Structural characterisation of apatite coatings

The current, most frequently employed, commercial route to produce hydroxyapatite prosthetic coatings is plasma spraying. However, this has several important limitations especially for textured surfaces. Low temperature methods of coating fabrication such as cathodic electrodeposition are attractive alternatives. However, quantitative characterisation of the phase composition of thin electrodeposited coatings can be problematic. An X-ray diffraction method, which provides quantitative compositional information without reference to external or internal standards, is introduced and validated. The method can also be applied when Bragg peaks from the supporting substrate are apparent within the data and preferred orientation can be tolerated. This method has been used to examine in detail the microstructure of electrodeposited coatings which are compared directly with those formed by a commercial plasma spraying process.We show that, unlike the plasma sprayed coatings, the electrodeposited material consists of a single crystalline phase (hydroxyapatite) and a significantly reduced amorphous phase. The electrodeposited coatings also possess significantly more microstrain and a smaller crystallite size than the corresponding plasma sprayed material.     

On the stabilizing behavior of zirconia: A Combined experimental and theoretical study

Reactive zirconia powder was synthesized by the complexation of zirconium metal from zirconium hydroxide using a solution of 8-hydroxiquinoline. The kinetics of zirconia crystallization was followed by X-ray diffraction, scanning electron microscopy and surface area measured by the nitrogen adsorption/desorption technique. The results indicated that zirconia with a surface area as high as 100 m²/g can be obtained by this method after calcination at 500°C. Zirconia presents three polymorphic phases (monoclinic, tetragonal and cubic), which are reversibly interconversible. The cluster model Zr₄O₈ and Zr₄O₇ ⁺² was used for a theoretical study of the stabilization process. The ab initio RHF method was employed with the Gaussian94 program and the total energies and the energy gap of the different phases were calculated and compared with the experimental energy gap. The theoretical results show good reproducibility of the energy gap for zirconia.