coatings

Article
Preparation of Intumescent Fire Protective Coating for
Fire Rated Timber Door
Jessica Jong Kwang Yin 1 , Ming Chian Yew 1, * , Ming Kun Yew 2 and Lip Huat Saw 1
1 Department of Mechanical and Material Engineering, Lee Kong Chian Faculty of Engineering and Science,
University of Tunku Abdul Rahman, Cheras, Kajang 43000, Malaysia; jessicajong727@gmail.com (J.J.K.Y.);
sawlh@utar.edu.my (L.H.S.)
2 Department of Civil Engineering, Lee Kong Chian Faculty of Engineering Science,
University of Tunku Abdul Rahman, Cheras, Kajang 43000, Malaysia; yewmk@utar.edu.my
* Correspondence: yewmc@utar.edu.my or yewmingchian@gmail.com; Tel.: +6-039-086-0288




Received: 29 June 2019; Accepted: 24 October 2019; Published: 6 November 2019


Abstract: Intumescent flame-retardant coating (IFRC) provides a protective barrier to heat and
mass transfer for the most efficient utilization of a wide variety of passive fire protection systems at
the recent development. This article highlights the fire-resistance, physical, chemical, mechanical,
and thermal properties of the IFRC using a Bunsen burner, furnace, Scanning Electron Microscope,
freeze-thaw stability test, Instron Micro Tester, and thermogravimetric analysis (TGA) test. The five
IFRC formulations were mixed with vermiculite and perlite for the fabrication of fire-resistant timber
door prototypes in this research project. Additionally, the best fire-resistance performance of the
fire-rated door prototype was selected and compared with a commercial prototype under the fire
endurance test. An inventive fire-rated door prototype (P2), with a low density of 636.45 kg/m3 ,
showed an outstanding fire-resistance rating performance, resulting in temperature reduction by up
to 54.9 ◦ C, as compared with that of the commercial prototype. Significantly, a novel fire-rated timber
door prototype with the addition of formulating intumescent coating has proven to be efficient in
preventing fires and maintaining its integrity by surviving a fire resistance period of 2 h.

Keywords: fire protection system; filler; fire rated timber door; flame retardant additives;
intumescent coating

1. Introduction
There are two kinds of fire protection systems in buildings, active and passive fire protection
systems, which are an integral part of any modern-day building to protect lives and assets by enhancing
the fire prevention and protection techniques [1]. The active fire protection system includes a fire
or smoke alarm, sprinkler, and fire extinguishers. However, this system has required some actions
to work efficiently in the event of a fire and this might fail due to lack of maintenance or other
possible problems such as frozen pipes and inadequate water pressure. Whereas passive fire protection
(PFP) system includes fire or smoke dampers, fire doors, and firewalls. This PFP system plays an
essential role to provide fire safety protection by using flame-retardant materials. Therefore, with
regards to this research, a new and innovative fire-resistant timber door is incorporated with the
intumescent flame-retardant coating (IFRC) that acts as an effective PFP system and its potential
application for lightweight fire-rated timber door. The intumescent coating reacts under the influence
of fire and swells in a controlled manner to many times its original thickness, and thus produces an
insulation carbonaceous char or foam that protects the substrate from the effects of the fire [2]. By such
effectiveness, intumescent coating plays a critical role in protecting the building, and it may also gain

Coatings 2019, 9, 738; doi:10.3390/coatings9110738 www.mdpi.com/journal/coatings

Coatings 2019, 9, 738 2 of 18

extra time for building occupants to escape safely during the outbreak of fire by trapping the fire and
smoke as well as insulating the heat.
IFRCs can either be coated as a thin film or act as a binder of PFPs to enhance the fire-resistance
performance. Boards are rigid prefabricated materials that usually come along with hydraulic
binders [3]. Common fire doors are made of magnesium oxide boards, gypsum boards and even heavy
timber wood [4–6]. However, there is one common problem in all the existing commercial fire doors
which is their high density [7]. According to Fire Industry Association, due to the sheer weight and
force produced when the heavy fire doors are opened and closed (density > 1200 kg/m3 ) [8], it may
cause human injury especially in places such as residential care or nursing homes.
In this research study, intumescent coatings and lightweight flame-retardant materials such as
vermiculite and perlite are used to construct the lightweight fire-resistant timber door prototypes
(density is about 600 ± 50 kg/m3 ) for 2-h fire rating. Intumescent paint is the recent trend in fire
retarding products in construction building materials because of its many beneficial properties such
as providing low-odor, lightweight, and is environmentally friendly. Exhaustive investigations have
revealed that the intumescent flame retardant coating has achieved good flammability and physical
and chemical performances though many linger widely on steel structure applications [9–12]. Up to
today, the performance of fire-resistant boards has yet to be tested and investigated with the addition
of intumescent fire protective coating for the development of a fire-resistant timber door. Furthermore,
this research project has also highlighted huge potential for incorporating the intumescent coating
composites, which consists of three main flame-retardant additives, namely ammonium polyphosphate
(APP), an acid source; pentaerythritol (PER), a carbon source; and melamine (MEL), blowing agents,
into the fire door. These are mixed in a weight ratio of 2:1:1 and are bonded together with flame
retardant fillers and vinyl acetate (VA) copolymer as well as vermiculite and perlite which react together
to form a protective thermal barrier at high temperature in fire doors [13]. It is important to note
that flame-retardant additives are useful chemical compounds for fire retardant to provide varying
degrees of flammability protection. A research study conducted by Xia and his co-workers has stated
that adding too much APP into the intumescent formulation may reduce the mechanical properties
of the intumescent coating. Hence, an appropriate ratio of APP/PER/MEL should be set prior to the
development of intumescent coating [14]. One of the ingredients, titanium dioxide (TiO2 ), is important
to formulate an intumescent coating in which it does not only provide the usual properties of colour
and opacity, but it also likely takes place in the intumescence process which stabilizes the insulating
foam at high temperatures when most of the carbon oxidizes and burn off [15]. Besides that, polymer
binder is also one of the final key materials to produce a uniform cellular structure to provide good
thermal insulation. In a research study conducted by Wang and Yang, the influence of the binder, vinyl
acetate (VA), copolymer emulsion in the water-based coating is used to minimize the smoke and toxic
fume emission without compromising the quality and effectiveness of the intumescent coating in fire
protection [16].
In addition to that, vermiculite and perlite act as flame-retardant materials promoting a very low
density, high porosity, good thermal insulation properties, chemical inertness, and good fire-retardant
materials. This makes them attractive to be used widely as pore-forming additives for heat insulation
applications [17]. Moreover, the uniqueness of the materials can insulate the heat from the fire by
expanding with small particles under high temperatures. Besides that, a highly porous aggregate
that can absorb moisture in varying degrees, the presence of moisture in the aggregate would
turn into steam and evaporate from the materials during a fire test, and this will extend the fire
duration [18]. As mentioned, the performance of the IFRC is based on the appropriate materials
combination and the compatibility of the flame-retardant fillers with a polymer binder. Therefore, it is
essential that the flame-retardant fillers provide good fire protective performance and fire retarding
efficiency properties [19,20]. The grouping of aluminium hydroxide, Al(OH)3 ; calcium silicate, CaSiO3 ;
magnesium hydroxide, Mg(OH)2 ; chicken eggshell (CES) powder (bio-filler derived from CES waste);
and calcium carbonate, CaCO3 is used in this research project [20]. This project aims to formulate an
Coatings 2019, 9, 738 3 of 18

appropriate combination of intumescent flame-retardant coating for the development of fire-resistant

timber door prototype. The performances of fire protection, mechanical, chemical and physical
properties of intumescent flame-retardant coatings are evaluated and investigated. This research work
is intended to design, fabricate, and examine the fire-resistant timber door prototype by incorporating
intumescent fire-protective coating in order to fulfil the 2-h fire rating.

2. Experimental Program

2.1. Materials and Sample Preparation

The first part of this project is to synthesize the water-based intumescent paint using a high-speed
disperse mixer for 30 min at room temperature until it is completely homogenous. The formulations
of intumescent coatings are tabulated in Table 1. APP, PER, and MEL were used as flame-retardant
additives. The aluminium hydroxide, magnesium hydroxide, calcium silicate, chicken eggshell (CES)
powder, calcium carbonate, and titanium dioxide were used as flame-retardant fillers, and vinyl acetate
(VA) copolymer emulsion acts as a water-based polymer binder in this study. The fire resistance and
physical properties of the intumescent coatings were characterized and assessed through a series
of tests such as Bunsen burner test, furnace test, scanning electron microscope (SEM) analysis test,
adhesion strength test, freeze-thaw cycle test, and thermogravimetric analysis (TGA) test.

Table 1. Specifications of experimental materials.

Ingredients (wt.%)
Samples
Flame-Retardant
Flame Retardant Additives Filler Flame-Retardant Fillers
(Pigment)
Vinyl
Acetate (VA)
APP PER MEL TiO2 Al(OH)3 Mg(OH)2 CaSiO3 CES CaCO3
Copolymer
Emulsion
J1 20 10 10 50 4.0 3.0 – 3.0 – –
J2 20 10 10 50 4.0 3.0 – – 3.0 –
J3 20 10 10 50 4.0 – 3.0 3.0 – –
J4 20 10 10 50 4.0 – 3.0 – 3.0 –
J5 20 10 10 50 4.0 – 3.0 – – 3.0

The second part of this project is to design and fabricate the fire-resistant timber door prototype
with a dimension of 300 mm (length) × 300 mm (width) × 40 mm (thickness). The fire protective
performance of the fire timber door prototype is determined through a small-scale fire test. Table 2
shows the details of the experimental prototypes.

Table 2. Details of experimental prototypes.

Fire Door Prototype

Dimensions: 300 mm (L) × P1 P2 P3 P4 P5
300 mm (W) × 40 mm (H)
Weight (g) 2565 2578 2589 2605 2610
Density (kg/m3 ) 633.44 636.45 639.23 643.22 644.52

Moreover, the fire endurance test and the temperature rise test are conducted to compare and
determine the best fire timber door prototype as compared to the commercial prototype in terms of
heat transmission and integrity failure or a significant leakage. The flow chart of the experimental work
details and the engineering drawing of the fire-resistant timber door prototype as well as thermocouple
locations (T1 and T2) are shown in Figure 1.
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Part 1: Sample characterization of IFRC

• Bunsen burner test

Part 2: Prototype testing
• Furnace test
Sample
• Scanning Electron Microscopy
preparation  Small scale fire test
(SEM) test
• Fire endurance test
• Adhesion strength test
• Temperature rise test
• Freeze-thaw cycle test
• Thermogravimetric analysis
(TGA) test

Figure1.1.Flow
Figure Flowchart
chartof
of the
the experimental
experimental work and
and the
the dimensions
dimensionsof
ofthe
theprototype.
prototype.

2.2.
2.2.Testing
Testingfor
forCoated
CoatedSamples
Samples
2.2.1. Bunsen Burner Test
2.2.1. Bunsen Burner Test
The coating samples were coated on a 100 mm × 100 mm × 3 mm steel plate with a thickness of
The coating samples were coated on a 100 mm × 100 mm × 3 mm steel plate with a thickness of 2
2 ±± 0.2
0.2 mm.
mm. TheThethermocouple
thermocoupleplateplateis isattached
attachedatatthe
thebackside
backsideofofthe
thesteel
steelplate
platecoated
coatedwithwith
intumescent flame-retardant coating and then connected to a digital handheld
intumescent flame-retardant coating and then connected to a digital handheld thermometer for thermometer for
temperature
temperaturemeasurement.
measurement. Figure
Figure 22 shows
shows the the experimental setupof
experimental setup ofthe
theBunsen
Bunsenburner
burnertest
testfor
forthe
the
coated
coated samples. The sample was exposed to a Bunsen burner flame spray gun blow torch for 1 h at a a
samples. The sample was exposed to a Bunsen burner flame spray gun blow torch for 1 h at
temperature ◦ C. The Bunsen burner gas consumption is about 160 g/h and the
temperatureflame
flameofofabout
about1000
1000 °C. The Bunsen burner gas consumption is about 160 g/h and the
distance
distancebetween
betweenthe
thesample
sampleand
andBunsen
Bunsenburner
burner nozzle
nozzle is
is about
about 77 cm.
cm.
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Figure 2. Schematic of the experimental

Figure 2. experimental setup
setup for
for coated
coated samples.
samples.

2.2.2.
2.2.2. Furnace
Furnace Test
Test
For
For the
the furnace
furnace test,
test, all
all steel
steel plates
plates (dimensions:
(dimensions: 50 mm ×× 50
50 mm mm ×
50 mm × 11 mm)
mm) were
were coated
coated with
with
IFRCs with a thickness of 2 ± 0.2 mm. The coated samples were then
IFRCs with a thickness of 2 ± 0.2 mm. The coated samples were then placed into the furnace placed into the furnace
(Barnstead
(Barnstead Thermolyne
Thermolyne62700,
62700,Barnstead
BarnsteadThermolyne,
Thermolyne,Dubuque,
Dubuque, IA,IA,
USA)
USA)with high
with temperatures
high temperaturesof
500 and 600 ◦ C, respectively (heating rate is 20 ◦ C/min). After that, the thickness of the char layer for
of 500 and 600 °C, respectively (heating rate is 20 °C/min). After that, the thickness of the char layer
each sample
for each was was
sample measured. Up toUp
measured. date, there there
to date, is no standard test to test
is no standard study tothe strength
study of a charofsample.
the strength a char
In
sample. In this experimental work, a small-scale compressive strength of char test wasand
this experimental work, a small-scale compressive strength of char test was designed conducted
designed and
by
conducted by stacking up the 50 g coin-shape metals one by one, which acts as a static load on for
stacking up the 50 g coin-shape metals one by one, which acts as a static load on the char layer the
measuring
char layer forandmeasuring
evaluatingandtheevaluating
char strength
theof thestrength
char sample. of the sample.

2.2.3. Scanning Electron Microscopy (SEM) Analysis

2.2.3. Scanning Electron Microscopy (SEM) Analysis
For SEM examination/analysis, all samples are initially coated with gold in order to eliminate
For SEM examination/analysis, all samples are initially coated with gold in order to eliminate
the possible charging effects. A low beam energy with 1 kV is conducted to decrease the possibility
the possible charging effects. A low beam energy with 1 kV is conducted to decrease the possibility
of any thermal damage to the samples. The main objectives of the SEM analysis are to conduct a
of any thermal damage to the samples. The main objectives of the SEM analysis are to conduct a
detailed examination using Hitachi EDAX S3400–N Scanning Electron Microscopy (SEM) machine
detailed examination using Hitachi EDAX S3400–N Scanning Electron Microscopy (SEM) machine
manufactured by Hitachi High Technologies America, Inc. in America and analysis on the IFRC
manufactured by Hitachi High Technologies America, Inc. in America and analysis on the IFRC
coating samples’ morphology and thus to determine and identify the interfacial bonding of each type
coating samples’ morphology and thus to determine and identify the interfacial bonding of each
of coating sample on the steel substrate.
type of coating sample on the steel substrate.
2.2.4. Adhesion Strength Test
2.2.4. Adhesion Strength Test
Figure 3 shows the experimental setup for the measurement of adhesion strength of the coating
Figure
samples. The3 samples
shows the experimental
were coated with setup for the measurement
a thickness of 2 ± 0.2 mm of adhesion
IFRC on onestrength
side of theof the coating
cylindrical
samples. The samples were coated with a thickness of 2 ± 0.2 mm IFRC on one side of the
steel rod. After that, the coated cylindrical steel rod was then attached to a bare cylindrical steel rodcylindrical
steel rod.
using After glue
an epoxy that,with
the coated cylindrical
a thickness of 2 ± steel rod Two
0.2 mm. was cylindrical
then attached
steeltorods
a bare
werecylindrical
then testedsteel rod
using
using
the an epoxy
Instron Microglue with a thickness
Tester–Universal of 2 ±machine
Testing 0.2 mm. Two cylindricalbysteel
manufactured rodsin
Instron were then tested
Norwood, MA,using
USA
the Instron Micro Tester–Universal Testing machine manufactured by Instron in
with a constant rate of 1 mm/min continually drawn apart in tensile mode until the coating samplesNorwood, MA,on
USA with a constant rate of 1 mm/min continually drawn apart in tensile mode until
the cylindrical steel rods tore apart. The adhesion strength of the coating sample in MPa is calculated the coating
samples
based on on
thethe cylindrical
following steel rods
Equation tore apart. The adhesion strength of the coating sample in MPa
(1) [21]:
is calculated based on the following Equation (1) [21]: F
fb = (1)
A (1)
 
strength (MPa);; F =maximum load at rupture
maximum load at ruptureN(N 2
where, fb = adhesion
where, adhesion strength ; ); Aadhered area
= adhered area mmmm . .
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Figure 3.
Figure Schematic of
3. Schematic of the
the experimental
experimental setup
setup for
for adhesion
adhesion strength.
strength.

2.2.5. Freeze-Thaw Cycle Test

2.2.5. Freeze-Thaw Cycle Test
The freeze–thaw resistance test was used to determine the ability of the coating sample to
The freeze–thaw resistance test was used to determine the ability of the coating sample to
withstand the highly destructive forces of cyclic freezing and thawing. The coating samples were
withstand the highly destructive forces of cyclic freezing and thawing. The coating samples were
coated onto different sets of 50 mm × 50 mm × 1 mm steel plates with a thickness of 2 ± 0.2 mm. The
coated onto different sets of 50 mm × 50 mm × 1◦mm steel plates with a thickness of 2 ± 0.2 mm. The
coating samples were placed in an air flow at 25 C for 8 h and then placed in the freezer at −20 ◦ C for
coating samples were placed in an air flow at 25 °C for 8 h and then placed in◦the freezer at −20 °C for
another 8 h. Lastly, the coating samples were heated in a drying oven at 50 C for another 8 h. This
another 8 h. Lastly, the coating samples were heated in a drying oven at 50 °C for another 8 h. This
process is noted as a freeze–thaw cycle period [22].
process is noted as a freeze–thaw cycle period [22].
2.2.6. Thermogravimetric Analysis (TGA) Test
2.2.6. Thermogravimetric Analysis (TGA) Test
Thermogravimetric analysis (TGA) was carried out using Perkin Elmer STA8000 model
Thermogravimetric
manufactured by Perkin analysis (TGA)
Elmer Inc., was carried
Waltham, MA, USA. out Test
using Perkinwith
samples ElmeraboutSTA8000
5–8 mgmodel
thick
manufactured by Perkin Elmer Inc., Waltham, MA, USA. Test samples
◦ with about
thin films were placed in a crucible and heated from 30 to 1000 C at a heating rate of 20 C/min under 5–8 mg
◦ thick thin
films were
nitrogen gas. placed in a crucible and heated from 30 to 1000 °C at a heating rate of 20 °C/min under
nitrogen gas.
2.2.7. Testing for Fire Resistant Timber Door Prototype
2.2.7. Testing for Fire Resistant Timber Door Prototype
• Small Scale Fire Test
• Small Scale Fire Test
The small-scale fire test was conducted on prototype 1–5; the intumescent binders for each
The small-scale
prototype, which is based fire test was
on the conductedJ1–J5
formulation on prototype 1–5; the
that is provided intumescent
in Table binders
1, is shown for each
in Section 2.1.
prototype, which
After that, the fireisprotection
based on performance
the formulation J1–J5
of the that is provided
prototypes was testedin Table
using1,theis Bunsen
shown in Section
burner at
2.1. After that,
◦ the fire protection performance of the prototypes was tested using the
about 1000 C for 2 h. The temperature profile of the backside of the fire-resistant timber door prototypeBunsen burner
at
wasabout
Coatings 1000
2019,
measured 9, x °C
andfor
FOR 2 h.
PEER Theusing
REVIEW
recorded temperature profile of thermometer.
a digital handheld the backside of the fire-resistant
Figure timber 7door
4 shows a small-scale of 20
fire
prototype was measured
test experimental setup forand recorded using
the fire-resistant a digital
timber handheld thermometer. Figure 4 shows a
door prototype.
small-scale fire test experimental setup for the fire-resistant timber door prototype.

Schematic of
Figure 4. Schematic of the
the experimental
experimental setup for fire-resistant timber door prototype.
Coatings 2019, 9, 738 7 of 18
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•• Fire
FireEndurance
Enduranceand
andTemperature
Temperature Rise
Rise Tests
Tests forfor
thethe Timber
Timber Door
Door Prototype
Prototype
The fire
fire endurance
endurancetest testwaswascarried
carriedout
outusing
using thethe
Bunsen
Bunsen burner
burner to determine
to determine andand
compare
comparethe
fire-resistance
the fire-resistancerating andand
rating integrity of of
integrity thethebest
bestprototype
prototypeand andcommercial
commercialprototype.
prototype. ForFor the
the fire
endurance test, the tested prototype
prototype can be qualified as a standard fire-rated timber door if it can
maintain its integrity when exposed to 2 h fire (at about 1000 ◦°C) C) without an integrity failure or
displaying a significant leakage [23]. Whereas, Whereas, the the temperature
temperature rise rise is also recorded over a 30-min
interval until
until120-min,
120-min,this thisisistoto
examine
examine thethe
heat riserise
heat on the backside
on the of the
backside offire-resistant timber
the fire-resistant door
timber
prototype. The thermocouples
door prototype. The thermocouples are fixed at two
are fixed at twopoints
pointsof of
the
thefire-resistant
fire-resistanttimber
timberdoor
door prototype
(centre (T1) and edge (T2)) to measure the transmission of heat from one point to another point of the
prototype. This
prototype. This isisto
toensure
ensurethatthatthe
the prototype
prototype hashas taken
taken adequate
adequate firefire protection
protection by reducing
by reducing the
the heat
heat transmission
transmission rate andrateflame
and flame propagation
propagation so thatso thatprolong
it can it can prolong the evacuation
the evacuation timebuilding
time for the for the
building
occupantsoccupants
if there isifa there
fire. is a fire.

3. Experimental Results and Discussion on Findings

3.1. Bunsen
3.1. Bunsen Burner
Burner Test
Test
The purpose
The purpose ofofthis
thisspecified
specifiedtest
testis is
to to
characterize thethe
characterize physical andand
physical chemical reactions
chemical of theofchar
reactions the
formation of the IFRC. The temperature profiles of the steel plates coated with
char formation of the IFRC. The temperature profiles of the steel plates coated with five IFRCfive IFRC formulations
(J1–J5) and the(J1–J5)
formulations bare steel
andplate
the were
barecompared
steel plateafter
were60 min of fire testing.
compared after 60Inmin
this experimental work,
of fire testing. the
In this
temperature of 400 ◦ C was chosen as the critical temperature for the coated sample with IFRC [24]. The
experimental work, the temperature of 400 °C was chosen as the critical temperature for the coated
fire protection
sample results
with IFRC of the
[24]. Thecoated steel platesresults
fire protection were then plotted
of the coated assteel
a function
platesofwere
timethen
and presented
plotted asin a
Figure 5.
function of time and presented in Figure 5.

450
Critical temperature (400 ℃)
400

350 J5

J3
Temperature (℃)

300
J4
250
J1
200 J2

150

100

50

0
0 10 20 30 40 50 60
Time (min)
Critical temperature Coating J1 Coating J2
Coating J3 Coating J4 Coating J5

Figure
Figure 5.
5. Evolution
Evolution of
of temperature
temperature on
on the
the coated
coated steel
steel plates.
plates.

The thickness of the char layer and equilibrium temperature of the intumescent coatings with
the influences of different types of flame-retardant fillers are shown in Table
Table 3.
3. The first 10 min have
showed that there is a similar pattern of temperatures for the coated samples, which is is below
below 300 ◦ C.
300 °C.
After that, the temperatures started to fluctuate at 20 min due to the physical and chemical reactions
of the coating formulations during the high-temperature test. The temperature continuescontinues to rise for
30 min, it is observed that the coating J5 starts to rapidly increase until reaching 360 °C at 42 min. This
may possibly be due to the fact this coated sample has started to lose its adherence strength or
Coatings 2019, 9, 738 8 of 18

30 min, it is observed that the coating J5 starts to rapidly increase until reaching 360 ◦ C at 42 min.
This may possibly be due to the fact this coated sample has started to lose its adherence strength or
interfacial bonding from the steel plate during the fire test. Whereas coating J1 drops rapidly after
reaching 205 ◦ C at 43 min, this might due to the reduction of gas pressure from the Bunsen burner
flame spray gun blow torch.

Table 3. Thickness of char layer and the equilibrium temperature of coated samples.

Coating Samples Thickness of Char Layer (±0.1 mm) Equilibrium Temperature of Coating (◦ C)
Original Steel Plate – >Critical Temperature (400 ◦ C)
J1 5.8 238
J2 6.0 217
J3 2.8 306
J4 3.8 279
J5 4.3 325

It is also observed that the temperature of all the coatings starts to fluctuate again until reaching
50 min. After 50 min of the test, the temperature reaches an equilibrium value and almost remains
unchanged until the last stage of the test. The equilibrium temperature of coating J2 that is 217 ◦ C is
considered to be significantly lower than the other coatings and thus it has showed to have the best
result for fire protective performance. The char combined the positive effects of the flame retardant
additives, intumescent paint and fillers (3 wt.% of Al(OH)3 and CES), promoting a good fire-protective
barrier and producing the thickest and most excellent char layer (i.e. about 6.0 mm) to block the fire
while safeguarding the formation of a uniform foam structure, which is in good agreement with other
researchers, as highlighted by Wang and Yang, 2010.
With regards to the other observation, coating J5 has the highest equilibrium temperature of
325 C, almost reaching the critical temperature (400 ◦ C) after 40 min of fire exposure. The equilibrium
◦

temperature of coating J5 might be due to its char layer showing porosity and lightness, resulting in
the loss of adherence of the char to the steel plate or by a loss of cohesion of the char layer; similar
observations have been made by other researchers too [24].

3.2. Furnace Test

The purpose of the furnace test is to investigate and critically assess the fire protection performance
of the coated samples by measuring the thickness of the char layer at temperatures of 500 and 600 ◦ C.
The thicknesses of the char layer have been measured and recorded in Figure 6. Based on the results,
all of the char layers have expanded from 500 to 600 ◦ C except coating J3. From the result obtained, it
can be observed that the char layer of coatings J3, J4 and J5 with the addition of magnesium hydroxide
has a slightly less thick char layer as compared to coatings J1 and J2. These phenomena are due
to the flame-retardant filler (i.e., magnesium hydroxide) that has a negative contribution toward a
fire-protective performance. It has a poor char expansion and resulted in failing to provide the required
thick insulating barriers to protect the underlying steel plate from the heat. The thickness of coating J3
increased at 500 ◦ C, this is because of the gaseous water phase during the decomposition of Mg(OH)2
filler envelop the flame, and thereby excluding the oxygen and diluting flammable gases [25]. Whereas
the thickness of the char layer of coating J3 decreased at 600 ◦ C, this is due to the fire that propagated
through the fire-protective barrier which thus led to a decrease of thickness of the char layer.
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7
J2
6
J1
Thickness of char layer (mm)

5 J2
J1 J5
4 J4
J3 J4
J5
3 J3

0
500 600
Temperature (℃)

Figure 6. Thickness of char layer of the coated samples at 500 and 600 ◦°C.
C.

The coating J2 has the thickest char layer of 4.6 mm and 6.0 mm at temperatures of 500 ◦°C C and
◦ C, respectively. This Thisindicates
indicatesthat thatit it has
600 °C, respectively. has thethe highest
highest expansion
expansion valuevalue of aofchar
a char
layerlayer
duedue to
to the
the addition
addition of Al(OH)
of Al(OH) 3 and 3 and
CES CES
that that
have have significantly
significantly exhibited
exhibited the the expansion
expansion of theof the
char char
layer. layer.
The
The formation
formation of aofcohesive
a cohesive structure
structure during
during burning
burning can canpotentially
potentiallybebeinitiated initiatedby by decarbonation.
decarbonation.
Decarbonation of
Decarbonation ofCESCEScan can release
release carbon
carbon dioxide
dioxidewhich whichcan trap
can the trapdegraded
the degraded product into theinto
product residue
the
and induce swelling [11]. The thickness of the char layer of coating J1 was 4.3 mm at 500 ◦ C and
residue and induce swelling [11]. The thickness of the char layer of coating J1 was 4.3 mm at 500 °C
◦ C. The expansion value of the thickness of the char layer of coating J1 is approximately
5.4 mm
mmatat600600 °C. The expansion value of the thickness of the char layer of coating J1 is
1.1 mm. The char
approximately 1.1 layer
mm. The of coating
char layer sample J1 is considered
of coating sample J1 to isbeconsidered
thicker than to the coating than
be thicker samples the
J3, J4 and
coating J5, which
samples J3, J4 is and
again J5,due
which to the addition
is again due of to Al(OH)
the addition3 , providing
of Al(OH) the3,strong reversibility
providing the strong of
dehydration reaction
reversibility of dehydrationwith water released
reaction withinside
waterthe released
particle recombining
inside the particle to the reactive surfaceto
recombining of the
freshly formed
reactive surfacealumina,
of the freshly resulting
formed in aalumina,
good flammability
resulting inresistance filler and expansion
a good flammability resistanceoffiller
the char
and
layer [25]. The
expansion of theexpansion
char layer values of the
[25]. The thicknessvalues
expansion of the of char
thelayers
thicknessof coatings J4 and
of the char J5 were
layers 0.4 mm
of coatings
and
J4 and1.2J5mm,
were respectively.
0.4 mm andAlthough the additionAlthough
1.2 mm, respectively. of CES in the coating J4 and
addition the addition
of CES in coating of J4
CaCO in
and 3the
coating J5 showed significantly good flame-retardant fillers, the combination
addition of CaCO3 in coating J5 showed significantly good flame-retardant fillers, the combination of3 of CES and/or CaCO
CES and/or
with Mg(OH) CaCO
2 filler3 with
mayMg(OH)
have led2 to filler mayfire-resistance
poorer have led to poorer fire-resistance
performance. Hence,performance.
it can be deduced Hence, it
that
can be deduced
Mg(OH) 2 filler can that Mg(OH)
restrict the filler
formation
2 can of restrict
the char the
layerformation
by declining of thethe char layer
fire-protectionby declining
performance. the
fire-protection
In addition, performance.
the strength of the char layer has also been determined for each coating sample after
In addition,
reaching the maximum the strengthheating of temperature
the char layer of has ◦ C through
600 also been determined
the furnace fortest.
eachThe coating
weight sample
load
after
of 50 reaching
g coin-shape the maximum
metal is stacked heating uptemperature
on-top of the ofchar
600 °Clayer through
one bythe onefurnace
until the test. The
char weight
layer has
load of 50 gcracked.
completely coin-shape metal is stacked
In summary, only coatingsup on-top
J1, J2 of
and theJ5char
havelayer one bythis
undergone onetestuntil the char
as the charlayers
layer
has completely
of coatings J3 and cracked.
J4 already In summary,
cracked after onlyheating
coatings upJ1,to J2 ◦ C J5
600and in have undergone
the furnace. The this test as
strength of the
the char
layers
layer of ofcoating
coatingsJ2J3can and J4 alreadythe
withstand cracked
maximum after load
heatingup to up650
to 600 g, as°Ccompared
in the furnace. The strength
to coatings J1 (400 of g)
the
andchar layer
J5 (600 g).ofThis
coating J2 can withstand
experimental test has the maximum
proven load up
that coating J2 to
can650 g, as compared
achieve the best fire to coatings
protection J1
(400 g) and J5and
performance (600theg). This experimental
strongest char layer againsttest has theproven
fire. that coating J2 can achieve the best fire
protection performance and the strongest char layer against the fire.
3.3. Surface Morphology of Char Layer of Coated Samples
3.3. Surface Morphology
Microscopic of Char
analyses Layer of Coated
are executed Samples
with the scanning electron microscope (SEM) to examine and
analyze the surfaceanalyses
Microscopic morphology of the intumescent
are executed coating. The
with the scanning SEM micrographic
electron imagestoofexamine
microscope (SEM) all char
layers
and of coated
analyze thesamples
surface after the Bunsen
morphology burner
of the test are shown
intumescent in Figure
coating. 7. The
The SEM orange colorimages
micrographic indicates
of
all char layers of coated samples after the Bunsen burner test are shown in Figure 7. The orange color
indicates the holes and voids in the char layer of the coated samples. The images of coatings J1, J3, J4
Coatings 2019, 9, 738 10 of 18

Coatings 2019, 9, x FOR PEER REVIEW 11 of 20

the holes and voids in the char layer of the coated samples. The images of coatings J1, J3, J4 and J5
illustrated larger holes and voids. These holes are formed because of trapped gas by its blowing agent
and J5 illustrated larger holes and voids. These holes are formed because of trapped gas by its
when the coating is exposed to fire [26]. The tiny holes and void structures can be the consequence
blowing agent when the coating is exposed to fire [26]. The tiny holes and void structures can be the
of fire and heat propagation. The fire and heat propagated to the crack lines on the foam structure
consequence of fire and heat propagation. The fire and heat propagated to the crack lines on the
can also lead to a poor fire-protective performance of the coating [14]. On the other hand, the char
foam structure can also lead to a poor fire-protective performance of the coating [14]. On the other
layer of coating J2 has displayed a more uniform and denser foam structure which can strongly adhere
hand, the char layer of coating J2 has displayed a more uniform and denser foam structure which
to the steel substrate after the fire test. This rigid formation can contribute to the enrichment of the
can strongly adhere to the steel substrate after the fire test. This rigid formation can contribute to the
fire-protective performance on the coated steel substrate and subsequently lead to better characteristic
enrichment of the fire-protective performance on the coated steel substrate and subsequently lead to
properties of the coating. Therefore, a fire protective performance which indicates the competency
better characteristic properties of the coating. Therefore, a fire protective performance which
of the char layer in fire resistance is highly dependent on its physical structure of the coating [27].
indicates the competency of the char layer in fire resistance is highly dependent on its physical
Hence, when selecting the specified formulation of flame-retardant fillers, it is worth noting that the
structure of the coating [27]. Hence, when selecting the specified formulation of flame-retardant
coating needs to be able to enhance the intumescent coating performance in terms of fire protection
fillers, it is worth noting that the coating needs to be able to enhance the intumescent coating
and thermal properties.
performance in terms of fire protection and thermal properties.

Figure 7. Cont.
Coatings 2019, 9, 738 11 of 18
Coatings 2019, 9, x FOR PEER REVIEW 12 of 20

Figure
Figure 7.
7. Surface
Surface morphology
morphology of
of the
the various
various char
char layer
layer samples.
samples.

Adhesion Strength
3.4. Adhesion Strength of
of Coated
Coated Samples
Samples
This test is carried out to determine the adhesion strength of the coated
This coated samples.
samples. The average
adhesion strength amongst all coating samples is tabulated and presented
strength amongst all coating samples is tabulated and presented in Figure in Figure 8. All the coating
8. All the
samplessamples
coating show goodshow adhesion strength strength
good adhesion values. The coatings
values. J1–J5 have
The coatings showed
J1–J5 have higher
showed adhesion
higher
strength values
adhesion ranging
strength valuesfrom 1.05 tofrom
ranging 1.45 MPa.
1.05 toThe increased
1.45 MPa. The adhesion strength
increased can bestrength
adhesion interpreted
canduebe
to the influence
interpreted due to of the carbonyl group between VA copolymer and the surface oxide
influence of the carbonyl group between VA copolymer and the surface oxide or hydroxide of
steel
or substrate of
hydroxide that has substrate
steel created a stronger
that has carbon–hydrogen
created a stronger (CH) bond in the mixture
carbon–hydrogen (CH)ofbond
the coating.
in the
The intermolecular
mixture bonding
of the coating. between the flame-retardant
The intermolecular bonding between fillers’
themolecules has further
flame-retardant improved
fillers’ moleculesthe
interaction
has further between
improved thethe
coating and thebetween
interaction steel substrate as well
the coating andas the
between
steel themselves
substrate as[28].
wellThis is not to
as between
disregard the[28].
themselves carbon–hydrogen
This is not to bonding, which
disregard theincarbon–hydrogen
fact has a significant role in the
bonding, adhesive
which properties
in fact has a
of the coating. The carbon–hydrogen bonding is formed between a strongly electronegative
significant role in the adhesive properties of the coating. The carbon–hydrogen bonding is formed atom that
is usuallya oxygen
between stronglyand a hydrogen atom.
electronegative atom The
that hydrogen
is usually bonds
oxygenare andformed between
a hydrogen a monomer
atom. of the
The hydrogen
VA copolymer
bonds molecule
are formed between and the steel substrate.
a monomer of the VA copolymer molecule and the steel substrate.
Judging from the results obtained, it is revealed that the coating J5 with the addition of Mg(OH)2
and CaCO3 have shown the highest adhesion strength that is 1.45 MPa. The increase in adhesion
strength of coating J5 is due to the strong bonding strength between the steel substrate surface and
the VA copolymer binder with the addition of Mg(OH)2 and CaCO3 fillers, which distribute stresses
effectively. Mechanical stress can encourage the development of voids in the matrix caused by the loss
of adhesion between the coating and the filler [29], whereas the coatings J2 and J4 with the addition
of Al(OH)3 + CES and Mg(OH)2 + CES show higher adhesion strength of 1.25 MPa and 1.26 MPa,
respectively, as compared to other coatings. The addition of CES filler has indeed shown improvement
in adhesion strength due to the improved reinforcement properties between the CES filler and VA
copolymer binder [30]. However, the adhesion strength of coating J4 with the addition of Mg(OH)2 and
CES is higher than the adhesion strength of the coating J2 with the addition of Al(OH)3 and CES due to
the Al(OH)3 filler leading to the reduction of adhesion strength. This is due to the aluminium hydroxide
which reduces the adhesion strength in the particular case under the influence of moisture where the
Coatings 2019, 9, 738 12 of 18

oxide layer transforms into a hydroxide with a morphological change. The adhesion strengths of the
coatings J1 and J3 with the addition of calcium silicate have showed lower adhesion strength of 1.05
and 0.95 MPa, respectively. This indicates that the coating formulation incorporated with calcium
silicate would decrease the adhesion strength. Therefore, choosing an appropriate flame-retardant
filler strongly influences the interfacial bonding strength between the intumescent coating and the
steel substrate [31].
Coatings 2019, 9, x FOR PEER REVIEW 13 of 20

50
J5
45
J2 J4
40
Adhesion Strength (MPa)

35 J1
J3
30

25

20

15

10

0
Coating Samples

Figure 8.
Figure 8. Adhesion
Adhesion strength of the
strength of the coating
coating samples.
samples.

3.5. Freeze-Thaw
Judging from Cycle
theTest
results obtained, it is revealed that the coating J5 with the addition of
Mg(OH) 2 and CaCO3 have shown the highest adhesion strength that is 1.45 MPa. The increase in
This test is conducted to evaluate the effect of room temperature, freezing temperature and high
adhesion strength
temperature, of coating
symbolizing J5 is due
different to the
weather strong bonding
conditions strengthspring,
such as winter, between the steel
autumn, andsubstrate
summer
surface and the VA copolymer binder with the addition of Mg(OH) 2 and CaCO3 fillers, which
on the coating surface. Figure 9 shows the results of all coated samples before and after 21 freeze–thaw
distribute
cycle tests.stresses effectively.
The coated samplesMechanical
are visuallystress can encourage
inspected the development
for cracks, blisters, coagulatedofparticles,
voids in and
the
matrix caused by the loss of adhesion between the coating and the filler [29], whereas
changes of color. In this research study, all the coated samples remain unchanged and free from any the coatings J2
and J4 cracks
visible with the
andaddition
coagulated of Al(OH) 3 + CES and Mg(OH)2 + CES show higher adhesion strength of
particles after freeze–thaw cycles. All coating samples have proven to be
1.25 MPa and 1.26 MPa, respectively, as compared
efficient in withstanding the highly destructive toofother
forces coatings.
cyclic freezingThe andaddition
thawing.of CES filler has
indeed shown improvement in adhesion strength due to the improved reinforcement properties
between the CES filler and VA copolymer binder [30]. However, the adhesion strength of coating J4
with the addition of Mg(OH)2 and CES is higher than the adhesion strength of the coating J2 with the
addition of Al(OH)3 and CES due to the Al(OH)3 filler leading to the reduction of adhesion strength.
This is due to the aluminium hydroxide which reduces the adhesion strength in the particular case
under the influence of moisture where the oxide layer transforms into a hydroxide with a
morphological change. The adhesion strengths of the coatings J1 and J3 with the addition of calcium
silicate have showed lower adhesion strength of 1.05 and 0.95 MPa, respectively. This indicates that
the coating formulation incorporated with calcium silicate would decrease the adhesion strength.
Therefore, choosing an appropriate flame-retardant filler strongly influences the interfacial bonding
strength between the intumescent coating and the steel substrate [31].

3.5. Freeze-Thaw Cycle Test

This test is conducted to evaluate the effect of room temperature, freezing temperature and high
temperature, symbolizing different weather conditions such as winter, spring, autumn, and summer
on the coating surface. Figure 9 shows the results of all coated samples before and after 21 freeze–
thaw cycle tests. The coated samples are visually inspected for cracks, blisters, coagulated particles,
and changes of color. In this research study, all the coated samples remain unchanged and free from
any visible cracks and coagulated particles after freeze–thaw cycles. All coating samples have
Coatings 2019, 9, 738 13 of 18
Coatings 2019, 9, x FOR PEER REVIEW 14 of 20

Before Freeze–Thaw After 21 Freeze–Thaw Before Freeze–Thaw After 21 Freeze–Thaw

Testing Cycles Testing Cycles

Coating Sample J1 Coating Sample J4

Coating Sample J2 Coating Sample J5

Coating Sample J3
Figure9.9.Before
Figure Beforeand
andafter
afterthe
thefreeze–thaw
freeze–thawcycles
cycles test
test of
of the
the coated samples.
samples.

3.6. Thermogravimetric
3.6. ThermogravimetricAnalysis
Analysis(TGA)
(TGA)Test
Test
This
Thistesttestis istotodetermine
determinethe thethermal
thermaldegradation
degradation by by calculating residual weight
calculating the residual weight of of the
the
intumescent coatings. From the
intumescent coatings. From the results obtained results obtained in Figure 10 under nitrogen gas, the
under nitrogen gas, the thermal thermal
decomposition
decompositionisismainly mainlyobserved
observedatataatemperature
temperature between 200–450 ◦°C.
between 200–450 C. However,
However, the the thermal
thermal
decomposition
decompositioncan canalso
alsooccur
occuratatdifferent
differentstages.
stages. In In this
this study,
study, the
the general
general thermogram
thermogram profiles profilesare are
quite similar
quite similar butbut the
thecurves
curvesare arefound
foundtotobe beslightly
slightlyshiftedshifted towards
towards higher temperature
temperature ranges rangeswithwith
gradual
gradual increments
increments inin heatingrates.
heating rates.FromFrom30 30toto100 100◦°C, around 2%
C, around 2% of of the initial weight is is lost.
lost. This
Thisisis
possibly
possibly dueduetotothe the releaseofofmoisture.
release moisture.Between
Between100–200 100–200 ◦°C, J1 and J2 showed
C, J1 showed slight
slight weight
weightloss lossof of
approximately 1%–2%, where J3, J4 and J5 showered
approximately 1%–2%, where J3, J4 and J5 showered around 5% of the initial around 5% of the initial weight losses. Between
losses. Between
200–300
200–300 ◦ C,
°C, a weightloss
a weight lossofof10%
10%ofofthe theinitial
initialweight
weightisisobserved.
observed. Between
Between 300–450
300–450 °C, ◦ C, aa measured
measured
weight
weight lossloss of approximately
of approximately 45% 45% is calculated.
is calculated. However,
However, between
between 450–1000
450–1000 ◦ C, °C, the weight
the weight loss loss is
is only
only 10% of the initial weight observed. This can be attributed
10% of the initial weight observed. This can be attributed to the fact that the degradation/decomposition to the fact that the
degradation/decomposition
reaction has reached a relatively reaction
stablehas reached
stage in theamixture.relatively stable stage in the mixture.
InIn summary,
summary, thethe residual
residual weights
weights ofJ2,
of J1, J1,J3,J2,J4,J3,and
J4,J5
and J5 at
at 950 ◦ C950
are°C are 34.28%,
34.28%, 34.55%,34.55%,
32.77%,32.77%,
33.82%,
33.82%, and 31.34% respectively. The TG curves have clearly demonstrated
and 31.34% respectively. The TG curves have clearly demonstrated that the residue weight of coating that the residue weight
of coating
sample J2 has sample J2 has residual
the highest the highest residual
weight which weight which
indicates indicates
that that theofaddition
the addition aluminum of aluminum
hydroxide
hydroxide and CES fillers content in intumescent binder could
and CES fillers content in intumescent binder could enhance anti-oxidation of the coatings [32]. enhance anti-oxidation of the
coatings [32].
Coatings 2019, 9, 738 14 of 18
Coatings 2019, 9, x FOR PEER REVIEW 15 of 20

Figure 10.
Figure 10. TGA
TGA curves of each
curves of each coating
coating sample.
sample.

3.7. Testing for Fire-Resistant

Fire-Resistant Timber
Timber Door
Door Prototypes
Prototypes

3.7.1. Small Scale

3.7.1. Small Scale Fire
Fire Test
Test
This
This test
test is
is to
to characterize
characterize the the fire
fire protective
protective performance
performance of of the
the fire-resistant
fire-resistant timber
timber door
door
prototypes (P1–P5). The results of each coating sample plotted as a function
prototypes (P1–P5). The results of each coating sample plotted as a function of time are presented of time are presented in
in Figure
Figure 11.11.
TheThe results
results showthat
show thatthe
thetemperature
temperatureofofeach eachfire-resistant
fire-resistant timber
timber door
door prototype
prototype has has
increased
increased gradually.
gradually.From From the the
results obtained,
results all the temperatures
obtained, of prototypes
all the temperatures of increase
prototypes significantly
increase
in the first 15 min, revealing a similar pattern. This phenomenon is because
significantly in the first 15 min, revealing a similar pattern. This phenomenon is because of the of the good thermal
good
insulation of vermiculite and perlite. These porous materials can dissipate
thermal insulation of vermiculite and perlite. These porous materials can dissipate the heat when the heat when exposed
to fire. After
exposed 15 After
to fire. min, P4 15 has
min,started
P4 hasto increase
started rapidly and
to increase gradually
rapidly until 20 until
and gradually min. 20This
min.may be may
This due
to the physical and chemical reactions of the intumescent coating during
be due to the physical and chemical reactions of the intumescent coating during the fire test. the fire test. After 20 min,
all
Afterthe20
prototypes
min, all the have showed ahave
prototypes similar pattern
showed of temperature
a similar pattern of profiles until profiles
temperature reachinguntil120 reaching
min. On
top of that, P2 has the lowest temperature of 140.7 ◦ C at the center of the prototype as compared to
120 min.
Coatings On9, top
2019, x FORofPEER
that,REVIEW
P2 has the lowest temperature of 140.7 °C at the center of the prototype 16 of as
20
other
comparedtypesto ofother
prototypes.
types ofItprototypes.
has also been indicated
It has that indicated
also been this prototype, P2, prototype,
that this has resulted P2,inhas
the resulted
best fire
protective
in the best performance
fire protective inperformance
retarding theinfire.
retarding the fire.

Figure
Figure 11.
11. Evolution
Evolution of
of temperature
temperature of
of fire-resistant timber door
fire-resistant timber door prototypes.
prototypes.

3.7.2. Fire Endurance

3.7.2. Fire Endurance and
and Temperature
Temperature Rise
Rise Tests
Tests
As
As aa building
building safety
safetyrequirement,
requirement,the
thesafety
safetyand
andthe
thereliability
reliabilityofofthe fire
the door
fire is is
door thethe
key aspect
key to
aspect
determining the effectiveness during the outbreak of the fire. In this research project, there
to determining the effectiveness during the outbreak of the fire. In this research project, there are are only
commercial prototypes,
only commercial and the
prototypes, lowest
and equilibrium
the lowest temperature
equilibrium of P2 have
temperature been
of P2 selected
have been to undergo
selected to
undergo the fire endurance [33] and temperature rise tests [34] to compare the fire-resistance rating
and heat transmission rate by visual observation/inspection. The fire endurance test is to
characterize the ability of the fire-resistant timber door prototypes to survive at a specified fire
condition for a certain time without an integrity failure or a significant leakage. In this project, the
magnesium oxide board acts as the commercial fire-resistant door prototype, which is used to
Coatings 2019, 9, 738 15 of 18

the fire endurance [33] and temperature rise tests [34] to compare the fire-resistance rating and heat
transmission rate by visual observation/inspection. The fire endurance test is to characterize the ability
of the fire-resistant timber door prototypes to survive at a specified fire condition for a certain time
without an integrity failure or a significant leakage. In this project, the magnesium oxide board acts
as the commercial fire-resistant door prototype, which is used to compare with prototype P2. The
results of fire endurance and temperature rise of prototypes after the 2 h fire is shown in Figure 12.
Coatings 2019, 9, x FOR PEER REVIEW 17 of 20
As a result, both prototypes achieved the 2-h fire-resistance rating without an integrity failure or a
significant leakage.

(a)

(b)
Temperature rise
Figure 12. Temperature rise ratings
ratings at
at the
the center
center (T1)
(T1) (a)
(a) and
and the
the edge
edge (T2)
(T2) (b)
(b) of
of the
the P2 and
commercial prototypes.

Based on
Based onthe
theresults
resultsobtained,
obtained,P2 P2
hashas
shown the best
shown the relatively low-temperature
best relatively rise rating
low-temperature rise during
rating
during a 120 min fire, which can be considered to have possessed a good quality of low at
a 120 min fire, which can be considered to have possessed a good quality of low heat transmission T1
heat
and T2, as compared
transmission at T1 andto aT2,
commercial
as comparedprototype. By analyzing
to a commercial the temperature
prototype. rises atthe
By analyzing different points
temperature
(T1 and T2), P2 has also indicated the best fire retardancy properties by promoting a
rises at different points (T1 and T2), P2 has also indicated the best fire retardancy properties by lower equilibrium
temperatureathan
promoting the commercial
lower equilibriumprototype.
temperature Moreover,
than the
themaximum
commercialtemperatures
prototype.of Moreover,
the commercial
the
prototype are merely 195.6 (T1) and 40.0 ◦ C (T2), respectively. For P2, the maximum temperatures at
maximum temperatures of the commercial prototype are merely 195.6 (T1) and 40.0 °C (T2),
T1 and T2 areFor merely 140.7 ◦ C, respectively. This has clearly indicated that P2 has a higher fire
and 32.0temperatures
respectively. P2, the maximum at T1 and T2 are merely 140.7 and 32.0 °C, respectively.
resistance
This than the
has clearly commercial
indicated that prototype. This phenomenon
P2 has a higher canthan
fire resistance be due
thetocommercial
the density prototype.
differences,This
i.e.,
the density of P2 (density = 636.45 kg/m 3 ) is lower as compared to the current existing commercial
phenomenon can be due to the density differences, i.e., the density of P2 (density = 636.45 kg/m ) is lower 3

prototype
as compared (density = 873.71
to the current kg/m3 ).
existing commercial prototype (density = 873.71 kg/m3).
Besides that, an appropriate combination of intumescent flame-retardant coating with
vermiculite and perlite can also lead to a lower heat transmission and reveal less surface cracks,
resulting in the reduction of temperature up to 54.9 °C as compared to the commercial prototype
after the 2 h fire test, as seen in Figure 13. Furthermore, the higher temperatures of the commercial
prototype measured at T1 and T2 are also higher than those measured for the P2 prototype as
evident in Figure 13b with numerous cracks on the surface of the prototype providing higher rates of
Coatings 2019, 9, 738 16 of 18

Besides that, an appropriate combination of intumescent flame-retardant coating with vermiculite

and perlite can also lead to a lower heat transmission and reveal less surface cracks, resulting in the
reduction of temperature up to 54.9 ◦ C as compared to the commercial prototype after the 2 h fire test,
as seen in Figure 13. Furthermore, the higher temperatures of the commercial prototype measured
at T1 and T2 are also higher than those measured for the P2 prototype as evident in Figure 13b with
numerous cracks on the surface of the prototype providing higher rates of heat transfer to the backside
of the prototype.
Coatings 2019, 9, x FOR PEER REVIEW 18 of 20

a b

Figure
Figure13.
13.Fire
Firedoor
doorprototypes
prototypes(a)
(a)P2
P2and
and(b)
(b)commercial
commercial after
after the
the 2-h
2-h fire
fire test.
test.

4. Conclusions
4. Conclusions
From the series of
From of experimental
experimentaltests,tests,the
thefollowing
followingconclusions
conclusionscan canbebededuced.
deduced. The
The selection
selectionof
suitable combinations of flame-retardant materials can directly affect the
of suitable combinations of flame-retardant materials can directly affect the fire-protective fire-protective performance
and the mechanical
performance and the properties
mechanicalof the intumescent
properties flame-retardant
of the intumescent coating ascoating
flame-retardant well asas the fireasdoor
well the
prototype.
fire AmongstAmongst
door prototype. all the coating
all thesamples
coating used/manufactured
samples used/manufacturedin this research
in thisproject,
researchthe coatingthe
project, J2
with the addition of 3 wt.% of aluminum hydroxide and 3 wt.% of renewable
coating J2 with the addition of 3 wt.% of aluminum hydroxide and 3 wt.% of renewable CES bio CES bio filler is concluded
to have
filler the best fire-protective
is concluded to have the bestperformance, thermal,
fire-protective mechanical,
performance, physical,
thermal, and chemical
mechanical, properties.
physical, and
On top ofproperties.
chemical that, the P2On prototype withthe
top of that, theP2addition
prototypeof J2 intumescent
with the additioncoating
of J2reveals to a better
intumescent fire
coating
protective result (temperature reduction by up to 54.9 ◦ C), as compared to the existing commercial
reveals to a better fire protective result (temperature reduction by up to 54.9 °C), as compared to the
fire-resistant
existing timber door
commercial prototype.
fire-resistant timber door prototype.
To summarize the conclusions
To summarize the conclusions based based on on the experimental
experimental results,
results, an innovative
innovative intumescent
intumescent
flame-retardant paint incorporated into the lightweight fire-resistant timber
flame-retardant paint incorporated into the lightweight fire-resistant timber door prototype (P2) door prototype (P2) has
has
indeed demonstrated
indeed demonstratedtotobebe more efficient
more in reducing
efficient the heat
in reducing the transmission by maintaining
heat transmission its integrity
by maintaining its
without showing a significant leakage against the 2-h fire
integrity without showing a significant leakage against the 2-h fire test. test.

Contributions: Conceptualization,
Author Contributions:
Author Conceptualization, J.J.K.Y and and
J.J.K.Y M.C.Y.; Methodology,
M.C.Y.; J.J.K.Y.; J.J.K.Y.;
Methodology, Software,Software,
J.J.K.Y.; Validation,
J.J.K.Y.;
M.C.Y., M.K.Y. and L.H.S.; Formal Analysis, J.J.K.Y. and M.C.Y.; Investigation, J.J.K.Y. and M.C.Y.; Resources,
Validation, M.C.Y., M.K.Y. and L.H.S.; Formal Analysis, J.J.K.Y. and M.C.Y.; Investigation, J.J.K.Y. and
M.C.Y.; Data Curation, J.J.K.Y. and M.C.Y.; Writing–Original Draft Preparation, J.J.K.Y.; Writing–Review & Editing, M.C.Y.;
Resources,
M.C.Y. andM.C.Y.;
M.K.Y.;Data Curation, M.K.Y.
Visualization, J.J.K.Y.and
andL.H.S.;
M.C.Y.; Writing–Original
Supervision, M.C.Y.;Draft Preparation,
Project J.J.K.Y.;M.C.Y.
Administration, Writing–
and
Review & Editing,
M.K.Y.; Funding M.C.Y. and
Acquisition, M.K.Y.; Visualization, M.K.Y. and L.H.S.; Supervision, M.C.Y.; Project
M.C.Y.
Administration, M.C.Y.was
Funding: This project and funded
M.K.Y.; by
Funding Acquisition,
University of TunkuM.C.Y.
Abdul Rahman Research Scheme (UTARRF) with
project number:
Funding: IPSR/RMC/UTARRF/2018-C2/Y03.
This project was funded by University of Tunku Abdul Rahman Research Scheme (UTARRF) with
project number: IPSR/RMC/UTARRF/2018-C2/Y03.
Acknowledgments: The authors would like to thank University of Tunku Abdul Rahman (UTAR) for the UTARRF
funding support.
Acknowledgments: The authors would like to thank University of Tunku Abdul Rahman (UTAR) for the
Conflicts funding
UTARRF of Interest: The authors declare no conflict of interest.
support.

Conflicts of Interest: The authors declare no conflict of interest.

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