I J A C

1 2 2 2 7

Journal Code

Manuscript No.

Dispatch: 20.1.14

CE: Malini J.

No. of pages: 7

PE: Raghu

Int. J. Appl. Ceram. Technol., 17 (2014)

DOI:10.1111/ijac.12227

Synthesis, Crystal Structure, Spectroscopic and Thermal Analysis of

Strontium Pyrophosphate Dihydrate Nanoparticles
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Pushpakant Solanki,* Sonal Vasant, and Mihir Joshi

Crystal Growth Laboratory, Department of Physics, Saurashtra University, Rajkot 360005, Gujarat, India

Various pyrophosphates are very useful as bioceramics; for instance, strontium pyrophosphate is one of the emerging forms
of alkaline phosphate. Strontium pyrophosphate dihydrate (Sr2P2O72H2O) nanoparticles were synthesized by the surfactant-mediated approach and characterized by different techniques. From the powder XRD study, the average crystallite size was evaluated
by applying Scherrers formula, which was found to be 33.57 nm. The average crystallite size and internal strain were also evaluated using WilliamsonHall (W-H) method. The FT-IR spectroscopy study confirmed the presence of symmetric and asymmetric stretching vibrations of POP and PO3. The UV-NIR absorption spectroscopy over the spectral range of 2101200 nm was
employed, and the energy band gap was calculated from Taucs plot which was found to be 4.9 eV. Thermogravimetric analysis
(TGA) confirmed the presence of two water molecules in the sample. From TGA, it was found that the sample become anhydrous and on heating above 410800C, the sample remained almost stable with slight weight gain due to adsorption of purged
gas. Various kinetic parameters and thermodynamic parameters were evaluated for dehydration process.

Introduction
Pyrophosphates are very useful as bioactive ceramics;
particularly, calcium pyrophosphate has made impressive
progress as biocompatible material promoting tissue formation.13 Strontium is alkaline earth metal found in
bones and teeth. As strontium is chemically similar to
calcium, it has pharmacological effects on bones when it
is present at levels higher than required for normal cell
physiology. Strontium enhances the replication of bone
cells and also stimulates the bone formation in calvarial
culture in vitro.4 The ionic strontium in humans has the
same physiological pathway as calcium5 and can be
deposited into the mineral structure of bone, especially,
in the region of high metabolic turn over.6 Apart from
this biologic application, pure strontium pyrophosphate
as well as certain metal-doped and mixed strontium
pyrophosphate compounds finds promising applications
in phosphor materials. Strontium pyrophosphate has
been suggested as adhesive in luminescent screens.7 Divalent europium is found to be more attractive for doping
in strontium pyrophosphate phosphor giving emission at
420 nm. Strontium pyrophosphate activated by europium has been used in the fluorescent lamps in photocopying system, which enables higher production rates.8
Photoluminescence and thermally stimulated luminescence has been reported in europium-doped strontium
pyrophosphate by Natarajan et al.9 There are patents
obtained based on strontium pyrophosphate phosphors10
*pds_2307@yahoo.co.in
2014 The American Ceramic Society

and europium-activated strontiummagnesium pyrophosphate phosphors.11 Altogether, the thermoluminescence

properties of strontium pyrophosphate doped with metals12 as well as luminescent properties of strontiumzinc
pyrophosphate co-activated by silver13 have been
reported.
Due to large surface to volume ratio, the nanoparticles are expected to alter physical and chemical properties
of pyrophosphates. Therefore, several pyrophosphates
have been synthesized, such as calcium pyrophosphate,14
cerium pyrophosphate, and15 zinc pyrophosphate.16 The
synthesis and characterization of doped nanocalcium
pyrophosphates are reported, for instance, the zinc-doped
nanocalcium pyrophosphate by Vasant and Joshi.17
Dielectric study and transmission electron microscopy
(TEM) of strontium pyrophosphate nanoparticles18 have
been reported. The present communication further characterizes strontium pyrophosphate nanoparticles by powder XRD, FT-IR, UV-NIR, and thermogravimetric
analysis (TGA).

Experimental Procedure
In the present investigation, the surfactant-mediated
approach was used to synthesize strontium pyrophosphate nanoparticles, which is discussed in detail elsewhere.19 Equal amount of 0.25M aqueous solution of
freshly prepared AR grade tetrasodium pyrophosphate
(Na4P2O7) and 0.5M aqueous solution of AR grade
strontium chloride hexahydrate (SrCl2.6H2O) was used.

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International Journal of Applied Ceramic TechnologySolanki, Vasant, and Joshi

Na4P2O7 solution was added dropwise into the 5:1 mixture of SrCl2.6H2O and Triton X-100 surfactant with
constant stirring at room temperature. The reaction of
SrCl2.6H2O with Na4P2O7 in a presence of nonionic
surfactant (Triton X-100) resulted in white precipitates
at the end of reaction with a pH value of the solution
8.57. The resulting precipitates were quickly filtered
using Whatman filter paper no 1 and washed with deionized water and air-dried. The following chemical reaction is to occur:
2SrCl2 :6H2 O Na4 P2 O7
4NaCl 10H2 O

Surfactant

! Sr2 P2 O7 :2H2 O
1

The synthesized nanocrystalline samples were characterized by several techniques. The powder XRD
(XPERT MPD, PHILIPS, Eindhoven, the Netherlands)
was carried out using Cu Ka radiation with 2h range
from 5 to 85 in 0.01 steps having 1 s dwell time/
step. The FT-IR (Nicolet 6700, Thermo Scientific)
spectrum of the sample in KBr powder pellet was
recorded in the range of 4004000/cm. The pellet was
prepared by mixing 1.0 mg powder sample with
300 mg IR transparent KBr. UV-NIR spectrophotometer (Lambda 750, Perkin Elmer, Shelton, CT) was used
to record optical absorption data of sample over the
spectral range of 210 nm to 1200 nm with A.R grade
methanol as a solvent and scanning speed of 2 nm/sec.
The TGA (Geratebau GmbH, NETZSCH, Selb,
Germany) was carried out from room temperature to
800C at a heating rate of 15C/min under the atmosphere of air.

Fig. 1. Powder X-ray diffractogram of Sr2P2O7.2H2O nanoparticles.

2014

Results and Discussion

In the case of synthesis of strontium pyrophosphate
by wet chemical technique, agglomeration of particles is
quite common, due to their tendency to aggregate themselves. This aggregation, however, can be avoided using
suitable water soluble surfactant, which plays a key role
in limiting the particle size as well as agglomeration.20
The amphiphilicity of the surfactant allows coating on
the surface by an adsorption process. As the surfactant is
dissolved in water, its hydrophilic tails are immersed in
water and play the role of extractant; on the other hand,
its hydrophobic tails remain in air play the role of a capping agent. Thus, the role of surfactant is very important
in the synthesis of nanoparticles of strontium pyrophosphate at room temperature. Various factors affect the
efficiency of surfactants such as molecular structure, nature of head group and the length of hydrophobic tail,
which is discussed elsewhere by Paria and Khilar.21 In
the present study, the authors have used nonionic surfactant Triton X-100.
The Sr2P2O7 exhibits two polymorphic forms, viz.
orthorhombic a-form and tetragonal b-form22 modifications; each one is metastable at room temperature. The
diffraction lines of a powder XRD pattern are very sharp
for the crystalline material consisting of sufficiently large
and strain-free crystallites,23 but for nanoparticles a characteristic line broadening is observed.24 Figure 1 represents the powder XRD pattern of hydrated strontium
pyrophosphate nanoparticles with selected zoom plot of
2h range 1565. The powder XRD data were analyzed
by software powder X, and the tetragonal structure was

www.ceramics.org/ACT

Strontium Pyrophosphate Nanoparticle

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found with estimated values of the unit cell parameters



as: a = b = 6.75 
A, c = 25.01 
A, a = b = c = 90.00,
which is closely matching with the reported values
1 (JCPDS No: 13-0194).25 The average crystallite size of
2 synthesized Sr2P2O7.2H2O nanoparticles was calculated
3 using the Scherrers formula as follows:
4
t kk=b cos h
2
5
A,
6 where t = average crystallite size, k = 1.54178 
7 b = full-width half maximum (FWHM) of the high8 intensity peaks, and k = constant.
The value of k can be taken as 0.9 for circular
9
grains.
In the Scherrers formula, the average crystallite
10
size
(t)
is calculated by considering the Gaussian fit to
11
the
peaks
in the XRD patterns and obtained by taking
12
average
for
all peaks.26 In the present study, the average
13
14 crystallite size is found to be 33.57 nm after considering
15 all major peaks in the XRD patterns, whereas William16 son and Hall considered both the limited crystallite size
17 and the presence of crystallographic distortion or strain
18 leading to the Lorentzian intensity distribution and can
27
19 be expressed as follows:
20
b cos h kk=L g sin h
3
21
22 Where b = FWHM, L = crystallite size, g = strain,
A.
23 k = 0.9, and k = 1.54178 
Figure 2 is the linear fitted plot of b cosh versus
24
25 sinh for different high-intensity peaks. From the inter26 cept of this linear plot on y-axis and its slope, the values
27 of average crystallite size (L) and average strain (g) are
28 calculated, which are found to be 32.80 nm and
29 0.00534, respectively. The average crystallite size
30 obtained from Williamson and Hall method is usually
31 less than that obtained from Scherrers formula because
32 the strain correction factor is considered in the William33
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49 Fig. 2. WilliamsonHull plot for b cosh versus sinh.

3 1

son and Hall method.28 Altogether, the particle size was

also determined using TEM and found to in the range
of 22.27 nm to 34.15 nm, which has been reported earlier by Solanki et al.18 It is to be noted that the average
crystallite size calculated by the WilliamsonHall plot
and the Scherrers formula is corresponds to the range of
particle size obtained from TEM.
The Fig. 3 shows the FT-IR spectrum of Sr2P2O7
hydrated sample, which closely resembles to those of
X2P2O7 (X = Cu, Ca, Cd, Fe, Mn).22,29,30 From the
spectrum, it is observed that the narrow absorption
bands occurring at 3588.6/cm and 1629.9/cm are due to
the OH stretching and OH in-plane bending vibration, respectively, due to the moisture content or water
of hydration. The absorptions due to the PO3 and the
POP bridge can be identified from the FT-IR spectrum. The asymmetric and symmetric stretching vibrations of the PO3 are generally observed in the range
1200950/cm. The deformation and rocking modes are
expected to occur in the region 600400/cm for PO3.
The symmetric POP bridge stretching vibration
observed at 726.5/cm is the most striking feature for
(P2O7)4 anions in Sr2P2O7.2H2O. The POP asymmetric and symmetric modes of vibrations are found
within the region of 7001000/cm. Metal-oxygen vibrations are generally too low to be seen in the 4004000/
cm domain. Table I represents the assignments of different absorptions bands in FT-IR spectrum. It confirms
the presence of OH stretching and in-plane bending
vibration and symmetric as well as asymmetric stretching
modes of POP and PO3. An attempt is made to calculate the force constant of simple OH stretching vibration from the FTIR spectrum. Considering a molecular 5
model where the nuclei are represented by point masses
and the interatomic bonds are represented by massless
spring, which follows Hookes law31
s
1
k
4
v
2pc l
Where l is the reduced mass (masses are expressed
in unified atomic mass unit), m is the absorption frequency in per cm, c is the speed of light, and the force
constant k is expressed in N/m. This model is more
applicable to diatomic vibrations, particularly stretching
vibrations. The force constant (k) for OH stretching
vibration is found to be 7.14 N/m.
Figure 4 shows UV-NIR absorbance spectrum of
Sr2P2O7.2H2O, nanoparticles recorded in the range of
210 nm to 1200 nm. Double beam UV-NIR spectrophotometer was used to record the spectrum taking
methanol as a reference solvent in quartz cuvettes with

International Journal of Applied Ceramic TechnologySolanki, Vasant, and Joshi

2014

C -LOW RESOLUTION FIG

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Fig. 3. FT-IR spectrum of Sr2P2O7.2H2O nanoparticles.

Table I. Assignments of Bands in the FT-IR Spectrum of Sr2P2O7.2H2O Nanoparticles

Band assignments

Observed
frequencies per cm

PO3 Rocking
PO3 deformation
POP Symmetric vibration
POP symmetric stretching
POP asymmetric stretching
PO3 symmetric stretching
PO3 asymmetric stretching
OH in-plane bending vibration
OH stretching vibration

459.5
504.5
726.5
884
980.3
1028.5
1140.3
1629.3
3588.6

the optical path length 10 mm. Solution of sample is

prepared in such a way that the absorbance value lies
within 0.05 A.U to 1.0 A.U. In this range, the absorbance is independent of concentration of solution and
follows BeerLamberts relation. Care is taken to avoid
the absorbance due to cuvettes and solvent by adjusting
auto zero so that a pure absorbance spectrum of the sample under investigation is obtained. The direct optical
energy band gap was calculated using Taucs formula:32
ahv Bhv

Eg 1=2

Where a is the absorption coefficient, hv is the photon energy, and B is a constant.

The direct energy band gap (Eg) has been estimated

from the inset plot of Fig. 4 known as Taucs plot. A
strong cutoff wavelength for methanol is observed at
210 nm, and hence, the plot of (ahv)2 versus (hv) is
drawn for the wavelength range 210 nm to 1200 nm,
and the linear portion of the curves is extrapolated to
energy axis.33 The direct optical energy band gap is
found to be 4.9 eV. Generally, this type of wide band
gap material is used in devices which find applications in
electric subsystems requiring high temperature and high
power operation.34
Thermogravimetric analysis (TGA) is carried out to
find out thermal stability of strontium pyrophosphate
nanoparticles and the amount of water molecules associated with them. Figure 5 shows the thermogram of
Sr2P2O7.2H2O nanoparticles, which indicates that the
sample is almost stable up to 200C; however, the small
mass loss corresponding to the release of adsorbed water
is observed. The mass loss from 99.19% to 89.77%
occurs between 200 and 300C, which is due to dehydration of the sample. Calculation shows found that two
water molecules are attached with the structure, which
begins to leave at 300C. Above 300C, the mass loss
occurs through a very slow process, followed by a stable
state from 410C to the end of the analysis at 800C,
where the mass loss is of 12.3243% of the original
hydrated mass. One can notice from the thermogram
that slight weight gain is observed beyond 600C temperature, which may be due to absorption of purged gas
by the sample. The thermogram indicates higher thermal

Strontium Pyrophosphate Nanoparticle

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Fig. 4. UV-NIR absorption spectra and Taucs plot of the

Sr2P2O7.2H2O nanoparticles.

stability of strontium pyrophosphate, which corresponds

to other pyrophosphates such as calcium pyrophosphate,35 zinc-doped calcium pyrophosphate,17 and zirconium pyrophosphate.36
The kinetic parameters of dehydration of strontium
pyrophosphate nanoparticles are evaluated by the Coats
and Redfern relation,37 which is as follows:
! 
 

1 1 a1 n
AR
1 2RT
log10

log
10
aE
E
T 2 1 n


E
2:3RT
6

5 1

Where a = fraction of the original substance decomW)/(W0

Wf), W0 = iniposed at time t, a = (W0
tial weight, W = weight at time t, Wf = final weight,
n = order of reaction, A = frequency factor, E = activation energy of the reaction, R = gas constant, and
a = heating rate in deg./min.
To determine the value of activation energy and
order of reaction, a plot of log10 [{1 (1
a)1 n}/
2
{T (1 n)}] versus 1/T is drawn for different values of
n and the best linear fit of plot gives the correct value
of n. The activation energy can be calculated from the
slope of the plot. Figure 6 is a plot of Coats and Redfern relation for n = 5/2, which gives the best linear fit.
Table II shows the values of different kinetic parameters
obtained from the Coats and Redfern relation.38
Table III summarizes the values of different thermodynamic parameters, that is, standard entropy (D# S),
standard enthalpy (D# H), standard Gibbs free energy
(D# G), and standard change in internal energy(D#
U),39 obtained for dehydration stage from the thermogram. Positive values of D# S and D# H as well as
negative value of standard Gibbs free energy suggest
thermodynamically stable nature of material, and the
reaction will occur spontaneously at high temperature.40
As strontium pyrophosphate dihydrate is having sufficiently large band gap and remains stable up to 200C,
the Sr2P2O7.2H2O nanoparticles may prove to be useful
in electric subsystems requiring high temperature and
high power operation.

Fig. 5. Thermogravimetric analysis (TGA) curves of Sr2P2O7.2H2O nanoparticles.

International Journal of Applied Ceramic TechnologySolanki, Vasant, and Joshi

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2014

33.57 nm from Scherrers formula and 32.80 nm from

Williamson and Hall formula. The FTIR spectra confirmed the presence of POP, PO3, and OH functional groups, and the force constant was calculated for
OH stretching vibration which was found to be
7.14 N/m. The direct energy band gap was evaluated
from UV-NIR absorption spectrum and found to be
4.9 eV, which suggested the wide band gap semiconductor type nature. TGA confirmed that two water molecules were associated with the material and on heating
above 410C anhydrous Sr2P2O7 was formed, which
exhibited higher thermal stability.
Fig. 6. The plot of
1/T.

log10 [{1 (1 a)1 n}/{T2(1 n)}] versus

Table II. The Kinetic Parameters for Dehydration

Obtained from the Coats and Redfern Relation
Sample
Strontium
Pyrophosphate
Sr2P2O7

Kinetic parameter
Order of reaction (n) = 5/2
Activation energy (E) =
64.624 kJ/Mol
Frequency factor (A) =
5.716 9 1018

Acknowledgment
The authors are thankful to Government of Gujarat
for giving financial assistance under the sanctioned project on, Nano-science and Technology and Environmental Physics and UGC, Delhi, India, for providing
research facility under DRS-SAP at Department of Physics, Saurashtra Unversity, Rajkot. Authors are thankful to
the Director, SAIF, CIL, and UCIM, Panjab University,
Chandigarh, India, for UV-NIR analysis. Authors are
thankful to Prof. H. H Joshi (HOD, Department of
Physics) for his keen interest and support.

Supporting Information
Table III. The Values of Different Thermodynamic
Parameters of Dehydration of Sr2P2O7 Nanoparticles
Sample
Strontium
pyrophosphate
Sr2P2O7

Thermodynamics parameters
Standard change in entropy
D# S = 1.4729 Jk/Mol
Standard change in enthalpy
D# H = 55.3933 kJ/Mol
Standard change in Gibbs free energy
D# G = 26.535 kJ/Mol
Standard change in internal energy
D# U = 60.0178 kJ/Mol

Conclusion
The nanoparticles of Sr2P2O7.2H2O were synthesized by surfactant-mediated approach. The characteristic
peak broadening of powder XRD pattern was observed,
and the crystal structure was found to be tetragonal with
unit cell parameters as: a = b = 6.75 
A, c = 25.01 
A,
and a = b = c = 90. The particle size was found to

Additional Supporting Information may be found in

the online version of this article:
Data S1. Pyrophosphates of various metals find dif- 8
ferent applications, Strontium pyrophosphate is known
for its application as phosphor.

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