Afsaneh Rabiei

Failure mechanisms associated with the thermally grown oxide in plasma-sprayed thermal barrier coatings

Abstract The microstructure and durability of a thermal barrier coating (TBC) produced by the thermal spray method have been characterized. Upon exposure, the bond coat chemistry and microstructure change by inter-diffusion with the substrate and upon thickening of the thermally grown oxide (TGO). A wedge impression test, in conjunction with observations by scanning electron microscopy, has been used to probe the failure mechanisms. At short exposure times, when the TGO thickness is less than about 5 μ m, the growth of the TGO does not affect the crack patterns in the TBC and delaminations induced by wedge impression propagate within the TBC about 30 μ m from the interface. An amorphous phase at the splat interfaces promotes this failure mode. As the thickness of TGO increases during exposure, cracks form in the TBC around imperfections at the interface. Moreover, induced delaminations develop a trajectory close to the interface, propagating not only through the TBC but also within the TGO and along the interfaces. A scaling result based on the misfit around imperfections caused by TGO growth has been used to rationalize the critical TGO thickness when the TBC fails.

Functionally graded hydroxyapatite coatings doped with antibacterial components.

A series of functionally graded hydroxyapatite (FGHA) coatings incorporated with various percentages of silver were deposited on titanium substrates using ion beam-assisted deposition. The analysis of the coatings cross-section using transmission electron microscopy (TEM) and scanning transmission electron microscopy equipped with energy dispersive X-ray spectroscopy has shown a decreased crystallinity as well as a distribution of nanoscale (10-50nm) silver particles from the coating/substrate interface to top surface. Both X-ray diffraction and fast Fourier transforms on high-resolution TEM images revealed the presence of hydroxyapatite within the coatings. The amount of Ag (wt.%) on the outer surface of the FGHA, as determined from X-ray photoelectron spectroscopy, ranged from 1.09 to 6.59, which was about half of the average Ag wt.% incorporated in the entire coating. Average adhesion strengths evaluated by pull-off tests were in the range of 83+/-6 to 88+/-3MPa, which is comparable to 85MPa for FGHA without silver. Further optical observations of failed areas illustrated that the dominant failure mechanism was epoxy failure, and FGHA coating delamination was not observed.

Compression fatigue of a cellular Al alloy

The cyclic compression of a cellular Al alloy has been evaluated. Plastic compression occurs beyond a critical number of cycles, NT. At N NT, strain accumulates rapidly and preferentially within deformation bands, until the densification strain has been reached. The bands form preferentially from large cells in the ensemble. Such cells develop plastically buckled membranes which experience large strains upon further cycling, which lead to cracks. The cracks, once formed, result in rapid cyclic straining. This feature controls the fatigue life.

Microstructure, deformation and cracking characteristics of thermal spray ferrous coatings

Abstract The microstructure and local mechanical characteristics of thermal spray ferrous coatings have been determined. The emphasis has been on coatings made by the high velocity oxyfuel (HVOF) process, especially the role of Al alloy additives. The oxide phase present in the material and preferred pathways for local cracking and separation have been determined. Thin intersplat oxide layers emerge as preferential sites. These oxides are amorphous and the cracks extend along the oxide/α–Fe interfaces with low local fracture toughness, in the range 0.2–1 MPa√m. These low toughness pathways govern coating deterioration.

Deposition and investigation of functionally graded calcium phosphate coatings on titanium

A series of calcium phosphate coatings with graded crystallinity were deposited onto heated titanium substrates using ion beam assisted deposition. The microstructure of the coating was examined using transmission electron microscopy (TEM). The coating thickness was observed to be in a range of 594-694 nm. The degree of crystallinity and microstructural grain size of the coating showed a clear decrease with increasing distance from the substrate-coating interface. Fourier transform infrared spectroscopy (FTIR) confirmed the presence of PO(4)(3-), and X-ray photoelectron spectroscopy (XPS) analysis on the coating top surface showed that the atomic Ca/P ratio was in the range of 1.52+/-0.15 to 1.61+/-0.07. The biological response to the coatings was also evaluated using an osteoblast precursor cell culture test. More cells and a higher integrin expression of cell attachment sites were observed on the coating surface when compared to the control group (blank titanium surface). The pull-off test showed average adhesion strengths at the coating-substrate interface to be higher than 85.12+/-5.37 MPa. Nanoindentation tests indicated that the Youngs moduli of all coatings are higher than 91.747+/-3.641 GPa and microhardness values are higher than 5.275+/-0.315 GPa. While the adhesion strength results helped us to identify the best setup for substrate temperature and processing parameters to begin the deposition, the culture test and XPS results helped identifying the optimum parameters for the last stage of deposition. TEM, X-ray diffraction, FTIR and nanoidentation results were used to further evaluate the quality of the coating and optimization of its processing parameters.

Processing and evaluation of bioactive coatings on polymeric implants

Polyetheretherketone (PEEK) is a high-performance polymer with advantages over metallic biomaterials for application in spinal implants. In this study, hydroxyapatite (HA) coatings were deposited onto PEEK substrates using radio-frequency magnetron sputtering for the purpose of improving bioactivity. An intermediate coating layer of yttria-stabilized zirconia (YSZ) was first deposited onto the PEEK substrates to provide heat shielding during subsequent post-deposition heat treatment to prevent degradation of PEEK substrates and coating/substrate interface. Plasma activation of the PEEK substrate surfaces before deposition resulted in a significant increase in coating adhesion strength. Post-deposition heat treatments of microwave and hydrothermal annealing were studied with the goal of forming crystalline HA without the use of high temperatures required in conventional annealing. Microstructural and compositional analyses by scanning electron microscopy (SEM) and X-ray diffraction revealed that the YSZ layer exhibited a crystalline structure as-deposited, with columnar grains oriented along the growth direction, whereas the HA layer was shown to be amorphous as-deposited. After microwave annealing, the HA coating exhibited a columnar crystalline microstructure, similar to that of the underlying YSZ crystalline layer; XRD analysis confirmed a crystalline HA phase in the coating. It is suggested that the existence of the crystalline YSZ layer aids in the formation of the HA layer upon heating, possibly lowering the activation energy for crystallization by providing nucleation sites for HA grain formation. Cell culture tests showed a significant increase in initial cell attachment and growth on the microwave-annealed coatings, compared with uncoated PEEK and amorphous HA surfaces.

Antibacterial effect and cytotoxicity of Ag-doped functionally graded hydroxyapatite coatings†

Functionally graded hydroxyapatite coatings (FGHA) doped with 1, 3, and 6.5 wt % silver (Ag) have been deposited on Titanium using ion-beam-assisted deposition. Scanning transmission electron microscopy on coating cross sections confirmed the presence of FGHA coating with mostly amorphous layers at the top and mostly crystalline layers toward the coating interface as well as the existence of 10-50 nm Ag particles distributed throughout the thickness of the coatings. Calcium release in phosphate buffered saline solution showed a high release rate of Ca at the beginning of the test, and a gradual decrease in release rate thereafter to a minimum level until day 7. Similarly, the release rate of Ag in ultra pure water was initially high in the first 4 h and then gradually decreased over a 7 days period. Antibacterial tests have shown a reduction in the viability of S. aureus in Ag-doped coatings particularly in samples with higher Ag concentrations of 3 and 6.5 wt %. Cytotoxicity tests using an osteoblast cell line, on the other hand, have demonstrated that the samples with 6.5 wt % Ag have a negative effect on osteoblast cell response, proliferation, and apoptosis as well as a negative effect on protein and osteocalcin production. It is notable that the samples with 3 wt % Ag or less presented minimal cytotoxicity compared with control surfaces. Considering both the antibacterial and cytotoxicity effects, it is suggested that the 3 wt % of Ag in FGHA coatings can be favorable.

A study on fracture behavior of particle reinforced metal matrix composites by using acoustic emission source characterization

Abstract A one directional acoustic emission (AE) source characterization has been used during a three point bending fracture toughness test on 6061 aluminum matrix composites with Al2O3 particle reinforcements of 5 and 10 μm sizes, in order to evaluate the dynamic process of micro-fracture in these materials. Different acoustic emission sources are characterized and, as a result, two types of AE events are distinguished. It is observed that at very low strain levels void nucleation is the main source for acoustic emission. At higher levels, the micro pop-in of primary voids and their eventual coalescence results in a different type of acoustic emission. In fine particle reinforced materials, when the amplitude of AE events in void nucleation at fine particles is not high enough to be detected, the main source of AE events is only the void coalescence. By increasing the particle size, the number of detectable events during void nucleation is increased.

Osteoblast adhesion to functionally graded hydroxyapatite coatings doped with silver

Silver-doped functionally graded hydroxyapatite (Ag-FGHA) coatings have been prepared on glass and titanium substrates by ion beam assisted deposition (IBAD) method with in situ heat treatment, and the biological response and dissolution properties of the coatings have been examined. Three Ag-FGHA coatings with different percentages of silver (1, 3, and 6.6 wt % Ag) were compared with pure FGHA (without Ag) as a control. MC 3T3-E1 murine osteoblast cells were cultured on FGHA and Ag-FGHA coating surfaces, and the number of adhered cells after 1, 4, and 7 days was counted. Micromanipulation of live single cells was performed to quantitatively compare cell affinity among the four coating compositions. Results showed that FGHA-Ag1 coating (with 1 wt % Ag) had the highest number of adhered cells after each incubation period, as well as the highest cell affinity after 24-h incubation. Surface profilometry was performed to determine surface roughness average (R(a) ) of coating surfaces before and after immersion in high-purity water, showing that all surfaces initially had roughness averages below 200 nm, while after immersion, roughness average of FGHA-Ag1 surface was significantly increased (R(a) = 404 +/- 100.8 nm), attributed to the highest rate of dissolution. Release rate of Ag+ ions in solution was measured, showing release rates of silver ions for all Ag-doped coatings were initially high and then gradually decreased to a minimum over time, which is the expected dissolution of functionally graded coatings. It is concluded that FGHA-Ag1 coating promoted the highest degree of osteoblast adhesion because of optimal dissolution rate and nontoxic Ag percentage.

New Composite Metal Foams under Compressive Cyclic Loadings

New composite metal foams are processed using powder metallurgy (PM) and gravity casting techniques. The foam is comprised of steel hollow spheres, with the interstitial spaces occupied by a solid metal matrix (Al or steel alloys). The cyclic compression loading of the products of both techniques has shown that the composite metal foams have high cyclic stability at very high maximum stress levels up to 68 MPa. Under cyclic loading, unlike other metal foams, the composite metal foams do not experience rapid strain accumulation within collapse bands and instead, a uniform distribution of deformation happen through the entire sample until the densification strain is reached. This is a result of more uniform cell structure in composite metal foams compared to other metal foams. As a result, the features controlling the fatigue life of the composite metal foams have been considered as sphere wall thickness and diameter, sphere and matrix materials, and processing techniques as well as bonding strength between the spheres and matrix.