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Improvement of in vitro titanium bioactivity by three different surface treatments.

OBJECTIVE: Dental implants are usually made from commercially pure titanium or titanium alloys. The aim of this investigation was to determine the influence of surface treatments of commercially pure titanium samples on in vitro bioactivity. METHODS: Commercially pure (cp) titanium (Ti) sheets were submitted to three different surface treatments, including, for all samples, etching with an HCl/H(2)SO(4) solution. Part of each etched sample was further submitted either to anodic oxidation by using an H(3)PO(4) solution or to thermal oxidation. Treated and non-treated samples were analyzed by using scanning electron microscopy (SEM), profilometry and photoelectron X-ray spectroscopy (XPS). The in vitro assessment was carried out through the immersion of samples in simulated body fluid (SBF). In vitro testing was carried out by SEM and by the determination of calcium (Ca) content in solution by atomic absorption spectrometry (AAS). The non-treated titanium samples were used as the control group. RESULTS: This study has shown that, after up to 7-day exposure, a calcium phosphate layer precipitated only on samples submitted to at least one of the three treatments used. This result, based on SEM images, is in good agreement with Ca content and XPS analysis, in which remarkable effects of surface modifications on Ti samples are highlighted. SIGNIFICANCE: These results suggest that suitable surface treatments, such as employed here, may improve in vitro titanium bioactivity in a SBF solution at 37 degrees C. This behavior suggests a possibility of a further favorable in vivo response.

Acid Etching, Dental↗

Effects of neurosurgical titanium mesh on radiation dose.

The purpose of this study was to determine the dosimetric impact of a neurosurgical titanium mesh in patients treated with 6- and 18-MV photon beams. The effects of a 0.4-mm-thick titanium mesh on the dose profile at 3 regions within a solid water phantom were measured using extended dose range-2 (EDR2) film for 6- and 18-MV photon beams. All measurements were performed with the titanium mesh placed at a depth of 1.5 cm in the phantom. Films were exposed immediately above the mesh, immediately below the mesh, and at a depth of 5 cm from the surface of the phantom. The films were scanned using a scanning densitometer. In the region directly above the titanium mesh, there was an increase in dose of 7.1% for 6-MV photons and 4.9% for 18-MV photons. Directly below the titanium mesh, there was an average decrease in dose of 1.5% for 6-MV photons and an increase of 1.0% for 18-MV photons. At 5-cm depth, for 6- and 18-MV photons, there was a decrease in dose of 2.2% and 0.6%, respectively. We concluded that for cranial irradiation with high-energy photons, the dosimetric impact of a 0.4-mm titanium mesh is small and does not require modification in treatment parameters.

Adult↗

Sphingomyelinase mediates macrophage activation by titanium particles independent of phagocytosis: a role for free radicals, NFkappaB, and TNFalpha.

The manner in which wear debris initiates intracellular signaling and macrophage activation remains poorly understood. While particle phagocytosis has been implicated in this process, recent studies have shown that phagocytosis is not required for macrophage activation. We examined the hypothesis that titanium particles stimulate macrophages through membrane associated signaling events involving free radicals, sphingomyelinase, NFkappaB, and TNFalpha. Titanium particles stimulated peroxidation of linoleic acid, producing malondialdehyde, while neither lipopolysaccharide nor PBS pre-incubated with particles did, suggesting that the increased peroxidation is related to the presence of the particles themselves. Furthermore, particles stimulated sphingomyelin metabolism in a neutral sphingomyelinase (NSmase) containing cell free system; this effect was inhibited by glutathione, indicating that NSmase activation was due to titanium induced free radicals. Titanium particles also stimulated NSmase activity in cultures of ANA-1 murine macrophages. Addition of purified NSmase to ANA-1 cell cultures stimulated NFkappaB binding, increased transcriptional activity in cells transfected with NFkappaB responsive promoters, and induced TNFalpha expression. These effects were also inhibited by addition of glutathione. Similarly, glutathione inhibited the ability of titanium particles to induce NFkappaB signaling and TNFalpha expression in ANA-1 cells. The findings demonstrate that titanium particles generate free radicals and induce plasma membrane peroxidation and NSmase activation. NSmase, in turn, hydrolyzes sphingomyelin, with activation of the NFkappaB signaling pathway and induction of responsive genes, including TNFalpha. This study demonstrates a mechanism for phagocytosis-independent macrophage activation and defines the sphingomyelin cycle as a potential therapeutic target for the prevention of wear debris induced osteolysis.

Animals↗

In vitro comparative analysis of the fit of gold alloy or commercially pure titanium implant-supported prostheses before and after electroerosion.

STATEMENT OF PROBLEM: For implant-supported prostheses, passive fit is critical for the success of rehabilitation, especially when alternative materials are used. PURPOSE: The purpose of this study was to compare interfacial fit of implant-supported prostheses cast in titanium to those cast in gold alloy. MATERIAL AND METHODS: Five 3-unit fixed partial dentures were fabricated in gold alloy (Degudent U) as 1-piece castings, and 5 others were similarly cast in commercially pure titanium (Grade 1). The interfacial gaps between the prostheses and the abutments were evaluated with an optical microscope, before and after electroerosion. Readings were made with both screws tightened (10 N.cm torque), and with only 1 side tightened, so as to also evaluate the passive fit of the prostheses. Data were compared statistically by 2-way analysis of variance and the post hoc Tukey multiple range test (alpha=.05). RESULTS: Before electroerosion, the interfacial gaps for the 1-piece prostheses were significantly smaller (P<.001) in the gold alloy group when the screws were tightened (Au=12.6 +/- 3.0 microm, compared to Ti=30.1 +/- 6.4 microm). When the side opposite the tightened side was analyzed, there was no significant difference between the gold alloy and titanium groups (Au=69.2 +/- 24.9 microm and Ti=94.2 +/- 39.6 microm). The electroerosion procedure significantly (P<.001) reduced the gaps at the interfaces for both groups under all conditions. Comparison between groups after electroerosion did not present significant differences when the side opposite the tightened side was analyzed, but the gold alloy group showed better fit when the tightened side was analyzed (12.8 +/- 1.4 microm for gold alloy; 29.6 +/- 4.4 microm for titanium) and when both screws were tightened (5.4 +/- 2.3 microm for gold alloy; 16.1 +/- 5.5 microm for titanium). CONCLUSIONS: Cast titanium prostheses, despite showing larger interfacial gaps between the prosthesis and abutment than those obtained with gold alloy, had improved fit after being subjected to electroerosion.

Analysis of Variance↗

The in vitro absorption of microfine zinc oxide and titanium dioxide through porcine skin.

Microfine metallic oxides such as titanium dioxide or zinc oxide have been found to be highly protective against harmful UV rays. Because their long-term use could potentially lead to health effects if significant amounts of these microfine metallic oxides would be absorbed through the skin, the in vitro absorption of microfine zinc oxide and titanium oxide in cosmetic formulations through porcine skin was investigated. In the experiments with a microfine zinc oxide formulation, the mean total recoveries of Zn were in the range from 102% to 107% of the total Zn applied. Virtually the total amount of applied Zn was recovered in the first five tape strips. The amounts of Zn found in the skin membrane and the receptor fluid were comparable in untreated, vehicle treated or test substance treated skin preparations. The absorption-time plots from diffusion cells treated with the vehicle did not differ from those treated with the ZnO containing formulation. In the experiments with microfine titanium dioxide formulations T-Lite SF-S and T-Lite SF, mean total recoveries of Ti ranged from 98% to 100% and 86% to 93% of the total Ti applied, respectively. Virtually the total amount of applied Ti could be removed from the skin surface by washing. The amounts of titanium found in the tape strips and skin preparations were in the order of the analytical determination limit. No Ti was found in the receptor fluid at any sampling time. The results show that neither zinc or titanium ions nor microfine zinc oxide or titanium dioxide particles were able to penetrate porcine stratum corneum. Therefore, from the absence of internal exposure we conclude that their use in sunscreens does not pose a health risk.

Animals↗

Unalloyed titanium for implants in bone surgery.

Commercially pure (c.p.) titanium has proven its suitability as an implant material in bone surgery over many years in the fields of osteosynthesis, oral implantology, and in certain applications in joint prosthetics. Excellent biocompatibility and corrosion resistance are outstanding features. Furthermore, c.p. titanium is known for not causing allergic reactions. The different grades of c.p. titanium and their minimum mechanical properties are specified in ISO and ASTM standards for implant materials. Typical mechanical properties are given for AO ASIF implant applications. The properties and clinical performance of c.p. titanium are discussed and compared to those of implant stainless steel and titanium alloys. In brief some specific features relating to c.p. titanium implant material are treated, including biocompatibility and soft tissue and bone response and taking into account the effects of implant surface configurations at the same time. In addition, issues are addressed which arise from frequent inquiries from clinics.

Alloys↗

Silane to enhance the bond between polymethyl methacrylate and titanium.

The machined surface of wrought titanium frameworks used in implant-supported, fixed prostheses does not bond well with acrylic resin. Surface pretreatment has been suggested to enhance the retention of polymethyl methacrylate to machined titanium surfaces. This study evaluated a new bonding material (Rocatec) to determine its effect on the bond strength between titanium and polymethyl methacrylate. Twenty rod-shaped specimens of grade 2 titanium (7.6 x 0.3 cm in diameter) were divided into two groups of 10 samples. Group A received no pretreatment and group B was pretreated with 110 microns alumina air abrasive and the Rocatec material. Heat-cured denture base resin was processed around each titanium sample in a cylindrical shape approximately 0.9 x 1.5 cm. A Shell-Nielsen shear test was performed with a universal testing machine at a crosshead speed of 0.5 mm/minute to determine the bond strength in megapascals (MPa). Group B specimens (23.8 +/- 1.78 MPa) had a shear strength 68% greater than group A (16.1 +/- 1.61 MPa) (p 0.0001). The results of this study indicated that surface pretreatment of grade 2 titanium with 110 microns alumina air abrasive plus Rocatec bonding material significantly enhances the shear bond strength to PMMA.

Air Pressure↗

Deflection fatigue of cobalt-chromium, titanium, and gold alloy cast denture clasp.

The aim of this study was to determine the fatigue resistance of the cast clasps of removable partial dentures. The different commercial types of metals used included five cobalt-chromium alloys, pure titanium, one titanium alloy (Ti-6A1-4V) and one gold alloy (type IV) that was either unhardened or age-hardened (n = 5 per group). The test method used was a constant-deflection fatigue test in which the force required to deflect the clasp for 0.6 mm and the number of loading cycles required to fracture the clasp were determined. The fatigue fracture surface of the clasps was examined with a scanning electron microscope. The results revealed that a fatigue fracture occurred in the cobalt-chromium clasp after approximately 25,000 loading cycles, in the pure titanium clasps after 4500 loading cycles, in the titanium alloy clasp after 20,000 loading cycles, and in the gold alloy clasp after 21,000 loading cycles. The means differed significantly (p < 0.001). Activation of the clasp by bending it 0.5 mm increased the fatigue resistance of the cobalt-chromium alloy and gold alloy clasps but decreased the fatigue resistance of both pure titanium and titanium alloy clasps (p < 0.005). The results of this study suggest that significant differences exist in the fatigue resistance of removable denture clasps made from different commercial cast metals, which may cause loss of retention of the removable partial denture and clasp failures.

Alloys↗

Effect of tip design of nickel-titanium and stainless steel files on root canal preparation.

The purpose of this study was to evaluate the effect of modified and non-modified tip designs of both stainless steel and nickel-titanium endodontic hand files on root canal preparation. Root canals of mesial roots of extracted mandibular molars were prepared using a quarter-turn-pull technique. The experimental design permitted comparison of the effects of nickel-titanium alloy construction or file tip modification alone, with effects when these two factors were incorporated into a single file design. Transportation, centering ratio, and dentin removal were evaluated using a modified Bramante technique. Nickel-titanium files, regardless of tip design, remained significantly more centered and demonstrated less apical transportation than stainless steel files at size 25. When instrumentation was continued to size 40 apically with step-back, there were no significant differences in transportation in the apical or coronal sections. However, during instrumentation to size 40 with step-back, the combination of modified tip and nickel-titanium alloy produced significantly more transportation and dentin removal, as well as greater deviation from the center at the mid-root level than did other file designs. Thus, of the file design parameters evaluated in this study, construction from nickel-titanium was most important in defining canal configuration at small file sizes in the apical region. Although the combination of nickel-titanium and modified tip design resulted in more transportation at larger file sizes in the midroot region, such alterations in canal configuration may be of little importance clinically. Nonetheless, it is suggested that other factors, such as tactile sensation and instrumentation technique, should be considered as important as the type of alloy or tip design.

Analysis of Variance↗

Radiographic appearance of titanium posts in endodontically treated teeth.

Titanium and titanium alloy posts are currently being used in complex dental restorations. Titanium posts have been shown to be less radiopaque than stainless steel and to have a radiographic density similar to gutta-percha. This radiographic similarity can make detection of a titanium post difficult. Failure to identify the presence of a titanium post before the initiation of retreatment could cause significant complications for the treating endodontist. Five cases are presented to describe the radiographic subtleties that can be used to detect the presence of a titanium post.

Dental Alloys↗

Corrosion susceptibility of titanium covered by dental cements.

OBJECTIVES: The aim of this study is to determine the influence of acidic fluorinated cements (as glass ionomer (GI) cements) on the passivation of titanium, using electrochemical investigations. METHODS: We realized experimental electrodes that associate titanium and dental cements. Polarization resistance of titanium electrodes has been determined for uncovered metal and electrodes covered with three dental cements. Student's t-tests proved the reproducibility. We also compared successive voltammograms for uncovered titanium and GI covered titanium. RESULTS: Correct passivation was observed with zinc eugenate, but fluorinated GI or zinc phosphate coverage increased the corrosion susceptibility. SIGNIFICANCE: However there is no evidence of titanium depassivation when covered with cement. No clinical contraindication can be held.

Coated Materials, Biocompatible↗

Characteristics of the surface oxides on turned and electrochemically oxidized pure titanium implants up to dielectric breakdown: the oxide thickness, micropore configurations, surface roughness, crystal structure and chemical composition.

Titanium implants have been used widely and successfully for various types of bone-anchored reconstructions. It is believed that properties of oxide films covering titanium implant surfaces are of crucial importance for a successful osseointegration, in particular at compromized bone sites. The aim of the present study is to investigate the surface properties of anodic oxides formed on commercially pure (c.p.) titanium screw implants as well as to study 'native' oxides on turned c.p. titanium implants. Anodic oxides were prepared by galvanostatic mode in CH3COOH up to the high forming voltage of dielectric breakdown and spark formation. The oxide thicknesses, measured with Auger electron spectroscopy (AES), were in the range of about 200-1000 nm. Barrier and porous structures dominated the surface morphology of the anodic film. Quantitative morphometric analyses of the micropore structures were performed using an image analysis system on scanning electron microscopy (SEM) negatives. The pore sizes were < or = 8 microm in diameter and had 1.27-2.1 microm2 opening area. The porosity was in the range of 12.7-24.4%. The surface roughness was in the range of 0.96-1.03 microm (Sa), measured with TopScan 3D. The crystal structures of the titanium oxide were amorphous, anatase, and a mixtures of anatase and rutile type, as analyzed with thin-film X-ray diffractometry (TF-XRD) and Raman spectroscopy. The chemical compositions consisted mainly of TiO2, characterized with X-ray photoelectron spectroscopy (XPS). The native (thermal) oxide on turned implants was 17.4 nm (+/- 6.2) thick and amorphous. Its chemical composition was TiO2. The surface roughness had an average height deviation of 0.83 microm (Sa). The present results are needed to elucidate the influence of the oxide properties on the biological reaction. The results of animal studies using the presently characterized surface oxides on titanium implants will be published separately.

Crystallography, X-Ray↗

Trabecular bone response to surface roughened and calcium phosphate (Ca-P) coated titanium implants.

The influence of calcium phosphate (Ca-P) coating and surface roughness on the trabecular bone response of titanium implants was investigated. Four types of titanium implants, i.e. blasted with titanium powder, sintered with titanium beads, titanium powder blasted and provided with an additional Ca-P coating, and titanium beads with Ca-P coating, were prepared. The Ca-P coating was deposited by ion beam dynamic mixing method. The Ca-P coating was rapid heat-treated with infrared radiation at 700 degrees C. The implants were inserted into the trabecular bone of the left and right femoral condyles of 16 rabbits. After implantation periods of 2, 3, 4 and 12 weeks, the bone-implant interface was evaluated histologically and histomorphometrically. Histological evaluation revealed new bone formation around different implant materials after already 3 weeks of implantation. After 12 weeks, mature trabecular bone surrounded all implants. At 3 and 4 weeks of implantation, no difference existed in bone contact to the various implant materials. On the other hand, after 12 weeks of implantation the highest percentage of bone contact was found around the Ca-P coated beads implants. Supported by the results, we concluded that the combination of surface geometry and Ca-P coating benefits the implant-bone response during the healing phase.

Animals↗

Mold filling of titanium alloys in two different wedge-shaped molds.

Pure titanium and titanium alloys are potential materials for the fabrication of cast dental appliances. One important factor in producing sound castings is the capacity of the metal to fill the mold. This study used a wedge-shaped mold to compare the mold filling of titanium with that of conventional dental casting alloys. The metals used were CP Ti, Ti-6Al-7Nb, Ti-6Al-4V, Ti with 1 and 4wt% Cu and ADA Type III gold alloy and an Ni-Cr alloy. The castings were cut into four pieces parallel to the triangular surface. Mold filling was evaluated as the distance between the tip of the cast wedge and theoretical tip of the triangle. The mold filling of the gold alloy was superior compared to all the metals tested, while the mold filling of the Ni-Cr alloy was the worst. There were no statistical differences at the 30 degrees marginal angle for all the cast titanium metals. At the sharper 15 degrees angle, CP Ti and Ti-6Al-7Nb was superior to both the Ti-Cu alloys. Although the mold filling of titanium was inferior compared to the gold alloy, the data justify the use of titanium for the production of dental appliances.

Dental Alloys↗

Fracture mechanisms of retrieved titanium screw thread in dental implant.

Titanium and its alloy are increasingly attracting attention for use as biomaterials. However, delayed fracture of titanium dental implants has been reported, and factors affecting the acceleration of corrosion and fatigue have to be determined. The fractured surface of a retrieved titanium screw and metallurgical structures of a dental implant system were analyzed. The outer surface of the retrieved screw had a structure different from that of the as-received screw. It was confirmed that a shear crack initiated at the root of the thread and propagated into the inner section of the screw. Gas chromatography revealed that the retrieved screw had absorbed a higher amount of hydrogen than the as-received sample. The grain structure of a titanium screw, immersed in a solution known to induce hydrogen absorption, showed features similar to those of the retrieved screw. It was concluded that titanium in a biological environment absorbs hydrogen and this may be the reason for delayed fracture of a titanium implant.

Biocompatible Materials↗

In vitro investigation of titanium and hydroxyapatite dental implant surfaces using a rat bone marrow stromal cell culture system.

In this study, rat bone marrow cells (RBM) were used to evaluate different titanium and hydroxyapatite dental implant surfaces. The implant surfaces investigated were: a titanium surface having a porous titanium plasma-sprayed coating (sample code Ti-TPS), a titanium surface with a deep profile structure (sample code Ti-DPS), an uncoated titanium substrate with a machined surface (sample code Ti-ma) and a machined titanium substrate with a porous hydroxyapatite plasma-sprayed coating (sample code Ti-HA). RBM cells were cultured on the disc-shaped test substrates for 14 days. The culture medium was changed daily and examined for calcium and phosphate concentrations. After 14 days specimens were examined by light microscopy, scanning electron microscopy, energy dispersive X-ray analysis and morphometry of the cell-covered substrate surface. All test substrates facilitated RBM growth of extracellular matrix formation. Ti-DPS and Ti-TPS to the highest degree, followed by Ti-ma and Ti-HA. Ti-DPS and Ti-TPS displayed the highest cell density and thus seem to be well suited for the endosseous portion of dental implants. RBM cells cultured on Ti-HA showed a delayed growth pattern. This may be related to its high phosphate ion release.

Animals↗

Detachment of titanium and fluorohydroxyapatite particles in unloaded endosseous implants.

The shape, surface composition and morphology of orthopaedic and endosseous dental titanium implants are key factors to achieve post-surgical and long-term mechanical stability and enhance implant osteointegration. In this study a comparison was made between 12 titanium screws, plasma-spray-coated with titanium powders (TPS), and 12 screws with an additional coating of fluorohydroxyapatite (FHA-Ti). Screws were implanted in the femoral and tibial diaphyses of two mongrel sheep and removed with peri-implant tissues 12 weeks after surgery. The vibrational spectroscopic, ultrastructural and morphological analyses showed good osteointegration for both types of implants in host cortical bone. The portion of the FHA-Ti implants in contact with the medullary canal showed a wider area of newly formed peri-implant bone than that of the TPS implants. Morphological and EDAX analyses demonstrated the presence of small titanium debris in the bone medullary spaces near the TPS surface, presumably due to the friction between the host bone and the implant during insertion. Few traces of titanium were detected around FHA-Ti implants, even if smaller FHA debris were present. The present findings suggest that the FHA coating may act as a barrier against the detachment of titanium debris stored in the medullary spaces near the implant surface.

Animals↗

Investigation of the dissolution of the bioceramic hydroxyapatite in the presence of titanium ions using ToF-SIMS and XPS.

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS) analyses have been used to investigate the dissolution of hydroxyapatite in the presence of titanium chloride suggesting the substitution of titanium ions for calcium in the hydroxyapatite structure. The surface analytical data suggest that titanium was incorporated within the solid phase as titanium phosphate. Comparison of relative ion intensities in the ToF-SIMS spectra reveals changes in the composition of the surface chemistry of hydroxyapatite. These relative ion intensities show that the maximum surface uptake of titanium occurred at a solution concentration of 500 ppm titanium chloride for a time of incubation of 30 min. These data correlate with that obtained using XPS highlighting the semi-quantitative information which ToF-SIMS can provide.

Biocompatible Materials↗