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Cyclic fatigue testing of nickel-titanium endodontic instruments.

Cyclic fatigue of nickel-titanium, engine-driven instruments was studied by determining the effect of canal curvature and operating speed on the breakage of Lightspeed instruments. A new method of canal curvature evaluation that addressed both angle and abruptness of curvature was introduced. Canal curvature was simulated by constructing six curved stainless-steel guide tubes with angles of curvature of 30, 45, or 60 degrees, and radii of curvature of 2 or 5 mm. Size #30 and #40 Light-speed instruments were placed through the guide tubes and the heads secured in the collet of a Mangtrol Dynamometer. A simulated operating load of 10 g-cm was applied. Instruments were able to rotate freely in the test apparatus at speeds of 750, 1300, or 2000 rpm until separation occurred. Cycles to failure were determined. Cycles to failure were not affected by rpm. Instruments did not separate at the head, but rather at the point of maximum flexure of the shaft, corresponding to the midpoint of curvature within the guide tube. The instruments with larger diameter shafts, #40, failed after significantly fewer cycles than did #30 instruments under identical test conditions. Multivariable analysis of variance indicated that cycles to failure significantly decreased as the radius of curvature decreased from 5 mm to 2 mm and as the angle of curvature increased greater than 30 degrees (p < 0.05, power = 0.9). Scanning electron microscopic evaluation revealed ductile fracture as the fatigue failure mode. These results indicate that, for nickel-titanium, engine-driven rotary instruments, the radius of curvature, angle of curvature, and instrument size are more important than operating speed for predicting separation. This study supports engineering concepts of cyclic fatigue failure and suggests that standardized fatigue tests of nickel-titanium rotary instruments should include dynamic operation in a flexed state. The results also suggest that the effect of the radius of curvature as an independent variable should be considered when evaluating studies of root canal instrumentation.

American Dental Association↗

Comparison of cutting efficiency and instrumentation of curved canals with nickel-titanium and stainless-steel instruments.

The cutting efficiency and the effects of instrumentation on curved canal shape of both stainless-steel and nickel-titanium nonstandardized ProFile Series 29 hand instruments and stainless-steel Flexoreamer were investigated under standardized conditions. Concerning cutting efficiency in rotary motion, the Flexoreamer had significantly (p < 0.01) greater cutting efficiency than stainless-steel ProFiles and nickel-titanium ProFiles. Changes in the canal shape differed significantly between the different instruments at all measuring points (p < 0.001). After instrumentation with Flexoreamers with inclusion of two half-sizes (#17 and #22), there were fewer undesirable changes in canal shape compared with both stainless-steel and nickel-titanium ProFile Series 29 instruments. In this study, it seemed that flexible stainless-steel instruments with noncutting tips were superior to the nonstandardized ProFile Series 29 instruments with regard to cutting efficiency and instrumentation of curved canals.

Analysis of Variance↗

Joint strength of laser-welded titanium.

OBJECTIVE: The objective of this study was to examine the joint strength of titanium laser-welding using several levels of laser output energy [current (A)]. METHODS: Cast titanium plates (0.5 x 3.0 x 40 and 1.0 x 3.0 x 40 mm(3)) were prepared and perpendicularly cut at the center of the plate. After the cut halves were fixed in a jig, they were laser-welded using a Nd: YAG laser at several levels of output energy in increments of 30A from 180 to 300A. The penetration depths of laser to titanium were measured under various conditions for output energy, pulse duration, and spot diameter to determine the appropriate conditions for these parameters. Based on the correlation between the results obtained for penetration depth and the size of the specimens (thickness: 0.5 and 1.0 mm, width: 3.0 mm), the pulse duration and spot diameter employed in this study were 10 ms and 1.0 mm, respectively. Three laser pulses (spot diameter: 1.0 mm) were applied from one side to weld the entire joint width (3.0 mm) of the specimens. Uncut specimens served as the non-welded control specimens. Tensile testing was conducted at a crosshead speed of 2 mm/min and a gage length of 10 mm. The breaking force (N) was recorded, and the data (n=5) were statistically analyzed. RESULTS: For the 0.5 mm thick specimens, the breaking force of the specimens laser-welded at currents of 240, 270, and 300A were not statistically (P>0.05) different from the non-welded control specimens. There were no significant differences in breaking force among the 1.0mm thick specimens laser-welded at currents of 270 and 300A, and the non-welded control specimens. SIGNIFICANCE: Under appropriate conditions, joint strengths similar to the strength of the non-welded parent metal were achieved.

Aluminum Silicates↗

Evaluating mechanical adhesion of sol-gel titanium dioxide coatings containing calcium phosphate for metal implant application.

The adhesion of thin (< 10 microm) sol-gel calcium phosphate-titanium dioxide films bonded to a titanium substrate was studied using two different tests: a rotating-bending test and a tensile bond test. The former evaluates the impact of both the coating procedure and the surface pre-treatment on the resistance to fatigue of the substrate as well as the adhesion of the coating; the latter measures the tensile adhesion strength of the coating. Both tests gave similar results. A reduction of the thickness of the coating or an increase of the roughness of the substrate improves the quality of the interface. A comparison of the adhesion of the calcium phosphate-titanium dioxide film with that of a pure calcium phosphate coating obtained by a similar route suggests the involvement of a chemical component in the binding.

Calcium Phosphates↗

Effect of calcium-ion implantation on the corrosion resistance and biocompatibility of titanium.

This work presents data on the structure and corrosion resistance of titanium after calcium-ion implantation with a dose of 10(17) Ca+/cm2. The ion energy was 25 keV. Transmission electron microscopy was used to investigate the microstructure of the implanted layer. The chemical composition of the surface layer was examined by XPS and SIMS. The corrosion resistance was examined by electrochemical methods in a simulated body fluid (SBF) at a temperature of 37 degrees C. Biocompatibility tests in vitro were performed in a culture of human derived bone cells (HDBC) in direct contact with the materials tested. Both, the viability of the cells determined by an XTT assay and activity of the cells evaluated by alkaline phosphatase activity measurements in contact with implanted and non-implanted titanium samples were detected. The morphology of the cells spread on the surface of the materials examined was also observed. The results confirmed the biocompatibility of both calcium-ion-implanted and non-implanted titanium under the conditions of the experiment. As shown by TEM results, the surface layer formed during calcium-ion implantation was amorphous. The results of electrochemical examinations indicate that calcium-ion implantation increases the corrosion resistance, but only under stationary conditions; during anodic polarization the calcium-ion-implanted samples undergo pitting corrosion. The breakdown potential is high (2.7-3 V).

Alkaline Phosphatase↗

Carbonate apatite coating on titanium induced rapidly by precalcification.

Chemical treatments have been thought to be promised methods for improving bioactivity of titanium. In this work, the effect of precalcification with boiling saturated Ca(OH)2 solution on bioactivation of titanium was investigated. After precalcification and soaking in supersaturated Ca-P solution (SCP), calcium phosphate rapidly precipitated onto the surfaces of titanium, and after only three days an uniform apatite layer was found up to thickness of a few micrometers. The observation using scanning electron microscopy (SEM) showed that the coating was composed of a number of small crystal grains. The investigation by X-ray energy dispersion spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) indicated that the coating was Ca-deficient carbonate apatite. Based on the analyses for the surfaces and SCP, a mechanism of precipitation of apatite was proposed in thermal dynamics and kinetics.

Apatites↗

Micro X-ray diffraction study of superelastic nickel-titanium orthodontic wires at different temperatures and stresses.

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.

Alloys↗

Hydrothermal modification of titanium surface in calcium solutions.

Hydrothermal modification of a titanium surface in calcium solutions was performed. The apatite precipitation on the modified surface in Hanks' solution, as a simulated body fluid, was evaluated and the surface microstructure changes after the modification were characterized by thin-film X-ray diffractometry (TF-XRD) and X-ray photoelectron spectroscopy (XPS). Hydrothermal modification in CaO solution enhanced the precipitation of apatite on the titanium surface. High pH, high pressure and high temperature of the CaO solution increased the thickness of the surface-modified layer and enhanced the synthesis of calcium titanate which possibly promoted the precipitation of apatite in Hanks' solution. Hydrothermal modification in CaCl2 solution, on the other hand, showed reverse effects. The modification of titanium in CaO solution with hydrothermal treatment is expected to result in excellent osteointegration and can be easily performed by using an autoclave, a clinical apparatus widely used.

Apatites↗

Bone response to calcium phosphate-coated and bisphosphonate-immobilized titanium implants.

Thin calcium phosphate (Ca-P) coatings have been introduced to overcome the shortcomings of plasma-sprayed Ca-P coatings. In our previous experiments, thin Ca-P coatings also enabled the immobilization of bisphosphonate, which is a drug used to treat osteoporosis. The present study was designed to evaluate the bone response to titanium implants treated with a thin Ca-P coating and bisphosphonate. Forty cylindrical commercially pure titanium implants with a length of 7 mm and a diameter of 3 mm were used as test implant fixtures. Three groups of surface-treated implants were prepared: (1) blasted with titanium powder and etched with a solution of 10% HF + 5% HNO3 (control); (2) modified with 0.5-microm thick Ca-P coatings and rapid heat-treating, and (3) immobilized with bisphosphonate by immersion in pamidronate disodium solution (10(-2) M) for 24 h at 37 degrees C. These surface-treated implants were inserted into edentulous areas in the mandibular molar region of five beagle dogs. After implantation periods of 4 and 12 weeks, the bone implant interface was evaluated histologically and histomorphometrically. All measurements were statistically evaluated using a one-way ANOVA and Fisher PLSD test for multiple comparisons among the means. Four weeks after the implantation, higher percentage of bone contact was found around the thin Ca-P-coated implants compared to that of the control group. The highest percentage of bone contact was found around the bisphosphonate-immobilized implants after 12 weeks of implantation. These data suggest that a thin coating of calcium phosphate followed by bisphosphonate-immobilization is effective in the promotion of osteogenesis on surfaces of dental implants.

Animals↗

Effect of phosphorus-ion implantation on the corrosion resistance and biocompatibility of titanium.

This work presents data on the structure and corrosion resistance of titanium after phosphorus-ion implantation with a dose of 10(17)P/cm2. The ion energy was 25keV. Transmission electron microscopy was used to investigate the microstructure of the implanted layer. The chemical composition of the surface layer was examined by X-ray photoelectron spectroscopy and secondary ion mass spectrometry. The corrosion resistance was examined by electrochemical methods in a simulated body fluid at a temperature of 37 C. Biocompatibility tests in vitro were performed in a culture of human derived bone cells in direct contact with the materials tested. Both, the viability of the cells determined by an XTT assay and activity of the cells evaluated by alkaline phosphatase activity measurements in contact with implanted and non-implanted titanium samples were detected. The morphology of the cells spread on the surface of the materials examined was also observed. The results confirmed the biocompatibility of both phosphorus-ion-implanted and non-implanted titanium under the conditions of the experiment. As shown by transmission electron microscope results, the surface layer formed during phosphorus-ion implantation was amorphous. The results of electrochemical examinations indicate that phosphorus-ion implantation increases the corrosion resistance after short-term as well as long-term exposures.

Biocompatible Materials↗

Electrochemical characterization of cast titanium alloys.

A reaction layer forms on cast titanium alloy surfaces due to the reaction of the molten metal with the investment. This surface layer may affect the corrosion of the alloy in the oral environment. The objective of this study was to characterize the in vitro corrosion behavior of cast titanium alloys. ASTM Grade 2 CP titanium, Ti-6Al-4V, Ti-6Al-7Nb and Ti-13Nb-13Zr alloys were cast into a MgO-based investment. Experiments were performed on castings (N=4) with three surface conditions: (A) as-cast surface after sandblasting, (B) polished surface after removal of the reaction layer, and (C) sandblasted surface after removal of the reaction layer. Open-circuit potential (OCP) measurement, linear polarization, and potentiodynamic cathodic polarization were performed in aerated (air+10% CO(2)) modified Tani-Zucchi synthetic saliva at 37 degrees C. Potentiodynamic anodic polarization was subsequently conducted in the same medium deaerated with N(2)+10% CO(2) gas 2 h before and during the experiment. Polarization resistance (R(P)) and corrosion rate (I(CORR)) were calculated. Numerical results were subjected to nonparametric statistical analysis at alpha=0.05. The OCP stabilized for all the specimens after 6 x 10(4)s. Apparent differences in anodic polarization were observed among the different surfaces for all the metals. A passivation region followed by breakdown and repassivation were seen on specimens with surfaces A and C. An extensive passive region was observed on all the metals with surface B. The Kruskal-Wallis test showed no significant differences in OCP, R(p), I(CORR) or break down potential for each of the three surfaces among all the metals. The Mann-Whitney test showed significantly lower R(P) and higher I(CORR) values for surface C compared to the other surfaces. Results indicate that the surface condition has more effect on corrosion of these alloys than the surface reaction layer. Within the oxidation potential range of the oral cavity, all the metal/surface combinations examined showed excellent corrosion resistance.

Alloys↗

Bone tissue reconstruction using titanium fiber mesh combined with rat bone marrow stromal cells.

The study aim was to evaluate the effect of bone marrow stromal cells (BMSCs) cultured in titanium fiber mesh and implanted in a rat cranial defect. A total of 24 titanium meshes were placed in a tube containing 10 ml BMSC suspension (3 x 10(6)cells/ml) and the tube was rotated on a rotation plate (2 rpm) during 3 h. Thereafter, meshes with cells were subcultured for 1 day under standard conditions. Cell-loaded implants and non-cell-loaded controls were placed in a 8 mm cranial defect and retrieved after 3, 15 and 30 days of implantation. Histology showed that after 3 days of implantation, the mesh porosity of both implant groups was mainly invaded with blood cells. On the other hand, at 15 days of implantation, the cell-loaded implants were filled for 15 +/- 10% of their volume with bone, while the controls showed 1.5 +/- 3.5% of bone. The 30-day cell-loaded implants showed 40 +/- 12.5% of bone and the 30-day control implants 17 +/- 14.5%. At both implantation times the differences were statistically significant. Therefore, we conclude that inoculation of titanium fiber mesh with BMSCs can improve the bone healing capacity of this material.

Animals↗

In situ imaging and impedance measurements of titanium surfaces using AFM and SPIS.

Surfaces of commercially pure titanium and titanium, 6-aluminum, 4-vanadium were subjected to simultaneous polarization/impedance testing and in situ electrochemical atomic force microscopy imaging to evaluate how the structure and properties of the passive oxide film is affected by varying potential and hydration. Current transients were acquired via a step polarization impedance spectroscopy technique: the voltage was stepped between -1 and 1 V in 50 mV increments, while current transients and surface morphology were digitally recorded. Numerical Laplace transformation applied to the current transient data provided frequency-dependent admittance (impedance(-1)). Simultaneous AFM imaging of dry surfaces, initially hydrated surfaces, and surfaces immersed and changing with potential revealed that all sample surfaces were covered with protective titanium oxide domes that grew in area and coalesced due to hydration and as a function of increasing applied voltage and time. Reversal of dome growth did not occur upon voltage reduction, while impedance behavior was quasi-reversible, suggesting independence between structural and electrical properties. Oxide growth appeared to occur in part by lateral spreading and overgrowth of domes at the oxide-solution interface. Interfacial impedance data reflect oxide passivity and n-type semiconductor behavior. Non-linear Mott-Schottky fits specified multi-layer donor concentrations between 10(18) and 10(19)cm(-3), depending on the surface.

Alloys↗

Repair of segmental long bone defect in rabbit femur using bioactive titanium cylindrical mesh cage.

A segmental rabbit femur defect was repaired using an empty bioactive titanium (BAT) mesh cage. A 10mm long titanium mesh cage was positioned in the bony defect and reinforced by intramedullary fixation. The BAT surface was prepared by chemical and thermal treatment. Pure titanium cages were used as a control. Torsional stiffness of the BAT group at 4 weeks was approximately equal to, and at 8 weeks twice, that of the intact femur. Differences between the torsional stiffness of the control and BAT groups were significant at both time intervals. Histological examinations showed that woven bone appeared around the cage by 4 weeks and transformed to lamella bone by 8 weeks. New bone bonded to the BAT surface without an intervening layer. The BAT cage enhanced the bone repairing process and achieved faster repair of long bone segmental defects.

Animals↗

The influence of niobium and vanadium on passivity of titanium-based implants in physiological solution.

Surface films play a key role in corrosion and osteointegration processes of titanium-based orthopedic implants. The influence of niobium and vanadium as alloying elements on titanium alloy passivity have been investigated in Hanks' Balanced Salt Solution (HBSS), at 37 degrees C and pH 6.9.Ti6Al4V and Ti6Al6Nb have been considered. The excellent passivating properties of the anodically formed Ti(IV)-based surface oxide film and high corrosion resistance of the Ti6Al6Nb alloy have been attributed to the stabilizing effect of Nb(5+) cations on the passive film, by annihilation of stoichiometric defects (anion vacancies) caused by the presence of titanium suboxides. Localized corrosion sensitivity of the Ti6Al4V alloy has been correlated to the dissolution of vanadium at the surface film/electrolyte interface coupled with generation of cation vacancies and their diffusion through the film as a part of the solid-state diffusion process. The presence of a high concentration of chloride ions (0.15gl(-1)) in HBSS further accelerates these processes.

Alloys↗

Influence of sterilization on the mineralization of titanium implants induced by incubation in various biological model fluids.

The aim of this work was to investigate the effect of the sterilization processes on the mineralization of titanium implants induced by incubation in various biological model fluids. Titanium samples were submitted to the following sterilization processes used for implant materials: steam autoclaving, glow discharge Ar plasma treatment and gamma-irradiation. The modification of the treated surfaces was evaluated by contact angle determinations, X-ray photoelectron spectroscopy (XPS), laser profilometry and X-ray diffraction. The most significant modifications were detected on the wettability: while the samples treated with Ar plasma became highly hydrophilic (water contact angle approximately 0 degrees), gamma-irradiation and steam sterilization induced an increase in the hydrophobicity. After being sterilized, the samples were incubated for one week in three biological model fluids: Hanks' Balanced Salt Solution, Kokubo's simulated body fluid (SBF) and a fluid, designated by SBF0, with the same composition of SBF but without buffer TRIS. The level of mineralization of the incubated Ti samples, assessed by dynamic contact angle analysis, scanning electron microscopy, electron dispersive spectroscopy and XPS, indicated that the early stages of mineralization are essentially independent of the sterilization method. In contrast, the incubating fluid plays a determinant role, SBFO being the most efficient medium for biomineralization of titanium.

Biocompatible Materials↗

Peptide functionalized poly(L-lysine)-g-poly(ethylene glycol) on titanium: resistance to protein adsorption in full heparinized human blood plasma.

The graft copolymer poly(L-lysine)-graft-poly(ethylene glycol) (PLL-g-PEG) and its RGD- and RDG-functionalized derivatives (PLL-g-PEG/PEG-peptide) were assembled from aqueous solutions on titanium (oxide) surfaces. The polymers were characterized by NMR in order to determine quantitatively the grafting ratio, g (Lys monomer units/PEG side chains), and the fraction of the PEG side chains carrying the terminal peptide group. The titanium surfaces modified with the polymeric monomolecular adlayers were exposed to full heparinized blood plasma. The adsorbed masses were measured by in situ ellipsometry. The different PLL-g-PEG-coated surfaces showed, within the detection limit of the ellipsometric technique, no statistically significant protein adsorption during exposure to plasma for 30 min at 22 degrees C or 37 degrees C, whereas clean, uncoated titanium surfaces adsorbed approximately 350 ng/cm2 of plasma proteins. The high degree of resistance of the PEGylated surface to non-specific adsorption makes peptide-modified PLL-g-PEG a useful candidate for the surface modification of biomedical devices such as implants that are capable of eliciting specific interactions with integrin-type cell receptors even in the presence of full blood plasma. The results refer to short-term blood plasma exposure that cannot be extrapolated a priori to long-term clinical performance.

Blood Proteins↗

Histological and mechanical investigation of the bone-bonding ability of anodically oxidized titanium in rabbits.

The purpose of this study was to histologically and mechanically investigate the in vivo bone-bonding ability of anodically oxidized titanium (AO Ti) with an anatase crystal layer on its surface. AO Ti plates, anodically oxidized at 155 V in 1 M H2SO4, were implanted into the proximal metaphyses of mature rabbit tibiae for 4, 8, 16, and 24 weeks and investigated by light microscopy, scanning electron microscopy and detaching test. High bone-bonding ability, comparable to our previous study data of the bioactive titanium produced by sodium-free alkali and heat treatment, was observed at the early stages of implantation. However, no substantial increase was demonstrated. AO Ti plates bonded to bone directly, with no intervening soft tissue layer, and no breakage of the AO Ti layer was observed. The AO Ti layer was porous through to the titanium substrate, while the porosity was low. Apatite-like deposition into the pores of the AO layer was observed only in the superficial zone. The lack of improvement of bone-bonding ability in the later stages of implantation may be attributed to the low porosity and to the superficial ingrowths of apatite-like deposits into the pores of the AO Ti layer.

Animals↗