1

American Institute of Aeronautics and Astronautics

Development of Insensitive High Energy Density
Nanomaterials

Ervin Beloni
1
and Edward L. Dreizin
2

New Jersey Institute of Technology, Newark, NJ 07102, USA
Energetic formulations with metal fuel additives are extensively used in propellants, explosives,
pyrotechnics, and incendiaries. Currently, replacement of regular metal powders with nanocomposite metal-
based materials is being considered. Such nanocomposite reactive materials are capable of very high reaction
rates while maintaining the high combustion enthalpies characteristic of metals. However, such novel
reactive nano-materials are often highly sensitive to impact, friction, and electrostatic discharge, making
them difficult to handle. In particular, their high electrostatic discharge sensitivity (ESD) was reported.
While ESD testing is very common and standardized, the mechanisms of powder ignition by electric spark
remain unclear. This project is aimed to establish the relationship between thermal ignition mechanism for
metal powders and related nanocomposites and their ESD sensitivity. Another objective is to develop
insensitive nanocomposite powders with high reaction rates and enthalpies. The project includes both
experimental and modeling components. An explicit numerical model of the heat transfer within a powder
bed subject to a pulsed electric discharge will be developed. The model will initially describe the behavior of
metal powders for which the thermal ignition kinetics is well established and quantified, such as spherical
magnesium. It will be further expanded for novel nanocomposite materials for which the kinetics of
exothermic processes leading to ignition will be determined in separate experiments. The predictions will be
validated experimentally using a standard ESD testing apparatus. Furthermore, the ignition sensitivity of
novel materials will be mitigated by coatings. The mitigation mechanisms will be described in the model and
validated experimentally. This paper will present initial model formulation as well as describe
nanocomposite powders with and without a desensitizing coating.


I. Introduction
he development of reactive materials on the micron to nano scale has been of interest in the past several years
1-
10
. The metal-based nanomaterials combine the high heat of combustion typical of metals with much accelerated
reaction rates. The reaction rates are increased due the large interface areas available for exothermic heterogeneous
reactions. Metal-based nanomaterials are being developed for uses in propellants, explosives, pyrotechnics, and
incendiaries. However, such materials are highly ignition sensitive when stimulated by electrostatic discharge
(ESD)
11-12
. Thus, reducing the ESD ignition sensitivity and understanding its nature are very important for further
development of energetic nanomaterials.
The current standards, such as USAF MIL-STD-1751A by which the ESD testing is performed today came about
through an effort in the 1940s by the US Bureau of Mines to test the hazards of explosives by electrical sparks
13
.
The sparks were produced by a test apparatus where a moving electrode needle discharged a spark upon approaching
the surface of the material. If some minimum threshold energy delivered to the powder caused sufficient chemical
reaction to produce enough heat to self-sustain further reaction within the remainder of the sample, ignition would
occur. The potential energy based on the capacitance of stored charge delivered to the pin electrode and the potential
difference between the electrodes offered a qualitative ranking of powder sensitivities. However the results of these
tests may be misleading and a number of issues need to be addressed before a reliable and useful ranking for new
reactive materials can be obtained.
There are two generic sets of issues that need to be addressed. The first set of issues has to do with the testing
procedure itself. Related test procedures for the ESD sensitivity of gas mixtures has been well developed and
documented
14
. It has been established that the material and shape of the electrodes, the discharge duration, the
presence of moisture, and other parameters affect the ESD sensitivity substantially. However, no comparable
studies are available for ESD sensitivity testing of powder-like materials. In the current testing standards, there is no

1
Graduate Research Assistant, Department of Mechanical Engineering, AIAA Member.
2
Professor, Department of Chemical Engineering, AIAA Senior Member.
T



2
American Institute of Aeronautics and Astronautics

clear guidance regarding the environmental factors that need to be considered, which could either accelerate or
mitigate ignition. There is also no detailed description for the shape and material of the high-voltage electrode. The
pin electrode used to transfer the stored charge from the capacitor to the test surface is important in how the
discharge is delivered to the surface. The pin shape affects the point of contact where the discharge will strike and it
is vital to have a consistent shape for repeatable results. Also pin material affects how the discharge energy is
transferred through the pin. For instance it has been reported that for high energies for nickel coated brass pins
which are typically used, the coating was vaporized which in turn reduced the discharge energy due to heat losses
13
.
The current standards do not specify the discharge duration, which can make it difficult to make meaningful
comparisons between different powders. In particular, the powder electric conductivity would affect the time
constant of the capacitor discharge, so that different discharge durations can occur for different powder tested using
the same experimental setup.
The second set of issues is unique to properties of powder-like energetic materials. For example, there is also
little to no guidance regarding the experimental pressure or sample confinement. In testing of propellants, pressure
can affect internal mechanical stresses which in turn affects ignition
15
. Confinement of the powder being tested can
be crucial as well. For example, it was reported that metal powders exhibit a greater ESD ignition sensitivity being
unconfined while black powder is more sensitive under confinement
13
. In addition to the issues common for all
powders, reactive nanocomposite materials pose additional challenges. Their inherently heterogeneous structure
with extremely developed reactive interface area can result in unusual thermal, mechanical, and electric properties,
all of which affect their ESD sensitivity. Some of the related heterogeneous processes have recently been
considered while modeling flame propagation for self-propagating high-temperature synthesis (SHS)
16
and similar
considerations are necessary for analysis of the ESD sensitivity.
Equally important to understanding the current practices and deficiencies in ESD testing is the mitigation of
sensitivity of the powders. The development of a coating to shield the powders from ESD is paramount in the
mitigation of sensitivity. Precipitation blending process developed at NASA for coating propellant binders can be
adapted to coat sensitive nanocomposite particles. As in previous work, Viton or a similar fluoropolymer (e.g.,
Flourel) protective coating
17
appears feasible. The coatings could offer thermal insulation between powder contact
points by increasing thermal resistance within a powder bed. However, the effect of coating and its thickness on the
reactivity of the nanocomposite powders as well as compatibility of specific nanocomposite powders with the
coating materials would have to be established. Such a tailoring of coatings would be necessary for various reactive
materials with different bulk compositions, surface morphologies, and particle sizes.
The goal of this work is therefore twofold. First, an understanding of ESD sensitivity as related to the ignition of
powders is to be established. A numerical model will be developed for the heat transfer in a powder bed subject to
ESD sparking. The numerical model will be developed and calibrated considering properties of spherical Mg
powder. This powder is selected as a benchmark material because of its well established properties and thermal
ignition kinetics. A connection will be made as to whether ESD is responsible for the thermal initiation of metal
powders. The numerical model solutions will be compared to actual experimental results based on current testing
methodology. The second goal of this work is to develop a reliable and simple process for desensitizing the reactive
nanocomposite powders. A Flourel-type coating will be developed for reactive materials produced by Arrested
Reactive Milling (ARM)
10,18
. The coated powders will be characterized experimentally. In the future, the model
will be validated for other metal powders and materials produced by ARM. The model will account for the
environmental effects, discharge duration, pin shape, and pin material factors not considered by current standards. It
is also expected that the model will be capable of describing behavior of coated powders as a function of the
coatings type and thickness. This paper presents only the initial effort aimed to achieve the goals stated above.


II. Model Formulations
A numerical heat transfer model was created for studying ignition by ESD. The powder is contained in a
cylindrical cup electrode. The domain in which the heat transfer is analyzed is a disk with elements taking the shape
of a series of inserted and stacked rings with central cylindrical elements, as illustrated in Fig. 1. The element radius
is r
m
and the elements vertical dimension is z
n
. The indices m and n were introduced to number ring-shaped
elements expanding in the radial direction, and elements stacked vertically, respectively.





3
American Institute of Aeronautics and Astronautics


For each element, the heat transfer equation is considered (with indices m,n removed for brevity) as
( ) ( )
Cond Conv Rad Disch Chem
T t t T t
VC Q Q Q Q Q
t

+
= + + + +

i i i i i
(1)
Where, is density, V is volume, C is specific heat, T is temperature, t is time, t is the time step and
i
Q
i
are
different heat transfer rate terms. For each control element, the external and internal radii were introduced as
, ,
,
mext min
r r , as shown in Fig. 1. For the central stack of cylindrical elements, m=1 and
1,
0
in
r = and the volume of
each control element was computed as
( )
2 2
, , , m n n m ext m in
V z r r = . The conductive heat transfer rate, in general,
included two axial (top and bottom) and two radial (internal and external) contributions, which were computed as:
, 1 , , 1 ,
, 1 , 1
1 1
1, , 1, ,
1, 1,
1 1
axi m n m n axi m n m n
Cond m n bot m n top
n n n n
rad m n m n rad m n m n
m n ext m n in
m m m m
T T T T
Q k A k A
z z z z
T T T T
k A k A
r r r r
+
+
+
+
+
+

= + +


+

i
(2)
where k
m,n-1
, k
m,n+1
, k
m+1,n
, and k
m-1,n
are the thermal conductivities of a specific control volume at the bottom, top,
exterior, and interior surfaces.
axi
bot
A ,
axi
top
A ,
rad
ext
A , and
rad
in
A are the bottom, top, exterior, and interior areas
respectively. They are calculated as
( )
2 2
, ,
axi axi
bot top m ext m in
A A r r = = and
,
2
rad
ext m ext n
A r z = and
,
2
rad
in m in n
A r z = (3)
For the top layer elements, there is only bottom axial contribution to
this heat transfer term. For the elements at the boundaries, the
boundary temperature is assumed to be equal to the room temperature.
For the central stack of cylindrical elements, there is only one radial
contribution (external) and the external radius of the cylinder is used to
calculate the surface areas. The thermal conductivity of the powder
bed which is constant is determined using a laser flash technique
19
. It is
primarily determined by the thermal resistance of the particle-particle
contacts while the thermal resistance of the bulk material (magnesium)
is negligibly small. Therefore, the control volume element dimensions
can be considered comparable to the size of the particle. This way, the
temperature within each particle equilibrates nearly instantaneously,
while the rate of conductive heat transfer between the particles is
relatively low. This rate is changing rapidly when the particles
experience phase changes, such as melting and boiling. In this initial
model, the change in the thermal conductivity upon melting is
neglected assuming that the oxide layer surrounding each Mg particle is
sufficiently rigid, so the molten particles still retain their nearly
spherical shapes. However, the thermal contact resistance must change
when the particles experience boiling. In this model, it is assumed that
the thermal conductivities of all the control volume elements adjacent
to the boiling element become equal to that of bulk Mg. Thus, if a
control element m,n is boiling, there must be no element above it and
for elements m-1,n; m+1,n; and m,n+1, the value of k is adjusted.
To consider melting and boiling in the context of the heat transfer
balance analysis, the gravimetric enthalpies of melting H
melt
and
boiling, H
boil
, are introduced. Once the melting temperature is reached for an element, its temperature is not
allowed to increase above the melting point until the following condition is met
,
,
i j m n melt
i j
Q t V H

(4)

Figure 1 Geometry of the
Computational Domain


4
American Institute of Aeronautics and Astronautics

where index i indicates the summation over all the heat transfer rate terms and index j shows summation over a
range of time steps during melting. The boiling is considered in a similar fashion. Once the boiling temperature is
reached for an element, its temperature is not allowed to increase above the boiling point until the following
condition is met.
,
,
i j m n boil
i j
Q t V H

(5)
H
boil
is the gravimetric enthalpy of boiling in condition (5).
As noted above, the thermal conductivities of the control elements adjacent to the boiling one are adjusted to
account for an enhanced heat transfer. Once the element is boiled off, the adjacent element below is modified to
account for convective heat transfer and if appropriate discharge input.
The convective heat transfer term,
Conv
Q
i
is calculated only for the elements in the top layer or for elements that
appear at the top when the layers above them evaporate. It is calculated assuming that convection occurs with
ambient air at room temperature, T

and that it can be described as natural convection over a flat plate.

Furthermore, the characteristic dimension of the top plate was assumed to be equal to the area directly heated by the
electric discharge. Therefore, the characteristic plate dimension was assumed to be equal to the radius of the
discharge column (see details below), r
disch
. Respective Rayleigh number, Ra, was calculated as
20

( )
3
,
2
Pr
m n disch
g T T r
Ra
v

= (6)
where g, is the gravitational constant,
1
film
T
= is the coefficient of gas thermal expansion calculated assuming
that air is an ideal gas at the film temperature
,
2
m n
film
T T
T

+
= , Pr and are Prandtl number and the kinematic
viscosity, respectively, both taken at film temperature. Dimensionless heat transfer coefficient, or Nusselt number
was then calculated as
20
:
0.25
0.54 Nu Ra = (7)
Finally, the convection heat transfer term was calculated as
( )
,
axi
air
Conv m m n
disch
k
Q Nu A T T
r

=
i
(8)
where k
air
is the thermal conductivity of air at the film temperature.
Similarly to the convection term, the radiation term is also calculated for the top layer only or for the
elements that appear at the top when the elements above them evaporate. The external wall surfaces also are
assumed to be at room temperature, so:
( )
4 4
,
axi
m m n Rad
Q A T T

=
i
(9)
where

is the emissivity of the powder and is Stefan-Boltzmann constant.
The energy from the electric discharge was assumed to decay in time exponentially. The time constant of this
decay, is determined by the characteristic of the respective electric circuit, =RC, where R is the equivalent
electrical resistance of the powder bed and C is the capacity of the high-voltage capacitor used to produce the
electric discharge. In the present model, the change of powder bed resistance as a function of time is neglected and
the value of is considered as a constant. In the future, this assumption can be relaxed. In addition to , the overall
discharge energy, Q, is considered as a constant. This energy can be selected to match the experimental data on the
minimum ignition energy measured for different materials. In addition, it is assumed that the discharge energy is
distributed spatially and a Gaussian energy density profile with a standard deviation was introduced. The
following equation was obtained for the discharge energy heat transfer rate as a function of the radial position and
time:
( )
2
2 2
, exp exp
2 2
axi m
m m Disch
r Q t
Q r t A

| |
| |
=
| |
\
\
i
(10)


5
American Institute of Aeronautics and Astronautics

The radius of discharge (used in Eq. (10) above) was introduced as
3
disch
r
= (see Fig. 1).
Finally, the term describing an exothermic reaction in the powder that can lead to the thermal runaway and self-
sustaining reaction,
Chem
Q
i
was analyzed. For thermal ignition of metallic particles, this chemical heat transfer
rate term is usually described using an Arrhenius function
21-22
:
0
,
,
exp
A
Chem m n
m n
E
Q V Z H
RT
| |
=
|
\

(11)
where H is the volumetric enthalpy of oxidation, E
A
is activation energy, Z is the pre-exponent, and R is the
universal gas constant. This expression describes the heat release due to a heterogeneous reaction while the amounts
of reactants are unlimited. The formalism is well suited for description of ignition of individual particles. For metal
particles, it is usually assumed that when a particle ignites, its temperature rapidly increases to the metals boiling
point and the reaction rate is no longer described by Eq. (11). Instead, it can be limited by the kinetics of the vapor-
phase reactions for very fine (typically, less than 1 m) particles or by the rate of oxygen diffusion to the flame for
particles of larger dimensions
9,23
. In the case considered here, it must be expected that at least some particles will
ignite and thus Eq. (11) will stop being valid for describing their reaction rate. On the other hand, it is important to
have a description of this heat transfer rate term valid even after ignition of some portion of the powder bed has
occurred. This description may be critical for understanding the mechanisms of ignition in the powder bed.
Because the dimensions of the entire bed are large, it is assumed that when a particle (or a specific control element)
ignites, its reaction rate will be limited by diffusion. Because the development of a full diffusion model is outside
the scope of this project, a number of simplifying assumptions is made and described below.
The number of moles of oxygen consumed as a result of reaction described by Eq. (11) during a single time step,
M, is calculated as
2
0
Chem
O
Q
M t
H
=

(12)
where
2
O
H is the combustion enthalpy normalized per mole of O
2
. The value of M was compared to the total
number of moles of oxygen available for reaction, M
0
. Initially, it was assumed that oxygen can be available from a
gas layer above the powder bed with a thickness h
ini
determined by the time step, t:
ini
h D t = , where D is the
gas diffusion coefficient calculated as
1.75
2
5
1.8 10
273
film
T
m
D
s

( | |
=
| (
\
(13)
Thus, for each stack of control volume elements, m, the total number of moles of oxygen available for reaction
during a single time step was estimated as

| |
0 2
axi
m ini
M O A h

= (14)

where | |
2
O

is the concentration of oxygen in air. When the amount of oxygen consumed during a time step
becomes a noticeable fraction of the oxygen available for the reaction, a correction is introduced. Therefore, the
following condition was introduced:
0
0
D
t
M
X
M

>

(15)
where X<<1 is an arbitrarily selected constant that is chosen to be equal to 0.05 for the initial calculation. Before
condition (15) is satisfied, the effect of diffusion on the reaction rate is considered negligible and the heat transfer
term
0
Chem Chem
Q Q =

. It is also assumed that the chemical reaction can occur in any layer of the powder bed, e.g.,
the diffusion resistance of the porous powder bed is neglected. After condition (15) is satisfied, it is assumed that


6
American Institute of Aeronautics and Astronautics

diffusion started to play a noticeable role in limiting the rate of chemical reaction. The chemical reaction is now
only allowed in the top layer of the powder bed, which is exposed to the ambient gas directly. A specific time t
D
, is
introduced when condition (15) is satisfied and for all times t>t
D
, the total number of moles of oxygen available for
reaction is computed as
| | | | ( ) ( )
2 2
axi axi
av top m D
M O A h O A D t t t

= = + (16)
In other words, the thickness of the layer of diffusion influence, h, or the layer from which the oxygen available for
reaction can diffuse to the reacting surface is calculated to increase in time. At the same time, a decrease in the
oxygen concentration at the surface of the sample is estimated. The estimate assumes a linear oxygen concentration
profile in the zone of diffusion influence, so that:
| |( )
0
2
t
av j
axi
top
M M
O t
A h

=

(17)
where for each new time step, the values of M are calculated considering the values of
Chem
Q

calculated for the

previous time step. The heat transfer rate term
Chem
Q

for each time step after t>t

D
is calculated using the Arrhenius
equation (18) with a corrected pre-exponent:
| |( )
| |
2
,
2 ,
exp
A
Chem m n
m n
O t E
Q V Z H
O RT

| |
=
|
\

(18)
Finally, if the oxygen concentration is half of | |
2
O

the amount of moles of O
2
consumed is estimated as:
( ) ( ) | |
2
1
2
axi
top
M t A D t t Dt O

(
= +

(19)
Based on the consumption of O
2
based on equation (19), the heat transfer rate term
Chem
Q

is defined as
( )
2
O
Chem
M t H
Q
t

=

(20)
To accelerate the computations, an adaptive time step is used. When the temperature increase in a control
element over a single time step increases a pre-selected threshold value, the time step is reduced by a factor of two
and the calculation is repeated. When the threshold value is not exceeded, the time step is allowed to increase for
the following calculation cycle. The specific procedure for increasing the time step is based on the computed
maximum temperature increase
max
, m n
T in a single control volume. This increase is compared to the pre-selected
threshold value, T
0
and a characteristic temperature difference for the specific time step,
step
T is calculated
max
, 0
0
m n
step
T T
T
T

=

(21)
The factor by which the time step for the next cycle of calculation is increased is directly proportional to this value.


III. Experimental
A schematic diagram of the experimental setup is shown in Fig. 2. ESD testing in accordance with the MIL-STD-
1751A standard will be performed suing a Model 931 Firing Test System by Electro-Tech Systems, Inc. Free
metallic powder is placed into a stainless steel cup 15 mm in diameter and 3 mm in depth which is affixed to a
grounded base. A capacitor bank stores charges in the range of 100 pF to 0.5 F and resistances vary between 0 to
5000 . The discharge pulse voltage that can be produced by the apparatus is on the order of 100 V to 26 kV. The
spark produced from the pin electrode traveling to the cup electrode strikes the powder surface; if sufficient
threshold energy is supplied at a specified capacitance and voltage, the powder ignites.


7
American Institute of Aeronautics and Astronautics

The tests will be performed in a controlled environment chamber. A data acquisition system will be used to
measure the pulse duration and current versus time dependence.

Figure 2 - Experimental setup to perform ESD tests on metallic powders


IV. Materials
Reactive nanocomposite materials to be
tested for ESD sensitivity and for which the
ESD sensitivity will be mitigated by coatings
are nanocomposite powders produced by
ARM. The ARM technique is based on
mechanical milling and is described in detail
elsewhere
8,10,18
. Materials produced by ARM
are capable of highly exothermic and rapid
reactions owing to their compositions and
heterogeneous structure
14
. Particular ARM
materials that are of interest to be tested by
ESD are Al-Ti alloys, Al-MoO
3

nanocomposites, and B-Ti nanocomposites.
Figure 3 shows an example of a typical
scanning electron microscopy image for a
nano-composite of B-Ti in which B and Ti are
mixed and combined at the nanometer scale.
As noted earlier, before testing and
desensitizing ARM materials, benchmark
experiments will be performed with a
commercially available spherical Mg powder.



V. Coatings
Inert coating is a technique being tested to reduce the ESD ignition sensitivity of energetic powders.
Conceptually similar approach was used to desensitize some of the US Navy pyrotechnic formulations
8
. The
formulations included compositions of magnesium, Teflon, and Viton (MTV) as well as nanosized aluminum
powders known under a brand name ALEX
8
. Pre-coating ALEX powders with Viton was found to reduce the
formulation sensitivity from 0.2 to 1.8 J
8
. Thus, it is clear that a Viton coating can significantly reduce the ESD
sensitivity. A similar Fluorel coating will be used for ARM nano-materials in this work. The coating technique used
is based on precipitation blending. A schematic diagram of the coating apparatus is shown in Fig. 4. Before
blending, a solution of Viton is dissolved in acetone. The solution is added into the container along with the powder

Figure 3 SEM image of B-Ti nanocomposite produced by ARM


8
American Institute of Aeronautics and Astronautics

to be coated. After a short period of mixing n-
hexane is added to the stirring mixture acting as
counter-solvent. The adding n-hexane leads to
precipitation of Viton out of solution. The
precipitated Viton solids stick to the surface of
the powder forming the desired coating. In the
schematic in Fig.4, the baffle serves to increase
the turbulence while the solvent/counter-solvent
and powder particles are stirred together. The
funnel and tube allows for the n-hexane to be
directed to the impeller so that it is evenly
distributed within the stirring solution. The wet
powder is poured into a sieve and further washed
with n-hexane to rid of any acetone that may
remain. The powder is then desiccated to remove
any remaining solvent/counter-solvent left on the
powder surface. An alloy with bulk composition
Al
2
Ti was used in the initial coating experiments.
This material was selected because it was readily
available and because the particle surface
morphology for this powder is very similar to
that of nanocomposite powders of interest in this
paper. An SEM image of the coated powder produced by this method is shown in Fig. 5. The image was taken at a
low electron beam voltage to resolve the surface features of a relatively thin, light-element based coating. The
rough surfaces shown are the exposed metallic surface that has not been coated. The smooth surface is Viton
coating. It is the objective of this work to produce a continuous coating layer on the particles.




























Figure 4 - Setup for coating of ESD sensitive powders by
precipitation blending

Figure 5 SEM image of coated Al
2
Ti powder


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American Institute of Aeronautics and Astronautics

VI. Conclusion
A heat transfer model was developed to determine whether the thermal initiation is the main cause of powder
ignition under the ESD stimulation. The model will be further developed and calibrated using a spherical Mg
powder as a convenient benchmark. The model considers the conductive heat transfer in a powder bed, which is
controlled by the thermal resistance of particle contacts. The model relies on an experimentally determined thermal
diffusivity in the powder bed. The model neglects the Joule heating of the powder and considers a spatially and
temporally non-uniform energy flux as an energy input from discharge to the powder. It also includes convection
and radiation heat transfer terms. The chemical reaction is introduced and described by an Arrhenius function. The
limitations on the reaction rate due to the finite rate of oxygen diffusion to the reacting surface are also considered.
A precipitation blending technique was adapted to coat metallic and nanocomposite powders with different
compositions with a thin protective surface layer of Fluorel (a Viton-like fluoropolymer). SEM imaging showed
that the uniform and continuous coating is achieved when about 10 volume % of Fluorel is used.
In the future, the model will be validated for a wide range of powders and testing conditions and used to study
and understand the mechanisms of ESD ignition sensitivity of reactive materials. Parametric studies, both
computational and experimental, will be conducted to establish the effect of the discharge power, duration, electrode
material and shape and other parameters on the ESD sensitivity of selected reactive powders. The effect of gas
environment will be addressed in particular. The findings from the study will then be incorporated into the ignition
model to further the understanding of ESD powder ignition processes. Lastly, using the precipitation coating
technique tailored engineered coatings will be developed for different reactive materials. An engineering study will
be performed to optimize the coating thickness for mitigating the powders ESD sensitivity and improving their
performance.


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1
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3
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5
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6
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