Defence Technology xxx (2017) 1e7

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Defence Technology
journal homepage: www.elsevier.com/locate/dt

Chemical stability, thermal behavior, and shelf life assessment of

extruded modified double-base propellants
Sherif Elbasuney*, Ahmed Fahd, Hosam E. Mostafa, Sherif F. Mostafa, Ramy Sadek
School of Chemical Engineering, Military Technical College, Kobry El-Kobba, Cairo, Egypt

a r t i c l e i n f o a b s t r a c t

Article history: Double base propellant suffers from lack of chemical stability; this could result in self ignition during
Received 31 July 2017 storing. Modified double base (MDB) propellant based on stoichiometric binary mixture of oxidizer-
Received in revised form metal fuel (Ammonium perchlorate/Aluminum), and energetic nitramines (HMX) offered enhanced
9 October 2017
thrust as well as combustion characteristics. This study is devoted to evaluate the impact of such en-
Accepted 14 November 2017
ergetic additives on thermal behavior, chemical stability, and shelf life. Extruded MDB formulations were
Available online xxx
manufactured by extrusion process. Artificial aging at 80
C for 28 days was conducted. Shelf life
assessment was performed using Van't Hoff's equation. Quantification of evolved NOx gases with aging
Keywords:
Double-base
time was performed using quantitative stability tests. MDB formulation based on HMX demonstrated
Chemical stability extended service life of 16 years compared with (AP/Al)-MDB which demonstrated 9 years. This finding
Thermal behavior was ascribed to the reactivity of AP with nitroglycerin with the formation of perchloric acid. Thermal
Artificial aging behavior of aged MDB, exhibited an increase in heat released with time; this was ascribed to the auto-
Shelf life assessment catalytic thermal degradation during artificial aging. The increase in released heat by 31% was found to be
equivalent to evolved NOx gases of 6.2 cm3/5 g and 2.5 cm3/1 g for Bergmann-Junk test, and Vacuum
stability test respectively. This manuscript shaded the light on a novel approach to quantify evolved NOx
gases to heat released with aging time. MDB based on HMX offered balanced ballistic performance,
chemical stability, and service life.
© 2017 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction offered a higher specific impulse (Fig. 1) [9,13e15].

Modified double base (MDB) propellants have found wide ap-
plications in modern military and space rocketry, in view of their
superior performance [1,2]. It is well known that MDB propellants
are evolved from double-base by integrating energetic fillers such
as HMX or RDX. There is also another trend to integrate potential
oxidizers such as ammonium perchlorate (AP), as well as active
metal fuels such as aluminum, magnesium, and boron [3e6]. This is
why MDB propellants have recently been used in booster, sustainer,
and dual thrust rocket motors [7e9].
MDB can exhibit a wide range of burning rate up to 40 mm/s;
specific impulse can also be varied from 220 to 270 s [9e12]. It has
been reported that integration of stoichometric binary mixture of
oxidizer-metal fuel (AP/Al), and energetic nitramine such as HMX
* Corresponding author.
E-mail addresses: s.elbasuney@mtc.edu.eg, sherif_basuney2000@yahoo.com
(S. Elbasuney).
Peer review under responsibility of China Ordnance Society
MDB based on binary mixture of AP/Al and HMX offered higher
specific impulse by 10% and 9% respectively compared with refer-
ence formulation [9]. Stoichometric binary mixture of AP/Al had a
dual effect by increasing the average operating pressure and
burning rate [9]. This action was ascribed to the gaseous decom-
position nature of AP (Equation (1)), and the exothermic oxidation
of Al metal fuel which could enhance the heat of combustion, and
flame temperature [1,2,7,16].
10NH4 ClO4 / 2:5 Cl2 þ 2N2 O þ 2:5NOCl þ HClO4 þ 1:5HCl
þ 18:75H2 O þ 1:75N2 þ 6:38O2
(1)
Aluminum metal fuel, with high exothermic heat of combustion
(7.4 kcal/g) and excellent thermal conductivity values, tended to
increase the burning rate [7,17,18]. Aluminum particles are able to
react not only with free oxygen resulted from oxidizer decompo-
sition; but also it is able to react with inert decomposition gaseous
products and add much more heat to the combustion process

https://doi.org/10.1016/j.dt.2017.11.003
2214-9147/© 2017 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Please cite this article in press as: Elbasuney S, et al., Chemical stability, thermal behavior, and shelf life assessment of extruded modified
double-base propellants, Defence Technology (2017), https://doi.org/10.1016/j.dt.2017.11.003
2 S. Elbasuney et al. / Defence Technology xxx (2017) 1e7
Fig. 1. Practical measurements of pressure-time curves of developed MDB using small-
scale ballistic evaluation test motor [9].
[18e20].
The great impact of HMX on ballistic performance was attrib-
uted to the positive heat of formation (þ353.8 kJ/kg). HMX is a
highly effective explosive material with heat of explosion 6197 kJ/
kg and gaseous product of 902 L/kg [13]. HMX also has a slightly
negative oxygen balance which means decomposition products of
low molecular weight [13,21]. Much research has been directed
toward the development of MDB propellants with enhanced com-
bustion characteristics and high specific impulse [22e25]. However
less attention has been directed to investigate the impact of
different energetic additives on chemical stability, thermal
behavior, and shelf life [26].
1.1. Chemical stability of MDB propellants
The nitrate esters (nitrocellulose & nitroglycerine), the main
constituents of double-base propellant, are molecules that aren't
chemically stable. Their decomposition is slow in ambient condi-
tions of temperature, pressure, and humidity. In severe environ-
ments, the chemical decomposition becomes autocatalytic [11].
There are many mechanisms through which chemical decomposi-
tion can occur; these mechanisms include:
1.1.1. Chain reactions
Chain reactions start with the homolytic breaking of the weak
O-NO2 bond, forming nitrogen dioxide and the corresponding
alkoxyl radical [27e29]. These reactive free radicals immediately
undergo consecutive reactions with nearby nitrate ester molecules
[29].
, ,
R  O  NO2 /R  O þ N O2
1.1.2. Saponification (hydrolysis)
Another main decomposition pathway is the neutral to acid
hydrolysis of the nitrate esters [28]. This reaction is catalyzed by
moisture and residual acids (which weren't fully removed after
nitrate ester synthesis), or by water, or by acids formed during
decomposition (Equation (3)).
þ 2.1. Manufacture of MDB formulations
R  O  NO2 þ 2H2 O


! H R  OH þ HNO3
A further decomposition reaction is the “enhanced hydrolysis”.
This reaction was found to have low activation energy of 71 kJ/mol.
Therefore it can be a dominant decomposition reaction at lower
temperatures [30].
Please cite this article in press as: Elbasuney S, et al., Chemical stability, thermal behavior, and shelf life assessment of extruded modified
double-base propellants, Defence Technology (2017), https://doi.org/10.1016/j.dt.2017.11.003
1.1.3. Auto-catalytic reactions
Decomposition products of reactions (2) can further trans-
formed in presence of moisture and oxygen as follow:
, ,
2N O þ O2 /2N O2 4N2 O4 (4)
, ,
N O þ N O2 þ H2 O/2HNO2 (5)
, ,
3N O2 þ H2 O/2HNO3 þ N O (6)
Whereas the primary homolytic reaction (2) can't be sup-
pressed, the consecutive reactions (3e6) can be slowed down
nearly to zero by binding or elimination of acids, nitric oxides, and
water from the system. This fact was employed for the stabilization
of double-base propellants by integrating stabilizing agents [30,31].
Stabilizers fulfill their purpose by reacting with the nitrogen oxides
and neutralize the decomposition products [32]. Conventional
double-base propellants, with proper percentage of stabilizer, can
offer a safe chemical life of at least 20 years [33]. For modified
systems containing energetic solid additives similar shelf life
should be secured [34]. A number of studies have been carried out
on the thermal stability of MDB propellants [35e38]. Complete
information regarding the influence of high energy ingredients
including (in organic oxidizers/high explosives) on MDB propellant
stability and shelf life is vital in regards of their handling, pro-
cessing, transportation, and storage.
1.2. Impact of different energetic additives on chemical stability
AP has a great impact on the degradation of propellants con-
taining nitrate esters. Many researchers have studied the rate of
stabilizer depletion and the time to ignition of such propellants
[39]. Asthana, Divekar et al. investigated the stability, auto ignition,
and stabilizer depletion of MDB propellants containing NG and AP
[40]. It was noted that the inclusion of AP increased the auto-
catalytic behavior of MDB propellants over time [41]. MDB based
on AP demonstrated ease of ignition suggesting faster decompo-
sition kinetics [42]. AP-MDB propellants possess shorter shelf life
than their conventional counterparts [40,43]. Further research
showed that MDB containing AP and NG exhibited less stability
than conventional double-base [44]. However, nitramine double-
base propellants exhibited relatively good thermal stability
[45e49]. This paper is devoted to investigate the effect of binary
mixture of oxidizer/metal fuel (AP/Al) and energetic nitramine
(HMX) on DB chemical stability, thermal behavior, as well as shelf
life assessment. MDB formulation based on HMX demonstrated
extended service life of 16 years compared to (AP/Al)-MDB which
(2) demonstrated 9 years. DSC outcomes demonstrated an increase in
heat released with aging time. The released heat was increased by
31, 41, and 25% for reference, (AP/Al)-MDB, and HMX-MDB for-
mulations respectively. This thermal behavior was ascribed to the
auto-catalytic thermal degradation over artificial aging. Correlation
between the increase in heat released and the evolved nitrogen
oxides was conducted.
2. Experimental
(3)
Screw extrusion technique emphasizes mixing of different in-
gredients to ensure good homogenization, high density, and
dimensional stability. This technique included many stages such as
blending, followed by rolling, grinding, granulation, and finally
 S. Elbasuney et al. / Defence Technology xxx (2017) 1e7
extrusion to obtain grains of desired shape and dimensions [50].
Different MDB formulations based on stoichiometric binary
mixture (AP/Al), and HMX at 10 wt % solid loading level, were
manufactured by screw extrusion.
2.2. Chemical stability of MDB
Evaluation of chemical stability, deals with the fact that the rate
of decomposition at normal temperature is judged from decom-
position at higher temperature [51,52]. Quantitative stability tests
were employed for fast and reliable evaluation of MDB chemical
stability; they were devoted to the direct measurement of evolved
gasses [53]. The most commonly used quantitative stability tests
are Bergmann-Junk test, and Vacuum stability test.
2.2.1. Bergmann-Junk test
Bergmann-Junk test is the main quantitative test for DB stability
evaluation. In this test, 5 g of the tested sample was heated at 120
C
for 5 h. The evolved nitrogen oxides (NOx) were entrapped in a
secondary tube containing 50 ml of de-ionized water. The evolved
NOx gases were quantitatively determined by titration using po-
tassium iodide solution. The acceptable limit for Bergmann-Junk
test is 10 ml of NOx/5 g sample [23,54].
2.2.2. Vacuum stability test
Vacuum stability test is a controlling, measuring, enabling
evaluation of temperature stability from measurements of evolved
gases from tested sample during long term isothermal heating. This
test was performed according to STANAG 4556, where 1 g of the
sample was heated at 90
C for 40 h with pressure measurement
reading each 1 min during the isothermal heating process.
2.3. Thermal behavior of MDB
Ignition temperature is one of the main important characteris-
tics which need to be evaluated for developed MDB formulation, in
an attempt to evaluate the impact of different energetic constitu-
ents on MDB heat sensitivity. A sample of 0.1 g was introduced in a
glass tube and heated at controlled rate of 5
C/min till ignition [32].
Phase change with temperature, onset decomposition temperature,
and heat released upon combustion are the main parameters for
MDB thermal stability evaluation. Differential scanning calorimetry
(DSC) measures heat flow associated with phase changes (i.e.
melting), endothermic/exothermic decomposition as a function of
temperature or time. DSC measurements were performed using
DSC 2920 by TA instruments. 2 mg of MDB propellants were heated
up to 300
C at 5
C/min, under nitrogen gas flow at 5 ml/min.
2.4. Artificial aging
Artificial aging was conducted in an attempt to reduce the time
scale by storing the propellant at elevated temperatures so that
prediction of service life can be made in shorter times. It facilitates
the planning of timeetemperature profile of MDB with limited
knowledge about their degradation behavior [55]. Artificial aging
was performed by isothermal heating at 80
C in temperature
controlled oven under ambient atmospheric conditions. The
developed MDB formulations were stored under isothermal heat-
ing for 4, 8, 14 and 28 days [56]. Consequently safe storage life of the
propellant can be predicted [56].
2.5. Shelf life assessment of MDB
Van't Hoff's formula (Equation (7)) enabled the estimation of in-
service periods at given in-storage temperatures, from the
Please cite this article in press as: Elbasuney S, et al., Chemical stability, thermal behavior, and shelf life assessment of extruded modified
double-base propellants, Defence Technology (2017), https://doi.org/10.1016/j.dt.2017.11.003
3
equivalent time-temperature loads during the artificial ageing.
Van't Hoff's formula has been proved by experience to be suitable to
establish the time-temperature profile [57].
TT  TE
1
TE ½y ¼ TT ½d : F D TF
: (7)
365:25
Where: TE, TT, F, and DTF are time in years at the in-service tem-
perature (TE in 0C), test time in days at the test temperature (TT in
0
C), reaction rate change factor per 10
C of temperature change (F
usually between 2 and 4), and temperature interval for actual value
F respectively. Factor F was determined using Arrhenius Equation
(8) [57].
!
Ea DTF
þ ,
R T2
F ¼ exp
T
(8)
Where, Ea is the activation energy (kJ/mol), and R is the ideal gas
constant [55]. F factor was deduced by compiling and comparing
reaction rates obtained at different temperatures [55]. The range for
this factor is often between 2 and 4 [57]. Table 1 demonstrates the
accelerated ageing conditions simulating an in-use time up to
32 years at 25
C for developed MDB propellants.
The change in chemical stability of aged MDB was tracked by
quantifying the evolved NOx gases with aging time. Their thermal
behavior was investigated and quantified using DSC. Novel corre-
lation between chemical stability (volume of evolved NOx gases)
and thermal behavior (Heat released) was represented.
3. Results and discussions
3.1. Chemical stability of MDB
The volume of nitrogen oxides evolved from freshly manufac-
tured MDB compositions was quantified using Bergman-Junk test.
The quantified NOx are listed in Table 2.
The volume of NOx evolved from reference DB and MDB for-
mulations were within the acceptable limits (10 ml of NOx/5 g
sample) [54]. HMX based formulation exhibited similar value of
evolved NOx to reference. This indicated that HMX is compatible
with double base constituents; no side chemical reactions could
take place. However AP based formulation exhibited the largest
volume of evolved NOx gases. This was attributed to the reactivity
of AP oxidizer to react with nitroglycerine to form perchloric acid
[30,58]. Vacuum stability test represents a fast way of chemical
stability determination. Results from vacuum stability test for
freshly manufactured MDB propellants are listed in Table 3. The
evolved NOx confirmed the obtained data from Berman-Junk test.
3.2. Thermal behavior of MDB
Ignition temperature test was conducted to measure the tem-
perature of spontaneous ignition by progressive heating. Even
though, MDB formulation exhibited an increase in heat released
during exothermic decomposition, there was no dramatic change in
Table 1
Ageing times calculated on the basis of thermal equivalent load at TE ¼ 25
C using
the generalized Van't Hoff's rule with factor F ¼ 3.
Accelerated aging periods at 80
C/Days In - use time TE/Years
4 4.5
8 9
14 16
28 32
4 S. Elbasuney et al. / Defence Technology xxx (2017) 1e7

Table 2
Quantified NOx gases evolved from freshly manufactured MDB using Bergmann-Junk test.

Formulation F0 F1 F2
(Reference) (7 wt % AP þ 3 wt % Al) (10 wt % HMX)

Volume of evolved gasses/(cm3$5 gm1) 4.4 6.3 4.5

Table 3
Vacuum stability test results of freshly developed MDB.

Formulation F0 F1 F2
(Reference) (7 wt % AP þ 3 wt % Al) (10 wt % HMX)

Volume of released gasses/(cm3$ g1) 1.546 2.368 1.888

quantified with aging time and shelf life prediction using Bergman-
Junk test (Table 5).
Results demonstrated that AP based formulation demonstrated
the least chemical stability. This behavior was attributed to the fact
that AP can degrade to form perchloric acid; which could cause
rapid hydrolysis of the nitrate ester. This degradation action could
accelerate the propellant decomposition (Equations (9)e(12))
[30,45,58].

NH4 ClO4 þ N2 O3 /NH4 NO2 þ NOClO4 (9)

NH4 NO2 / N2 þ 2H2 O (10)

NOClO4 þ H2 O /HNO2 þ HClO4 (11)

Fig. 2. DSC thermograms of fresh manufactured MDB formulations.
HClO4 þ 4NO /4NO2 þ HCl (12)
MDB propellants based on HMX revealed stability similar to
ignition temperature. The ignition temperature for reference, AP/
reference formulation. This was ascribed to the high thermal sta-
Al-MDB, and HMX-MDB was found to be 171, 172, 170
C respec-
bility of HMX. Furthermore, no side reactions could take place be-
tively. DSC was employed to monitor any chemical/physical
tween HMX and DB constituents. Quantification of evolved NOx
changes which involve the evolution/absorption of heat. The total
gases with aging time was performed using vacuum stability test
heat released, the maximum decomposition temperature, and the
(Table 6). Vacuum stability test outcomes confirmed the findings of
onset decomposition temperature were measured and evaluated
Bergmann-Junk test.
using DSC (Fig. 2).
There was an increase in volume of evolved NOx with aging
All Formulations demonstrated one exothermic decomposition
time. The volume of evolved NOx gases from HMX-MDB was higher
peak. Energetic additives did not greatly affect the maximum
than reference formulation but lower than AP-MDB. HMX-MDB and
decomposition temperature but they positively impact the total
reference formulation exhibited similar shelf life of at least 16 years.
heat released upon combustion. Summary of total heat released (J/
On the other hand MDB based on binary mixture of AP/Al exhibited
g) and maximum peak temperature (
C) are tabulated in Table 4.
shelf life of 9 years. This was attributed to the induced catalytic
The inclusion different energetic additives including binary
degradation upon inclusion of AP with the formation of perchloric
mixture of AP/Al, and HMX into DB propellants increased the
acid.
released heat upon decomposition due to the favorable heat added
by these modifiers. Formulation 2 based on HMX exhibited the
3.4. Thermal behavior of aged MDB
highest released heat. This was ascribed to the fact that HMX de-
composes with the release of large amount of heat 6197 J/g.
MDB demonstrated a decrease in ignition temperature with
isothermal aging time (Table 7).
3.3. Shelf life assessment It is clear that sensitivity to heat of different MDB formulations
increased with aging. This behavior was ascribed to the decrease in
The developed MDB were isothermally aged at 80
C for the required activation energy to start the chemical conversion
different periods. The increase in evolved NOx oxides was [34]. HMX based formulation demonstrated the highest thermal

Table 4
Thermal behavior characteristics of fresh manufactured MDB.

DSC outcomes

Total Heat released/(J$g1) Max. peak temperature/(
C)

F0 (Reference) 1591 193.83

F1 (7 wt % AP þ 3 wt % Al) 1733 195.53
F2 (10 wt % HMX) 1998 192.88

Please cite this article in press as: Elbasuney S, et al., Chemical stability, thermal behavior, and shelf life assessment of extruded modified
double-base propellants, Defence Technology (2017), https://doi.org/10.1016/j.dt.2017.11.003
 S. Elbasuney et al. / Defence Technology xxx (2017) 1e7 5

Table 5
Bergmann-Junk test results after aging at 80
C.

Accelerated aging periods at 80
C/Days Shelf life prediction/Years Volume of gas evolved/(Cm3$ 5 g1)

F0 F1 F2
(Reference) (7 wt % AP þ 3 wt % Al) (10 wt % HMX)

0 Fresh 4.4 6.3 4.5

4 4.5 4.7 6.8 5.1
8 9 5.3 8.6 6
14 16 6.2 Decomposition 7.3
28 32 (refused) Decomposition

Table 6
Quantification of NOx with aging using vacuum stability test.

Accelerated aging Shelf life Volume released gas/ (Cm 3· g-1)

periods at 80 0C predicƟon F0 F1 F2
/Days /Years (Reference) (7 Wt % AP + 3 Wt % Al) (10 Wt % HMX)

0 ---- 1.546 2.368 1.888

4 (4.5) 1.851 2.726 1.981

8 (9) 1.991 2.987 2.243

14 (16) 2.477 Failure 2.705

(14.355)
28 (32) Failure Failure
(14.688) (14.211)

Table 7
Ignition temperature for aged MDBP.

Accelerated aging periods at 80
C/Days Shelf life prediction/Years Ignition temperature/(
C)

F0 (Reference) F3 (7 wt % AP þ 3 wt % Al) F4 (10 wt % HMX)

0 e 171 172 170

4 4.5 169 171 170
8 9 168 167 169
14 16 166 163 167
28 32 164 161 166

Fig. 3. DSC thermogram of fresh and aged reference formulation. Fig. 4. DSC thermogram of fresh and aged MDB based on (7 wt % AP þ 3 wt % Al).

stability; this was attributed to the fact that higher energy is
required for the activation of HMX compared with AP [13]. The
thermal behavior of aged MDB after aging period of 14 days were
investigated with DSC to that of freshly manufactured formulation.
DSC thermograms of aged MDB formulations ensured the findings
of Bergman-Junk and Vacuum stability tests. The main findings
from DSC thermograms included: shifting of maximum decompo-
sition peak temperature to lower value, and an increase in total
heat released with aging. Figs. 3e5 demonstrate the DSC thermo-
grams for fresh and aged formulations.
All investigated MDB formulations exhibited similar thermal
behavior with aging. This behavior encompasses an increase in heat

Please cite this article in press as: Elbasuney S, et al., Chemical stability, thermal behavior, and shelf life assessment of extruded modified
double-base propellants, Defence Technology (2017), https://doi.org/10.1016/j.dt.2017.11.003
6 S. Elbasuney et al. / Defence Technology xxx (2017) 1e7
Fig. 5. DSC thermogram of fresh and aged MDB based on HMX.
Table 8
The increase in heat released with isothermal aging time.
DSC results
Total Heat released The increase in total
for fresh formulation/ heat released after
(J$mm1) aging/%
F1 (Reference) 2085 31
F2 (7 wt % AP þ 3 wt % 2076 41
Al)
F3 (10 wt % HMX) 2496 25
released as well as a decrease in the temperature at maximum heat
released. This thermal behavior was ascribed to the degradation of
MDB over aging. MDB propellants could degrade by thermal
decomposition of NC and NG, which might start with the homolytic
breakdown of the OeNO2 bond [55]. This reaction might be cata-
lyzed by moisture and residual acids formed as products during the
decomposition process [55]. Table 8 summarized the increase in
total heat released of aged formulations, to fresh manufactured
formulations.
DSC out comes ensured the findings of Bergmann-Junk and
Vacuum stability tests. The total heat released was increased by 31,
41 and 25% for reference formulation, binary mixture of (AP & Al),
and HMX respectively. HMX based formulation demonstrated su-
perior thermal stability. This behavior was attributed to the great
consumption of heat energy for the activation of HMX compared to
AP, as well as the reactivity of AP toward NG.
4. Conclusion
MDB based on HMX exhibited good chemical and thermal sta-
bilities using quantitative chemical stability tests and DSC respec-
tively. MDB based on HMX exhibited service life of 16 years, similar
to reference formulation. MDB based on AP demonstrated service
life of 9 years. Low service life of MDB based on AP was ascribed to
the reactivity of AP towards NG with the formation of perchloric
acid. All MDB formulations exhibited an increase in evolved NOx,
and total heat released with aging time. The increase in heat
released by 31% was found to be equivalent to evolved NOx gases of
6.2 cm3/5 g and 2.5 cm3/1 g for Bergman-Junk, and Vacuum sta-
bility test respectively. These values should not be exceeded for safe
storage. This manuscript shaded the light on HMX which offered
MDB with balanced ballistic performance, thermal and chemical
stability, as well as extended service life.
Please cite this article in press as: Elbasuney S, et al., Chemical stability, thermal behavior, and shelf life assessment of extruded modified
double-base propellants, Defence Technology (2017), https://doi.org/10.1016/j.dt.2017.11.003
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Please cite this article in press as: Elbasuney S, et al., Chemical stability, thermal behavior, and shelf life assessment of extruded modified
double-base propellants, Defence Technology (2017), https://doi.org/10.1016/j.dt.2017.11.003