Importance of FTIR spectra deconvolution for the analysis of amorphous calcium phosphates

Publisher Copyright: © Published under licence by IOP Publishing Ltd. Copyright: Copyright 2015 Elsevier B.V., All rights reserved.This work will consider Fourier transform infrared spectroscopy-diffuse reflectance infrared reflection (FTIR-DRIFT) for collecting the spectra and deconvolution to identify changes in bonding as a means of more powerful detection. Spectra were recorded from amorphous calcium phosphate synthesized by wet precipitation, and from bone. FTIR-DRIFT was used to study the chemical environments of PO4, CO3 and amide. Deconvolution of spectra separated overlapping bands in the 4PO4, 2CO3, 3CO3 and amide region allowing a more detailed analysis of changes at the atomic level. Amorphous calcium phosphate dried at 80 oC, despite showing an X-ray diffraction amorphous structure, displayed carbonate in positions resembling a carbonated hydroxyapatite. Additional peaks were designated as A1 type, A2 type or B type. Deconvolution allowed the separation of CO3 positions in bone from amide peaks. FTIR-DRIFT spectrometry in combination with deconvolution offers an advanced tool for qualitative and quantitative determination of CO3, PO4 and HPO4 and shows promise to measure the degree of order.publishersversionPeer reviewe

Production and Characterization of Oxyhydroxyapatites

The amount and alignment of hydroxyl ions influence the bioactivity of hydroxyapatite. Hydroxyl ions in hydroxyapatite are the most mobile and upon heating are the first to leave the lattice to form oxyhydroxyapatite. This work describes a method for producing hydroxyapatite with different amounts of hydroxyl ions, and reports on the changes in Fourier transform infrared absorption at increasing level of dehydroxylation. Detailed analysis of spectra in the 500 – 700 cm-1 range showed a peak shift for the hydroxyl ion absorption line at 632 cm-1 to 637 cm-1 and an increase in the wavenumber for the phosphate line at 575 cm-1

Surface Hierarchy: Macroscopic and Microscopic Design Elements for Improved Sliding on Ice

Frictional interaction with a surface will depend on the features and topography within the contact zone. Describing this interaction is particularly complex when considering ice friction, which needs to look at both the macroscopic and microscopic levels. Since Leonardo da Vinci shared his findings that roughness increases friction, emphasis has been placed on measuring surface coarseness, neglecting the contact area. Here, a profilometer was used to measure the contact area at different slicing depths and identify contact points. Metal blocks were polished to a curved surface to reduce the contact area; further reduced by milling 400 µm grooves or laser-micromachining grooves with widths of 50 µm, 100 µm, and 150 µm. Sliding speed was measured on an inclined ice track. Asperities from pileup reduced sliding speed, but a smaller contact area from grooves and a curved sliding surface increased sliding speed. An analysis of sliding speed versus contact area from incremental slicing depths showed that a larger asperity contact surface pointed to faster sliding, but an increase in the polished surface area reduced sliding. As such, analysis of the surface at different length scales has revealed different design elements—asperities, grooves, curved zones—to alter the sliding speed on ice

Structural and Chemical Hierarchy in Hydroxyapatite Coatings

Hydroxyapatite coatings need similarly shaped splats as building blocks and then a homogeneous microstructure to unravel the structural and chemical hierarchy for more refined improvements to implant surfaces. Coatings were thermally sprayed with differently sized powders (20-40, 40-63 and 63-80 m) to produce flattened homogeneous splats. The surface was characterized for splat shape by profilometry and AFM, crystal size by AFM, crystal orientation by X-ray diffraction (XRD) and structural variations by XRD. Chemical composition was assessed by phase analysis, but variations in chemistry were detected by XRD and Raman spectroscopy. The resulting surface electrical potential was measured by Kelvin probe AFM. Five levels of structural hierarchy were suggested: the coating, the splat, oriented crystals, alternate layers of oxyapatite and HAp, and the suggested anion orientation. Chemical hierarchy was present over a lower range of order for smaller splats. Coatings made from smaller splats exhibited a greater electrical potential, inferred to arise from oxyapatite, and supplemented by ordered OH- ions in a rehydroxylated surface layer. A model has been proposed to show the influence of structural hierarchy on the electrical surface potential. Structural hierarchy is proposed as a means to further refine the properties of implant surfaces