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Background: Previous temperature-modulated differential scanning calorimetry (TMDSC) study of nickel-titanium orthodontic wires revealed a large exothermic low-temperature peak that was attributed to transformation within martensitic NiTi., Purpose: The purpose of this study was to use transmission electron microscopy (TEM) to verify this phase transformation in a clinically popular nickel-titanium wire, identify its mechanism and confirm other phase transformations found by TMDSC, and to provide detailed information about the microstructure of this wire., Methods: The 35 degrees C Copper nickel-titanium wire (Ormco) with cross-section dimensions of 0.016 in. x 0.022 in. used in the earlier TMDSC investigation was selected. Foils were prepared for TEM analyses by mechanical grinding, polishing, dimpling, ion milling and plasma cleaning. Standard bright-field and dark-field TEM images were obtained, along with convergent-beam electron diffraction patterns. A cryo-stage with the electron microscope (Phillips CM 200) permitted the specimen to be observed at -187, -45, and 50 degrees C, as well as at room temperature. Microstructures were also observed with an optical microscope and a scanning electron microscope., Results: Room temperature microstructures had randomly oriented, elongated grains that were twinned. Electron diffraction patterns confirmed that phase transformations took place over temperature ranges previously found by TMDSC. TEM observations revealed a high dislocation density and fine-scale oxide particles, and that twinning is the mechanism for the low-temperature transformation in martensitic NiTi., Conclusions: TEM confirmed the low-temperature peak and other phase transformations observed by TMDSC, and revealed that twinning in martensite is the mechanism for the low-temperature peak. The high dislocation density and fine-scale oxide particles in the microstructure are the result of the wire manufacturing process.

Laser welding 0.016 x 0.022 in. beta-Ti, Ni-Ti, and Co-Cr-Ni orthodontic wires was investigated by measuring joint tensile strength, measuring laser penetration depth, determining metallurgical phases using micro X-ray diffraction (micro-XRD), and examining microstructures with an scanning electron microscope (SEM). Welding was performed from 150 to 230 V. Mean tensile strength for Ni-Ti groups was significantly lower (p < 0.05) than for most other groups of laser-welded specimens. Although mean tensile strength for beta-Ti and Co-Cr-Ni was significantly lower than for control specimens joined by silver soldering, it was sufficient for clinical use. The beta-Ti orthodontic wire showed deeper penetration depth from laser welding than the Ni-Ti and Co-Cr-Ni orthodontic wires. Micro-XRD patterns of laser-welded beta-Ti and Ni-Ti obtained 2 mm from the boundary were similar to as-received specimens, indicating that original microstructures were maintained. When output voltages of 190 V and higher were used, most peaks from joint areas disappeared or were much weaker, perhaps because of a directional solidification effect, evidenced by SEM observation of fine striations in welded beta-Ti. Laser welding beta-Ti and Co-Cr-Ni wires may be acceptable clinically, since joints had sufficient strength and metallurgical phases in the original wires were not greatly altered.

Objectives: Employ differential scanning calorimetry (DSC) and temperature-modulated DSC (TMDSC) to investigate thermal transformations in three mouthguard materials and provide insight into their previously investigated energy absorption., Methods: Samples (13-21mg) were obtained from (a) conventional ethylene vinyl acetate (EVA), (b) Pro-form, another EVA polymer, and (c) PolyShok, an EVA polymer containing polyurethane. Conventional DSC (n=5) was first performed from -80 to 150 degrees C at a heating rate of 10 degrees C/min to determine the temperature range for structural transformations. Subsequently, TMDSC (n=5) was performed from -20 to 150 degrees C at a heating rate of 1 degrees C/min. Onset and peak temperatures were compared using ANOVA and the Tukey-Kramer HSD test. Other samples were coated with a gold-palladium film and examined with an SEM., Results: DSC and TMDSC curves were similar for both conventional EVA and Pro-form, showing two endothermic peaks suggestive of melting processes, with crystallization after the higher-temperature peak. Evidence for crystallization and the second endothermic peak were much less prominent for PolyShok, which had no peaks associated with the polyurethane constituent. The onset of the lower-temperature endothermic transformation is near body temperature. No glass transitions were observed in the materials. SEM examination revealed different surface morphology and possible cushioning effect for PolyShok, compared to Pro-form and EVA., Significance: The difference in thermal behavior for PolyShok is tentatively attributed to disruption of EVA crystal formation, which may contribute to its superior impact resistance. The lower-temperature endothermic peak suggests that impact testing of these materials should be performed at 37 degrees C.

Objective: The purpose of this study was to investigate the metallurgical phases in beta-titanium soldered joints prepared by infrared soldering, using the Micro X-ray diffraction technique (Micro-XRD), and to characterize the Vickers hardness in the soldered beta-titanium wires., Methods: Beta-titanium wires with cross-section dimensions of 0.032in.x0.032in. (TMA, Ormco), and both titanium-based solder (Ti-30Ni-20Cu, Selec) and silver-based solder (Ag-22Cu-17Zn-5Sn, Tomy) were selected. Soldering was performed using infrared radiation (RS-1, Morita) under argon atmosphere. Micro-XRD analyses were performed at room temperature. Micro-XRD spectra were obtained for the boundary region of the soldered beta-titanium wires using 50microm and 10microm diameter analysis regions. Hardness was measured at 30microm intervals from boundary of the diffusion layer and beta-titanium wire. The Kruskal-Wallis test with the Bonferroni and Wilcoxson Mann-Whitney tests for nonparametric means were employed as statistical methods (P<0.05)., Results: For both types of soldered beta-titanium samples, the Micro-XRD spectra contained four major peaks for body-centered cubic (bcc) beta-titanium. Additional peaks at about 41 and 45 degrees are attributed to Cu-Ti intermetallic phase(s), which may be metastable under soldering conditions. The diffusion layer had greater hardness than bulk beta-titanium for both types of soldered specimens (P<0.05)., Significance: Soldering of beta-titanium orthodontic wire by infrared radiation may be acceptable for clinical use, since Micro-XRD spectra revealed that both types of soldered specimens largely retained the bcc beta-titanium structure. Further research is needed to investigate the mechanical properties and corrosion behavior of infrared-soldered beta-titanium wire.

By means of X-ray photoelectron spectroscopy (XPS) and differential scanning calorimetry (DSC), this study set out to investigate the application of plasma immersion ion implantation (PIII) for the surface modification of ProTaper NiTi rotary instruments. This study was undertaken because the PIII method was perceived to have the potential of developing into a standard surface modification technique that improves clinical quality and outcome. Specimens received nitrogen ion or nitrogen plus argon ion implantation. XPS analyses with and without argon ion etching were obtained for all specimens. In addition, DSC analysis was performed to investigate the phase transformation behavior of the bulk material. Results indicated that the surfaces of NiTi instruments were successfully modified by nitrogen PIII, whereby a light golden TiN layer was yielded. Moreover, the PIII technique did not alter the superelastic character of NiTi instruments because it was carried out at near-room temperature. We thus concluded that nitrogen PIII is a promising surface modification technique to improve the surface characteristics of NiTi rotary instruments.

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.

A contributing mechanism for clinical failure of NiTi rotary instruments might be excessive work hardening. Vickers hardness was measured with 300 gm load near the flutes in three regions (D2-D4, D6-D10, and D14 towards the shank) for nine representative clinically used ProFile GT instruments that had been axially sectioned (10 measurements in each region). Consistent values could not be obtained at D1. Minimum hardness occurred at D2 to D4, with means from 313 to 324 (SD from 7 to 16). Maximum hardness with means ranging widely from 330 to 481 was found beyond D14. Mean hardness at D2 to D4 was 320 for an as-received ProFile instrument. Because a mean Vickers hardness of 326 has been reported for a shape-memory NiTi orthodontic wire product, it can be concluded that the NiTi instruments did not experience substantial work hardening at D2 to D4 during clinical use, in agreement with previous differential scanning calorimetric analyses.

Statement of Problem: Viscoelastic behavior can influence the fracture properties of glass ionomers, which is of clinical relevance. Glass-ionomer cements can display viscoelastic behavior, defined as having displacement rate- or strain rate-dependent mechanical properties. Understanding and describing the viscoelastic behavior of glass ionomers is important to understanding their clinical behavior., Purpose: The purpose of this study was to evaluate the viscoelastic behavior of 6 glass-ionomer cements and determine whether there was a correlation to fracture toughness., Material and Methods: Three conventional glass-ionomer cements (alpha-Silver, alpha-Fil, and Ketac-Molar) and 3 resin-modified glass-ionomer cements (Vitremer, Fuji II LC, and Photac-Fil Quick) were evaluated using measurements of compressive strength (CS), flexural strength (FS), and diametral tensile strength (DTS) at displacement rates of 0.5, 1.0, 1.5, and 2.0 mm/min. The CS and DTS specimens were cured in glass tubes and cut to 4 x 6-mm and 4 x 2-mm disk-shaped specimens, respectively. The FS specimens were cured in bar molds (2 x 2 x 15 mm). The fracture toughness (FT) specimens were cured in a minicompact mold to obtain precracked specimens. The mechanical testing results were compared statistically using generalized linear model/analysis of covariance and the Ryan-Einot-Gabriel-Welsch multiple range test at the alpha=.05 level., Results: For all 3 mechanical properties, there was a displacement-rate dependence on the mechanical property. However, there were no differences in the displacement-rate dependence based on the type of material-conventional glass ionomer or resin-modified glass ionomer-for any of the mechanical properties. Only for FS test was there a significant difference based on the brand of material. There was no statistical difference in FT among the glass-ionomer cements tested, although the resin-modified glass ionomers tended to display higher FT., Conclusion: A larger sample size and a much wider range of crosshead speeds are necessary to support a correlation between viscoelastic behavior and FT.

The microstructures and interdiffusion in brazed beta-titanium orthodontic wires were investigated by scanning electron microscopy and electron probe microanalysis, respectively. Beta-titanium wire (Ti-11Mo-6Zr-4Sn) with cross-section dimensions of 0.032 in. x 0.032 in., titanium-based braze alloy (Ti-30Ni-20Cu), and silver-based braze alloy (Ag-22Cu-17Zn-5Sn) were selected for the study. Brazing was performed using infrared radiation (RS-1) under an argon atmosphere. Specimens were etched with two solutions (2.5% HF + 2.5% HNO(3) + 95% H(2)O; 25% HN(4)OH + 30% H(2)O(2) + 45%H(2)O). It was found that the silver-based braze alloy has a eutectic structure. In the diffusion layer between the beta-titanium wire and this silver-based braze alloy, Cu and Ti were enriched on the wire side, and Sn and Ti were enriched on the braze alloy side. The titanium-based braze alloy has a dendritic structure. Beta-titanium wire specimens brazed with the titanium-based braze alloy had a thicker intermediate area compared to the silver alloy; Ti in the diffusion layer had an irregular concentration gradient, and the braze alloy side had higher Ti concentration. The original microstructure of the beta-titanium wire was not altered with the use of either braze alloy. Infrared brazing of beta-titanium orthodontic wire is acceptable for clinical use, since the wire microstructure did not deteriorate with either the titanium-based or silver-based braze alloy. The differing microstructures of the joint regions for the two braze alloys suggest that the joint strengths may also differ.

ProFile nickel-titanium Gates Glidden drills were tested in bending fatigue to simulate clinical conditions. Ten samples each in sizes #1 through #6 were placed in a device that deflected the drill head 4 mm from the axis. The drill head was placed inside a ball bearing fixture, which allowed it to run free at 4000 rpm, and the total number of revolutions was recorded until failure. Fracture surfaces were examined with a scanning electron microscope to determine the initiation site and nature of the failure process. Mean +/- SD for the number of revolutions to failure for the drill sizes were: #1: 1826.3 +/- 542.5; #2: 5395.7 +/- 2581.5; #3: 694.4 +/- 516.8; #4: 261.0 +/- 138.0; #5: 49.6 +/- 14.9; #6: 195.9 +/- 78.5. All drills failed in a ductile mode, and fracture initiation sites appeared to be coincident with machining grooves or other flaws, suggesting the need for improved manufacturing procedures.

Numerous discarded ProFile GT, ProFile, and ProTaper nickel-titanium rotary instruments obtained from two graduate endodontic clinics were examined by scanning electron microscopy. These instruments had an unknown history of clinical use and had fractured or experienced considerable permanent torsional deformation without complete separation. The failure processes generally exhibited substantial ductile character, evidenced by a dimpled rupture fracture surface. Crack propagation at grain boundaries and cleavage surfaces indicative of transgranular fracture were observed for some specimens. It appeared that oxide particles from the manufacturing process served as nucleating sites for the microvoids, leading to dimpled rupture. A previously unreported fracture mode also was observed, in which crack propagation, approximately parallel to the local flute orientation, connected pitted regions on the surface. Combining present and previous scanning electron microscopy observations of clinically failed instruments, suggestions are offered for improving their fracture resistance.

The purpose of this study was to investigate the glass transition temperatures (T(g)) of representative elastomeric chain products (plastic modules) in the as-received condition and after orthodontic use to determine differences between brands and pigments. Values of T(g) were determined by differential scanning calorimetry. Products were obtained from 3 manufacturers: Rocky Mountain Orthodontics (RMO, Denver, Colo), Ormco (Glendora, Calif), and G&H (Greenwood, Ind). Three colors (gray, red, and purple) were selected for each brand-pigment combination to evaluate the as-received products, and test specimens for each brand-pigment combination from the same batches were placed in patients' mouths for 4 weeks to evaluate the products after clinical use (sample size of 7 specimens for both groups of experiments). Results were analyzed statistically by multiple nonparametric Mann-Whitney tests. A post hoc step-down Bonferroni analysis followed, to examine differences in T(g) due to pigmentation within brands and differences due to brands within each pigmentation category. For the as-received products, the RMO modules had mean T(g) ranging from -24 degrees C to -21 degrees C, whereas the Ormco and G&H modules had significantly lower mean T(g), ranging from -46 degrees C to -39 degrees C, indicating substantial compositional or polymer structural differences compared with the RMO modules. After clinical use, the RMO products had mean T(g) ranging from -31 degrees C to -25 degrees C, whereas the Ormco and G&H products had mean T(g) ranging from -46 degrees C to -30 degrees C. The in vivo specimens also exhibited a second, higher-temperature glass transition of unknown origin. Results suggest that the Ormco and G&H products should have greater flexibility than the RMO products and that there should be significant differences in clinical force-degradation behavior for the Ormco and G&H products compared with the RMO products.

Statement of Problem: The color of dental porcelain depends on the type of metal substrate. Little research has been done to document the effects of different types of high-palladium alloys on the color of dental porcelain., Purpose: The purpose of this in vitro study was to evaluate the effects of different high-palladium alloys on the resulting color of dentin porcelain, as well as on that of opaque porcelain after simulated dentin and glazing firing cycles., Material and Methods: Three Pd-Cu-Ga alloys, Spartan Plus (S), Liberty (B), and Freedom Plus (F), and 5 Pd-Ga alloys, Legacy (L), IS 85 (I), Protocol (P), Legacy XT (X), and Jelenko No.1 (N), were examined. A Pd-Ag alloy, Super Star (T), was included for comparison to the high-palladium alloys, and the Au-Pd alloy, Olympia (O), served as the control. Six cast discs (16 x 1 mm) were prepared from each of the alloys. Shade B1 opaque porcelain (Vita-Omega) was applied at a final thickness of 0.1 mm. After 2 opaque porcelain firing cycles, the surfaces were airborne-particle abraded, and the specimens were divided into 2 groups. In the first group, 0.9 mm of B1 dentin porcelain was applied. The other group of specimens with only opaque porcelain underwent the same dentin porcelain and glazing firing cycles. Color differences (DeltaE) were determined with a colorimeter between the control and each experimental group, after the second opaque porcelain, second dentin porcelain, and glazing firing cycles. One-way analysis of variance and Dunnett's multiple range test were performed on the DeltaE data (alpha=.05)., Results: After the application of dentin porcelain, the 3 Pd-Cu-Ga alloys showed significantly different (P<.05) DeltaE values (S=2.3 +/- 0.5, B=1.4 +/- 0.3, and F=1.3 +/- 0.7) than the control group. After the glazing cycle of this group, the 3 Pd-Cu-Ga alloys and the Pd-Ag alloy exhibited significantly different (P<.05) DeltaE values (S=2.8 +/- 0.8, B=2.2 +/- 0.3, F=1.9 +/- 1.0, and T=1.4 +/- 0.5) than the control group. After the simulated dentin porcelain firing cycles, the specimens with only opaque porcelain exhibited significantly different (P<.05) DeltaE values (S=5.2 +/- 1.4, B=5.4 +/- 0.6, and F=3.9 +/- 0.2) than the control group. The color difference between the 3 Pd-Cu-Ga alloys with only opaque porcelain and the control group increased more after the simulated glazing cycle (S=6.6 +/- 1.5, B=6.3 +/- 0.5, and F=4.6 +/- 0.1). The observed color differences between the Pd-Ga alloys and the control group were not statistically significant at any point., Conclusions: The Pd-Cu-Ga alloys with only opaque porcelain, after the simulated dentin porcelain and glazing firing cycles, exhibited clinically unacceptable color differences. The application of dentin porcelain to the Pd-Cu-Ga alloys resulted in clinically acceptable color differences. The application of dentin porcelain to the Pd-Ag alloy, after the glazing firing cycle, resulted in clinically acceptable color differences (approximately 2.8 to 3.7 DeltaE CIELAB units). The Pd-Ag alloy specimens with only opaque porcelain did not exhibit significant color differences from the control group, whereas significant color differences from the control group after the dentin porcelain and glazing firing cycles were still clinically acceptable.

This in vitro study compared the force-deflection behavior of 6 superelastic nickel-titanium orthodontic archwires (0.016 x 0.022 in) under controlled moment and temperature. To simulate leveling, maxillary canine brackets and first molar tubes were bonded in such a manner as to remove the tip and angulation from the system. The wires (n = 10) were passively self-ligated into stainless steel brackets attached to an acrylic jig to simulate the maxillary arch. A testing machine recorded deactivations of 3 distances (5, 4, and 3 mm) at 37 degrees C in the canine position. Force-deflection measurements were recorded from the deactivations only. Forces produced during deactivation, at deflections of 2.5, 2.0, and 1.5 mm, were compared by analysis of variance. Significant differences (P < 0.0001) in forces were observed among the wires at the various deflections. All wires exhibited superelastic behavior, and rankings were derived according to statistically significant differences for each deflection distance.

Teeth with white spot lesions (WSL) might be more prone to enamel loss during bracket debonding. This in vitro study compared enamel loss from teeth with (n = 14) and without (n = 14) WSL after polishing with low-speed finishing burs or disks (Sof-Lex, 3M ESPE, St Paul, Minn). Debonded surfaces were analyzed with a contact stylus profilometer, and digitized data were compared with baseline readings by using AnSur NT software (Regents, University of Minnesota, Minneapolis, Minn). Specimen surfaces were also examined with a scanning electron microscope. Two-way analysis of variance was performed to analyze the data. In teeth without WSL, the volume losses were 0.16 mm(3) for the bur group and 0.10 mm(3) for the disk group; the mean maximum depths were 47.7 microm for the bur group and 54.3 microm for the disk group. In teeth with WSL, the volume losses were 0.06 and 0.17 mm(3), and the mean maximum depths were 35.1 and 48.7 microm for the bur and disk groups, respectively. There were no significant differences in enamel loss between the 2 groups of teeth without WSL (P =.12). However, in teeth with WSL, the burs removed less enamel than the disks (P = 0.006). Scanning electron microscope examination showed that any damage on the enamel surface was usually located in the cervical third of the teeth. On most specimens, even though tooth surfaces appeared resin-free to the naked eye, there were remnants of it. The differences between groups were so small that they might be clinically insignificant.

Discarded ProFile and ProTaper nickel-titanium rotary instruments, with unknown history of clinical use, were obtained from graduate endodontic clinics at Ohio State University and University of Texas Health Science Center at Houston Dental Branch. These discarded instruments and as-received instruments of both types were examined with a scanning electron microscope to investigate effects of clinical use and causes of failure. For used ProTaper instruments, dentinal debris was wedged mostly in narrow, radial, land-type regions and less on convex flute surfaces. For used ProFile instruments, dentinal debris was wedged mostly in the metal rollover and on concave flute surfaces. Used instruments of both types exhibited widened machining grooves, and elongated and stretched roll-over. Dentin chips were wedged in surface micro-cracks that appeared to propagate from original machining flaws and widen during in vivo root canal preparation. From our observational study, wedged dentinal deposits seem to play a pivotal role for clinical failure of these instruments.

A micro-X-ray diffraction (micro-XRD) technique has been employed to determine the phases in two superelastic nickel-titanium orthodontic wires that exhibit shape memory in the oral environment and one superelastic nickel-titanium wire that does not exhibit shape memory in vivo. The micro-XRD analyses were performed over the clinically relevant temperature range of 0-55 degrees C, which corresponds to the ingestion of cold and hot liquids, and both straight and bent (135 degrees ) test samples were analyzed. The results showed that for straight (as-received) test samples, the rhombohedral phase (R-phase) was definitely present in one shape memory wire product and perhaps in the other shape memory wire product, but was apparently absent in the superelastic wire product that did not display shape memory. Martensite was observed in all three wire products after bending. Phase transformations occurred with temperature changes simulating the oral environment for straight test samples of the two shape memory wires, but the micro-XRD pattern changed minimally with temperature for straight test samples of the superelastic wire and for bent test samples of all three wire products. The phase transformations revealed by micro-XRD were consistent with results recently found by temperature-modulated differential scanning calorimetry.

The appearances of the tip sections of ProFile 0.04 taper and Lightspeed 25-mm long, ISO size 25, nickel-titanium rotary instruments were compared with a scanning electron microscope in the as-received condition and after one, three, and six simulated clinical uses to prepare mesial canals of extracted mandibular molars. For the used ProFile instruments, there was some flattening of the characteristic material rollover and minor apparent wear at the edges of the flutes, but there was little change in the tip regions of the used Lightspeed instruments. Deposits on the surfaces of the instruments were attributed to the manufacturing processes and the in vitro preparation of root canals in the extracted teeth. The simulated clinical use did not cause substantial changes in the regions of these two brands of rotary instruments that are involved in the clinical preparation of root canals.

Differential scanning calorimetry (DSC) is a well-known method for investigating phase transformations in nickel-titanium orthodontic wires; the microstructural phases and phase transformations in these wires have central importance for their clinical performance. The purpose of this study was to use the more recently developed technique of temperature-modulated DSC (TMDSC) to gain insight into transformations in 3 nickel-titanium orthodontic wires: Neo Sentalloy (GAC International, Islandia, NY), 35 degrees C Copper Ni-Ti (Ormco, Glendora, Calif) and Nitinol SE (3M Unitek, Monrovia, Calif). In the oral environment, the first 2 superelastic wires have shape memory, and the third wire has superelastic behavior but not shape memory. All wires had cross-section dimensions of 0.016 x 0.022 in. Archwires in the as-received condition and after bending 135 degrees were cut into 5 or 6 segments for test specimens. TMDSC analyses (Model 2910 DSC, TA Instruments, Wilmington, Del) were conducted between -125 degrees C and 100 degrees C, using a linear heating and cooling rate of 2 degrees C per min, an oscillation amplitude of 0.318 degrees C with a period of 60 seconds, and helium as the purge gas. For all 3 wire alloys, strong low-temperature martensitic transformations, resolved on the nonreversing heat-flow curves, were not present on the reversing heat-flow curves, and bending appeared to increase the enthalpy change for these peaks in some cases. For Neo Sentalloy, TMDSC showed that transformation between martensitic and austenitic nickel-titanium, suggested as occurring directly in the forward and reverse directions by conventional DSC, was instead a 2-step process involving the R-phase. Two-step transformations in the forward and reverse directions were also found for 35 degrees C Copper Ni-Ti and Nitinol SE. The TMDSC results show that structural transformations in these wires are complex. Some possible clinical implications of these observations are discussed.

Objective. The purpose of this study was to employ transmission electron microscopy (TEM) to investigate the microstructures of Pd-Cu-Ga and Pd-Ga dental alloys that had been permanently deformed, in order to obtain information about the deformation behavior of individual phases and changes in microstructure brought about by that deformation.Methods. Heavily deformed regions taken from fractured tensile test bars of the two alloys in the as-cast condition were prepared for TEM analysis, using mechanical grinding and polishing, ion milling, and plasma cleaning. The specimens were examined in the TEM using bright-field and dark-field diffraction contrast imaging. Selected-area and convergent-beam electron diffraction patterns were employed to analyze the structures of the phases, and standardless energy-dispersive X-ray spectrometry was used to determine their mean compositions.Results. For both alloys, tweed structures underwent permanent deformation by twinning, whereas dislocation movement occurred in the face-centered cubic (fcc) palladium solid solution matrix. A body-centered cubic (bcc) phase, previously unreported in our TEM studies and containing a high density of dislocations, was identified in the Pd-Cu-Ga alloy, while fine-scale, stress-induced precipitates were found in some regions of the fcc matrix in the Pd-Ga alloy.Significance. The present results have provided novel information about the mechanical deformation behavior of high-palladium alloys. The stress-induced precipitation in the Pd-Ga dental alloy studied may be a critical component of strengthening mechanisms.

With the price volatility of palladium, there has been renewed interest in palladium-silver alloys for metal-ceramic restorations in dentistry. The microstructures of a popular Pd-Ag dental alloy were investigated in the as-cast and simulated porcelain-firing heat-treated conditions, using transmission electron microscopy. In the as-cast condition, the microstructure was strongly influenced by microsegregation, and contained the face-centered cubic Pd solid solution matrix, a eutectic structure with lattice parameters that varied for the two phases, and a face-centered tetragonal (fct) precipitate. After heat treatment, the lattice parameters for the two phases in the eutectic structure were uniform, and discontinuous precipitates with [011](matrix) habit planes and dislocations appeared in the matrix. An unusual nanostructured constituent was found in the fct set of eutectic lamellae in the heat-treated alloys., (Copyright 2003 Elsevier Science Ltd.)

Differential scanning calorimetric (DSC) analyses have been performed between -130 degrees and 100 degrees C on single-segment specimens obtained from ProFile and Lightspeed nickel-titanium rotary endodontic instruments in the as-received condition and after one, three, and six periods of simulated clinical use in extracted teeth. The DSC analyses showed that both brands of instruments were always in the superelastic condition, although the enthalpy values for the transformation from martensitic NiTi to austenitic NiTi were much smaller for the Lightspeed instruments. Simulated clinical use had no evident effect upon this transformation for both brands, which is attributed to insufficient mechanical deformation of the instruments. There were substantial differences in the enthalpy change associated with the transformation from martensitic NiTi to austenitic NiTi for test segments from different positions along the shafts of the instruments and for as-received instruments from two different batches that were analyzed in this study and a previous study. These differences are attributed to variations in work hardening along the shaft during instrument fabrication and to processing differences during production of the two batches of each instrument brand.

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 phase transformation behavior in three commercial nickel-titanium orthodontic wires having different transformation temperatures was studied by micro X-ray diffraction (micro-XRD). Micro-XRD spectra were obtained at three different included bending angles (135 degrees, 146 degrees and 157 degrees) and three different temperatures (25 degrees C, 37 degrees C and 60 degrees C). The regions analyzed by micro-XRD were within the separate areas of a given wire specimen that experienced only tensile or compressive strain. The intensity ratio (M002/A110) between the 002 peak for martensitic NiTi and the 110 peak for austenitic NiTi was employed as the index to the proportions of the martensite and austenite phases. The ratio of martensite to austenite increased in all three nickel-titanium wires with decreasing included bending angle (greater permanent bending deformation), and was lower within the compression area for all wires at all bending angles than within the tension area. Micro-XRD provides an effective method for quantitative evaluation of the proportions of these two phases in nickel-titanium orthodontic wires, even though considerable preferred crystallographic orientation exists because of the wire drawing process.

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.

Statement of Problem: The biocompatibility of high-palladium alloy restorations has been of some concern due to the release of palladium into the oral environment and sensitivity reactions in patients., Purpose: This study measured the in vitro elemental release from a Pd-Cu-Ga alloy and a Pd-Ga alloy into a corrosion testing medium., Material and Methods: Both alloys were cast into 12-mm-diameter x 1-mm-thick disks, subjected to heat treatment that simulated porcelain firing cycles, polished to a 0.05-mm surface finish, and ultrasonically cleaned in ethanol. Two specimens of each alloy were immersed 3 times (at 7, 70, and 700 hours) in an aqueous lactic acid/NaCl solution used for in vitro corrosion testing and maintained at 37 degrees C. The specimens were removed after each immersion time, and the elemental compositions of the solutions were analyzed with inductively coupled plasma-mass spectroscopy (ICP-MS). Elemental concentrations for the 2 alloys at each immersion time were compared with Student t test (alpha=.05)., Results: No significant differences in palladium release were found for the 7- and 70-hour solutions, but significant differences were found for the 700-hour solutions. Mean concentrations of palladium and gallium in the 700-hour solutions, expressed as mass per unit area of alloy surface, were 97 (Pd) and 46 (Ga) microg/cm(2) for the Pd-Cu-Ga alloy and 5 (Pd) and 18 (Ga) microg/cm(2) for the Pd-Ga alloy., Conclusion: Relative proportions of the elements in the solutions were consistent with the release of palladium and breakdown of microstructural phases found in the alloys. The results suggest that there may be a lower risk of adverse biological reactions with the Pd-Ga alloy than with the Pd-Cu-Ga alloy tested.

Statement of Problem: Corrosion of cast alloy restorations may lead to their failure or adversely affect their biocompatibility. Although some documentation of the corrosion behavior of the high-palladium dental alloys exists, questions remain about their corrosion resistance and mechanisms., Purpose: This study compared the in vitro corrosion characteristics of 3 high-palladium alloys and 1 gold-palladium alloy in simulated body fluid and oral environments., Material and Methods: Two Pd-Cu-Ga alloys and 1 Pd-Ga alloy were selected; an Au-Pd alloy served as the control. The corrosion behavior for the as-cast and simulated porcelain-firing (heat-treated) conditions of each alloy (N = 5) was evaluated in 0.9% NaCl, 0.09% NaCl, and Fusayama solutions. Heat-treated specimens of each alloy (N = 5) were also tested in N(2)-deaerated 0.09% NaCl and Fusayama solutions (pH 4). After immersion in the electrolyte for 24 hours, the open-circuit potential (OCP) was measured, and linear polarization was performed from -20 mV to +20 mV (vs. OCP) at a scanning rate of 0.125 mV/s. Cyclic polarization was performed from -300 mV to +1000 mV and back to -300 mV (vs. OCP) at a scanning rate of 1 mV/s. Data were evaluated with analysis of variance and the Ryan-Einot-Gabriel-Welsch multiple-range test (alpha=.05)., Results: The OCP of each alloy varied with the condition (as-cast or heat-treated) and electrolyte used. Corrosion resistance was similar for the 4 alloys tested. For cyclic polarization, all alloys showed active-passive or spontaneous passive behavior in nearly all electrolytes. During some reverse scans, the 3 high-palladium alloys displayed 3 or 5 anodic peaks. No positive hysteresis was observed for any of the alloy/electrolyte combinations evaluated., Conclusion: The corrosion resistances of the 3 high-palladium alloys in simulated body fluid and oral environments were comparable to that of the gold-palladium alloy. The similar corrosion resistance for the 3 high-palladium alloys was attributed to their high noble metal content and theorized stable structure at the submicron level. Selective corrosion of different phases and elements, surface enrichment of palladium, and adsorption of species are possible corrosion mechanisms. The cyclic polarization results suggest that none of the 4 alloys would be prone to pitting or crevice corrosion under in vivo conditions, but crevice conditions should nonetheless be avoided for these alloys in the oral environment.

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)

Statement of Problem: Crown fit is a prerequisite for long-term clinical success; however, crown distortion may occur during porcelain firing. The dimensional stability of some high-palladium alloys at high temperatures has been questioned., Purpose: The purpose of this study was to use a new method to measure the distortion of copings for metal-ceramic single units of selected high-palladium alloys with compositions representative of commercial alloys., Material and Methods: Four high-palladium alloys containing copper and 3 containing no copper were tested. A palladium-silver alloy was included for comparison, and a gold-palladium alloy served as the control. By using reference points scribed on the margin, the mesiodistal and buccolingual margin diameters of identical copings were measured with a traveling microscope at 4 stages: as-cast, oxidized, after 2 simulated opaque porcelain firings, and after 2 simulated dentin porcelain firings. The margin distortions for the various specimen groups representing combinations of alloys, stages, and measurement diameters were compared with the use of 1-way analysis of variance and a multiple range test., Results: Most of the high-palladium alloys had high-temperature distortions that were not significantly different from those of the control alloy. The distortions occurred principally during the oxidation cycle. The effect of mesiodistal groove reinforcement on preventing distortion was not the same for all alloys., Conclusion: The results suggest that small observed distortions of these alloys will not produce clinical problems. Several laboratory techniques are available to counteract the distortions.

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)

Purpose: The purpose of this study was to assess the effect of different high-palladium alloys on the resulting color of opaque porcelain. Three Pd-Cu-Ga alloys, Spartan Plus (S; Williams Dental Co/Division of Ivoclar North America, Amhest, NY), Liberty (B; J.F. Jelenko & Co, Armonk, NY), and Freedom Plus (F; J.F. Jelenko & Co); 4 Pd-Ga alloys, Legacy (L; J.F. Jelenko & Co), IS 85 (I; Williams Dental Co), Protocol (P; Williams Dental Co), and Legacy XT (X; J.F. Jelenko & Co); and a Pd-Ag alloy, Super Star (T; J.F. Jelenko & Co), were examined. The Au-Pd alloy Olympia (O; J.F. Jelenko & Co) served as the control., Materials and Methods: Three cast 16-mm discs, 1-mm thick, were prepared from each of the alloys. After metallurgically polishing and air-abrading, the specimens were oxidized following the manufacturer's recommendations. Shade B1 opaque porcelain (Vita-Omega; Vident, Baldwin Park, CA) was applied at a final thickness of 0.1 mm using a mold. After 2 opaque porcelain firing cycles, the surfaces were air-abraded. The colors of the specimens were measured using a colorimeter and expressed in Commission International de l'Eclairage (CIE) L*a*b* coordinates. Color differences (delta E) were determined between the control and each experimental group. Analysis of Variance and Tukey-Kramer tests were performed on the delta E data., Results: The 3 Pd-Cu-Ga alloys showed significantly greater (p < .01) delta E values (S = 2.8 +/- 1.1, B = 3.0 +/- 0.6, and F = 2.1 +/- 0.2) than the remaining 5 experimental groups (L = 0.7 +/- 0.5, I = 0.7 +/- 0.4, P = 0.7 +/- 0.2, X = 0.7 +/- 0.4, and T = 0.7 +/- 0.5). The directions of the significant color changes were relatively equally distributed along the L*, a*, and b* axes, and all delta L*, delta a*, and delta b* values were negative (lower value, more green and blue relative to control O)., Conclusions: This work suggests that a 0.1-mm-thick layer of opaque porcelain in the Pd-Cu-Ga alloys studied, did not reliably reproduce the color of porcelain.

Objective: The objective of this study was to determine the flexural strength (FS), compressive strength (CS), diametral tensile strength (DTS), Knoop hardness (KHN) and wear resistance of ten commercial glass-ionomer cements (GICs). The fracture surfaces of these cements were examined using scanning electron microscopic (SEM) techniques to ascertain relationships between the mechanical properties and microstructures of these cements., Methods: Specimens were fabricated according to the instructions from each manufacturer. The FS, CS, DTS, KHN and wear rate were measured after conditioning the specimens for 7 d in distilled water at 37 degrees C. One-way analysis of variance with the post hoc Tukey-Kramer multiple range test was used to determine which specimen groups were significantly different for each test. The fracture surface of one representative specimen of each GIC from the FS tests was examined using a scanning electron microscope., Results: The resin-modified GICs (RM GICs) exhibited much higher FS and DTS, not generally higher CS, often lower Knoop hardness and generally lower wear resistance, compared to the conventional GICs (C GICs). Vitremer (3M) had the highest values of FS and DTS; Fuji II LC (GC International) and Ketac-Molar (ESPE) had the highest CS; Ketac-Fil (ESPE) had the highest KHN. Ketac-Bond (ESPE) had the lowest FS; alpha-Silver (DMG-Hamburg) had the lowest CS. Four GICs (alpha-Fil (DMG-Hamburg), alpha-Silver, Ketac-Bond and Fuji II) had the lowest values of DTS, which were not significantly different from each other; alpha-Silver and Ketac-Silver had the lowest values of KHN. The highest wear resistance was exhibited by alpha-Silver and Ketac-Fil; F2LC had the lowest wear resistance. The C GICs exhibited brittle behavior, whereas the RM GICs underwent substantial plastic deformation in compression. The more integrated the microstructure, the higher were the FS and DTS. Higher CS was correlated with smaller glass particles, and higher KHN was found where there was a combination of smaller glass particles and lower porosity. Larger glass particle sizes and a more integrated microstructure contributed to a higher wear resistance., Significance: The mechanical properties of GICs were closely related to their microstructures. Factors such as the integrity of the interface between the glass particles and the polymer matrix, the particle size, and the number and size of voids have important roles in determining the mechanical properties.

Purpose: This study compared denture base resin shear bond strengths to silicoated Au-Pd, Au-Pd-Ag, Au-Ag-Pd-Cu, high-Pd, and Ni-Cr-Be alloys used to fabricate frameworks for hybrid implant prostheses. Microleakage between alloy and resin was also compared among groups after specimen fracture., Materials and Methods: Twelve cylindrical specimens were cast for each alloy. Each specimen was made from a ring-shaped pattern (diameter [d] = 12 mm and height = 4 mm) and machined to achieve uniform hollow centers (d = 6.5 mm). Castings were abraded with 250-micron aluminum oxide and ultrasonically cleaned in distilled water before silicoating. Denture base resin was processed to the internal surfaces of the silicoated specimens. All specimens were thermocycled (1,000 cycles) between 4 degrees C and 50 degrees C, and placed in basic fuchsin dye for a week. A punch (d = 3.8 mm) driven at a cross-head speed of 0.5 mm/min was used to push out the resin specimens. The force required to cause failure was converted to the nominal shear bond strength for each specimen, and mean shear bond strengths for the 5 groups of specimens (N = 12) were compared using one-way analysis of variance and the Tukey-Kramer HSD multiple range test (alpha = 0.05). Six of the 12 debonded resin samples for each alloy were selected at random and evaluated for dye penetration. Using an 80-square grid, the percentage of dye penetration was evaluated with an optical microscope (x25) to determine the percentage of grid area penetrated by the dye. One-way analysis of variance was used to compare the degree of microleakage among groups., Results: The mean resin-alloy shear bond strengths for the Au-Pd (9.6 +/- 3.7 MPa) and Au-Ag-Pd-Cu (9.2 +/- 1.5 MPa) alloys were significantly greater than mean resin-alloy shear bond strength for the Au-Pd-Ag alloy (5.6 +/- 1.9 MPa). No other significant differences in resin-alloy shear bond strengths were noted among the alloy groups. No significant differences were noted for dye penetration into the resin specimens bonded to any of the 5 alloys. The mean grid area penetrated by the dye was 25% when results for the alloys were pooled., Conclusions: Alloy type influences the shear bond strength of a denture base resin to silicoated alloys, but no difference in bond strength was found between Au-Pd, Au-Ag-Pd-Cu, high-Pd, and Ni-Cr-Be alloys. In addition, under the conditions of this study, all groups showed a similar degree of microleakage, which penetrated approximately 25% of the bonded specimen surface area.

The purpose of this study was to investigate the crystallographic characteristics of 3 sets of plasma-sprayed hydroxyapatite (HA) coatings prepared with different degrees of crystallinity on Ti-6Al-4V substrates. X-ray diffraction analyses were performed on the coatings to determine mean percent crystallinity, calcium phosphate phases present, average crystallite size, and residual strain. The mean percent crystallinity for the 3 sets of coatings ranged from 49 to 60%. The coatings that achieved the highest crystallinity consisted almost entirely of HA. As the coating crystallinity decreased, increasing amounts of alpha- and beta-tricalcium phosphate and tetracalcium phosphate were detected. The mean HA crystallite size for the 3 sets of coatings ranged from 0.02 to 0.05 micron. Differences in mean interplanar spacing for selected crystallographic planes of HA, compared with the pure ICDD (International Center for Diffraction Data) powder standards, implied that the coatings were in an uneven state of tensile strain.

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)

Objective: The objective of this study was to characterize the in vitro corrosion behavior of five high-palladium dental alloys in two media using a potentiodynamic polarization technique., Methods: Potentiodynamic cyclic polarization between -1000 and +1000 mV (SCE), 12 h open-circuit potential measurement, and linear polarization were performed on cast specimens of three Pd-Cu-Ga alloys and two Pd-Ga alloys in deaerated 0.09% NaCl solution and Fusayama artificial saliva at 37 degrees C. Zero-current potential, corrosion current density, open-circuit potential, and polarization resistance were determined. The Kruskal-Wallis test and the Mann-Whitney U-test were used to analyze the numeric findings., Results: The Pd-Cu-Ga and Pd-Ga alloys in both the as-cast and heat-treated conditions showed spontaneous passive behavior under electrochemical conditions similar to those in the oral environment. The Pd-Cu-Ga alloys Liberty and Spartan Plus exhibited increased activity in the Fusayama artificial saliva after the porcelain-firing heat treatment, which may have arisen from internal oxidation of casting defects. Heat-treated Freedom Plus had an unstable oxide film to form on the surface during anodic polarization and may have a limited tendency for pitting corrosion in the Fusayama artificial saliva. The two heat-treated Pd-Ga alloys remained passive in the test media. As a group, the high-palladium alloys exhibited satisfactory corrosion resistance., Significance: Corrosion of high-palladium alloys in the oral environment involves a release of ions that is related to their biocompatibility. Knowledge of the in vitro corrosion behavior of these alloys may lead to better understanding of any biologically adverse effects in vivo.

Statement of Problem: Little information is available on the optimum technique for soldering high-palladium alloys, which have gained considerable popularity for prosthodontic applications., Purpose: The objective of this study was to compare the flexural stress at the proportional limit of four noble dental alloy specimens soldered with torch, oven, and infrared-techniques., Materials and Methods: The high-palladium alloys studied were Legacy XT (Jelenko), Freedom Plus (Jelenko), and IS 85 (Williams/Ivoclar). A gold-palladium alloy, Olympia (Jelenko), served as the control. Thirty round bars, 18 x 3 mm, were cast from each alloy, cut in half, aligned, and joined using Olympia Pre solder (Jelenko) for the gas-oxygen torch and the infrared technique and Alboro LF solder (Jelenko) for the oven technique. Each soldered bar was subjected to three-point bending, and the maximum elastic stress or strength of the solder joint was calculated at the proportional limit. Data were analyzed by two-way ANOVA and the Ryan-Einot-Gabriel-Welsch (REGW) multiple range test at the 0.05 level of significance., Results: There was no significant difference between torch and oven-soldering, but both were significantly different from the infrared technique. ANOVA showed a significant difference between alloys, but this difference could not be detected with the REGW test. SEM examination of the fracture surfaces revealed grooves associated with the path of crack propagation. X-ray energy-dispersive spectroscopic analysis failed to detect copper in the solders, and there were no significant changes in the solder compositions after the melting procedures., Conclusions: All three techniques can yield satisfactory solder joints in high-palladium alloys. These joints should be well-polished to achieve optimal strength.

Purpose: This study assessed the effects of dental laboratory processing variables and testing medium on porcelain adherence of representative high-palladium alloys., Material and Methods: The processing variables were recasting two and three times, porcelain stripping with hydrofluoric acid and rebuilding, and changing the recommended oxidation procedures. The testing medium was air for these four groups and the nontreatment group. In the last group, the specimens were stored and tested in artificial saliva. The metal ceramic specimens were fractured with biaxial flexure in constant strain. The area fraction of adherent porcelain (%) was calculated with a standardized spectrometric technique. A gold-palladium alloy served as the control., Results: Recasting without adding new alloy negatively affected some high-palladium alloys. Porcelain stripping did not cause a decrease in adherence of the tested alloys. The alternate oxidation treatment reduced significantly the porcelain adherence of the Au-Pd and one Pd-Cu-Ga alloy. Storage and testing in artificial saliva did not significantly affect the porcelain adherence of the alloys. The Au-Pd alloy exhibited the highest porcelain adherence.

Objectives: The purpose of this study was to characterize the metal-ceramic bond of four commercial Pd-Ga alloys by two separate tests: porcelain adherence and bond failure force. A Pd-Ag alloy was the control. A secondary goal was to investigate a possible correlation between the percent porcelain retained and bond failure forces., Methods: For adherence testing, five cast plates of each alloy were air abraded and oxidized. The porcelain was applied on a circular area in the center of each plate and fractured using constant-strain flexure. The area fraction of adherent porcelain (%) was calculated via a standardized spectrometric technique. Bond failure forces were measured in three-point bending using bar specimens. The modulus of elasticity of the five alloys was also measured. No attempt was made to calculate bond strength since the residual thermal stresses at the interfacial region were unknown. Data were compared via ANOVA and the Tukey multiple range test (p < 0.05)., Results: All failures occurred at the porcelain termination sites with no tensile fracture of the porcelain. Two Pd-Ga alloys exhibited porcelain adherence comparable with previously studied Pd-Cu-Ga alloys. There was no correlation between the porcelain adherence and the force to failure (r2 = 0.0159). Additionally, no statistically significant differences were found among the moduli of elasticity of the five alloys., Significance: The new Pd-Ga alloys have been commercially introduced with little information on the quality of the bond with porcelain. The use of two different means for assessing the metal-ceramic bond provides information on the relationship of data using different experimental techniques.

Objective: The purpose of this study was to use transmission electron microscopy to examine four representative high-palladium alloys and gain insight into possible strengthening mechanisms., Methods: Castings of two Pd-Cu-Ga alloys and two Pd-Ga alloys were thinned by jet polishing and ion milling, followed by plasma cleaning, to yield foil specimens. Multiple specimens were prepared for each alloy. Bright-field images, dark-field images and selected-area electron diffraction patterns for the alloys in the as-cast condition, after simulated porcelain-firing heat treatment, and after annealing at 980 degrees C were analyzed by standard transmission electron microscope (TEM) techniques. The overall compositions of the ultrastructures for the specimen foils were determined by conventional standardless energy-dispersive spectroscopic analyses with the TEM, and mean values of the elemental compositions were compared to the nominal alloy compositions provided by the manufacturers., Results: There was generally good agreement (differences less than 2 wt%) between the overall ultrastructure composition and each nominal alloy composition, except for Protocol from which in may have been lost during casting or formed intermetallic compounds that were not detected by TEM. The same fine-scale tweed structure within parallel bands of approximately 100-200 nm width was observed for all four alloys in the as-cast condition and after simulated porcelain-firing heat treatment. The persistence of the ultrastructure in the specimens of the two Pd-Cu-Ga alloys annealed at 980 degrees C and quenched in ice water indicated very rapid formation from the palladium solid solution. The presence of ¿100¿ and ¿110¿ forbidden reflections for the <001> zone suggested that the tweed structure is ordered, although further research is necessary to establish this conclusion., Significance: The presence of a similar tweed structure in both the Pd-Cu-Ga alloys and the Pd-Ga alloys of substantially lower hardness shows that some other strengthening mechanism accounts for the high hardness and strength generally observed for Pd-Cu-Ga alloys.

The purpose of this study was to investigate the microstructure of plasma-sprayed hydroxyapatite coatings and the elemental composition near the coating-substrate interface for two commercial implants, using the scanning electron microscope. Both coating surfaces and cross-sectioned specimens were examined. The results indicated that while the surface microstructures of both implants were consistent with the plasma-spraying process, the scale of the constituents was much finer for one product. In cross-section, both coatings exhibited minimal porosity and intimate contact with the titanium alloy substrate. It was found that limited interdiffusion of titanium and calcium occurred near the interface.

Purpose: This investigation compared the Vickers hardness and microstructures of four recently marketed, palladium-based alloys for metal-ceramic restorations., Materials and Methods: Wax patterns simulating copings for maxillary central incisors were invested in a fine-grained, carbon-free, phosphate-bonded investment. Following burnout, the palladium alloys were fused with a gas-oxygen torch, centrifugally cast, and bench-cooled. Representative castings were embedded in transparent metallographic resin and sectioned to yield two mirror-image specimens. The specimens were evaluated in either the as-cast condition or following heat treatment simulating the firing cycles for Vita VMK porcelain. Vickers hardness measurements (n = 50) were made using a 1-kg load, and photomicrographs of polished and etched specimens were obtained with a scanning electron microscope., Results: The measured values of microhardness for the as-cast alloys were in excellent agreement with values reported by the manufacturer. The hardness in the as-cast condition was significantly greater for the Pd-Cu-Ga-In alloy, compared with the other three alloys, which did not contain copper. For the three high-palladium (> or = 75 wt%) alloys, there were small (4%-8%) decreases in hardness following heat treatment, whereas a larger decrease (13%) in hardness occurred for the Pd-Ag-In-Sn alloy after heat treatment. The porcelain firing cycles caused microstructural homogenization for all four alloys, and the relatively thick near-surface oxidation region in the Pd-Cu-Ga-In and Pd-Ag-In-Sn alloys was not observed in the two heat-treated Pd-Ga-Ag-In-Au alloys., Conclusions: The multiphasic microstructures of these alloys may have some significance for the in vitro and clinical corrosion behavior and the metal-ceramic bond strength. The hardness for the three high-palladium alloys may be controlled by submicroscopic precipitates that remain unaltered by heat treatment. The significantly greater hardness for the Pd-Cu-Ga-In alloy may cause greater difficulty for finishing castings in the dental laboratory compared with the other three alloys studied. The strengthening mechanism for the Pd-Ag-In-Sn alloy has significant temperature dependence, which might be exploited to achieve optimum mechanical properties.

Objective: The purpose of this study was to use x-ray diffraction (XRD) to obtain new information about the oxide layers on four representative oxidized high-palladium alloys., Methods: Cast specimens of two Pd-Cu-Ga alloys and two Pd-Ga alloys, with both polished and etched surfaces and air-abraded surfaces, were subjected to oxidation procedures recommended by the manufacturers. The specimens were analyzed by x-ray diffraction using CuK alpha radiation, and the peaks were compared to appropriate Joint Committee on Powder Diffraction Standards (JCPDS)., Results: The surface preparation procedure had a profound effect on the phases present in the oxide layers. For the specimens that had been polished and etched, CuGa2O4 and beta-Ga2O3 were detected on the 79Pd-10Cu-9Ga-2Au alloy, whereas SnO2 and CuGa2O4 were detected on the 76Pd-10Cu-5.5Ga-6Sn-2Au alloy. The oxide layers on both Pd-Cu-Ga alloys contained Cu2O1 and the oxide layer on the 76Pd-10Cu-5.5Ga-6Sn-2Au alloy may contain beta-Ga2O3. The principal phase in the oxide layers on both Pd-Ga alloys that had been polished and etched was ln2O3, which exhibited extreme preferred orientation. No other phase was detected in the oxide layer on the 85Pd-10Ga-2Au-1Ag-1 ln alloy, whereas beta-Ga2O3 was found in the oxide layer on the 75Pd-6Ga-6Au-6Ag-6.5ln alloy. For the air-abraded specimens, beta-Ga2O2 was not present in the oxide layers on the Pd-Cu-Ga alloys, and beta-Ga2O3 was the major phase in the oxide layers on the Pd-Ga alloys. Palladium oxide(s) in varying amounts were detected for both surface preparations of the Pd-Cu-Ga alloys and for the air-abraded Pd-Ga alloys. Except for the 76Pd-10Cu-5.5Ga-6Sn-2Au alloy, the oxide layer caused minimal change in the lattice parameter of the palladium solid solution compared to that for the as-cast alloy., Significance: Knowledge of the phases found in the oxide layers on these high-palladium alloys is of fundamental importance for interpreting differences in the adherence of dental porcelain to the metal substrates under static and dynamic conditions, and may provide guidance in the development of new high-palladium alloys with improved metal-ceramic bonding.

This study evaluated the shear bond strength of Rexillium III (Jeneric Pentron, Wallingford, CT) to enamel using various resin composite luting systems. Cast alloy cylinders (3.9 mm X 6.0 mm) were bonded with each cement to human molar buccal enamel surfaces (n = 8). The enamel was etched using a 35% phosphoric acid solution for 30 seconds. Bonded specimens were stored in distilled water for 7 days at 37 degrees C and thermocycled (1,500 cycles) in 5 degrees C and 55 degrees C water baths (1-minute dwell time). Specimens were randomly tested in shear using a crosshead speed of 0.5 mm per minute. Use of a one-way analysis of variance (P < .001) and Ryan-Einot-Gabriel-Welsh multiple range test showed significant differences between several of the resin cements. Panavia exhibited a significantly higher shear bond strength than any of the other cements tested.

This investigation studied the metal ceramic interface for two representative high-palladium alloys each of the Pd-Cu-Ga and Pd-Ga systems, using scanning electron microscopy and x-ray energy dispersive spectroscopy. The Pd-Cu-Ga alloys produced complex subsurface oxidation regions with thickness ranging from 15 to 20 microns for one alloy and 5 to 10 microns for the other alloy. Ga, In, and Sn accumulated at the interfaces, and Ga-rich deposits were found in the subsurface scale. One Pd-Ga alloy presented a surface oxidation region which dissolved in the ceramic, producing "islands" rich in Pd and Ga with a width that ranged from 1 to 2 microns. These islands were separated from the alloy by a band rich in Ga and Si which was 1 to 2.5 microns thick. While the other Pd-Ga alloy presented similar interfacial microstructures, the "islands" formed for this alloy were relatively sparse. The Pd-Cu-Ga alloys had a more favorable interface for metal ceramic bonding, which agrees with previous characterization of bond failures between these alloys and dental porcelain.

The purpose of this study was to determine the transformation temperatures for the austenitic, martensitic, and rhombohedral (R) structure phases in representative as-received commercial nitinol (NiTi) orthodontic wire alloys, to reconcile discrepancies among recent publications. Specimens were examined by differential scanning calorimetry (DSC) over a temperature range from approximately -170 degrees C to 100 degrees C, with a scanning rate of 10 degrees C per minute. Two different pathways, with the intermediate R structure either absent or present, were observed for the transformation from martensitic to austenitic NiTi, whereas the reverse transformation from austenitic to martensitic NiTi always included the R structure. The enthalpy (delta H) for the transformation from martensite to austenite ranged from 0.3 to 3.5 calories per gram. The lowest delta H value for the nonsuperelastic Nitinol wire is consistent with a largely work-hardened, stable, martensitic microstructure in this product. The DSC results indicate that the transformation processes are broadly similar in superelastic, body-temperature shape-memory, and nonsuperelastic NiTi wires. Differences in bending properties for the NiTi orthodontic wires at room temperature and 37 degrees C are due to the relative proportions of the metallurgical phases in the microstructures.

A common procedure in the fabrication of implant prostheses is the use of premade wrought cylinders in cast frameworks. Although manufacturers outline some precautions in the use of these components, detailed information about the metal interface between cylinders and cast alloys is lacking. This article, following a previous report that compared titanium-based implant cylinders used with two different classes of cast alloys, compares conventional noble metal cylinders from three different manufacturers combined with these two classes of cast noble alloys. Analysis of the as-received cylinders revealed that the implant cylinders as a group are predominantly composed of metals commonly found in noble dental alloys, namely, platinum, palladium, gold, and silver. The interfaces created by casting both high-fusing and low-fusing alloys around the cylinders exhibited a general elemental concentration variability compared with the bulk alloy regions, but continuous concentrations for shared elements suggested alloy-cylinder compatibility. Vickers hardness values, which ranged from 212 to 276 for the as-received cylinders, decreased from 12% to 43% for the various cylinders after casting. This study suggests characteristics of an ideal cast interface that include maintenance of the cylinder and casting alloy microstructures up to the interface, absence of interfacial reaction regions, lack of porosity created by volatilization of components from either alloy or the casting process, and sufficient strength to maintain anticipated loads.