Int. Journal of Applied Sciences and Engineering Research, Vol.

1, Issue 6, 2012
2012 by the authors Licensee IJASER- Under Creative Commons License 3.0
Research article

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ISSN 2277 9442

Synthesis and Characterization of Aluminium Phosphate

Nanoparticles
1

R. Hepzi Pramila Devamani, 2M. Alagar

Post Graduate Department of Physics, V.V.Vanniaperumal College, Virudhunagar.
2
Centre for Research and Post Graduate Department of Physics, Ayya Nadar Janaki Ammal College,
Sivakasi
DOI: 10.6088/ijaser.0020101078
1

Abstract: Nano particles of Aluminium phosphate have been prepared by chemical co-precipitation
method. The particle size and crystal structure of Aluminium phosphate nano powders are characterized by
X-ray diffraction (XRD).The surface morphology of the sample is studied from SEM images. The FTIR
spectrum is used to study the stretching and bending frequencies of functional groups in the sample. The
absorption spectra of the sample are recorded in the UV range. From the analysis of absorption spectra,
Aluminium phosphate is found to have a direct band gap of 5.41eV.
Keywords: XRD, SEM, FTIR, UV.

1. Introduction
One route to increase the energy output of explosives and propellants is through metallization. Aluminum,
in particular, is an attractive additive to energetic materials due to its high energy density (Horn,
2012),(Jouet,2006),(Rai,2006),(Jouet,2005). However, the practicality of using aluminum in energetics
applications has been hindered by the rate of oxidation in the bulk metal. In order to reduce the diffusion
time and increase reaction rate, metal composite nanoparticles are being explored. Although nano scale
aluminum is theoretically a good fit for energetics applications, there are some significant concerns
associated with using it. For example, there is the potential for excessive oxidation of the aluminum nano
particle before combustion. Aluminum particles typically contain a naturally occurring oxide coating that
ranges from 1.7 to 6.0 nm thick, regardless of particle size(Horn, 2012),(Pesri,2004). For larger particles,
this oxide layer represents a small percentage of the total particle. However, as particle size decreases into
the nano scale regime, the oxide layer becomes a significant percentage of total particle mass, i.e.
approximately 45% of the mass of a 40 nm aluminum particle consists of aluminum oxide. By removing or
altering this parasitic aluminum oxide layer, the energy content of aluminum nanoparticles can be
increased. However, the surface of the aluminum particle must be passivated in order to avoid additional
oxidation from oxygen in the atmosphere (Horn, 2012).
Aluminium particle is used in rocket propellant formulations. Aluminium phosphate is used industrially
as a high-temperature dehydrating agent. It is used as flux for ceramics; as cement in combination with
calcium sulfate and sodium silicate and in the manufacture of special glasses. It is also used in dried gel
and therapeutically as antacid. Aluminium phosphate has the characteristics of a catalyst and a
catalyst support as well as of an adsorbent. Aluminium phosphate has been found to catalyse almost
all the reactions catalysed by boron phosphate, but with a lower
activity. The
acid-base
properties of aluminium phosphate reported that aluminium phosphate can promote the Prins
reaction (the preparation of isoprene from isobutylene and formaldehyde) which requires

*Corresponding author (e-mail: fbdpatel@gmail.com)

Received on October 19, 2012; Accepted on December 09, 2012; Published on December 18, 2012

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Synthesis and Characterization of Aluminium Phosphate Nanoparticles

strongly acidic sites (Vetrivel,1984). Aluminium phosphate is mostly used as binder and curing agent in
the production of high temperature refractory materials for kiln. It also serve as fluxing agent in the
production of special glass, as binder in fabrication of ceramics or tooth and as catalyst in organic synthesis.
Alumino phosphate, or AlPO4, exhibits a rich structural diversity in both dense and crystalline micro
porous series frameworks (Chung Sung Yang,2005),(Hu,1995). The commercially available micro porous
AlPO4-X series products, made under the Union Carbide patent, have been widely applied in ion exchange,
separations, and catalysis (Chung Sung Yang,2005),(Davis, 1992).AlPO4, in its dense state, is no longer
only of interest to those working in novel phase discovery. Generally, the dense phase framework lacks the
porous structure, which has a chiral tetrahedra configuration that is potentially useful in enantiomer
separation of amino acids and their ester derivatives (Chung Sung Yang, 2005), (Cao, 1992),
(Kavasmaneck, 1976). However, the dense polymorphs of AlPO4, i.e., berlinite, tridymite and cristobalite,
have valuable information to assist in interpreting the evolution of framework topology between the
condensation and micro porous phases; this is because the formation of micro porous AlPO4 frame-works,
in an aqueous environment, is only -11 to -30 kJ/mol less stable in enthalpy than berlinite (quartz structure).
To investigate the morphology evolution and structural diversity for the systems mentioned above, it was
essential to closely monitor the crystal growth by systematic chemical variation, in order to control the
evolution environment during the reaction progress. The simultaneous control over size, morphology, and
size distribution of nano crystals is an on-going challenge. In fact, the control of morphology alone is
extremely difficult (Chung Sung Yang, 2005), (Peng, 2001). Unfortunately, in decades past, morphology
evolution was not a major topic for researchers in the fields of zeolites and molecular sieves; this makes
available information for crystallization in general, and crystal shape or morphology control in particular,
for AlPO4 nano crystals. Sparse (Chung Sung Yang, 2005). Nano crystalline A1P04 has been
extensively used as a catalyst, ion- exchanger, adsorbent and so on. In these usages,
understanding of the interaction between A1P04 surface and other substances (Mathews, 2010) is of great
interest. This interaction relates to the surface structure and properties of AIP04, such as surface functional
groups, surface charge, hydrophilicity and porosity. Many workers' reported that the Alp04 surface
possesses P-OH and AI- OH groups. Therefore, the regulation of these surface sites may be expected to
give rise to many properties, such as acidity and basicity, affinity and reactivity to molecules and catalytic
activity (Mathews, 2010).

2. Materials and methods

Nano particles of Aluminium phosphate was prepared by chemical precipitation method, adding
aluminium sulphate and sodium phosphate. Precise amount of the reagents taking into account their purity
were weighed and dissolved separately in distilled water into 0.1 M concentration. After obtaining a
homogeneous solution, the reagents were mixed using magnetic stirring. The precipitate was separated
from the reaction mixture and washed several times with distilled water. The wet precipitate is dried and
thoroughly ground using an agate mortar to obtain the samples in the form of fine powder.

3. Tests conducted
X-ray diffraction is an ideal technique for the determination of crystallite size of the powder samples. The
basic principle for such a determination involves precise quantification of the broadening of the peaks.
XRD line broadening method of particle size estimation was chosen in this
investigation for
R. Hepzi Pramila Devamani, M. Alagar
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Synthesis and Characterization of Aluminium Phosphate Nanoparticles

determining the crystallite size of the powder sample. XRD study and the morphology of the powder
samples were carried out by scanning electron microscope (SEM) at Centre for Electro Chemical Research
Institute, Karaikudi. The infra red spectroscopic (IR) studies of Aluminium phosphate nano particles were
made by using SHIMADZU FTIR 8400S model spectrometer through KBr method. The UV spectrum
was taken in the absorbance mode in the wavelength range from 200 to 800 nm.

4. Results and discussion

4.1. XRD studies
The XRD patterns of the prepared samples of aluminium phosphate are shown in fig.1. XRD studies reveal
that the samples are nano sized and crystalline. The fine particle nature of the samples is reflected in the
X-ray line broadening. The size of the synthesized aluminum phosphate nano particles are calculated using
Scherrer equation D = 0.9/ cos where represents wavelength of X rays , represents half width at full
maximum and is the diffraction angle. The average grain size of the particles is found to be 55.75nm.The
peak list in the XRD pattern is given in table1.
Table 1: Peak list in the XRD pattern of Aluminium phosphate nano particle
Pos. [2Th.]

Height [cts]

FWHM [2Th.]

d-spacing []

Rel. Int. [%]

19.1609

413.88

0.1574

4.63210

60.08

20.4837

365.92

0.3149

4.33586

53.12

21.5852

466.44

0.3149

4.11703

67.72

22.8604

456.57

0.3936

3.89017

66.28

25.6815

223.12

0.9446

3.46889

32.39

28.1711

406.43

0.2362

3.16773

59.00

29.1105

404.03

0.2362

3.06761

58.65

32.2514

688.83

0.1574

2.77567

100.00

33.9976

414.91

0.2755

2.63700

60.23

38.2142

49.09

0.9446

2.35518

7.13

48.9208

124.60

0.3360

1.86034

18.09

Counts
aluminium phosphate

1600

900

400

100

0
10

20

30

40

50

60

70

Position [2Theta]

Figure 1: XRD pattern of Aluminium Phosphate Nanoparticles

R. Hepzi Pramila Devamani, M. Alagar
Int. Journal of Applied Sciences and Engineering Research, Vol. 1, Issue 6, 2012

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Synthesis and Characterization of Aluminium Phosphate Nanoparticles

(i) 2Theta = 32.2514

Theta = 32.2514/2 = 16.1257 * 3.14 / 180
= 0.2813
D = (0.9 * 0.154) / (0.001574) * cos (0.2813) = 0.1386 / 0.001574 = 88.05 nm
(ii) 2Theta = 21.5852
Theta = 21.5852/2 = 10.7926 * 3.14 / 180
= 0.1822
D = (0.9 * 0.154) / (0.003149) * cos (0.1822) = 0.1386 / 0.003149 = 44.01nm
(iii) 2Theta = 22.8604
Theta = 22.8604/2 = 11.4302 * 3.14 / 180
= 0.1995
D = (0.9 * 0.154) / (0.003936) * cos (0.1995) = 0.1386 / 0.003936 = 35.21nm
Average D = 88.05 + 44.01 + 35.21 / 3 = 167.27 / 3 = 55.75nm

4.2 SEM studies

To identify the morphology of nano particles, the synthesized sample Aluminium Phosphate was subjected
to SEM studies. From the SEM studies, the morphology of the particles are identified. The morphology of
most of the particles in SEM were observed to be tetrahedral .The fig.2 and fig.3 show the SEM images of
Aluminium Phosphate sample.

Figure 2: SEM image of aluminium phosphate at 3.00 kx

Figure 3: SEM image of aluminium phosphate at 5.00 kx

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Synthesis and Characterization of Aluminium Phosphate Nanoparticles

4.3 FTIR Studies

The FTIR spectrum of the bulk sample shows that the basic structural elements of A1P04 are
tetrahedral units although there are two types of tetrahedra in the framework structure,
that is, [AIO4]5-. and [PO4]3- Thus, there are two different bonds present in the structure of AlP04:
a stronger P-0, and a weaker Al-O. For a pure bulk A1P04 sample, the individual P-0
symmetric stretching (1100 cm-1), asymmetric stretching (1250 cm-1), symmetric bending (480 cm-1)
and asymmetric bending (695cm-l) modes are expected in the IR spectrum.
Thus the band observed in the FTIR spectrum of nano crystalline Alp04 (Fig.4) around the band
1122.49cm-1 (Mathews, 2010) corresponds to the symmetric stretching mode of [PO4]3-. The strong peak at
3404.13cm-1 corresponds to the O-H stretching. Another strong and sharp peak with a maximum of
1666.38cm-1 is due to water molecule. The spectrum also shows peak at 1402.15 cm-1 indicating CH2
bending and the presence of the peaks at 661.54 cm-1 and 611.39 cm-1 indicates the presence of nano
aluminium and the peak at 466.74 cm-1
indicates the symmetric bending.

Figure 4: The FTIR spectrum for Aluminium phosphate nano particles

4.4 UV Studies
The band gap of the prepared sample Aluminium phosphate was determined by using UV visible studies.
From the UV spectrum the optical band gap of Aluminium phosphate is 5.41ev. Fig.5 shows the graph to
find the band gap of Aluminium phosphate.

R. Hepzi Pramila Devamani, M. Alagar

Int. Journal of Applied Sciences and Engineering Research, Vol. 1, Issue 6, 2012

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Synthesis and Characterization of Aluminium Phosphate Nanoparticles

uv for alpo4
6.00E-36

5.00E-36

ahu*ahu

4.00E-36

3.00E-36

2.00E-36

1.00E-36

9.88E-43
3.11E+00

4.11E+00

5.11E+00

6.11E+00

E(ev)

Figure 5: Graph to find Band gap of Aluminium Phosphate Nanoparticles

5. Conclusions
The aluminium phosphate nanoparticles have been prepared by chemical co-precipitation method. XRD
analysis and SEM suggest that the average particle size is in the nano range. The SEM picture reveals the
morphology of the particles. The sizes of the small individual particles are less than 100nm in diameter,
while the composite particles in lower resolution would appear higher in particle size. When the SEM
images are magnified they show the same region. From the FTIR spectrum, the stretching and bending
frequencies of the molecular functional groups in the sample are studied. From the UV spectra, the band
gap was found.

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