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PubMed2002

Hydroxyapatite formation on alkali-treated titanium with different content of Na+ in the surface layer.

Titanium can form a bone-like apatite layer on its surface in SBF when it is treated in NaOH. When pre-treated titanium is exposed to SBF, the alkali ions are released from the surface into the surrounding fluid. The Na+ ions increase the degree of supersaturation of the soaking solution with respect to apatite by increasing pH. On the other hand, the released Na+ cause an increase in external alkalinity that triggers an inflammatory response and leads to cell death. Therefore, it would be beneficial to decrease the release of Na+ into the surrounding tissue. The purpose of this study was to evaluate the hydroxyapatite formation on alkali-treated titanium with different content of Na+ in the surface layer. Using SEM, gravimetric analysis and measurement of calcium and phosphate concentration, it was found that the rate of apatite formation was not significantly influenced by a lower amount of Na+ in the surface layer. Titanium with the lowest content of Na+ could be more suitable for implantation in the human body. The amount of alkali ions released in the surrounding tissue is lower and the rate of apatite formation is identical to titanium with the highest content of Na+ in the surface layer.

Alkalies↗
PubMed2003

Immuno-inflammatory tissue reaction to stainless-steel and titanium plates used for internal fixation of long bones.

The immuno-inflammatory responses to stainless-steel (21 implants in 20 patients) and titanium plates (22 implants in 20 patients) used in the treatment of long bone fractures were studied immunohistochemically. All fractures healed without complications. In the soft tissue adjacent to the surface of the implants a dark discolouration of the tissue was visible in 18/21 stainless-steel and 20/22 titanium plates. Tissue specimens of all patients contained positive staining for macrophages (CD68-positive cells). Serial sections showed that the majority of cells were found to express the HLA-DR molecule indicating their activation. Many of the macrophages were surrounded by clusters of T-lymphocytes (CD3-positive cells). 17 out of 21 steel specimens and 15 out of 22 titanium specimens showed the infiltration of moderate amounts of cytotoxic T-lymphocytes (CD8-positive cells). Moderate amounts of B-lymphocytes (CD79alpha positive cells) were evident in four patients with steel and six patients with titanium implants. The results of the present study clearly demonstrate the presence of a marked inflammation and tissue reaction in the soft tissue covering stainless-steel and titanium plates used for internal fixation of fractures of long bones independently from the material used.

Adult↗
PubMed2003

Casting behavior of titanium alloys in a centrifugal casting machine.

Since dental casting requires replication of complex shapes with great accuracy, this study examined how well some commercial titanium alloys and experimental titanium-copper alloys filled a mold cavity. The metals examined were three types of commercial dental titanium [commercially pure titanium (hereinafter noted as CP-Ti), Ti-6Al-4V (T64) and Ti-6Al-7Nb (T67)], and experimental titanium-copper alloys [3%, 5% and 10% Cu (mass %)]. The volume percentage filling the cavity was evaluated in castings prepared in a very thin perforated sheet pattern and cast in a centrifugal casting machine. The flow behavior of the molten metal was also examined using a so-called "tracer element technique." The amounts of CP-Ti and all the Ti-Cu alloys filling the cavity were similar; less T64 and T67 filled the cavity. However, the Ti-Cu alloys failed to reach the end of the cavities due to a lower fluidity compared to the other metals. A mold prepared with specially designed perforated sheets was effective at differentiating the flow behavior of the metals tested. The present technique also revealed that the more viscous Ti-Cu alloys with a wide freezing range failed to sequentially flow to the end of the cavity.

Alloys↗
PubMed2003

The removal torque of titanium screw inserted in rabbit tibia treated by dual acid etching.

Chemical acid etching alone of the titanium implant surface have the potential to greatly enhance osseointegration without adding particulate matter (e.g. TPS or hydroxyapatite) or embedding surface contaminants (e.g. grit particles). The aims of the present study were to evaluate any differences between the machined and dual acid etching implants with the removal torque as well as topographic analysis. A total of 40 custom-made, screw-shaped, commercially pure titanium implants with length of 5 mm and an outer diameter of 3.75 mm were divided into 4 groups, 10 screws in each, and chemical modification of the titanium implant surfaces were achieved using HF and HCl/H(2)SO(4) dual acid etching. The first exposure was to hydrofluoric acid and the second was to a combination of hydrochloric acid and sulfuric acid. The tibia metaphysics was exposed by incisions through the skin, fascia, and periosteum. One implant of each group was inserted in every rabbit, 2 in each proximal tibia metaphysics. Every rabbit received 3 implants with acid etched surfaces and 1 implant with a machined surface. Twelve weeks post-surgically, 7 rabbits were sacrificed, Subsequently, the leg was stabilized and the implant was removed under reverse torque rotation with a digital torque gauge (Mark-10 Corporation, USA) (Fig. 1). Twelve weeks after implant placement, the removal torque mean values were the dual acid etched implants (24%HF+HCl/H(2)SO(4), group C) required a higher average force (34.7 Ncm), than the machined surface implants (group A) (p=0.045) (Mann-Whiteney test). Scanning electron micrographs of acid etching of the titanium surface created an even distribution of very small (1-2 microm) peaks and valleys, while machining of the titanium surface created typical microscopically grooved surface characteristics. Nonetheless, there was no difference in surface topography between each acid etched implant groups. Therefore, chemically acid etching implant surfaces have higher strengths of osseointegration than machined implant surfaces. There is less correlation between removal torque and the difference in HF volume%.

Acids↗
PubMed2003

Apatite deposition on thermally and anodically oxidized titanium surfaces in a simulated body fluid.

By application of a special specimen set-up, thermally oxidized titanium specimen pairs were found able to deposit apatite on the contact surfaces after soaking for 7 days in the simulated body fluid (SBF) of Kokubo's recipe. The specimens oxidized at 400 degrees C and 500 degrees C showed the highest ability of apatite deposition. Both increase and decrease in oxidation temperature from this range caused the apatite deposition ability to decrease. The specimen without treatment failed to deposit any apatite. Specimens anodically oxidized in electrolytes of H(3)PO(4), H(2)SO(4) and acetic acid exhibited very low ability of apatite deposition. Furthermore, the specimen thermally oxidized at 400 degrees C was even able to help the surfaces of PTFE and silicone deposit apatite in the PTFE-Ti and silicone-Ti pairs. This in vitro experimental results indicated that the difference in apatite deposition among various titanium oxides does exist and can be distinguished by applying the present specimen set-up. The mechanism of the apatite deposition on the contact surfaces was discussed in relation to the passive dissolution of titanium in SBF. The release of titanium hydroxide and OH(-) ions from the titanium surfaces and their accumulation inside the confined space between the two contact surfaces were suggested to be responsible for the apatite deposition.

Adsorption↗
PubMed2004

Osteoinduction of porous bioactive titanium metal.

This is the first report of bone induction in a non-osseous site by titanium metal, which has long been recognized as a non-bioactive material. After undergoing specific chemical and thermal treatments, porous bioactive titanium induced bone formation without the need of additional osteogenic cells or osteoinductive agents. Four types of titanium implants were implanted in the dorsal muscles of mature beagle dogs, and were examined histologically after periods of 3 and 12 months. Chemically and thermally treated titanium, as well as pure titanium, was implanted either as porous blocks or as fibre mesh cylinders. Bone formation was found only in the chemically and thermally treated porous block implants removed after 12 months. The present study shows that even a non-soluble metal that contains no calcium or phosphorus can be an osteoinductive material when treated to form an appropriate macrostructure and microstructure. This finding may elucidate the nature of osteoinduction, and lead to the advent of epochal osteoinductive biomaterials for tissue regeneration.

Animals↗
PubMed2004

Anodic plasma-chemical treatment of CP titanium surfaces for biomedical applications.

The anodic plasma-chemical (APC) process was used to modify CP titanium surfaces for biomedical applications. This technique allows for the combined chemical and morphological modification of titanium surfaces in a single process step. The resulting conversion coatings, typically several micrometer thick, consist mainly of titanium oxide and significant amounts of electrolyte constituents. In this study, a new electrolyte was developed containing both calcium-stabilized by complexation with EDTA-and phosphate ions at pH 14. The presence of the Ca-EDTA complex, negatively charged at high pH, favors incorporation of high amounts of calcium into the APC coatings during the anodic (positive) polarization. The coating properties were evaluated as a function of the process variables by XPS, GD-OES, Raman spectroscopy, SEM and tensile testing, and compared to those of calcium-free APC coatings and uncoated CP titanium surfaces. The maximal Ca/P atomic ratio in the coating produced with the new APC electrolyte was approximately 1.3, with higher Ca concentrations than reported in conventional APC coatings. The dissolution behavior of the incorporated, amorphous CaP phases was investigated by exposure to a diluted EDTA solution. The coatings produced in the new electrolyte system exhibit favorable mechanical stability. The new APC technology is believed to be a versatile and cost-effective coating technique to render titanium implant surfaces bioactive.

Adsorption↗
PubMed1998

Titanium alloys in total joint replacement--a materials science perspective.

Increased use of titanium alloys as biomaterials is occurring due to their lower modulus, superior biocompatibility and enhanced corrosion resistance when compared to more conventional stainless steels and cobalt-based alloys. These attractive properties were a driving force for the early introduction of alpha (cpTi) and alpha + beta (Ti-6A1-4V) alloys as well as for the more recent development of new Ti-alloy compositions and orthopaedic metastable beta titanium alloys. The later possess enhanced biocompatibility, reduced elastic modulus, and superior strain-controlled and notch fatigue resistance. However, the poor shear strength and wear resistance of titanium alloys have nevertheless limited their biomedical use. Although the wear resistance of beta-Ti alloys has shown some improvement when compared to alpha + beta alloys, the ultimate utility of orthopaedic titanium alloys as wear components will require a more complete fundamental understanding of the wear mechanisms involved. This review examines current information on the physical and mechanical characteristics of titanium alloys used in artifical joint replacement prostheses, with a special focus on those issues associated with the long-term prosthetic requirements, e.g., fatigue and wear.

Alloys↗
PubMedDate not supplied

Effects of fluorides on titanium and other dental alloys in dentistry.

Fluoride ions are the only aggressive ions for the protective oxide layer of titanium and titanium alloys. Thus their presence may possibly start a localized corrosive degradation by pitting and crevice corrosion processes. Since hygiene products like toothpastes and prophylactic gels contain fluoride ions, the present study has been completed to evaluate the effect of fluoride ions on titanium and dental alloys used, for example, as dental implants and superstructures. Two different milieu based on the Fusayama artificial saliva and an electrolyte solution containing NaCl, with and without fluoride ions, have been used for the electrochemical tests, in a pH range of 6.15 to 3.0. Open circuit potentials, potentiodynamic curves, Tafel slopes, galvanic couplings and crevice potentials are the electrochemical procedures selected for this work. Based on the experimental results obtained with these procedures, the mixed potential theory was applied to predict couple potentials and couple currents. It has thus been shown that: (a) with and without fluoride ions, galvanic currents are weak (10E - 7 to 10E - 8 A cm(-2)) within a pH range of 6.15 to 3.5; (b) titanium submitted to anodic polarization in an electrolyte, even one containing fluoride, merely develops an oxide layer and does not corrode within that same pH range of 6.15 to 3.5; (c) in confined areas where fluoride ions are present, titanium and the dental alloys tested undergo as corrosive process, in the form of crevice and pitting, as soon as the pH drops below 3.5.

Dental Alloys↗
PubMedDate not supplied

Blood compatibility of amorphous titanium oxide films synthesized by ion beam enhanced deposition.

Titanium oxide films were synthesized on titanium, cobalt alloy and low-temperature isotropic pryolytic carbon by ion beam enhanced deposition. The non-stoichiometrical titanium oxide films were obtained. Blood compatibility of the films were evaluated by clotting time measurement, platelet adhesion investigation and hemolysis analyses. The results revealed that blood compatibility of the materials was improved by the coating of titanium oxide films. Semiconductor nature of non-stoichiometric titanium oxide films might be responsible for the improvement of blood compatibility.

Animals↗
PubMed1997

Tissue response to titanium plates: a transmitted electron microscopic study.

PURPOSE: This study investigated the tissue response associated with titanium plates. MATERIALS AND METHODS: Titanium miniplates were used to stabilize fractured bones and a bone graft in 14 patients. At the time of plate removal, the osteosynthesis sites were carefully examined macroscopically. After the removal of the plates, biopsies of the 14 soft tissues and two bony sites surrounding the plates were performed for light microscopic and transmitted electron microscopic examination. RESULTS: Macroscopically, visible pigmentation was found in the soft tissue in 14% of the patients, but none in the bone. With light microscopy, pigmentation was found in the soft tissue of 10 of 14 sites and in one of two bony sites. Transmitted electron microscopy showed suspected titanium particles in the connective tissue of all specimens. The small particles were located between the collagen fibers. In some specimens, small particles were noted within the fibroblasts and macrophages. There were degenerative changes around the minute particles in the bone matrix. CONCLUSION: Local macroscopic or microscopic tissue destruction was observed in hard and soft tissue near the titanium miniplates. If the plates remain for a long time, there is a possibility that they may cause further tissue damage. These findings suggest that the titanium miniplates should be removed routinely after bone healing.

Adolescent↗
PubMed1995

Titanium contamination of recycled Cell Saver blood in revision hip arthroplasty.

The use of Cell Saver blood during revision hip arthroplasty has many benefits, both medical and economic. After a review of the current literature, to our knowledge, no case of metallic debris has been reported in the blood after complete treatment with the Haemonetics Cell Saver (Braintree, MA) and appropriate filter system. A case of total hip revision of a loose, cemented acetabular component with a commercially pure titanium metal backing and a titanium alloy plasma-spray textured surface was undertaken. The titanium alloy femoral component was not visibly loose and was not revised. The joint lining tissues were black. Throughout the procedure, the operative site was suctioned with a double-lumen heparinized catheter that delivered blood and other materials to a Haemonetics Cell Saver 3 Plus. The reservoir and filter unit used were the compatible Bentley BCR-3500 (Baxter, Irvine, CA), a system capable of filtering particulates down to 20 microns. Prior to infusion of the salvaged blood, many large black clumps of material were observed mixed in the blood. Some measured 10 x 5 x 5 mm and could easily be seen macroscopically. Light microscopy demonstrated red blood cells with intermixed neutrophils, and black foreign material scattered as separate particles and within the cytoplasm of the scattered histiocytes. Energy dispersive analysis of the black material confirmed the composition as primarily titanium with minute quantities of copper, iron, phosphorous, and sulfur. A scanning electron photomicrograph of one of the specimens demonstrated a large conglomerate, approximately 2,000 microns in diameter, composed primarily of titanium and organic material.(ABSTRACT TRUNCATED AT 250 WORDS)

Aged↗
PubMed1998

Influence of various structure treatments on histological fixation of titanium implants.

In this study, three types of titanium test pieces were manufactured with different surfaces and implanted into dog femoral condyles, and tissue response was assessed histologically and radiographically for 24 weeks thereafter. The study confirmed that thickening of lamellar bone could be observed around titanium plasma spray-coated titanium alloy implants 24 weeks after implantation, whereas thick fibrous tissue surrounded by corticalized bone formed around those made of smooth-sided titanium alloy. With an implant made of an artificial osteochondral composite material, thickening of ingrown trabeculae could be observed as early as 4 weeks, and abundant bone growth into the titanium fiber mesh continued to increased with time. This bone ingrowth resulted in the complete integration of this composite device implant and the host bone. Our findings suggest that cell response to the various implants is quite different, even though the implants were made of the same kind of material. The implants with the open-pore structure has great significance in the ideal fixation between the implants and the viable bone.

Alloys↗
PubMed2001

The electrochemical oxide growth behaviour on titanium in acid and alkaline electrolytes.

Titanium implants have a thin oxide surface layer. The properties of this oxide layer may explain the good biocompatibility of titanium implants. Anodic oxidation results in a thickening of the oxide film, with possible improved biocompatability of anodized implants. The aim of the present study was twofold: (1) firstly, to characterize the growth behaviour of galvanostatically prepared anodic oxide films on commercially pure (c.p.) titanium and (2) secondly, to establish a better understanding of the electroche0mical growth behaviour of anodic oxide on commercially pure titanium (ASTM grade 1) after changes of the electrochemical parameters in acetic acid, phosphoric acid, calcium hydroxide, and sodium hydroxide under galvanostatic anodizing mode. The oxide thickness was measured by Ar sputter etching in Auger Electron spectroscopy (AES) and the colours were estimated by an L*a*b* system (lightness, hue and saturation) using a spectrophotometer. In the first part of our study, it was demonstrated that the interference colours were useful to identify the thickness of titanium oxide. It was also found that the anodic forming voltages with slope (dV/dt) in acid electrolytes were higher than in alkaline electrolytes. Each of the used electrolytes demonstrates an intrinsically specific growth constant (nm/V) in the range of 1.4--2.78 nm/V. In the second part of our study we found, as a general trend, that an increase of electrolyte concentration and electrolyte temperature respectively decreases the anodic forming voltage, the anodic forming rate (nm/s) and the current efficiency (nm.cm(2)/C), while an increase of the current density and the surface area ratio of the anode to cathode increase the anodic forming voltage, the anodic forming rate and the current efficiency. The effects of electrolyte concentration, electrolyte temperature, and agitation speed were explained on the basis of the model of the electrical double layer.

Acetic Acid↗
PubMed2004

Unprecedented oxo-titanium citrate complex precipitated from aqueous citrate solutions, exhibiting a novel bilayered Ti8O10 structural core.

Aqueous titanium citrate solutions were prepared from the reaction of citric acid with titanium 2-propoxide in a range of molar ratios. Solutions containing two or fewer citrates per titanium resulted in the slow crystallization of an insoluble titanium oxo-citrate complex. Single-crystal X-ray analysis identified the species as Ti(8)O(10)(citrate)(4)(H(2)O)(12).14H(2)O.3HOPr(i)(), crystallized in the tetragonal space group I4(1)/a, with a = 30.775(7) A, c = 14.528(7) A, V = 13 759(8) A(3), and Z = 8. The trianionic citrate ligands supply both carboxylate and alkoxide coordination and stabilize the structure using simultaneous chelating and bridging modes of attachment. The compound is a neutral species, exhibiting titanium in three contrasting environments. Laser Raman microscopy and (13)C CPMAS solid-state NMR data were consistent with those of the X-ray crystal structure. When exposed to air, the crystals rapidly lost water and became a powder. The dehydrated powder was noncrystalline to X-rays and insoluble, but (13)C NMR results demonstrated retention of the carboxylate linkages.

Citrates↗
PubMed2002

Mechanism of propylene insertion using bis(phenoxyimine)-based titanium catalysts: an unusual secondary insertion of propylene in a group IV catalyst system.

A highly regioselective secondary enchainment of propylene in a group IV catalyst system is reported. End-group analysis of polypropylene formed using the phenoxyimine-based titanium catalysts revealed a reversal in the regioselectivity of insertion for this class of catalysts. To the best of our knowledge, bis(phenoxyimine)-based titanium complexes are the only known group IV catalysts that insert propylene with exclusive 2,1-regiochemistry. Insertion of propylene into the initiating titanium hydride occurs with high 1,2-regiochemistry. Subsequent insertions into primary titanium alkyls are regiorandom, while insertions into secondary titanium alkyls proceed with high 2,1-regioselectivity. Cyclopolymerization and ethylene/propylene copolymerization strategies are employed to support this proposal.

Alkenes↗
PubMed2002

Insight into the mechanism of the asymmetric addition of alkyl groups to aldehydes catalyzed by titanium-BINOLate species.

The asymmetric addition of alkyl groups to aldehydes catalyzed by BINOLate-titanium complexes has become the testing grounds to evaluate the potential of new BINOL-based ligands. We have investigated the mechanism of this reaction and report our findings here. Model systems for the open form of the catalyst, (BINOLate)[Ti(O-i-Pr)(3)](2), based on mono-oxygen-alkylated BINOL ligands have been examined. Comparison of the reactivity and enantioselectivity of the mono-alkyl BINOL derivatives with those of BINOL indicate that the open form of the catalyst, (BINOLate)[Ti(O-i-Pr)(3)](2), is not active in the asymmetric addition reaction. Several BINOLate-titanium complexes have been synthesized and characterized by X-ray crystallography. These include the dinuclear (BINOLate)Ti(O-i-Pr)(2).Ti(O-i-Pr)(4), which contains a bridging naphtholate and isopropoxy group, trinuclear (BINOLate)Ti(O-i-Pr)(2).[Ti(O-i-Pr)(4)](2), and trimeric [(BINOL)Ti(O-i-Pr)(2)](3). The solid-state and solution structures reported here indicate that (BINOLate)Ti(O-i-Pr)(2) prefers to bind to titanium tetraisopropoxide rather than to itself, explaining why no nonlinear effects are observed in the catalytic reaction. Additionally, experimental evidence suggests that the BINOLate-titanium species responsible for the catalytic and stoichiometric asymmetric addition reactions are different, indicating that the proposed intermediate, (BINOLate)Ti(R)(aldehyde)(O-i-Pr), is not involved in either of these processes. Reactions were examined using different sources of the alkyl group [ZnMe(2) or MeTi(O-i-Pr)(3)]. Under similar conditions, it was found that the product ee's were the same, independent of whether ZnMe(2) or Me-Ti(O-i-Pr)(3) was used as the source of the alkyl groups. This indicates that the role of the dialkylzinc is not to add the alkyl group to the carbonyl but rather to transfer the alkyl group to titanium. On the basis of these results, we hypothesize that the intermediate in the asymmetric addition involves (BINOLate)Ti(O-i-Pr)(2)(aldehyde).MeTi(O-i-Pr)(3).

Alcohols↗
PubMed2002

Highly selective addition of chiral, sulfonimidoyl substituted bis(allyl)titanium complexes to N-sulfonyl alpha-imino esters: asymmetric synthesis of gamma,delta-unsaturated alpha-amino acids bearing a chiral, electron-withdrawing nucleofuge at the delta-position.

Selective addition of the chiral, sulfonimidoyl substituted bis(allyl)titanium complexes 5a-d, which are configurationally labile in regard to the Calpha-atoms, to N-toluenesulfonyl (Ts)-, N-2-trimethylsilylethanesulfonyl (SES)-, and N-tert-butylsulfonyl (Bus) alpha-imino ester (9a-c) in the presence of Ti(OiPr)(4) and ClTi(OiPr)(3) afforded with high regio- and diastereoselectivities in good yields the (syn, E)-configured beta-alkyl-gamma,delta-unsaturated alpha-amino acid derivatives 2a-g, which carry a chiral, electron-withdrawing nucleofuge at the delta-position and a cyclohexyl, an isopropyl, a phenyl, and a methyl group at the beta-position. Addition of the cyclic bis(allyl)titanium complex 14 to N-Bus alpha-imino ester 9c afforded with similar high regio- and diastereoselectivities the (E)- and (Z)-configured amino acid derivatives (E)-8 and (Z)-8. Reaction of complexes 5a-d with alpha-imino esters 9a-c in the presence of Ti(OiPr)(4) occurs stepwise to give first the mono(allyl)titanium complexes containing 2a-g as ligands, which react in the presence of ClTi(OiPr)(3) with a second molecule of 9a-c with formation of two molecules of 2a-g. Formation of (S,R,E)-configured homoallylic amines 2a-g entails Si,Re,E processes of alpha-imino esters 9a-c with the (R,R)-configured bis(allyl)titanium complexes (R,R)-5a-d and (R)-configured mono(allyl)titanium complexes (R)-17a-d, both of which are most likely in rapid equilibrium with their (S,S)-diastereomers and (S)-diastereomers, respectively. Interestingly, in the reaction of 5a-d with aldehydes, the (S,S)-configured complexes (S,S)-5a-d are the ones which react faster. Reaction of the N-titanated amino acid derivatives Ti-2a and Ti-2b with N-Ts alpha-imino ester 9a led to the highly diastereoselective formation of imidazolidinones 15a and 15b, respectively. Cleavage of the sulfonamide group of the N-Bus amino acid derivative 2d with CF(3)SO(3)H gave quantitatively the sulfonimidoyl functionalized amino acid H-2d. A Ni-catalyzed cross-coupling reaction of the amino acid derivative 2e with ZnPh(2) led to a substitution of the sulfonimidoyl group by a phenyl group and furnished the enantiomerically pure protected alpha-amino acid Bus-1. Two new N-sulfonyl alpha-imino esters, the SES and the Bus alpha-imino esters 9b and 9c, respectively, have been synthesized from the corresponding sulfonamides by the Kresze method in medium to good yields. The N-SES alpha-imino ester 9b and the N-Bus alpha-imino ester 9c should find many synthetic applications, in particular, in cases where the N-Ts alpha-imino ester 9a had been used before.

Amino Acids↗