Materials Express

2158-5849/2014/4/235/007
Copyright © 2014 by American Scientific Publishers
All rights reserved. doi:10.1166/mex.2014.1162
Printed in the United States of America www.aspbs.com/mex

Single step preparation of nano size gamma

alumina exhibiting enhanced fluoride adsorption
L. A. Avinash Chunduri, Tanu Mimani Rattan, Muralikrishna Molli, and Venkataramaniah Kamisetti∗
Department of Physics, Sri Sathya Sai Institute of Higher Learning, Prasanthinilayam 515134, India

ABSTRACT
A direct single step solution combustion synthesis is adopted to prepare nano -Al2 O3 using aluminium nitrate
as oxidizer and urea or hexamethylenetetramine (HMT) as fuel in the presence of a variety of surfactants.
The obtained products were characterized by powder XRD and IR. The phase and size of the product was
found to be depending on the nature of surfactant or fuel used. FESEM and TEM analysis of urea-surfactant

Article
based gamma alumina shows a fairly uniform spherical morphology of particle aggregates with lower nano size
distribution of 40–60 nm. In HMT based -Al2 O3On:
IP: 14.97.148.194 theThu, 15 Feb
particle size2024
was 15:26:11
greater than 200 nm. DLS analysis of
Copyright: American Scientific Publishers
the sample also showed the narrow size distribution in the urea-surfactant based -Al2 O3 compared to HMT
Delivered by Ingenta
based -Al2 O3 which shows broad size distribution. The nano gamma alumina powders also show specific
area of 160–240 m2 g−1 . The urea-CTAB synthesized -Al2 O3 was tested for its fluoride adsorption, exhibited
adsorption capacity of 6.49 mg · g−1 .

Keywords: Nano -Alumina, Solution Combustion Method, Single Step Synthesis, Strong Fluoride Adsorption.

1. INTRODUCTION well as a catalyst support in the automotive and petroleum

Alumina powders with controlled size distribution find industries.6 7 Wide experimental evidence indicates that
a wide variety of applications for advanced engineer- the preparation history has an important bearing on the
ing materials.1 2 Among all the metastable polymorphic type of -Al2 O3 structure that is produced for example,
forms of alumina that exist, the highly stable phase is gelatinous or highly crystalline. The preparation history
-alumina and the less stable form is -alumina.3 The can influence phase composition, bulk and surface chemi-
occurrence of the different phases depends on the prepar- cal composition, local microstructure of the oxide as well
ative procedures as well as defects or impurities present as its stability and textural properties.8 9
in the crystal lattice, which finally give a unique crys- The past few years have witnessed marked progress in
tal structure.4 The gamma (-Al2 O3 ) phase is important the synthesis of -Al2 O3 . This topic is quite attractive,
and nano--alumina powder is one of the new and most as revealed by the recent vast literature, which definitely
important fine ceramic materials. The usefulness of this demonstrates the sensitivity of the final product formed
nano oxide can be traced to a favorable combination of to the experimental conditions used during production.
its textural properties, such as specific surface area, pore -Al2 O3 is typically prepared by the popular wet chemical
volume, and pore size distribution and its acid/base charac- methods such as sol–gel and hydrothermal methods.10–13
teristics which are mainly related to surface chemical com- The main focus of all such methods of preparation is
position, local microstructure, and phase composition.5 to have control over the morphology of the material and
Gamma alumina has direct application as a catalyst as the size.14 15 These are achieved by adjusting experi-
mental parameters and adding cationic, anionic, and non-
∗
Author to whom correspondence should be addressed. ionic surfactants16–18 and also some structure directing
Email: [email protected] agents.19 The main drawback of these methods is removal

Mater. Express, Vol. 4, No. 3, 2014 235

 Materials Express Single step preparation of nano size gamma alumina
Chunduri et al.

of surfactant after synthesis, as is the case in sol–gel and Citric acid-C6 H8 O7 , 99.5%, (Merck); sodium fluoride-NaF,
hydrothermal routes. 98%, (Fisher Scientific).
In the direct single step preparative route of solu- A stock solution of 1000 ppm of sodium fluoride was
tion combustion synthesis, polycrystalline aluminum oxide prepared using distilled water. Required concentrations of
synthesized with urea as the fuel predominately shows the samples were prepared by serial dilutions of the stock
the high temperature stabilized -phase. The formation of solution.
amorphous alumina phase occurs when fuel lean mixtures Alumina was synthesized by solution combustion syn-
of nitrate and urea undergo combustion, which has been thesis (SCS) route containing aluminium nitrate as oxi-
extensively reported.20 Alternately oxalyldihydrazide- dizer and urea/HMT as fuel in the presence of cationic and
C2 H6 N4 O2 (ODH) or amino acids can be used as the anionic surfactants. The concepts used in propellant chem-
alternative fuels to yield amorphous -phase.21–23 The istry are employed wherein the highest heat is produced
preparation of -Al2 O3 via the combustion route using when the equivalence ratio (= Oxidizer/Fuel) is unity.29
above alternative fuels appears to be less attractive as they Assuming complete combustion, the theoretical equa-
are both expensive and not readily available commercially. tion for the formation of alumina can be written as follows:
In this paper we report for the first time a single step 2AlNO3 3 + 5NH2 CONH2
combustion reaction using urea and HMT as fuels and sur-
factants, which are readily available, to directly yield crys- −→ Al2 O3 + 8N2 + 5CO2 + 10H2 O (1)
talline nano size -Al2 O3 . Apart from being a single step 12AlNO3 3 + 5C6 H12 N4
method, the proposed solution combustion synthesis has
many more advantages over the sol–gel or other wet chem- −→ 6Al2 O3 + 28N2 + 30CO2 + 30H2 O (2)
ical methods. It is free from the use of organic solvents, the In a typical experiment, based on Eq. (1), about 10 g
small time taken for direct product formation; it’s scaling of aluminum nitrate and 4 g of urea are taken in pyrex
up capacity and more importantly the self-removal mech- dish and 3 ml of distilled water is added to this reac-
anism of surfactants during the synthesis process itself tion mixture. To this redox mixture, solutions of various
Article

avoiding the post preparative steps. concentrations (0.1%–1%) of cationic, anionic and non-
It has been demonstrated thatIP:nano crystalline metal
14.97.148.194 On: Thu,ionic
15 Feb 2024 15:26:11
surfactants like CTAB, SDS, citric acid, Tween 80
oxides, especially MgO, CaO, Al2 O3 and Copyright:
ZnO have American
unpar- Scientific Publishers
and Triton-X-100 are added individually as phase and size
alleled sorption properties for polar organics, acid Delivered
gases, bycontrolling
Ingenta agents. A glass crucible containing the redox
and chemical species such as fluoride.24 25 The alumina mixture is then introduced into a pre-heated muffle fur-
matrix is considered to be a potentially efficient adsorbent nace maintained at 500  C. The glass crucible containing
material for fluoride. Of the various commercial activated the redox mixture begins to boil, foam and then undergoes
aluminas, mesoporous aluminas demonstrate significantly combustion within five minutes to produce a homogenous
improved adsorptivity. It has also been recognized that white powder.
the impregnation of fluoride ions into metal oxide cata-
lysts improve their reactivity for many acid catalyzed reac- 2.2. Characterization
tions e.g., hydrocracking or hydrogenation processes26 All the synthesized samples were examined for their phase
and also esterification reactions.27 It is supposed that this and crystallinity by powder X-ray diffraction method using
enhancement of activity, which occurs easily in -Al2 O3 PANalytical X’pert Pro MPD powder X-ray diffractometer
is associated with increased surface acidity caused by the with Cu K ( = 154 Å) radiation, at room temperature.
replacement of oxide/hydroxide by fluoride ions.28 In the The crystallite size was calculated using Scherrer’s equa-
present study an attempt is made to evaluate the fluoride tion after fitting the XRD patterns by Gaussian.30 The
adsorption capacity of the as prepared nano size -Al2 O3 . phase of the alumina matrix was also further confirmed by
Fourier transform infrared (FTIR) spectroscopy. All FTIR
measurements were carried out in transmission mode and
2. EXPERIMENTAL DETAILS in the wavenumber range of 400–4000 cm−1 by KBr disc
2.1. Materials technique, using a Fourier transform infrared spectropho-
The following chemicals were procured and used tometer (SHIMADZU IR Affinity-1).
as received without further purification: aluminium Surface morphology of the synthesized materials was
nitrate-Al(NO3 )3 · 9H2 O, 98%, (Fisher Scientific); urea- evaluated by field emission scanning electron microscope
NH2 CONH2 , 99%, (Fisher Scientific); hexamethylene- (LEO VP-1530) operated at 30 kV. Particle size distribu-
tetramine-(CH2 )6 N4 , 99.5%, (Sd-fine); cetyl trimethyl tion studies were performed by dynamic light scattering
ammonium bromide (CTAB)-C19 H14 BrN, 98%, (Sd-Fine); method using a MALVERIN (ZETASIZER Nano range)
sodium dodecyl sulphate (SDS)-C12 H25 NaO4 S, 94%, (Sd- instrument. HRTEM images were recorded using Tecnai
Fine); Oleic Acid-C18 H34 O2 (Merck); Tween 80-C64 H124 F30 (FEI, Eindhoven, Netherlands) microscope operating
O26 , (Thomas Baker); Triton-X-100-C14 H22 O(C2 H4 O)10 ; at 200 kV. Specific surface area was determined using the

236 Mater. Express, Vol. 4, 2014

Single step preparation of nano size gamma alumina
Chunduri et al.
Materials Express
nitrogen gas adsorption multipoint BET method (Accusorb Table I. Characteristics of the reactions with various fuels/surfactants.
2100E, Micromeritics) assuming a cross sectional area of
Nature of combustion
0.162 nm2 for the nitrogen molecule. Phase of
Fuel/surfactant Fumes Fire Combustion type alumina
2.3. Fluoride Adsorption Study Urea More Bright flame Flaming -Al2 O3
Adsorption of fluoride onto different -alumina samples HMT More Mild flame Smoldering -Al2 O3
was carried out by taking 0.2 g of alumina sample in 100 Urea-CTAB More Mild flame Smoldering -Al2 O3
Urea-SDS More Mild flame Smoldering -Al2 O3
ml of 10 ppm fluoride solution in a 500 ml stoppered con-
Urea-Tween 80 Less Bright flame Flaming -Al2 O3
ical flask. The contents of the flask were kept for shaking Urea-Triton-X-100 Less Bright flame Flaming -Al2 O3
over a period of 12 hours using a mechanical shaker. The Urea-Citric acid Less Bright flame Flaming -Al2 O3
solution was then filtered and residual concentration of
fluoride ion in water samples was measured by a poten-
tiometric method using an Orion potentiometer, (Model ascribed to rhombohedral structure and assigned to JCPDS
SA 720), with a fluoride ion selective electrode (FISE). No. 82-1468.
This method requires the use of a calibration curve pre- From the XRD results it is clear that nature of the sur-
pared with standardized solutions and provides for fluoride factants play an important role in the phase formation
determination in the range of 0.01–100 ppm. A total ionic as well as size control as reported earlier.32 It can be
strength adjusting buffer (TISAB) is used to adjust the pH seen from Table I that tween 80, triton-x-100 and citric
and suppress the activity of other ions present in the solu- acid might be functioning as extra fuel thereby increasing
tion during measurement.31 the exothermicity of the reaction. This might be enabling
the formation of highest stable phase alpha alumina and
also increase in the crystallite size. The flame retarding
3. RESULTS AND DISCUSSION
properties of bromides and sulfates present in the surfac-
Alumina synthesized with urea as the fuel in the pres-
tants, CTAB and SDS, might also be functioning as natural
ence of various cationic, anionic, and nonionic surfactants

Article
and controlled fire retarding agents resulting in metastable
as well as HMT fuel alone were characterized by pow-
IP: 14.97.148.194 On: phase
Thu, of gamma
15 Feb alumina which occurs at lower tempera-
2024 15:26:11
der XRD for material identification, crystallinity and phase
tures. ThePublishers
Copyright: American Scientific crystallite size is calculated to be 2.1 and 2.2 nm
formation (Fig. 1). The role of different surfactants on by Ingenta
Delivered for CTAB and SDS prepared -alumina samples. All the
the characteristic phase of alumina formed is quite evi-
XRD peaks of gamma alumina correspond to a crystalline
dent in the XRD patterns of the samples recorded. While
phase of -alumina with a cubic structure (JCPDS No.10-
HMT, CTAB and SDS exclusively lead to gamma phase
0425). The broadened peaks reflect the nano size of the
of alumina with partial crystallinity, other surfactants like
-alumina samples.
Tween 80, Triton-x-100, and citric acid resulted in crys-
Gamma Alumina synthesized using urea as fuel and
talline phase -alumina. The XRD peaks of -alumina are
CTAB as surfactant was further investigated for their phase
transition by both XRD and FTIR. Figure 2 shows the
XRD patterns of -Al2 O3 sample prepared with urea-
CTAB heated from 600  C to 1100  C. It is observed

Fig. 1. XRD patterns of samples prepared with (a) Urea-CTAB Fig. 2. XRD patterns showing the phase transition of -Al2 O3 at dif-
(b) HMT as fuel (c) Urea-SDS (d) Urea–citric acid (e) Urea-Tween 80 ferent temperatures (a) as prepared (b) 600  C (c) 800  C (d) 900  C
(f) Urea-triton × 100. (e) 1000  C (f) 1100  C.

Mater. Express, Vol. 4, 2014 237

 Materials Express Single step preparation of nano size gamma alumina
Chunduri et al.

Table II. Crystal size calculated from XRD data of the Urea-CTAB is heated to 600  C, broad bands at 3440 cm−1 and
sample calcined at different temperatures. 1650 cm−1 are observed. The 3440 cm−1 and 1650 cm−1
As are O H stretching and bending bands, respectively. The
Temperature prepared 600  C 800  C 900  C 1000  C 1100  C appearance of the broad band is due to disordered dis-
tribution of vacancies for -Al2 O3 nano powders, which
Phase of -Al2 O3 -Al2 O3 -Al2 O3 -Al2 O3 -Al2 O3 -Al2 O3
alumina is caused by incomplete crystallization of -Al2 O3 . The
Crystallite 2.1 3.9 4.9 46.6 48.2 51.4 shoulder at 890 cm−1 and the line at 800 cm−1 are
size (nm) assigned to -AlO4 whereas the broad band in the region of
500–750 cm−1 is assigned to -AlO6 . Thus, -Al2 O3 phase
contains both tetrahedral and octahedral co-ordination.10
that the crystallinity of the sample increased on heating On heating the sample to around 1000  C, three bands
from 600  C to 800  C while the gamma phase of alu- emerge at 640 cm−1 , 602 cm−1 , and 453 cm−1 corre-
mina remains intact. When the samples were further heated sponding to the highly crystalline phase of -Al2 O3 .34
to 900  C and above till 1100  C -Al2 O3 changed into With the increase of heating temperature, the decrease in
highly crystalline -Al2 O3 by destroying the vacancies of intensity of the bands of 3440 cm−1 and 1650 cm−1 is
spinel lattice leading to structural rearrangement and also attributed to loss of O H group due to the transition of
increasing the crystallite size. This transformation how- more easily hydrated -Al2 O3 to the less hydrated form of
ever, did not show any other metastable phase in between -Al2 O3 .
gamma and alpha alumina. The formation of alpha alumina Gamma alumina synthesized using urea as fuel in pres-
occurred below 900  C which is lesser than the tempera- ence of cationic surfactant CTAB and that prepared by
ture reported in the literature.30 HMT as fuel alone were further investigated in detail
The crystallite size of -Al2 O3 has increased from 2.1 to by FESEM, TEM and DLS. FESEM images (Figs. 4(a)
4.9 nm indicating the growth of the crystal with increase in and (b)) show that -Al2 O3 synthesized using urea-CTAB
temperature from 500  C–800  C (Table II). At 900  C the are largely smaller in size than the sample synthesized
Article

crystallite size has increased to 46.6 nm and because of the by HMT fuel alone. It is well reported in the literature
structural rearrangement of atoms and the whole -Al2 O3
IP: 14.97.148.194
is converted into -Al2 O3 . The formation On: Thu, 15 Feb 2024 15:26:11
of alpha alumina
 Copyright: American Scientific Publishers
occurring below 900 C could be because of the higher by Ingenta
Delivered
number of defects present in sample which is known when
combustion synthesis was used. These defects could have
lowered activation energies required for the transformation
by promoting the nucleation and diffusion.33
Figure 3 shows the infrared absorption spectra recorded
for as prepared -Al2 O3 powder made by using urea-
CTAB fuel and then on heating for 1 hr each at tempera-
tures ranging from 600–1200  C. When -Al2 O3 powder

Fig. 3. Infrared spectrum of -Al2 O3 (a) as prepared, heated at Fig. 4. FESEM image of (a) Urea-CTAB synthesized -Al2 O3 ,
(b) 600  C (c) 800  C (d) 1000  C (e) 1100  C. (b) HMT synthesized -Al2 O3 .

238 Mater. Express, Vol. 4, 2014

Single step preparation of nano size gamma alumina
Chunduri et al.
Materials Express
Table III. Comparison of particulate properties of alpha and gamma
alumina.

Density Surface area Particle

Sample (g cm−3 ) (m2 g−1 ) size (nm)∗

Alpha alumina (urea) 3.21 8.60 >800.36

Gamma alumina (HMT as fuel) 2.39 168 >250.37
Gamma alumina (Urea-CTAB) 2.35 221 ∼40

Note: ∗ From TEM.

that surfactant could really play an important role in con-

trolling the size for forming nano size particles.
The test samples were further analyzed for their par-
ticle size distribution by DLS. The DLS graph of HMT
synthesized -Al2 O3 (Figs. 6(a) and (b)) shows the size
distribution from 500 nm to 1000 nm. The average parti-
cle diameter is around 674 nm. The DLS graph of urea-
CTAB synthesized -Al2 O3 shows the size distribution in
Fig. 5. TEM image of Urea-CTAB synthesized -Al2 O3 with inset 2 regions. The high intense peak present at around 100 nm
showing the electron diffraction pattern. indicates that the small particles are in higher number.
The particulate properties of -Al2 O3 prepared under
both the above mentioned conditions were further com-
that when urea alone is used as the fuel the particles of
pared with -Al2 O3 prepared with urea (Table III). It is
alpha alumina obtained are in micron size,29 and by using
interesting to note that -Al2 O3 prepared in the pres-
Tween as the surfactant the particle size reduces to around
ence of the surfactant has large specific surface area of

Article
400 nm.35
221 m2 g−1 compared to those prepared only in the pres-
The TEM image of -Al2 O3 IP: synthesized using urea-
14.97.148.194 On: Thu,ence
15 Feb
of a2024
fuel. 15:26:11
This variation in particulate and surface
CTAB are shown in Figure 5. The image Copyright:
shows American
that the Scientific Publishers
Delivered properties could be attributed to the role of surfactant in
particles are agglomerated partially and their size is around bycontrolling
Ingenta
the nature of combustion, either flaming or
40 nm. The particles are of spherical shape as observed by smoldering. The surfactant also seems to be combating the
TEM image. The electron diffraction pattern (inset) shows problem of agglomeration which is significantly observed
the diffused ring pattern confirming to the partial crys- in combustion derived powders thereby yielding smaller
talline feature of gamma alumina. TEM images confirmed size particles.
A detailed fluoride adsorption study was made on the
synthesized products to study the effect of surfactants,
which regulate the phase, extent of agglomeration and par-
ticle size of the formed alumina (Table IV). The adsorption
of fluoride on alumina matrix was evaluated by measur-
ing the residual fluoride concentration in water. This study
shows that gamma alumina has more affinity for fluoride
adsorption because of its catalytic sites and highly reactive
surface.

Table IV. Adsorption of fluoride on aluminas synthesized by various

surfactants.

pH Final Adsorption
Alumina Quantity conc. capacity
Surfactant type (mg) Before After (ppm) (mg g−1 )

CTAB -alumina 200 657 6.2 0.2 49

Citric acid -alumina 200 70 6.5 7.7 115
SDS -alumina 200 695 6.5 8.5 075
Tween 80 -alumina 200 72 7.6 7.3 135
Without -alumina 200 65 6.5 8.9 055
surfactant
Commercial -alumina 200 66 6.6 9.2 04
Fig. 6. DLS data showing the size distribution of (a) HMT synthe-
alumina
sized -Al2 O3 , (b) Urea-CTAB synthesized -Al2 O3 .

Mater. Express, Vol. 4, 2014 239

 Materials Express Single step preparation of nano size gamma alumina
Chunduri et al.

Table V. Fluoride adsorption capacity on gamma alumina obtained by References and Notes
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Received: 1 November 2013. Accepted: 8 February 2014.

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