The researches done on particle size of explosive materials show that with reducing
of particle size of explosive materials, reduced impact, friction and shock waves
sensitivity. also by using of ultrafine explosive materials in propellant in comparison to
larger particle size improved density, stability, calory and mechanical properties. Meanwhile
the reduction of particle size of explosive materials influence on combustion
mechanism of propellant and reduced burning rate and exponent pressure of different
methods used for reduction of particle size, for example, milling, crystallization and etc.
In this article for preparation of ultrafine HMX the method of solvent-anti solvent has
been used by assistance of ultrasonic device. In optimum state the average size of particle
is 106 nm and size distribution is narrow.
When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/2068

Bayat, F.

Bayat, Ya.

Gholamhosseini, T.

Mousavi, S.H.

Nasad, G.R.

SocioEconomic Challenges Journal (Sumy State University)

322                  Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II           
 
PREPARATION NANO SIZED HMX BY USING  
ULTRASONIC WAVES 
Yadollah Bayat1, Seyed Hamed Mousavi1,2, Fatemeh Bayat2, 
Gholamhossein Rastegar Nasab2, Tahereh Gholamhosseini2 
 
1 Faculty of Chemistry and Engineering Chemistry, Malek Ashtar University of Technology, 
16765-3454, Tehran, Iran 
2 Zakaria Razi Student Research Center, Rey City, 18735-677, Tehran, Iran 
 
ABSTRACT 
The researches done on particle size of explosive materials show that with reduc-
ing of particle size of explosive materials, reduced impact, friction and shock waves 
sensitivity. also by using of ultrafine explosive materials in propellant in comparison to 
larger particle size improved density, stability, calory and mechanical properties. Mean-
while the reduction of particle size of explosive materials influence on combustion 
mechanism of propellant and reduced burning rate and exponent pressure of different 
methods used for reduction of particle size, for example, milling, crystallization and etc. 
In this article for preparation of ultrafine HMX the method of solvent-anti solvent has 
been used by assistance of ultrasonic device. In optimum state the average size of parti-
cle is 106 nm and size distribution is narrow.  
 
Key words: Sedimentary Crystallization, Ultrasonic, Reduce Particle Size, HMX 
 
INTRODUCTION 
By the development of explosive materials with improvement perfor-
mance and the reduction of sensitivity to mechanical stimuli such as impact and 
friction is one of the important researches goals in energetic fields. With reduc-
ing particle size of explosive materials decrease crystal defects and inclusion. 
This will reduce the sensitivity of explosive materials. Therefore safety of ma-
terials increases during handelling, processing, warehousing, and transporta-
tion. There searches done on the role of superfine particles of explosive materi-
als in propellant show that with reducing of particles size increase density, 
calory, stability, and mechanical properties. Also one of the most important 
affecting issues on burning rate of propellant is the particles size of explosive 
materials. By using these ultrafine explosive materials in the propellant, the 
burning rate and exponent pressure decrease [1]. Various methods used for the 
reduction of the particles size of materials that the selection methods depend 
materials and expected properties such as the particles size distribution. Two 
general methods used for the reduction of the particles size up to down method 
                                               
 e-mail: mousavi.seyedhamed@gmail.com, tel: (+98)21333625  
Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II                  323 
 
including mechanical methods (grinding) and down to up method, including 
crystallization method (sediment crystallization fusion, supercritical fluid, and 
etc . In the reduction of particles size in mechanical technique reduction of 
particles size in mechanical technique, solids construction elements have been 
broken by mechanical forces and increasing the mass distribution happens. To 
reduce the particles size with mechanical method used various equipment such 
as pinned disk mill, jet mill, colloid mill, ball mill, etc. . Mentioned methods 
have disadvantages such as static, electricity, pressure, and trituration that with 
considering the disadvantages, these methods are powerless and insecure to 
produce these ultrafine explosive materials [2-6]. Crystallization is the conver-
sion of one or more material from liquid or gas state to crystalline state. This 
method used for modifying the physical properties of substance. In addition, the 
crystallization is a process for thickening pure material  from solution, melt or 
gas  phase one of the suitable methods for producing these ultrafine crystal of 
explosive materials is sedimentary crystallization method solvent-anti solvent . 
Because in method nucleation is high and high degree of saturation is seen. 
Although crystallization methods for preparing explosive materials have signif-
icant and advantages and crystals can grow slowly away from stress and obtain 
an ideal crystal. These methods have disadvantages such as [6-9]: 
A: Sample should be soluble in one or more solvent solution and 
precipitate with reduction of temperature or increasing of anti-solvent.  
B: Contaminate crystals to solvent and other solvate. 
C: They spend too much energy. 
D: Having lower yield (Because occurs in several stages) 
A new method to produce ultrafine explosive is the kinetic spray 
crystallization that submicron size HMX and RDX are prepared with this 
method. The obtained particles size distribution with this method is very 
narrow. This schematic has been shown in Fig.1 [10] Solvent/anti-solvent for 
spray  solution  by  air  into  anti-solvent  is  used  to  produce  ultrafine  HMX  The  
average of the obtained particles size with this method is 245 nm [1]. Also Mr. 
Lee and et al. by using sedimentary crystallization method have achieved HMX 
with an average particle size of 300 nm [11]. 
 
Fig. 1 – Principle of kinetic spray crystallizing method [10]. 
324                  Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II           
 
In this research solvent/anti-solvent method has been used for producing 
ultrafine HMX by the assistance of ultrasonic device. In this method for 
controlling the crystallization process, the ultrasonic energy is used. To create 
ultrasonic waves, piezoelectric converters are used. These converters converted 
electrical energy into mechanical vibration with the same frequency. 
Mechanism to reduce the particles size of solid and emulsions by ultrasonic 
waves  is  cavitation.  Cavitation  is  used  as  the  center  of  nucleation  of  new  
crystals and growing. Also producing bubbles and bursting them caused 
trituration and grinding of solid particles [12]. 
SAFETY 
Generally by development of nanotechnology and producing nano parti-
cles in different scientific fields duet to the specific nature of nano particles 
produced  and creating risk for human health, Considering the work, safety 
during producing, transportation, warehousing, and applying of nano particles 
should be considered. Therefore at the same time by growing the technology in 
producing nano particles, safety problems and diseases have been considered. 
In Considering the risks of  toxicity of nano material in three contact areas in 
human body with the environment can be mentioned: skin, respiratory system, 
lungs, digestive system (mouth-esophagus).These three elements  are  the enter-
ies for the nano particles in human body and  from the way it can be entered in 
blood stream and internal systems and nervous. Of course it should be men-
tioned that the safety hints for producing nano explosive materials are not 
available. There fore, the respiratory mask, gloves, and suitable ventilation 
system can be away to control damages [13].  
EXPERIMENT 
Equipment 
Ultrasonic device used 
H80 model is made in Elma 
Company of Germany. To 
determine the morphology and 
particle size of electronic 
Microscope XL30 
manufactured in Philips 
Company of Dutch has been 
used. Installed equipment for 
doing the experiment is shown 
in Fig.2. 
 Procedure 
In this method certain concentrations of HMX in acetone solvent prepared 
at room temperature (Table 1)  and  then  by  using  of  a  burette  of  0.5  cc  are  
injected into an erlenmeyer flask containing anti–solvent (water) that its 
 
Fig. 2 – Installed Equipment 
Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II                  325 
 
temperature is zero degrees Celsius. Solvent injection rate is about 0.7 ml per 
minute. Ultrasonic frequency is 80 Hz and its power is 750 Watt. 
 
Table 1 – Characteristic of produced samples 
Sample 
name 
Amount of 
HMX (gr.) 
Solvent 
(acetone) (ml) 
Anti-
solvent(water)(ml) 
Anti-solvent 
Temperature 
(centigrade 
degree) 
Sample-1 0.1 5 80 0 
Sample-2 0.1 10 80 0 
Sample-3 0.1 20 80 0 
 
RESULTS AND DISCUSSION 
SEM image and the particles size distribution graph of sample respectively have 
been shown in Fig. 3 and Fig. 4. Also SEM image and the particles size distribution 
graph of sample-2 in Fig. 5, Fig. 6 and sample-3 in Fig. 7, Fig.  8 have been shown 
respectively.  
 
 
 Fig. 3 – SEM image of sample -1 
 
Fig. 4 – The particles size distribution by 
analysis of sample -1 
 
Fig. 5 – SEM image of sample -2 
 
Fig. 6 – The particles size distribution by 
analysis of sample -2 
326                  Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II           
 
 
Fig. 7 – SEM image of sample -3 
 
Fig. 8 – The particles size distribution by 
analysis of sample -3 
 
According to the images and the particles size distribution graph, it is 
observed with reduction of concentration samples can be achieved to smaller 
particle size. The best particle size is related to sample -3 that have the lowest 
concentration among the prepared solutions. The obtained average particles 
size is 106 nm. The reason for the reduction of the particles size with reduction 
of concentration is expressed with the degree of relative supersaturated 
theories. In other words, with reduction of samples concentration increases the 
degree of relative super saturation. Consequently, nucleation rate is more than 
nuclei growth and obtained smaller particle size. The results about the obtained 
particles size have been shown in Table 2. 
 
Table 2 – The analysis of particles size distribution 
Sample name Number of particles 
Average of 
particles 
Minimum  of  
particles  size 
Maximum  of 
particles  size 
Sample-1 80 0.0141 0.061 0.261 
Sample-2 85 0.133 0.043 0.0210 
Sample-3 85 0.106 0.037 0.0261 
 
CONCLUSION 
By the development of science in various fields application of nano 
materials has been expanded considerably. Among its applications can be 
mentioned to pharmaceutics, explosive materials, and etc. Various methods 
such as grinding, crystallization and sol-gel are used for producing materials in 
nano scale. One of the most common methods for producing nano-size 
explosive is sedimentary crystallization or solvent/anti-solvent method. 
Ultrasonic method combining this method and it can be a good idea for 
producing materials in nano scale. In this method different factors can influence 
on the particles size and the particles size distribution production. One of these 
factors is the concentration of produced solution. Investigation results showed 
that by reduction of solution concentration can achieve to smaller particle. In 
Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II                  327 
 
optimum state, the average of particle size was 106 nm One of the most 
important factors for producing of the nano particles that should be considered 
is agglomeration  of them that it has been a little reduced by using of ultrasonic. 
But research should be done to prevent agglomeration of nano-sized particles. 
REFERENCES  
[1] S.H. Mousavi, M.sc. thesis, Malek Ashtar University of Technology, 2010, P. 82-86, 
[2] M.H. Prior, M. Rhodes, "Size reduction", Principles of Powder Technology, Whily, 
Chichester, 1980, P. 227-297. 
[3] D. Eskin, H.  Kalman, Chemical Engineering Technology, Vol. 25, No. 1, 2002, 
P. 57-64,  
[4] U. Teipel, Journal of Propellants, Explosives, Pyrotechnics, Vol. 24,1999, P. 134-
149. 
[5] S. Miranda, S. Yaegeer, Chemical Engineering, Vol. 11, No. 12, , 1998 P. 102-110. 
[6] R. Brooks, A.T. Horton, J.L Torgesen, Journal of Crystal Growth, 1968, P. 279-283. 
[7] W.H.M. Welland, Van Der Heijden, A.E.D.M., Cianfanelli, S., Batenburg, L.F., 43rd 
AIAA/ASME/SAE/ASEE Joint Propulsion Conference & Exhibit, 2007, P. 1-7. 
[8] W.H.M. Veltmans, A.E.D.M. Van Der Heijden, J.M. Bellerby, M.I. Rodgers, , 
"Nitroformate Product Chracteristics", Proceedings 30th International Annual Con-
ference of Fraunhofer-Institut fur Chemische Technologie(ICT), Karlsmhe, "The Ef-
fect of Different Crystalization Techniques on Morphology and Stability of HNF", 
Proceedings 31st International Annual Conference of Fraunhofer-Institut fur Chem-
ische Technologie(ICT), Karlsmhe, 2000, P. 22. 
[9] A.E.D.M. Van Der Heijden, G.M. Van Rosmalen, D.T.J. Hurle, , Handbook of 
Crystal Growth, Elsevier, Amsterdam, 1994, Vol. 2, part A, P. 315. 
[10] Z. Shuhai, Z. Jinglin, W. Jingyu, Fraunhofer-Institut fur Chemische Technolo-
gie(ICT), 2004, P. 100-1 – 100-4. 
[11] K.Y. Lee, D.S. Moore, B.W. Asay, A.  Llobet, Journal of Energetic Materials, 
Vol. 25, 2007, P. 161-171. 
[12] U. Teipel, I. Mikonsaari, Propellants, explosives, pyrotechnics, Vol. 27, 2002, 
P. 168-174. 
[13] Y. Bayat, H. Dehgani, N. Zekri, F. Abrishami, "Investigation and producing nano-
sizde HMX in lab scale" Project report, Malek Ashtar University of Technology, 
2005, P. 215-225. 
 
  


Preparation nano sized HMX by using ultrasonic waves

Electronic Sumy State University Institutional Repository

322                  Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II            PREPARATION NANO SIZED HMX BY USING  ULTRASONIC WAVES Yadollah Bayat1, Seyed Hamed Mousavi1,2, Fatemeh Bayat2, Gholamhossein Rastegar Nasab2, Tahereh Gholamhosseini2  1 Faculty of Chemistry and Engineering Chemistry, Malek Ashtar University of Technology, 16765-3454, Tehran, Iran 2 Zakaria Razi Student Research Center, Rey City, 18735-677, Tehran, Iran  ABSTRACT The researches done on particle size of explosive materials show that with reduc-ing of particle size of explosive materials, reduced impact, friction and shock waves sensitivity. also by using of ultrafine explosive materials in propellant in comparison to larger particle size improved density, stability, calory and mechanical properties. Mean-while the reduction of particle size of explosive materials influence on combustion mechanism of propellant and reduced burning rate and exponent pressure of different methods used for reduction of particle size, for example, milling, crystallization and etc. In this article for preparation of ultrafine HMX the method of solvent-anti solvent has been used by assistance of ultrasonic device. In optimum state the average size of parti-cle is 106 nm and size distribution is narrow.   Key words: Sedimentary Crystallization, Ultrasonic, Reduce Particle Size, HMX  INTRODUCTION By the development of explosive materials with improvement perfor-mance and the reduction of sensitivity to mechanical stimuli such as impact and friction is one of the important researches goals in energetic fields. With reduc-ing particle size of explosive materials decrease crystal defects and inclusion. This will reduce the sensitivity of explosive materials. Therefore safety of ma-terials increases during handelling, processing, warehousing, and transporta-tion. There searches done on the role of superfine particles of explosive materi-als in propellant show that with reducing of particles size increase density, calory, stability, and mechanical properties. Also one of the most important affecting issues on burning rate of propellant is the particles size of explosive materials. By using these ultrafine explosive materials in the propellant, the burning rate and exponent pressure decrease [1]. Various methods used for the reduction of the particles size of materials that the selection methods depend materials and expected properties such as the particles size distribution. Two general methods used for the reduction of the particles size up to down method                                                 e-mail: mousavi.seyedhamed@gmail.com, tel: (+98)21333625  Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II                  323  including mechanical methods (grinding) and down to up method, including crystallization method (sediment crystallization fusion, supercritical fluid, and etc . In the reduction of particles size in mechanical technique reduction of particles size in mechanical technique, solids construction elements have been broken by mechanical forces and increasing the mass distribution happens. To reduce the particles size with mechanical method used various equipment such as pinned disk mill, jet mill, colloid mill, ball mill, etc. . Mentioned methods have disadvantages such as static, electricity, pressure, and trituration that with considering the disadvantages, these methods are powerless and insecure to produce these ultrafine explosive materials [2-6]. Crystallization is the conver-sion of one or more material from liquid or gas state to crystalline state. This method used for modifying the physical properties of substance. In addition, the crystallization is a process for thickening pure material  from solution, melt or gas  phase one of the suitable methods for producing these ultrafine crystal of explosive materials is sedimentary crystallization method solvent-anti solvent . Because in method nucleation is high and high degree of saturation is seen. Although crystallization methods for preparing explosive materials have signif-icant and advantages and crystals can grow slowly away from stress and obtain an ideal crystal. These methods have disadvantages such as [6-9]: A: Sample should be soluble in one or more solvent solution and precipitate with reduction of temperature or increasing of anti-solvent.  B: Contaminate crystals to solvent and other solvate. C: They spend too much energy. D: Having lower yield (Because occurs in several stages) A new method to produce ultrafine explosive is the kinetic spray crystallization that submicron size HMX and RDX are prepared with this method. The obtained particles size distribution with this method is very narrow. This schematic has been shown in Fig.1 [10] Solvent/anti-solvent for spray  solution  by  air  into  anti-solvent  is  used  to  produce  ultrafine  HMX  The  average of the obtained particles size with this method is 245 nm [1]. Also Mr. Lee and et al. by using sedimentary crystallization method have achieved HMX with an average particle size of 300 nm [11].  Fig. 1 – Principle of kinetic spray crystallizing method [10]. 324                  Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II            In this research solvent/anti-solvent method has been used for producing ultrafine HMX by the assistance of ultrasonic device. In this method for controlling the crystallization process, the ultrasonic energy is used. To create ultrasonic waves, piezoelectric converters are used. These converters converted electrical energy into mechanical vibration with the same frequency. Mechanism to reduce the particles size of solid and emulsions by ultrasonic waves  is  cavitation.  Cavitation  is  used  as  the  center  of  nucleation  of  new  crystals and growing. Also producing bubbles and bursting them caused trituration and grinding of solid particles [12]. SAFETY Generally by development of nanotechnology and producing nano parti-cles in different scientific fields duet to the specific nature of nano particles produced  and creating risk for human health, Considering the work, safety during producing, transportation, warehousing, and applying of nano particles should be considered. Therefore at the same time by growing the technology in producing nano particles, safety problems and diseases have been considered. In Considering the risks of  toxicity of nano material in three contact areas in human body with the environment can be mentioned: skin, respiratory system, lungs, digestive system (mouth-esophagus).These three elements  are  the enter-ies for the nano particles in human body and  from the way it can be entered in blood stream and internal systems and nervous. Of course it should be men-tioned that the safety hints for producing nano explosive materials are not available. There fore, the respiratory mask, gloves, and suitable ventilation system can be away to control damages [13].  EXPERIMENT Equipment Ultrasonic device used H80 model is made in Elma Company of Germany. To determine the morphology and particle size of electronic Microscope XL30 manufactured in Philips Company of Dutch has been used. Installed equipment for doing the experiment is shown in Fig.2.  Procedure In this method certain concentrations of HMX in acetone solvent prepared at room temperature (Table 1)  and  then  by  using  of  a  burette  of  0.5  cc  are  injected into an erlenmeyer flask containing anti–solvent (water) that its  Fig. 2 – Installed Equipment Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II                  325  temperature is zero degrees Celsius. Solvent injection rate is about 0.7 ml per minute. Ultrasonic frequency is 80 Hz and its power is 750 Watt.  Table 1 – Characteristic of produced samples Sample name Amount of HMX (gr.) Solvent (acetone) (ml) Anti-solvent(water)(ml) Anti-solvent Temperature (centigrade degree) Sample-1 0.1 5 80 0 Sample-2 0.1 10 80 0 Sample-3 0.1 20 80 0  RESULTS AND DISCUSSION SEM image and the particles size distribution graph of sample respectively have been shown in Fig. 3 and Fig. 4. Also SEM image and the particles size distribution graph of sample-2 in Fig. 5, Fig. 6 and sample-3 in Fig. 7, Fig.  8 have been shown respectively.     Fig. 3 – SEM image of sample -1  Fig. 4 – The particles size distribution by analysis of sample -1  Fig. 5 – SEM image of sample -2  Fig. 6 – The particles size distribution by analysis of sample -2 326                  Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II             Fig. 7 – SEM image of sample -3  Fig. 8 – The particles size distribution by analysis of sample -3  According to the images and the particles size distribution graph, it is observed with reduction of concentration samples can be achieved to smaller particle size. The best particle size is related to sample -3 that have the lowest concentration among the prepared solutions. The obtained average particles size is 106 nm. The reason for the reduction of the particles size with reduction of concentration is expressed with the degree of relative supersaturated theories. In other words, with reduction of samples concentration increases the degree of relative super saturation. Consequently, nucleation rate is more than nuclei growth and obtained smaller particle size. The results about the obtained particles size have been shown in Table 2.  Table 2 – The analysis of particles size distribution Sample name Number of particles Average of particles Minimum  of  particles  size Maximum  of particles  size Sample-1 80 0.0141 0.061 0.261 Sample-2 85 0.133 0.043 0.0210 Sample-3 85 0.106 0.037 0.0261  CONCLUSION By the development of science in various fields application of nano materials has been expanded considerably. Among its applications can be mentioned to pharmaceutics, explosive materials, and etc. Various methods such as grinding, crystallization and sol-gel are used for producing materials in nano scale. One of the most common methods for producing nano-size explosive is sedimentary crystallization or solvent/anti-solvent method. Ultrasonic method combining this method and it can be a good idea for producing materials in nano scale. In this method different factors can influence on the particles size and the particles size distribution production. One of these factors is the concentration of produced solution. Investigation results showed that by reduction of solution concentration can achieve to smaller particle. In Nanomaterials: Applications and Properties (NAP-2011). Vol. 2, Part II                  327  optimum state, the average of particle size was 106 nm One of the most important factors for producing of the nano particles that should be considered is agglomeration  of them that it has been a little reduced by using of ultrasonic. But research should be done to prevent agglomeration of nano-sized particles. REFERENCES  [1] S.H. Mousavi, M.sc. thesis, Malek Ashtar University of Technology, 2010, P. 82-86, [2] M.H. Prior, M. Rhodes, "Size reduction", Principles of Powder Technology, Whily, Chichester, 1980, P. 227-297. [3] D. Eskin, H.  Kalman, Chemical Engineering Technology, Vol. 25, No. 1, 2002, P. 57-64,  [4] U. Teipel, Journal of Propellants, Explosives, Pyrotechnics, Vol. 24,1999, P. 134-149. [5] S. Miranda, S. Yaegeer, Chemical Engineering, Vol. 11, No. 12, , 1998 P. 102-110. [6] R. Brooks, A.T. Horton, J.L Torgesen, Journal of Crystal Growth, 1968, P. 279-283. [7] W.H.M. Welland, Van Der Heijden, A.E.D.M., Cianfanelli, S., Batenburg, L.F., 43rd AIAA/ASME/SAE/ASEE Joint Propulsion Conference & Exhibit, 2007, P. 1-7. [8] W.H.M. Veltmans, A.E.D.M. Van Der Heijden, J.M. Bellerby, M.I. Rodgers, , "Nitroformate Product Chracteristics", Proceedings 30th International Annual Con-ference of Fraunhofer-Institut fur Chemische Technologie(ICT), Karlsmhe, "The Ef-fect of Different Crystalization Techniques on Morphology and Stability of HNF", Proceedings 31st International Annual Conference of Fraunhofer-Institut fur Chem-ische Technologie(ICT), Karlsmhe, 2000, P. 22. [9] A.E.D.M. Van Der Heijden, G.M. Van Rosmalen, D.T.J. Hurle, , Handbook of Crystal Growth, Elsevier, Amsterdam, 1994, Vol. 2, part A, P. 315. [10] Z. Shuhai, Z. Jinglin, W. Jingyu, Fraunhofer-Institut fur Chemische Technolo-gie(ICT), 2004, P. 100-1 – 100-4. [11] K.Y. Lee, D.S. Moore, B.W. Asay, A.  Llobet, Journal of Energetic Materials, Vol. 25, 2007, P. 161-171. [12] U. Teipel, I. Mikonsaari, Propellants, explosives, pyrotechnics, Vol. 27, 2002, P. 168-174. [13] Y. Bayat, H. Dehgani, N. Zekri, F. Abrishami, "Investigation and producing nano-sizde HMX in lab scale" Project report, Malek Ashtar University of Technology, 2005, P. 215-225.    

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Preparation nano sized HMX by using ultrasonic waves

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