Full Paper
DOI: 10.1002/prep.201400238
Enhanced Combustion Characteristics of Bismuth Trioxide-
Aluminum Nanocomposites Prepared through Graphene
Oxide Directed Self-Assembly
Rajagopalan Thiruvengadathan,[a, b] Clay Staley,[a, b] Jordan M. Geeson,[a] Stephen Chung,[a]
Kristofer E. Raymond,[b] Keshab Gangopadhyay,[a, b] and Shubhra Gangopadhyay*[a]
Abstract: We present a facile, spontaneous, and surfactant-
free method to controllably self-assemble aluminum and
bismuth trioxide nanoparticles through the introduction of
graphene oxide as a self-assembly directing agent. The self-
assembled nanocomposites demonstrate significant com-
bustion performance improvements in comparison to ran-
domly mixed aluminum and bismuth trioxide nanoparticles
with enhanced pressure generation from 60 to 200 MPa,
pressurization rate from 3 to 16 MPa ms1, burning rate
Keywords: Graphene Directed self-assembly Combustion Nanocomposites Reactive materials Thermites
1 Introduction
The synthesis of nanocomposites is a strong and broaden-
ing field of research seeking to advance the capabilities of
conventional energetic material systems [110]. Energetic
nanocomposites are generally comprised of discrete fuel
and oxidizer particles with nanoscale dimensions. Nanopar-
ticle fuels and oxidizers enable very rapid reactivity as
a result of reducing the heat and mass diffusion lengths re-
quired for combustion. The arrangement and intimacy of
the fuel and oxidizer nanoparticles in energetic nanocom-
posites profoundly impacts reactivity. Maximizing fuel and
oxidizer interfacial contact is paramount for achieving opti-
mum reaction kinetics, and numerous approaches have
been reported with the goal of intelligently self-assembling
nanocomposites [3, 4, 7, 9, 11]. We have previously demon-
strated that functionalized graphene in the form of gra-
phene oxide (GO) can be employed as a self-assembly di-
recting agent to produce highly-reactive macroparticulates
of nanocomposites [9]. GO was shown to enhance the
energy content of aluminum and bismuth trioxide (Al/
Bi2O3) nanocomposites up to 92 % as a function of GO
weight percentage. Enhanced energy content was due to
improved fuel and oxidizer intermixing from self-assembly
as well as the participation of GO as a reactant during com-
bustion.
The motivation of this work was to evaluate the role of
GO directed self-assembly in modifying the combustion be-
haviors and ignition sensitivities of Al/Bi2O3 nanocompo-
sites. Al/Bi2O3 was the material system of interest here due
Propellants Explos. Pyrotech. 2015, 40, 729 734 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
from 1.15 to 1.55 km s1, and specific impulse from 41 to
71 s. The sensitivity of the self-assembled aluminum and
bismuth trioxide to electrostatic discharge was reduced by
four orders of magnitude, without decreasing the combus-
tion performance. Graphene oxide directed self-assembly
can be used to synthesize nanocomposites with diverse
combustion properties and controlled ignition sensitivity,
which lays the foundation for preparing multi-functional,
highly-reactive, combustion systems in the future.
to its high density, energy content, and gas production by
weight, which have encouraged many other recent studies
[9, 1216]. The pressure generating capability, linear com-
bustion rate, thrust behavior, and electrostatic discharge
(ESD) sensitivity of GO self-assembled Al/Bi2O3 were mea-
sured in direct comparison to randomly mixed Al/Bi2O3
nanopowders. Combustion behaviors were measured
across a range of % Theoretical Maximum Densities (TMD)
to evaluate the effect of GO self-assembly in various com-
bustion regimes [1517]. We postulate that the enhanced
energy content realized through GO directed self-assembly
extends towards predictably improving the combustion
performance of Al/Bi2O3 nanocomposites. The formation of
macroparticulates from the self-assembly process and
introduction of carbon also augers well for reducing the
ignition sensitivities of the nanocomposites, which in their
pure state can be extremely sensitive. The fundamental
[a] R. Thiruvengadathan, C. Staley, J. M. Geeson, S. Chung,
K. Gangopadhyay, S. Gangopadhyay
Department of Electrical and Computer Engineering
University of Missouri
Columbia, Missouri 65211, USA
*e-mail: gangopadhyays@missouri.edu
[b] R. Thiruvengadathan, C. Staley, K. E. Raymond, K. Gangopadhyay
NEMS/MEMS Works, LLC
8850 W. Westlake Road
Columbia, Missouri, 65203, USA
[] Authors contributed equally to work
729
Full Paper R. Thiruvengadathan, C. Staley, J. Geeson, S. Chung, K. Raymond, K. Gangopadhyay, S. Gangopadhyay
goal of this study was to synthesize highly-reactive nano-
composites with reduced sensitivity to ESD and enhanced
combustion performance through GO directed self-assem-
bly.
2 Experimental
Bi2O3 spherical nanoparticles (90210 nm avg. diameter as
per the specification by Accumet Materials, NY) and Al
spherical nanoparticles (80 nm avg. diameter, 80 % active
Al, 2.2 nm Al2O3 passivation as per the specification given
by Novacentrix, TX) were purchased and used as received.
GO was synthesized using the modified Hummers method
[18, 19]. Nanocomposites were prepared by mixing Bi2O3
and Al in accordance with an equivalence mixing ratio of
1.0 calculated from the theoretical Al/Bi2O3 reaction. The
Al2O3 dead mass was accounted in calculating equivalence
mixing ratios. Self-assembled nanocomposites were synthe-
sized by adding various amounts of GO to the Bi2O3 and Al
(0 % to 5 % GO by weight relative to weight of Al and
Bi2O3).
The exact synthesis protocols and fundamental science
driving the GO directed self-assembly of Bi2O3 and Al are
reported in our prior publication [9]. Briefly, Al, GO, and
Bi2O3 suspensions were separately prepared by dispersion
in a 1 : 1 volume ratio of 2-propanol (IPA) and N,N-dimethyl-
formamide (DMF) using ultrasonic agitation (output power
of 250 W at 44 kHz frequency) for varied durations of 4 to
8 h. While Al and Bi2O3 dispersions were prepared by sub-
jecting it to ultrasonic agitation for 4 h, and GO dispersions
in 1 : 1 volume mixtures of IPA and DMF were ultrasonically
agitated for 8 h. Precursor dispersion quality was evaluated
through zeta potential analysis (Delsa Nano C instrument,
Beckman Coulter), which showed + 70, + 40, and 59 mV
potentials for Al, Bi2O3, and GO suspensions respectively to
qualify precursor suspension stability [9]. The GO and Al
suspensions were mixed together, ultrasonically agitated
for 1 h, and then Bi2O3 suspensions were added and the
dispersions were sonicated for 1 h further. Following the
last mixing step, all suspensions were removed from the ul-
trasonic bath and left undisturbed until complete solids
precipitation upon self-assembly, which occurred in mi-
nutes to hours depending on GO content. Higher GO con-
tent (3.5 to 5.0 %) nanocomposites self-assembled within
2 min, while lower concentration nanocomposites (< 2.0 %)
self-assembled in 2436 h. Electron microscope images of
the precursor materials and self-assembled GO nanocom-
posites are presented in our prior work [9].
Combustion performance tests were performed on dried
nanocomposites. For this purpose, GO(x%)/Al/Bi2O3 nano-
composites were obtained by separating the precipitates
from the supernatant (suspension) phase through decanta-
tion. Subsequently, the precipitates were dried at 65 8C
under rough vacuum for 16 h. Al/Bi2O3 control samples
(without GO) were made following standard procedures re-
730 www.pep.wiley-vch.de 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
ported in our previous works [15, 16]. However, to remain
consistent in the preparation of samples with and without
the inclusion of GO, we have always used in 1 : 1 volume
ratio of DMF and IPA as the solvent system. Randomly
mixed Al/Bi2O3 samples were collected by drying well-dis-
persed suspensions of Bi2O3 mixed with Al at 65 8C for 16 h.
The pressurization rates of all nanocomposites prepared
in this work were determined by measuring the pressure
generated during the propagation of reaction front as
a function of time. For this purpose, a 60 mm3 closed com-
bustion cell (6.35 mm diameter, 2 mm depth) equipped
with a pressure transducer (PCB 119B12, 862 MPa maximum
rating, 400 kHz resonance frequency, 2 ms rise time) was
used. All of the samples were tested at approximately 14 %
TMD. The well was completely filled for each test with
dried nanocomposites without applying any external pres-
sure. A Ni-alloy fuse wire with a diameter of 0.13 mm was
used to ignite each sample. The slope of the rising pressure
signal from 10 % to 90 % peak pressure was used to quanti-
fy pressurization rate [8, 20]. At least three identical tests
were performed for each nanocomposite to account for ex-
perimental error. The pressure sensor was calibrated using
a hydraulic press with oil gauge before testing to quantify
sensitivity. Further details about the closed cell combustion
test measurement configuration are provided in our previ-
ous publications [8, 20].
A theoretical peak pressure was also calculated for each
nanocomposite for comparison to the experimental peak
pressures measured using closed cell combustion tests.
First the volume of gas evolved from the nanocomposite
was calculated at standard temperature and pressure using
the ideal gas law:
n1 RT 1
V1 1
P1
where V1 is the volume of gas generated in an unconfined
environment, n1 is the amount of gas in moles, R is the uni-
versal gas constant, T1 is standard temperature, and P1 is
standard pressure. The moles of gas produced were de-
rived using 0.0047 mol of gas per g for the theoretical Al/
Bi2O3 reaction, and assuming GO reacts purely as carbon
with ambient oxygen to produce 0.083 mol of gas per g
[21]. C-Bi2O3 and C-Al reaction pathways were neglected
from the calculation. The dead mass of the Al2O3 shell was
included in the calculation by reducing the mass of active
Al accordingly. Assuming an isochoric combustion process,
the pressure generated in the closed combustion chamber
of volume V2 = 60 mm3 is expressed as:
P1 V 1 T 2
P2 2
V 2T 1
where P2 is the closed cell pressure and T2 is the adiabatic
flame temperature of the nancomposite. [22] The adiabatic
Propellants Explos. Pyrotech. 2015, 40, 729 734
Bismuth Trioxide-Aluminum Nanocomposites
flame temperature of the Al/Bi2O3 reaction of 3253 K was
used for all nanocomposites regardless of GO content.
Combustion wave speed was measured using an optical
method, wherein a combination of photodiodes and fiber
optics, and a National Instruments data acquisition (NI
DAQ) board connected to a computer were used. A Lexan
tube of 3.2 mm inner diameter and of 95 mm length was
loaded with 250 mg of nanocomposites. The % TMD esti-
mated in this test configuration ranged from 4 to 5.5 %
TMD for various compositions. The loaded Lexan tube was
inserted into an aluminum block fitted with four fiber optic
photodetectors spaced 10 mm apart. The tube was open-
ended in all of the experiments. A spark gap igniter was
positioned at one end of the tube, and triggered to initiate
the reactions. Combustion wave speed was measured by
monitoring the detection of light from the flame front at
each photodiode as a function of time. The photodiodes
were positioned far away from the ignition end so that the
combustion wave speed was measured in the steady state.
Similar experimental arrangements for the combustion
wave speed measurements were reported earlier by several
research groups [8, 14, 23].
A thrust measurement configuration was used to investi-
gate the effects of GO on nanocomposite combustion per-
formance at approximately 55 % TMD. Dried nanocompo-
site powders were loaded in 1.6 mm diameter, 6 mm deep
combustion chambers in an iterative filling and cold press-
ing procedure (315 MPa applied pressure) until completely
full. The filled engines were mounted on a Kister 9222
thrust transducer, top ignited, and thrust force and burning
duration were measured to acquire total impulse. Specific
impulse, a metric of thrust efficiency, was calculated using
the thrust-time data and loaded nanocomposite mass [24].
Further details of the thrust measurement configuration are
provided in our prior work [15, 16].
ESD sensitivity measurements were performed using
a test system fabricated by Electro-Tech Systems (ETS) Inc
(Model 931) in accordance with standard US military proto-
cols as provided in MIL-STD-1751A. This instrument in-
cludes a capacitor bank (30020,000 pF), which can be
charged to a voltage ranging from 100 V to 26 kV. Typically
5 mg of nanocomposite powder was placed in a stainless
steel sample holder. The % TMD used in ESD measurements
for different samples in this work is about 4 %. The high-
voltage pin electrode (a stainless steel needle) was placed
1 mm above the surface of the powder prior to subjecting
the powder to 24 consecutive discharge cycles at a known
energy level typically beginning with the lowest energy
level of 0.16 mJ. If ignition was not observed, the voltage
and/or capacitance were increased, and the same sample
was again subjected to 24 consecutive discharges at
a slightly higher energy level until ignition occurred. A
sample was considered ESD safe for an energy level if it did
not ignite upon 24 consecutive discharges.
Propellants Explos. Pyrotech. 2015, 40, 729 734 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
3 Results and Discussion
Directly after synthesis, nanocomposites with higher GO
content by weight (3.5 % and 5 %) exhibited complete solid
phase precipitation within 2 min after being left undistur-
bed, while lower GO content nanocomposites ( 2 %) fully
precipitated from the solvent phase within 2436 h. The
complementary surface potentials of GO (59 mV), Al (+
70 mV), and Bi2O3 (+ 40 mV) in suspension (as obtained
from measurements using Zeta potential analyzer) pro-
motes electrostatic attraction in suspension [9]. Subsequent
chemical and electrostatic bonding in the short range (as
verified by XPS measurements) yield macroscale particu-
lates of self-assembled GO/Al/Bi2O3 that precipitate from
suspension [9]. It is important to note that the precursor
GO, Al, and Bi2O3, and Al/Bi2O3 suspensions remained stable
for several hours to days. Moreover, without GO directed
self-assembly, Bi2O3 and Al phase separate over time. There-
fore, to limit phase separation, randomly mixed Al and
Bi2O3 nanocomposites (0 % GO content) were prepared
using standard procedures, which are described in our pre-
vious publications [9, 15, 16].
The pressure-time profiles, theoretical peak pressure, ex-
perimental peak pressure, pressurization rates, and linear
combustion rates of the GO/Al/Bi2O3 nancomposites are
shown in Figure 1 and Figure 2 respectively. Peak pressure
generation increased with greater GO content from ca.
85 MPa for randomly mixed Al/Bi2O3 (0.0 % GO) to ca.
200 MPa for 5.0 % GO composites. Pressurization rate also
increased from 5.1 MPa ms1 for Al/Bi2O3 to 16.4 MPa ms1
for 3.5 % GO composites, but reduced to 10.5 MPa ms1 for
5.0 % GO composites. Theoretical peak pressure was shown
to increase with GO content. Linear combustion rates ex-
hibited a similar trend vs. GO content as pressurization rate
measurements. Average linear combustion rates of
1.15 km s1, 1.55 km s1, and 1.26 km s1 were observed for
randomly mixed Al/Bi2O3, 3.5 % GO composites, and 5.0 %
GO composites, respectively.
The relationship between GO content and increasing
peak pressure is attributed to greater gaseous product evo-
lution and the larger energy content available for nano-
composites with greater amounts of GO [9]. Differential
scanning calorimetry and thermogravimetric analysis (DSC/
TGA) of GO/Al/Bi2O3 showed GO functional group decom-
position and subsequent participation of GO as a fuel
(carbon) for Bi2O3 that occurs prior to the primary Al/Bi2O3
reaction [9, 25]. The evolution of gaseous CO species and
GO functional group decomposition promotes greater peak
pressures for higher GO content nanocomposites. The en-
hancements in pressurization and linear combustion rates
from randomly mixed to 3.5 % GO composites are attribut-
ed to improved fuel and oxidizer intermixing from self-as-
sembly and the energetic decomposition of GO. Decreased
pressurization rates and linear combustion rates from 3.5 %
to 5.0 % GO content composites are likely due to imbal-
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Full Paper R. Thiruvengadathan, C. Staley, J. Geeson, S. Chung, K. Raymond, K. Gangopadhyay, S. Gangopadhyay
Figure 1. Closed pressure cell measurements of GO/Al/Bi2O3
against GO content: (A) Pressure-time data. (B) Peak pressures and
pressurization rates (data points are average values from three in-
dependent tests one standard deviation).
anced stoichiometry offsetting the benefits of self-assembly
as GO participates as a fuel during combustion [9].
The theoretical peak pressure increased for nanocompo-
sites with greater GO content due to the extra gaseous
product evolution associated with the GO additive. For the
low GO content nanocomposites (0.0 % to 1.0 %) the theo-
retical peak pressure was substantially higher than the ex-
perimental peak pressure, likely due to partial phase sepa-
ration leading to incomplete combustion, and thermal
energy loss to the surroundings associated with the finite
time of the reaction. The difference between experimental
peak pressure and theoretical peak pressure reduced with
increasing GO content until 5.0 % nanocomposites, where
experimental pressure was measured to be higher on aver-
732 www.pep.wiley-vch.de 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
Figure 2. Linear combustion rates of GO/Al/Bi2O3 against GO con-
tent (data points are average values from three independent tests
one standard deviation).
age than the predicted value. This is likely due to not ac-
counting for the increased heat of reaction of GO in the
calculation and gaseous product evolution from GO func-
tional group decomposition.
The thrust behaviors of the GO/Al/Bi2O3 nanocomposites
are presented in Figure 3. With greater GO content, the
average thrust forces reduced while the burning durations
increased. Although it is intuitive to expect faster burning
durations for composites with larger amounts of GO, as ob-
served in the low % TMD tests (pressurization and linear
combustion rate), in high % TMD conditions, combustion is
dominated by a conductive thermal transfer mechanism as
opposed to the convective thermal transfer mechanism
that governs low % TMD combustion [5, 15]. Consequential-
ly, the increased thrust durations as a function of GO con-
tent are due to the participation of GO during combustion
as a slow burning reactant, which impedes the primary Al
and Bi2O3 reaction under conductive burning conditions.
Specific impulse (thrust efficiency) improved continuously
for composites with greater GO content from 41 s for ran-
domly mixed Al/Bi2O3 to 71 s for 5.0 % GO composites. Im-
provements in specific impulse were due to complete com-
bustion resulting from self-assembly and enhanced gas
production for higher GO content composites.
The ESD sensitivity of the GO/Al/Bi2O3 nanocomposites is
shown in Figure 4. Randomly mixed Al/Bi2O3 failed at
0.125 mJ (measured for 40 nm Bi2O3 and 41 nm Al in [13]),
but self-assembled GO/Al/Bi2O3 composites showed tre-
mendous reductions in ESD sensitivities. A maximum pass-
ing energy of 1.2 mJ was observed for 5.0 % GO compo-
sites. The possible reasons for the reduced ESD sensitivity
of self-assembled GO/Al/Bi2O3 composites to ESD are dis-
cussed as follows: Although the electrical conductivity of
GO is lower than that of pristine graphene, a recent work
Propellants Explos. Pyrotech. 2015, 40, 729 734
Bismuth Trioxide-Aluminum Nanocomposites
Figure 3. Thrust behaviors of GO/Al/Bi2O3 against GO content: (A) thrust-time data, (B) average thrust force, thrust duration, and specific
impulse (data points are average values from three independent tests one standard deviation).
has shown the electrical conductivity of GO (with similar
carbon to oxygen ratio of 2.3 as obtained in our work
versus 2.6 in their work) is 3.2 102 S cm1, which is quite
high [26]. Besides, the XPS data analysis reported in our
earlier publication[9] confirms the removal of oxygen
during the self-assembly with Al nanoparticles through
short range covalent interactions, which suggests the GO
obtains even greater electrical conductivity upon self-as-
sembly. In a study on the development of energetic nano-
composites with variable ESD ignition thresholds reported
by Foley et al., it has been shown that one can reduce the
Figure 4. Electrostatic discharge sensitivities of GO/Al/Bi2O3 against
GO content measured using ETS model 931 with a minimum
0.16 mJ spark. The randomly mixed Al/Bi2O3 (0 % GO) datum of
0.125 mJ lowest energy failed is provided by reference [17]. The
fractions above the lowest energy failed data points indicate the
discharge number when ignition occurred out of 24 consecutive
charge-discharge cycles.
Propellants Explos. Pyrotech. 2015, 40, 729 734 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
ESD sensitivity by increasing the electrical conductivity of
the composite [27].
Furthermore, the lower ESD sensitivity measured for GO/
Al/Bi2O3 composites in comparison to randomly mixed Al/
Bi2O3 is attributed to surface charge reduction due to the
formation of macroparticulates from the nanoparticle pre-
cursors due to self-assembly [9]. The surface charge density
of the nanocomposite powders can be inferred from zeta
potential analysis of the suspensions by interchanging zeta
potential with the surface field as has been illustrated in
the literature [28]. Our prior work has demonstrated a re-
duction in surface charge density from 23658 e mm2 for Al/
Bi2O3 nanocomposites to 300 e mm2 for GO/Al/Bi2O3 nano-
composites due to self-assembly. [9] Thus, the drastic re-
duction of surface charge density by nearly two orders as
a result of self-assembly on GO, and enhanced electrical
conductivity of the resulting nanocomposites are the signif-
icant factors in decreasing the ESD sensitivity by four
orders. Therefore in addition to facilitating self-assembly
and supporting enhanced reaction kinetics, GO proved to
be a viable mechanism for engineering the ESD sensitivity
of the self-assembled nanocomposites, which is a very val-
uable tool in the design of combustion systems.
4 Conclusions
We have shown that GO directed self-assembly can be har-
nessed to tune the combustion performance and ignition
sensitivity of Al/Bi2O3 nanocomposite through both the
self-assembly process and introduction of carbon as a terti-
ary reactant in the nanocomposite. Drastic improvements
in peak pressure generation, pressurization rate, combus-
tion rate, and specific impulse were observed when using
GO to direct the self-assembly of Al/Bi2O3 as opposed to
randomly mixing Al and Bi2O3 nanopowders. Additionally,
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Full Paper R. Thiruvengadathan, C. Staley, J. Geeson, S. Chung, K. Raymond, K. Gangopadhyay, S. Gangopadhyay
the ESD sensitivity of Al/Bi2O3 was reduced by four orders
of magnitude through GO directed self-assembly, without
impeding combustion performance. GO directed self-as-
sembly is a viable process for synthesizing highly-reactive
nanocomposites with application-tailored combustion be-
haviors and ignition sensitivities.
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Received: October 7, 2014
Revised: March 7, 2015
Published online: April 16, 2015
Propellants Explos. Pyrotech. 2015, 40, 729 734