In vitro testing of Nd:YAG laser processed calcium phosphate coatings.

Nd:YAG laser cladding is a new method for deposition of a calcium phosphate onto metallic surfaces of interest in implantology. The aim of this study was to compare the biologic response of MG-63 human osteoblast-like cells grown on Ti-6Al-4V substrates coated with a calcium phosphate layer applied using different methods: plasma spraying as reference material and Nd:YAG laser cladding as test material. Tissue culture polystyrene was used as negative control. The Nd:YAG laser clad material showed a behaviour similar to the reference material, plasma spray, respective to cell morphology (SEM observations), cell proliferation (AlamarBlue assay) and cytotoxicity of extracts (MTT assay). Proliferation, as measured by the AlamarBlue assay, showed little difference in the metabolic activity of the cells on the materials over an 18 day culture period. There were no significant differences in the cellular growth response on the test material when compared to the ones exhibited by the reference material. In the solvent extraction test all the extracts had some detrimental effect on cellular activity at 100% concentration, although cells incubated in the test material extract showed a proliferation rate similar to that of the reference material. To better understand the scope of these results it should be taken into account that the Nd:YAG clad coating has recently been developed. The fact that its in vitro performance is comparable to that produced by plasma spray, a material commercially available for more than ten years, indicates that this new laser based method could be of commercial interest in the near future.

New biomorphic SiC ceramics coated with bioactive glass for biomedical applications.

A new generation of light, tough and high-strength material for medical implants for bone substitutions with a good biological response is presented. The innovative product that fulfills all these requirements is based on biomorphic silicon carbide ceramics coated with a bioactive glass layer. The combination of the excellent mechanical properties and low density of the biomorphic SiC ceramics, used as a base material for implants, with the osteoconducting properties of the bioactive glass materials opens new possibilities for the development of alternative dental and orthopedic implants with enhanced mechanical and biochemical properties that ensures optimum fixation to living tissue. Biomorphic SiC is fabricated by molten-Si infiltration of carbon templates obtained by controlled pyrolysis of wood. Through this process, the microstructure of the final SiC product mimics that of the starting wood, which has been perfected by natural evolution. The basic features of such microstructure are its porosity (ranging from 30% to 70%) and its anisotropy, which resembles the cellular microstructure and the mechanical characteristics of the bone. The SiC ceramics have been successfully coated with a uniform and adherent bioactive glass film by pulsed laser ablation using an excimer ArF laser. The excellent coverage of the SiC rough surface without film spallation or detachment is demonstrated. In order to assess the coating bioactivity, in vitro tests by soaking the samples in simulated body fluid have been carried out. After 72 h, the formation of a dense apatite layer has been observed even in interconnecting pores by SEM and energy dispersive X-ray spectroscopy analysis demonstrating the bioactive response of this product.

Micro- and nano-testing of calcium phosphate coatings produced by pulsed laser deposition.

Micro- and nano-testing methods have been explored to study the thin calcium phosphate coatings with high adhesive strength. The pulsed laser deposition (PLD) technique was utilised to produce calcium phosphate coatings on metal substrates, because this type of coatings exhibit much higher adhesive strength with substrates than conventional plasma-sprayed coatings. Due to the limitations of the conventional techniques to evaluate the mechanical properties of these thin coatings (1 microm thick), micro-scratch testing has been applied to evaluate the coating-to-substrate adhesion, and nano-indentation to determine the coating hardness and elastic modulus. The test results showed that the PLD produced amorphous and crystalline HA coatings are more ductile than titanium substrates, and the PLD coatings are not delaminated from the substrates by scratch. Also, the results showed that the crystalline HA coating is superior in internal cohesion to the amorphous one, even though the lower elastic modulus of amorphous coating could be more mechanically compatible with natural bone.

Calcium phosphate coatings obtained by Nd:YAG laser cladding: physicochemical and biologic properties.

The plasma spray (PS) technique is the most popular method commercially in use to produce calcium phosphate (CaP) coatings to promote fixation and osteointegration of the cementless prosthesis. Nevertheless, PS has some disadvantages, such as the poor coating-to-substrate adhesion, low mechanical strength, and brittleness of the coating. In order to overcome the drawbacks of plasma spraying, we introduce in this work a new method to apply a CaP coating on a Ti alloy using a well-known technique in the metallurgical field: laser surface cladding. The physicochemical characterization of the coatings has been carried out by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray analysis (EDX). The biologic properties of the coatings have been assessed in vitro with human osteoblast-like MG-63 cells. The overall results of this study affirm that the Nd:YAG laser cladding technique is a promising method in the biomedical field.

Alloying of hydroxyapatite onto Ti6Al-4V by high power laser irradiation.

In the biomedical field, the synthetic hydroxyapatite [Ca(10)(PO)(4)(OH)(2)], with similarity to the inorganic component of bone but brittle, has been considered as the appropriate coating on stronger implant materials, such as metallic implants, for presenting a surface which is conductive to bone formation. Many industrial and laboratory techniques were developed to apply hydroxyapatite onto metallic substrates, such as electrophoretic deposition, ion sputtering, hot isostatic pressing, pulsed laser deposition and the only widely used method commercially available: plasma spraying. This work presents a new approach on how to bind calcium phosphate (CaP) to the Ti alloy with a well-known technique in the metallurgical field: laser surface alloying, in order to overcome the drawbacks of plasma spraying. The analysis of the results obtained and the description of the phenomena that take place in the coating process will complete this explorative study.

Influence of the non-bridging oxygen groups on the bioactivity of silicate glasses.

The effect of the composition and bonding configuration of the bioactive silica-based glasses on the initial stage in vitro bioactivity is presented. Information of the IR active Si-O groups of glass in the system SiO(2)-P(2)O(5)-CaO-Na(2)O-K(2)O-MgO-B(2)O(3) was obtained by fourier transform Infrared (FTIR) spectroscopy. Two different bands associated to non-bridging oxygen stretching vibrations (Si-O-1NBO and Si-O-2NBO) and a gradual shifting of the bridging oxygen stretching vibration (Si-O) have been observed and evaluated. Both effects are attributed to a decrease of the local symmetry originating from the incorporation of alkali ions into the vitreous silica network. The Si-O-NBO(s)/Si-O(s) absorbance intensity ratio increases with a gradual incorporation of the alkali ions (diminution of SiO(2) content) following a linear dependence up to values close to 50 wt % of SiO(2). In vitro test analysis by scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDXA) showed a correlation between the amount and type of the non-bridging oxygen functional groups and the growth of the silica-rich and CaP layers. It was found that a minimum concentration of Si-O-NBO bonds in the glass network is required in order to have an efficient ion exchange and dissolution of the silica network. Finally, the bioactivity of the glass is favored by the presence of the Si-O-2NBO groups in the glassy network. The role of these functional groups in the dissolution of the silica network through the formation of silanol groups and the adsorption of water is discussed.

Enhancing the sensitivity to small phase changes in double-exposure stroboscopic television holography.

We present a new technique for enhancing the sensitivity of double-exposure stroboscopic television holography (TVH) to detect and measure vibrations of small amplitude. The technique is based in the modulation of the phase of the reference beam in synchronism with the vibration of the measurand and derives from a former technique that we originally contrived for phase evaluation. We propose two variants, characterized by the demodulation process used to generate the secondary correlograms, with different behaviors in terms of the sensitivity to the sign of the measurand and of the ease in detecting the presence and shape of the vibration. We have implemented this new technique in an electronic speckle-pattern interferometer and compared its performance with standard TVH techniques; vibrations with amplitudes as small as 8 nm have been observed with this setup.

Physicochemical properties of calcium phosphate coatings produced by pulsed laser deposition at different water vapour pressures.

Calcium phosphate coatings were produced by pulsed laser deposition from targets of non-stoichiometric hydroxyapatite (Ca/P = 1.70) at a substrate temperature of 485 degrees C and different processing pressures of water vapour: 0.15, 0.30, 0.45, 0.60 and 0.80 mbar. The physicochemical properties of these coatings were studied using Fourier-transform IR spectroscopy (FT-IR) and energy dispersive X-ray analysis (EDX). A minimum pressure of water vapour was necessary in order to obtain a crystalline coating, as deduced from the FT-IR spectroscopy of these coatings. This analysis also revealed that when the deposition pressure of water vapour was further increased, the coatings were less crystalline and the content of hydroxyl groups, the carbonate substitution for phosphate, and the Ca/P ratio, as measured by EDX, were lower. These effects can be explained by a combined substitution of carbonate and HPO4(2-) for phosphate, being predominant the carbonate substitution at low pressures and the HPO4(2-) substitution at high pressures.

Effect of heat treatment on pulsed laser deposited amorphous calcium phosphate coatings.

Amorphous calcium phosphate coatings were produced by pulsed laser deposition from targets of nonstoichiometric hydroxyapatite (Ca/P = 1.70) at a low substrate temperature of 300 degrees C. They were heated in air at different temperatures: 300, 450, 525 and 650 degrees C. Chemical and structural analyses of these coatings were performed using X-ray diffraction (XRD), FTIR, and SEM, XRD analysis of the as-deposited and heated coatings revealed that their crystallinity improved as heat treatment temperature increased. The main phase was apatitic, with some beta-tricalcium phosphate in the coatings heated at 525 and 600 degrees C. In the apatitic phase there was some carbonate substitution for phosphate and hydroxyl ions at 450 degrees C and almost solely for phosphate at 525 and 600 degrees C as identified by FTIR. This was accompanied by a higher hydroxyl content at 525 and 600 degrees C. At 450 degrees C a texture on the coating surface was observable by SEM that was attributable to a calcium hydroxide and calcite formation by XRD. These phases almost disappeared at 600 degrees C, probably due to a transformation into calcium oxide.

Multiplicative moiré two-beam phase-stepping and fourier-transform methods for the evaluation of multiple-beam fizeau patterns: a comparison.

A phase-evaluation method of multiple-beam Fizeau patterns that combines two-beam phase-stepping algorithms with the moiré effect was previously reported [Appl. Opt. 34, 3639-3643(1995)]. The method is based on a multiplicative moiréimage-formation process obtained by the direct superposition of high-frequency multiple-beam Fizeau carrier fringes upon a transmission grating (working as a phase modulator). We present a comparison between this multiplicative moiré two-beam phase-stepping method and the well-known Fourier-transform method for the topographic measurement of an undoped silicon wafer. The discrepancy between the two methods yields a rms phase-difference value of the order of(~2pi/90).

Transient Deformation Measurement by Double-Pulsed-Subtraction TV Holography and the Fourier Transform Method.

We report the measurement of transient bending waves with double-pulsed-subtraction TV holography. The correlation fringe patterns are automatically quantitatively analyzed by the application of Fourier methods. A novel optical setup with two different object-beam optical paths is demonstrated for the generation of carrier fringes. The proposed system is highly immune to environmental disturbances because the optical setup imposes no lower limit on the time separation between laser pulses. One removes the linear phase distribution due to the spatial carrier in the spatial domain by subtracting the phase of the undeformed carrier fringes from the phase of the modulated fringes. Experimental results obtained with an aluminum plate excited by the impact of a piezoelectric translator are presented.

Measurement range analysis in moiré evaluation Fizeau interferometry.

Fizeau interferograms are evaluated by two-beam phase-stepping algorithms. The sinusoidal intensity profile pattern needed for the application of these algorithms is obtained by low-pass filtering the moiré pattern provided by the superposition of the interferogram onto a Ronchi grid. The phase modulation is performed by the in-plane displacement of the grid by means of a motorized stage. In this research the measurement range of the evaluation method as a function of the maximum derivative of height surfaces is calculated. A spherical surface is measured in different configurations in order to verify the obtained results.

Hydroxyapatite coatings: a comparative study between plasma-spray and pulsed laser deposition techniques.

A comparative study between hydroxyapatite coatings produced by two different techniques, plasma spray (PS) and pulsed-laser deposition (PLD) was carried out. Plasma spray is currently commercially used for coating dental and orthopaedical implant devices, and pulsed-laser deposition (or laser-ablation deposition) gave good results in the field of high critical temperature superconductive thin films, and is being applied to produce calcium phosphate coatings for biomedical purposes. X-ray diffraction was used to control the crystallinity of the coatings, scanning electron microscopy for the surface and cross-sectional morphology, and the pull test to determine the tensile strength of the coatings. This study reveals that the pulsed-laser deposition technique appears to be a very good candidate to replace the plasma spray in many biomedical applications, because it overcomes most of the drawbacks of the plasma spray.

Structural analysis of calcium phosphate coatings produced by pulsed laser deposition at different water-vapour pressures.

Calcium phosphate coatings have been produced by pulsed laser deposition (PLD) at different water-vapour pressures. Rietveld refinement of X-ray diffraction (XRD) data allows us to determine that the structure of these coatings is apatitic with carbonate substitution for phosphate. The carbonate substitution decreases when the chamber pressure is raised, a fact that has been corroborated by Fourier transform-infrared (FT-IR) spectroscopy. Carbonate concentrations between 5 and 17 wt% have been calculated for the crystalline samples. Amorphous coatings are produced at the lowest and highest pressures due to the high carbonate concentration in the first case, and possibly to another type of substitution (Mg(2+), HPO(2-)4, P2O(4-)7) or the inherent kinetics of the PLD process, in the second case.

Phase error calculation in a Fizeau interferometer by Fourier expansion of the intensity profile.

The spectrum of the intensity profile of multiple-beam Fizeau interferograms is presented. Knowledge of this spectrum provides valuable information about the characteristics of Fizeau interferograms, allowing one to calculate the phase error when the Fizeau profile is evaluated by means of two-beam phase-stepping algorithms, as is usual for low-reflectivity coefficients.

Fizeau phase-measuring interferometry using the moiré effect.

The automation of the fringe pattern analysis in Fizeau interferometry combining the moiré effect with the phase-stepping evaluation method is presented. In this case the phase modulator is a Ronchi grid placed at the interferometer image plane yielding a moiré image, and the necessary phase steps are obtained, simply translating the grid in its own plane, perpendicular to the optical axis. A detailed description of the moiré image formation as an incoherent superposition is developed. Measurements were carried out in a Fizeau interferometer built by the authors, and rms repeatabilities of less than 3 deg in the phase-difference values were attained.

Fringe localization control in holographic interferometry.

The practical use of holographic interferometry in nondestructive testing leads to many situations in which the characteristics of the fringe patterns make the observation and subsequent interpretation of the fringes difficult. Fringe control may then be employed to correct the troublesome parameters, the most commonly treated of which is fringe spacing. To gain more powerful control, a novel method is presented here that also permits one to change the localization of the fringe pattern. General vectorial expressions are derived that relate a tilt in the reference beam to a change in the fringe localization. Moreover the changes introduced into the fringe vector by this tilt can be suppressed by an adequate shift of the illumination beam focus. Some illustrative examples for a plane object are presented.

Annulling parasitic fringes in real time holographic interferometry: a new method.

A method for annulling parasitic fringes in real time holographicin terferometrya nd its theoreticalj ustification is presented. The main advantage relates to cancellation of nondesired object motions or deformations with experimental simplicity.