Full Paper
Influence of Particle Size and Mixing Technology on Combustion of
HMX/Al Compositions
Nikita Muravyev*, Yurii Frolov, Alla Pivkina, Konstantin Monogarov, Olga Ordzhonikidze
N. N. Semenov Institute of Chemical Physics, Russian Academy of Sciences, Moscow 119991 (Russia)
Ivan Bushmarinov, Alexander Korlyukov
Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, Moscow 119991 (Russia)
Received: January 18, 2010; revised version: February 16, 2010
DOI: 10.1002/prep.201000028
Dedicated to Dr. Bernard E. Douda on the occasion of his 80th birthday
Abstract
In this work, two widely used components of high-energy
condensed systems – HMX and aluminium – were studied.
Morphology, thermal behaviour, chemical purity and combustion
parameters of HMX as a monopropellant and Al/HMX as a
binary system were investigated using particles of different sizes.
It was shown that in spite of the differences in composition and
particle size, combustion velocities are almost identical for
micrometer-sized HMX (m-HMX) and ultrafine HMX (u-
HMX) monopropellants under pressure from 2 to 10 MPa.
Replacement of the micrometer-sized aluminium with ultrafine
one in the system with m-HMX leads to a burning rate increase by
a factor of 2.5 and the combustion completeness raise by a factor
of 4. Two mixing techniques to prepare binary Al/HMX compo-
sitions were applied: conventional and wet technique with
ultrasonic processing in liquid. Applying wet mixing results in a
burning rate increase of 18% compared to the conventional
mixing for systems with ultrafine metal. The influence of the
components particle size and the composition microstructure on
the burning rate of energetic systems is discussed and analysed.
Keywords: High-Energy Condensed Systems, Ultrafine HMX,
Ultrasonic Mixing
1 Introduction
A need to improve the performance of solid rocket motors
requires an enhanced efficiency of the solid propellants.
Nowadays, along with the elaboration of new energetic
components, a growing attention is paid to an upgrading of
the existing components by decreasing the particle size
down to nanometer-scale and by changing the physical and
chemical state of the particle surface. According to the
literature, the intensive study of the nanometer-sized high-
* Corresponding author; e-mail: a7777@center.chph.ras.ru
226 Propellants Explos. Pyrotech. 2010, 35, 226 – 232  2010 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
energy components and of compositions with nanometer-
sized components shows that the burning rate could be
sufficiently increased in comparison to systems with con-
ventional components. At the same time, the pressure
dependence of the burning rate, the ignition delay time and
the agglomeration phenomena could be decreased.
A typical nitramine is octahydro-1,3,5,7-tetranitro-
1,3,5,7-tetrazocine (C4H8N8O8), known as HMX, one of
the most important energetic ingredients of various propel-
lants and explosives. Four different polymorphs are known
for HMX, a to d. Preferable for high-energy systems is the b-
form with the highest density and the lowest impact
sensitivity. The HMX-based systems have many advantages,
i.e.: high density, potentially high specific impulse, low
signature compared to ammonium perchlorate, lower
toxicity and corrosion. However, their combustion charac-
teristics are somewhat non-ideal. For a given HMX-
energetic binder composition, the burning rate law is locked
[1] and there is no way to tailor it by decreasing the particle
size (as it can be done for ammonium perchlorate) [2].
Furthermore, the pressure exponent is too high to be
acceptable for a rocket motor operation. The attempts to act
upon the HMX burning rate by the use of catalysts have not
been successful [1, 2]. One of the ways to tailor the gas phase
zone, where the highest energy release takes place, is the
addition of aluminium powder.
Aluminium is one of the main components in propellants
with a typical amount of about 20%. Many factors, such as
the metal content (activity), the particle size of the
aluminium powder and its spatial localization within a
propellant can influence the combustion characteristics and
define the chemical and two-phase losses of the specific
impulse.
Influence of Particle Size and Mixing Technology on Combustion of HMX/Al Compositions
Our previous work [3] shows that a monopropellant of
pressed nanometer-sized RDX (C3H6N6O6) particles, pro-
duced by a vacuum deposition technique, exhibits a two
times greater burning rate than that of micrometer-sized
RDX at an elevated pressure. Recently [4], it was found that
the detonation velocity of ultrafine HMX (u-HMX) par-
ticles, synthesized by a pulverization drying, is higher than
that of conventional HMX at the same density, whereas the
impact sensitivity remains the same [5]. The feasibility of
ultrafine material benefits from nitramines phase compo-
sition, because usually submicron HMX is formed in
polymorphs, other than b [6, 7].
This paper deals with the combustion parameters of u-
HMX, produced by a cryochemical technique (details of the
production technique are presented elsewhere [8]). The
morphology, the mixing quality and the combustion param-
eters of mono- (HMX) and binary (Al/HMX) compositions
are investigated using particles of different size.
2 Experimental Part
2.1 Materials
The materials used in this work were: u-HMX, micro-
meter-sized HMX (m-HMX), two types of micrometer-
sized aluminium, i.e., ASD-4 (M-Al) and ASD-6 (m-Al),
and ultrafine aluminium ALEXTM (Argonide Corporation,
USA; u-Al). The mass fraction of the aluminium additive to
HMX was constant and equal to 25%. Additionally, a binary
system with aluminium oxide (reagent grade) instead of
aluminium was investigated.
2.2 Equipment
The energetic materials were generally characterized with
regard to the particle mean size, purity, thermal and
combustion properties.
To investigate the morphology of the materials scanning
electron microscopy (SEM, Phenom and Quanta 200 3D,
FEI, The Netherlands) and atomic force microscopy (AFM,
NTEGRA Prima, NT-MDT, Russia; cantilevers Tl02,
MikroMash, Estonia with curvature radius  10 nm) were
used. The BET surface area was measured with FlowSorb
III 2305 (Micromeritics, USA) by measuring the adsorption
of a gas mixture (30%N2/70%He) on the powders surface.
The particle size distributions (PSD) were obtained using
laser diffractometry (Laska-1K, Lumex, Russia and Master-
sizer 2000, Malvern, England).
The investigation of the thermal behaviour was carried
out using a simultaneous thermal analyzer STA 449PC
(NETZSCH, Germany). Differential scanning calorimetry
(DSC) and thermal gravimetric analysis (TGA) data were
recorded in the same experiment. For HMX samples with a
sample mass of  2 mg and at heating rates from 0.5 to 50 8C
min1 experiments were performed in closed alumina pans
with pierced lids under dynamic argon flow (70 mL min1).
Propellants Explos. Pyrotech. 2010, 35, 226 – 232  2010 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
A heating rate of 10 8C min1 (covering the temperature
range from 20 to 1100 8C) was employed to determine the
aluminium content within the initial metal powders and
within the agglomerates collected during the combustion of
the binary compositions. A comparative technique based on
the analysis of the endothermic melting peak of a reference
metal sample and the sample under study was applied.
Powder X-ray diffraction (XRD) patterns were recorded
in transmission mode in a 2V range from 10 to 608 on a
diffractometer D8 Advance (Bruker, Germany) with
curved Ge(111) monochromator. The pure Cu Ka1 (lav ¼
154.06 pm) radiation was used. Samples were deposited
on a sticky tape, the opening of LynxEye position sensitive
detector was set to 38, and the measurement was performed
in V/2V continuous mode with a step size of 0.0093758
and a scanning speed of 0.58 min1. The experimental
patterns were analysed using the DIFFAC Topas program
suite.
Initial components were mixed in a Turbula-type mixer
for 60 min (the so-called conventional mixing). An ultra-
sonic probe SONOPULS HD2070 (Bandelin, Germany)
was used to prepare compositions by wet mixing technique
at 30 – 60% of the maximum power (70 W) and a frequency
of 20 kHz. After mixing, the compositions were pressed by a
cold isostatic technique at a pressure load of 350 MPa for
3 min. The sample pellets were cylindrical, 8 mm in diam-
eter, coated on the lateral surface with an epoxy. The
experimental investigation of the burning rate was per-
formed using a constant pressure bomb (volume 1.5 L)
under nitrogen and argon atmosphere. The combustion
velocity was measured using a digitized pressure-time signal
and a high-speed video recording (1200 fps, Casio EX-F1,
Japan) with an accuracy of  5%. To collect the condensed
combustion products (agglomerates) from the burning
surface a quench particle collection bomb technique
(QPCB) [9, 10] was used.
3 Results and Discussion
3.2 Initial Components
3.1.1 Aluminium
The particles of the micrometer-sized aluminium are
spherical with an average volume diameter D43 of 3.3 mm for
m-Al and 8.5 mm for M-Al, as was obtained from the SEM
image processing. A particle size distribution with D43 ¼
180 nm was obtained by the analysis of AFM images of
ultrafine aluminium ALEX. The XRD pattern of the u-Al
sample reveals the presence of only one crystalline phase –
metal aluminium, and the absence of crystalline Al2O3 and
AlN; apparently alumina is present in the amorphous state.
Table 1 summarizes the PSD characteristics, i.e., the
average linear hDi, surface D32 and volume D43 diameters,
the BET specific surface SBET and the active aluminium
content CAl of the investigated powders in comparison with
some literature data. There is a difference between obtained
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Full Paper N. Muravyev, Y. Frolov, A. Pivkina, K. Monogarov, O. Ordzhonikidze, I. Bushmarinov, A. Korlyukov

Table 1. Characteristics of aluminium powders.

Powder hDi D32 D43 SBET CAl
(mm) (mm) (mm) (m2/g1) (%)
M-Al 2.8 6.5 8.5 4.4 98
[11] 4.3 7.4 10.1
[12] 1.23 4.34 7.34 0.512
m-Al 1.4 2.7 3.3 1.4 95
[12] 0.85 4.72 0.739
[11] 4 5.2 6.5
u-Al 0.12 0.17 0.18 11.9 84
[12] 0.12 0.16 0.18 13.89
[13] 0.49 11.3 86

data and literature values, caused by using a numerical PSD Figure 2. AFM image of the u-HMX fine fraction.
in our calculations, whereas authors [11 – 13] examined
weight or volume distributions. The value of SBET for M-Al
powder, measured by a gas adsorption, unlike data in Ref.
[12] obtained by gas permeability, characterizes the surface
roughness rather than the dispersity.

3.1.2 HMX

The effective particle size of the conventional m-HMX

powder derived from the BET surface area (0.3 m2 g1) is
11 mm. The PSD with D32 ¼ 37 mm and D43 ¼ 39 mm was
obtained by laser diffractometry. A typical SEM image of
the coarse particles of m-HMX is shown in Figure 1a.
An SEM image of the as-received u-HMX powder is
Figure 3. Density of the volume PSD (fv) for u-HMX.
presented in Figure 1b. For the AFM investigation of the
finest particles a specially elaborated procedure was con-
ducted [14]. Figure 2 presents an image of the finest fraction;
a height bar is shown on the right side. The effective
diameter of the u-HMX particles obtained from SBET (1.9 m2
g1) is 1.6 mm, which is close to the literature value of
1.38 mm received for u-HMX produced by pulverization
drying [5]. The laser diffractometry curve is shown in
Figure 3. Re-calculation of the volume PSD to the numer-
ical one reveals that most particles (> 85%) have submi-
crometer size.
The above-mentioned methods clarify a complex struc-
ture of u-HMX: nanometer-sized (20 – 50 nm) and submi-
crometer sized particles ( 300 nm), corresponding to the
first mode in PSD, constitute porous conglomerates with
sizes about 10 mm (second mode in PSD, Figure 3). Figure 4. Diffraction patterns of as-received (A) and pressed (B)
u-HMX.

X-ray analysis of as-received u-HMX reveals that the

Figure 1. SEM images of the: (a) m-HMX; (b) u-HMX.
powder contains two polymorphs, i.e., a and b-HMX
(pattern A, Figure 4). According to Rietveld refinement
data, the u-HMX powder consists of a (40 wt.-%) and b
(60%) phases (Rp/Rwp/Rexp ¼ 3.1/4.26/3.28). The Lorentzian
crystallite size for both polymorphs, calculated according to
[15], exceeds 400 nm, so the exact value could not be
estimated, as at the high crystallite size the instrumental line
broadening overcomes the effects of the crystallite size.

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Influence of Particle Size and Mixing Technology on Combustion of HMX/Al Compositions

During the sample fabrication for the combustion experi-

ments the u-HMX particles are subjected to a pressure
loading. It is known from the literature [7] that a phase
transition can occur during pressing of u-HMX powder. To
investigate this effect X-ray analysis of the pressed pellet of
u-HMX was performed. The pressing of the u-HMX
particles results in a change of the polymorphs ratio and
the crystallite size (pattern B, Figure 4). The content of a
phase, according to Rietveld refinement (Rp/Rwp/Rexp ¼ 1.42/
1.96/1.15), decreases to 31 wt.-%. The Lorentzian crystallite
size of both polymorphs decreases by an order of magnitude,
i.e., to 53 nm for a polymorph and 77 nm for b one.
Moore reported that g polymorph of u-HMX completely Figure 6. Peak phase transition temperature versus heating rate:
transforms into b-phase under a loading of 207 MPa for u-HMX (grey points and line) and m-HMX (black).
5 min [7]. We observed a 10% conversion of a ! b for u-
HMX after a pressure loading of 350 MPa for 3 min. Both
results qualitatively correspond to Brills data obtained in a (average on three experiments) at a heating rate of 5 8C
diamond anvil cell, i.e., a-HMX is stable up to 4200 MPa, min1.
whereas g-HMX transforms into b-HMX at 550 MPa [16].
The DSC and TG curves obtained for m-HMX and u-
HMX powders during heating with a constant rate of 10 8C 3.2 Binary Compositions
min1 are presented in Figure 5. The endothermic peak at
192 8C corresponds to the phase transition b ! d of m-HMX, Figure 7 presents SEM images of the pressed pellet
whereas for u-HMX it occurs at a higher temperature surface of the aluminium/HMX compositions. Light points
(197.5 8C). The higher phase transition temperatures for u- correspond to aluminium particles (due to a backscattered
HMX were also observed at other heating rates, the peak electron detector). Black spots on HMX-images, which look
temperature-heating rate dependences were approximated like pores, are artefacts. It is the result of the interaction of
by the power laws (Figure 6). The phase transition shift may HMX with the electron beam. A mixture of ultrafine
be caused either by the particle size or by the a-phase components has a more uniform spatial distribution of the
transition in u-HMX samples. The first reason is proved by aluminium compared to a mixture of micrometer-sized
the increase in the phase transition temperature for b-HMX components. However, the intermixing can be further
with a particle size decrease for the fraction above 74 mm improved with the ultrasonic technique by the so-called
[17]. Another reason can be the occurrence of the a ! d wet mixing. The components were mixed in diethyl ether
transformation in u-HMX samples in the temperature range under ultrasonic processing for 30 min. The obtained paste
of 188 – 200 8C, and the b ! d conversion at 166 – 194 8C [18]. was dried for 1 h under vacuum. The SEM images show that
The endothermic peak at 280 8C for both samples is
caused by the melting process followed by the subsequent
exothermic decomposition. The difference in the onset and
peak decomposition temperatures for m-HMX and u-HMX
is negligible. The thermal effect of u-HMX decomposition is
1440 J kg1, and of m-HMX this value is equal to 1520 J kg1

Figure 7. SEM images of the pressed pellets: (a) u-Al/u-HMX;

(b) u-Al/m-HMX (white particles are aluminium).

Figure 5. DSC/TG curves for u-HMX (grey lines) and m-HMX Figure 8. SEM images of the pellets surface of the system with
(black) obtained in argon flow 10 8C min1, exo-up. both ultrafine components: (a) conventional, (b) wet mixing.

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Full Paper N. Muravyev, Y. Frolov, A. Pivkina, K. Monogarov, O. Ordzhonikidze, I. Bushmarinov, A. Korlyukov

the wet mixing leads to an enhanced homogeneity of the Table 2. Burning law parameters for investigated systems.
compositions, compared to the dry technique (Figure 8). N Composition B n P
The BET surface area values of the final mixtures were (%)
about the same for both investigated mixing techniques (wet
1 m-HMX 2.0 0.93  0.05 7
and dry ones), and in turn approximately equal to the 2 u-HMX 2.1 0.93  0.04 11
calculated SBET as an additive function of the ingredients HMX [19] 2.1 0.91 3
specific surface. This result reveals that no particles HMX [20] 2.3 0.89 13
fragmentation/conglomeration occurs during the mixing. 3 u-Al/m-HMX 6.1 0.83  0.05 12
4 u-Al/u-HMX 5.1 0.81  0.07 14
5 m-Al/m-HMX 2.1 0.80  0.03 7
6 M-Al/m-HMX 2.17 0.83  0.01 7
3.3 Combustion Parameters 7 Al2O3/m-HMX 1.40 0.93  0.02 20

3.3.1 Burning Rate

The burning rate values (U) for m-HMX and u-HMX

monopropellants under a nitrogen pressure of P ¼ 2 –
10 MPa almost coincide and are close to the data of Refs.
[19 – 25], as shown in Figure 9. The density increase for m-
HMX samples from 1.8 to 1.9 g m3 (porosities 8 and 4%,
respectively) does not result in a noticeable burning rate
change. Obtained parameters B, v in the burning laws
(U[mm s1] ¼ BP[MPa]v) and the average sample porosities
P are presented in Table 2 along with the literature data for
the same [19] and wider (0.3 – 40 MPa [20]) pressure range.
For the binary Al/HMX systems the burning rates were
measured at a pressure range of 3 – 10 MPa (Figure 10, Figure 10. Combustion velocities versus pressure for investigat-
Table 2). Experiments in nitrogen were repeated in argon ed systems (compositions numbers from Table 2).
showing no differences in U. The highest combustion
velocity was observed for u-Al/m-HMX, which was 30%
higher than that for the system with both ultrafine compo-
nents, and  2.5 times greater than U for the monopropel- The ultrafine aluminium addition leads to a combustion
lant. The burning rate of the composition with the micro- velocity increase. Fine metal particles burns out within the
meter-sized components is even smaller than that for the maximum energy-release zone of HMX, approaching the
HMX-monopropellant, and with increase in pressure this temperature maximum to burning surface and, consequent-
difference increases. Regardless of the particle size, all ly, producing an enhanced heat flux into the condensed
binary systems have a pressure exponent v  0.83 that is phase [26]. Apparently, the burning rate enhancement for
smaller than for neat HMX. Alumina addition does not the composition with u-Al and m-HMX compared to the
result in any change of v of HMX, and only decreases the system u-Al/u-HMX is due to the burning surface roughness
burning rate level. increase in the case of coarser HMX particles.

3.3.2 Combustion Residue

The combustion residue was collected during the com-

Figure 9. Burning rate-pressure dependencies for m-HMX, u-
HMX and literature data [19 – 25] (log – log scale).
bustion under a nitrogen pressure of 6.0 MPa at a distance of
23 mm from the burning surface. Agglomerates of the
binary compositions with ultrafine aluminium and two types
of HMX contain at least two modes of particle size. One
mode is in the range of tens of micrometers, and another one
lies in the submicrometer range. The amount of unburnt
aluminium was determined using the comparative thermal
analysis technique. For the coarse sieve fraction (> 40 mm)
PSD was obtained by SEM image processing. The results are
summarized in Table 3, and reveal that the replacement of
the micrometer-sized aluminium by the ultrafine one leads
to a combustion efficiency increase of factor of 4. The use of
u-HMX allows an additional enhancement of the combus-
tion completeness and reduces the agglomerates size, which

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Influence of Particle Size and Mixing Technology on Combustion of HMX/Al Compositions
Table 3. Combustion residue properties for the binary systems.
Composition hDi CAl
(mm) (wt.-%)
m-Al/m-HMX 84 20.6
u-Al/m-HMX 70 5.8
u-Al/u-HMX 66 5.0
must decrease the specific impulse losses in the propulsion
plants.
3.3.3 Mixing Influence
Burning rate values obtained under a nitrogen pressure of
6.0 MPa for the compositions prepared by two different
mixing techniques, i.e., conventional and wet one, are
presented in Figure 11. The application of the wet mixing
results in an 18% burning rate increase as compared to the
dry technique, when ultrafine aluminium was used, for the
system with m-Al this augmentation is 6%. As it was shown,
Figure 11. Influence of mixing type on burning rate: conven-
tional (black bars) and wet (grey) mixing.
no fragmentation occurs during the mixing; therefore such a
rise could be attributed to a better intermixing of the
particles. For the system with coarse metal (M-Al) the type
of mixing is not reflected in a combustion velocity change.
4 Conclusion
The morphology, phase purity, thermal and combustion
properties for systems based on ultrafine and m-HMX were
investigated. The ultrafine aluminium has an average
volume diameter of 180 nm and a chemical activity of
84%, and the micrometer-sized one has a diameter of 3.3 mm
at 94.7% activity. The m-HMX consists of large crystals of
about 50 mm, whereas the microstructure of the u-HMX
powder is more complicated and generally formed by the
submicrometer particles. The u-HMX powder presents two
polymorphs: a (40 wt.-%) and b. After the pressing, the
content of the b-phase increases for about 10%. It was
established, that the temperature of the phase transition for
u-HMX is shifted to higher values. The obtained mono-
Propellants Explos. Pyrotech. 2010, 35, 226 – 232  2010 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
propellant burning rate values are almost identical for the
m-HMX and u-HMX, and are close to the literature data.
The addition of ultrafine aluminium allows an increase in
the combustion velocity by a factor 2.5, compared to the
monopropellant with a corresponding pressure exponent
reduction from 0.93 to 0.83. It was shown that the wet mixing
increased the homogeneity of the compositions and raised
the burning rate by 18% compared to dry mixing, when the
ultrafine aluminium was used. For the binary Al/HMX
systems, the combustion residue analysis revealed that the
replacement of micrometer-sized aluminium by ultrafine
one leads to a combustion efficiency increase by a factor of 4.
The use of u-HMX allows to additionally enhance the
combustion completeness and to reduce the agglomerates
size that must decrease the specific impulse losses.
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Acknowledgements
Financial support of the Russian Foundation of Basic Research
(RFFI grant No. 07-03-00894) is gratefully acknowledged.
Propellants Explos. Pyrotech. 2010, 35, 226 – 232