Accepted Manuscript

Title: Application of Water@Silica Core-Shell Particles for

Suppressing Gasoline Pool Fires

Authors: Xiaomin Ni, Shaogang Zhang, Zhong Zheng, Xishi

Wang

PII: S0304-3894(17)30548-4
DOI: http://dx.doi.org/doi:10.1016/j.jhazmat.2017.07.040
Reference: HAZMAT 18732

To appear in: Journal of Hazardous Materials

Received date: 11-4-2017

Revised date: 18-7-2017
Accepted date: 19-7-2017

Please cite this article as: Xiaomin Ni, Shaogang Zhang, Zhong Zheng, Xishi Wang,
Application of Water@Silica Core-Shell Particles for Suppressing Gasoline Pool Fires,
Journal of Hazardous Materialshttp://dx.doi.org/10.1016/j.jhazmat.2017.07.040

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 Application of Water@Silica Core-Shell Particles for
Suppressing Gasoline Pool Fires

Xiaomin Nia,*, Shaogang Zhanga, Zhong Zhengb, Xishi Wanga

aThe State Key Laboratory of Fire Science,

University of Science and Technology of China,

Hefei 230027, P.R. China

bDepartment of Electronic Science and Technology,

University of Science and Technology of China,

Hefei 230027, P.R. China

* Corresponding author, Email: nxmin@ustc.edu.cn, Tel: 86-551-63606430-802, Fax: 86-551-63601669

1
 Highlights

• A new type of fire suppressants with water@silica core-shell structures was

fabricated as through a simple stirring method.

• The capsular particles showed excellent performance in extinguishing gasoline

pool fires in terms of time and agent mass.

• The work presented a novel route to produce small sized water droplets and store

them without coalescence for long time.

Abstract
A new type of dry powders with capsular structure was fabricated for fire suppression,
in which the content of water approached 60%. The capsules with the size of 3~5 μm
consisted of liquid core and solid shell, where the core was water droplet and the shell
was assembled silicon dioxide particles with surface hydrophobic modification. The
shell of close-packed silica particles surrounding each water droplet provided the
structural rigidity of the capsules and enabled their application as powder fire
suppressants. Two different scaled real fire tests showed that thus-prepared solid
powders could extinguish 0.21 MW gasoline pool fire in 2.0 s with agent mass of
0.055 kg, and 1.0 MW gasoline pool fire in 5.0 s with agent mass of 0.49 kg. Such fire
extinguishing performance greatly outperformed the conventional monoammonium
phosphate (ABC) powders, neat silica powders and water mist, with significantly
reduced fire extinguishing time and mass of agent consumed. Mechanism of the
core-shell particles in fire suppression was discussed based on established theories
and experimental results.

2
Keywords: fire suppressant; capsular particles; water; silicon dioxide; gasoline pool fire

1. Introduction

Gasoline is one of the most commonly known liquid fuels, which is highly ignitable
and volatile. Gasoline has a comparatively low flash point of about -65°C and the
ignition temperature of about 232°C. While burning gasoline has a temperature above
945°C, which can heat objects in the fire area above its ignition temperature [1].
Meanwhile, gasoline is so volatile that a large amount of vapor is quickly generated
from the liquid surface. The flammable range of gasoline is only 1.4% to 7.1% [2].
When the gasoline vapor in an enclosure is ignited, it will burn explosively and causes
extensive damage. Gasoline vapor is heavier than air. It tends to flow downhill and
downwind from liquid gasoline, making it possible for explosive mixtures to collect
in low points such as pipe trenches or terrain depressions. Usually, a crash is often
followed by a gasoline fire. At present, gasoline is widely used in cars, aeroplanes and
some machines. The distressing and increasingly frequent incidence of fatal fires in
employing gasoline [3], has repeatedly directed attention to the need for an effective
fire suppressant for gasoline fires.

Highly efficient fire suppressants could fast control the fire and greatly reduce the loss.
Since the phase out of halon, water mist as one of the halon replacer has been paid
great attention for its high efficiency and environmental friendliness [4]. As naturally
clean agent, water mist would not decompose or produce any toxic products when
exposed to flame. In comparison to conventional water spray, water mist with much
smaller droplet size (with 99% of the volume of droplets with diameters less than
1000 microns) showed much higher efficiency in fire suppression. But water mist is
not so efficient in extinguishing small liquid fuel fires in the open space because a
small fire may not be able to generate enough heat for the transformation of water
droplets into vapor to displace sufficient oxygen [5,6]. It is noted that even if a liquid
fire is extinguished by water mist, re-ignition may occur at any time for the poor
covering effect of water mist from contacting oxygen [7]. To prevent re-ignition after

3
extinguishment, water mist must be applied for sufficient time to allow hot objects in
the fire area to cool below the ignition temperature of gasoline. This is time
consuming and may cause water damage. Droplet size greatly affects the fire
suppression capability of water mist [8]. It is difficult for water mist with small
droplet size and low momentum to penetrate the flame fume to extinguish the fire.
While water mist with big droplet size and high momentum would usually spoil out
the liquid fuel or raise its level in a container and so result in larger combustible area.
Production of water mist with proper droplet size was crucial for successful fire
extinguishment. Conventionally, production of water mist depends on specific
technique, such as specially designed nozzles and pressure. This makes the practical
application of water mist become conditional. In comparison to water mist, dry
powders as fire suppressants even showed superior fire extinguishing capabilities on a
mass basis while consuming minimal space [9,10]. Furthermore, dry powders
consisting of small particles could be easily discharged to the flame zone without any
special nozzle.

Considering the shortcomings of conventional methods in producing water mist and

the advantages of dry powders, here we reported a simple stirring route to produce a
new type of water@silica capsular particles as fire suppressant. The water droplets
with size of several microns were capsulated by silicon dioxide nanoparticles to form
core-shell structures. Under the protection of outside hydrophobic solid shell, the
particles with a high content of water approaching 60% behaved like dry powder fire
suppressants with good flowability, which was named as “dry water” (denoted as
DW). Details of the preparation, physicochemical properties and fire suppression
performance of the DW suppressants were studied. Mechanism of the DW particles in
fire suppression was discussed based on established fire suppression theories and
experimental results.

2. Experimental

2.1 Sample Preparation

All chemicals and reagents were used as received from commercial sources without
4
further purification. Hydrophobic SiO2 particles were purchased from Degussa. In a
typical experiment, 100.0 g distilled water was mixed with 25.0 g SiO2 and stirred at
the rate of 13000 r/min for 30 s. The resulted samples were free-flowing white
particles.

2.2 Characterization

Structure and morphology of the samples were characterized by X-ray diffraction

(XRD, Philips X’Pert), ZEISS Axioskop2 plus optical microscopy, and scanning
electron microscopy (SEM, QUANTA 200FEG). The Fourier transform infrared
(FTIR) spectrum of KBr wafer was recorded using a Nicolet 6700 Fourier Transform
Spectrometer. Thermogravimetry-differential scanning calorimeter (TG-DSC) curve
was acquired through the SHIMADZUDTG-60H instrument.

2.3 Fire tests

Generally, the standard testing procedures for evaluating the fire extinguishing
performance of dry powders includes ISO 7202-2012, NFPA 17, ANSI/UL 299, and
etc. However, in these standards, the experimental setup is quite large, which is
expensive and time consuming to build. For the limit of our experimental conditions,
large fire tests following these standards were difficult to undertake. Two laboratory
scaled tests were designed with relatively small fire sources and less agents to reduce
the cost. But the test methods were basically in conformance with the regulations in
international standards.

The small scale fire tests, were conducted in a 27 m3 (3 m × 3 m × 3 m) confined

space with natural ventilation. Details of the experimental apparatus were
schematically shown in Fig. 1. Gasoline was contained in the oil pan with the
diameter of 0.50 m. A thermocouple tree, containing six thermocouples with interval
of 0.20 m and the lowest thermocouple 0.25 m above the fuel pan, was set up to
measure the flame temperatures. In each test, 200.0 g powders were added into a tank
with the volume of 1000 ml and pressurized by nitrogen to a pre-assigned value of
5
0.50 MPa. Before powder discharging, 400 ml gasoline was added into the pan,
ignited and pre-burned for 30 s. The flame power was estimated as 0.21 MW. The
distance from the extinguisher nozzle to the pan center was set as 1.0 m. The valve of
the powder tank was turned off as soon as the fire was extinguished. The weight of the
tank was measured before and after each test to determine the total mass of
suppressants consumed for fire extinguishment. Each test was repeated at least three
times to get a converged result. The fire suppression process was recorded by a video
camera.

The bigger scale fire tests were conducted in a 1000 m3 (10 m × 10 m × 10 m) large
space hall with natural ventilation to further evaluate fire extinguishing performance
of as-prepared powders. 500 g powders were contained in a hanged powder
extinguishing equipment and pressurized by nitrogen to 1.0 MPa. The circular oil pan
with the diameter of 0.95 m contained 21.0 L gasoline. The flame power was
estimated as 1.0 MW. The perpendicular distance from the hanged extinguisher nozzle
to the fuel surface was 1.5 m. The gasoline was ignited and pre-burned for 30 s before
powder discharging. After the fire was extinguished, the agent mass consumed was
measured and recorded. Considering the agent flow calibration uncertainty and
measurement variance, the relative expanded uncertainty of the fire extinguishing
time and the agent mass consumed in firefighting was estimated as ±15% and ±10%,
respectively.

3. Results and Discussion

3.1 Structure and Morphology

Fig.2 showed a typical XRD pattern of as-prepared “dry water” particles, in which
only a broad peak with 2θ centered at about 22°was seen. It indicated that the
material was amorphous SiO2 [12]. Fig.3 presented FTIR spectrum of the sample,
where the peaks could be reasonably ascribed to SiO2 and H2O [13]. The broad band
around 3450 cm-1 and the peak at 1640 cm-1 was due to stretching vibration and the

6
bending vibration of water molecules adsorbed on the silica surface. The strong band
at 1112 cm-1 corresponded to the asymmetric vibration of Si-O-Si. The absorption
bands at 800 cm-1 and 485 cm-1 were assigned to the stretching vibration and
bending vibration of Si-O-Si bond, respectively.

Morphological images of the sample were shown in Fig. 4. As revealed by Fig. 4a, the
sample consisted of free-flowing powders. Optical microscopy image of Fig. 4b
showed that the particles were spherical and ellipsoidal with the size in the range of
10~30 μm. SEM images of Fig.4c and d gave more details of the particles, revealing
that the particle shell was made up of loosely arranged small particles with the
diameter of 30~50 nm.

3.2 Fire extinguishing performance

A series of laboratory scale fire extinguishing tests were conducted to assess the
performance of as-prepared DW suppressants (denoted as sample A). For comparison,
hydrophobic silica particles (denoted as sample B), neat water mist with the mean size
of 30~40 μm (denoted as sample C), and commercially available ABC dry powders
(NH4H2PO4 50 w.t.%, (NH4)2SO4 25 w.t.%, and inert additives 25 w.t.%, denoted as
sample D), were also tested under the similar conditions. Table 1 listed the agent
composition, particle size distribution, flame power, fire extinction time and agent
mass consumed in the two kinds of fire tests. It was shown that sample A exhibited
much better performance than the three counterparts. The capsular particles could fast
extinguish 0.21 MW gasoline pool fires in 2.0 s with 54.7 g agent consumed and no
re-ignition occurred. While neat silica powders could not extinguish the fire even with
all of the originally added agent was nearly consumed out (187.5 g). The fire was just
suppressed but not extinguished. Water mist with droplet size of 30-40 μm could
extinguish the fire, but a long time of 12 s and a large amount of water of 272.6 g was
consumed. Commercial ABC dry powders could not extinguish the fire even with
191.3 g power consumed. Such results revealed that fire extinguishing performance of
the capsular particles was much superior to that of the three counterparts in terms of

7
the fire extinguishing time and the agent mass required. Typical snapshots from the
fire suppression process of the tests with different samples were shown in Fig. 5.

Although the above experiments clearly ranked the fire suppression effectiveness of
four samples, fire tests in relatively large scale gave more direct check on the
firefighting capacity of agents. Therefore, a bigger sized gasoline pool fire test was
conducted with the flame power of about 1.0 MW. As-prepared “dry water” powders
could extinguish the fire in 4.8 s with 487.4 g consumed. While the other three
samples of silica, water mist and commercial ABC dry powders all failed to
extinguish the big fire. Typical snapshot images of the big fire test using the DW
powders were shown in Fig.6.

The above two different scaled fire experiments revealed that neither water mist nor
silica particles of the same amount used alone could extinguish the fire. But when the
two components were combined and transformed into capsular particles, the fire could
be fast extinguished. The composite greatly outperformed each component.

3.3 Fire Suppression Mechanism

Successful fire suppression required that one or more of the four factors of fuel,
oxygen, heat and chain reaction which tend to propagate a fire be suppressed. It was
assumed that solid particulates functioned as fire suppressants through several
mechanisms, including chemical inhibition of the chain reactions via the catalytic
combination of active species, heat absorption and cooling by decomposition and
vaporization of the solid particles, oxygen dilution in the flame regions by the inert
gases produced and the chemical reaction of the particles and active species [14,15].
Here, for the capsular particles containing water and silicon oxides, they would not
decompose in the flame and produce any species to stop the combustion reactions. So,
it was considered that as-prepared capsular particles should have the following three
mechanisms in extinguishing the gasoline pool fires: cooling effect, dilution of
oxygen, and heterogeneous chemical effect.

8
When discharged into the flame, the capsular particles would be heated and the inner
water cores would be released out. As revealed by the TG-DSC curve of sample A
from room temperature to 800oC in Fig. 7, the particles were fast dehydrated and the
mass loss stopped at about 140oC. During this dehydrating process, a big exothermal
peak was exhibited, which could be ascribed to the evaporation of water. Here, it was
assumed that the “water cores” played an important role in extinguishing the gasoline
pool fires.

The suppression mechanism of water mist on fire was believed to be basically

physical, through heat extraction on the flame by water evaporation, oxygen
displacement and attenuation of thermal radiation by increased water vapor
concentration [16]. As shown by Fig.7, the exothermal peak from water evaporation
contributed to decrease the flame temperatures. Meanwhile, the resulted water vapor
diluted the oxygen concentration around the flame. Oxygen dilution was the main
mechanism of suppressing fires by water mist in an enclosed space. In the enclosure,
the oxygen concentration around the flame may be greatly diluted by the resulted
water vapor and then satisfied fire suppression performance would be exhibited. But
under the conditions with adequate oxygen, the effect of oxygen dilution became
weak. In the present tests with small fires relative to the compartment with adequate
supply of oxygen, the oxygen dilution effect was minor [17]. So the cooling effect
from water was considered the dominant mechanism.

But different to regular water mist, here, water droplets were encapsulated in the solid
silica particles shells, which made them easier to reach the flame zone to exert its
suppressing effect. An important practical issue in employing highly effective
suppressants was getting sufficiently high concentrations into the flame zone. For
regular neat water mist, most of the water droplets evaporated when contacting with
the flame edge and only a small amount of water droplets could penetrate into the
flame zone. But for the water droplets loaded in the silica particles, they could reach
the flame zone more easily. Furthermore, the core-shell particles with a proper density

9
could fast distribute and suspend in the flame zone. Upon heating, the in-situ desorbed
water molecules would pavilion the flame and form a water vapor atmosphere, which
contributed to the flame suppression. Thus the cooling effect and oxygen dilution of
the water droplets could be fully experienced by the flame. As a result, excellent fire
extinguishing performance was exhibited by the capsular particles, but failed for the
regular water mist. For the limitation of instrument, the oxygen concentrations in the
flame could not be measured accurately. The discussion on the contribution of the
water cores for fire extinguishment was still a hypothesis requiring justification at the
moment.

Fig. 8 gave typical flame temperature variations of the four tests, providing more
information on the different cooling effect of the samples. In comparison to that of
Figs.8b and d, temperatures of the thermocouples in Figs.8a and c declined much
more quickly. It meant that the cooling effect of capsular particles and water mist
were much bigger than that of silica particles and ABC powders, reflecting the
cooling effect of water contained in samples A and C.

In addition to the cores of water, the shells of silica also contributed to fire
suppression. Neat silica particles could not extinguish the fires, but they could partly
suppress the flame (as shown in Fig.6b). Silica particles were inert, which would not
decompose in the flame. They would neither produce any species to scavenge
combustion radicals nor absorb heat (as shown in Fig.8b, the cooling effect of silica
was minor). But silica particles could act as a wall or window to inhibit the fire [18].
The solid particles as an inert wall could absorb part of FFRs’ energy to fast thermal
destruction or recombination of free flame radicals (FFRs) for collision with the
particle surface. As described by Krasnyansky, the surface defects of particles acted
as the centers of adsorption during the adsorption process and chain interruption
reactions [19]. Efficiency of heterogeneous inhibition of fire extinguishing powders
depended on several factors, such as surface area, adsorption properties, degree of
defects, etc. The silica particles with unique porous structure, nanosize, large surface
area and a lot of defects could effectively capture FFRs [20,21]. But such an effect of

10
heterogeneous inhibition alone was not strong enough to extinguish the fire. As
shown by the experimental results, the fire was just suppressed rather than
extinguished by neat silica particles. When combined with water to form capsular
particles, the fire extinguishing capacity of silica particles was greatly improved for
the synergetic effect.

For as-prepared capsular particles, the small size of water domains greatly enhanced
surface area to volume ratio in comparison with the equivalent reaction in bulk water,
which led to a marked increase of the contact between flame and water. From an
energy perspective, the DW method presented here a very simple route to produce
small sized water droplets and stored them in dispersed state without coalescence.
While in conventional method for producing small sized water droplets, specially
designed nozzles must be produced, which was time-consuming and costly.
Furthermore, the simple stirring technology could also be used to produce DW
particles containing different chemicals, offering a safe way to transport and storage
of various aqueous solutions in the form of solid powders.

3.4 Stability and toxicity

Dry water is a free-flowing powder obtained by mixing ordinary water and

hydrophobic nanoparticles of fumed silica at high speed in an air atmosphere. Due to
the presence of nanoparticles of fumed silica on the surface of the microdroplets, the
powder could be long time stored without coalescence. For as-prepared DW fire
suppressants, it was observed that could be stored in tanks for up to 12 months
(denoted as sample E) without coalescence of the droplets and the appearance of a
bulk water phase. As shown in Table 1, Fire tests revealed that extinguishing
performance of sample E was little affected by the long time storage.

Both water and silica were safe to human beings. Silica was usually used as a food
additive, which served as an anticaking agent to prevent various powdered ingredients
from sticking together. On one hand, there were not any toxic elements in silica and
11
water. On the other hand, the interaction between water cores and silica shells was
physical and no new substances were produced in the composite. Although toxic tests
had not been performed yet, the DW fire suppressant was believed to be safe for
human beings.

4. Conclusion

Gasoline pool fires were highly dangerous and difficult to be extinguished for its
volatility and flammability. Regular water mist and dry powders showed limited
capacity in extinguishing gasoline pool fires. In this article, a novel type of
water@silica core-shell particles was reported for extinguishing gasoline pool fires
with excellent performance.
· In the core-shell structured particles, the closely assembled hydrophobic silica
nanoparticles acted as the shells surrounding each water microdroplet core, which
provided the structural rigidity of the capsules and enabled their application as
solid powder fire suppressants.
· As-prepared capsular particles could extinguish 0.21 MW gasoline pool fire in 2 s
with agent mass of 0.055 kg, and 1.0 MW gasoline pool fire in 5 s with agent
mass of 0.49 kg, which greatly outperformed the conventional ABC powders, neat
silica powders and water mist.
· The clean, nontoxic and low cost powder suppressants were fabricated through a
simple stirring method. The behaved like solid powders with good flowability,
which could be long-time stored in dispersed state without coalescence.

In comparison to the conventional method for producing water mist, the DW method
presented here was more simple and convenient. In addition, fluidity and moisture
resistance of the resulted DW particles were similar to that of the conventional dry
powders, which ensured their compatibility with existing powder fire suppression
systems without any changes. Such DW powders are expected to be used for
scalability to actual fires for their advantages of easy production, high efficiency and
low cost. The present work just gave a preliminary study on the preparation,
firefighting capacity and mechanism of the water@silica particles, which provided

12
information for the numerical investigation on the suppression mechanism and
practical firefighting applications. More tests on the suppression efficiency and
mechanism of the capsular particles are in progress.

Acknowledgements
The work was supported by Fundamental Research Funds for the Central Universities
(No.WK23200000037) and National Natural Science Foundation of China (No.
51574120).

13
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14
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15
Table Legend and Figure Captions:
Figure 1 Schematic illustration of the experimental set up in a 27 m3 compartment
Figure 2 X-ray diffraction pattern of as-prepared capsular particles.
Figure 3 FTIR spectrum of as-prepared capsular particles.
Figure 4 Morphologic images of as-prepared capsular particles: (a) free-flowing
particles, (b) optical micrograph of the particles, (c) and (d) SEM images
of the particles.
Figure 5 Snapshots of the fire suppression processes of the tests (flame power = of
0.21 MW) with different samples: (a) sample A (capsular particles), (b)
sample B (silicon dioxides), (c) sample C (water mist), (d) sample D
(ABC powders).
Figure 6 Snapshots of the fire suppression process of the test (flame power = 1.0
MW) with capsular particles
Figure 7 TG-DSC of the capsular particles
Figure 8 Variation of the flame temperature in tests with four samples as
suppressants: (a) sample A (capsular particles), (b) sample B (silicon
dioxides), (c) sample C (water mist), (d) sample D (ABC powders).

16
Figure 1

Fig. 1
Figure 2

Relative Intensity (a.u.)

10 20 30 40 50 60
2(degree)

Fig. 2
Figure 3

 H2O
Si-OH
Si-O
Transmittance (a.u.)

 H2O
Si-O-Si

Si-O-Si

500 1000 1500 2000 2500

3000 3500 4000
-1
Wavenumber (cm )

Fig. 3
Figure 4

Fig. 4
Figure 5

0s 0.5 s 1.0 s 1.5 s 1.8 s 2.0 s

(a) Sample A (capsule particles)

0s 0.5 s 1.0 s 2.0 s 4.0 s 7.0 s

(b) Sample B (Silicon dioxides)

0s 1.0 s 2.0 s 3.0 s 8.0 s 12.0 s

(c) Sample C (neat water mist)

0s 0.5 s 1.0 s 2.0 s 4.0 s 7.0 s

(d) Sample D (ABC powders)

Fig. 5
Figure 6

0s 0.5 s 1.0 s 2.0 s

3.0 s 4.0 s 4.8 s

Fig. 6
Figure 7

110 10

100 Mass/%
DSC/(mW/mg)

90

80

DSC/(mW/mg)
5
Mass/%

70

60

50 0

40 o
59.26%, 136 C

30
200 400 600 800
Temperature (oC)

Fig. 7
Figure 8

800
800
capsule particles silica oxides
agent discharge
600 agent discharge
600

Temperature ( C)
Temperature ( C)

o
o

400 400

200
200

0
0
0 50 100 150 200 250 300 350 0 50 100 150 200 250 300 350
Time (s) Time (s)

(a) sample A (b) sample B

800
800

700 water mist ABC powders

600
agent discharge 600
agent discharge
Temperature ( C)

Temperature( C)
o

o
500

400 400

300

200 200

100

0 0
0 50 100 150 200 250 300 350 0 50 100 150 200 250 300 350
Time (s) Time (s)

(c) Sample C (d) sample D

Fig. 8
Table 1 Performance of the four samples in extinguishing gasoline pool fires
Table 1 Performance of the four samples in extinguishing gasoline pool fires

Samples Main composition Particle/droplet Flame power Extinguishing Mass of agent

size (μm) (MW) time (s) consumed (g)
Capsular particles
A 10~30 0.21 2.0 54.7
(40wt% SiO2 + 60wt% H2O)

Hydrophobic SiO2
B 0.03~0.05 0.21 --- 187.5
(95%SiO2 +5% surfactant)

Neat water mist

C 30~40 0.21 12.0 272.6
(100wt% water without additives)

Commercial ABC powder

D 70~100 0.21 --- 191.3
(50%NH4H2PO4 + 25%(NH4)2SO4)

Capsular particles
A 10~30 1.0 4.8 487.4
(40wt% SiO2 + 60wt% H2O)

Capsular particles stored for 1 year

E 10~30 0.21 2.2 52.1
(40wt% SiO2 + 60wt% H2O)

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