burning characteristics and thermochemical behavior of ap/htpb composite propellant using coarse and...

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Burning Characteristics and Thermochemical Behavior of AP/HTPB Composite Propellant Using Coarse and Fine AP Particles

Makoto Kohga*

Department of Applied Chemistry, National Defense Academy, Hashirimizu 1-10-20, Yokosuka, Kanagawa 239-8686(Japan)e-mail: [email protected]

Received: October 15, 2009; revised version: January 14, 2010

DOI: 10.1002/prep.200900088

Abstract

The burning rate of AP/HTPB composite propellant increaseswith increasing AP content and with decreasing AP size. In addi-tion, the burning rate can be enhanced with the addition ofFe2O3. The burning characteristics and thermal decompositionbehavior of AP/HTPB composite propellant using coarse andfine AP particles with and without Fe2O3 at various AP contentswere investigated to obtain an exhaustive set of data. As the APcontent decreased, the burning rate decreased and the propel-lants containing less than a certain AP content self-quenched ordid not ignite. The self-quenched combustion began at bothlower and higher pressures. The lower limit of AP content toburn the propellant with coarse AP was lower than that with fineAP. The lower limit of AP content to burn was decreased by theaddition of Fe2O3. The thermal decomposition behavior of pro-pellants prepared with 20–80% AP was investigated. The de-crease in the peak temperature of the exothermic decompositionsuggested an increased burning rate. However, a quantitative re-lationship between the thermochemical behavior and the burningcharacteristics, such as the burning rate and the lower limit ofAP content to burn, could not be determined.

Keywords: Ammonium Perchlorate, Burning Rate, BurningCatalyst, Composite Propellant, Thermal Decomposition

1 Introduction

The burning rate of the AP/HTPB composite propellantdepends on the AP content. The burning rate decreasesas the AP content decreases, and propellants containingless than a certain AP content self-quench or do notignite. Therefore, the propellants do not have self-sus-tained burning. A lower limit of AP content to burn, fmin,exists, and the fmin of the propellant with coarse AP islower than that with fine AP [1].

The addition of a burning catalyst greatly affects theburning rate characteristics of the propellant, and Fe2O3

is a good catalyst for an AP-based propellant. The fmin isdecreased by the addition of Fe2O3 to the propellant [2].The main thermal decomposition temperature range ofthe propellant is shifted to lower temperatures by the ad-dition of Fe2O3 [2–6], indicating that Fe2O3 improves thechemical reaction in the solid and/or gas phases of thepropellant [3,7].

The burning process of the AP/HTPB composite pro-pellant begins with the decomposition gases of AP andHTPB being produced at the burning surface by the heatfeedback from a flame. These gases diffuse and mix inthe gas phase and finally burn. The combustion mecha-nism of AP-based composite propellants has been investi-gated for many years and is almost established [8]. How-ever, sufficient experimental data have not yet been col-lected in order to describe the combustion mechanism.

The possibility of self-quenched combustion for theAP/HTPB composite propellant is dependent on complexfactors such as the AP content, pressure, particle proper-ties, thermal conductivity, and thermal decomposition be-havior. However, the experimental data to support amechanism and cause of the self-quenched burning havenot yet been obtained.

As mentioned above, the decomposition gases of APand HTPB are produced at the burning surface and theburning of the propellant is maintained by combustion re-actions of those decomposition gases. Therefore, the ther-mal decomposition behavior of the propellant influencesthe burning characteristics and is some of the causes ofthe self-quenched burning.

TG–DTA is a popular method to investigate the ther-mal decomposition behavior of materials and has beenused to investigate several kinds of propellants [1–6, 9–

Propellants Explos. Pyrotech. 2011, 36, 57 – 64 � 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim 57

13]. In previous reports, the AP content of the propellantwas constant and the relationship between the decompo-sition behavior and the burning characteristics for theAP/HTPB-based composite propellants at various APcontents has not been systematically investigated.

In this study, the burning characteristics and thermaldecomposition behavior of the AP/HTPB composite pro-pellant using coarse and fine AP particles with and with-out Fe2O3 at various AP contents were measured in orderto obtain an exhaustive experimental data set. Based onthis data, the relationship between the decomposition be-havior and the burning rate characteristics of AP/HTPBpropellant was investigated. This paper is one of a seriesrevealing the cause of self-quenched burning of AP-basedcomposite propellant.

2 Experiment

2.1 Materials and Propellant Samples

Coarse AP (CAP) and fine AP (FAP) were used as oxi-dizers in this study. CAP was prepared by grinding a com-mercial AP for 5 min in a vibration ball mill. FAP wasprepared by the freeze-drying method [14]. The meanparticle diameters of CAP and FAP were about 110 and4 mm, respectively.

The propellant samples were prepared with less than80% AP. HTPB was used as binder and was cured withisophorone diisocyanate. 8 % of isophorone diisocyanatewas added to HTPB, and Fe2O3 was used as a burningrate catalyst. First 1 % of Fe2O3 was added to the propel-lant, and the propellant mixtures were then cured for 7days at 333 K. The size of each strand was 10 mm in di-ameter and 40 mm in length. The side of each strand wasinhibited by silicon resin.

2.2 Measurement of Burning Rates

The burning rates were measured in a chimney-type strandburner, which was pressurized with nitrogen. The strandburner was set in a temperature conditioner operating at atemperature of around 290 K. The ignition of each strandwas conducted by an electrically heated nichrome wire at-tached to the top of each strand. The propellant strandwas combusted in a pressure range of 0.5–7 MPa. Theburning phenomenon of the propellant was recorded witha high-speed video recorder. The collected pictures wereused to measure the burning rates. Three lots of propel-lants were prepared at the same AP content. It was judgedthat the propellant could not combust when one of thethree lots of the propellants was self-quenched.

2.3 TG–DTA

The thermal decomposition behavior of the propellantwas investigated using TG–DTA over a temperaturerange from 473–723 K. The equipment was operated witha nitrogen flow (50 mL min�1) and at atmospheric pres-

sure. Six different heating rates (b) were used: 1, 2, 5, 10,15, and 20 K min�1.

Generally, TG–DTA is carried out with a small quanti-ty of a homogeneous sample. Reproducible TG–DTAcurves of the composite propellant were not obtainedwith a small amount of sample because the propellantwas heterogeneous. The scattering in TG–DTA curveswas reduced by increasing the sample mass. The heat re-leased in the exothermic decomposition increased with ahigher sample mass. When the sample mass was morethan 2 mg, the heating rate increased at the stage of theexothermic decomposition, indicating that the rate wasnot constant in the temperature range at the exothermicdecomposition. The sample masses were approximately1.5 mg in this study. The TG–DTA measurements wereconducted more than four times for each sample. Theaverages of the TG–DTA curves from the data were usedin this experiment.

2.4 Kinetic Analysis

The activation energy is an important thermal decomposi-tion property, and can be estimated by TG with theOzawa-Flynn-Wall method [15–17] or determined byDTA with Kissinger method [18]. As these methods donot need to know the reaction order or the reactionmodels, they are widely applicable. They quickly andsimply determine the activation energies directly fromTG–DTA data at several heating rates if the thermal de-composition behavior of the material is within the appli-cation of these methods. Because the activation energydetermined by these methods is the sum of the activationenergies of the chemical reactions and physical processesof thermal decomposition, it is called the apparent activa-tion energy.

The thermal decomposition of a solid is a heterogene-ous reaction that is generated locally within the reactivenucleus of a solid and then propagates to unreacted mate-rial. The thermal decomposition of the composite propel-lants involve multiple steps that are likely to have differ-ent activation energies, but the reaction models have notyet been determined. Some researchers have investigatedthe activation energies of solid high-energy materials andcomposite propellants with the Ozawa-Flynn-Wall andKissinger methods [6,10–13]. Though the thermal decom-position behavior of energetic materials and compositepropellants is very complex, these are useful methods fordetermining the activation energy of the composite pro-pellants.

In this study, the Ozawa-Flynn-Wall and Kissingermethods were applied to determine the activation energyof the decomposition process. Although differential scan-ning calorimetry is preferred over DTA for activationenergy determination, DTA was used in our experiments,because a differential scanning calorimeter was not avail-able. The activation energies determined by the Ozawa-Flynn-Wall and Kissinger methods are represented by Eo

and Ek, respectively.

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According to the Ozawa-Flynn-Wall method [15–17],Eo is determined by the following equation:

Eo

R¼ �2:19

d log b

dT�1o

ð1Þ

where To is the temperature at a constant degree of con-version and R is the gas constant. Eo can be calculatedfrom the slope of a plot of logb against T�1

o .According to the Kissinger method [18], Ek is deter-

mined from the maximum rate condition which will occurat the exothermic peak temperature, Tp, of the DTAcurves. Ek is represented by the following equation:

Ek

R¼ �

d ln bT�2

p

� �

dT�1

p

ð2Þ

and the value of Ek can be calculated from the slope of aplot of ln(bT�2

p ) against Tp�1.

3 Results and Discussion

3.1 Burning rate Characteristics

The burning rate characteristics of the propellants areshown in Fig. 1. The burning rate was reduced with de-creasing AP content. The propellants prepared with CAPand containing more than 64% AP burned in the pres-sure range adopted in this study. The propellant contain-ing 63% AP self-quenched at 0.5 MPa, and the propellantcontaining 62% AP self-quenched between 5 and 7 MPa.The burnable pressure range decreased with decreasingAP content. The propellant containing 55 % AP burnedonly between 1.5 and 2 MPa, whereas the propellant con-taining 54 % AP did not burn in the pressure rangeadopted in this study.

The propellants prepared with FAP and containingmore than 69 % AP burned between 0.5 and 7 MPa. Thepropellant containing 68 % AP self-quenched at 0.5 and7 MPa. The burnable pressure range was reduced with de-creasing AP content. The propellant containing 63% AP

burned only between 2 and 3 MPa, but the propellantcontaining 62 % AP did not burn in the pressure range ofthis study. These results indicated that the fmin values ofCAP and FAP were 55 % and 63 %, respectively. The fmin

of coarse AP was lower than that of fine AP, suggestingthat the combustion of the AP/HTPB composite propel-lant was dependent on the AP content, pressure and par-ticle size of AP.

The burning rate characteristics of the propellants withFe2O3 are shown in Fig. 2. The burning rate decreased asthe AP content decreased. The propellants prepared withCAP containing more than 52 % AP burned, whereasthose containing 51 % AP burned only between 1 and3 MPa. The propellants containing less than 50% AP didnot burn in the pressure range adopted in this study (0.5–7 MPa). The propellants prepared with FAP containingmore than 35% AP burned between 0.5 and 7 MPa,whereas the propellant containing 30 % AP burned onlybetween 2 and 5 MPa. The propellants containing lessthan 29% AP did not burn in the pressure range used inthis study.

The fmin of the propellant with Fe2O3 is represented bycfmin. The cfmin values of CAP and FAP were 51 % and30%, respectively. The lower limit of the AP content nec-essary to burn was decreased by the addition of Fe2O3.The difference between the cfmin and fmin values of thepropellant prepared with FAP was larger than that of thepropellant prepared with CAP, indicating that the dimin-ishing effect of Fe2O3 on the lower limit of AP content toburn became more significant as the size of AP particleswas decreased.

The relationship between the burning rate and the APcontent is illustrated graphically in Fig. 3. The burningrate was reduced with decreasing AP content. The burn-ing rates of the propellants with Fe2O3 were larger thanthose of the propellants without Fe2O3 at all pressures.For the propellant with CAP, the variation in burningrate against AP content slightly increased with increasingpressure and the variation of the propellant with Fe2O3

was slightly larger than that of the propellant withoutFe2O3.

Figure 1. Burning rate characteristics of: a) propellants withCAP; b) propellants with FAP.

Figure 2. Burning rate characteristics of propellants with Fe2O3:a) propellants with CAP; b) propellants with FAP.

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Burning Characteristics and Thermochemical Behavior of AP/HTPB Composite Propellant Using Coarse


On the other hand, the variation of the propellant pre-pared with FAP increased with increasing pressure, espe-cially with higher AP contents. The variations in theburning rate of the propellants with Fe2O3 were smallerthan those of the propellant without Fe2O3 and almostconstant with less than 45% AP.

The AP content greatly affected the burning character-istics of the propellant. The variation in the burning rateagainst the AP content of the propellant prepared withFAP was larger than that of the propellant prepared withCAP. From the results described above, we concludedthat the burning characteristics of the AP/HTPB propel-lants were affected by the AP size and content, combus-tion pressure, and addition of Fe2O3.

3.2 Thermal Decomposition Behavior

For all AP samples, the cfmin value was smaller than fmin.The cfmin values of the propellant prepared with CAPand FAP were 51 % and 30 %, respectively. The TG–DTA thermograms of some of the propellants containing40–80% CAP and 20–80% FAP were obtained to investi-gate the influence of the AP content and of the catalyston the decomposition behavior of the propellant.

The fmin values of the propellant with CAP and FAPwere 55% and 63 %, respectively. Figure 4 shows theTG–DTA curves of the propellants with 55 % CAP and63% FAP with and without Fe2O3. The endothermic peakwas observed at 514 K in the DTA curve due to the crys-tal transformation of AP and followed by exothermic de-composition. For the propellant containing CAP withoutFe2O3, the values of Tp at 1, 10, and 20 K min�1 were 611,643, and 665 K, respectively, and those for the propellantcontaining CAP with Fe2O3 were 592, 634, and 651 K, re-spectively. The Tp and the end temperature of the exo-thermic decomposition decreased with decreasing b. Atconstant b, the peak temperatures of the propellant withFe2O3 were lower than those of the propellant withoutFe2O3.

For the propellant with 63 % FAP and Fe2O3, the exo-thermic peak was not observed on the DTA curve at b of1 K min�1 because the endothermic peak of the crystaltransition point of AP overlapped with the exothermic

peak of the propellant. Therefore, the Tp value could notbe determined. For the propellant with FAP withoutFe2O3, the values of Tp at 1, 10, and 20 K min�1 were 576,643, and 656 K, respectively, and those for the propellantwith Fe2O3 at 10 and 20 K min�1 were 540 and 555 K, re-spectively.

Based on the TG curves, most of the consumption oc-curred between the beginning and end temperatures ofthe exothermic decomposition. The mass loss at the endtemperature of the exothermic decomposition decreasedwith decreasing AP content. As mentioned above, the Tp

and the end temperature of the exothermic decomposi-tion were shifted to lower values with the addition ofFe2O3 and decreased with decreasing b. Therefore, theTG curve was also affected by the value of b and thepresence of Fe2O3, even when the AP content was con-stant.

Figure 5 illustrates the relationship between Tp and theAP content. Tp decreased with decreasing b. At constantb, the values of Tp were almost constant, except for thepropellant with FAP and without Fe2O3, for which thevalues of Tp below 28% FAP were lower than thoseabove 29% FAP.

The value of Tp of the propellant with FAP was lowerthan that of the propellant with CAP, and Tp was de-creased by the addition of Fe2O3. For the propellant withFAP, the maximum decrease in Tp by the addition ofFe2O3 was 105 K (at 40 % FAP), whereas it was 33 K (at73% CAP) for the propellant with CAP. The differencein Tp of the propellant with FAP was greater than that ofthe propellant with CAP. The increase in the burning rateof the propellant containing FAP by the addition ofFe2O3 was larger than that of the propellant containingCAP, as shown in Fig. 3. The decrease in Tp suggested anincreased burning rate when Fe2O3 was added to the pro-pellant. However, a quantitative estimation of the in-crease in the burning rate could not be established withthe change in Tp in this experiment.

As mentioned in Section 3.1, the burning rate de-creased with decreasing AP content. The fmin values ofpropellant with CAP and FAP were 55% and 63 %, andthe cfmin values of the propellant with CAP and FAPwere 51 % and 30 %, respectively. At constant b, thevalue of Tp was independent of the AP content and didnot change at fmin and cfmin, indicating that Tp was not di-rectly dependent on the burning characteristics.

3.3 Kinetics of Thermal Decomposition

Sell et al. [10] measured the Eo values of the AP/HTPBpropellant with 70.25 % AP by the Ozawa-Flynn-Wallmethod and reported that Eo was about 100 kJ mol�1

below a degree of conversion of 0.08 and was between175 and 200 kJ mol�1 at degrees of 0.2–0.6. Therefore, thevariation in Eo was small for a degree of conversion of0.2–0.8. The consumption at the main thermal decomposi-tion decreased with decreasing AP content, and the massloss of the propellant with 20% FAP was approximately

Figure 3. Relationship between burning rate and AP content:a) propellants with CAP; b) propellants with FAP.


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30%. In this experiment, the Eo values were determinedat degrees of conversion of 0.25–0.5.

To calculate Eo, logb was plotted as a function of theT�1

o values obtained from the TG curves. RepresentativeOzawa-Flynn-Wall plots are shown in Fig. 6. For each APcontent, the plots roughly followed the form of Eq. (1),and displayed an approximately linear relationship. Theslope of the line was calculated from these plots, and Eo

was calculated by substituting the slope into Eq. (1).

Figure 7 shows the influence of the AP content on Eo.The value of Eo increased with increasing AP content,and the relationship was not affected by the addition ofFe2O3. The variation in Eo against the AP content of thepropellant with CAP was larger than that of the propel-lant with FAP. The Eo value slightly depended on the sizeof AP, whereas the presence of Fe2O3 hardly influencedEo.

Figure 4. TG–DTA curves of propellant: a) with 55 %CAP; b) with 55%CAP and Fe2O3; c) with 63% FAP; d) with 63 % FAP andFe2O3.




To calculate Ek, lnðbT�2p Þ was plotted as a function of

T�1p values obtained from the DTA curves. Several Kis-

singer plots are shown in Fig. 8, and exhibited almost

straight lines for each AP content. The slopes of the lineswere determined and Ek was calculated by substitutingthe slopes into Eq. (2). Figure 9 shows the influence of

Figure 5. Relationship between Tp and AP content: a) propellant using CAP; b) propellant using CAP with Fe2O3; c) propellantusing FAP; d) propellant using FAP with Fe2O3.

Figure 6. Ozawa-Flynn-Wall plots: a) propellant with CAP; b)propellant with CAP and Fe2O3; c) propellant with FAP; d) pro-pellant with FAP and Fe2O3.

Figure 7. Dependence of AP content on Eo: a) propellant withCAP; b) propellant with CAP and Fe2O3; c) propellant withFAP; d) propellant with FAP and Fe2O3.


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the AP content on Ek. The values of Ek for the propellantwith CAP and FAP were determined to be approximately150 and 130 kJ mol�1, respectively. The Ek of the propel-lant with CAP was larger than that of the propellant withFAP. These values depended on neither the AP contentnor the presence of Fe2O3. The Ek decreased with de-creasing AP size, but was influenced by the AP contentand Fe2O3.

Once Ek was determined, the values of pre-exponentialfactor, A, were calculated with the equation:

A ¼bEk expðEkR�1T�1

p ÞRT 2

p

ð3Þ

The values of A of the propellant containing CAP with-out and with Fe2O3 were 1.0 �109–7.2�1014 min�1 and9.6 �1010–1.6� 1014 min�1, respectively. The A values ofthe propellant containing FAP without and with Fe2O3

were 7.9� 107–6.3 �1013 min�1 and 1.1 �109–1.1 �1013

min�1, respectively. The value of A did not depend on theAP particle size, AP content, or Fe2O3 in this study.

As described in Section 3.1, the burning rate increasedwith increasing AP content, and at a constant AP con-tent, the burning rate of the propellant with FAP washigher than that with CAP. Furthermore, the burning rateof the propellant with Fe2O3 was about twice that withoutFe2O3. The self-quenched combustion began at bothlower and higher pressures. The lower limit of AP contentto burn was dependent of the AP size and presence ofFe2O3. In conclusion, the burning characteristics of theAP/HTPB composite propellant greatly depended on theAP content, AP size, pressure, and presence of Fe2O3.

For the AP/HTPB composite propellant, the decompo-sition gases of AP and HTPB are produced at the burningsurface and the combustion of the propellant is sustainedby the burning of the decomposition gases. Therefore, thedecomposition behavior of the propellant should influ-ence the burning characteristics.

Herein, an exhaustive experimental data set on thethermal decomposition behavior of the AP/HTPB com-posite propellant was obtained. However, the thermal de-composition properties, such as Tp, Ek, and Eo, did not in-fluence the burning characteristics, such as the burningrate, fmin, or cfmin, within the limit of this study.

The burning rate was measured in the range of 0.5–7 MPa, and the thermal decomposition behavior was in-vestigated at atmospheric pressure. The heating rate ofTG–DTA was studied over the range of 1–20 K min�1.The thermal decomposition at the burning surface of apropellant was more than 10000 times higher than that ofthe TG–DTA heating rates. The thermal decompositionbehavior under rapid heating and high pressure should beinvestigated further to explore the relationship betweenthe burning characteristics and thermal decomposition.

4 Conclusions

The burning characteristics and thermal decompositionbehavior of the AP/HTPB composite propellant usingcoarse and fine AP particles with and without Fe2O3 atvarious AP contents were investigated. As the AP con-tent decreased, the burning rate decreased and the pro-pellants containing less than a certain AP content self-quenched or did not ignite. The self-quenched combus-

Figure 8. Kissinger plots: a) propellant with CAP; b) propellantwith CAP and Fe2O3; c) propellant with FAP; d) propellant withFAP and Fe2O3.

Figure 9. Influence of AP content on Ek: a) propellant withCAP; b) propellant with CAP and Fe2O3; c) propellant withFAP; d) propellant with FAP and Fe2O3.




tion began at both lower and higher pressures. The lowerlimit of AP content for the propellant without Fe2O3 toburn was lower with coarse AP than with fine AP. Thelower limit of AP content to burn was decreased by theaddition of Fe2O3 and that for the propellant with Fe2O3

using fine AP was lower than that with coarse AP. Theburning characteristics of the AP/HTPB composite pro-pellant greatly depended on the AP content, AP size,pressure, and presence of Fe2O3.

The TG–DTA curves were dependent on the AP parti-cle size, heating rate, and presence of Fe2O3. The decreasein the exothermic peak temperature of the DTA curvesuggested the possibility of an increased burning rate.However, a quantitative estimation of the increase in theburning rate could not be established with the change inpeak temperature. The activation energies for the thermaldecomposition of the propellants were determined withthe Ozawa-Flynn-Wall and Kissinger methods, and deter-mined not to be clearly associated with the burning char-acteristics, such as the burning rate and the lower limit ofAP content to burn.

Symbols and Abbreviations

Chemicals:AP Ammonium perchlorateFe2O3 Iron(III) oxideHTPB Hydroxyl-terminated polybutadieneAcronyms:CAP Coarse APDTA Differential thermal analysisFAP Fine APTG ThermogravimetryOther:A Pre-exponential factorEk Activation energy determined by the Kissinger

methodEo Activation energy determined by the Ozawa-

Flynn-Wall methodR Gas constantTo Temperature at constant degree of conversionTp Temperature of exothermic peakb Heating ratefmin Lower limit of AP content to burncfmin fmin of propellant with Fe2O3

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