V.B. Bhatkar et al.

/ (IJAEST) INTERNATIONAL JOURNAL OF ADVANCED ENGINEERING SCIENCES AND TECHNOLOGIES

Vol No. 5, Issue No. 2, 184 -186

Combustion Synthesis and Photoluminescence

Characteristics of Akermanite: A Novel
Biomaterial

V.B. Bhatkar N.V.Bhatkar

Department of Physics Department of Zoology
Shri Shivaji College Shri Shivaji College
AKOT (MS) 444101 India AKOT (MS) 444101 India
bhatkar_vinod@yahoo.com bhatkarneha@hotmail.com

Abstract— Silicate based bioceramics are the promising candidates Akermanite and wollastonite have also been studied for drug
as biomaterials for tissue engineering. The combustion synthesis delivery [18].

T
method provides the control on the morphology and the particle size
of the synthesised material. This paper discusses the combustion Akermanite belongs to the Tetragonal crystal system with
synthesis of Akermanite (Ca2MgSi2O7 and Sr2MgSi2O7), which has Space Group, P421m where a = 7.8288(8) c = 5.0052(5) Z = 2
been shown to have good In vitro and in vivo bioactivity by the and point group: 42m. It is optically transparent to translucent
earlier studies. Both Ca2MgSi2O7 and Sr2MgSi2O7 have akermanite and colorless. The X-ray powder pattern is characterized by
structure. Ca2MgSi2O7 and Sr2MgSi2O7 were prepared using urea strong lines at 2.87 (100), 3.09 (30), 1.764 (30), 2.039 (20),
ES
and ammonium nitrate. The combustion synthesis using Urea and
Ammonium Nitrate was found to be cost effective and efficient
method of synthesis. The photoluminescence study of Ca 2MgSi2O7:
Eu2+ and Sr2MgSi2O7: Eu2+ shows host specific intense emission of
Eu2+.
2.488 (18), 3.73 (14), 5.55 (12). Most of the silicates have
high melting points. Moreover, they can appear in crystalline
as well as glassy form. Synthesis of silicates is rather tricky
for these reasons. Conventionally, solid-state diffusion
methods have been used for the synthesis of silicates.
Keywords- Biomaterials, Silicates, Akermanite, Combustion Akermanite ceramics prepared by sintering akermanite
synthesis, Photoluminescence powder compacts at 1370° C for 6 h, is previously reported
[19]. Pure akermanite (Ca2MgSi2O7) powders with
I. INTRODUCTION polycrystalline particles with dimensions of 5–40 μm, were
It is essential to develop biocompatible, bioactive, synthesized by sol–gel method [20].
bioresorbable and durable materials for orthopaedic and dental
The combustion synthesis as a preparation process to
implants, that are capable of bearing high stress and loads, and
A
produce homogeneous, very fine crystalline, unagglomerated,
that invoke positive cellular and genetic responses for the
multicomponent oxide ceramic powders without the
rapid repair, modification, regeneration and maintenance of
intermediate decomposition and/or calcining steps has
the affected tissue in the human body [1]. Silicate-based
attracted a good deal of attention [21, 22]. The combustion
bioceramics, including silicate bioglass 45S5 [2, 3],
synthesis is based on the exothermic reaction between fuel and
wollastonite (CaSiO3) [4-6], akermanite (Ca2MgSi2O7) [3],
oxidiser. The combustion process has several advantages over
diopside (Ca2MgSi2O6) [7] and merwinite (Ca3MgSi2O8) [8]
the other methods in terms of simplicity, cost-effectiveness,
ceramics, have been shown to have excellent apatite forming
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energy saving, purity and homogeneity. The combustion-

abilities in stimulated body fluids. Other studies showed that
derived powders have narrow size distribution with average
these silicate ceramics also possess good in vivo bioactivity [9-
agglomerate particle sizes in the range of 0.5-5 μm. The fine
12]. In vitro and in vivo investigations of a calcium
particle nature of the combustion derived powder is attributed
magnesium silicate (Ca2MgSi2O7) bioceramic for bone
to the low exothermicity of the combustion reaction and
regeneration showed that akermanite extract promoted
evolution of large amount of gases (NH3, H2O, CO2), which
proliferation and osteogenic differentiation These results
help to dissipate the heat thereby preventing the oxides from
suggest that akermanite might be a potential and attractive
sintering.
bioceramic for tissue engineering [13-16]. A bioactive,
degradable, and cytocompatible akermanite (Ca2MgSi2O7)
scaffold with high porosity (63.5-90.3%) and pore
interconnectivity with a corresponding compressive strength
between 1130 and 530 kPa has been reported [17].

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Vol No. 5, Issue No. 2, 184 -186

II. MATERIALS AND METHODS have akermanite structure. In this type of structure there is one
calcium or strontium site, which is coordinated by eight
In this study (Ca2-x Srx)MgSi2O7: Eu2+ with x- values 0, 0.5,
oxygen ions. The review of the data from the earlier studies
1.5 and 2 were synthesised by combustion method. The
[24, 25] on the nature of emission and the decay time for these
detailed description of the methods can be found in our earlier
works [21, 22]. Ingredients used were metal carbonates, Silicic phosphors, are summarized in Table 2.
acid (SiO2.xH2O), and the dopant salts. The dopant europium TABLE II. REVIEW OF THE DATA (NATURE OF EMISSION AND THE
concentration was 2 mole % of the AE ion. The equivalent DECAY TIME)
amount of Eu2O3 was dissolved in 3M nitric acid for this
S/ Name of the Emission Emission T50 Decay Reference
purpose. Urea was used as a fuel and ammonium nitrate as N compound Peak Peak(nm) (K) time (μs)
oxidizer. Fuel to oxidizer ratio, optimised as described by (nm)* @
Bhatkar et. al., [21, 22] was used. The details of the molar ratio 1 Ca2MgSi2O7: Eu 2+
535 475 bb 285 0.2 Blasse1968
of ingredients used in the synthesis of all compounds are given 545 280 1.1 Poort 1997
2 Ca1.5Sr0.5MgSi2O7: 525 448 280 1.0 Poort 1997
in Table 1. Eu2+
3 Ca0.5Sr1.5MgSi2O7: 490 450 280 0.8 Poort 1997
TABLE I. DETAILS OF THE MOLAR RATIO OF INGREDIENTS Eu2+
4 Sr2MgSi2O7: Eu2+ 470 457 305 0.3 Blasse1968
475 300 0.7 Poort 1997
S/N Name of the Starting Materials
compound @ This work for PL measurements at room temperature. * Literature values at 4.2 K
1 Ca2MgSi2O7: Eu2+ CaCO3, SiO2.xH2O Eu NH4NO3 UREA G. Blasse, et al., Philips Res. Repts, 23, 189, 1968.

T
S. M. H Poort,., et al., J. Phys. Chem. Solid., 58, 1451, 1997
Mg(NO3)2 (NO3)2
Mole ratio:-> 1.96, 2 0.04 30 35
1 The PL properties of individual compounds are discussed
2 Ca1.5Sr0.5MgSi2O7:
2+
CaCO3, SiO2.xH2O Eu NH4NO3 UREA below:
Eu SrCO3, (NO3)2
Mg(NO3)2 Fig. 1 shows the excitation spectra for Ca2MgSi2O7:Eu2+,
Mole ratio:-> 1.46, 0.5, 2 0.04 30 35 Ca1.5Sr0.5MgSi2O7:Eu2+, Ca0.5Sr1.5MgSi2O7:Eu2+, and
1,
3 Ca0.5Sr1.5MgSi2O7:
Eu2+

Mole ratio:->
CaCO3,
SrCO3,
Mg(NO3)2
0.5, 1.46,
1,
SiO2.xH2O

2
ES
Eu
(NO3)2

0.04
NH4NO3 UREA

30 35
2+
Sr2MgSi2O7:Eu . The emission spectra are shown in fig. 2.
Efficient excitation by 385 nm, was observed for Eu2+ doped
disilicates as seen from fig. 1. The emission spectrum of
Ca2MgSi2O7:Eu2+, (curve a), is a broad band at 475 nm.
4 Sr2MgSi2O7: Eu2+ SrCO3, SiO2.xH2O Eu NH4NO3 UREA Ca1.5Sr0.5MgSi2O7:Eu2+ (curve b) exhibit blue emission around
Mg(NO3)2 (NO3)2 448 nm. Emission in Ca0.5Sr1.5MgSi2O7:Eu2+ (curve c) peaks at
Mole ratio:-> 1.96, 2 0.04 30 35 450 nm. Emission in Sr 2MgSi2O7:Eu2+ (curve d) peaks around
1 457 nm.
All constituents in stoichiometric proportions, along with
fuel and oxidizer were mixed together and small quantity of
double distilled water was added. The mixture on thoroughly
A
mixing was transferred to a pre-heated furnace at 500 oC. On
rapid heating the mixture evaporates and ignites at 450 oC, with
the evolution of a large amount of gases, to yield silicates.
Entire process completes within few minutes. The as-prepared
phosphors did not show intense emission, probably the
activator Eu is not incorporated in divalent form. The
phosphors were reheated, in the reducing atmosphere provided
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by heating in a closed box with charcoal, at 900 oC for 1 hour.

Photoluminescence spectra were recorded on Hitachi F-4000
spectro-fluorimeter with spectral slit width of 1.5 nm, at room
temperature. To confirm the structure of the synthesized
phosphors, powder photographs were obtained using Philips
diffractometer, PW 1710.
III. RESULTS AND DISCUSSION
Akermanite belongs to the Tetragonal crystal system with Figure 1, PL spectra for Eu2+ doped disilicate phosphors
Space Group, P421m where a = 7.8288, c = 5.0052, Z = 2 and
point group 42m. It is optically transparent to translucent and a) (Red) Ca2MgSi2O7 excitation for 447 nm emission
colorless. The X-ray powder pattern is characterized by strong b) (Blue) Ca1.5Sr0.5MgSi2O7 excitation for 448 nm emission
c) (Black) Ca0.5Sr1.5MgSi2O7 excitation for 478 nm emission
lines at 2.87 (100), 3.09 (30), 1.764 (30), 2.039 (20), 2.488 d) (Green) Sr2MgSi2O7 excitation for 460 nm emission.
(18), 3.73 (14), 5.55 (12). Both Ca2MgSi2O7 and Sr2MgSi2O7

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 V.B. Bhatkar et al. / (IJAEST) INTERNATIONAL JOURNAL OF ADVANCED ENGINEERING SCIENCES AND TECHNOLOGIES
100
80
Intensity (arb.units)
60
40
20
0 “Preparation and in vitro bioactivity of novel merwinite ceramic”,
400 450
Wavelength (nm)
Figure 2. PL spectra for Eu2+ doped disilicate phosphors
a) (Black) Ca2MgSi2O7 emission for 385 nm excitation
b) (Green) Ca1.5Sr0.5MgSi2O7 emission for 385 nm excitation
c) (Blue) Ca0.5Sr1.5MgSi2O7 emission for 385 nm excitation
d) (Red) Sr2MgSi2O7 emission for 385 nm excitation
Excitation spectrum of all the samples (Fig 1, curves a-d)
shows considerable intensity at 385 nm. At room temperature
the intensity of emission, except for Sr2MgSi2O7:Eu2+ is
considerably quenched, which is consistent with the literature
data. The luminescence process of Eu2+-activated phosphor is
characterized by the 4f6 5d→4f7 transition of Eu2+ acting as an
activator center. The absorption and emission due to the
transition between 4f7 and 4f6 5d states of Eu2+, strongly depend
on host material cations replaceable by Eu2+ in the host matrix
and the crystal field acting on Eu2+.
A
IV. CONCLUSIONS
Both Ca2MgSi2O7:Eu2+ and Sr2MgSi2O7:Eu2+ has
akermanite structures. The combustion synthesis using urea
and ammonium nitrate is the easy, time saving and cost
effective method for the synthesis. The photoluminescence
study of these materials shows the strong emission of Eu 2+ in
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alkaline earth silicates which agrees well with the literature.
The biocompatibility of the akermanite has already been
reported by many researchers. The luminescence properties of
these biomaterials may be useful in their use as biomarkers
and in the controlled drug delivery.
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