Phase transitions in single phase Si–Ca–P-based ceramic under thermal treatment

Abstract The influence of thermal treatment on phase transformations of Si–Ca–P (Nurse's A ss ) single phase ceramic was investigated. The results showed that the phase evolution during the synthesis of ceramic was influenced by the type of raw materials used. While annealing within the 1000–1500 °C range for 2 h, the interdiffusion of silica and phosphorous took place. Different polymorphs appeared at lower temperatures than that observed in pure compounds, and different intermediate phases also appeared in the samples. The obtained results allowed us to conclude that the formation of a single phase ceramic with a Ca 2 SiO 4 /Ca 3 (PO 4 ) 2 molar ratio equal to 2/1 is a complex slow process. In order to optimise the synthesis conditions, two-step synthesis conditions were used: firstly, heating at 1550 °C/3 h then liquid-nitrogen was quenched, ground and pressed; secondly, heating at 1300 °C/3 h and subsequent annealing at 1200 °C for 24 h.

[1]  M. Lombardi,et al.  Si-substituted hydroxyapatite nanopowders: synthesis, thermal stability and sinterability , 2009 .

[2]  M. Bredig Isomorphism and allotropy in compounds of the type A_2XO_4 , 1942 .

[3]  R. Cuscó,et al.  Hydration and carbonation of monoclinic C2S and C3S studied by Raman spectroscopy , 2007 .

[4]  Zhang Zhenxi,et al.  Investigation of Phase Evolution During the Thermochemical Synthesis of Tricalcium Phosphate , 2001 .

[5]  P. Aza,et al.  Materiales biocerámicos cristalinos , 2005 .

[6]  P. Velásquez,et al.  Synthesis and stability of α-tricalcium phosphate doped with dicalcium silicate in the system Ca3(PO4)2–Ca2SiO4 , 2010 .

[7]  M. Sayer,et al.  Structure and composition of silicon-stabilized tricalcium phosphate. , 2003, Biomaterials.

[8]  M. Sayer,et al.  Synthesis and characterization of single-phase silicon-substituted α-tricalcium phosphate , 2006 .

[9]  R. Frank,et al.  Untersuchungen über Kalk‐Alkaliphosphate. I. Ein Beitrag zur Kenntnis des Rhenaniaphosphates , 1936 .

[10]  M. Bredig,et al.  Untersuchungen Über Kalk‐Alkali‐Phosphate. II. Über Calcium‐Kalium‐Phosphate , 1938 .

[11]  M. Bredig Isomorphism and allotrophy in compounds of the type A2XO4 , 1942 .

[12]  R. Cuscó,et al.  Vibrational Properties of Calcium Phosphate Compounds. 2. Comparison between Hydroxyapatite and β-Tricalcium Phosphate , 1997 .

[13]  Piedad N. De Aza,et al.  The System Ca3(PO4)2–Ca2SiO4: The Sub-System Ca2SiO4–7CaOP2O52SiO2 , 2011 .

[14]  F. Puertas,et al.  Examinations by infra-red spectroscopy for the polymorphs of dicalcium silicate , 1985 .

[15]  J. Chevalier,et al.  Ceramics for medical applications: A picture for the next 20 years , 2009 .

[16]  H. Heymann,et al.  Subsolidus Relations in the System 2CaO·SiO2‐3CaO·P2O5 , 1969 .

[17]  P. N. Aza,et al.  Vibrational Properties of Calcium Phosphate Compounds. 1. Raman Spectrum of β-Tricalcium Phosphate , 1997 .

[18]  M. Sitarz,et al.  Vibrational spectra of phosphate–silicate biomaterials , 2003 .

[19]  P. Velásquez,et al.  The Sub‐System α‐TCPss‐Silicocarnotite Within the Binary System Ca3(PO4)2–Ca2SiO4 , 2011 .

[21]  W. Bonfield,et al.  Chemical characterization of silicon-substituted hydroxyapatite. , 1999, Journal of biomedical materials research.

[22]  R. A. Condrate,et al.  The Infrared and Raman Spectra of β-and α-Tricalcium Phosphate (Ca3(Po4)2) , 1998 .

[23]  D. Sheptyakov,et al.  Silicon Location in Silicate-Substituted Calcium Phosphate Ceramics Determined by Neutron Diffraction , 2011 .

[24]  S. Ghosh,et al.  The chemistry of dicalcium silicate mineral , 1979 .

[25]  Matthias Epple,et al.  Biological and medical significance of calcium phosphates. , 2002, Angewandte Chemie.

[26]  M. Bredig High-temperature Crystal Chemistry of AmBXn Compounds with Particular Reference to Calcium Orthosilicate , 1945 .

[27]  L. Meseguer-Olmo,et al.  Production and study of in vitro behaviour of monolithic α-tricalcium phosphate based ceramics in the system Ca3(PO4)2–Ca2SiO4 , 2011 .

[28]  B. Reynard,et al.  Raman Spectroscopic Investigations of Dicalcium Silicate: Polymorphs and High‐Temperature Phase Transformations , 2005 .

[29]  X. Turrillas,et al.  New Approach to the β→α Polymorphic Transformation in Magnesium-Substituted Tricalcium Phosphate and its Practical Implications , 2008 .