نجوى واسر Al-Khwarizmi Engineering Journal,Vol. 11, No. 4, P.P. Synthesis and Characterization of Nano Najwa Saber Majeed* * Department of Chemical Engineering ** Department of Student Affairs and Authentication (Received 2 Abstract Nano-crystalline ZSM-5 zeolite was synthesized by hydrothermal method using chelating agent and two gel compositions:Compositionɪ:Al2O3:86SiO 10Na2O:2.6Trien:2626H2O.Study of hydrothermal reaction factors on characteristics of nano carried on ,among them are crystallization temperature, crystallization time and concentrati solution. Synthesis was accomplished in PTFE lined autoclave ( reactor ) . The product were characterized by X diffraction ( XRD ),Atomic force microscopy ( AFM ),scanning electron microscopy, Fourier transform infrared ( FTIR ) and Brunauer-Emmet-Teller (N2 absorption synthesized zeolite increase with increasing crystallization time and temperature. AFM results indicate that a nano level of about 50nm was reached for "particle average diameter". "1080,800,550,450 cm-1" have been clearly obtained, (TPAOH) solution concentration on crystallinity and Keywords: Crystallization , Template, Synthesis, 1. Introduction ZSM-5 is a member of MFI- with high Si/Al ratio from 10-100+.It is a zeolite with three dimensional channels, and it has two kinds of channels, straight channels with pore opening of 0.54nm x 0.56nm and sinusoidal channels with a pore opening of 0.51nm x 0.55nm[1]. ZSM-5 has been given a great attention by researchers because of its splendi specifications concerning thermal stability, high surface area, strong acidity, and presence of Nano-spaces ,The sizes of intra-crystalline pores and nano- spaces are nearly the same as molecular diameter of light hydrocarbons [2]. Strong acid sites exist on the nanoporous surfaces enable the zeolite to be used as shape selective "catalyst" especially in petroleum and petrochemical industries, such as isomerization, fluid catalytic cracking and also in adsorption processes[2] . The crystal size of zeolite is much larger than the Khwarizmi Engineering Journal,Vol. 11, No. 4, P.P. 8- 19 (2015) Synthesis and Characterization of Nano-crystalline ZSM Najwa Saber Majeed* Asir Abduljabbar Alnaama** mical Engineering/ College of engineering/ University of Baghdad ** Department of Student Affairs and Authentication/ University of Bagdad Email: dr.najwa_saber@yahoo.com Email: a.alnaama53@gmail.com (Received 23 March 2015 ; accepted 7 May 2015) 5 zeolite was synthesized by hydrothermal method using chelating agent and two gel :86SiO2:5.5TPA:12.7Na2O:3.4Trien:3320H2O.Composition O.Study of hydrothermal reaction factors on characteristics of nano carried on ,among them are crystallization temperature, crystallization time and concentration of template ( TPAOH ) solution. Synthesis was accomplished in PTFE lined autoclave ( reactor ) . The product were characterized by X diffraction ( XRD ),Atomic force microscopy ( AFM ),scanning electron microscopy, Fourier transform infrared ( FTIR absorption-desorption isotherm).SEM and XRD results indicate that crystallinity of synthesized zeolite increase with increasing crystallization time and temperature. AFM results indicate that a nano was reached for "particle average diameter". FTIR results showed that the required peaks near have been clearly obtained, Furthermore the results showed strong effect of template (TPAOH) solution concentration on crystallinity and decreasing of particle size towards nano Crystallization , Template, Synthesis, Nanocrystalline, ZSM-5 zeolite. -zeolite family 100+.It is a zeolite e dimensional channels, and it has two kinds of channels, straight channels with pore opening of 0.54nm x 0.56nm and sinusoidal channels with a pore opening of 0.51nm x 5 has been given a great attention by researchers because of its splendid specifications concerning thermal stability, high surface area, strong acidity, and presence of crystalline pores spaces are nearly the same as molecular diameter of light hydrocarbons [2]. Strong acid ist on the nanoporous surfaces enable the zeolite to be used as shape selective "catalyst" especially in petroleum and petrochemical industries, such as isomerization, fluid catalytic cracking and also in adsorption processes[2] . The ite is much larger than the micropore size ,and this will result in a low diffusion rate of reacting hydrocarbon molecules leading to low mass transfer, and consequently lower reaction rate, low selectivity of intermediates and coke formation followed b short catalyst life time. proposed solutions have been implemented, the first one was the formation of meso crystal structure of the zeolite, the second solution was to prepare nano-sized crystalline zeolite, so that the diffusion path for reacting molecules will be decreased as crystal size decrease these two factors are effective in improving catalytic activity[2]. Different methods and procedures have been utilized to synthesize ZSM hydrothermal crystallization of reactive alumina silicate gels[1,3,4,5,6,10,11,17]. the product properties are highly affected by many factors such as alumina and silica sources[4,11],Si/Al Al-Khwarizmi Engineering Journal (2015) crystalline ZSM-5 Zeolite Asir Abduljabbar Alnaama** University of Baghdad University of Bagdad 5 zeolite was synthesized by hydrothermal method using chelating agent and two gel O.Compositionɪɪ:Al2O3:68SiO2:5.4TPA: O.Study of hydrothermal reaction factors on characteristics of nano- sized zsm-5 has been on of template ( TPAOH ) solution. Synthesis was accomplished in PTFE lined autoclave ( reactor ) . The product were characterized by X-ray diffraction ( XRD ),Atomic force microscopy ( AFM ),scanning electron microscopy, Fourier transform infrared ( FTIR desorption isotherm).SEM and XRD results indicate that crystallinity of synthesized zeolite increase with increasing crystallization time and temperature. AFM results indicate that a nano-sized FTIR results showed that the required peaks near Furthermore the results showed strong effect of template decreasing of particle size towards nano-size level. micropore size ,and this will result in a low diffusion rate of reacting hydrocarbon molecules leading to low mass transfer, and consequently lower reaction rate, low selectivity of intermediates and coke formation followed by a A methodology of two proposed solutions have been implemented, the first one was the formation of meso-pores in the crystal structure of the zeolite, the second solution sized crystalline zeolite, so the diffusion path for reacting molecules will be decreased as crystal size decrease these two factors are effective in improving catalytic Different methods and procedures have been utilized to synthesize ZSM-5 which involve a rystallization of reactive alumina silicate gels[1,3,4,5,6,10,11,17]. the product properties are highly affected by many factors such as alumina and silica sources[4,11],Si/Al Najwa Saber Majeed Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) 9 ratio [4,5,11,14],template [1], crystallization time [1,7] and crystallization temperature [1,4,7,8,9]. R. karimi et al[1].used hydrothermal synthesis by stainless steel autoclave lined with PTFE , they investigated the effect of crystallization temperature and time also studies the effect of the type of organic structure directing agent (OSDA) on the synthesized zeolite , a Nano level sized of ZSM-5 has been produced with high crystallinity at temperature range of 170-180 and 120h for crystallization time, .They found that the template (OSDA) content has a great effect on ZSM-5 properties , a ratio of 0.058 for TPAOH/Si was optimum. M.Abrishamkar et al [3] followed a clear solution method under atmospheric pressure using TPAOH as template, aluminum isopropoxide as alumina source , TEOS as silica source with NaOH and H2O as mineralizer and solvent respectively , they reported a new path for producing nano-crystalline ZSM-5 Zeolite. R. Mohamed et al [4] studies the effect of the silica source on the crystallinity of Nano sized ZSM-5 Zeolite ,they concluded that crystallinity of ZSM-5 produced is increased in the following order colloidal silica < TEOS < fumed silica. R. Mohammed et al[7] studies the influence of the crystallization time on the synthesis of Nano sized ZSM-5 , they found that a time of crystallization of 45h gave the highest crystallization with 55.6 nm for average particle size and the BET surface of 360 m2/g , using 20wt% TPAOH as template (OSDA). In this research work tetrapropyl ammonium hydroxide (TPAOH) was used as template .A detailed parameter study to get the desired properties in the final zeolite product has been accomplished including crystallization time ,temperature ,gel composition ,template solution concentration and chelating agent. 2. Experimental 2.1. Technical Procedure Tetraethylorthosilicate (TEOS-Sigma Aldrich ) was used as silica source, aluminum is opropoxide (AIP-Sigma Aldrich) as alumina source, tetrapropyl ammonium hydroxide (TPAOH) as template, sodium hydroxide as alkaline agent, triethylenetetramine as chelating agent, and deionized water as solvent. Nano-sized ZSM-5 zeolite was synthesized using twin stainless steel autoclaves lined with polytetraflouroethylene (PTFE), and by hydrothermal reaction of silica source with alumina source in presence of TPAOH as template and Trien as chelating agent .Two compositions was studied and chosen, the first one with silica to alumina ratio Si/Al is 86, and the second is with Si/Al=68.The preparation procedure was kept the same, the differences are in the amount of alumina source(AIP) and Template (TPAOH). Composition ɪ : Al2O3:86SiO2:5.5TPA:12.7Na2O:3.4Trien:3320H2 O. Composition ɪɪ: Al2O3:68SiO2:5.4TPA:10Na2O:2.6Trien:2600H2O 2.2. Preparation Composition I The template TPAOH (2.2g) and TEOS (36g) were mixed with (40ml) deionised water for 1h of stirring. Trien (1ml) was added , NaOH (2.05g) was dissolved in 40ml deionised water and added also to make solution 1. Aluminum is opropoxide (AIP) 0.82g was added to 40ml deionised water and stirred for 1h to make solution 2. The resulting mixture(solution 2 ) was added dropwise to (solution 1) with vigorous stirring (500rpm) in mechanical stirrer for 120min. The resulting gel was poured into a stainless steel autoclave lined with PTFE(polytetraflouroethylene), the volume of PTFE insert is 200 ml and were filled to about 65% of its inside volume .A stir bar was placed inside the PTFE insert for stirring purpose. The sealed autoclave was equipped with electric heating jacket providing 500w and thermocouple t-type, also pressure indicator for measuring the autogeneous pressure. An electronic board with (PID) to control the temperature inside the autoclave during the hydrothermal reaction ,twin autoclaves were used as shown in Fig.1. 2.3. Preparation of Composition II The same procedure except that the amount of "template" TPAOH used was (2.9g) and the amount of alumina source (AIP) was (1.025g) .For both compositions and after collapsing the desired time at specific temperature ,the autoclave was left to cool overnight and the solid product was filtered, washed with distilled water many times and finally with ethanol, then the product left to dry at 110 ̊C overnight. Then the material was calcined at 550 ̊C for 5h with temperature ramp 1 ̊C/min. The hydrogel compositions and crystallization conditions ( time& temperature ) of hydrothermal synthesis for various samples are tabulated2in2Table2. Najwa Saber Majeed Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) 10 Fig. 1. Twin autoclaves lined with PTFE. Najwa Saber Majeed Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) 11 Table .1 Sample Conditions. Table.2, Parameters of samples. Si/AL Wt% TPAOH Composition crystallization temp.0C crystallization time ,h Sample 86 10 ɪ 140 24 S1 86 10 ɪ 150 72 S2 86 10 ɪ 160 72 S3 86 20 ɪ 160 72 S4 86 40 ɪ 160 72 S5 86 40 ɪ 160 96 S6 86 40 ɪ 170 96 S7 86 40 ɪ 175 80 S8 68 40 ɪɪ 150 48 S9 68 40 ɪɪ 150 72 S10 68 40 ɪɪ 150 96 S11 68 40 ɪɪ 160 48 S12 68 40 ɪɪ 160 72 S13 68 40 ɪɪ 160 96 S14 68 40 ɪɪ 170 48 S15 68 40 ɪɪ 170 72 S16 68 40 ɪɪ 170 96 S17 68 40 ɪɪ 180 48 S18 68 40 ɪɪ 180 72 S19 68 40 ɪɪ 180 96 S20 Crystallinity% Pore volume cm³/g s.surface m²/g Ave.particle.diam.,nm Sample 78 0.111 155.9 84.7 S1 98.4 0.1477 229.8 76.3 S2 110 0.15181 259.7 80.2 S3 88.4 0.2007 347 73.6 S4 104.7 0.20721 355.1 79.2 S5 90.3 0.2022 345.88 74 S6 82.8 0.225 380.9 79.4 S7 95.5 0.192 334.13 74.4 S8 77 0.2016 334.5 84.43 S9 99.5 0.1878 336.4 71.98 S10 88.8 0.18405 335.86 90.8 S11 84.4 0.2117 360.4 85.08 S12 92.9 0.1959 351.9 91.2 S13 96 0.206 351.76 65.9 S14 114.4 0.2239 365.1 50.8 S15 100 0.1997 336.1 81.68 S16 98.8 0.18852 322.39 60.5 S17 102 0.1967 332.8 86.8 S18 107.4 0.1920 303.96 63.4 S19 95.2 0.18997 327.53 51.9 S20 Najwa Saber Majeed Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) 12 3. Characterization The XRD patterns of zsm-5 zeolite were determined using a D2 PHASER/ Bruker (Germany 2010) using CuKα radiation Nickel filter (λ=1.54A).Data were collected within the 2Ɵ range of 2 ̊ and 50 ̊ with a 0.02 ̊ 2Ɵ-step and 0.5s per step ( 30kv and 10mA )X-ray diffraction was implemented to check the required pattern of ZSM-5 and its crystallinity. Fourier Transform Infrared (FTIR) by Shimazdu-IRA AFFINITY- 1,using KBr wafer 1% wt zeolite and 99% KBr to check and record the peaks at specified wave lengths corresponding to ZSM-5 In the range of 400-4000 cm-1 wave number. The morphology of zsm-5 zeolite was studied by scanning electron microscopy using Te Scan,Vega ɪɪɪ LM,CZECH. The particle size and morphology on nano-level size were ,determined by atomic force microscopy using an AA3000/Angstrom Advance Inc, USA ,scanning probe microscope(SPM) gave granularity cumulation distribution and surface roughness. Table 2 shows parameters of samples, Average particle diameter measured by , in which the increase in crystallinity is only from 99.5% to 107.4%, in averaging the value of (AFM),specific.surface(BET), pore volume, and crystallinity (XRD) for both compositions.BET surface and pore volume for all samples were measured by surface area analyzer/Q surf series/Italy ,two samples S7 and S20 was repeated by micrometrics ASAP 2020/USA. BET surface is based on BET theory (Brunauer . Emmet and Teller) which described five basic adsorption isotherms . but IUPAC classification added one more adsorption isotherms .BET theory is an extension of the Langmuir theory (monolayer adsorption model) to the multi adsorption model. Adsorption can be defined as the adhesion of atoms or molecules of gas to a surface , the amount of gas adsorption depends on surface area. gas pressure, temperature and strength of interaction between the gas and solids . Nitrogen is usually used in BET surface analysis because of its purity , strong interaction with most solids and availability BET equation for determining surface area in its simplest form. 11111111111111111111 St=k(1-p/po)*Va Where St=total surface area of sample being analyzed K=A constant for nitrogen , assuming STP condition=4.03 p/po=0.294 for gas mixture of 30% N2/70% He Va=volume of gas (N2) adsorbed Each cubic centimeter of N2 adsorbed (then desorbed) by the sample is equivalent to total surface area (St) of 2.84 m2 , the specific surface is found by dividing St by the weight of the sample in the cell in grams The complex form of BET equation. 1111111111111111111111111111 ��(����) = � � + �� � � � ��� [11,19] P=pressure , Kpa Po=saturation pressure , KPa V=total volume of gas adsorbed , cm3 Vm=volume of gas absorbed in monolayer , cm3 C=constant and related to the heart of adsorption ���� ������ = ���� �� � !" [11] V=volume of adsorbed gas Mg=molecular Wight ρg= gas density For BET surface area analysis a mixture of nitrogen balance helium is passed through the reference channel of the thermal conductivity detector(TCD)to the sample housed within a flow- through glass cell and finally into the TCD analytical channel the signal produced by the TCD detector is collected by the microprocessor control board. The procedure starts with the degassing of the sample with the carrier gas at the programmable temperature when the sample is dried , the operator simply transfer the sample holders to the analytical ports and fit them into place. Pressing the start button will automatically raise the liquid nitrogen flask carriage initiating the analysis... Fig. 2. BET surface area analyzer. Najwa Saber Majeed Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) 13 Fig. 3. ASPA 2020 Accelerated surface area and porosimetry system ASTMD3663, ASTMD4222, ASTMD4365, ASTMD4641. 4. Results and Discussion 4.1. Crystallization Temperature The most important factor in the synthesis of zeolite is crystallization temperature, so a set of samples were prepared for both compositions I & II ranging from 140 ̊C-180 ̊C as shown in Table 2, the results show a strong dependency of crystallinity on temperature and these results coincide with previous work[1,4,11]. Comparing sample S9(150 ̊C,48h) with S18(180C̊,48h) it can be noticed that the crystallinity increased from 77% to 102% , this increase of crystallinity would be less as time of crystallization increase to 72 when comparing sample S10(150 ̊C-72h) and S19(180C̊,72h). The average crystallinity with temperature (see Table 3), showed an increase in the average value of crystallinity from 88.4% at 150 ̊C to 91% at 160 ̊C and 104.4% at 170C̊, keeping almost the same level at 180C̊ , indicating that the crystallinity, reached its optimum value around 170-180C , Figs.3 and 4 are XRD patterns and SEM micrographs of ZSM5 products the effect of temperature on average particle diameter and the nano-level size was observed and a tendency to have a decrease in average particle diameter as temperature is increased, and particle diameter decreased from about 82nm at 150 ̊C to 67nm at 180C̊ (see Table 3), these results of nano- level size are associated with a high crystallinity degree, support the hypothesis and results revealed recently by Lupulescu and Rimer[19], which suggested a non-classical pathway of zeolite crystallization by the presence and gradual consumption of nano-particles, while most crystals grow through classical means (the addition of atoms or molecules to the crystal). SEM images show that samples which were prepared at temperature 150 ̊C has amorphous phase which coincide with average results of XRD patterns and crystallinity (88%), and crystallized in spherical form,but for samples prepared at 170 and 180 ̊C crystallized mostly in orthorhombic shape crystals. 4.2. Crystallization Time To study the effect of this important factor, a series of samples was prepared using gel composition ɪ, and composition ɪɪ . XRD patterns (Figs.3) at different temperatures (150,160,170,180 ̊C) , show that zsm-5 phase is the only one obtained in all experiments and the peak at 2Ɵ=7-9 and 2Ɵ=22.5-24.5 are typical for ZSM-5[13]. The crystallinity of samples show a tendency to increase due to increase in crystal nucleation and growth rate , as the time increase in temperatures range of 150 & 160 C but for temperature 170 and 180 C the crystallinity increased up to 72h. Comparing SEM images of S19 (72h,180 C) with S20 (96h,180 C) show that the increased crystallization time cause to have a lower crystallinity and beginning of losing the orthorhombic shape crystals to spherical. but a little decline observed in crystallinity when time increased above 72h, the crystallinity begins to decrease slightly , this behavior can be explained by the cause of a reverse process of recrystallization occurs leads to this declination , and it seems that the template(TPAOH) begins to lose its performance at higher temperature when the time of crystallization increased above 72h, the reports of AFM showed that the nano-sized level of crystalline ZSM-5 are influenced by temperature and time and as shown in Tables 2 and 3 and Fig.2 . the spectra of (FTIR) for synthesized samples at various crystallization times and temperature are showed in Fig.5 the findings show that the bands near1085CM- 1(internalasymmetricstretch), 799CM-1(external symmetric stretch),546 CM-1(double ring vibration) and 452 CM-1(T-O band) and the formation of ZSM-5 phase only.The peak near 550CM-1 is attributed to the five- membered ring of the ZSM-5 zeolite structure (pentasil)[17]. The evidence for getting nano-sized level of ZSM-5 Najwa Saber Majeed was the peak near 1225CM-1 and it is an asymmetric stretch vibration of the "T which is attributed to external linkages between tetrahedral TO4 [18]. In spite of the decrease in Si/AL ratio in gel compositions II comparing with gel compositions I , the effect of increasing the amount of TPAOH ie TPA/Si ratio gave better results concerning nano-sized l 4.3. Template Solution Concentration The concentration by weight of template (organic structure directing agent OSDA,TPAOH)solution was studied by using three kind of solutions 10%wt , 20%wt and 40%wt , using gel composition I, the samples S3 , S4 , S5 represent 10%wt , 20%wt and 40%wt(TPAOH) respectively. Fig. 4. Atomic force microscopy reports for samp Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 14 1 and it is an asymmetric stretch vibration of the "T-O" bond to external linkages between tetrahedral TO4 [18]. In spite of the decrease in Si/AL ratio in gel compositions II comparing with gel compositions I , the effect of increasing the amount of TPAOH ie TPA/Si ratio gave sized level. Template Solution Concentration The concentration by weight of template (organic structure directing agent- OSDA,TPAOH)solution was studied by using three kind of solutions 10%wt , 20%wt and 40%wt , using gel composition I, the samples S3 , , S5 represent 10%wt , 20%wt and These samples were prepared at the same temperature 160̊C and same crystallization time 72h .the results show that the best result in surface area and pore volume for S5 (355 m2/g and 0.20721 cm3/g respectively 40%wt(TPAOH) was used with very good crystallinity. 4.4. Gel Compositions Two gel compositions were studied I and II which they are different in Si/AL ratio and more template (TPAOH) introduced in the gel compositions II so TPA/Si ratio is more in gel compositions II . the results reveals ( as shown in the Table 2 ) that a decrease in particle diameter down to 50 nm (S15 and S20) are given by compositions II. Atomic force microscopy reports for samples of composition Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) These samples were prepared at the same C and same crystallization time 72h .the results show that the best result in surface area and pore volume for S5 (355 m2/g and /g respectively ) in which 40%wt(TPAOH) was used with very good Two gel compositions were studied I and II which they are different in Si/AL ratio and more template (TPAOH) introduced in the gel A/Si ratio is more in gel compositions II . the results reveals ( as shown in the Table 2 ) that a decrease in particle diameter down to 50 nm (S15 and S20) are given by les of composition ɪ &ɪɪ. Najwa Saber Majeed Table 3, Average parameter value at different crystallization time and temperatures Fig. 5. XRD patterns at different crystallization temperatures (150,160,170 and 180 C) for different crystallization times (48,72,and 96h). Average crystallinity% Sample code 88.4 S9,S10,S11 (48,72,96h) And 150 0C 91.1 S12,S13,S14 (48,72,96h) And 160 0C 104.4 S15,S16,S17 (48,72,96h) And 170 0C 101.4 S18,S19,S20 (48,72,96h) And 180 0C Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 15 Average parameter value at different crystallization time and temperatures. For 48h For 72h For 96h XRD patterns at different crystallization temperatures (150,160,170 and 180 C) for different Average BET surface area m2/g Average particle diameter ,nm crystallinity% 338.5 82.4 354.7 80.7 341.2 69.3 321.4 67.3 Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) XRD patterns at different crystallization temperatures (150,160,170 and 180 C) for different Average pore volume Cm3/g Average BET surface 0.19115 0.2045 0.20404 0.1929 Najwa Saber Majeed Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) 16 Group 1 for 72h and different temperature 180,170,160,150 C. Group 2 for 96h and different temperature 180,170,160,150 C. Fig. 6. Scanning electron microstructure images. Fig. 7. FTIR spectra for the samples prepared at variuos crystallization time (96h,72h,48h) and temperatures of (180,170,160 and150 C). Najwa Saber Majeed Al-Khwarizmi Engineering Journal, Vol. 11, No. 4, P.P. 8- 19(2015) 17 5. Conclusion Nano- Crystalline ZSM-5 was synthesized with considerably matched specifications with theory and previous works. A hydrothermal method was adopted using twin autoclaves carefully designed to meet the requirements( heating, stirring, sealing). The effect of temperature and time of the crystallization also the concentration of template solution on final product specifications like morphology and crystallization were studied. The result showed that the crystallization time, which is the most important parameter, and has a great effect on crystallinity and particle size, crystallization time between 72h-96h gave the best results. Crystallization temperature had also a strong effect on crystallinty, purity and morphology of the prepared ZSM-5 zeolite .it has noticed that an increase in temperature range between (170 C-180 C),tends to get an increase in crystallinity, which is coincided with previous work[1].Template(OSDA)solution concentration showed that the increase of weight percent of the solution from 10% to 20% to 40% has its strong effect on both increase of crystallinity and decrease of particle size to nano-level size. 11111 Acknowledgements The authors express their grateful appreciation to the Ministry of oil-Petroleum R&D center for conducting BET surface area, the Ministry of Science and Technology for SEM, College of Science for XRD , AFM and FTIR. 6. References [1] R. 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