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The effect of anodizing on corrosion resistance of Ti-xHf alloys has been investigated. Ti-xHf alloys were prepared and anodized at 120, 170 and 220 V in 1 M H(3)PO(4) solution, and crystallized at 300 and 500°C. Corrosion experiments were carried out using a potentiostat in 0.15 M NaCl solution at 36.5 ± 1°C. The Ti-xHf alloys exhibited the α' and anatase phases. The pore size on the anodized surface increases as the applied voltage is increased, whereas the pore size decreases as the Hf content is increased. The anodized Ti-xHf alloys exhibited better corrosion resistance than non-anodized Ti-xHf alloys.

The goals of this study were to investigate the fatigue limits of two Pd-Ag alloys (Ivoclar Vivadent) with differing mechanical properties and varying proportions of secondary alloying elements, examine the effect of casting porosity on fatigue behavior, and determine the effect of casting size on microstructures and Vickers hardness. The alloys selected were: IPS d.SIGN 59 (59.2Pd-27.9Ag-8.2Sn-2.7In-1.3Zn); and IS 64 (59.9Pd-26.0Ag-7.0Sn-2.8Au-1.8 Ga-1.5In-1.0Pt). Tension test bars, heat-treated to simulate dental porcelain application, were subjected to cyclic loading at 10 Hz, with R-ratio of -1 for amplitudes of compressive and tensile stress. Two replicate specimens were tested at each stress amplitude. Fracture surfaces were examined with a scanning electron microscope (SEM). Sectioned fatigue specimens and additional cast specimens simulating copings for a maxillary central incisor restoration were also examined with the SEM, and Vickers hardness was measured using 1 kg load. Casting porosity was evaluated in sectioned fatigue fracture specimens, using an image analysis program. The fatigue limit (2 × 10(6) loading cycles) of IS 64 was approximately 0.20 of its 0.2% yield strength, while the fatigue limit of d.SIGN 59 was approximately 0.25 of its 0.2% yield strength. These relatively low ratios of fatigue limit to 0.2% yield strength are similar to those found previously for high-palladium dental alloys, and are attributed to their complex microstructures and casting porosity. Complex fatigue fracture surfaces with striations were observed for both alloys. Substantial further decrease in the number of cycles for fatigue failure only occurred when the pore size and volume percentage became excessive. While the heat-treated alloys had equiaxed grains with precipitates, the microstructural homogenization resulting from simulated porcelain firing differed considerably for the coping and fatigue test specimens; the latter specimens had significantly higher values of Vickers hardness.

The fatigue limits and fracture characteristics for three Pd-Ag dental casting alloys (Super Star, Heraeus Kulzer; Rx 91, Pentron; W-1, Ivoclar Vivadent) were studied. Specimens meeting the dimensions for ADA Specifications No. 5 and 38, and having the as-cast surface condition, were subjected to heat treatment simulating dental porcelain firing cycles and fatigued in air at room temperature under uniaxial tension-compression at 10 Hz. A ratio of compressive stress amplitude to tensile stress amplitude (R-ratio) of -1 was used. Alloy microstructures and fracture surfaces were examined with a scanning electron microscope and a transmission electron microscope. Fatigue limits for the three alloys had low values of approximately 15% of the yield strength for 0.2% permanent tensile strain. Complex fracture surfaces with characteristic striations were observed for all three fatigued alloys. Planar slip of dislocations occurred in the Pd solid solution matrix, along with dislocation-precipitate interactions and dislocation networks in the interfaces between the precipitates and surrounding matrix. Twinning occurred in the Pd solid solution matrix of Rx 91, and within discontinuous precipitates in Super Star and Rx 91. The low fatigue limits for these alloys are attributed to their complex microstructures and perhaps to casting defects.

Three Pd-Ag dental alloys for metal-ceramic restorations, W-1 (Ivoclar Vivadent), Rx 91 (Pentron) and Super Star (Heraeus Kulzer), were subjected to isothermal annealing for 0.5 hr periods in a nitrogen atmosphere at temperatures from approximately 400 degrees to 950 degrees C. The annealing behavior was investigated by Vickers hardness measurements (1 kg load) and SEM microstructural observations. The highest Vickers hardness occurred at approximately 700 degrees C for W-1 and 650 degrees C for Rx 91. For Super Star, there were two peaks in hardness at approximately 500 degrees and 650 degrees C. Additional use of light indenting loads (25 g for W-1; 10 g for Rx 91 and Super Star) revealed that hardness variations during annealing for W-1 and Rx 91 were related to the palladium solid solution matrix phase. For Super Star, the lower-temperature peak was controlled by multi-phase regions and the higher-temperature peak by the matrix phase. While microstructural changes due to annealing were evident with the SEM for Rx 91 and Super Star, no correlation was possible for W-1 because of its finer-scale microstructure. Although commercial Pd-Ag alloys have a relatively narrow composition range, their microstructures and annealing behavior can vary because of differences in proportions of secondary elements utilized for porcelain adherence and grain refinement elements, as well as other proprietary strategies employed by the manufacturers.

Electrochemical impedance spectroscopic (EIS) analyses were performed on three high-palladium alloys and a gold-palladium alloy at active and passive potentials in five electrolytes that simulated body fluid and oral environmental conditions. All four alloys were previously found to have excellent corrosion resistance in these in vitro environments. Before performing the EIS analyses, alloy specimens were subjected to a clinically relevant heat treatment that simulated the firing cycles for a dental porcelain. It was found that the EIS spectra varied with test potential and electrolyte. Diffusional effects, related to the dealloying and subsequent surface enrichment in palladium of the high-palladium alloys, along with species adsorption and passivation, were revealed at both active and passive potentials, although these effects were more evident at the passive potentials.

Electrochemical impedance spectroscopy (EIS) was used to study the in vitro corrosion of three representative high-palladium alloys and a gold-palladium alloy for comparison. The corrosion resistances (measured as the charge transfer resistance R(CT) from an equivalent circuit) of the high-palladium alloys and the gold-palladium alloy were comparable in simulated body fluid and oral environments, and under simulated dental plaque. The great similarity in corrosion behavior for the three high-palladium alloys is largely attributed to their substantial palladium content and passivity in the laboratory test media, and possibly to their similar structure at the submicron level. Differences in composition and microstructure at the micron level and greater, including the effects of heat treatment simulating the firing cycles for dental porcelain, do not have noteworthy effects on the in vitro corrosion of the three high-palladium alloys. Good accuracy and convenience of extracting corrosion characteristics from equivalent circuit modeling, along with the capability of providing intrinsic information about the corrosion mechanism, enable EIS to be an excellent alternative method to conventional potentiodynamic polarization for evaluating the corrosion behavior of noble dental alloys.

The microstructures of two representative high-palladium dental alloys, a Pd-Cu-Ga alloy and a Pd-Ga alloy, which had been subjected to cyclic fatigue in uniaxial tension were investigated by transmission electron microscopy (TEM). Two different mechanisms were found to dominate microplastic deformation during fatigue: twinning in the Pd-Cu-Ga alloy, and planar slip of dislocations in the Pd-Ga alloy. In addition, stress-induced precipitation occurred in the Pd-Ga alloy during cyclic loading. Heat treatment simulating the firing cycles for dental porcelain resulted in the formation of a previously unreported bcc phase in the Pd-Cu-Ga alloy, and in the elimination of the characteristic tweed structure found in the Pd-Ga alloy for the as-cast condition.

The fatigue limits and fracture characteristics for a Pd-Cu-Ga alloy and a Pd-Ga alloy were studied. The alloys were cast into tensile test bars with gauge diameter of 3 mm and gauge length of 15 mm, and the surfaces of the castings were neither air-abraded nor polished after removal from the investment. Specimens were prepared from all-new metal (not previously melted), a combination of 50% new metal and 50% old metal (previously melted one time) and 100% old metal. The cast bars were subjected to heat treatment simulating the complete firing cycles for dental porcelain, and fatigued in air at room temperature under uniaxial tension-compression stress at 10 Hz and a ratio of tensile stress amplitude to compressive stress amplitude (R-ratio) of -1. The alloy microstructures and fracture surfaces were examined with a scanning electron microscope (SEM). Results showed that the fatigue limits at 2 x 10(6)cycles of the Pd-Cu-Ga and Pd-Ga alloys were approximately 0.20 and 0.15 of their 0.1% yield strength (YS) in tension, respectively. The fatigue resistance for specimens from both alloys containing 50% old metal and 50% new metal was comparable to that of specimens containing all-new metal, although this decreased dramatically for Pd-Cu-Ga alloy specimens containing all-old metal. The fatigue resistance of the Pd-Cu-Ga alloy subjected to heat treatment simulating the porcelain firing cycles was not adversely affected by remnants of the original as-cast dendritic microstructure that remained in the relatively large test specimens. A longer heat treatment than recommended by the manufacturer for the porcelain firing cycles is needed to completely eliminate the as-cast dendritic structure in these specimens. The Pd-Cu-Ga alloy exhibited superior fatigue resistance to the Pd-Ga alloy, which has an equiaxed-grain microstructure and lower yield strength.

X-ray diffraction (XRD) was employed to study dental alloy-ceramic interfaces. A Au-Pd-In alloy, which requires oxidation before porcelain firing, and a Au-Pt-Pd-In alloy, which does not require oxidation before porcelain firing, were selected in this study. Alloy specimens were centrifugally cast. Specimen surfaces were metallographically polished through 0.05 microm Al2O3 slurries. A thin layer (< 50 microm) of a dental opaque porcelain was fired on the alloy surfaces with and without initial oxidation. XRD was conducted at room temperature on four types of alloy specimens: polished, oxidized, porcelain fired after alloy oxidation, and porcelain fired without initial alloy oxidation. XRD was also performed on fired opaque porcelain without an alloy substrate. The detection of prominent gold solid solution peaks from alloy-ceramic specimens indicated that the incident X-ray beam reached the alloy-ceramic interface. In2O3 and beta-Ga2O3 were identified on the oxidized Au-Pd-In alloy, while In2O3 and SnO2 were detected on the oxidized Au-Pt-Pd-In alloy. Preferred orientation was observed for all the oxides formed on the alloys. Minimum lattice parameter changes (<1%) for the gold solid solutions were observed for both alloys before and after oxidation and porcelain firing. Leucite (KAlSi2O6, TiO2, ZrO2 and SnO2 were detected on the fired opaque porcelain. For both alloys, no additional oxides were identified at the metal-ceramic interfaces beyond those present in the oxidized alloys and the opaque porcelain. Similar results were obtained from alloy-ceramic interfaces where there was no prior alloy oxidation. The results indicate the critical role of alloy surface oxides in metal-ceramic bonding and support the chemical bonding mechanism for porcelain adherence., (Copyright 2001 Kluwer Academic Publishers)

Two Pd-Cu-Ga alloys and a Pd-Ga alloy were selected for study. Bars of each alloy were tested in tension for the as-cast and simulated porcelain-firing conditions, and values of mechanical properties were measured. Fracture surfaces and microstructures of axially sectioned fracture specimens were observed with the SEM. The two Pd-Cu-Ga alloys exhibited similar mechanical properties. The Pd-Ga alloy had lower strength and higher percentage elongation. Heat treatment simulating porcelain firing cycles decreased the strength of both Pd-Cu-Ga alloys and increased their ductility. However, this heat treatment did not significantly affect the mechanical properties of the Pd-Ga alloy. All three high-palladium alloys had the same modulus of elasticity. The amount of overall porosity was relatively minimal (< 1%) and not significantly different among the three alloys. However, porosity was a significant factor for UTS of one Pd-Cu-Ga alloy and the Pd-Ga alloy., (Copyright 2000 Kluwer Academic Publishers)

Transmission electron microscopy and convergent-beam electron diffraction were used to study three high-palladium dental alloys: an as-cast Pd-Ga alloy, a cast Pd-Cu-Ga alloy aged at room temperature for over 5 years, and a cast Pd-Cu-Ga alloy annealed at 1023 K for 2 h and slowly cooled to room temperature. Bands containing a tweed structure in the Pd-Ga alloy were 120degrees twins with (1 1 0 mirror planes. Within these bands the alloy had a face-centered tetragonal structure with a c/a ratio of 1.03. The aged Pd-Cu-Ga alloy contained a larger amount of tweed structure than the original as-cast alloy, along with randomly oriented bands and thin lath-like regions. The annealed Pd-Cu-Ga alloy contained rectangular particles of a secondary phase that may be Pd2Ga, Pd5Ga2 or Pd13Ga5. The microtwinned band structure relieves the strain energy arising from transformation of the f.c.c. palladium solid solution on cooling., (Copyright 1999 Kluwer Academic Publishers)