Articles written in Bulletin of Materials Science
Volume 23 Issue 2 April 2000 pp 135-140 Biomaterials
Development of an apatitic calcium phosphate bone cement is reported. 100 μ Particles of tetracalcium phosphate (TTCP) and dicalcium phosphate dihydrate (DCPD) were mixed in equimolar ratio to form the cement powder. The wetting medium used was distilled water with Na2HPO4 as accelerator to manipulate the setting time. The cement powder, on wetting with the medium, formed a workable putty. The setting times of the putty were measured using a Vicat type apparatus and the compressive strength was determined with a Universal Testing Machine. The nature of the precipitated cement was analyzed through X-ray diffraction (XRD), fourier transform infrared spectrometry (FTIR) and energy dispersive electron microprobe (EDAX). The results showed the phase to be apatitic with a calcium-to-phosphorous ratio close to that of hydroxyapatite. The microstructure analysis using scanning electron microscopy (SEM) showed hydroxyapatite nano-crystallite growth over particulate matrix surface. The structure has an apparent porosity of ∼ 52%. There were no appreciable dimensional or thermal changes during setting. The cement passed the in vitro toxicological screening (cytotoxicity and haemolysis) tests. Optimization of the cement was done by manipulating the accelerator concentration so that the setting time, hardening time and the compressive strength had clinically relevant values.
Volume 26 Issue 4 June 2003 pp 415-422 Biomaterials
A study on the development of a fully injectable calcium phosphate cement for orthopedic and dental applications is presented. The paper describes its characteristic properties including results of bio- compatibility studies.
A conventional two-component calcium phosphate cement formulation (having a powder part containing dry mixture of acidic and basic calcium phosphate particles and a liquid part containing phosphate solution) is modified with a biocompatible gelling agent, to induce flow properties and cohesion. The quantity of the gelling agent is optimized to get a viscous paste, which is smoothly injectable through an 18-gauge needle, with clinically relevant setting parameters.
The new formulation has a setting time of 20 min and a compressive strength of 11 MPa. The X-ray diffraction, Fourier transform infrared spectrometry, and energy dispersive electron microprobe analyses showed the phase to be hydroxyapatite, the basic bone mineral. Scanning electron microscopy revealed a porous structure with particle sizes of a few micrometers. The cement did not show any appreciable dimensional or thermal change during setting. The injectability is estimated by extruding through needle and the cohesive property is assessed by water contact method. The cement passed the in vitro biocompatibility screening (cytotoxicity and haemolysis) tests.
Volume 30 Issue 5 October 2007 pp 527-534 Thermal Properties
The suitability of calcium phosphate crystals for thermoluminescence dosimetry (TLD) applications is investigated, owing to their equivalence to bone mineral. The 𝛼 and 𝛽 phases of tricalcium phosphate (TCP) were synthesized through wet precipitation and high temperature solid state routes and doped with Dy and Eu. The photoluminescence and thermoluminescence studies of the phosphors have been carried out.
The TL properties were found to be highly dependent on the method of preparation of the material. Eu doping gave good PL emission, whereas Dy doping was more efficient in TL emission. 𝛽-TCP was found to be less TL sensitive than 𝛼-TCP, yet it was identified as a better phosphor material owing to its better fading characteristics.
The dependence of TL of 𝛽-TCP : Dy on the energy and dose of radiation, and on the doping concentration were studied. The TL intensity was observed to fade exponentially during a storage period of 20 days, but it stabilized at 70% of the initial value after 30 days. The optimum doping concentration was found to be 0.5 mol%.
Volume 34 Issue 2 April 2011 pp 389-399
Pulsed laser deposition (PLD) has emerged as an acceptable technique to coat hydroxyapatite on titanium-based permanent implants for the use in orthopedics and dentistry. It requires substrate temperature higher than 400°C to form coatings of good adhesion and crystallinity. As this range of temperatures is likely to affect the bulk mechanical properties of the implant, lowering the substrate temperature during the coating process is crucial for the long-term performance of the implant. In the present study, hydroxyapatite target was ablated using a pulsed Nd:YAG laser (355 nm) onto commercially pure titanium substrates kept at 200°C. The coating thus obtained has been subjected to hydrothermal treatment at 200°C in an alkaline medium. The coatings were analysed using microscratch test, optical profilometry, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and infrared spectroscopy (FTIR). XRD, EDS and FTIR showed that the as-deposited coating contained amorphous calcium phosphate and the hydrothermal treatment converted it into crystalline hydroxyapatite. The micro-morphology was granular, with an average size of 1 micron. In the microscratch test, a remarkable increase in adhesion with the substrate was seen as a result of the treatment. The plasma plume during the deposition has been analysed using optical emission spectroscopy, which revealed atomic and ionic species of calcium, phosphorous and oxygen. The outcomes demonstrate the possibility of obtaining adherent and crystalline hydroxyapatite on titanium substrate at 200°C through pulsed laser deposition and subsequent hydrothermal treatment.
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