinforced polymer, fire testing, heat flux, mechanical testing, post-fire testing,
tension, three-point bending.

1 | I N T RO DU CT I O N manufacturing costs, more durable matrix resins and increasingly robust


and stiffer carbon fibres (CF), CFRP laminates have been utilised in highly
Carbon fibre reinforced polymer (CFRP) laminates have been used in hazardous primary structural locations, such as jet engine components
aircraft structures for more than half a century1 and are at present the (i.e. inlet fan blades), wings and fuselage sections and close to adjoining
most common fibre-reinforced polymer (FRP) material used in construct- fuel tanks.2 Furthermore, CFRP laminates are also used extensively in
ing new aircraft.1 In past applications, the use of CFRP laminates in air- engineering sectors outside of aerospace due to the material's high spe-
craft structures has remained limited to secondary non-load-bearing cific strength and tensile rigidity, ease of installation and handling, corro-
components such as interior sections, cockpit controls, and auxiliary sion resistance, and relatively good durability, which have facilitated their
power units to minimise weight and maximise structural efficiency.2 In use as both reinforcing material (for the rehabilitation and strengthening
recent years, however, due to modern developments such as lower of existing structures) and in stand-alone applications.3–6

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.
© 2023 The Authors. Fire and Materials published by John Wiley & Sons Ltd.

Fire and Materials. 2023;1–23. wileyonlinelibrary.com/journal/fam 1


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2 ASPINALL ET AL.

As an engineered material, the manufacture of CFRP laminates 1. Ambient (room) temperature conditions: at temperatures below
can vary. Most importantly, the ability to customise the fibre orienta- those required for glass transition of the matrix resin and no
tion of each ply layer means their mechanical properties can be opti- change in mechanical performance.
mised to suit the requirements of the application or load.7 Therefore, 2. Low exposure (LE): temperatures equal to the glass transition
fibre reinforcements may take different forms. For example, when temperature (Tg) of the matrix resin.
CFRP laminates are used adjacent to hazardous locations within air- 3. Medium exposure (ME): temperatures equal to the matrix thermal
craft structures, such as the wing rib which surrounds the fuel tank, decomposition (pyrolysis) temperature (Td).
they often employ a near isotropic fibre orientation,8 such as a woven 4. High exposure (HE): the temperatures equal to the oxidation
quasi-isotropic [0 , 90 ] or cross-plied quasi-isotropic [0 , 45 , 90 ] temperature (To) of the char and CF.
fibre orientation to distribute stresses. However, in other sections,
not necessarily adjacent to the fuel tank but located close to it, such
as wing sections main spar,2 unidirectional [0 ] carbon fibre's orien- 1.1 | Existing studies
tated parallel to the loading direction are often used to carry longitu-
dinal tensile or bending loads, meaning that CFRP laminates with Whilst existing studies examining the post-fire mechanical behaviour
different fibre orientations are often used near or adjacent to aircraft of CFRP laminates have shown that the reduction in the post-fire
fuel tanks which poses a fire risk. mechanical properties can be attributed to thermal degradation and
CFRP laminates are intrinsically different to metallic alloys due to damage caused by the heat from a fire, these studies were restricted
their combustible matrix resin.9 The combustibility of the matrix resin to measuring the post-fire behaviour of CFRP containing a single fibre
is a well-known, long-standing problem that can result in a loss of orientation17–20 without comparing this behaviour to other commonly
load-bearing capacity after exposure to heat from a fire in the event used fibre orientations, even though the mechanical properties of
of an in-flight or post-crash fire.10,11 CFRP laminates are heavily dependent on the type of fibre orienta-
Upon exposure to heat from a fire, a CFRP laminate's tempera- tion.21,22 Furthermore, in studies investigating fibre orientation on
ture (nearest the heated surface) will rise. As the duration of expo- post-fire behaviour, only one study, to the author's knowledge, has
sure increases, a thermal wave will begin to penetrate the thickness. been carried out in tension,20 with no study evaluating the influence
As the temperature increases, the matrix resin will undergo glass of fibre orientation on post-fire bending behaviour. On the other
transition when it reaches the glass transition temperature (Tg), hand, in the studies that do compare fibre orientation of CFRP lami-
resulting in a loss in matrix stiffness. Further heating above the Tg nates in tension and bending,23–26 the focus has been on the mechan-
will lead to the matrix resin's thermal decomposition (pyrolysis) at ical properties or influence of fibre orientation and thermal ageing on
the thermal decomposition temperature (Td). In the event of the cor- the performance of said materials with no focus on post-fire residual
rect conditions for combustion, the pyrolysis gases may ignite, and a behaviour. That said, in the studies that have examined the influence
flame will form on the CFRP laminate. This flame will provide further of fibre orientation on post-fire behaviour, only a few have focussed
thermal energy to the solid, increasing the heating rate and fire size, on the influence of fibre orientation specifically on the post-fire
thus resulting in an increased hazard to adjacent materials and behaviour of CFRP laminates, with most studies in this area focussing
mechanically resulting in a loss in strength and load-transferring on either glass, aramid or other fibres, or resin systems.27–30 In addi-
12
capacity. However, the high threshold temperature for the CF may tion to these points, most of the referenced literature above charac-
allow them to carry some load in the loading direction at the Td.13 As terise the ‘fire conditions’ using circulating hot air with temperature
the CFRP laminate continues to be heated to very high tempera- boundary conditions, limiting the conditions that can be tested and
tures, the char and CF will begin to thermally oxidise.9 Oxidation typically requiring thermal equilibrium to be established prior to
damage begins at the oxidation temperature (To) of the char and mechanical testing to ensure a well-characterised temperature in the
CF. The exothermic heterogeneous oxidation of the char can reduce material. This approach is a limitation, as many structures will not
the char layer thickness and release additional energy, which can be reach thermal equilibrium during a fire. Therefore, the thermal bound-
transferred into the material, promoting further thermal decomposi- ary conditions are better defined using heat flux31,32 to allow the
tion resulting in a loss in those mechanical properties dominated by material's mechanical response to be explicitly linked to the thermal
the CF, for example, the tensile strength. After oxidation, only inert environment. Consequently, the influence of different thermal expo-
ash concentrations will remain.14 Further descriptions of the glass sures on the post-fire properties of CFRP laminates containing differ-
transition, pyrolysis and oxidation processes on CFRP laminates and ent fibre orientations has not been well established.
9,15
their influence on mechanical properties can be found elsewhere ; Because of the abovementioned issues, this study will investigate
however, the characteristic behaviour of CFRP laminates means, for the influence of fibre orientation and thermal exposure (heat flux) on
the most part, that when a CFRP laminate has been exposed to fire the post-fire tensile and three-point bending behaviour in terms of
conditions, even after the fire is quickly extinguished, the mechanical temperature distribution, failure load, stress–strain relationship, failure
performance may be reduced and the load-bearing ability lower than mode, and failure time. The motivation for this study is due to the
originally.16 This behaviour can be described based on four condi- paucity of existing knowledge regarding the post-fire behaviour of
tions of exposure. These are at: CFRP laminates created using common fibre orientations utilised in
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ASPINALL ET AL. 3

hazardous locations of aircraft structures, all of which have been In total, 48 specimens were produced, 16 specimens from each of
known to compromise aircraft safety.9 the S1, S2 and S3 CFRP laminates, of which 8 specimens were desig-
Acquiring this knowledge is therefore important to confidently nated tensile specimens, and 8 were designated bending specimens.
design safe fire-resilient aircraft made of CFRP laminates. Furthermore, The eight specimens were chosen as this allowed two specimens at
the loading conditions and thermal environments represent those likely each of the ambient, LE, ME and HE, where one specimen would be
to be experienced due to a fire nearby and adjacent to a leak from a embedded with thermocouples and one without (other than at ambi-
fuel tank during an accidental fire during flight. Hence, experiments are ent room temperature where neither would have thermocouples
performed on aircraft structural-grade CF and a high-performance embedded). A total of three K-type thermocouples were embedded at
epoxy resin (ER) following exposure to a one-sided radiant heating the exposed (x ¼ 1 mm) denoted TC1, middle (x ¼ 2:5 mm) denoted
representative of the critical (critical due to the impact these heating TC2 and unexposed surfaces (x ¼ 5 mm) denoted TC3 at the horizon-
conditions have on the load-bearing mechanical properties of CFRP tal midspan to generate temperature distribution data. Thermocouples
laminates) temperatures based on the four conditions of exposure enu- were embedded into a select few specimens, not all of them, as their
merated above. To clarify, these are (1) ambient (room temperature), (2) presence could reduce the mechanical performance.
LE ¼ T g , (3) ME ¼ T d , and (4) HE ¼ T o .

2.2 | Fibre-to-resin volume ratio


2 | MATERIALS
The fibre-to-resin ratio of each laminate was determined by running
A total of three CFRP laminates were produced for this study. Each three repeat burn-off tests using small 8 mg sample crucibles for each
laminate contained a unique fibre orientation and comprised 8 plies laminate using standard thermogravimetric analysis (TGA) (TGA/DSC
bonded with ER and a hardener (curing agent). The CF was supplied 1, Mettler Toledo®) and following ASTM standards,33 Procedure G.
by Hexcel Composites GmbH, and the ER and hardener were supplied These burn-off tests were run in an air atmosphere at a heating rate
by Easycomposites Ltd, UK, and nominally applied using a 70:30 of 2.5 C/min. The fibre-to-resin ratio has an important effect on the
resin-to-hardener ratio as per the manufacturer's instructions. A nomi- mechanical properties of CFRP laminates. In theory, the higher
nal 50:50 fibre-to-resin ratio was pursued whilst manufacturing the carbon fibre content, the lower the resin content and the higher
the CFRP laminates to provide a composite with good tensile and the strength and stiffness of the composite. Suppose the composite
compressive strength and stiffness properties. All laminates were has a resin content that is too low. In that case, it will result in poor
produced identically using a hand lay-up technique, which involved interlaminar adhesion (due to the lack of space for the matrix to fully
applying a release agent to a glass mould and then stacking the dry surround and bond with the fibres), causing the carbon fibres to bond
fabric plies to the glass mould whilst coating each of the 8 plies with too quickly and reducing the mechanical properties of the composite.
resin layer-by-layer. If the composite has a resin content that is too high, it will cause a
decrease in the strength and stiffness properties of the composite
material, as fibres are the main load-carrying members of the compos-
2.1 | Curing process and specimen preparation ite. Therefore, the resin content of carbon fibre reinforced composites
should be controlled optimally.
After the hand lay-up of each laminate, they were left to cure at
room temperature for 24 h. The average thickness of the laminates
(calculated from five measurements taken from each) was 6.37 3 | E X P E R I M E N T A L P RO G R A M M E
± 0.3 mm. After curing at room temperature for 24 h, specimens
were prepared using a water-cooled diamond wheel saw and dried 3.1 | Characterising the critical temperatures
at 20 C for 12 h in a gravity convection oven. After drying for 12 h,
the specimens were visually inspected for surface defects to check The critical temperatures, Tg, Td and To were determined using
that they were free from external delamination, pinholes, cracks or dynamic mechanical analysis (DMA) and TGA. The Tg was quantified
voids. After the visual inspection, small bonding tabs measuring using the Perkin Elmer® DMA 8000 Dynamic Mechanical Analyser
50 mm  30 mm were carefully attached to each end of the tensile with a built-in displacement sensor and a 500 N load cell. The DMA
specimens using an adhesive (Sikadur 330). Bonding tabs were experiments were carried out in a standard three-point bending orien-
attached to avoid gripping damage from the universal testing tation in which the temperature inside the testing chamber increased
machine (UTM) clamps during the tensile experiments and prevent from 25 to 250 C at a heating rate of 10 C/min allowing the glass
mechanical failure outside the fire-tested gauge region during the transition to be identified. The specimens were small rectangular
post-fire experiments. All specimen's dimensions were identical, specimens measuring 15 mm  10 mm  5mm (L  W  H), weighing
measuring 250 mm  30 mm and 5 mm in thickness. An illustration approximately 8 mg produced from each of the CFRP laminates.
showing the fibre orientations of each CFRP laminate used in this Three repeat runs under identical conditions were performed on each
study is shown in Figure 1. CFRP laminate, and a mean temperature was taken as the Tg. In this
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4 ASPINALL ET AL.

FIGURE 1 An illustration of the fibre orientations of the CFRP laminates used in this study.

study, the temperature at the tangential onset of the increase in the degradation of CFRP laminates. The dimensions of all specimens were
tan δ definition has been used to identify the Tg from the DMA data identical. Specimens were horizontally orientated perpendicular to the
because it defines the beginning of the loss of load-bearing capacity. heater. The distance between the cone heater and the exposed sur-
Therefore it would be undesirable to use the material beyond this face of the specimens was identical for each experiment and fixed at
temperature. 25 mm. The 25 mm spacing distance was chosen because it gives the
The Td and To were identified using a Mettler Toledo TGA/DSC1. best results concerning the mitigation of ‘fire-plume wander’ and ade-
Experiments were carried out in an air atmosphere using a flow rate of quately capturing the combustion products within the confines of the
50 mL/min at a heating rate of 2.5 C/min from 25 to 900 C. The nomi- cone calorimeter exhaust hood.34 During the experiments, each speci-
nal size of the crucibles was 2 mm3 . Specimens were prepared by dril- men's 100 mm  30 mm midspan section was exposed directly to the
ling through each CFRP laminate using a 5 mm tungsten carbide bit, external heat fluxes. The lateral specimen surface, unexposed face
grinding the chippings using a mortar and pestle and placing them into and ends (nearest the bonding tabs) were insulated to minimise heat
ceramic crucibles. Crucible preparation was performed carefully to losses and promote one-dimensional heat transfer. The duration of
ensure that the intended fibre-to-resin ratio of each of the CFRP lami- the heat fluxes was chosen to allow sufficient damage to the speci-
nates was representative of the bulk material since this factor could mens to weaken them to their LE, ME and HE scenarios. The required
affect the data due to the heterogeneity of the CFRP laminates. Dur- level of degradation was known when a thermocouple located at the
ing TGA, three repeat runs under identical conditions were performed unexposed surface at the centre of the midspan section recorded the
on each CFRP laminate to improve the reliability of the data, and a critical temperatures.
mean Td and To were reported. In this study, the Td and To are consid- Initially, the solid-phase temperature distribution was measured
ered the temperatures corresponding to the tangential onset of the for one of each specimen at each heat flux under identical conditions
DTG for the ER (first peak) and the CF (third peak). These two defini- (i.e. room temperature, airflow) to determine the time taken for LE,
tions have been chosen because they represent conservative values. ME and HE to reach the unexposed surface and obtain temperature
profiles. After the temperature distribution data had been generated,
the cone heater subjected the remaining specimens containing no
3.2 | Characterising the thermal exposure thermocouples to the required level of damage corresponding to LE,
ME and HE. After the cone experiments, those specimens containing
Thermal exposure of the specimens was performed using a cone calo- thermocouples were carefully trimmed to remove the thermocouples
rimeter apparatus (Fire Testing Technology, UK) utilising a 3, 15 and before being mechanically tested. The thermocouples were trimmed
30 kW=m2 heat fluxes. These heat fluxes correspond to the LE, ME to avoid getting caught in the UTM cross-head or pose a tripping
and HE scenarios associated with the known physico-chemical hazard.
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ASPINALL ET AL. 5

3.3 | Post-fire experiments identical conditions (i.e. room temperature, airflow). Images were captured
during each experiment using a single ultra-high definitions (UHD) camera
Post-fire tensile and bending mechanical properties were obtained using (Canon® EOS 5D Mark IV) capable of recording high-quality videography
an industry-standard UTM (Instron 3380 series) using a loading rate and capturing images simultaneously. Images were captured at 2-s inter-
(cross-head speed) of 2 mm/min. Each experiment was carried out under vals. The camera was placed at an offset distance measuring 450 mm

TABLE 1 Three-point bending failure identification codes based on ASTM D7264.36

First character Code Second character Code Third character Code


Tension T At loading nose A Top T
Compression C Between loading nose B Bottom B
Buckling B At support nose S Left L
Interlaminar Shear S Between loading and support nose L Right R
Multi-mode M(x,y,z) Unknown U Middle M
Other O Various V
Unknown U

T A B L E 2 Tensile failure
First character Code Second character Code Third character Code
identification codes based on ASTM
D3039.35 Angled A Inside grip/tab I Bottom B
Edge delamination D At grip/tab A Top T
Grip/tab G <1 W from grip/tab W Left L
Lateral L Gage G Right R
Multi-mode M(x,y,z) Multiple areas M Middle M
Long splitting S Various V Various V
Explosive X Unknown U Unknown U
Other O

F I G U R E 2 Results from the


DMA and TGA showing the glass
transition (Tg), pyrolysis (Td) and
oxidation (To) temperatures.
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6 ASPINALL ET AL.

from the lateral surface of the specimen and used to capture the midspan specimens were placed using a customised double overhanging three-
behaviour of the material at the location directly opposite the loading point bending specimen holder and loading nose. This customised
grips/nose. The lighting used during the post-fire experiments was pro- bending apparatus contained steel roller-type supports with a span
vided by a 200-W LED light (Godox® SL-200W) at 2000 mm from the distance measuring 200 mm. This span distance remained the same
specimen's lateral surface. for each of the three-point bending experiments. To prevent speci-
men slippage whilst in the supports, the length of the specimens was
equal to the span length plus 50 mm overhangs at either end. The
3.3.1 | Tensile experiments load and corresponding vertical displacement were recorded continu-
ously by the UTM. The experiments were stopped when mechanical
In total, 24 tensile experiments were carried out and loaded in the longi- failure of the specimens, indicated by a drop in load and runaway
tudinal x-direction using wedge action grips attached to bonding tabs. displacement, was recorded.
The undamaged specimens were initially tested until failure in orders S1,
S2 and then S3. This procedure was followed by the fire-damaged LE,
ME and HE CFRP specimens in orders S1, S2 and then S3. The experi- 3.3.3 | Mechanical failure modes
ments were stopped when mechanical failure of the specimens, indicated
by a drop in load and a runaway displacement, was recorded. Failure modes and mechanisms were studied through macroscopic
and microscopic observations using a high-resolution flatbed
scanner (Epson® V800) and scanning electron microscopy (SEM)
3.3.2 | Three-point bending experiments (Jeol® JSM-6010LA), respectively. SEM was carried out to study
the topography of the CFRP laminates and acquire imagery of the
A total of 24 bending specimens were loaded on their unexposed specimens before and after the experiments in microscopic detail.
(undamaged) surface using a constant vertical compressive load. All At the same time, the high-resolution scanner provided detailed

FIGURE 3 Temperature distribution data for the S1 CFRP laminate.


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ASPINALL ET AL. 7

FIGURE 4 Temperature distribution data for the S2 CFRP laminate.

HD imagery of the fire-damaged areas observable with the naked one another, which the S1 CFRP laminate does not have as it is a
eye. Failure modes were characterised based on the failure codes unidirectional CFRP.
described by ASTM for tension35 and three-point bending.36 This
classification used a three-part notation to identify each failure
characteristic. Tables 1 and 2 represent the notations used for ten- 4.2 | DMA and TGA data
sion and three-point bending, respectively.
Figure 2 shows the DMA and TGA results. Analysis of the DMA data
shows that the Tg of the CFRP laminates is 70 C. On the other hand,
4 | RESULTS AND DISCUSSION the analysis of the TGA data shows that the Td and To of the CFRP
laminates are 230 and 630 C, respectively. Because the method of
4.1 | Fibre-to-resin volume ratio obtaining these critical temperatures is performed in a kinetically
dominated regime (controlled by the rate of the chemical reaction),
The thermogravimetry results revealed fibre-to-resin volume these temperatures do not depend on the fibre orientation. Hence
ratios of 52%, 55% and 57% for the S1, S2 and S3 CFRP laminates, these temperatures are the same for all CFRP laminates.
respectively. The minor variation in the fibre-to-resin ratio
between the CFRP laminates can be attributed to the fact that S2
and S3 CFRP laminates required more resin to completely embed 4.3 | Temperature distribution data
the fibres in the resin, reducing the possibility of matrix voids
between ply layers and resulting in a smooth surface finish. The Figures 3–5 show the temperature distribution measurements for the
S2 and S3 required more resin because they have carbon fibres S1, S2 and S3 CFRP laminates, respectively. In addition, images of the
oriented in multiple directions and, therefore, small lumps caused frontal and lateral surfaces following the experiments are provided in
by the warp and weft yarns of carbon fibre passing over and under Figures 6–8 for the S1, S2 and S3 CFRP laminates, respectively.
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8 ASPINALL ET AL.

4.3.1 | S1 CFRP laminate x ¼ 2:5 mm and x ¼ 5 mm depths below the heated surface in 101, 185
and 305 s, respectively. On the other hand, the Td and To are not
Figure 3 shows the temperature distribution data for the S1 CFRP recorded. These temperature measurements show that the through-
laminate at LE, ME and HE. At LE, the Tg is recorded at x ¼ 1 mm, thickness temperature gradients are small and evenly distributed because
the temperatures are not high enough to pyrolyse or oxidise the speci-
men. Because pyrolysis nor oxidation occurs, char formation, delamina-
tion, voids or cracks in the ER do not occur, meaning there is no
reduction in the heat transfer rate or associated distortion in the energy
balance across the specimen. Hence the S1 CFRP laminate after LE is
dominated by the effects of the glass transition only.
After ME, the Tg is recorded at x ¼ 1 mm, x ¼ 2:5 mm and
x ¼ 5 mm, in 27, 109 and 135 s, respectively. The data also shows that
the Td was recorded at x ¼ 1 mm, x ¼ 2:5 mm and x ¼ 5 mm in 64, 391
and 549 s, respectively. On the other hand, the To is not recorded;
therefore, after ME, the S1 CFRP laminate is first dominated by the
effects of the glass transition, followed by the pyrolysis of the
ER. These temperature measurements also show a large temperature
gradient forming between the exposed and middle of the specimen.
This behaviour is due to char formation, which prevents migrating and
pyrolysing gas species flow, reducing heat transfer and pyrolysis rate.
After HE, the data shows that the Tg is recorded at x ¼ 1 mm,
x ¼ 2:5 mm and x ¼ 5 mm in 22, 34 and 105 s, respectively. It also
shows that the Td was recorded at x ¼ 1 mm, x ¼ 2:5 mm and x ¼ 5 mm
FIGURE 5 Temperature distribution data for the S3 CFRP laminate. in 51, 102 and 517 s, respectively. The To, on the other hand, was

FIGURE 6 Post-fire high-resolution images of the S1 CFRP laminate showing damage after different exposure intensities.
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ASPINALL ET AL. 9

F I G U R E 7 Post-fire high-resolution
images of the S2 CFRP laminate showing
damage after different exposure
intensities.

recorded at x ¼ 1 mm in 218 s. These measurements show that the contrast, the lateral images show that the middle and unexposed
temperatures are not evenly distributed in the specimen and vary spa- surfaces appear undamaged. After HE, the images show delamination
tially and temporally, resulting in a large temperature gradient. This and cracking from the exposed surface through to the mid-thickness
behaviour is because the ER has quickly heated, raising its tempera- of the specimen. They can be most likely attributed to a build-up of
ture to produce pyrolysis products containing gaseous fuel that interlaminar internal pressure due to pyrolysis gases. The pressure
ignites. When ignition occurs, a char layer forms, impacting the heat exerted due to this inter-ply pressure appears to have forced the plies
and mass transport resulting in additional heat release. Ignition is indi- nearest the exposed surface apart from the bulk specimen, causing
cated in the data by a steep temperature increase over a very short damage around this area.
time increment. The data also shows that the temperature at x ¼ 1 mm
is sufficient to oxidise the char and fibre reinforcement, causing the
regression of the char layer resulting in the exposure of the CF, which 4.3.2 | S2 CFRP laminate
then oxidises. The regression of the char is also indicated in the TC1
temperature data at HE, which appears to fluctuate when reaching Figure 4 shows the temperature distribution data for the S2 CFRP
the To. This behaviour is due to surface regression and char oxidation laminate. At LE, the temperature data shows that the Tg is measured
resulting in TC1 no longer being embedded in the specimen and at x ¼ 1 mm, x ¼ 2:5 mm and x ¼ 5 mm below the heated surface in
becoming exposed to the heat source resulting in what looks like gas 239, 286 and 442 s, respectively, whereas the Td and To were not
phase measurements. When this occurs, the recorded temperature recorded. This behaviour shows that the glass transition is the only
fluctuates, becomes unstable and can no longer be considered reli- physico-chemical process occurring in the S1 CFRP specimen at LE.
able. This behaviour is reflected in the data for TC1 at x ¼ 1 mm from At ME, the Tg is measured at x ¼ 1 mm, x ¼ 2:5 mm and x ¼ 5 mm
approximately 450 s until the end of the experiment. Temperatures in 37, 48 and 201 s, respectively, whilst the Td is recorded at x ¼ 1 mm
recorded at x ¼ 2:5 mm and x ¼ 5 mm, on the other hand, are below and x ¼ 2:5 mm at 252 and 446 s, respectively. The To, on the other
those required for char and fibre oxidation, resulting in those fibres hand, is not recorded. This behaviour shows that glass transition
not being damaged. occurs throughout the depth, and pyrolysis occurs and the exposed
Figure 6 displays post-fire images of the frontal and lateral sur- and middle.
faces of the S1 CFRP specimen. After LE, damage appears very lim- During HE, the specimens ignited, causing additional heat release
ited. After ME, the frontal image shows that the ER has pyrolysed, and a rapid temperature increase. The temperature data reflects this
producing a small char layer and cracks in the residual resin. In as the Tg is measured at x ¼ 1 mm, x ¼ 2:5 mm and x ¼ 5 mm in 20, 92
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10 ASPINALL ET AL.

FIGURE 8 Post-fire high-resolution images of the S3 CFRP laminate showing damage after different exposure intensities.

and 128 s, respectively. The Td is measured at x ¼ 1 mm, x ¼ 2:5 mm 4.3.3 | S3 CFRP laminate
and x ¼ 5 mm in 56, 224 and 367 s, respectively, whereas the To, is
measured at x ¼ 1 mm and x ¼ 2:5 mm in 651 and 742 s respectively Figure 5 presents the temperature distribution data for the S3 CFRP
but not at x ¼ 5 mm. This behaviour shows that at HE, the ER has pyr- laminate. At LE, the data shows that the Tg is measured at x ¼ 1 mm,
olysed throughout the specimen whilst also experiencing char and x ¼ 2:5 mm and x ¼ 5 mm in 98, 141 and 302 s, respectively. Glass
fibre oxidation damage at x ¼ 1 mm and x ¼ 2:5 mm. This oxidation is transition is the only physico-chemical process occurring at LE. The
likely to have damaged the fibres in these locations and resulted in data also shows that the temperatures at x ¼ 2:5 mm and x ¼ 5 mm
the thermocouples being no longer embedded in the specimen, as begin to converge; this is most likely due to variability in the thermo-
shown by the converging temperature in TC1 and TC2. couple placements and is unlikely to result from a char layer forming
Figure 7 shows post-fire high-resolution frontal and lateral sur- and slowing the heat transfer rate.
face images of the S2 CFRP laminate. After LE, some discolouration At ME, the temperature measurements show that the Tg is mea-
(yellowing) about the specimen midspan can be observed; otherwise, sured at x ¼ 1 mm, x ¼ 2:5 mm and x ¼ 5 mm in 36, 43 and 270 s,
physical damage appears limited. After ME, the ER has some disco- respectively, the Td is measured at x ¼ 1 mm and x ¼ 2:5 mm in 302
louration (yellowing) due to the pyrolysis of the ER. The lateral view and 450 s respectively but not at x ¼ 5 mm, whereas the To is not
also shows delamination and the formation of large voids due to a recorded. This temperature differential shows that half of the
build-up of interlaminar internal pressure and general deformation. through-thickness remains below the Td but above the Tg. This behav-
This deformation of the S2 CFRP specimens appeared to be the most iour shows that the specimen is weaker at the exposed and middle
visible at the centre of the exposed surface around the midspan loca- surfaces than towards the unexposed surface.
tion, where the heat flux would have been the highest due to the At HE, the temperature measurements show that the Tg is mea-
non-uniformity of the cone heater-emitting surface. After HE, the sured at x ¼ 1 mm, x ¼ 2:5 mm and x ¼ 5 mm in 22, 37 and 142 s,
pyrolysis of the ER appears complete at the exposed and midspan respectively. On the other hand, the Td is measured at x ¼ 1 mm,
locations, which has resulted in delamination of the plies closest to x ¼ 2:5 mm and x ¼ 5 mm in 59, 103 and 731 s, respectively. In con-
the exposed surface. trast, the To is not recorded.
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ASPINALL ET AL. 11

TABLE 3 Results by each specimen.

Tensile Failure loada (kN) Ultimate tensile strength (MPa) Failure modeb (–) Number of specimens (–)
Specimen designation
S1-A-T 85.5 792.9 LAT 2
S1-LE-T 72.2 456.2 LGV 2
S1-ME-T 28.9 186.9 DGV 2
S1-HE-T 5.4 44.2 XGV 2
S2-A-T 95.5 580.7 LGM 2
S2-LE-T 64.9 507.4 LGM 2
S2-ME-T 25.5 181.8 DGM 2
S2-HE-T 2.0 28.5 XGM 2
S3-A-T 89.9 587.9 LGM 2
S3-LE-T 71.7 410.8 AGM 2
S3-ME-T 31.8 125.8 DGM 2
S3-HE-T 1.2 14.7 XGM 2
Three-point bending Failure loada (kN) Ultimate bending strength (MPa) Failure modec Number of specimens
S1-A-B 2.7 164.3 TAB 2
S1-LE-B 1.6 127.2 CBV 2
S1-ME-B 1.1 71.5 M(T,C,B)LV 2
S1-HE-B 0.66 39.8 M(C,B,S)LV 2
S2-A-B 1.9 117.7 TAB 2
S2-LE-B 1.3 99.5 CBV 2
S2-ME-B 0.9 59.4 M(T,C,B)LV 2
S2-HE-B 0.68 41.7 M(C,B,S)LV 2
S3-A-B 2.2 134.5 TAB 2
S3-LE-B 2.1 127.4 CBV 2
S3-ME-B 1.1 70.3 M(T,C,B)LV 2
S3-HE-B 0.69 41.8 M(C,B,S)LV 2

Note: A, LE, ME, and HE denotes ambient, low, medium and high exposure, whereas T and B correspond to the type of test, T being tensile and B
representing three-point bending.
a
Average value taken from two repeat experiments.
b
Based on ASTM D3039/D3039M.
c
Based on ASTM D7264/D7264M.

Overall the data shows that the temperatures after HE, irrespec- After ME, discolouration (yellowing) and char formation can be
tive of through-thickness location, are generally lower than those in observed between the exposed surface and mid-thickness. In addition,
the S1 and S2 CFRP specimens. Lower temperatures result from the the char appears to have tiny bubbles propagating from its surface.
cross-plied quasi-isotropic nature of the carbon reinforcement used These bubbles are produced by an accumulation of migrating pyrolysis
for the S3 CFRP specimen, which provides more stability, is less likely gases from the unexposed to the exposed surface that eventually
to delaminate and has a lower resin fraction. Less resin means there is erupts closest to the heat source and causes swelling. Bubbles that
less combustible fraction able to exhibit cracks and voids or pyrolyse, appear visible but remain trapped below the surface are due to the
the latter of those issues resulting in the formation of pyrolysis gases residue cooling quickly and hardening, causing the gases to remain
that are known to increase inter-ply pressure, which is one of the encircled and unable to propagate.
main contributors leading to interfacial delamination of CFRP lami- After HE, the ER at the exposed and middle surface has experi-
nates exposed to fire.9 enced pyrolysis and further discolouration (yellowing) (increasing
Figure 8 presents post-fire images of frontal and lateral sur- degrees of discolouration are observed with increasing heat flux,
faces of the S3 CFRP specimens. After LE, physical damage appears which translates to higher degrees of thermal decomposition across
in the form of small bubbles in the resin surface around the mid- the depth of the specimen). This pyrolysis has resulted in cracks and
span location and localised delamination of the surface ply close to delamination forming at the exposed surface and localised char forma-
the heat source. tion at the unexposed surface.
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12 ASPINALL ET AL.

FIGURE 9 Results from the post-fire tensile experiments.

4.3.4 | Summary TC3. The result of this damage means these specimens will likely have
reduced failure modes, bending strength and different failure modes
To summarise the results from this section, the data shows that, gen- than the other specimens.
erally, the highest temperatures are recorded in the S1 CFRP speci-
mens and the lowest in the S3 CFRP specimens. Higher temperatures
result in further damage to the CFRP laminate resulting in them 4.4 | Post-fire experiments
becoming mechanically weaker. However, the data in this section also
shows that when a CFRP laminate is exposed to a fire, not all the The data relating to the post-fire experiments using the UTM appara-
material can be considered damaged but rather a series of sections, tus is shown in Table 3. The results from the tensile experiments are
each containing respective residual mechanical properties and perfor- presented in Figures 9 and 10 whilst the results from the three-point
mance levels. For example, the unexposed surface may be considered bending experiments are presented in Figures 11 and 12.
undamaged, whereas the sections that have experienced glass transi-
tion but then rehardened may have resulted in further curing, possibly
improving their mechanical properties. In contrast, those sections that 4.4.1 | Tensile experiments
have pyrolysed but not experienced oxidation may still be able to sup-
port applications requiring tensile strength. On the other hand, those Figures 9 and 13 show the tensile load–displacement and tensile
sections that have experienced oxidation temperatures may have lost stress–strain relationship for each CFRP laminate, whilst Figure 10
a portion of the load-carrying ability. shows the ultimate tensile strength and tensile failure load as a func-
Furthermore, as the temperature recorded at TC3 has also tion of temperature for each CFRP laminate. The data in Figure 9
exceeded the Td in Figure 3 at 12 and 40 kW=m2 and Figures 4 and 5 shows that all CFRP specimens exhibit linear behaviour until they
at 40 kW=m2 , the validity of the testing procedure will be impacted as reach peak load and fail, irrespective of fibre orientation. The S1 spec-
damage will have occurred in the form of pyrolysis damage to the imens reach peak load over the smallest displacement, whereas the S3
epoxy resin, which will have weakened these specimens to a greater specimen reaches peak load over the largest displacement. The cause
degree than the those that have not experienced pyrolysis damage at of this behaviour is that all the fibres are orientated parallel to the load
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13

F I G U R E 1 1 Results from the


F I G U R E 1 0 Ultimate tensile

post-fire three-point bending


strength and ultimate tensile
failure load data.
ASPINALL ET AL.

experiments.
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14 ASPINALL ET AL.

FIGURE 12 Ultimate bending strength and ultimate bending failure load data.

in the S1 CFRP specimens, whereas, in the S2 and S3 CFRP speci- and displacement shows that the ER plays an important fundamental
mens, they are not. Because CF is stiff and does not yield under stress role in assisting the CF to resist failure by providing support through
when undamaged, the fibres and resin retain a good interfacial bond the redistribution of the stresses. Therefore, if the ER pyrolyses, it
that provides optimal load-bearing support meaning they will fracture cannot support the fibre to retain the load.
rather than deform. After HE, the specimen's load–displacement relationship
After LE, the effect of the Tg on the specimens has increased the behaviour demonstrates more displacement before failure and very
variability of the maximum displacement and resulted in lower peak low peak loads relative to the undamaged specimens. This behav-
failure load values. However, all CFRP specimens still exhibit linear iour is due degradation of the CF. It is why the largest decrease in
behaviour. The cause of the variability, however, can be attributed to load-carrying capacity is observed after HE (due to oxidation and
the effects that the Tg has on the specimens, which causes a tempo- weakening of the fibre reinforcement) and not after LE or ME,
rary loss of interfacial bond between the fibre and resin as the speci- where the CF remain undamaged.
men is heated. Although temporary, this loss of interfacial bond allows On the other hand, Figure 10 shows that all the specimens, irre-
the fibres to slip relative to one another, causing them to move out of spective of fibre orientation, show a small decrease in tensile strength
optimal alignment with the load direction. When the fibres slip rela- and failure load between the undamaged specimens and LE. However,
tive to one another, this causes them to lose performance resulting in this increases between LE and ME and between the ME and HE speci-
less consistent behaviour and a reduction in load-bearing capacity. mens. The data also shows that, on average, the S2 CFRP laminate
After ME, the load, displacement and data variability all decrease has the lowest ultimate tensile strength, whereas the S1 CFRP lami-
compared to the undamaged and LE specimens. This behaviour is due nate has the highest ultimate tensile strength.
to the pyrolysis of the ER, which has resulted in these specimens
retaining less than 50% and 34% of their undamaged peak load and
displacement, respectively. The reason for the reduction in variability, 4.4.2 | Bending experiments
however, is unknown. Furthermore, although the temperatures
recorded in the specimens exposed to ME were well below the To, Figures 11 and 14 show the load–displacement and stress–strain rela-
meaning the fact that such a large reduction is observed in the load tionship for each CFRP laminate, whilst Figure 12 shows the ultimate
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15

bending stress–strain curves for


F I G U R E 1 3 Tensile stress–

F I G U R E 1 4 Three-point
strain curves for each CFRP

each CFRP laminate.


ASPINALL ET AL.

laminate.
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16 ASPINALL ET AL.

FIGURE 15 Photographs showing the progressive tensile failure of the S2 CFRP specimens at ambient, LE, ME and HE.

F I G U R E 1 6 Photographs show the tensile failure of the different CFRP specimens at different thermal exposures. Images (A) and (B) show
the S1 CFRP laminate after LE and HE, respectively; images (B) and (C) show the S2 CFRP laminate after LE and HE, respectively, whereas images
(E) and (F) show the S3 CFRP laminate at the LE and HE, respectively.

bending strength and ultimate bending failure load as a function of and S3 CFRP specimens whilst also displaying a larger yield strength
temperature for each CFRP laminate. based on the stress–strain relationship in Figure 14. In addition, the
The data in Figure 11 shows that the undamaged specimens S1 CFRP specimens have a larger initial elastic linear loading response
exhibit initial linear elastic behaviour up until peak load before failing than the S2 and S3 CFRP specimens because all the fibres run parallel
gradually over a large displacement. The data also shows that the S1 to the loading direction in the S1 CFRP laminate, whereas in the S2
specimen has a larger failure load and bending strength than the S2 and S3, they do not.
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ASPINALL ET AL. 17

FIGURE 17 General tension failure mechanisms for the CFRP specimens.

After LE, the S1 specimens exhibit similar behaviour to the unda- a given stress, the overall load-carrying capacity decreases but redis-
maged S1 specimens; however, the S2 and S3 specimens show tributes across the remaining plies (or fibre tows), causing the mate-
completely different behaviour than the undamaged S2 and S3 speci- rials load-bearing capacity to either sustain itself or increase, albeit
mens. The S2 and S3 specimens' behaviour after LE can be attributed for a short duration. Because of this unique behaviour, CFRP lami-
to the fact that these specimens have experienced glass transition, nates can continue to support an applied load (even with some loss
resulting in a loss of interfacial bond strength (although temporary) in strength) after the ER has partially pyrolysed due to the retained
and physical weakening of the ER. This process can result in unpre- strength of the load-bearing CF.
dictable behaviour and a loss of interfacial bond after the resin re- The HE specimens are also characterised by irregular fluctuations
hardens because the fibres have been allowed to move. This results in due to the fracture and pull out of the individual plies from what
the fibres being positioned in a sub-optimal direction to carry the load remains of the char on the exposed surface. This behaviour is because,
and adequately prevent failure. after HE, oxidation has attacked the centre of the specimens, meaning
After ME, the specimen's load–displacement and stress–strain when bending occurs, the strength of the specimen is governed solely
relationship appear very different to the undamaged and LE speci- by damaged CF above the neutral axis at the convex surface. Therefore,
mens. They are marked by significant displacements, lower peak like the specimen's behaviour in the tensile experiments, if a ply or fibre
loads and smaller yield strengths. The data for these specimens also tow fails in isolation, the overall load-carrying capacity reduces but
show small and irregular fluctuations in the loading response. These redistributes across the remaining plies and different layers, causing it
fluctuations are due to the individual ply layers, whose strength and to continue to maintain partial resistance.
stiffness properties are independent variables failing in isolation On the other hand, Figure 12 shows increased variability between
rather than more broadly. Therefore, in principle, if a single-ply layer, the specimens and generally shows that the S1 CFRP laminate has the
or even a single fibre tow (a bundle of fibres), fail in isolation due to highest ultimate bending strength and failure load. In contrast, the S2
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18 ASPINALL ET AL.

F I G U R E 1 8 Typical failure modes due to three-point bending, showing (A) delamination, (B) more delamination, (C) debonding of the
inter-ply layer, (D) matrix and fibre shearing and finally (E) micro-buckling.

and S3 CFRP specimens present similar behaviour to one another, approach is affected by the fact that the damaged areas are no
albeit with lower ultimate bending strengths and failure loads than the longer in composite action.
S1 CFRP specimens.
Another factor influencing the behaviour of the bending speci-
mens behaviour during the experiments is which surface (damaged 4.5 | Post-fire tensile failure modes and
or undamaged) is placed under tension and which one is in com- mechanisms
pression. This factor is important as, unlike in tensile specimens, in
bending, one surface of the material will act in tension, and the This section presents images detailing the tensile failure modes and
other surface will act in compression. The heating effect on either mechanisms. Failure of the tensile specimens at ambient (undamaged)
of these faces will likely result in drastically different outcomes. For and LE occurred as a transverse brittle fracture. After ME and HE,
example, heating of the tension surface will mean that the CF oxi- on the other hand, failure was attributed to an explosive failure.
dation can dominate the failure and can take a long time compared Figure 15 shows a clear chronological series of images showing the
to heating onto the compression surface, which will be dominated propensity for the specimen to fail explosively as heat damage
by the loss of the mechanical performance of the epoxy resin. This increases. On the other hand, Figure 16 shows photographs of the
behaviour is because the carbon fibres perform poorly in compres- tensile failure modes of all the CFRP specimens containing different
sion and become more susceptible to micro-buckling as fibre inter- fibre orientations.
actions are reduced due to softening of the polymer matrix. This Figure 17 illustrates the general tension failure mechanisms for
behaviour is due to the carbon fibre reinforcement primarily the CFRP specimens at ambient, LE, ME and HE leading up to failure.
controlling the material's response in tension and the epoxy resin In addition, an analysis of this kind was performed to provide insight
primarily controlling the material's response during compression. into possible damage that could have contributed to the failure of the
Therefore, heating the tensile surface exposes the fibre reinforce- specimens. During the tensile experiments, it was observed that brit-
ment to maximum thermal and mechanical stress. For this reason tle (at ambient (undamaged) and LE) and explosive failure (after ME
alone, the data obtained for the bending specimens shown are only and HE) were the two most common failure modes for the specimens;
representative of such scenarios where the fibre reinforcement however, the mechanical failure mechanisms that contributed to
dominates the exposed surface whilst the load is applied on the failure were different depending on the level of fire damage and fibre
unexposed surface. These data show that the validity of the testing orientation of those specimens.
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ASPINALL ET AL. 19

FIGURE 19 General three-point bending failure mechanisms for the CFRP specimens.

The tensile failure mechanisms for the S1 CFRP laminate under ambient (undamaged) conditions and LE, the S2 and S3 CFRP specimens
ambient (undamaged) conditions were due to a rapid build-up of loca- exhibited similar mechanical failure mechanisms to the S1 CFRP lami-
lised strain that occurred disproportionately over a small region at the nate. This behaviour can be characterised by a progressive brittle failure
midpoint leading to all the fibres in this zone fracturing on the same [0 ] caused by stress concentrations and a gradual release of pockets of
plane. This small transverse area was when the nominal stress against stored energy. The stored energy culminates in localised tow failure due
nominal strain was maximum. After LE, the failure mechanisms occurred to stress propagation across the fibre-matrix interface, which results in
as a brittle failure caused by stress concentrations and the gradual near-neighbour tow failure. After ME and HE, on the other hand, the fail-
release of energy. This gradual release of energy resulted in an audible ure mechanisms are different from those experienced by the S1 CFRP
loud ‘pinging’ sound as a fibre tow reached its maximum stress and failed laminate. For these specimens, failure can be attributed to transverse
in isolation. When a fibre tow reaches its maximum stress, the stress and splitting matrix cracking caused by a large amount of stored energy
released is transferred to neighbouring fibres, and consequently, the released simultaneously; this release of stored energy culminated in
stress in the fibres nearest to the break magnifies. Transferring the stress explosive delamination damage and failure.
overload begins sequential overloading of the other fibre tows, albeit
with a shorter duration between each ‘ping’. When the stress concentra-
tions increased, the ER responded by cracking. After ME, the S1 CFRP 4.6 | Post-fire bending failure modes and
laminate experiences fibre pullout and debonding of the ply layers due to mechanisms
the pyrolysis of the ER. After HE, further delamination damage caused
by the internal pressure build-up was observed in addition to the mecha- This section discusses the bending failure modes and mechanisms.
nisms observed after ME. Furthermore, at HE, the CF was also damaged Typical failure modes of the CFRP specimens during bending are
due to surface oxidation, with close coupling observed between the shown in Figure 18 where the images demonstrate (1) delamination,
completely pyrolysed areas of the ER and the oxidation of the fibres. At (2) more delamination, (3) debonding of the inter-ply layer, (4) matrix
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20 ASPINALL ET AL.

FIGURE 20 Photographs showing the progressive three-point bending failure of the S2 CFRP specimens at ambient, LE, ME and HE.

and fibre shearing and finally (5) micro-buckling. The failure modes of surface all increasing. These failure mechanisms caused delamination
the S1 CFRP at ambient (undamaged) temperature and LE, failure of the damage to propagate down the entire middle of the specimen, causing a
S1 CFRP laminate was attributed to a combination of brittle tensile failure complete fracture along the direction of the fibre, effectively splitting the
on the convex tensile surface opposite to the loading nose and a small specimen into two separate parts. Finally, after HE, the failure was attrib-
interlaminar shear failure on the concave compression surface around the uted to fibre pullout on the convex tension surface and kinking, a form
area of the loading nose. Thus, the mechanisms leading to the failure of of micro-buckling, on the concave compression surface.
the S1 specimen were due to localised crushing and interlaminar shear The S2 and S3 CFRP specimens presented very similar behaviour;
damage above the area of the loading nose. An illustration showing the therefore, they will be discussed in unity. At ambient (undamaged)
general bending failure mechanisms for the CFRP specimens at ambient, conditions, the specimens exhibit brittle behaviour characterised by
LE, ME and HE leading up to failure has been provided in Figure 19. tensile failure of the fibre reinforcement on the convex tensile surface
After ME, failure was predominately concentrated around the load- and interlaminar shearing due to the formation of cracks below the
ing nose on the concave compression surface. The mechanisms that con- loading nose on the concave compression surface. After LE, the
tributed to this were fibre breaking, interfacial debonding on the convex behaviour is very similar to those of the undamaged specimens; how-
tension surface and matrix cracking around the loading nose area due to ever, after ME, the ER had pyrolysed, failing due to the fibres ruptur-
the pyrolysis of the ER and the limited mechanical properties of the char. ing and separating from the bulk material in the longitudinal direction.
As the load increases, the specimen's behaviour becomes more complex, This behaviour reduces the longitudinal resistance of the specimen as
with fibre breaking, pullout and delamination on the convex tension the longitudinal tension and compression stresses distribute over the
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ASPINALL ET AL. 21

FIGURE 21 Post-fire SEM images detailing the damage to the S1 CFRP laminate after (A) LE, (B) ME and (C) HE.

FIGURE 22 Post-fire SEM images detailing the damage to the S2 CFRP laminate after (A) LE, (B) ME and (C) HE.

remaining fibres over the depth of the cross-section when they sepa- isolated CF. After ME (Figure 21B), the ER has pyrolysed, and surface
rate. As a result, the CF cannot support the load when the longitudinal damage is much more evident in the image than after LE. Surface dam-
resistance is low. Finally, after HE, the specimens experience delami- age increases because the pyrolysis of the ER has caused the individual
nation, splitting the specimen from the midspan location down one fibre to break free from their respective ply layers due to low interfa-
leading edge. Images detailing this degradation are shown in cial bond strength. After HE, pyrolysis reactions of the ER appear com-
Figure 20, where a clear chronological series of images detailing the plete as a char layer has formed and begun to regress in places due to
three-point failure modes of the S2 CFRP laminate at ambient, LE, ME surface oxidation. This behaviour has resulted in the exposure of CF to
and HE. oxygen in the air causing them to weaken. A damaged section of a sin-
gle filament due to oxidation is shown in Figure 21C.

4.7 | Microstructural analysis


4.7.2 | S2 SEM
In order to obtain further information about CFRP laminates post-fire
response, the specimens have been examined by SEM. Figures 21, 22 Figure 22A–C shows SEM images detailing the progressive damage to
and 23 show the SEM images for the S1, S2 and S3 CFRP specimens, the S2 CFRP specimens after LE, ME and HE, respectively. After LE,
respectively. The black squares in the images outline and indicate the the ER shows signs of superficial damage with surface bubbling and
specimen's damaged area. flaking. After ME, the ER has pyrolysed, causing char to form in places.
In addition, the negligible mechanical properties of the char have
resulted in fibres breaking free from their original alignment. Finally,
4.7.1 | S1 SEM after HE, similar behaviour to the S1 CFRP laminate has occurred,
and pyrolysis of the ER is complete, exposing the CF to oxygen and
Figure 21 shows SEM images detailing the progressive damage to the leading to complex oxidation reactions that attack and weaken the
S1 CFRP specimens after LE, ME and HE. At the LE (Figure 21A), the surface of the fibre reinforcement. This surface damage is shown in
ER appears relatively undamaged other than a few surface flaws due Figure 22C, where a large, damaged section of a single carbon-fibre
to a loss of temporary interfacial bond and repositioning of some filament is shown.
10991018, 0, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/fam.3163 by University Of Auckland, Wiley Online Library on [06/12/2023]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
22 ASPINALL ET AL.

FIGURE 23 Post-fire SEM images detailing the damage to the S3 CFRP laminate after (A) LE, (B) ME and (C) HE.

4.7.3 | S3 SEM specimens, respectively, relative to the undamaged CFRP speci-


mens. This behaviour shows that the S1 CFRP specimens retain
Figure 23A–C shows the progressive damage to the S3 CFRP speci- the most post-fire bending properties, whereas the S2 CFRP speci-
mens after LE, ME and HE, respectively. After LE, the ER displays mens retain the least. Furthermore, this shows that during bending,
signs of pyrolysis damage and some char formation around the areas the pyrolysis of the ER has a large impact on the residual proper-
of pyrolysis damage. After ME, the images show the widespread dam- ties. This behaviour is because the ER supports and redistributes
age due to the pyrolysis of the ER and char formation that appears to the stresses across the CF. Hence, when the matrix pyrolyses
have spread proportionately across the specimen. Finally, after HE, after ME, a loss of stiffness and interfacial bond strength occurs,
the pyrolysis of the ER largely occurred, exposing the CF to oxygen resulting in delamination and a general loss of interfacial bond
and leading to the thermal decomposition of the CF via heteroge- between the residual char that encapsulates the fibres and the
neous oxidation reactions. This oxidation damage is shown in the form fibres themselves.
of crenulations in Figure 23C. 4. The results also show that after HE, the post-fire tensile properties
decrease 93%, 97% and 98% for the S1, S2 and S3 CFRP speci-
mens, respectively, relative to the undamaged CFRP specimens.
5 | C O N CL U S I O N S This behaviour shows that the S1 CFRP specimens retain the most
post-fire bending properties, whereas the S3 CFRP specimens
This study has investigated the effect of fibre orientation and thermal retain the least highlighting the influence of HE oxidation on
exposure on the post-fire mechanical behaviour of CFRP laminates. In the CF.
addition, DMA and TGA have been carried out to quantify the CFRP 5. The data has also shown that when failure of the undamaged and
laminates Tg, Td and To, whilst microstructural (SEM) and macrostruc- LE tensile specimens occurs, they exhibit brittle behaviour. After
tural (scanning techniques) analyses have also been performed to ME and HE, the failure can be characterised as explosive and
investigate failure modes and mechanisms of the CFRP specimens. sudden, irrespective of the fibre orientation. However, a mixture
Regarding the obtained results, the following conclusions can of failure modes was observed in bending depending on the fibre
be made: orientation and exposure intensity.
6. The data from this study also shows that the type of failure modes
1. The results have shown that CFRP's post-fire tensile and three- in bending and tensile experiments is sensitive to the in-depth
point bending behaviour and failure modes are sensitive to fibre temperature gradient. These in-depth temperatures, in turn,
orientation and heat flux. depend on the fibre orientation due to the low through-thickness
2. The results have also shown that, on average, the tensile and bend- thermal conductivity of the CF. This behaviour is because the level
ing properties of the CFRP specimens decreased the most between of exposure directly influences the physico-chemical processes
LE and ME. However, the overall largest decrease in tensile and occurring in the specimens, hence the changes to the chemical
bending properties of the CFRP specimens was found in specimens composition. The results also demonstrate that the validity of the
after HE, as expected. These results show that the ER plays an testing approach is also affected by the fact that the damaged
important fundamental role in assisting the CF to resist failure by areas are no longer in composite action.
providing support by redistributing the stresses. Therefore, if the ER
pyrolyses, it cannot support the fibre to retain the load. ACKNOWLEDG MENTS
3. The results also show that after HE, the post-fire bending proper- The authors gratefully acknowledge the financial support for this work
ties decrease 61%, 95% and 85% for the S1, S2 and S3 CFRP from the Defence Science and Technology Laboratory (Dstl).
10991018, 0, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/fam.3163 by University Of Auckland, Wiley Online Library on [06/12/2023]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
ASPINALL ET AL. 23

ORCID 20. Quach THY, Benelfellah A, Batiot B, et al. Determination of the ten-
Tim J. Aspinall https://orcid.org/0000-0003-2506-1603 sile residual properties of a wound carbon/epoxy composite first
exposed to fire. J Compos Mater. 2017;51(1):17-29. doi:10.1177/
Emmajane L. Erskine https://orcid.org/0000-0003-4795-6336
0021998316637419
Rory M. Hadden https://orcid.org/0000-0001-6985-8900 21. Jones RM. Mechanics of Composite Materials. 2nd ed. Taylor & Francis;
1999:519, ISBN: 0938994247. doi:10.1115/1.3423688, 42.
RE FE R ENC E S 22. Aspinall TJ, Erskine EL, Taylor DC, Hadden RM. Influence of thermal
exposure and carbon fibre orientation on the post-fire tensile behaviour
1. Irving PE, Soutis C. In: Soutis C, ed. Polymer Composites in the
of CFRP laminates. Defence and Security Doctoral Symposium (DSDS22),
Aerospace Industry. 1st ed. Woodhead Publishing; 2017:1-17, ISBN:
Cranfield University, 9–10 Nov, 2022. Cranfield University; 2023. doi:10.
9788578110796. doi:10.1017/CBO9781107415324.004
17862/cranfield.rd.21821025.v2
2. Mouritz AP. Introduction to Aerospace Materials. Vol 55. Woodhead Publish-
23. Ogunleye RO, Rusnakova S, Zaludek M, Emebu S. The influence of ply
ing; 2012:611, ISBN: 9781845695323. doi:10.5124/jkma.2012.55.7.649
stacking sequence on mechanical properties of carbon/epoxy composite
3. Chawla KK. Composite Materials: Science and Engineering. 3rd ed.
laminates. Polymers. 2022;14(24):1-12. doi:10.3390/polym14245566
Springer; 2012:542, ISBN: 9780387743646. doi:10.1201/b19346-39
24. Mlyniec A, Korta J, Kudelski R, Uhl T. The influence of the laminate
4. Chung DD. Carbon Fiber Composites. 1st ed. Butterworth Heinemann;
thickness, stacking sequence and thermal aging on the static and
1994:682 ISBN: 9780128044599.
dynamic behavior of carbon/epoxy composites. Compos Struct. 2014;
5. Tiwari A, Shukla S. In: Tiwari A, Shukla S, eds. Advanced Carbon
118(1):208-216. 10.1016/j.compstruct.2014.07.047
Materials and Technology. 1st ed. Scrivener Publishing; 2014:481
25. Anton H, Florin B, Andrei-Daniel V, Daniel V, Daniela-Ioana T,
ISBN: 9781118686232.
Cataalin A. Mechanical characteristics evaluation of a single ply and
6. Garcez M, Menegthetti L, Filho TRLCPS, et al. In: Masuelli MA,
multi-ply carbon fiber-reinforced plastic subjected to tensile and bend-
ed. Fiber Reinforced Polymers—The Technology Applied for Concrete
ing loads. Polymers. 2022;14(15):1-24. doi:10.3390/polym14153213
Repair. 1st ed. InTech; 2013:229 ISBN: 9789535109389.
26. Kalantari M, Dong C, Davies IJ. Effect of matrix voids, fibre misalign-
7. Clyne TW, Hull D. An Introduction to Composite Materials. 3rd ed. Cam-
ment and thickness variation on multi-objective robust optimization
bridge University Press; 2019:345, ISBN: 9781119130536. doi:10.
of carbon/glass fibre-reinforced hybrid composites under flexural
1017/CBO9781139170130
loading. Compos Part B Eng. Aug. 2017;123:136-147. doi:10.1016/J.
8. Grigoriou K, Mouritz AP. Influence of ply stacking pattern on the
COMPOSITESB.2017.05.022
structural properties of quasi-isotropic carbon-epoxy laminates in fire.
27. Mouritz AP. Post-fire flexural properties of fibre-reinforced polyester,
Compos Part A: Appl Sci Manuf. 2017;99:113-120. doi:10.1016/j.
epoxy and phenolic composites. J Mater Sci. 2002;37(7):1377-1386.
compositesa.2017.04.008
doi:10.1023/A:1014520628915
9. Mouritz AP, Gibson AG. Fire Properties of Polymer Composite
28. Berlin P, Dickman O, Larsson F. Effects of heat radiation on carbon/-
Materials. In: First GG, ed. Springer; 2006:394, ISBN: 9788578110796.
PEEK, carbon/epoxy and glass/epoxy composites. Composites. 1992;
doi:10.1017/CBO9781107415324.004
23(4):235-243. doi:10.1016/0010-4361(92)90183-U
10. Mouritz AP. Fire Safety of Advanced Composites for Aircraft. Australian
29. Gibson AG, Wright PN, Wu YS, Mouritz AP, Mathys Z, Gardiner CP.
Transport Safety Bureau, Tech. Rep; 2006:30.
Modelling residual mechanical properties of polymer composites
11. Aspinall TJ, Erskine EL, Taylor DC, Hadden RM. A study of the thermo-
after fire. Plast Rubber Compos. 2003;32(2):81-90. doi:10.1179/
mechanical behaviour of CFRP laminate using small-scale apparatus.
146580103225009040
Compos Struct. 2022;302:1-16. doi:10.1016/j.compstruct.2022.116206
30. Sorathia U, Beck C, Dapp T. Residual strength of composites during
12. Bai Y, Vall'ee T, Keller T. Modeling of thermal responses for FRP com-
and after fire exposure. J Fire Sci. 1993;11(3):255-270. doi:10.1177/
posites under elevated and high temperatures. Compos Sci Technol.
073490419301100305
2008;68(1):47-56. doi:10.1016/j.compscitech.2007.05.039
31. Aspinall TJ. Quantifying the thermomechanical behaviour of carbon fibre
13. Bazli M, Ashrafi H, Jafari A, Zhao XL, Gholipour H, Oskouei AV. Effect of
reinforced polymer materials exposed to fire conditions. Ph.D. Disserta-
thickness and reinforcement configuration on flexural and impact behav-
tion, The University of Edinburgh. 2022, p. 316. doi:10.7488/era/2689
iour of GFRP laminates after exposure to elevated temperatures. Compos
32. Drysdale D. An Introduction to Fire Dynamics. Vol 66. 3rd ed. Wiley;
Part B Eng. 2018;157(8):76-99. doi:10.1016/j.compositesb.2018.08.054
2011:551. doi:10.1016/0010-2180(86)90037-4
14. Aspinall TJ, Erskine EL, Taylor DC, Hadden RM. Thermomechanical
33. ASTM. Standard Test Methods for Constituent Content of Composite
behaviour of carbon fibre reinforced polymer exposed to fire conditions.
Materials—D3171 22. Annual Book of ASTM Standards; 2016:1-6.
Defence and Security Doctoral Symposium (DSDS20), 10–11 November.
doi:10.1520/D3171-22.Copyright
Cranfield University; 2020. doi:10.17862/cranfield.rd.13341887.v1
34. Babrauskas V. Development of the Cone Calorimeter—A Bench-Scale
15. Bai Y, Keller T. High Temperature Performance of Polymer Composites.
Heat Release Rate Apparatus Based on Oxygen Consumption. National
1st ed. Wiley; 2014:223, ISBN: 9783527334391. doi:10.1002/
Bureau of Standards, Tech. Rep.; 1982:75.
9783527654147
35. ASTM. Standard Test Method for Tensile Properties of Polymer Matrix
16. Feih S, Mouritz AP. Tensile properties of carbon fibres and carbon
Composite Materials—D3039/D3039M 17. ASTM, Tech. Rep.; 2014.
fibre-polymer composites in fire. Compos A: Appl Sci Manuf. 2012;
doi:10.1520/D3039
43(5):765-772. doi:10.1016/j.compositesa.2011.06.016
36. ASTM. Standard Test Method for Flexural Properties of Polymer Matrix
17. Vieille B, Coppalle A, Carpier Y, Maaroufi MA, Barbe F. Influence of
Composite Materials—D 7264/D 7264M-07. ASTM, Tech. Rep.; 2020.
matrix nature on the post-fire mechanical behaviour of notched
polymer-based composite structures for high temperature applica-
tions. Compos Part B Eng. 2016, ISSN: 13598368;100:114-124. doi:
10.1016/j.compositesb.2016.06.059 How to cite this article: Aspinall TJ, Erskine EL, Taylor DC,
18. Zhu C, Li J, Clement M, Yi X, Rudd C, Liu X. The effect of intumescent
Hadden RM. Effect of fibre orientation and thermal exposure
mat on post-fire performance of carbon fibre reinforced composites.
J Fire Sci. 2019;37(3):257-272. doi:10.1177/0734904119849395 on the post-fire mechanical behaviour of carbon fibre
19. Li J, Zhu C, Zhao Z, et al. Fire properties of carbon fiber reinforced reinforced polymer material. Fire and Materials. 2023;1‐23.
polymer improved by coating nonwoven flame retardant mat for doi:10.1002/fam.3163
aerospace application. J Appl Polym Sci. 2019;136(30):1-14. doi:10.
1002/app.47801

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