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PubMed2002

Effect of water treatment on the apatite-forming ability of NaOH-treated titanium metal.

NaOH and heat treatments of titanium metal induce an apatite-forming ability on the metal by producing a bioactive graded sodium titanate structure on its surface. An enhancement of the apatite-forming ability of titanium metal induced by the NaOH treatment was attempted by conjoining the water and heat treatments. These treatments are assumed to convert the sodium titanate into anatase, which is presumed to be more effective for apatite nucleation. The sodium titanate gel on the metal formed from the NaOH treatment was shown to transform into anatase by a simple immersion in pure water, with subsequent heat treatments. Forming anatase on the metal significantly improved the apatite-forming ability of the metal in a simulated body fluid (SBF). The apatite-forming ability correlated directly with the amount of anatase on the metal. It is therefore expected that bioactive titanium metal and its alloys with a higher bone-bonding ability can be obtained with the use of the water and subsequent heat treatments after the NaOH treatment.

Apatites↗
PubMed2002

Effect of water vapor treatment on apatite formation on precalcified titanium and bond strength of coatings to substrates.

In previous investigations, a simple method, precalcification, was developed for bioactivating titanium. After a titanium sample was precalcified in a boiling saturated Ca(OH)(2) solution and then immersed in a calcium phosphate supersaturated solution, an apatite coating rapidly precipitated onto its surface. In the present study, heat-treatment in water vapor was carried out prior to precalcification. Heat-treatment in water vapor stimulated the chemical reaction between titanium, calcium, and phosphate. Coating properties were improved, and the bond strength of the coating to substrate was enhanced.

Apatites↗
PubMed1987

The effect of surface macrotexture and hydroxylapatite coating on the mechanical strengths and histologic profiles of titanium implant materials.

A mechanical and histological evaluation of uncoated and hydroxylapatite-coated titanium implant materials was performed. Cylindrical implants of uncoated commercially pure (CP) titanium and hydroxylapatite-coated Ti-6Al-4V alloy were studied using a transcortical model, with implants evaluated after periods of 3, 5, 10, and 32 weeks. All implants had a surface macrotexture consisting of a series of semicircular annular grooves, approximately 750 micron in maximum depth. The attachment characteristics of interface shear stiffness and interface shear strength were determined by mechanical push-out testing. Nondecalcified histologic and microradiographic techniques, with implants in situ, were used to evaluate the response to the implant materials and the presence of the surface macrotexture. Mechanical testing results indicated that the hydroxylapatite-coated implants exhibited significantly greater values of maximum interface shear strength than the uncoated implants after all time periods. Interface shear stiffness was also significantly greater at all time periods for the hydroxylapatite-coated implants as compared to the uncoated implants. Histological evaluation after 3 weeks revealed an osteoid layer covering on all areas coated with the hydroxylapatite material; mineralization of this layer appeared to be complete after 10 weeks. In all cases, longer-term implants demonstrated mineralization of interface bone directly onto the hydroxylapatite coating, and in no case was a fibrous layer observed between the hydroxylapatite coating and the interface bone. Sections from the uncoated CP titanium implants revealed a thin fibrous layer present in nearly all areas. Only isolated regions of direct bone-implant apposition were observed for the uncoated implants. The presence of this fibrous tissue layer, however, apparently did not adversely affect the development of considerable attachment strength. The results from this study indicate that the hydroxylapatite coating can significantly increase the attachment strength of implants which rely upon bone apposition for fixation. In addition, the hydroxylapatite coating provides an osteophilic surface for bone deposition, and allows for a more rapid development of implant-bone attachment.

Animals↗
PubMed1988

The effect of plasma-sprayed calcium phosphate ceramic coatings on the metal ion release from porous titanium and cobalt-chromium alloys.

Bone tissue ingrowth in porous materials is enhanced by the deposition of bioactive calcium phosphate ceramic linings onto the pore walls. These bioactive coatings can be deposited using several methods which yield a variety of coating efficiencies and thereby influence the mechanisms and kinetics of ion release from the metal. We analyzed the effect of plasma-spraying hydroxyapatite onto titanium and cobalt-chromium alloys by measuring the release of Ti, Al, V, Co, and Cr in vitro. Plasma-sprayed coatings significantly reduced the Ti and Al release from titanium-based alloy specimens. The tendencies of release from the cobalt-based specimens are less pronounced. The data substantiate that neither localized enhanced passive dissolution of metal ions nor ceramic shielding of the metal occurs. The Scanning Auger Electron Microprobe Spectroscopic data suggest that the dissipation of thermal and kinetic energy of the ceramic particle at the time of impact can produce compositional and structural changes in the metal surfaces. The resulting effects are significant for the titanium alloy but less significant for the Co-Cr alloy system.

Alloys↗
PubMed1989

Ultrastructural comparisons of ceramic and titanium dental implants in vivo: a scanning electron microscopic study.

Identically prepared, screw-type ceramic and titanium endosteal dental implants were inserted in the jaws of adult mongrel dogs for periods of up to 6 months. Sixteen of the 32 total implants supported fixed bridgework. The interface of bone and soft connective tissues with the dental implants was examined by routine and innovative scanning electron microscopic (SEM) techniques using both secondary and backscattered electron imaging. Results demonstrated excellent bone adaptation to both titanium and ceramic implants. Direct adaptation of bone to the upper third of both type implants was observed with only minimal amounts of any intervening fibrous connective tissue. A composite of trabecular bone and fibrous connective tissue was observed in the lower two-thirds of the implants examined. Areas of bone alteration suggestive of osteoid were observed at the thread apicis of some loaded implants. From this investigation we concluded that similar longitudinal tissue responses were generated to one-piece, cylindrical screw-type titanium and alpha alumina oxide ceramic dental implants. Possible bone remodeling was observed at the thread apicis of the loaded implants, an area where occlusal forces may be distributed. We further suggest that one-stage endosteal implants are capable of maintaining a proportional bone-to-implant interface at the apical support region, similar to that suggested to two-stage implant systems.

Animals↗
PubMed1991

Plasma-sprayed coatings of tetracalciumphosphate, hydroxyl-apatite, and alpha-TCP on titanium alloy: an interface study.

In order to study the interaction of calcium phosphate coatings with bone tissue, coated titanium cylinders with a standard size were implanted in dog femora. Coatings were made by plasma spraying powders of hydroxylapatite, beta-whitlockite, and tetracalciumphosphate particles. The plasma spraying process turns beta-whitlockite into alpha-TCP. Bone bonding and bone formation were evaluated by mechanical push-out tests and histological observations. Hydroxylapatite and tetracalciumphosphate coatings show an interface strength after 3 months of implantation of 34.3 +/- 6.5 MPa and 26.8 +/- 3.9 MPa, respectively, while alpha-TCP and blanco titanium lead to an interface strength of 10.0 +/- 3.5 MPa and 9.7 +/- 1.3 MPa, respectively. Histological examinations revealed that hydroxylapatite and tetracalciumphosphate give rise to an excellent bone formation, while alpha-TCP and blanco titanium evoked remodeling and less bone contact.

Alloys↗
PubMed1991

Torsional properties of implant grade titanium.

The purpose of this research was to evaluate the torsional strength and ductility of CP titanium in the as received condition, heat treated below the alpha----beta transition temperature, and glass bead blasted. Results were compared to as-received samples of implant quality 316L stainless steel. Little or no effect of any of the treatments was noted. The torsional strength of all titanium samples was comparable to 316L stainless and the torsional ductility of the titanium was significantly greater than 316L stainless (p less than .01). These results are significantly different than those obtained when torsion testing bone screws of the same material. A hypothesis is proposed for the differences in these results.

Bone Screws↗
PubMed1994

Electrochemical and XPS studies of titanium for biomaterial applications with respect to the effect of hydrogen peroxide.

Electrochemical measurements, x-ray photoelectron spectroscopy, and scanning tunneling microscopy have been used to study the effect of hydrogen peroxide on the passivity of titanium in a phosphate-buffered saline (PBS) solution. The results indicate that the passive film formed in the PBS solution--with and without addition of H2O2--may be described with a two-layer structure model. The inner layer has a structure close to TiO2 whereas the outer layer consists of hydroxylated compounds. The introduction of H2O2 in the PBS solution broadens the hydroxylate-rich region, probably due to the formation of a Ti(IV)-H2O2 complex. Furthermore, the presence of H2O2 results in enhanced dissolution of titanium and a rougher surface on a microscopic scale. Finally, a dark pigmentation (blue color) is observed when titanium has been exposed--for several weeks--to PBS with additions of H2O2.

Color↗
PubMed1995

Crystal structure of the surface oxide layer on titanium and its changes arising from immersion.

The passivating surface oxide on titanium is one of the elements considered in the explanation of the favorable biologic response of this metal in implant applications. In the present study, transmission electron microscopy was used to identify the crystal structure and morphology of the oxide film on commercially pure titanium specimens before and after immersion in simulated physiologic fluids. The results show that the oxide layer is composed mainly of anatase and rutile, both of which are tetragonal in structure. Although the simulated physiologic fluids did not induce an observable change in the crystal structure for the immersion times investigated, the results indicate an immersion-induced change in microstructure from a fine-grained to a coarser-grained structure. The grain growth observed could be attributed to the growth of the native oxide crystals; however, it most likely results from the formation of a new oxide layer. The results also support oxide thickening as one of the processes associated with passive dissolution of titanium.

Chemical Phenomena↗
PubMed2003

Electrochemical deposition of hydroxyapatite with vinyl acetate on titanium implants.

A novel approach to electrochemical processing of hydroxyapatite (HA) coating was explored. Vinyl acetate was added in the electrolytes of calcium and phosphorous in order to improve the adhesion between HA coating and titanium substrate. X-ray powder diffractometer (XRD) spectra indicated that the vinyl acetate did not interfere with the deposition of HA on the surface of titanium cathodes. X-ray photoelectron spectroscopy (XPS) and scanning electron microscope (SEM) results revealed that both vinyl acetate and HA were deposited on the titanium cathodes. The vinyl acetate changed the HA crystalline morphology in the deposition layer. The shape and growth direction of the HA crystals in the coating with vinyl acetate differed from those of HA deposition along. The addition of vinyl acetate increased the coating strength considerably, even though further improvement is needed for clinical applications. Moreover, a preliminary study of the bioactivity showed that osteoblastic cells exhibited higher cell proliferation potential on the HA/vinyl acetate coating than on that of pure HA.

Adhesiveness↗
PubMed2003

Peptide-modified p(AAm-co-EG/AAc) IPNs grafted to bulk titanium modulate osteoblast behavior in vitro.

Interpenetrating polymer networks (IPNs) of poly(acrylamide-co-ethylene glycol/acrylic acid) (p(AAm-co-EG/AAc) applied to model surfaces prevent protein adsorption and cell adhesion. Subsequently, IPN surfaces functionalized with the RGD cell-binding domain from rat bone sialoprotein (BSP) modulated bone cell adhesion, proliferation, and matrix mineralization. The objective of this study was to utilize the same biomimetic modification strategy to produce functionally similar p(AAm-co-EG/AAc) IPNs on clinically relevant titanium surfaces. Contact angle goniometry and X-ray photoelectron spectroscopy (XPS) data were consistent with the presence of the intended surface modifications. Cellular response was gauged by challenging the surfaces with primary rat calvarial osteoblast (RCO) surfaces in serum-containing media. IPN modified titanium and negative control (RGE-IPN) surfaces inhibit cell adhesion and proliferation, while RGD-modified IPNs on titanium supported osteoblast attachment and spreading. Furthermore, the latter surfaces supported significant mineralization despite exhibiting lower levels of proliferation than positive control surfaces. These results suggest that with the appropriate optimization, this approach may be practical for surface engineering of osseous implants.

Amino Acid Sequence↗
PubMed2003

Behavior of the bone-titanium interface after push-in testing: a morphological study.

Fourteen titanium dental implants (Tioblast) were implanted singly in the proximal tibia of New Zealand rabbits for 120 days. A bone defect was surgically produced and filled with Bio-Oss around six of these implants. After the animals were sacrificed and their organs harvested, bone segments were fixed and methacrylate embedded after the push-in test had been performed. Microradiography was performed on longitudinal sections of the implants, whereas scanning electron microscope analysis was performed on the remaining embedded half-implants using secondary electrons only. The results showed that the implants were apically and coronally surrounded by bone, whether Bio-Oss was used or not. Fractures were evident through the newly formed bone and between the pre-existing and newly formed bone. Some fracture lines propagated through the bone and stopped at the implant surface without continuing along the bone-titanium interface. Detachment between the implant and the bone occurred at the coronal extremity of the implants and along its cervical region. These results highlight the fact that the bone-titanium interface has a high resistance to loading. It exhibited greater resistance than the newly formed bone and seems to behave in a manner similar to the cement lines of osteons.

Animals↗
PubMed2004

Matrix metalloproteinases MMP-2, -9 and tissue inhibitors TIMP-1, -2 expression and secretion by primary human osteoblast cells in response to titanium, zirconia, and alumina ceramics.

Osteogenic properties of bone cells are a key parameter governing osseointegration of implant devices. In this context, osteoblasts have a central role via extracellular matrix synthesis and remodeling that they regulate through different protease activity. In this study, we have analyzed the expression of two matrix metalloproteinases (MMPs): MMP-2 (72 kDa) and MMP-9 (92 kDa) and their specific tissue inhibitors TIMP-1 and TIMP-2 in primary human osteoblastic cells. The effect of titanium, zirconia, and alumina ceramics on the synthesis of these proteases was assessed using reverse transcriptase-polymerase chain reaction, enzyme-linked immunosorbent assay, and zymographic analysis. Our results showed that osteoblasts express MMP-2 and -9 mRNA. Furthermore, MMP-2 mRNA expression was decreased by titanium and increased by alumina whereas zirconia did not have any significant effect. Conversely, MMP-9 mRNA expression was stimulated by titanium but decreased with zirconia, whereas alumina induced no significant changes. Zymographic analysis has evidenced pro-MMP-2 gelatinolytic activity in all cell populations with time-dependent increase profile; pro-MMP-9, however, was not detected. Enzyme-linked immunosorbent assay data confirmed the production of MMP-2 and very low levels of MMP-9. In addition, TIMP-1 was secreted in 24-h-cultured cells and increased to maximal level at 48-72 h whereas TIMP-2 levels were very low. The interactions between human osteoblasts and the studied biomaterials altered both MMP-2, -9 and TIMP-1expression indicating that biomaterials may influence osseointegration and bone remodeling.

Aluminum Oxide↗
PubMed2004

Growth behavior, matrix production, and gene expression of human osteoblasts in defined cylindrical titanium channels.

The purpose of the current study was to investigate the effect of different diameters of cylindrical titanium channels on human osteoblasts. Titanium samples having continuous drill channels with diameters of 300, 400, 500, 600, and 1000 microm were put into osteoblast cell cultures that were isolated from 12 adult human trauma patients. Cell migration into the drill channels was investigated by transmitted-light microscopy. The DNA content in the drill channels was measured photometrically, collagen type I production was analyzed by enzyme-linked immunosorbent assay (ELISA) and osteocalcin gene expression by reverse transcriptase-polymerase chain reaction (RT-PCR). Formation of mineralized tissue was assessed by microradiographs of histological sections. Within 20 days, cells grew an average of 838 microm (+/-128 microm) into the drill channels with a diameter of 600 microm and were significantly faster (p < 0.05) than in all other channels. Cells produced significantly more osteocalcin messenger RNA (mRNA) in 600-microm channels (p < 0.05) than they did in 1000-microm channels and demonstrated the highest osteogenic differentiation. The channel diameter did not influence collagen type I production. The highest cell density was found in 300-microm channels (p < 0.05). The DNA content of the channels linearly decreased with increasing channel diameters. After 40 days of culture, the proportion of mineralized tissue at the mouth section amounted to 6% in 300-microm channels and to 9-11% in 400-600-microm channels. In 1000-microm channels, only traces of mineralization were detected. Our data suggest that the diameter of cylindrical titanium channels has a significant effect on migration, gene expression, and mineralization of human osteoblasts.

Biocompatible Materials↗
PubMed2003

Surface potential change in bioactive titanium metal during the process of apatite formation in simulated body fluid.

Bioactive titanium metal can be prepared by NaOH and heat treatments that present the metal with a graded bioactive surface layer of amorphous sodium titanate. This study used laser electrophoresis together with transmission electron microscopy (TEM) and energy-dispersive X-ray microanalysis (EDX) to relate the surface potential change of the bioactive titanium metal with its surface structural change in simulated body fluid (SBF). The surface potential of the metal was highly negative immediately after immersion in SBF. With increasing soaking time, the surface potential increased, revealing a maximum positive value, and then decreased to a constant negative value. TEM-EDX showed that immediately after immersion in SBF, the metal surface formed Ti-OH groups by exchanging Na(+) ions in the surface sodium titanate with H3O(+) ions in the fluid. Thereafter, with increasing soaking time the metal surface formed an amorphous calcium titanate, then an amorphous calcium phosphate, and, finally, apatite with bone-like composition and structure. These results indicate that the process of apatite formation on bioactive titanium metal is initiated by the formation of Ti-OH groups with negative charges that interact with calcium ions with positive charges to form calcium titanate. The calcium titanate gains a positive charge and later interacts with phosphate ions with negative charges, forming amorphous calcium phosphate. The amorphous calcium phosphate eventually transforms and stabilizes into bone-like crystalline apatite with a negative charge.

Apatites↗
PubMed2004

Thermal residual stresses near the interface between plasma-sprayed hydroxyapatite coating and titanium substrate: finite element analysis and synchrotron radiation measurements.

Plasma-sprayed hydroxyapatite (HA) coatings on titanium alloy are often used in prosthetic implants. The metallic substrate gives the implant good mechanical strength which is combined with good biocompatibility and osteointegration of the ceramic coating. However, the interface between the HA coating and titanium alloy substrate is an area of critical weakness when compared with the interlamellar cohesive strength of the HA coating structure. Knowledge of the stresses in materials near the interface seems to be an important step in understanding why failure occurs. Synchrotron radiation, using Beamline BM16 at the European Synchrotron Radiation Facility (Grenoble, France), has been used to determine local stresses near the interface, down to 10 microm in resolution, between a plasma-sprayed HA coating and a titanium alloy substrate. This experimental determination of residual stresses is compared with the results found by a finite element analysis modeling the thermal effects of the plasma-spraying process. Residual stresses have been found in deposited ceramic near the interface due to a thermal properties mismatch of the materials. If the plane stress state is assumed, meaning the perpendicular component of residual stress is ignored (sigma(z) = 0), then the synchrotron residual stress measurements should be interpreted as mainly compressive in the ceramic coating. This is in contradiction with the coefficient of thermal expansion mismatch; therefore, the simplified plane stresses assumption seems to be inappropriate for the deposited morphology characterized by pores and a network of microcracks. The detailed finite element analysis model, taking into account the real morphology of the coating and the real three-dimensional stress field distribution, allowed the estimation of sigma(z), leading to a more accurate interpretation of synchrotron measurements, which is validated by the experimental results.

Algorithms↗
PubMed2004

Photoexcited formation of bone apatite-like coatings on micro-arc oxidized titanium.

A novel method to rapidly deposit bone apatite-like coatings on titanium implants in simulated body fluid (SBF) is proposed in this article. The processing was composed of two steps; for example, micro-arc oxidation (MAO) of titanium to form titania films, and UV-light illumination of the titania-coated titanium in SBF. The morphology, crystalline structure, and bond strength of the MAO films were investigated as a function of the applied voltage (in the range of 250-400 V) by using scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectrometry, Fourier transform infrared spectroscopy, adhesion-tensile test, and scratch test. Results showed that the MAO films were porous and nanocrystalline with pore sizes varying from 1 to 3 microm and grain sizes varying from 10-20 to 70-80 nm; the predominant phase in titania films changed from anatase to rutile, and the bond strength of the films decreased from 43.4 to 32.9 MPa as the applied voltage increased from 250 to 400 V. After UV-light illumination of the films in SBF for 2 h, bone apatite-like coating was deposited on the MAO film formed at 250 V. The bond strength of the apatite/titania bilayer was about 44.2 MPa. However, no apatite was observed on the MAO film formed at 400 V after UV-light illumination.

Apatites↗
PubMed2005

Adherent apatite coating on titanium substrate using chemical deposition.

Plasma-sprayed "HA" coatings on commercial orthopedic and dental implants consist of mixtures of calcium phosphate phases, predominantly a crystalline calcium phosphate phase, hydroxyapatite (HA) and an amorphous calcium phosphate (ACP) with varying HA/ACP ratios. Alternatives to the plasma-spray method are being explored because of some of its disadvantages. The purpose of this study was to deposit an adherent apatite coating on titanium substrate using a two-step method. First, titanium substrates were immersed in acidic solution of calcium phosphate resulting in the deposition of a monetite (CaHPO4) coating. Second, the monetite crystals were transformed to apatite by hydrolysis in NaOH solution. Composition and morphology of the initial and final coatings were identified using X-ray diffraction (XRD), Scanning Electron Microscopy, and Energy Dispersive Spectroscopy (EDS). The final coating was porous and the apatite crystals were agglomerated and followed the outline of the large monetite crystals. EDS revealed the presence of calcium and phosphorous elements on the titanium substrate after removing the coating using tensile or scratching tests. The average tensile bond of the coating was 5.2 MPa and cohesion failures were observed more frequently than adhesion failures. The coating adhesion measured using scratch test with a 200-microm-radius stylus was 13.1N. Images from the scratch tracks demonstrated that the coating materials were squashed without fracturing inside and/or at the border of the tracks until the failure point of the coating. In conclusion, this study showed the potential of a chemical deposition method for depositing a coating consisting of either monetite or apatite. This method has the advantage of producing a coating with homogenous composition on even implants of complex geometry or porosity. This method involves low temperatures and, therefore, can allow the incorporation of growth factors or biogenic molecules.

Apatites↗