Full Paper

DOI: 10.1002/prep.201400263

Reducing Agglomeration of Ammonium Perchlorate Using

Activated Charcoal
Kumar Ishitha*[a] and P. A. Ramakrishna[a]

Abstract: Ammonium perchlorate is the most widely em- particle size this problem becomes more evident. Experi-
ployed oxidizer for composite solid propellants. When ex- mental studies aimed at reducing the agglomeration of am-
posed to atmosphere, it absorbs moisture and agglomer- monium perchlorate by coating it with activated charcoal.
ates. It is usually vacuum dried in order to avoid this ag- Ammonium perchlorate coated with 1 % activated charcoal
glomeration. When ammonium perchlorate that has been showed almost no agglomeration, even when the particle
exposed to atmosphere for a certain period of time, is used size of ammonium perchlorate is approx. 1 mm. The burn-
in making a composite solid propellant, the burning rate is ing rates also remained unchanged when ammonium per-
different because of the change in particle size distribution chlorate coated with 1 % activated charcoal was employed
due to its agglomeration. This change in burning rate will in propellant composition, after it has been exposed to the
change the thrust-time profile from that of what it is de- atmosphere for a period of 1 h.
signed for. As one goes to a finer ammonium perchlorate
Keywords: Activated charcoal · Ammonium perchlorate · Agglomeration · Burning rates

1 Introduction

Ammonium perchlorate (AP) is the most widely employed ture due to its porous nature. Thus, when AC coated AP is
oxidizer for composite solid propellants. AP is a crystalline used, AC is able to absorb moisture while AP doesn’t and
material, which offers the possibility to modify the burning hence result in reduced agglomeration. These observations
rates of composite solid propellants by modification in the triggered the curiosity and experiments are conducted to
size of AP [1–3]. A decrease in the particle size of AP in- examine if there is a decrease in the rate of agglomeration
creases the burning rate of the composite solid propellant for AP coated with AC as against AP alone. Experiments are
[1–3]. Usually, AP of desired particle sizes would be ob- also conducted to examine the burning rate behavior of
tained when exposed to atmosphere with high humidity propellants made from AP coated with AC as against pro-
since AP tends to coalesce. If coalescing is not prevented pellants made with AP alone, wherein they are exposed to
between the time the desired particle sizes are obtained atmosphere for increased periods (1 h and 6 h) of time.
and the time when the propellant is prepared, the particle Again, AP coated with AC, here, will only mean that AC is
size of AP being employed in the propellant can be in close proximity to AP. These experimental studies are
changed. This change would cause deviation of the burn- presented below.
ing rates of a composite solid propellant from the designed
values. More generally, a solid rocket motor is designed
based on the thrust-time profile it has to follow for the ac-
2 Experimental Section
complishment of the mission. The propellant composition
is also so chosen that the required thrust-time profile is re- Table 1 shows details and source of the various ingredients
alized. An undesired change in the burning rates of the employed for performing the experiments in this study. De-
composition due to the agglomeration of AP would alter tailed descriptions on the purpose of these ingredients are
the thrust-time profile. As one goes to a finer AP particle dealt later in this paper.
size this problem becomes more pronounced and could
lead to the failure of a mission.
It is noticed while performing the experiments to obtain
a high burning rate and low n propellant composition em-
[a] K. Ishitha, P. A. Ramakrishna
ploying AP coated with activated charcoal (AC) [4] that this
Department of Aerospace Engineering
AP does not show any perceivable agglomeration even Indian Institute of Technology Madras
after it is exposed to atmosphere for a few days. Also, Chennai, India
Verma and Ramakrishna [5] noticed that AC absorbs mois- *e-mail: ishikumar86@gmail.com

838 Ó 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim Propellants Explos. Pyrotech. 2015, 40, 838 – 847
Reducing Agglomeration of Ammonium Perchlorate Using Activated Charcoal

Table 1. Details and source of ingredients.

Ingredient Purpose Source
AP (NH4ClO4) Oxidizer Tamil Chlorates, Madurai
Hydroxyl-terminated polybutadiene ((C4H6(OH)2)n Binder and fuel Satish Dhawan Space Centre, Sriharikota
Isophoronediisocynate (C12H18N2O2) Curing agent Satish Dhawan Space Centre, Sriharikota
Dioctyladipate (C22H42O4) Plasticizer Satish Dhawan Space Centre, Sriharikota
AC (C) (5–10 mm) Burning rate modifier Merck, Mumbai

2.1 Preparation of Ammonium Perchlorate Samples

trapped gases. The degassed slurry along with the plastic
The initial range of particle size of AP, as obtained, is 300– sheet covering it is then transferred to a hollow cylindrical
400 mm. To study the decrease in the rate of agglomeration chamber of 40 mm (same diameter as vacuum-casting
when AC is coated to AP, various types of AP are prepared chamber). It is maintained under a pressure of around
by coating 0.1 % AC, 0.4 % AC and 1 % AC. To obtain AP 0.25 MPa for 10 days under the ambient conditions (aver-
coated with AC, a new proprietary process developed in age temperature being 306 K). The cured propellants are
the laboratory is employed here. Though dry mixing could taken out by tearing off the plastic sheet and cut in to sam-
be employed for the same, the method is not effective as ples of 5 mm Õ 5 mm Õ 35 mm.
the AC is only loosely coated over AP surface. These are The propellants obtained are ensured to be free from
represented as AP + 0.1 % AC, AP + 0.4 % AC and AP + 1 % blow holes and the density of the propellants is measured
AC, respectively, and are studied in comparison with AP by volume displacement method. Samples are cut into
alone. The various particle sizes of AP and AP coated with a 15 mm cube and covered with a thin plastic sheet. The
AC employed in this study are 45–25 mm, 15–5 mm and mass of these samples are measured using a weighing bal-
approx. 1 mm. Here, as received AP particles in the particle ance of 10 mg least count. Distilled water with the specific
size range < 425 mm are crushed to obtain AP between 45– gravity of 1.002 is used as a measuring liquid. Samples are
25 mm and 15–5 mm of size using appropriate sieves. A size immersed in distilled water. Knowing the volume of water
of 45–25 mm is obtained using sieves of mesh numbers 325 displaced and the mass of the samples, the density of a pro-
and 500. 15–5 mm is obtained using sieves of mesh num- pellant is calculated. The significance of the density ob-
bers 800 and 2500. The sieves used in this study are made tained for a propellant, in measuring the burning rates and
from stainless steel. A ball mill is employed to obtain parti- burning rate pressure index has been discussed by Verma
cle sizes of the order of 1 mm. Same particle sizes are ob- and Ramakrishna [6].
tained for AP coated with AC. The propellants are prepared from AP and AP + 1 % AC
which are exposed to atmosphere for 0 h, 1 h and 6 h, to
study their burning rate behavior. These propellants are
2.2 Preparation of Propellants
prepared with particle size ranging from 45–25 mm and 15–
The procedure followed is similar to the one described by 5 mm. Propellants were not made with AP of particle size of
Verma and Ramakrishna [6]. All the ingredients are hand the order of 1 mm, as preparation of these compositions
mixed for 15–20 min. The propellant slurry thus obtained is was difficult. All the compositions are prepared with 80 %
transferred in to a mixer of 200 g capacity, where it is solid loading. The percentage of other ingredients in these
mixed for an hour. The mixture is then transferred to compositions being: hydroxyl-terminated poly butadiene-
a vacuum casting chamber of 40 mm diameter, where the 12.7, isophorone di-isocynate-2.5 and di octyl adipate-4.8.
propellant is cured under vacuum to further remove the Table 2 gives the details of the compositions prepared.

Table 2. List of propellants prepared.

Notation used for the composition Details of the composition
Mix 1 Prepared with AP of particle size range of 45–25 mm and unexposed to atmosphere
Mix 2 Prepared with AP of particle size range of 45–25 mm and exposed to atmosphere for 6 h
Mix 3 Prepared with AP of particle size range of 15–5 mm and unexposed to atmosphere
Mix 4 Prepared with AP of particle size range of 15–5 mm and exposed to atmosphere for 1 h
Mix 5 Prepared with AP of particle size range of 15–5 mm and exposed to atmosphere for 6 h
Mix 6 Prepared with AP + 1 % AC of particle size range of 15–5 mm and unexposed to atmosphere
Mix 7 Prepared with AP + 1 % AC of particle size range of 15–5 mm and exposed to atmosphere for 1 h
Mix 8 Prepared with AP + 1 % AC of particle size range of 15–5 mm and exposed to atmosphere for 6 h
Mix 9 Prepared with AP + 1 % AC of particle size range of 15–5 mm and exposed to atmosphere for 126 h

Propellants Explos. Pyrotech. 2015, 40, 838 – 847 Ó 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim www.pep.wiley-vch.de 839
Full Paper K. Ishitha, P. A. Ramakrishna

2.3 Agglomeration Studies

Two kinds analysis is performed, here, to study the agglom-

eration behaviour of AP. Firstly, to compare the rates of ag-
glomeration of AP and samples of AP coated with AC,
sieves analysis has been employed. A brief description of
sieves analysis would be appropriate. After obtaining AP
and various types of AP coated with AC, in the particle size
range of 45–25 mm and 15–5 mm, these samples were ex-
posed to the atmosphere with a typical relative humidity of
89 % and temperature of 30 8C. These values of relative hu-
midity and temperature are the average values on any day
and, for all the presented experiments these vary by œ 5 %
and œ 6 %, respectively, from the above mentioned values.
The periods of exposure considered for this study are 1 h,
2 h, 4 h and 6 h. After exposing these AP powders to at-
mosphere for the desired period of time, the AP particles
which is within its initial particle size range is retrieved by
sieving with appropriate sieves. This analysis was not per-
formed on the AP with particle size of the order of 1 mm
due to unavailability of sieves of this size (ball mill is used
to obtain this size).
Another study performed in conjunction with sieves
analysis is to compare the high resolution-SEM pictures of
various AP powders, after exposing the samples to atmo-
sphere for increasing periods of time. The advantage with
this analysis is that one can visually quantify the change in
the particle size with time. This analysis is performed on
the samples in particle size range of 15–5 mm and on AP
particles of the order of 1 mm.

2.4 Experimental Set-Up

A crawford bomb or standard window bomb is employed
to obtain burning rates of pellets, sandwich propellants
and composite solid propellants. This set-up in conjunction
with timer circuit is employed to obtain the burning rates
of composite solid propellants. Figure 1 (a) shows the sche-
matic of the set-up. Figure 1 (b) shows the propellant
Figure 1. Schematic of window bomb set-up (a). Schematic of the
sample holder employed in the set-up.
propellant sample holder (b).
The sample is placed on a propellant holder through
which the supply line runs. Commercial nitrogen cylinder is
connected to the supply line and is used to pressurize the (5 Õ 2 mm) and can initiate combustion when current is al-
bomb. A pressure regulator is positioned as shown in lowed to pass through the electrodes. An electric current
Figure 1 (a) to maintain the pressure within the bomb at of 22 V and 1 A is used for ignition. The diameter of the ni-
the desired value. An exit valve that exhausts the gases to chrome wire used is 0.5 mm.
the ambient is also provided for as shown in Figure 1 (a). A thin layer of inhibitor (silicon grease) is coated on the
The propellant holder used here has 6 electrode rods, two four side-surfaces (5 mm Õ 35 mm) of the samples to ensure
of them for ignition purpose and the remaining four to that the burning surface area (5 mm Õ 5 mm) of the sample
complete connections for the timer circuit, as shown in remained same during the regression. Then three 200 mm
Figure 1 (b). The two electrodes to facilitate ignition of the nichrome wires are passed through the propellant sample
sample are connected to a D. C. power supply through and distance between the wires was maintained around
a switch, with the help of which current is allowed to pass 10 mm. The least count of the timer circuit is 1 ms and
through the electrodes during ignition. This circuit is closed maximum time it can measure is 9.999 s. With the knowl-
by a nichrome wire tied between the two electrodes and edge of the distance between the wires and the corre-
positioned such that it touches the sample at the top face sponding time duration for the burning surface to travel

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Reducing Agglomeration of Ammonium Perchlorate Using Activated Charcoal

between the two wires, we can calculate the burning rate

of the sample. At a particular pressure two readings of the
burning rate are obtained using a single sample. Burning
rates have been calculated in the pressure range of 1–
7 MPa and the difference between two pressure readings
chosen is 1 MPa.

3 Results and Discussion

3.1 Sieve and SEM Analyses
Initial experiments are performed on particle size range of
45–25 mm. The time required to obtain 20 g of this particu-
lar particle size range is approximately 10 min. After obtain-
ing various types of AP in this particle size range, 20 g of
sample from each type are simultaneously exposed to the
atmosphere with a typical relative humidity of 80 %. The Figure 2. Digital photographs of a) AP at 0 h, b) AP after 1 h, c)
AP + 1 % AC at 0 h and d) AP + 1 % AC after 1 h of exposure to at-
periods of exposure are 1 h, 2 h, 4 h and 6 h. Sieve analysis
mosphere.
is performed on these samples. The results of these analy-
ses are presented in Table 3. It is apparent from this analy-
sis that the amount of AP that can be retrieved remains formed on AC and charcoal, using micrometrics instrument,
almost constant with time, when AP is coated with 1 % AC. to emphasize the porous nature of AC in quantitative
Generally, the rate of agglomeration is noticed to reduce terms. The surface area of AC is obtained to be 914.85 m2/
when AP is coated with AC and this reduction is seen to be g, while that for charcoal is obtained to be 314.70 m2/g.
increasing with increasing percentage of AC. The rate of ag- The experiments on AP + 1 % C are carried out to exam-
glomeration appears close to zero for AP coated with 1 % ine if it is the porous nature of AC that is responsible for
AC. absorbing moisture and preventing the agglomeration of
AC coated AP or some other chemical process. The same
procedure, as described earlier with respect to AC, has
Table 3. Sieve analysis results.
been employed to perform sieves analysis with AP + 1 % C.
AP Amount of AP between 45–25 mm [g] The results obtained for AP + 1 % C showed that charcoal is
1h 2h 4h 6h not effective in reducing the agglomeration of AP. These re-
AP 10.9 10 7.6 7 sults are given in Table 3, above. Thus, the postulate that
AP + 0.1 % AC 14 12.6 8 7.5 the pores of AC could be holding the moisture, when AP is
AP + 0.4 % AC 15 13.4 12.5 10 exposed to the atmosphere gained credence with this ex-
AP + 1 % AC 17.52 17.32 17.6 17.2 periment. As the AC is coated over AP, direct contact be-
AP + 1 % C 8.72 8.4 6.84 5.67 tween two AP particles is less probable, thus preventing AP
from agglomerating. In the case of AP coated with char-
coal, there is very little provision for holding moisture and
These results are further augmented with pictures taken it is seen that charcoal coating is extremely ineffective in
for AP and AP + 1 % AC after 0 h and 1 h of their exposure preventing AP agglomeration.
to atmosphere. These pictures are taken using a digital The experiments are preliminary, as the humidity
camera (Canon EOS 1100). Figure 2 shows these pictures. changes were not tracked during these studies. Also, the
The change in particle size is apparent with AP (Figure 2 (a) pictures presented in Figure 2 are just taken with a digital
and (b)), which is not the case when 1 % AC was coated camera. Further, refined experiments, by keeping track of
over it (Figure 2 (c) and (d)). humidity in the atmosphere and by studying high resolu-
Another sieve analysis study has been conducted by em- tion SEM pictures (instead of digital pictures), are conduct-
ploying just dry mixing to coat AC over AP. Coating AC ed.
over AP using dry mixing was seen to be completely inef- To understand the effectiveness of 1 % AC to prevent AP
fective in reducing the agglomeration of AP. It confirmed from agglomerating two different studies are performed
the ingenuity of the process employed to coat AC over AP. here. Apart from employing sieves analysis on a different
AP coated with 1 % AC prevents AP from agglomerating particle size range for AP, high-resolution SEM pictures are
almost completely. Thus, further experiments are per- also used as tool here. Analysis is done on 15–5 mm particle
formed on AP coated with 1 % charcoal (represented as size range. This is a lower particle size range than the earli-
AP + 1 % C). The difference between AC and charcoal is er one and would give a better perspective on the effec-
that AC is porous. Surface area measurements are per- tiveness of AC. Figure 3 gives the amount of AP, in the ini-

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Full Paper K. Ishitha, P. A. Ramakrishna

Figure 3. Sieve analysis results for a particle size of 15–5 mm

range.
Figure 4. Comparison of sieve analysis results between particle
size range of 45–15 mm and 15–5 mm.

Table 4. Atmospheric conditions during the studies on 15–5 mm

particle size range.
attributed to issues of poor resolution. In order to see the
Time Atmospheric Conditions at the hour change in particle size it was thought that lowering the
0h RH: 83 %; T = 29.8 8C particle size of AP might be a better bet. Further studies
6h RH: 89 %; T = 32.4 8C are carried out in the particle size range of approx. 1 mm
and SEM images are obtained accordingly (Table 5).
AP and AP + 1 % AC particles of the order of 1 mm are
tial particle size range, that could be retrieved back after obtained and SEM images for these samples are taken after
exposing it to the atmosphere for increasing periods of 0 h, 1 h, 3 h and 6 h of their exposure to atmosphere as
time. Table 4 gives the atmospheric conditions, obtained shown in Figure 6. The images indicate that AP when
using a digital thermo hygrometer at the beginning and coated with 1 % AC prevents its agglomeration. It was ob-
end of the experimental period. Here, 80 g of sample is served that when the exposure time to atmosphere in-
used to perform the sieves analysis and the time used for creased, the AP particle size increased while the particle
which samples are sieved is 20 min. It is observed that the size of AP + 1 % AC remains mostly unchanged. At a finer
amount of AP that could be retrieved is around 50 % of its ammonium perchlorate particle size the rate at which it ag-
initial quantity, after just an hour of its exposure to the at- glomerates increases. This reduces the timeframe for am-
mosphere. In the case of AP + 1 % AC, this amount re- monium perchlorate to be used in propellants before the
trieved remained around 94 % even after 6 h of its exposure particle size distribution changes due to agglomeration. For
to atmosphere. The interesting outcome is that this re- gas generator applications propellant compositions that
trieved amount remained constant at around 94 %, though contain very fine particle size for AP are chosen and the ag-
the exposure time to atmosphere increased from 1 h to glomeration could become a serious “trouble-maker“.
6 h. Clearly, a coating of 1 % AC to AP is preventing AP
from agglomerating.
3.2 Burning Rate Studies
Figure 4 shows the comparison between the percentage
weight that could be retrieved for particle size range of 45– With the confidence gained from the above experiments
25 mm and 15–5 mm. In the case of gas generator motors, that 1 % AC coated over AP is very effective in preventing
where very high burning rates are required often, fine AP AP from agglomerating, further experiments are carried out
particles are employed. The agglomeration of AP can on the propellant compositions. These experiments were
become a major problem here, if AP is exposed to atmo- done in order to understand the effect of agglomeration
sphere even for an hour (as can be observed from Figure 3 on the burning rate of the propellant.
and Figure 4) while handling before being employed in Initially, burning rates are obtained for Mix 1 and Mix 2.
preparing the propellant composition. Figure 7 shows the results obtained for these compositions.
Further high-res SEM images are obtained using Quanta It can be observed that the propellant burning rates re-
200 manufactured by FEI for AP and AP + 1 % AC, after ex- duced when it contained AP which is exposed to the at-
posing them to atmosphere for increasing periods of time. mosphere for 6 h (Mix 2). This could be attributed to the
Figure 5 shows these pictures. As can be observed from agglomeration of AP particles. Burning rates of the propel-
these pictures, these were not conclusive. The results with lants are measured when AP particle size in the range of
the sieves analysis were very conclusive and this could be 15–5 mm is employed in them (Mix 3, Mix 4 and Mix 5).

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Reducing Agglomeration of Ammonium Perchlorate Using Activated Charcoal

Figure 7 shows the burning rates obtained for these pro-

pellants. It can be noticed that there is drop in the burning
rates when the propellant contained AP exposed to the at-
mosphere for 6 h. The decrease is larger when particle sizes
were in the range of 15–5 mm. This drop in burning rates
can be noted from Figure 8 for these compositions, which
also gives the percentage decrease in burning rates when
the propellant composition contained AP which is exposed
to the atmosphere for 6 h. This emphasizes the severity to
which agglomeration can affect the burning rate character-
istics of a propellant. The results shown here are at a partic-
ular humidity and temperature of the atmosphere and re-
sults could be different if these are modified.
Having observed the significance of maintaining particle
size range of AP that is being employed in preparing pro-
pellant compositions, further experiments are performed to
obtain the burning rates for the propellant compositions
that are prepared from AP + 1 % AC (Mix 6, Mix 7 and Mix
8). These results are also shown in Figure 9. The burning
rates for Mix 6 (propellant containing AP coated with 1 %
AC) are higher as compared to that for Mix 3 (propellant
with AP). This increase in the burning rates for Mix 6 is ex-
pected following the discussion on the mechanism of
action of AC by Ishitha and Ramakrishna [4]. When AP is
coated with AC, AC is at the AP-binder interfacial location
in the propellant and this was proposed to be the location
of action of AC in [4]. Also, it is seen here that the burning
rates of propellant composition that is prepared from AP +
1 % AC exposed to atmosphere for 6 h (Mix 8) are slightly
higher than that obtained for the composition prepared
from AP + 1 % AC unexposed to atmosphere (Mix 6). The
burning rate pressure index is also observed to have in-
creased for Mix 8. This behavior is attributed to the increase
in burning rates observed with AC containing moisture, as
has been reported by Verma and Ramakrishna [5]. This has
been further corroborated with the results obtained for
a propellant that contained 36 % of moisture in 1 % AC
(0.36 % in the propellant; Mix 9), wherein burning rates in-
creased significantly. These results are shown in Figure 10.
For 1 % AC to absorb 36 % of moisture, it is exposed to at-
mosphere for 126 h.
When AP + 1 % AC is exposed to atmosphere, it is not
only retaining its particle size, but also picking moisture
from the atmosphere. AP + 1 % AC after exposing to atmos-
phere for 6 h is observed to have increased in weight by
around 0.015 %. This increase in its weight could be
attributed to its absorption of moisture from atmosphere.
Though exposure to atmosphere is modifying the burning
rates of propellant even with AP + 1 % AC, the percentage
change is still lower than that with AP alone (see Figure 8).
Also, earlier studies (Verma and Ramakrishna [5]) demon-
strated that the mechanical properties of a propellant are
Figure 5. High-res SEM images with 4000 Õ magnification for (a) not modified due to the presence of moisture in AC.
AP after 0h of exposure to atmosphere, (b) AP after 6 h of expo- From the studies of Verma and Ramakrishna [5], if there
sure to atmosphere, (c) AP + 1 %AC after 0h of exposure to atmo- is moisture in the propellants (could be absorbed by AP)
sphere and (d) AP + 1 %AC after 6 h of exposure to atmosphere.
their burning rates increase. To examine the amount of

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Full Paper K. Ishitha, P. A. Ramakrishna

Figure 6. High-res SEM images with a magnification of 10,000 Õ for (a) AP after 0 h of exposure to atmosphere, (b) AP + 1 % AC after 0 h of
exposure to atmosphere, (c) AP after 1 h of exposure to atmosphere, (d) AP + 1 % AC after 1 h of exposure to atmosphere, (e) AP after 3 h
of exposure to atmosphere, (f) AP + 1 % AC after 3 h of exposure to atmosphere, (g) AP after 6 h of exposure to atmosphere and (h) AP +
1 % AC after 6 h of exposure to atmosphere.

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Reducing Agglomeration of Ammonium Perchlorate Using Activated Charcoal

Figure 7. Burning rates of propellant compositions. Figure 9. Comparison between burning rates of propellants with
AP alone and with AP coated with AC.

Figure 8. Comparison of burning rate results for compositions

with (a) AP of 45–25 mm at 1 MPa pressure, (b) AP of 45–25 mm at
7 MPa pressure, (c) AP of 15–5 mm at 1 MPa pressure, (d) AP of 15–
5 mm at 7 MPa pressure, (e) AP + 1 % AC of 15–5 mm at 1 MPa pres-
sure and (f) AP + 1 % AC of 15–5 mm at 7 MPa pressure; the per- Figure 10. Effect on burning rates if AC contains moisture.
centage change in the burning rates is also represented.

moisture being absorbed by AP on exposure to atmo- it follows that half the AP content is in a different particle
sphere (humidity and temperature), the weight of AP size range from that of the intended one. This decreases
(300 g) is monitored at the end of 1 h and 6 h using the burning rates of the propellant.
a weighing balance whose least count is 0.01 g. For the When considering 300 g of AP + 1 % AC, exposed to at-
period of experiment, the change in the weight of AP is in- mosphere for one hour, there is no increase in the weight
discernible. These experiments indicated the following: 1) as measured using a weighing balance with a least count
Exposure of AP to atmosphere is not causing AP to absorb of 0.01 g. There is negligible change in the particle size
as much moisture as AP + 1 % AC. However, AP particles range when exposed to atmosphere. This would mean that
size increases due to agglomeration, on its exposure to the burning rates of the propellants would remain unchanged,
atmosphere. The AP crystals could be just fusing with just with AP + 1 % AC when exposed to atmosphere for one
a small quantity of moisture it is picking from the atmos- hour (as can be observed from Figure 9).
phere. 2) If the handling time of AP is small, from Figure 3

Table 5. Observations corresponding to Figure 5.

Time Atmospheric conditions Observation
0h RH: 73 %; T = 35.2 8C No difference between AP and AP + 1 %AC SEM images
1h RH: 82 %; T = 38.2 8C Agglomeration of AP to around 1.5 mm can be noticed, no difference in AP + 1 %AC from 0 h
3h RH: 75 %; T = 39.6 8C Agglomeration of AP to around 3 mm can be noticed, no difference in AP + 1 %AC from 0 h
6h RH: 74 %; T = 38.5 8C Agglomeration of AP to around 5 mm can be noticed, no difference in AP + 1 %AC from 0 h is noticed

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Full Paper K. Ishitha, P. A. Ramakrishna

Experiments were also conducted to observe the ag-

glomeration characteristics of AP + 1 % AC, exposed to at-
mosphere for 126 h. These results are provided in
Figure 11. As can be observed from these SEM pictures,
AP + 1 % AC when exposed to atmosphere for 126 h
(Figure 11 (C)) seems to have slightly agglomerated as com-
pared with AP + 1 % AC, exposed to atmosphere for 6 h
(Figure 11 (b)).
It can be stated that when AP of lower particle size is
employed in a propellant composition, coating with AC is
an option to ensure that the burning rate characteristics
are not modified even if the handling time is more than
one hour.

4 Conclusions
Experimental studies are conducted to understand the
reason for the agglomeration of ammonium perchlorate
and to possibly reduce it. Sieve analysis and high resolution
SEM are employed to analyze AP samples. It is observed
that an increase in activated charcoal percentage coated
over ammonium perchlorate decreases the rate at which
AP agglomerates. A 1 % AC coating on AP completely pre-
vented the agglomeration of AP. The decrease in rate of ag-
glomeration of AP when coated with AC is attributed to
the porous nature of AC. When AC is coated over AP, AC is
exposed to the atmosphere (instead of AP) and the pores
of AC absorb the moisture, thereby preventing AP from ag-
glomerating.
The burning rate characteristics of propellant composi-
tions containing AP and AP coated with AC, exposed to at-
mosphere for 1 and 6 h, were studied in order to draw at-
tention to the severity of the problem of AP agglomeration.
The burning rates decreased for a propellant composition
that contained AP, which is exposed to the atmosphere, as
compared to the propellant composition prepared from AP,
which is unexposed to atmosphere. This reduction in the
burning rates has been attributed to the increase in the
particle size of AP (due to agglomeration). The reduction in
burning rates observed is even more significant when the
initial AP particle size range is decreased. In contrast, the
burning rates remained constant for a propellant composi-
tion that contained AP coated with 1 % AC, which is ex-
posed to atmosphere for 1 h, as compared to the propel-
lant composition which had AP coated with 1 % AC, which
isn’t exposed to atmosphere. The burning rates increased
for a propellant composition that contained AP coated
with 1 % AC, which is exposed to atmosphere for 6 h. This
increase in burning rates has been attributed to the mois-
ture absorbed by AC, coated over AP, on exposure to the
atmosphere. Though AP coated with 1 % AC also modifies
the burning rates of a composition on its exposure to the
Figure 11. High-res SEM images with 4000 Õ magnification (a) atmosphere for increased period of time, the percentage
AP + 1 %AC after 0 h of exposure to atmosphere, (b) AP + 1 %AC change is only half that for compositions with AP. Again,
after 6 h of exposure to atmosphere and (c) AP + 1 %AC after 126 h AP coated with 1 % AC is observed not to absorb any mois-
of exposure to atmosphere.

846 www.pep.wiley-vch.de Ó 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim Propellants Explos. Pyrotech. 2015, 40, 838 – 847
Reducing Agglomeration of Ammonium Perchlorate Using Activated Charcoal

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The authors acknowledge Dr. Subramanya Sarma Vadlamani and
Mr. T. Raghavaiah, Department of Metallurgical and Materials Engi- Received: November 5, 2014
neering, IIT Madras; Nikunj Rathi, PhD scholar, Aerospace Depart- Revised: July 16, 2015
ment, IIT Madras for their help in this study. Published online: September 23, 2015

Propellants Explos. Pyrotech. 2015, 40, 838 – 847 Ó 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim www.pep.wiley-vch.de 847