This paper reported a novel coating approach to deposit a (HA) film on Ti6Al4V alloy with Al2O3 buffer layer for thin, crack free and nano-structured hydroxyapatite biomedical implants. The Al2O3 buffer layer was de...This paper reported a novel coating approach to deposit a (HA) film on Ti6Al4V alloy with Al2O3 buffer layer for thin, crack free and nano-structured hydroxyapatite biomedical implants. The Al2O3 buffer layer was deposited by plasma spraying while the HA top layer was applied by dip coating technique. The X-ray diffraction (XRD) and Raman reflections of alumina buffer layer showed α- to γ-Al2O3 phase transformation; and the fractographic analysis of the sample revealed the formation of columnar grains in well melted splats. The bonding strength between Al2O3 coating and Ti6Al4V substrate was estimated to be about 40 MPa. The presence of dip coated HA layer was confirmed using XRD, scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) analysis. The SEM images exhibited that HA top layer enveloped homogenously the troughs and crests of the underneath rough (Ra = 2.91 μm) Al2O3 surface. It is believed that the novel coating approach adopted might render the implant suitable for rapid cement-less fixation as well as biocompatible for longer periods.展开更多
The carburizing of titanium (Ti) is accomplished by utilizing energetic ion pulses of a 1.5 kJ Mather type dense plasma focus (DPF) device operated in methane discharge. X-ray diffraction (XRD) analysis confirms...The carburizing of titanium (Ti) is accomplished by utilizing energetic ion pulses of a 1.5 kJ Mather type dense plasma focus (DPF) device operated in methane discharge. X-ray diffraction (XRD) analysis confirms the deposition of polycrystalline titanium carbide (TIC). The samples carburized at lower axial and angular positions show an improved texture for a typical (200)TIC plane. The Williamson-Hall method is employed to estimate average crystallite size and microstrains in the carburized Ti surface. Crystallite size is found to vary from - 50 to 100 nm, depending on the deposition parameters. Microstrains vary with the sample position and hence ion flux, and are converted from tensile to compressive by increasing the flux. The carburizing of Ti is confirmed by two major doublets extending from 300 to 390 cm^-1 and from 560 to 620 cm^-1 corresponding to acoustic and optical active modes in Raman spectra, respectively. Analyses by scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS) have provided qualitative and quantitative profiles of the carburized surface. The Vickers microhardness of Ti is significantly improved after carburizing.展开更多
AlON nanolayers are synthesized on Al substrate by the irradiation of energetic nitrogen ions using plasma focusing. Samples are exposed to multiple (5, 10, 15, 20 and 25) focus shots. Ion energy and ion number dens...AlON nanolayers are synthesized on Al substrate by the irradiation of energetic nitrogen ions using plasma focusing. Samples are exposed to multiple (5, 10, 15, 20 and 25) focus shots. Ion energy and ion number density range from 80 keV to 1.4 MeV and 5.6×10^19 m^- 3 to 1.3×10^19 m ^-3, respectively. Moreover, the effect of continuous annealing (473 K and 523 K) on an AlN surface layer synthesized with 25 focus shots is also examined. The main features of the X-ray diffraction (XRD) patterns with increasing focus shots are: (i) variation in the crystallinity of AlN along (111), (200) and (311) planes, (ii) increasing average crystallite size of AlN (111) plane, and (iii) stress relaxation observed in AlN (111) and (200) planes. The crystallinity of AlN surface layer is comparatively better at 473 K annealing temperature. A broadened diffraction peak related to an aluminium oxide phase showing weak crystallinity is observed for 15 focus shots while non-bounded oxides are present in all other deposited layers. Raman and Fourier transform infrared spectroscopy (FTIR) analysis confirm the presence of AlN and Al203 for the surface layer annealed at 473 K temperature. Raman analysis shows that the overlapping of AlN and Al2Oa results in the development of residual stresses. Scanning electron microscope (SEM) results demonstrate that the formation of rounded grains (range from 20 nm to 200 nm) and variations in their microstructures features depend on the increasing number of focus shots. Decomposition of larger clusters into smaller ones is observed.展开更多
The Al/a-C nanocomposite thin films are synthesized on Si substrates using a dense plasma focus device with alu- minum fitted anode and operating with CH4/Ar admixture. X-ray diffractometer results confirm the formati...The Al/a-C nanocomposite thin films are synthesized on Si substrates using a dense plasma focus device with alu- minum fitted anode and operating with CH4/Ar admixture. X-ray diffractometer results confirm the formation of metallic crystalline Al phases using different numbers of focus shots. Raman analyses show the formation of D and G peaks for all thin film samples, confirming the presence of a-C in the nanocomposite thin films. The formation of Al/a-C nanocomposite thin films is further confirmed using X-ray photoelectron spectroscopy analysis. The scanning electron microscope results show that the deposited thin films consist of nanoparticles and their agglomerates. The sizes of th agglomerates increase with increasing numbers of focus deposition shots. The nanoindentation results show the variations in hardness and elastic modulus values of nanocomposite thin film with increasing the number of focus shots. Maximum values of hardness and elastic modulus of the composite thin film prepared using 20 focus shots are found to be about 10.7 GPa and 189.2 GPa, respectively.展开更多
ZrSiN thin films are synthesized by using plasma focus through various numbers of focus shots (10, 20, and 30), with samples placed at 9 cm away from the tip of the anode. Crystal structures, surface morphologies, a...ZrSiN thin films are synthesized by using plasma focus through various numbers of focus shots (10, 20, and 30), with samples placed at 9 cm away from the tip of the anode. Crystal structures, surface morphologies, and elemental compositions of ZrSiN films are characterized by an X-ray diffractometer (XRD) and scanning electron microscope (SEM) attached with energy dispersive X-ray spectroscopy (EDS). XRD patterns confirm the formations of polycrystalline ZrSiN films. Crystallinity of nitride increases with the increase of focus shot number. The average crystallite size of zirconium nitride increases from 27 ± 3 nm to 73±8 nm and microstrain decreases from 2.28 to 1.0 with the increase of the focus shot number. SEM results exhibit the formations of granular and oval-shaped microstructures, depending on the number of focus shots. EDS results confirm the presences of silicon, zirconium, nitrogen, and oxygen in the composite films. The content values of Zr and N in the composite films increase with the increase of the focus shot number.展开更多
Nanostructured multiphase zirconia films (MZFs) are deposited on Zr substrate by the irradiation of energetic oxygen ions emanated from a plasma focus device. The oxygen operating gas pressure of 1 mbar (1 bar=105...Nanostructured multiphase zirconia films (MZFs) are deposited on Zr substrate by the irradiation of energetic oxygen ions emanated from a plasma focus device. The oxygen operating gas pressure of 1 mbar (1 bar=105 Pa) provides the most appropriate ion energy flux to deposit crystalline ZrO2 films. X-ray diffraction (XRD) patterns reveal the formation of polycrystalline ZrO2 films. The crystallite size (CS), crystal growth, and dislocation densities are attributed to increasing focus shots, sample axial distances, and working gas pressures. Phase and orientation transformations from t-ZrO2 to m-ZrO2 and c-ZrO2 are associated with increasing focus shots and continuous annealing. For lower (200 ℃) annealing temperature (AT), full width at half maximum (FWHM) of diffraction peak, CS, and dislocation density (δ) for (020) plane are found to be 0.494, 16.6 nm, and 3.63×10-3 nm-2 while for higher (400 ℃) AT, these parameters for (111) plane are found to be 0.388, 20.87 nm, and 2.29×10-3 nm-2, respectively. Scanning electron microscope (SEM) results demonstrate the formation of rounded grains with uniform distribution. The estimated values of atomic ratio (O/Zr) in ZrO2 films deposited for different axial distances (6 cm, 9 cm, and 12 cm) are found to be 2.1, 2.2, and 2.3, respectively. Fourier transform infrared (FTIR) analysis reveals that the bands appearing at 441 cm-1 and 480 cm-1 belong to m-ZrO2 and t-ZrO2 phases, respectively. Maximum microhardness (8.65±0.45 GPa) of ZrO2 film is ~ 6.7 times higher than the microhardness of virgin Zr.展开更多
文摘This paper reported a novel coating approach to deposit a (HA) film on Ti6Al4V alloy with Al2O3 buffer layer for thin, crack free and nano-structured hydroxyapatite biomedical implants. The Al2O3 buffer layer was deposited by plasma spraying while the HA top layer was applied by dip coating technique. The X-ray diffraction (XRD) and Raman reflections of alumina buffer layer showed α- to γ-Al2O3 phase transformation; and the fractographic analysis of the sample revealed the formation of columnar grains in well melted splats. The bonding strength between Al2O3 coating and Ti6Al4V substrate was estimated to be about 40 MPa. The presence of dip coated HA layer was confirmed using XRD, scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) analysis. The SEM images exhibited that HA top layer enveloped homogenously the troughs and crests of the underneath rough (Ra = 2.91 μm) Al2O3 surface. It is believed that the novel coating approach adopted might render the implant suitable for rapid cement-less fixation as well as biocompatible for longer periods.
基金Project partially supported by the HEC research project at QAU Islamabadthe NESCOM for providing financial support for his M. Phil studies
文摘The carburizing of titanium (Ti) is accomplished by utilizing energetic ion pulses of a 1.5 kJ Mather type dense plasma focus (DPF) device operated in methane discharge. X-ray diffraction (XRD) analysis confirms the deposition of polycrystalline titanium carbide (TIC). The samples carburized at lower axial and angular positions show an improved texture for a typical (200)TIC plane. The Williamson-Hall method is employed to estimate average crystallite size and microstrains in the carburized Ti surface. Crystallite size is found to vary from - 50 to 100 nm, depending on the deposition parameters. Microstrains vary with the sample position and hence ion flux, and are converted from tensile to compressive by increasing the flux. The carburizing of Ti is confirmed by two major doublets extending from 300 to 390 cm^-1 and from 560 to 620 cm^-1 corresponding to acoustic and optical active modes in Raman spectra, respectively. Analyses by scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDS) have provided qualitative and quantitative profiles of the carburized surface. The Vickers microhardness of Ti is significantly improved after carburizing.
基金supported by the Higher Education Commission of Pakistan
文摘AlON nanolayers are synthesized on Al substrate by the irradiation of energetic nitrogen ions using plasma focusing. Samples are exposed to multiple (5, 10, 15, 20 and 25) focus shots. Ion energy and ion number density range from 80 keV to 1.4 MeV and 5.6×10^19 m^- 3 to 1.3×10^19 m ^-3, respectively. Moreover, the effect of continuous annealing (473 K and 523 K) on an AlN surface layer synthesized with 25 focus shots is also examined. The main features of the X-ray diffraction (XRD) patterns with increasing focus shots are: (i) variation in the crystallinity of AlN along (111), (200) and (311) planes, (ii) increasing average crystallite size of AlN (111) plane, and (iii) stress relaxation observed in AlN (111) and (200) planes. The crystallinity of AlN surface layer is comparatively better at 473 K annealing temperature. A broadened diffraction peak related to an aluminium oxide phase showing weak crystallinity is observed for 15 focus shots while non-bounded oxides are present in all other deposited layers. Raman and Fourier transform infrared spectroscopy (FTIR) analysis confirm the presence of AlN and Al203 for the surface layer annealed at 473 K temperature. Raman analysis shows that the overlapping of AlN and Al2Oa results in the development of residual stresses. Scanning electron microscope (SEM) results demonstrate that the formation of rounded grains (range from 20 nm to 200 nm) and variations in their microstructures features depend on the increasing number of focus shots. Decomposition of larger clusters into smaller ones is observed.
文摘The Al/a-C nanocomposite thin films are synthesized on Si substrates using a dense plasma focus device with alu- minum fitted anode and operating with CH4/Ar admixture. X-ray diffractometer results confirm the formation of metallic crystalline Al phases using different numbers of focus shots. Raman analyses show the formation of D and G peaks for all thin film samples, confirming the presence of a-C in the nanocomposite thin films. The formation of Al/a-C nanocomposite thin films is further confirmed using X-ray photoelectron spectroscopy analysis. The scanning electron microscope results show that the deposited thin films consist of nanoparticles and their agglomerates. The sizes of th agglomerates increase with increasing numbers of focus deposition shots. The nanoindentation results show the variations in hardness and elastic modulus values of nanocomposite thin film with increasing the number of focus shots. Maximum values of hardness and elastic modulus of the composite thin film prepared using 20 focus shots are found to be about 10.7 GPa and 189.2 GPa, respectively.
基金supported by the National Project for Research for University,the Higher Education Commission(HEC),Pakistan
文摘ZrSiN thin films are synthesized by using plasma focus through various numbers of focus shots (10, 20, and 30), with samples placed at 9 cm away from the tip of the anode. Crystal structures, surface morphologies, and elemental compositions of ZrSiN films are characterized by an X-ray diffractometer (XRD) and scanning electron microscope (SEM) attached with energy dispersive X-ray spectroscopy (EDS). XRD patterns confirm the formations of polycrystalline ZrSiN films. Crystallinity of nitride increases with the increase of focus shot number. The average crystallite size of zirconium nitride increases from 27 ± 3 nm to 73±8 nm and microstrain decreases from 2.28 to 1.0 with the increase of the focus shot number. SEM results exhibit the formations of granular and oval-shaped microstructures, depending on the number of focus shots. EDS results confirm the presences of silicon, zirconium, nitrogen, and oxygen in the composite films. The content values of Zr and N in the composite films increase with the increase of the focus shot number.
基金Project supported by the Higher Education Commission of Pakistan
文摘Nanostructured multiphase zirconia films (MZFs) are deposited on Zr substrate by the irradiation of energetic oxygen ions emanated from a plasma focus device. The oxygen operating gas pressure of 1 mbar (1 bar=105 Pa) provides the most appropriate ion energy flux to deposit crystalline ZrO2 films. X-ray diffraction (XRD) patterns reveal the formation of polycrystalline ZrO2 films. The crystallite size (CS), crystal growth, and dislocation densities are attributed to increasing focus shots, sample axial distances, and working gas pressures. Phase and orientation transformations from t-ZrO2 to m-ZrO2 and c-ZrO2 are associated with increasing focus shots and continuous annealing. For lower (200 ℃) annealing temperature (AT), full width at half maximum (FWHM) of diffraction peak, CS, and dislocation density (δ) for (020) plane are found to be 0.494, 16.6 nm, and 3.63×10-3 nm-2 while for higher (400 ℃) AT, these parameters for (111) plane are found to be 0.388, 20.87 nm, and 2.29×10-3 nm-2, respectively. Scanning electron microscope (SEM) results demonstrate the formation of rounded grains with uniform distribution. The estimated values of atomic ratio (O/Zr) in ZrO2 films deposited for different axial distances (6 cm, 9 cm, and 12 cm) are found to be 2.1, 2.2, and 2.3, respectively. Fourier transform infrared (FTIR) analysis reveals that the bands appearing at 441 cm-1 and 480 cm-1 belong to m-ZrO2 and t-ZrO2 phases, respectively. Maximum microhardness (8.65±0.45 GPa) of ZrO2 film is ~ 6.7 times higher than the microhardness of virgin Zr.