Effects of organophosphorus and mineral

based flame retardants on combustibility and

mechanical performances of natural fiber
reinforced composites
Pooria Khalili, Kim Yeow Tshai and Ing Kong
Faculty of Engineering, Department of Mechanical, Materials and Manufacturing Engineering,
The University of Nottingham Malaysia Campus, Selangor, Malaysia

Abstract
Purpose – The study aimed to investigate epoxy composites reinforced with mechanical performances, thermal decomposition and ignitibility of
natural fiber (NF) and doped with 5 wt.% of varying flame-retardant (FR) compounds. The incorporation of ammonium polyphosphate (APP) and
zinc borate (ZB) showed improvement in modulus and elongation to break compared to the empty fruit bunch-filled epoxy (control). However, slightly
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lower tensile and impact strengths were recorded in all FR-containing composites.
Design/methodology/approach – Among the FR-loaded specimens, enhancement in flexural property was observed in composites with APP,
whereas the addition of ZB and alumina trihydrate (ATH) resulted in the reduction of flexural strength. Thermogravimetric analysis results indicated
that the introduction of APP and ATH negatively impacted the thermal degradation temperature (Td) of the NF-filled composites. Greater mass
residue with FR-filled composites, where increment was in the range from 32-80 per cent compared to the control, was observed, with the greatest
being the ZB-containing formulation. Vertical Bunsen burner experiment revealed that the addition of ZB and APP led to a zero dripping flame
system, whereas such a phenomenon was absent in both the control and NF composites loaded with ATH. The bomb calorimeter results revealed
that addition of NF into neat epoxy significantly enhanced the FR behavior of the composite, and the gross heat of combustion was greatly reduced
when FRs were incorporated into the control sample.
Findings – Results from the current study concluded that non-halogenated FRs including APP, ZB and ATH were able to enhance the fire retardancy
of EFB epoxy composite without significantly deteriorate the mechanical behaviors.
Originality/value – It can be shown from scanning electron microscopy micrographs that the fabrication technique produced composites with good
interfacial adhesion between NF and epoxy matrix, and homogenous distribution of FRs were achieved.
Keywords Epoxy, Flammability and mechanical properties, ATH, APP, ZB, Palm fiber
Paper type Research paper

1. Introduction flame retardancy of composites has evolved as a crucial aspect for

The merits of using natural fiber (NF) as the reinforcing filler
in polymeric matrices are that these bio-derived sources are
abundantly available; are sustainable, recyclable, economically
non-abrasive and of low density; and possess highly specific
performance to weight ratio (Bakar et al., 2010; Tshai et al.,
2014, 2015). Over the past decade, bio-based fiber-reinforced
polymer composites have been utilized in a wide array of
industries, including, but not limited to, the upholstery,
automotive and food packaging (Rowell, 2006).
Nevertheless, the main disadvantage of NF-filled polymer
composites lies in its ease of ignitibility because the main
constituents – NFs and polymeric matrices – show high
flammability properties in nature. Therefore, enhancement in the
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fulfilling the safety specifications of the NF-based products
(Bakar et al., 2010). Among the many approaches available, one
of the main strategies to improve flame retardancy is to use
flame-retardant (FR) compounds into the polymeric matrix or
composite blend during fabrication process. Halogenated FRs
compounded with bromine and chlorine are among the available
additives. Nevertheless, these types of FRs are rarely used
because of their menace to the human and environment health.
The variants of FRs most broadly applied to bio-based
composites include mineral-based boron compounds, mainly
borates (Sain and Kokta, 1994; Sain et al., 1993) and metal
hydroxide types, such as alumina trihydrate (ATH), (Sain et al.,
2004; Wu et al., 1999) and those of organophosphorus-based
compound, such as ammonium polyphosphate (APP) (Li and
He, 2004).
Boron-based FRs are less toxic and cheaper alternatives to
antimony oxide (as a traditional FR) (Shen et al., 2008). Zinc

This work was supported in part by the Ministry of Science, Technology

World Journal of Engineering
13/3 (2016) 193–198 and Innovation (MOSTI), Malaysia, under Grant 03-02-12-SF0212 and
© Emerald Group Publishing Limited [ISSN 1708-5284] the Faculty of Engineering at The University of Nottingham Malaysia
[DOI 10.1108/WJE-06-2016-025] Campus.

193
 Effects of organophosphorus and mineral based flame retardants
Pooria Khalili, Kim Yeow Tshai and Ing Kong
borates (ZBs) have been used as a smoke suppressant and an
FR compound for polymers, where the intrinsic flame
retardation function can be contributed through hindrance of
oxygen’s entry to the underlying layers via the formation of a
porous borate surface coating and water release (Nelson,
1990). APP on the other hand is capable of producing a
thermal shielding layer from its reaction with carbonaceous
parts of the NF, leading to a retardation of further fire spread
(Samyn et al., 2007). Also, ATH, which is broadly used as a
metal hydroxide FR, can enhance the fire retardancy by
liberation of water and formation of a protecting charred layer
upon combustion.
In the current work, three of the most widely used FRs –
ZB, APP and ATH – were incorporated into NF-filled epoxy
composite, and their effects on the thermal–mechanical
properties and fire retardancy were investigated.
2. Materials and methods
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2.1 Materials
Pulverized oil palm empty fruit bunch (EFB) fibers with
average bundle diameter in the range of 100-200 ␮m and 10
mm in length were purchased from Szetech Engineering Sdn.
Bhd., Malaysia. APP phase II powder of trademark Exolit AP
422 with degree of polymerization being more than 1,000 was
provided by Clariant (Singapore) Pte Ltd. ATH with particle
size in microns and ZB 400 with particle size 3-5 ␮m were
provided by J.M. Huber Corporation, Malaysia branch. The
matrix system, an ambient cure two-part epoxy resin Ultimeg
U2020, was supplied by AEV Asia Sdn. Bhd., Malaysia. The
epoxy/hardener mixture has a specific viscosity of 1.1, and its
viscosity at 25°C was measured 0.2-0.6 Pa·s. The water based
formaldehyde-free crosslinked acrylate binding agent Acrodur
DS 3,530 was supplied by BASF Sdn. Bhd., Malaysia.
2.2 Preparation of fiber mats
Palm EFB fibers of 20 g were contained into a customized
rectangular sieve measuring 180 ⫻ 320 mm (length ⫻ width)
and then soaked in a mixture of water and Acrodur binder at
a 10:1 ratio. The sieve was gently vibrated to enhance fiber
distribution across the sieve, whereas the suspension was
mechanically stirred to enhance dispersion of the binding
agents in the aqueous medium. The wet fiber mat was taken
out from the water-binder suspension, and few minutes were
allowed for draining out the excess water. An assembly of
heavy metal plate, blotting papers and top load weighing of 10
kg was used to press out the remaining water. The fiber mats
were then kept for 24 h in an oven heated to 70°C to eliminate
the residual moisture.
2.3 Fabrication of FR-filled EFB epoxy composites
The FR and palm EFB-filled epoxy composite specimens
were prepared through vacuum resin infusion techniques.
Sonication was used to enhance the dispersion of the FR
microparticles in the epoxy matrix. The composition for each
of the constituent is given in Table I.
For FR-filled specimen, 5 wt.% of the three types of FRs
(ATH, ZB and APP) was separately added to the base epoxy
resin, and the mixture was exposed to sonication for a period
of 15 min with the aid of Hielscher UP400S ultrasonic
processor, operating at 20 kHz and the amplitude was tuned
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Volume 13 · Number 3 · 2016 · 193–198
Table I Composition of constituent materials
Wt.%
Sample Epoxy EFB ATH ZB APP
E 100 – – – –
EFB/E 82 18 – – –
EFB/E/ATH 77 18 5 – –
E/ZB 77 18 – 5 –
E/APP 77 18 – – 5
Notes: E ⫽ neat epoxy; EFB ⫽ empty fruit bunch fiber
to 50 per cent. Stoichiometric amount of hardener (20 parts
hardener to 100 parts base epoxy resin by mass as
recommended by the manufacturer) was added to the
sonicated volume. The mixture was left to de-gas for 10 min
prior to infusion.
A custom-built mold was used for the fabrication of the FR
EFB-filled epoxy composite. To obtain a flat top specimen
surface and uniform thickness, a cut to dimension peel ply,
infusion mesh, thin aluminum plate and vacuum bagging were
aligned in sequence on top of the dried fiber mat such that a
more even compression pressure could be achieved during
vacuum-assisted resin infusion. An initial procedure was
performed to ensure that the system is leakage free, i.e. full
vacuum condition could be established; the catalyzed epoxy
FR mixture was infused into the mold, where the flow path of
the mixture was guided by a series of spiral tubing to achieve
full wetting of the dried fiber mat. Curing of the composite
was allowed for 24 h under ambient conditions (humidity and
temperature). The cured FR-filled EFB epoxy composites
were removed from mold and cut into dedicated specimens
size for mechanical, thermal and combustion analyses.
2.4 Characterization of mechanical properties
A bench type tensile machine Lloyd Instruments LR50K Plus
was used to characterize the tensile and flexural properties of
the composites. The tensile and flexural experiments were
conducted in accordance to the ASTM D3039/3039M and
ASTM D790 standards, respectively. A constant crosshead
speed of 2 mm/min was applied to the tensile specimens
measuring 120 ⫻ 20 ⫻ 2 mm (length ⫻ width ⫻ thickness).
Flexural samples having dimensions 100 ⫻ 20 ⫻ 2 mm
(length ⫻ width ⫻ thickness) were subjected to a uniform
crosshead speed of 5 mm/min at mid-point over a span length
of 60 mm. The impact strength was tested on rectangular
specimens of 63.5 ⫻ 12.7 ⫻ 2 mm in accordance to ASTM
D6110 standard with the aid of MH-358 Charpy Impact
Tester. Three samples from each material composition were
tested and the average value of the respective property was
analyzed.
2.5 Characterization of thermal properties
A Mettler-Toledo simultaneous TGA/DSC 1 instrument was
used for characterization of the thermal properties. Sample
weighing of 10-15 mg placed within an open alumina crucible
was heated from room temperature to 600°C at a constant
20°C/min ramp, and the assembly was maintained under
nitrogen environment supplied at 20 ml/min. Three tests were
performed for each formulation, and the average thermal
 Effects of organophosphorus and mineral based flame retardants
Pooria Khalili, Kim Yeow Tshai and Ing Kong
degradation curve (in percentage weight loss) plot against
temperature variation was analyzed.
2.6 Characterization of combustibility properties
A bomb calorimeter PARR 6100 was used to characterize the
gross heat of combustion (GHC) of the composite specimens
in accordance to ASTM D-240 standard. The dedicated fuse
wire was positioned such as it touched the top surface of the
solid specimen fragment for combustion to occur. In all cases,
a specimen fragment of less than 1 g was used.
2.7 Characterization of flammability properties
Vertical burn tests were set up in accordance with the
specification of Federal Aviation Regulation (FAR) 25.853
12s vertical burn test standard. Rectangular specimen
equivalent to half of the standard FAR dimension, measuring
152.5 ⫻ 37.5 ⫻ 2 mm, were vertically suspended by a clamp
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on a lab stand. A natural gas Bunsen flame was applied to the
leading edge of the bottom specimen surface for a period of 12
s and then detached. The flame time, drip flame time and final
mass loss (%) were recorded.
2.8 Characterization of morphological properties
A FEI Quanta 400F field emission scanning electron
microscopy (FESEM) was used for the analysis of specimen
surface topography. The fractured surface of composite
specimens was mounted upright, and scannings were
performed under accelerating voltage of 20 kV and
low-vacuum environment.
3. Results and discussions
3.1 Mechanical performances
The measured tensile strength, modulus and elongation to
break of the EFB-filled epoxy composites containing various
types of FR are summarized in Table II.
It can be observed that addition of ATH and APP FRs
resulted in a much reduced tensile strength, whereas the
incorporation of ZB produced a relatively similar response
with that of the control (i.e. composite without FR). The
percentage drop in tensile strength for ATH- and APP-loaded
composites was approximately 19 and 21 per cent,
respectively. Typical with additives, the inclusion of FR into
polymeric matrices generally resulted in deterioration of the
tensile performances, which can be attributed to the weakened
mechanical interlocking between the EFB and epoxy matrix as
a consequence of the present of FR (Kurt and Mengeloğlu,
2011; Shen et al., 2008). However, such an effect appeared to
be less significant with ZB. The measured modulus and
elongation to break indicated that E/APP and E/ZB
formulations tend to produce much higher values compared to
E/ATH and the control.
Table II Tensile properties of EFB-filled epoxy composites with ATH, APP and ZB
Sample Tensile strength (MPa)
EFB/E 32.62
E/ATH 26.39
E/APP 25.60
E/ZB 31.26
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Figure 1 reveals the flexural properties of the composite
specimens. As observed, the inclusion of FR caused a negative
effect on the flexural behavior of the composites, where the
flexural strength and strain decreased for ATH- and ZB-filled
composites, ascribed to the poor wettability of the epoxy resin
in the present of FR. However, the E/APP formulation
demonstrated better flexural strength relative to other
formulations.
The impact behavior of neat epoxy, EFB/E and FR-filled
compositions are exhibited in Figure 2.
It can be seen that addition of EFB fibers provided a
reinforcing effect in terms of the impact strength of the
composite contributed by the establishment of good interfacial
adhesion between the EFB fiber and epoxy resin. Inclusion of
FRs however reduced the impact strength; in general, the
FR filler disturbed the epoxy continuity, acting as a
stress-concentrated site, and as a result, prone to the initiation
of micro-crack (Mareri et al., 1998).
3.2 Thermal properties
Thermogravimetric analysis (TGA) curves of the composites
with varying formulation are depicted in Figure 3. The mass
residue at 600°C and the thermal degradation temperature
(Td) corresponding to 50 wt.% mass loss, i.e. at peak DTG,
are shown in Table III.
The composites were thermally stable up to approximately
300°C where the main decomposition took place. The
ZB-loaded composite showed the best thermal properties
relative to other FR-based composites and the control. In
terms of the thermal degradation, it can be observed that the
Td for ZB-containing composite increased by about 4°C
compared to the control. Furthermore, the residual mass of
ZB-loaded composite at 600°C was found to be approximately
80 per cent greater than the control. The results imply that the
ZB additive is much superior in enhancing thermal behavior of
the composite at an elevated temperature and is capable of
forming a large quantity of residue. Such phenomena could be
attributed to the formation of a glassy insulating layer, which
dilutes combustible gases, and also the reaction of ZB residue
with hydroxyl (OH) functional group of natural fiber, such as
hemicelluloses and celluloses, produces extra amount of water
vapor, which contributes to the improved char formation
(Khelfa et al., 2008).
Overall, the residue attained increased with the
incorporation of FRs relative to the control. ATH and APP
generate alumina (metal oxide) and ammonia (phosphoric
acid), respectively, throughout their reactions with EFB
and epoxy resin, leading to the formation of a charred
barrier layer against thermal decomposition, insulting the
substrates (Bourbigot et al., 2006). Neat EFB fiber showed
a large amount of residue, mainly because of the presence of
lignin constituents that are highly thermally stable, and
Modulus (GPa) Elongation to break (%)
2.53 4.05
2.42 3.87
3.12 4.33
3.13 5.62
 Effects of organophosphorus and mineral based flame retardants World Journal of Engineering
Pooria Khalili, Kim Yeow Tshai and Ing Kong Volume 13 · Number 3 · 2016 · 193–198

Figure 1 Flexural behavior of the composites Figure 4 Bunsen burner test observations of the composite
specimens
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their thermal decomposition resulted into a large quantity

of char residual.
Figure 2 Impact behavior of the composites
3.3 Combustibility properties
Figure 4 exhibits the observations from the vertical Bunsen
burn tests, which provide further qualitative observations of
fire spread and pyrolysis on the composites.
The results showed comparable mass loss pattern to that of
the TGA for FR-filled composites, where ZB followed by
APP-loaded composites demonstrated higher mass residue
relative to the ATH containing formulation. With regard to
the drip flame time, ZB- and APP-based compositions did not
generate any dripping, whereas ATH and EFB/E recorded
dripping for approximately 25 and 55 s, respectively. This
indicated that ZB and APP provide greater effect on reducing
ignitibility behavior of the EFB epoxy composites. ATH-filled
Figure 3 TGA curves of the composites composite was observed to burn more rigorously than other
FR-based samples, where an approximately 4 min flame time
and dripping were recorded, suggesting that ATH is poorer in
restricting the liberation of flammable gases during the event
of fire. Furthermore, APP- and ZB-loaded composites
maintained the physical integrity and shape throughout
the combustion, whereas the control and ATH-containing
samples experienced shrinkage and warp, resulting in the loss
of their original structure.
The large drip flame time for EFB/E was owing to an
increasingly deteriorating NF network, which was not
protected by the dilution of ignitable oxidizable gases via ZB
and APP-containing formulations. This resulted in extensive
pyrolysis of the EFB/E sample and consequently accelerated
the burning progression, increasing the dropped parts.
The flammability behaviors were also investigated with a
bomb calorimeter instrument, where gross heat release and
fire decomposition were analyzed. Figure 5 showed the GHC
Table III Thermogravimetric analysis (TGA) data under nitrogen
atmosphere
of the formulation with varying FR additives.
The neat epoxy specimen E100 demonstrated the highest
Sample name Char residual at T600 (wt.%) Td (°C) GHC owing to its inherent nature to flammability. Addition of
EFB/E (control) 15.56 385.87 EFB fibers into epoxy significantly dropped the GHC from
E/ATH 20.47 383.37 about 35 to 31.8 MJ/kg.
E/APP 21.41 376.784 Incorporation of FRs had a considerable positive effect of
E/ZB 27.92 389.49 reducing the GHC of the EFB epoxy composites, which is
Nest EFB fiber 30.72 346.864 favorable to fire retarding performance. The enhanced fire
retardancy could be related to the shielding char layer formed

196
 Effects of organophosphorus and mineral based flame retardants
Pooria Khalili, Kim Yeow Tshai and Ing Kong
by the presence of ATH, APP and ZB. ATH and ZB is
capable of producing metal oxide, whereas APP forms
phosphorous acid. In addition, the FR investigated in the
current work has the tendency to generate water vapor from
their thermal decomposition. Water absorbs the heat released
by combustion and reduces the amount of flammable gases in
the combustive zone, thereby improving the formation of char.
Figure 5 Gross heat of combustion
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Figure 6 SEM micrograph of the composites
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3.4 Combustibility properties
The tensile fractured surfaces were subjected to scanning
electron microscopy (SEM). The SEM micrographs of the FR
formulations are illustrated in Figure 6.
The image shown in Figure 6(a) revealed establishment of
good bonding between EFB fiber and epoxy matrix.
Moreover, the micrographs in Figure 6(b-d) showed good
dispersion of ATH, APP and ZB within the epoxy, which
indicated the good compatibility between FRs, EFB and
epoxy polymer.
4. Conclusions
Results from the current study concluded that non-halogenated
FRs, including APP, ZB and ATH, were able to enhance the fire
retardancy of EFB epoxy composite without significantly
deteriorating the mechanical behaviors. The tensile strength of
ATH- and APP-loaded composites were reduced by
approximately 19 and 21 MPa, respectively, in comparison with
the neat EFB epoxy composite (control), whereas elongation at
break and modulus were improved with the addition of APP and
ZB particles. The flexural and impact strength of FR-based
composites seem to reduce compared to the control, with the
exception for the APP-containing sample, which was found to
experience enhancement by around 35 per cent. The reason for
such improvement merit further investigation.
 Effects of organophosphorus and mineral based flame retardants
Pooria Khalili, Kim Yeow Tshai and Ing Kong
Upon the event of fire, the char formed among EFB, FR
and epoxy was found capable of inhibiting the mass and heat
transfer into the bulk of the substrate, leading to larger mass
residue as evident from TGA, the reduced GHC and zero
molten drip flame for ZB- and APP-filled composites. In
general, NF and FRs contributed to the improvement in
thermal properties and fire retardancy of epoxy polymer.
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Corresponding author
Pooria Khalili can be contacted at: pooria.khalili@gmail.com