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Effect of Fire-Retardant Ceram Powder On The Properties of Phenolic-Based GFRP Composites
Effect of Fire-Retardant Ceram Powder On The Properties of Phenolic-Based GFRP Composites
Composites Part B
journal homepage: www.elsevier.com/locate/compositesb
A R T I C LE I N FO A B S T R A C T
Keywords: This paper investigated the effect of ceram powder on the properties of composite laminates based on glass fibres
Laminated composites and phenolic resin. The amount of ceram in the polymer matrix was varied between 30% and 50% of the weight
Phenolic resin of resin. The density, void ratio, tensile strength, interlaminar shear strength, bond strength, bending modulus
Ceram powder and glass transition temperature were studied, and the effect of ceram on these properties was assessed. A
Properties
systemic decision-making strategy is applied to evaluate the optimal amount of ceram in the polymer matrix.
Optimal design
Results showed that while the increase of ceram decreased the strength properties of the composite laminates,
the bulk density and bending modulus increased. Moreover, the glass transition temperature increased by 32 °C
with the addition of 50% (by weight of resin) ceram powder. The strategic decision-making approach suggested
that a good balance of physical, mechanical, and thermos-mechanical properties can be achieved when ceram is
added at a fraction of 50% of the weight of resin, and this amount is considered as optimal for designing
laminated fibre composites.
∗
Corresponding author. ARC Training Centre for Advanced Manufacturing of Prefabricated Housing, Department of Infrastructure Engineering, The University of
Melbourne, Parkville, VIC 3010, Australia.
∗∗
Corresponding author. Centre for Future Materials (CFM), School of Civil Engineering and Surveying, University of Southern Queensland, Toowoomba, QLD
4350, Australia.
E-mail addresses: wahid.ferdous@unimelb.edu.au (W. Ferdous), dtngo@unimelb.edu.au (T.D. Ngo), kate.nguyen@unimelb.edu.au (K.T.Q. Nguyen),
abdallah.ghazlan@unimelb.edu.au (A. Ghazlan), pamendis@unimelb.edu.au (P. Mendis), allan.manalo@usq.edu.au (A. Manalo).
https://doi.org/10.1016/j.compositesb.2018.09.032
Received 28 April 2018; Received in revised form 15 September 2018; Accepted 15 September 2018
Available online 17 September 2018
1359-8368/ © 2018 Elsevier Ltd. All rights reserved.
W. Ferdous et al. Composites Part B 155 (2018) 414–424
mechanical properties of composites may degrade, the addition of fire reinforced composites once activated by high temperature (from 350 °C
retardant filler can greatly improve their fire resistance [12,24]. For to 800 °C or higher) under fire conditions [26]. The off-white colour
example, the bending strength of an epoxy-based polymer matrix was ceram powder has a specific gravity of 1.80 and is also effective in
reduced with the addition of ATH fillers but increased its glass transi- reducing overall weight, resisting moisture, and controlling smoke de-
tion temperature by 5 °C [25]. For composite laminates, the mechanical velopment. This material was supplied by Ceram Polymerik Pty Ltd,
properties cannot be sacrificed significantly for meeting fire require- Australia.
ments. Therefore, the present study focused on investigating the prop-
erties of phenolic-based laminated GFRP composites with the addition 2.2. Specimen preparation
of ceram powder and determining the optimal volume of ceram powder
to achieve a balance in mechanical properties. The laminated composite specimens were fabricated by three layers
Different percentages of ceram powder were added to the matrix of of fabrics with a stacking sequence of [0/-45/+45/+45/-45/90/
the laminated composites during the fabrication. The mechanical +45/-45/0], which were bonded with a phenolic polymer matrix. The
properties of these composites were then evaluated including tensile, longitudinal (0°), transverse (90°) and diagonal ( ± 45°) fibres provide
interlaminar shear, bond and bending properties. The effect of ceram a balance of strength and stiffness in all directions. Polymer matrices
powder on the glass transition temperature of laminates was also in- were produced with different mixing ratios of resin, hardener, urepac
vestigated. Finally, the optimal volume of ceram was determined using and ceram. The liquid resin, hardener and urepac were mixed together
a structured technique based on the experimental results. The outcome before adding the ceram powder. In all mixtures, the fractions of the
of this study will contribute scientific knowledge for designing lami- hardener and urepac were 20% and 10% of the weight of phenolic
nated composites for with optimal mechanical and fire resistance per- resin, respectively, while the ceram was added at 0%, 30%, 40% and
formance. 50% of the resin weight, thereby producing four different matrices
named C0, C30, C40 and C50, respectively. These percentages of filler
2. Experimental program were based on the previous study by Ferdous et al. [25] wherein they
found that epoxy-based polymer resin with 30%–50% of fillers will
2.1. Materials produce a matrix with reasonable properties. Furthermore, the addition
of ceram over 50% by weight did not produce a workable polymer
The materials employed in this investigation were fabrics, resin and matrix. The laminated composite without Ceram (C0) is considered as a
filler. reference specimen for comparing the performance of the C30, C40 and
C50 samples.
2.1.1. GFRP fabrics After hand laminating the GFRP laminates (nominal dimensions of
The glass fibre reinforced fabrics were composed of three plies of 375 mm × 375 mm × 2.5 mm), they were placed in an oven for heat
reinforcement in a stacking sequence of [0/-45/+45]. The bonded curing. In the oven, the laminates were positioned between two plain
fabrics strictly control fibre alignment, allowing for stronger, stiffer and aluminium sheets and non-stick hot plate liner to facilitate a smooth
lightweight laminates; and improve surface quality while minimising non-stick surface. Each specimen was then loaded with a 20 kg plate to
the formation of resin-rich pockets. The stacking sequence allows compress it during heating. The oven was preheated at 95 °C and each
flexibility in engineering laminated composites for specific strength specimen was subjected to three different temperatures, namely 95 °C,
requirements using different fibre orientations. 115 °C and 165 °C. The total curing time was approximately 100 min,
which consisted of the following phases: starting with an initial tem-
2.1.2. Phenolic resin perature of 95 °C for 20 min; increasing the temperature from 95 °C to
In this study, GP 486G34 Phenolic impregnating resin was used as a 115 °C over 10 min; settling at a temperature of 115 °C for 20 min; again
binder of fibreglass mat. The liquid amber resin was formulated by increasing the temperature from 115 °C to 165 °C over 20 min; and fi-
phenol and formaldehyde, which have a specific gravity of 1.24. To nally heating the sample at 165 °C for the final 30 min. This curing
enhance the polymerisation reaction within a practical time period, the regime was implemented to minimise pitting on the composites surface
resin was mixed with hardener. The liquid brown hardener (GP 4826C caused by gas release. When heated at 165 °C, the surface colour of the
Hardener) with a specific gravity of 1.41 was formulated by phosphoric, specimen C0 turned into light orange while the other samples with
arylsulphonic and sulphuric acid. UrePac+1008 with specific gravity of ceram (C30, C40 and C50) turned into light yellow as shown in Fig. 1.
1.14 was also introduced in the resin system to maintain the pH and
improve the workability of the polymer matrix. The resin and hardener 2.3. Mechanical testing
were supplied by Pacific Urethanes Pty Ltd, Australia.
The tensile, interlaminar shear, bond and bending properties of la-
2.1.3. Fire-retardant filler minated composites with different ceram volumes were evaluated fol-
The filler material used in this study is Ceram Polymerik FM-3H, lowing the relevant ASTM standards. The tests were conducted at room
which is a development grade of ceramifying additives in powder form. temperature under displacement controlled conditions at a rate of
This powder, when added to the resin, creates a ceramic shell in fibre 1–2 mm/min [27] using a 100 kN MTS testing machine. Five specimens
Fig. 1. Changes of colour with the increase of ceram in the laminated composites. (For interpretation of the references to colour in this figure legend, the reader is
referred to the Web version of this article.)
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W. Ferdous et al. Composites Part B 155 (2018) 414–424
Table 1 5.3%, 7.4% and 11.9% for C0, C30, C40 and C50 samples, respectively.
Specimen details and test standards. This range of voids is similar to that of other laminated fabric compo-
Type of test Nominal dimensions (L × W × T) No. Of Test Ref. sites, e.g. between 5.09% and 11.2% according to the findings of
samples standard Jeong's [33] study. The increase of ceram reduced the flowability of the
matrix, thereby increasing the void content. This finding is further
Tensile 250 mm × 25 mm × 2.5 mm 5 ASTM [27]
supported by the microscopic images as presented in Fig. 2(b) and 2(e).
D3039
Short beam 15 mm × 5 mm × 2.5 mm 5 ASTM [28]
The optical microscope captured the voids at the surface and it can be
shear D2344 seen that more and larger voids were formed with the increase of ceram
Lap shear Each leg 100 × 25 × 2.5 mm 5 ASTM [29] powder.
D5868
Bending 80 mm × 25 mm × 2.5 mm 5 ASTM [30]
3.2. Tensile properties
D790
DMA 55 mm × 10 mm × 2.5 mm 2 ASTM [31]
D4065 The failure modes of the tensile specimen in the longitudinal and
transverse directions are shown in Fig. 3(a) and (b), respectively. In the
longitudinal direction, all of the specimens failed due to tensile failure
were tested for each specimen type to account for statistical variation of the glass fibres within the gauge length with no observed slip or
and to achieve reliable results. The load and corresponding displace- failure in the anchorage zone. However, delamination was observed for
ments were directly recorded by the instruments and the failure beha- C50 specimen as shown in Fig. 3(a). This delamination can be due to
viour was observed during the testing. The specimens’ length (L), width the existence of large voids in this specimen. The delamination ob-
(W) and thickness (T) and the test standards followed are provided in served for C50 in the longitudinal direction is also reflected in the
Table 1. stress-strain behaviour shown in Fig. 3(c). As can be seen from the
figure, the stress in the laminates dropped when delamination occurred
2.4. Dynamic mechanical analysis (DMA) at a strain of around 1% and stress of 80 MPa but continued to carry
load until rupture of the longitudinal fibres. Similarly, a slight decrease
The thermomechanical behavior of the composite laminates was in stiffness was observed at the same level of strain for all longitudinal
investigated under the dynamic mechanical analysis (DMA) with a (Fig. 3(c)) and transverse (Fig. 3(d)) specimens. This decrease in stiff-
NETZCH 242 E Artemis according to the ASTM D4065 [31] testing ness was due to the formation of cracks in the matrix. The nonlinearity
standard. Two samples from each laminate type were prepared with a could also be from the progressive interfacial bond failure of ± 45° and
nominal thickness of 2.5 mm, width of 10 mm, and length of 55 mm. 90° GFRP layers as was also suggested by Manalo et al. [34] these fibres
These laminates were then loaded in a dual-cantilever setup at a fre- are not continuous throughout the length of the specimens. The non-
quency of 1 Hz from room temperature to 180 °C at a heating rate of linear stress-strain behaviour became more obvious with the increase of
3 °C/min. The storage modulus (E’) was recorded and plotted against ceram due to the increase in voids as highlighted in the previous sec-
temperature. The glass transition temperature (Tg) of the laminates was tion.
then measured based on the onset of the storage modulus curve. Fig. 3(c) and (d) indicates that the increase of ceram reduced the
tensile strength of the laminates. The ultimate tensile strength of C0,
3. Results and discussion C30, C40 and C50 specimens are 267, 247, 245 and 225 MPa in the
longitudinal direction or a reduction of strength by 7.5%, 8.2% and
3.1. Density and void content 15.7%, respectively. On the other hand, the tensile strength in the
transverse direction is 168, 142, 132 and 125 MPa for C0, C30, C40 and
The bulk density and void content of the laminated composites C50 specimens, respectively or a decrease of 15.5%, 21.4% and 25.6%
containing ceram powder was measured prior as they can have influ- for the samples with a ceram content of 30%, 40% and 50%, respec-
ence on the performance of composites. Fig. 2(a) shows the theoretical tively. This reduction of strength was due to the increased amount and
and measured density with the percentage of voids. The bulk density size of voids in the laminates. These defects tend to open in tension
was measured by the weight per unit volume and calculated theoreti- loading and continue to grow significantly with increased loading
cally using Eq. (1). The volume of void content is measured by Eq. (2). therefore giving a lower stiffness and overall strength. This behaviour
was also observed by Haj-Ali and Kilic [35] for their composite mate-
⎛w w w w wf ⎞ rials.
γt = 100/ ⎜ r + h + u + c +
γr γh γu γc γf ⎟ (1)
⎝ ⎠ 3.3. Interlaminar shear strength
v = 100(γt − γm)/ γt (2)
The interlaminar shear strength is an important characteristic to
In Eq. (1) and Eq. (2): γt and γm are the theoretical and measured evaluate the integrity of the fiber-resin interface in laminated compo-
density of the laminates; wr , wh , wu , wc and wf are the percentage sites [36]. When the transverse shear stress of a laminated composite
weights of resin, hardener, urepac, ceram and fibre in the laminates exceeds the interlaminar shear strength (ILSS), delamination failure
respectively; γr , γh , γu , γc and γf are the densities of these constituents; will occur between the fibre layers. From the experimental results, it
and v is the percentage void content. It is interesting to observe that the was observed that all specimens failed along the length at the mid-plane
theoretical density is increasing with an increase of ceram while the (Fig. 4(a)). Fig. 4(b) illustrates the load displacement behaviour of
measured bulk density is decreasing. The theoretical density obtained GFRP laminates with different ceram content. It can be seen that the
for C0, C30, C40 and C50 laminates are 1.777, 1.790, 1.792 and load displacement in ILSS are almost same for all specimens up to a load
1.795 g/cm3, respectively, while the corresponding measured densities of 50kN. After this load level, the load-displacement curve for laminates
are 1.705, 1.695, 1.659 and 1.581 g/cm3. This opposite trend between with ceram powder began to behave differently. This was due to the
theoretical and measured densities can be attributed to the formation of initiation of failure in these laminates, resulting in lower ILSS compared
voids in the polymer matrix. The formation of voids is a common to C0. The ILSS is determined from the ultimate load (P) and cross-
phenomenon that is unavoidable in composite materials, which is sectional area (A) relationship (ILSS = 0.75P/A) according to ASTM
caused by the mixing and consolidation of two or more discrete mate- D2344 [28]. Fig. 4(c) illustrates the ILSS for samples with different
rial components [32]. Fig. 2(a) shows that the void percentage is at 4%, percentages of ceram. The ILSS decreased from 14 MPa to 10.7, 9.4 and
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W. Ferdous et al. Composites Part B 155 (2018) 414–424
5.7 MPa with the increase of ceram by 30%, 40% and 50%, respec- the fracture surface for C0 (Fig. 5(a)) was rougher than other laminates
tively. The decrease of ILSS with the increase of ceram can be attributed (Fig. 5b and d) and became smoother with the increase percentage with
to the decrease of resin content and the formation of voids on which the ceram. Fig. 5(d) showed C50 had the smoothest fracture surface among
bond properties of the matrix are primarily dependant. Moreover, the the laminates, which explained the lowest ILSS for this sample.
decreasing ILSS for laminates with increasing percentage of ceram can
be explained by the failure behaviour. Fig. 5 showed the fracture sur-
face observed under a microscope. As can be noticed from the figures,
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W. Ferdous et al. Composites Part B 155 (2018) 414–424
3.4. Bond strength in Fig. 6(b) indicates that the increase of ceram in the matrix reduces
the ultimate failure load. The bond strength (Fig. 6(c)) obtained for C0,
The lap shear test was performed to further understand the effec- C30, C40 and C50 specimens are 10.1, 7.8, 7.2 and 5.1 MPa indicating a
tiveness of the ceram powder in bonding fibres. Fig. 6(a) shows the reduction of bond strength by 23%, 29% and 50% when ceram is added
bond failure under the lap shear test. In all specimens, failure was ob- at 30%, 40% and 50%, respectively. This is mainly due to the decrease
served due to adhesion. The load-displacement relationship illustrated in adhesion of the matrix with the increase of ceram. Compared to the
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W. Ferdous et al. Composites Part B 155 (2018) 414–424
short beam test, the measured bond strength from the lap shear test was 3.5. Bending properties
39%, 37%, 31% and 12% lower for C0, C30, C40 and C50 specimens,
respectively. This is because of the different loading mechanisms Failure of the specimen under three-point bending is shown in
wherein in the lap shear method, the failure plane was loaded in shear Fig. 7(a). It was observed that the specimens with ceram under bending
simultaneously with tension while the short beam method measures the load failed prematurely due to delamination. This can be explained by
almost pure shear of the laminates. the reduced ILSS shear strength of laminates as discussed in the pre-
vious section. Fig. 7(b) illustrates the load-displacement relationship for
C0, C30, C40 and C50 specimens under three-point bending while
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Fig. 7(c) illustrates a plot of the bending modulus with respect to dif- 3.6. Glass transition temperature
ferent ceram contents. The bending modulus (E = PL3/48δI) was de-
termined from the initial slope of the load-displacement curve (P/δ). It Fig. 8 shows the composite laminates after the test as well as the
can be seen from Fig. 7(b) that the bending strength of the laminates DMA plots. Fig. 8(b) shows an almost constant storage modulus (E′) was
decreased with the increase of ceram while the bending modulus observed for sample C0 from 30 °C up to around 75 °C. This indicates
(slope) increased with the addition of ceram. As mentioned previously, that the molecular chain mobility of the phenolic resin did not change,
the specimens failed due to delamination and the failure load is not since the temperature was below Tg. On the other hand, the samples
representative of the ultimate bending capacity for ceram-based lami- C30, C40 and C50 retained most of their storage modulus up to a
nates. The bending modulus on the other hand obtained for C0, C30, temperature of 90 °C. This result suggests that the addition of the ceram
C40 and C50 specimens are 18.6, 21.9, 24.2 and 25.5 GPa, respectively, powder made the mechanical properties of composite laminates stable
which indicated that the bending modulus increases by 18%, 30% and at elevated temperature. A rapid decrease in E’ was then observed at a
37% with the addition of 30%, 40% and 50% of ceram, respectively. temperature higher than 90 °C. This behavior indicates the transition of
The increase of bending modulus with the increase of ceram can be the matrix from a glassy to a leathery state. Under these conditions, the
attributed to the partial replacement of low modulus resin by high breakdown of secondary molecular bonds started leading to a decrease
modulus ceram in the polymer matrix. in mechanical properties.
At the onset of the storage modulus curves, Tg values of almost
86 °C, 97 °C, 103 °C, and 118 °C were recorded for the samples C0, C30,
C40, and C50, respectively. For composite laminates without ceram
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W. Ferdous et al. Composites Part B 155 (2018) 414–424
Table 4
Pairwise comparison of criteria.
Criteria Importance Intensity Criteria Importance Intensity
A B A B
Table 5
Change of performance with respect to C0 and normalised relative intensities.
Properties % Improvement (+ve) or reduction (-ve) Normalised relative intensities
Table 6
Global priorities of the laminates.
Samples Density Void Tensile Bond ILSS Modulus Cost Tg Total
C30 0.0026 0.0168 0.0319 0.0337 0.0360 0.0374 0.0429 0.0664 0.268
C40 0.0065 0.0064 0.0290 0.0268 0.0258 0.0633 0.0620 0.1028 0.323
C50 0.0169 0.0027 0.0152 0.0156 0.0143 0.0780 0.0739 0.1934 0.410
and bending modulus. The tensile strength, bond strength and inter- importance and intensities of the properties in criteria are provided in
laminar shear strength are given almost equal priority as they all re- Table 4.
present the strength of the composites and give moderate importance
over void content and density. Thus, the highest priority was given to 4.1.2. Relative intensities of alternatives
the glass transition temperature followed by the cost, bending modulus, The relative weightings of the alternative composite laminates (i.e.,
ILSS, bond strength, tensile strength, void and density. The relative C30, C40 and C50) are calculated based on their performances obtained
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in this study. As previously mentioned, some of the properties were composite laminates can be used for civil infrastructure exposed to
found to be good for C30 while others were good for C50. The per- an in-service elevated temperature of up to 95 °C.
centage improvement or reduction of performance with respect to the • The amount of ceram in the polymer matrix is found to be optimal
control specimen (i.e., C0) is tabulated in Table 5. The increase of when it is added by 50% to the weight of resin. This amount of
ceram reduces the cost of the matrix and the percentage improvement is ceram can provide a good balance among the physical, mechanical
calculated based on the consideration that resin is 8 times more ex- and thermo-mechanical properties.
pensive than ceram. The intensity of the weak specimen is given 1 in
pairwise comparison for a particular property and increased pro- An in-depth investigation on the effect of fire-retardant ceram
portionally for the strong one. For example, when comparing normal- powder on the fire performance of laminated composites is currently
ised relative intensities between C30 and C40, the intensity of the being conducted and has shown promising results. The results of this
density attribute for C40 is 2.5 (i.e., 2.9/1.2) relative to 1.0 (i.e., 1.2/ work are currently being analysed and the significant findings will be
1.2) for C30. Using this concept, the normalised relative intensities of published in the near future.
the alternatives are determined and provided in Table 5.
Acknowledgements
4.1.3. Determination of priorities for laminates
The priorities of the alternatives with respect to the criteria and This project was funded through the ARC Training Centre for
those of the criteria with respect to the goal are calculated and pre- Advanced Manufacturing of Prefabricated Housing (ARC-CAMP.H) at
sented in Fig. 9. The global priority of GFRP laminates containing dif- the University of Melbourne. The technical assistance from Ms Jinghan
ferent amounts of ceram is determined by multiplying its corresponding Lu during specimen testing is highly acknowledged.
local priorities and summing them as expressed in Eq. (7).
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