Composites Part B: George Irven, Declan Carolan, Alexander Fergusson, John P. Dear
Composites Part B: George Irven, Declan Carolan, Alexander Fergusson, John P. Dear
                                                                        Composites Part B
                                                      journal homepage: www.elsevier.com/locate/compositesb
A R T I C L E I N F O A B S T R A C T
Keywords:                                                 Low density aramid and carbon fibre-reinforced epoxy foam has been synthesised with the aim of improving
Epoxy foam                                                mechanical properties, principally fracture performance. The foam properties measured were fracture energy,
Fracture toughness                                        compressive strength, and density. The influence of fibre type, loading, and length was investigated. In addition,
Fibre-reinforced
                                                          composite face-sheet bond tests were performed to ascertain how effective toughness transferred from individual
Fractography
                                                          component to composite structure. In general, the addition of fibres improved the mechanical performance of
                                                          reinforced samples compared to the control foam. Increases in compressive strength were moderate whilst
                                                          fracture energy was increased by up to 107% from 124 J/m2 to 256 J/m2 by the addition of 0.75 mm aramid
                                                          fibres. Increased fracture energy of the foam and the presence of fibres on the foam surface, caused an increase in
                                                          face-sheet bond propagation fracture toughness of 50% from 277 J/m2 to 416 J/m2.
1. Introduction                                                                            variety of researchers in recent years, Song et al. [6] produced short
                                                                                           carbon fibre-reinforced epoxy foams via mechanical frothing and ach
    The combination of high specific strength, corrosion resistance and                    ieved an increase in toughness of up to 113% at densities ranging from
low radar signature makes composite sandwich structures an attractive                      362 to 475 kg/m3. Alonso et al. [7] synthesised short fibre-reinforced
structural choice for many disciplines [1]. However, the brittle nature of                 epoxy foam with both glass and aramid fibres at a density of 300
composite materials can lead to substantial overdesign of sandwich                         kg/m3. Improvements in shear and compressive strength were sub
structure components, counteracting their weight and cost savings                          stantial, especially in the foam rise direction. Alonso et al. highlight the
benefits. The toughness of a composite sandwich structure, which is a                      importance of using a suitable coupling agent between fibre and matrix
critical parameter for it to withstand damage, can be improved by                          to ensure effective strengthening. They also worked on modelling of the
improving the toughness of the individual components. Previous                             compressive properties of glass fibre-reinforced epoxy foam using a
research by this group has demonstrated that by altering the layup of the                  statistical approach [8]. The foams ranged from 250 to 550 kg/m3 and
individual plies in the composite face-sheets, a significant increase in                   the variables that were studied were density, fibre weight fraction, and
impact resistance of the structure can be obtained [2]. More recently,                     fibre length. They note that more variables such as fibre aspect ratio and
impact performance of sandwich structures has been improved through                        stiffness could be included for increased accuracy.
toughening the matrix of the sandwich face-sheet [3]. During the impact                        Fibre modification of polymer foams has been the subject of research
testing of the epoxy-foam-core sandwich structures in the previous                         for some time. Cotgreave and Shortall [9–11] investigated polyurethane
research, extensive cracking within the core was found. As such, this                      foams reinforced with chopped glass fibres. Increases in tensile strength
project builds on this research further and details a systematic study of                  were moderate, up to 22%, while increases in toughness were more
the effect of reinforcing epoxy foam with short-cut carbon and aramid                      pronounced, up to 45%. Fibres were found to lie within struts and shown
fibres with the aim of increasing strength and toughness. Toughness is a                   to arrest or deflect cracks propagating through the foam matrix causing
crucial property for foams as in tension they fail by the propagation of a                 fibre pull-out to occur. They found that individual filaments well
single crack [4]. Marsavina and Linul [5] recently conducted a                             distributed within the foam were more effective than fibre bundles.
comprehensive review of the fracture toughness of polymer foams                            Carling [12] tested polyurethane foams reinforced with 7 mm glass fi
including reinforcement methods.                                                           bres at a density of 80 kg/m3 Limited gains in fracture energy were
    Reinforcement of epoxy foam has experienced attention from a                           realised, however, modulus and critical stress intensity factor were
    * Corresponding author. FAC Technology, 53 Lydden Grove, London, SW18 4LW, UK.
      E-mail address: d.carolan@imperial.ac.uk (D. Carolan).
https://doi.org/10.1016/j.compositesb.2022.110433
Received 28 March 2022; Received in revised form 9 October 2022; Accepted 17 November 2022
Available online 18 November 2022
1359-8368/© 2022 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
G. Irven et al.                                                                                                              Composites Part B 250 (2023) 110433
improved. It was noted that improvements in mechanical performance                temperature is required when manufacturing foams as the viscosity,
were limited due to the fibres being bundled together as opposed to               particularly the thixotropic response, of the foam is critical to devel
being individually distributed throughout the foam. Significant work              oping and maintaining an optimal microstructure at a target density.
has been carried out on fibre-reinforced phenolic foams [13–16], im              The fibre loadings used in parts per hundred resin (PHR) were 0.5, 1,
provements in compressive, tensile, shear, and friability properties were         2.5, and 5. For 3 mm and 6 mm fibres, it was only possible to load the
substantial.                                                                      resin with 0.5 and 1 PHR, higher loading caused a drastic increase in
    The failure mode of face-core debonding can cause significant de             viscosity and resulted in a poor-quality foam.
creases in the structural integrity of sandwich panels as it prevents shear           Carbon fibre-reinforced polymer (CFRP) composite sandwich panels
transfer between face sheets [17]. Recent single cantilever beam (SCB)            were manufactured for single cantilever beam (SCB) testing. The carbon
tests by Irven et al. [3] found that systematically modifying the matrix          fibre used was 385 gsm of H2550 fibres in 12 k tows in a 0/90 non-crimp
resin of the sandwich face-sheet caused a change in failure mode at the           fabric, the SCB sandwich panels used [[0/90]4]s for 8 plies in each face-
face-core interface. When the matrix resin has high strength, the failure         sheet. An amine-cured epoxy system formed the matrix of the SCB
mode involves significant foam fracture whereby portions of foam                  panels. The resin was a standard diglycidyl ether of bisphenol-A
remain on the face after testing. As such, it was expected that an                (DGEBA) with an epoxide equivalent weight of 185 g/eq. This was
improvement in foam fracture performance caused by the addition of                cured with a stoichiometric amount of a difunctional primary amine
short fibres would translate to an improvement in SCB interface                   (JEFFAMINE D-230) from Huntsman, UK. The composite sandwich
toughness. Furthermore, Shen et al. [16] reported a seven-fold increase           panels were laid up on a flat release-coated aluminium plate and sealed
in peel resistance with the addition of 3 wt percentage (wt%) 6.4 mm              using a vacuum bag. The infusion then took place over a period of 5–10
aramid fibres in phenolic foam.                                                   min and was then cured under vacuum for 10 h at 40 ◦ C and 10 h at
    The current research investigates reinforced epoxy foams at a nom            55 ◦ C.
inal density of 170 kg/m3 with the aim of improving the mechanical
properties of the epoxy foam. A key aim of this work was to maintain a            3. Methods
low density for all reinforced foams to maximise utility in real-world
applications. Previous research in the literature has mainly focussed                 Single-edge notched bending (SENB) tests in three-point bend
on high density epoxy foams [6,7].                                                configuration were conducted to determine the fracture energy, Gc, in
                                                                                  accordance with ASTM D-5045 [18]. Multiple studies have confirmed
2. Materials                                                                      the SENB specimen to be suitable for fracture toughness testing in foam
                                                                                  [19,20]. In order to satisfy the plane strain condition, test specimens
    A commercially sensitive epoxy based foaming resin formed the basis           were machined with dimensions 140 mm × 28 mm × 14 mm. These
of the materials investigated in the current work. The nominal density of         specimens were notched to a depth of 14 mm with a razor blade held in a
the cured foam in the current work is 170 kg/m3. Short-cut para-aramid            custom device that was fixed to a drill press, allowing a consistent notch
and carbon fibres were sourced from Barnet Europe. Aramid fibres had              depth to be achieved. Razor blades are frequently used in the literature
cut lengths of 0.75 mm, 3 mm, and 6 mm and an average diameter of 12              to create cracks in foam fracture toughness specimens [11,12,17,21,22].
μm. Carbon fibres had cut lengths of 1.5 mm, 3 mm, and 6 mm and an                All mechanical testing was conducted using an ‘Instron 4466’
average diameter of 8 μm. Manufacturing limitations prevented 0.75                screw-driven universal testing machine fitted with a 10 kN load cell. The
mm carbon fibres being cut. Both short-cut fibre types were appropri             SENB specimens were tested at a constant crosshead displacement rate
ately sized for use with epoxy. Milled carbon fibres were sourced from            of 1 mm/min. The fracture energy, GIc was calculated using the energy
ELG Carbon Fibre with average length 0.6 mm and an average diameter               method via:
of 7 μm. The milled fibres used were unsized prior to milling and were
                                                                                                  U
used as received.                                                                 GIc (bulk) =                                                              (1)
    Reinforced epoxy foams were synthesised via a dispersing homoge                             bwφ
nising blade attached to a mounted mixer with a maximum rotational
                                                                                  Where U is the energy under the corrected load-displacement curve and
speed of 2800 rpm to disperse fibres in the foaming resin. High-speed
                                                                                  φ is an energy calibration factor as defined in the ASTM standard (b and
mixing took place with a resin temperature of 70 ◦ C to minimise vis
                                                                                  w are the breadth and width of the sample respectively) [18]. At least
cosity and ensure the good dispersion of the various fibres. A stoichio
                                                                                  five replicate specimens were tested for each formulation.
metric amount of a commercially sensitive amine-based hardener was
                                                                                      The compressive properties of the epoxy foam were tested according
then added, these constituents were then mixed thoroughly again. The
                                                                                  to ASTM D1621 [23] using a screw-driven universal testing machine.
mixture was noted to begin foaming shortly after mixing and was poured
                                                                                  Samples with dimensions of 30 × 30 × 30 mm3 cubes were cut from
into a rectangular mould and cured at 21 ◦ C for 24 h, followed by a 24 h
                                                                                  foam panels with a diamond saw. The samples were placed between
post-cure at 40 ◦ C. The long cure cycle at a precisely controlled
                                                                                  stainless steel testing platens, and a load was then applied with a
                                                                              2
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Fig. 2. SEM images of polished aramid foam samples. (a): Control (b): 0.75 mm 2.5 PHR (c): 3 mm 0.5 PHR. (d): 6 mm 1 PHR.
crosshead rate of 2 mm/min. Compressive strength was calculated from              mode-I dominant but not pure mode-I. It should be noted that it is ex
the maximum stress within a strain of 10%. The compression samples                pected that the mode-mixity for the SCB test used in this research is
were also used to calculate density. The sampls.es were measured and              minimal. Adams et al. [27,28] conducted finite element analyses to
weighed with an electronic balance. Measuring multiple samples                    evaluate the mode-mixity of various face-sheet debonding test methods.
allowed for variations in density across a foam panel to be monitored.            They found that the SCB test method was the most appropriate for
    Imaging of both polished and fractured foam samples was conducted             minimising bending stresses in the core, eliminating crack kinking, and
using a Tescan Mira scanning electron microscope (SEM). Polished                  minimising any mode-II component at the crack tip to below 5%. In fact,
samples were prepared using a standard wet grinding technique up to               they found that the mode-I component is over 98% for the sandwich
2000 grit sandpaper. Imaging of the polished samples revealed valuable            configurations evaluated.
information regarding the morphology and microstructure of the foams.                 SCB tests were conducted with both the control foam and the 2.5
A tight distribution of void size is typically a good indicator of subse         PHR 0.75 mm Aramid fibre foam. Test specimens of 25 mm × 185 mm
quent good mechanical performance. Additional images of the fractured             were cut from a panel with a core thickness of 10 mm and a face-sheet
samples were also taken with a high-resolution digital camera. The                thickness of 3.2 mm. A 12 μm thick PTFE crack starter film of length
camera used was a Canon EOS 5DS R with a 100 mm macro lens.                       55 mm was used to ensure an appropriately sharp starter crack. The
    Many test methods have been developed to test mode I debonding of             corrected beam theory (CBT) method was employed to calculate both
a sandwich skin, they are summarised by Ratcliffe [24,25] who also                the initiation fracture energy, Gc,init, and the steady-state propagation
developed a test using a lengthened loading arm in an attempt to stan            fracture energy, Gc,prop, of the composites. Each specimen is clamped to
dardise the test. However, the focus here will be on the SCB test as used         a roller that is free to move on a track perpendicular to the crosshead
by Glaessgen et al. [26] illustrated in Fig. 1. This method allows an             direction but is otherwise built-in. The tests were conducted at a con
apparent mode I critical strain energy release rate to be measured most           stant crosshead displacement rate of 2 mm/min using a screw-driven
accurately as discussed by Ratcliffe [24] and Adams [27,28]. Ratcliffe            tensile testing machine. The loads and displacements were recorded,
also carried out a sizing study which proposes an algorithm, based on             and the crack lengths monitored using a high-resolution digital camera
limitations of the material used, to determine appropriate dimensions             setup for magnification and periodic imaging. At least five replicate
for SCB specimens [24,25]. Dimension limitations such as sizing the               specimens were tested for each foam used.
initial debond length to ensure bending is the dominant deformation
mode of the loaded face sheet are outlined in a step-by-step manner. This         4. Results
sizing system has been followed for the material properties of the
sandwich structures in the current research. There are difficulties to            4.1. Microscopy: polished aramid-reinforced foam
measuring pure mode-I fracture properties of an interface between dis
similar materials; indeed, the measured mode is often mixed [29]. The                 Each foam sample was cut and polished to give a smooth surface to
difference of elastic properties between, in this instance, the skin and          image using an SEM. An SEM image of one foam containing each aramid
core, will disrupt the symmetry even if the geometry and loading are              fibre length is shown in Fig. 2. The images show cells surrounded by
symmetric. The mismatch in modulus will couple the normal and shear               nodes connected by cell walls. The images show the foams have bi-
deformations ahead of the debond front [24]. Consequently, the                    modal cell size distributions with many small cells surrounding fewer
measured critical strain energy release rate will not be referred to as           larger cells. The cell sizes do not appear to change significantly across
mode-I, GIc , but Gc and should be considered as a fracture energy that is        the aramid fibre-reinforced formulations. However, the small cells in the
                                                                              3
G. Irven et al.                                                                                                                       Composites Part B 250 (2023) 110433
Fig. 3. SEM images of polished aramid foam samples. (a): Large void in 6 mm 1 PHR. (b): Epoxy covered fibres in 0.75 mm 2.5 PHR.
Fig. 4. SEM images of polished carbon foam samples. (a): Milled fibre 2.5 PHR. (b): 1.5 mm 1 PHR. (c): 3 mm 1 PHR. (d): 6 mm 1 PHR.
aramid fibre-reinforced foams appear somewhat smaller than in the                         microscope. Large voids in fibre-reinforced foam with fibres of similar
control foam. The images also show that there is a slight loss of spher                  length have been previously reported in the literature [6,12].
oidicity in the cells between Fig. 2 (a) and Fig. 2 (b), (c), and (d). In the 3               During the manufacturing process of the foam, all fibres are
mm and 6 mm aramid foams, very large voids could be found. This is                        completely wetted with liquid epoxy. Furthermore, the aramid fibres are
shown clearly in Fig. 3 (a). These voids could measure up to 6 mm across                  sized appropriately for use in epoxy. As a result, the fibres in the finished
and were difficult to get an entire void within the field of view of the                  foam are covered in epoxy. This is the case even if the fibres do not
Table 1
Measured properties of aramid reinforced foam.
  Fibre Length          Fibre Loading     Fracture Energy GIc   %         Compressive Yield Strength     %           Density [kg/    %          Compressive Modulus
  [mm]                  [PHR]             [J/m2]                change    [MPa]                          change      m3]             change     [MPa]
                                                                                     4
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Table 2
Measured properties of carbon reinforced foam.
  Fibre Length    Fibre Loading        Fracture Energy GIc      %            Compressive Yield Strength     %           Density [kg/    %          Compressive Modulus
  [mm]            [PHR]                [J/m2]                   change       [MPa]                          change      m3]             change     [MPa]
                                                                                             completely lie within a natural cell wall, epoxy will encapsulate the fibre
                                                                                             and bridge to the cell wall, an example of this is shown in Fig. 3 (b).
                                                                                             Exposed fibres, with no epoxy sheath, are very rare within the polished
                                                                                             samples.
4.3. Compression
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4.4. Density
Fig. 9. SEM images of SENB fracture surfaces. (a): Control sample. (b): 6 mm 1 PHR aramid sample showing exposed aramid fibres up to 1 mm in length.
                                                                             6
G. Irven et al.                                                                                                                   Composites Part B 250 (2023) 110433
Fig. 10. SENB fracture surfaces 0.75 mm Aramid. (a): Fibres exposed after pull-out and fracture. (b): Fibres exposed after surrounding matrix failure.
Fig. 11. SENB fracture surfaces 6 mm Aramid. (a): Fibre pulled out with epoxy remaining on the end. (b): Image showing how long aramid fibres fray when broken.
sandwich structures. This is otherwise achieved through increased safety             plane around the base of a pulled-out fibre. Fig. 10 (a) exhibits a case
factors leading to an increase in structure weight.                                  where a microcrack is formed as a fibre debonds from the matrix. In
                                                                                     Fig. 10 (b) fibres are seen bridging across where a secondary crack has
4.5.2. Fracture morphology: Aramid-Reinforced Foam                                   caused epoxy to fracture off around them. These images clearly
    It can be seen in Fig. 9 that the toughening mechanisms of aramid                demonstrate that the presence of the fibres cause the crack path to
foams include fibre pull-out and fracture as well as crack deflection. The           deflect and lengthen which require additional energy to propagate [31]
crack direction in all fracture micrographs is from bottom to top. Fig. 9            and for additional lesser cracks to form leading to an increase in fracture
(a) shows the fracture surface of a control sample. The foam structure is            energy.
clearly visible and not dissimilar to the polished samples examined in                   Fig. 11 (a) shows an image of a pulled-out fibre while (b) shows a
Fig. 2. Moreover, the fracture surface was observed to have no signifi              series of fractured fibres, the bases of which are situated in nodes and
cant deviations from the initial crack plane over the entire crack prop             cell walls. It is clear from Fig. 11 (a) that, while the fibre is not
agation length. Fig. 9 (b) shows the fracture surface of a foam modified             completely encased in polymer, there is a significant amount of epoxy in
with 1 PHR 6 mm aramid fibres. Significant deviations from the initial               small pieces remaining adhered to the end of the fibre. This contrasts
crack plane were noted, indicating that the presence of the fibres in the            with the clean exposed fibres shown in Fig. 10. The cutting process to
foam caused the crack to deflect. In addition, many exposed fibres can be            prepare the fibres is an aggressive process. It is probable that it affects
observed, up to 1 mm long. On the contrary, in the polished sample                   the sizing of the virgin fibre, especially close to the cutting plane. The
images, Fig. 2, no exposed fibres were observed. Thus, the visible fibres            shorter 0.75 mm fibres will therefore be more affected by the cutting
in Fig. 9 (b) are as a consequence of the fracture process, i.e., they were          process than the longer fibres. The broken fibres in Fig. 11 (b) have split
pulled out of the opposite fracture surface. Fibre pull-out appears to be a          and frayed upon fracture. Furthermore, some amount of pull-out has
principal toughening mechanism within all the aramid fibre-reinforced                occurred before failure as the fibres are exposed. As the fibres are pulled
foams studied here. The fibres shown in Fig. 9 (b) are solitary fibres               out, they bridge the crack before failure. Sequential failure of groups of
and appear well dispersed within the foam rather than manifesting as                 these fibres are responsible for the progressive load-displacement traces,
bundles or agglomerates. This represents a key development on fibre-                 such as the one shown in Fig. 8.
reinforced foams previously reported in the literature where bundles
of fibres are mentioned as a manufacturing issue and being less effective            4.5.3. Fracture energy: carbon-Reinforced Foam
at improving mechanical and fracture properties [10,12].                                 The experimentally determined fracture energies for all of the
    The 0.75 mm aramid fibres caused large increases in the fracture                 manufactured carbon fibre-reinforced foams are given in Table 2. The
energy of the foam and allowed for a higher fibre loading than longer                addition of carbon fibres was found to greatly increase the toughness of
fibres. Fig. 10 presents examples of fibres on SENB fracture surfaces,               the foam from 124 J/m2 to a maximum of 245 J/m2. All the carbon fibre-
Fig. 10 (a) demonstrates that fibres are pulled out but does not show                reinforced foams showed an increase in fracture energy over the un
significant amounts of epoxy left on the surfaces of the fibres. It can be           modified foams. However, the link between fibre length and increase in
seen that the crack is deflected by a fibre as it deviates from its main             fracture energy is not as clearly defined as with the foams modified with
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Fig. 12. Photos of 6 mm carbon foam SENB samples. (a): Zoomed in image of the front of a sample during a test. The crack can be seen to initially cross the path of
fibres, fracturing them, then deflect to follow a path between aligned fibres within the foam. (b): Fracture surface of a sample showing a crack that has been deflected
multiple times and fractured fibres protruding from the fracture surface.
                                                                                       pouring the mixture into a separate foaming and casting mould, there is
                                                                                       no prevailing global direction for these aligned fibres within the foaming
                                                                                       and casting mould. The alignment of fibres is only local. However, since
                                                                                       fracture initiation is a local process, this local alignment of fibres is
                                                                                       critically important. In Fig. 12 (a), the fracture initially progresses up
                                                                                       wards from the initial crack tip from point A to point B, fracturing the
                                                                                       fibres in its path. After approximately 2 mm of crack propagation, it
                                                                                       straightens to progress mainly upwards to point C before deflecting
                                                                                       again to progress upwards to point D, taking a less obstructive path
                                                                                       between the aligned fibres within the foam. Fig. 13 plots the raw load
                                                                                       versus displacement data for this sample, as the load climbs from 20 to
                                                                                       35 N, small sharp dips in load are clearly visible. During this period of
                                                                                       the test, cracking noises were heard, however, periodic imaging
                                                                                       revealed no advancement of the main crack during this period. The
                                                                                       control foam did not produce these cracking noises; therefore, the noises
                                                                                       pre-failure in the fibre reinforced foams are attributable to the failure of
                                                                                       the fibres. Based on the analysis of Fig. 12 (a), Fig. 13, the periodic
                                                                                       imaging of the test, and the noises heard, the fibres fail before the crack
                                                                                       advances. The failure strain of the carbon fibres is lower than that of the
                                                                                       epoxy. As a result, when the sample is loaded and the area ahead of the
                                                                                       crack is strained past the fibre failure strain, the fibres fail sequentially.
                                                                                       When the epoxy failure strain is reached the broken fibres provide a path
                                                                                       for the crack to travel through until intact fibres prevent further prop
Fig. 13. Load-displacement curves for the SENB testing of carbon 6 mm
and control.                                                                           agation in that direction. The crack then deflects along the aligned fibres
                                                                                       and the sample fails suddenly. This deviation from the main plane of the
                                                                                       crack will give rise to mode II contributions and a resultant increase in
aramid fibres.
                                                                                       fracture energy. The crack path in this sample is also longer than an
                                                                                       unreinforced sample, again causing an increase in fracture energy.
4.5.4. Fracture morphology: carbon-Reinforced Foam
                                                                                            The toughening mechanisms taking place within this sample
    From fractographic analyses conducted on SENB samples, it can be
                                                                                       depended greatly upon the state of fibre-reinforcement ahead of the
seen that the toughening mechanisms for carbon fibre-reinforced foams
                                                                                       crack tip, in this instance the arrangement of the fibres was conducive to
also include fibre pull-out and fracture as well as crack deflection.
                                                                                       a high fracture energy. Some samples did not have fibres positioned in
Fig. 12 shows high-fidelity photographs of two 6 mm carbon 1 PHR
                                                                                       such a way as to give as high a fracture energy. This fact explains the
samples. Fig. 12 (a) shows fibres aligned beneath the surface of the foam
                                                                                       larger standard deviations in Tables 1 and 2 for the fracture data of long
of one of the samples. These fibres are 6 mm long and span the whole
                                                                                       fibre foams. Fig. 12 (b) shows the fracture surface of a different sample,
width of the image. The process of manufacturing the foam involves
                                                                                       it is clear from the upper image that the crack path has been deflected.
mixing the resin and fibres together with a rotating blade. During this
                                                                                       The lower image shows broken fibres protruding from the surface, the
process, the fibres tend to align tangential to the tip of the mixing blade
                                                                                       fibres appear to be individual and well dispersed. From these images it is
within the foam mixture. This is especially relevant for longer fibres.
                                                                                       clear that fibre breakage is a key toughening mechanism. Similar pho
    As a result of the circular mixing motion and the subsequent step of
                                                                                       tographs are not shown for aramid foams as the yellow fibres are
                                                                                   8
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Fig. 14. SENB fracture surfaces of carbon foams. (a): Empty fibre track from a 3 mm fibre. (b) Example of both a pulled out and fractured 3 mm fibre. (c): Example of
two 6 mm fibres pulled out.
Fig. 15. SENB fracture surfaces of carbon foam. (a) 3 mm fibres bridging after epoxy has fractured off. (b): 1.5 mm fibre pulled out with epoxy remaining. (c): Pair of
6 mm fibres pulled out coated with epoxy.
                                                                                       wher7e a fibre has been pulled during the fracture event. The fibre was
                                                                                       encased in epoxy, this is evident as the track is 2 μm wider than the 8-μm
                                                                                       diameter fibres. The rough surface of the fibre track reinforces this, a
                                                                                       smooth track would indicate that the fibre was not well adhered. Fig. 14
                                                                                       (b) demonstrates an example of how fibres can lie within a cell wall. One
                                                                                       fibre is fractured at the crack plane while the second fibre has been
                                                                                       pulled-out and is mostly encased in epoxy. Fig. 14 (c) exhibits a pair of
                                                                                       fibres lying within a node that have been pulled out and are also both
                                                                                       encased in epoxy. Fig. 15 (a) and (b) show long exposed fibres with
                                                                                       significant parts of cell walls remaining after fracture. The extra fracture
                                                                                       surfaces created by these fibres, and the associated energy absorption,
                                                                                       represents a significant toughening mechanism. The main toughening
                                                                                       from fibre pull-out is from the shear at the interface due to interfacial
                                                                                       fictional sliding [32]. Fig. 15 (c) shows a pair of fibres pulled out encased
                                                                                       in epoxy showing clear signs of epoxy shear failure on the surface. While
                                                                                       the aramid fibres were found by themselves, it was not uncommon to
                                                                                       find longer carbon fibres in pairs such as in Fig. 14 (c) and Fig. 15 (a) and
                                                                                       (c). Furthermore, while aramid fibres frayed and split when broken,
                                                                                       carbon fibres exhibited clean fractures.
Fig. 16. SEM image of a SENB fracture surface showing milled carbon fibres                 Fig. 16 shows a series of milled fibres protruding from the fracture
pulled out. Note the relatively clean surfaces of the milled fibres.                   surface. A key difference between these fibres and the longer, chopped
                                                                                       carbon fibres discussed earlier is the lack of epoxy polymer adhering to
difficult to distinguish.                                                              the fibre. The chopped fibres were originally sized for use with epoxy as
    The toughening mechanisms in carbon fibre-reinforced foams are                     the matrix and so are encased in epoxy when pulled out, whereas the
highlighted in Fig. 14. Fig. 14 (a) shows an empty fibre track, from                   milled fibres did not have any appropriate sizing and so pull out with a
                                                                                       very clean surface, almost devoid of polymer. Despite this, the milled
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Fig. 17. SEM image of a 6 mm fibre below the surface of a fractured node
having been loaded.
fibres provide benefit as the pull-out of clean fibres still absorbs energy
through interfacial frictional sliding [32].
    Fig. 17 shows a carbon fibre below the surface of a fractured node
from an SENB sample. From the striations leading to the cell wall and               Fig. 18. Load-displacement curves for the SCB testing of a control and a 2.5
node, it is clear that the fibre and the surrounding polymer material was           PHR 0.75 mm aramid sample.
loaded as the crack passed along the main fracture plane, providing a
stiffening effect. It is interesting to note that the fibres within the foam
causing this stiffening effect and increasing constraint may well be
reducing the fracture energy if they are not within the crack path trig            Fig. 21. Exposed fibres on the surface can be clearly observed. This is the
gering energy absorption mechanisms.                                                surface that the face-sheet will ultimately be infused on. The aramid
                                                                                    fibres are much tougher and difficult to machine than the relatively
                                                                                    friable polymer foam structure. As a result, during the machining pro
4.6. Effect on face-core interface                                                  cess, they tend to deflect under the cutting blade and bounce back once
                                                                                    the blade has passed. Fibres exposed during foam machining leave an
    Once the improvements in fracture performance of fibre-reinforced               ideal surface for the face-sheet matrix resin to bond to. Control foam
foams had been confirmed, a set of SCB face-core debond tests were                  samples showed failure partially within the foam. It was hypothesised
carried out on both a control foam and a 2.5 PHR 0.75 mm aramid foam.               that were the foam made tougher, the failure of the SCB specimens
The results of this SCB testing can be found in Table 3. An example of a            would be mostly interfacial and the foam would be left intact. However,
load versus displacement for each type of sample is shown in Fig. 18.               it is clear from the results presented here, that in adding fibres to the
Adding 0.75 mm 2.5 PHR aramid fibres to the foam core of a sandwich                 foam the interfacial bond itself has also been improved due to the
structure increases face-core propagation fracture toughness by 50%                 exposed fibres on the surface.
and initiation fracture toughness by 30%. Fig. 19 shows images taken of
the side of both types of SCB samples during testing, the images show               5. Conclusion
that foam is fractured off the core and remains on the face-sheet surface.
As a result, similar toughening mechanisms observed in SENB foam                        Low density short carbon and aramid fibre-reinforced epoxy foams
fracture have caused the increase in toughness of this interface. These             have been successfully synthesised for the first time. Improvements in
mechanisms are clear in face-sheet -side fracture surface images in                 the fracture performance of epoxy foams have been achieved through
Fig. 20 (a) and (b), exposed fibres that have been pulled out are clear in          the addition of these fibres. The effect of fibre type, length and loading
both photographs and SEM images. There is an increase in the difference             have been investigated. The incorporation of 5 PHR 0.75 mm aramid led
between the propagation and initiation fracture toughness with the                  to a maximum increase in fracture energy of 107% from 124 J/m2 to
addition of aramid fibres. This increase suggests an increase in the R-             256 J/m2. The main toughening mechanisms observed were fibre pull-
curve behaviour. This is due to material, mainly the fibres, bridging the           out, fibre fracture and crack deflection and arrest. The addition of 2.5
gap behind the crack tip. As the aramid foam fractures, the fibres are              PHR 0.75 mm aramid fibre and 0.6 mm carbon fibre both cause an in
often pulled out as seen in the side-on image in Fig. 19, and both the SEM          crease in compressive yield strength of ~10%, further additions cause a
micrograph and microscope image of the fracture surfaces in Fig. 20.                drop in strength. The addition of aramid fibre causes an increase in foam
Therefore, the fibres are being pulled out of the foam behind the crack             density of up to 16%, short carbon fibres only increased density up to 5%
tip, causing an increase in R-curve behaviour and a large increase in the           while 3 and 6 mm carbon fibres reduced density by up to 2%. When used
difference between propagation and initiation fracture toughness.                   in a composite sandwich structure, 0.75 mm 2.5 PHR aramid fibre-
    To further demonstrate the role of fibre bridging on improving the              reinforced foam improves face-core initiation and propagation fracture
toughness of the face-core interface, a side-on micrograph was taken                toughness by 30 and 50% respectively. This investigation has shown
using SEM of the surface of an ‘as-machined’ foam. This is shown in                 that fibre reinforced epoxy foams can outperform their unreinforced
Table 3
SCB results for aramid 0.75 mm 2.5 PHR foam and control foam.
  Fibre Length [mm]     Fibre Loading [PHR]    Initiation Gc [J/m2]   % change         Propagation Gc [J/m2]   % change       Prop – Init Gc [J/m2]    % change
  –                     –                      231 ± 43               –                277 ± 38                –              46 ± 7                   –
  0.75                  2.5                    301 ± 52               +30              416 ± 24                +50            115 ± 54                 +150
                                                                               10
G. Irven et al.                                                                                                                   Composites Part B 250 (2023) 110433
Fig. 19. Side view of SCB tests showing exposed fibres in the aramid foam sample.
Fig. 20. SCB face-sheet side fracture surface. (a) Digital photograph. (b) SEM image.
Data availability
                                                                                 Acknowledgements
Fig. 21. SEM image showing the edge of a machined sample of aramid foam
showing exposed fibres on the surface.                                               George Irven would like to acknowledge an EPSRC faculty CASE PhD
                                                                                 studentship with FAC Technology. Grant number [EP/R513052/1].
counterparts with few drawbacks other than a slight increase in density              Declan Carolan acknowledges the support of UKRI, Future Leaders
and increased manufacturing complexity. There are more gains to be               Fellowship. Grant number [MR/T023406/1].
realised if longer fibres can be used to manufacture low density foams
without large voids which reduce compressive strength. Large voids will          References
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