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].
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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),
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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
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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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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.
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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
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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
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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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vivo evaluation of akermanite bioceramics for bone regeneration”.
Figure 2. PL spectra for Eu2+ doped disilicate phosphors Biomaterials.; 30(28):5041-8, 2009.
[11] S. Xu, Lin K, Wang Z, Chang J, Wang L, Lu J, et al.; “Reconstruction of
a) (Black) Ca2MgSi2O7 emission for 385 nm excitation calvarial defect of rabbits using porous calcium silicate bioactive
b) (Green) Ca1.5Sr0.5MgSi2O7 emission for 385 nm excitation ceramics”. Biomaterials. 29(17):2588–96, 2008.
c) (Blue) Ca0.5Sr1.5MgSi2O7 emission for 385 nm excitation [12] T. Nonami, Tsutsumi S.; “Study of diopside ceramics for biomaterials”.
d) (Red) Sr2MgSi2O7 emission for 385 nm excitation J Mater Sci Mater Med. 10(8):475–9, 1999.
[13] H.Yan, J. Xiaogang, Z. Xiaoling, S. Hongli, T. Jinwen, T. Tingting, C.
alkaline earth silicates which agrees well with the literature. [19] C. Wu, J. Chang, “A Novel Akermanite Bioceramic: Preparation and
Characteristics”, Journal of biomaterials applications, 21(2): 119-129,
The biocompatibility of the akermanite has already been 2006.
reported by many researchers. The luminescence properties of [20] C. Wu, and J. Chang,; “Synthesis and apatite-formation ability of
these biomaterials may be useful in their use as biomarkers akermanite”, Materials Letters, 58 (19): 2415-2417, 2004.
and in the controlled drug delivery. [21] V.B. Bhatkar, S.K.Omanwar, and S.V.Moharil, “Combustion Synthesis
of Zn2SiO4:Mn phosphor”, Phys. Stat. Sol. (a) 191, No.1, 272-276,
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