Iraqi Journal of Chemical and Petroleum Engineering 

 Vol.18 No.2 (June 2017) 1 - 11 

ISSN: 1997-4884 

 
 
 
 
 

The Effect of Crystallization Time and Acid Type on the Synthesis of 

Nano-Gamma Alumina Using Double Hydrothermal Method 

 
Abdul-Halim A.K. Mohammed

1
,
 
Hussein Q. Hussein

2
 and Mohammed Sabah 

Mohammed
3 

1. Gas and Petroleum Engineering Department, College of Al-Faraby University  

2. Chemical Engineering Department, College of Engineering, University of Baghdad  

3. Office of Assit. Dean for Scientific and Student Affairs, College of Engineering, Al-

Nahrain University 

 

Abstract 

Double hydrothermal method was used to prepare nano gamma alumina   using 

aluminum nitrate nano hydrate and sodium aluminate as an aluminum source, CTAB 

(cetyltrimethylammonium bromide) as surfactant, and variable acids: weak acids like; 

citric, and acitic acids, and strong acids like; hydrochloric and nitric acids as a bridge 

between aluminum salts and surfactant. Different crystallization times  12, 24, 48, and 

72 hrs were applied. All the batches were prepared at pH equals to 9. XRD diffraction 

technique was used to investigate the crystalline nano gamma alumina pure from 

surfactant. N2 adsorption-desorption (BET) was used to measure the surface area and 

pore volume of the prepared nano alumina, the average particle size and the 

morphology of the surface of nano gamma alumina were estimated using AFM and 

SEM techniques, respectively. The sharpness of the peaks increased with increasing 

of crystallization time. The surface area, pore volume, and average particle size were 

decreased with increasing crystallization time. The best result of surface area was 383 

m
2
/gm obtained using citric acid at 12 hr crystallization time, while the best results of 

pore volume and average particle size were 0.54cm
3
/gm and 72.37nm obtained using 

hydrochloric acid at12 hr crystallization time. Low agglomeration with hexagonal 

structure obtained using weak acids, while agglomeration occurred and clusters 

formed using strong acids. 

 

Key words: Gamma alumina, nanoparticle, double hydrothermal, CTAB, 

crystallization time and acid type. 

 

Introduction  

The nano structured alumina material is 

a porous crystalline system having a 

nano particle size range 1-100 nm used 

in form of particles. Aluminum oxide 

exists in various structures; only two 

phases are of interest, namely the 

nonporous crystallographically ordered 

alpha-Al2O3 which was composed to 

spherical shape, and the porous 

amorphous gamma-Al2O3 which was 

composed to spherical or non-spherical 

or irregular hexagonal shape. Gamma-

Al2O3 is used as a catalyst by itself, and 

University of Baghdad 
College of Engineering 

Iraqi Journal of Chemical and 
Petroleum Engineering 

 



The Effect of Crystallization Time and Acid Type on the Synthesis of Nano-Gamma Alumina Using 

Double Hydrothermal Method 

  

  

2                                  IJCPE Vol.18 No.2 (June 2017)                -Available online at: www.iasj.net 
 

also used as adsorbent because of its 

porous structure [1, 2]. 

Gamma alumina is used as a 

support alone, or as a support of active 

metals in catalysis reactions due to its 

high thermal stability and the ability to 

be shaped into mechanically stable 

extrudes and pellets, also alumina is a 

poly anion of positive charge at pH 

values below 7 and negative at higher 

values, offering many possibilities to 

bind many ionic catalyst precursors [3]. 

Supported nano alumina with 

high surface area and pore volume is 

used extensively as catalyst, catalytic 

supports, and adsorbent for chemical 

processes. The surface of the nano 

particles plays an important role in 

their catalytic properties [4, 5 and 6]. 

The starting materials of 

synthesis nano gamma alumina are 

either expensiveand sensitive to 

moisture content like aluminium 

alkoxides or cheap and available 

materials like aluminium salts, clays, 

and pure aluminium powder [6]. 

different materials like; surfactant, 

dispercents and tamplets were used in 

the synthesis  of nano gamma alumina 

with high texture properties using 

different methods like; sol gel, 

hydrothermal treatment, precipitation, 

lazer oblation, solution composition, 

spray pyrolysis…etc [7, 8, 9 and 10]
 
.
 

Aguado et al. 2005 [11] used sol-gel 

techniques to prepare nano gamma 

alumina using two types of surfactant 

and aluminum alkoxides source of 

aluminum, and hydrochloric acid. 

Uniform structure of produced catalyst 

was achieved with increasing acid/Al 

source (wt/wt) ratio, while decreasing 

the amounts of surfactant used causes 

decreasing in pore size of the prepared 

catalyst. Yi Jian Hong 2009 [12] used 

precipitation technique to prepare nano 

gamma alumina using sodium 

aluminate and oxalic acid as a 

precipitation agent. The effect of the 

pH of sodium aluminate and oxalic 

mixtures and the pH of washing at pH 

range 7-9 on the purity of the catalyst 

was studied, and found that Pure 

crystalline gamma alumina was 

obtained using pH <8, while beta 

alumina was obtained at pH >8. Ming 

Bao et.al.2010 [13] prepared nano 

gamma alumina in the presence of two 

sources of alumina, 

Cetyltrimethylammonium bromide 

(CTAB) as surfactant, citria acid, and 

different molar ratios of sodium citrate 

by double hydrothermal treatment  

using auto clave with temperature 170 
0
C for 24 hrs,the optimum results 

acting in 0.2 molar ratio of sodium 

citrate with respect to aluminium salts 

with surface area 398 m
2
/gm, and pore 

volume 0.59 m
2
/gm [12]. Dahlan et.al. 

2012 [14] prepared nano alumina 

adding urea as a fuel with molar ratio 

29:153:1:2028 of aluminium 

salt,CTAB,urea,and water using 

hydrothermal method producing 203 

m
2
/gm, 0.14 cm

3
/gm of nano gamma 

alumina.
 

Faramawy et.al. 2014 [15] 

synthesis of nano gamma alumina by 

hydrothermal technique using 

microwave irradiation for the 

crystallization of aluminium salt and 

CTAB surfactant and found that the 

increasing in the time and power of the 

reaction leads to increase the 

crystinallity and the texture properties 

of the prepared catalyst
 
.Hawraa 2016 

[16] prepared nano gamma alumina 

with 56 nm, 256 m
2
/gm surface area, 

and 0.374 cm
3
/gm pore volume by sol 

gel method using aluminum chloride 

dissolved in ethanol and ammonia. 

The aim of this work is to prepare nano 

   alumina by using double 
hydrothermal treatment method, and  

to study the effect of crystallization 

time and acid type on the characterstics 

of prepared catalyst like; XRD, AFM, 

surface area, pore volume and SEM. 

 

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Abdul-Halim A.K. Mohammed, Hussein Q. Hussein and Mohammed Sabah Mohammed 

 

-Available online at: www.iasj.net                      IJCPE Vol.18 No.2 (June 2017)                        3 
 

Experimental Work 

 

Materials 

Aluminum nitrate nona hydrate 

(Al(No3)3.9H20, 100% purity, Himedia 

Company), and sodium aluminate 

(NaAlO2, 100 % purity, Himedia 

Company) were used as sources of  

aluminium. Cetyltrimethylammonium 

bromide (CTAB, 99%  purity, Wuhan 

kemi-Works, Chemical Co.Ltd) was 

used as a surfactant, different acids 

like; cirtic  acid (CA, 100% purity), 

acetic acid (AA, 100% purity), 

hydrochloric acid (HCL, 99% purity), 

and nitric acid( HNO3, 99% purity) 

acting from Riedel-De Haen were used 

as a structure direct agent, and finally 

sodium hydroxide (NaOH, 99% purity, 

Sigma) was used to adjust the ph of the 

mixtures. 

 

Preparation of Nano           
The nano gamma alumina was 

prepared depending on the previous 

work of Ming Bao et. al. 2010 [13] by 

dissolving aluminium nitrate 

nonahydrate, citric acid and CTAB 

surfactant in suitable amount of 

dionized water, then sodium aluminate 

was dissolved in suitable amount of 

dionized water and added drop by drop 

to the first mixture under vigorous 

stirring 1000 rpm. The molar 

composition of the mixture 

AL/CTAB/citric acid/H2O is 

1.0/0.1/0.2/125, a white gel formed 

immediately, after further stirring for  

3 hrs, the mixtures adjusted at pH 

equal to  9. The produced gel was then 

placed in a Teflon-Lined stainless steel 

auto clave to start the crystallization at 

180 
0
C crystallization temperatures   

for crystallization time of 12, 24, 48, 

and 72 hrs.  The crystallization product 

was filtered using nano filter papers 

(slow), and washed by deionized water 

and ethanol for several times to 

eliminate the contaminants. The 

product was dried at temperature 100
 

0
C for 24 hrs, and then calcined at 600 

0
C. The procedure above was repeated 

using acetic acid, hydrochloric acid, 

and nitric acid instead of citric acid. 

    

Characterization of Nano             
X-ray diffraction analysis was used to 

characteristic the phase of the prepared 

samples using X-Ray Diffract meter 

type Shimadzu SRD 6000, Japan, with 

Cu wave length radiation (1.54060) in 

the 2 theta range from 10-80 
0
, and 

fixed power source (40 Kv, 30 mA) by   

the Ministry of Science and 

Technology. The surface area, and 

pore volume of the samples were 

conducted at the   Petroleum Research 

and Development Center in Baghdad 

using Brunauer Emmett and Teller 

(BET) method with Thermo 

analyzer/USA device. The average 

particle size and the morphology of 

surface of each sample were calculated 

at the Department of Chemistry / 

College of Science /University of 

Baghdad using Atomic Force 

Microscope device (type Angstrom, 

Scanning Probe Microscope, 

Advanced Inc, AA 3000, USA). The 

morphology of the structure of nano 

gamma alumina was studied using FEI 

NOVA NANO SEM device   located at 

Chemical Engineering department / 

Tehran University. The specimen of 

prepared nano gamma alumina was 

dispersed in ethanol and coated by 

gold using special cell. 

 

Results and Discussions 

 

X-Ray Diffraction (XRD) 
From the Figures 1 to 7 it is clear that 

all the coordinates of the peaks of 

prepared samples were accepted the 

three strong standard peaks of gamma 

alumina (311-65b intensity-2.39 d 

spacing), (400-80b intensity-1.98 d 

spacing), and (410-100 b intensity-1.4 

d spacing) which represents the pure 

substantial crystallization of 

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The Effect of Crystallization Time and Acid Type on the Synthesis of Nano-Gamma Alumina Using 

Double Hydrothermal Method 

  

  

4                                  IJCPE Vol.18 No.2 (June 2017)                -Available online at: www.iasj.net 
 

international alumina card (JCPDS) 

files no. (29.0063). All the XRD-

diffraction Figures from 1 to 7 

represented high crystalline gamma 

alumina at pH equal to 9. The broading 

of the peaks may be occurred due to 

the role of the CTAB surfactant used in 

the process which was released after 

calcination producing nano particle 

size [17, 11]. The increasing in 

crystallization time from 12 to 72 hrs 

causes little increasing in crystinallity 

and increasing in the sharpness of the 

peaks shown in Figures 1 to 4  as 

observed by Marzieh Jalilpour, 2012 

[18]. The effect of varying the acid 

type on the XRD diffraction is shown 

in the Figures 1, 5, 6 and 7. The 

broading in the peaks occurred from 

using hydrochloric and nitric acids are 

larger than that occurred from using 

weak acids like; citric and acetic acids 

with the same degree of crystinallity 

because these experiments were 

attempted at the same conditions. 

 

 
Fig. 1: XRD diffraction of the nano gamma alumina prepared using citric acid at 180 

0
C crystallization 

temperature, 12 hrs crystallization time and  calcination temperature 600 
0
C 

 

 

 
Fig. 2: XRD diffraction of the nano gamma alumina prepared using citric acid at 180 

0
C crystallization 

temperature, 24 hrs crystallization time and calcination temperature 600 
0
C 

 

 

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Abdul-Halim A.K. Mohammed, Hussein Q. Hussein and Mohammed Sabah Mohammed 

 

-Available online at: www.iasj.net                      IJCPE Vol.18 No.2 (June 2017)                        5 
 

Fig. 3: XRD diffraction of the nano gamma alumina prepared using citric acid at 180 
0
C crystallization 

temperature, 48 hrs crystallization time and calcination temperature 600 
0
C 

 

 
Fig. 4: XRD diffraction of the nano gamma alumina prepared using citric acid at 180 

0
C crystallization 

temperature, 72 hrs crystallization time and calcination temperature 600 
0
C 

 

 
Fig. 5: XRD diffraction of the nano gamma alumina prepared using acetic acid at 180

 0
C crystallization 

temperature, 12 hrs crystallization time and calcination temperature 600 
0
C 

 

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The Effect of Crystallization Time and Acid Type on the Synthesis of Nano-Gamma Alumina Using 

Double Hydrothermal Method 

  

  

6                                  IJCPE Vol.18 No.2 (June 2017)                -Available online at: www.iasj.net 
 

 
Fig. 6: XRD diffraction of the nano gamma alumina prepared using hydrochloric acid at 180 

0
C 

crystallization temperature, 12 hrs crystallization time and calcination temperature 600 
0
C 

 

 
Fig. 7: XRD diffraction of the nano gamma alumina prepared using nitric acid at 180

 0
C crystallization 

temperature, 12 hrs crystallization time and calcination temperature 600 
0
C 

 

Surface Area and Pore Volume 

The surface area and pore volume of 

the nano catalyst play a very important 

role for the activity of the nano 

catalyst, because high surface area 

leads to high active sites causes 

increasing in activity. Table 1 shows 

the results of surface area and pore 

volume of the samples for different 

conditions. 

Keeping the mixtures at 180 
0
C 

crystallization temperature during 24 

hrs may allow the particles to become 

close to each other causes decreasing 

in surface area besides the reduction in 

pore volume. The increasing in 

crystallization time from 48 to72 hrs 

did not effect on the results of surface 

area and pore volume because the 

stable structure of boehmite occurred 

causes no change in these values as 

mentioned by Yvan J.et al. 2012. The 

addition of acids beside the surfactant 

to the starting materials had very 

important role, because it represents 

the bridge between the surfactant and 

the source of aluminum ions, besides 

its role as a dispersant agent as 

mentioned by Ki Wom Jun et al. 2009. 

The dispersant degree varies from acid 

to another one in the order of 

hydrochloric acid <nitric acid <acetic 

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-Available online at: www.iasj.net                      IJCPE Vol.18 No.2 (June 2017)                        7 
 

acid   < citric acid prevent the 

agglomeration of the particles causes 

low surface area with high pore 

volume. 

 
Table 1: the values of surface area and pore volume at different conditions 

Synthesis conditions Acid type 
Surface 

area,m
2
/gm  

Pore 

volume,cm
3
/gm  

180
0
C,12hrs,and 600

0
C 

Citric acid 

383.0  0.430 

180
0
C,24hrs,and 600

0
C 338.8 0.430 

180
0
C,48hrs,and 600

0
C 339.0  0.430 

180
0
C,72hrs,and 600

0
C 338.8 0.365 

180
0
C,12hrs,and 600

0
C Acetic acid 203.0 0.500 

180
0
C,12hrs,and 600

0
C Hydrochloric acid 183.4 0.540 

180
0
C,12hrs,and 600

0
C Nitric acid 183.1  0.500 

 

Particle Size 
The atomic force microscopy (AFM) 

method was used to find the average 

particle size, particle size distribution, 

and the results of the particle size are 

listed in Table 2. 

The average particle size of the 

prepared nano alumina was in the nano 

scale catalyst for all crystallization 

temperatures. Increasing the 

crystallization time at 180
 0

C causes 

drop in surface area and pore volume 

of the prepared samples, and the 

particles became bigger due to 

agglomeration reaching to the levels 

out of the nano scale level at 

crystallization time higher than 24 hrs 

as observed by Y van.et al.2012 [19]. 

Using variable acids in the presence of 

the surfactant produced different 

ranges of average nano gamma 

alumina. hydrochloric and nitric acids 

produced nano gamma alumina with 

average particle size less than 75 

nm,while weak acids like; aceti and 

citric acids produced nano gamma 

alumina with average particle size 

above 95 nm.These results are near the 

results obtained by Hawraa 2016 [16]. 

 

Table 2: the values of particle size distribution and average particle size at different conditions  

Synthesis conditions Acid type 
particle size 

distribution,nm  

 average particle 

size,nm  

180
0
C,12hrs,and 600

0
C 

citric acid 

75-160 92.72 

180
0
C,24hrs,and 600

0
C 50-140 103.17 

180
0
C,48hrs,and 600

0
C 40-160 106.59 

180
0
C,72hrs,and 600

0
C 70-150 110.37 

180
0
C,12hrs,and 600

0
C acetic acid 70-130 96.44 

180
0
C,12hrs,and 600

0
C hydrochloric acid 35-100 72.37 

180
0
C,12hrs,and 600

0
C nitric acid 55-130 74.82 

 

Scanning Electron Microscopy 

(SEM) 

The morphology of the surface of 

prepared nano gamma alumina 

samples is obtained at magnification of 

60 kx and zoom of 500 nm. Increasing 

crystallization time shown in Figures  

8 to 11. Using crystallization time 

above 12 hrs causes agglomeration in 

particles, and reduces nano particles   

lead to drop in surface area and pore 

volume as observed by Y van. et al. 

2012 [19]. Uniform hexagonal shape 

of particles with low agglomeration is 

observed by using weak acids like; 

citric and acetic acids shown in Figures 

8 and 12. Agglomeration and 

formation of clusters is observed by 

using strong hydrochloric and nitric 

acids shown in Figures 13 and 14 leads 

to low surface area with high pore 

volume. This morphology is the same 

with the morphology acting by hawraa 

2016 [16]. 

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The Effect of Crystallization Time and Acid Type on the Synthesis of Nano-Gamma Alumina Using 

Double Hydrothermal Method 

  

  

8                                  IJCPE Vol.18 No.2 (June 2017)                -Available online at: www.iasj.net 
 

 
Fig. 8: SEM image of the nano gamma alumina prepared using citric acid at 180 

0
C crystallization 

temperature, 12 hrs crystallization time and  calcination temperature 600 
0
C 

 

 
Fig. 9: SEM image of the nano gamma alumina prepared using citric acid at 180 

0
C crystallization 

temperature, 24 hrs crystallization time and calcination temperature 600 
0
C 

 

 
Fig. 10: SEM image of the nano gamma alumina prepared using citric acid at 180 

0
C crystallization 

temperature, 48 hrs crystallization time and  calcination temperature 600 
0
C 

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Abdul-Halim A.K. Mohammed, Hussein Q. Hussein and Mohammed Sabah Mohammed 

 

-Available online at: www.iasj.net                      IJCPE Vol.18 No.2 (June 2017)                        9 
 

 
Fig. 11: SEM image of the nano gamma alumina prepared using citric acid at 180 

0
C crystallization 

temperature,72 hrs crystallization time and calcination temperature 600
 0
C 

 

 
Fig. 12: SEM image of the nano gamma alumina prepared using acetic acid at 180 

0
C crystallization 

temperature, 12 hrs crystallization time and calcination temperature 600
 0
C 

 

 
Fig. 13: SEM image of the nano gamma alumina prepared using hydrochloric acid at 180 

0
C 

crystallization temperature, 12 hrs crystallization time and  calcination temperature 600 
0
C 

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The Effect of Crystallization Time and Acid Type on the Synthesis of Nano-Gamma Alumina Using 

Double Hydrothermal Method 

  

  

10                                  IJCPE Vol.18 No.2 (June 2017)                -Available online at: www.iasj.net 
 

 
Fig. 14: SEM image of the nano gamma alumina prepared using nitric acid at 180 

0
C crystallization 

temperature, 12 hrs crystallization time and  calcination temperature 600
 0
C 

 

Conclusions 

Nano gamma alumina was 

successfully synthesized using double 

hydrothermal method in the presence 

of CTAB surfactant using different 

crystallization times, and different 

structure direct agent. XRD 

diffractions represent the crystalline 

nano gamma alumina pure from 

surfactant. The sharpness of the peaks 

increased with increasing of 

crystallization time. Using strong acids 

causes broading in peaks larger than 

that occurred in peaks using weak 

acids. The surface area, pore volume, 

and average particle size were 

decreased with increasing 

crystallization time. The best result of 

surface area obtained using citric acid 

at 12 hr crystallization time, while the 

best results of pore volume and 

average particle size obtained using 

hydrochloric acid at 12 hr 

crystallization time. Low 

agglomeration with hexagonal 

structure obtained using weak acids, 

while agglomeration occurred and 

clusters formed using strong acids.  

 

 

 

 

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Abdul-Halim A.K. Mohammed, Hussein Q. Hussein and Mohammed Sabah Mohammed 

 

-Available online at: www.iasj.net                      IJCPE Vol.18 No.2 (June 2017)                        11 
 

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