PMC:2871132 / 104082-122790 JSONTXT

{"target":"https://pubannotation.org/docs/sourcedb/PMC/sourceid/2871132","sourcedb":"PMC","sourceid":"2871132","source_url":"http://www.ncbi.nlm.nih.gov/pmc/2871132","text":"3.4.3. Ca-P Coating\nAs we have just reviewed the evidence showed a formation of an apatite-like film containing Ca and P ions when Ti was pre-treated in NaOH, followed by immersion in SBF (simulated body fluid) or PBL (phosphate buffered liquid). Clinically, it was found that for Ti an increase in oxide thickness and an incorporation of Ca and P were found in placed Ti implants which were in the shape of screws, and had been osseointegrated in patients’ jaws for times ranging from 0.5 to 8 years [30]. These provide “hindsight” knowledge, where later on people will use this knowledge to modify the Ti surfaces.\nFormation of calcium-phosphate on alkali- (10 M NaOH at 60 °C for 24 h) and heat-treated (alkali-treated then at 600 °C for 1 hfollowed by furnace cooling) CpTi was tested. Samples were immersed in the revised SBF with the same HCO3− concentration level as in human blood plasma. It was reported that (i) electron diffraction for the precipitates revealed that octacalcium phosphate, instead of HA, directly nucleates from amorphous calcium-phosphate, (ii) the octacalcium phosphate (OCP) crystals continuously grew on the Ti surfaces rather than transforming to AP, and (iii) calcium titanate (CaTiO3) was identified by electron diffraction [188]. Hanawa et al. [189] characterized surface films formed on titanium specimens which were immersed in electrolyte solutions (pH: 4.5, 5.1, 7.4) at 37 °C for 1 h, 1 day, 30 days and 60 days by XPS, FTIR-RAS Fourier transform infrared reflection absorption spectroscopy to understand the reaction between Ti and inorganic ions. For comparison, the surfaces of Ti-6Al-4V and NiTi were also characterized. XPS data revealed that calcium phosphates (CP) were naturally formed on these specimens. In particular, compared with the CP formed on the Ti alloys, the CP formed on Ti immersed for 30 days in the solution with pH 7.4 was more like HA. It was also reported that (i) the compositions of the CP formed on the specimens changed with the immersion time and the pH value of the solution (the solution with pH 7.4 was Hank’s balanced solution without organic species, solution with pH 4.5 was the artificial saliva without sodium sulphide and urea), and (ii) a CP similar to AP is naturally formed on Ti in a neutral electrolyte solution in 30 days [189].\nCalcium phosphate (Ca-P) coatings have been applied onto titanium alloy prostheses to combine the strength of the metals with the bioactivity of Ca-P. It has been clearly shown in many publications that a Ca-P coating accelerates bone formation around the implant. However, longevity of the Ca-P coating for an optimal bone apposition onto the prosthesis remains controversial. Barrère et al. [190] evaluated biomimetic bone-like carbonate apatite (BCA) and octacalcium phosphate (OCP) coatings which were deposited on Ti-6Al-4V samples to evaluate their in vitro and in vivo dissolution properties. The coated plates were soaked in α-MEM for 1, 2, and 4 weeks, and they were analyzed by Back Scattering Electron Microscopy (BSEM) and by Fourier Transform Infra Red spectroscopy (FTIR). Identical coated plates were implanted subcutaneously in Wistar rats for similar periods. BSEM, FTIR, and histomorphometry were performed on the explants. In vitro and in vivo, a carbonate apatite (CA) formed onto OCP and BCA coatings via a dissolution-precipitation process. It was reported that (i) in vitro, both coatings dissolved overtime, whereas in vivo BCA calcified and OCP partially dissolved after 1 week, and (ii) thereafter, OCP remained stable. This different in vivo behavior can be attributed to (1) different organic compounds that might prevent or enhance Ca-P dissolution, (2) a greater reactivity of OCP due to its large open structure, or (3) different thermodynamic stability between OCP and BCA phases. It was, therefore, concluded that these structural and compositional differences promote either the progressive loss or calcification of the Ca-P coating, and might lead to different osseointegration of coated implants [190]. Barrère et al. [191] studied the nucleation and growth of a calcium phosphate (Ca-P) coating deposited on titanium implants from simulated body fluid (SBF), using atomic force microscopy (AFM) and environmental scanning electron microscopy (ESEM). Forty titanium alloy plates were assigned into two groups: a smooth surface group having a maximum roughness Rmax \u003c 0.10 μm, and a rough surface group with an Rmax \u003c 0.25 μm. Titanium samples were immersed in SBF concentrated by five (SBF × 5) from 10 min to 5 hours and examined by AFM and ESEM. It was observed that scattered Ca-P deposits of approximately 15 nm in diameter appeared after only 10 min of immersion in SBF × 5, and (ii) these Ca-P deposits grew up to 60–100 nm after 4 h on both smooth and rough Ti-6Al-4V substrates. It was found that (i) a continuous Ca-P film formed on titanium substrates, (ii) a direct contact between the Ca-P coating and the Ti-6Al-4V surface was observed, and (iii) the Ca-P coating was composed of nanosized deposits and of an interfacial glassy matrix, which might ensure the adhesion between the Ca-P coating and the Ti-6Al-4V substrate. The Ca-P coating detached from the smooth substrate, whereas the Ca-P film extended onto the whole rough titanium surface over time. In the case of rough Ti-6Al-4V, the Ca-P coating evenly covered the substrate after immersion in SBF × 5 for 5 h. Accordingly, it was suggested that (i) the heterogeneous nucleation of Ca-P on titanium was immediate and did not depend on the Ti-6Al-4V surface topography, and (ii) the further growth and mechanical attachment of the final Ca-P coating strongly depended on the surface, for which a rough topography was beneficial [191].\nThe bioconductivity of a new biomedical Ti-29Nb-13Ta-6Zr alloy was achieved by a combination of surface oxidation and alkaline treatment [192]. It was reported that (i) immersion in a protein-free SBF and fast calcification solution led to the growth of CP phase on the oxidized and alkali-treated (10 M NaOH at 40 °C for 24 h) alloy, and the new bioconductive surface was still harder than the substrate, (ii) oxidation at 400 °C × 24 h led to the formation of a hard layer, (iii) the oxides are mainly composed of TiO2, with small amounts of Nb2O5 and ZrO2; an oxygen diffusion layer exists beneath the surface oxide layer, and (iv) a titanate layer forms on the pre-oxidized surface after alkali treatment, and growth of a layer of Ca-P has been successfully induced on the titanate layer by immersing in SBF [192]. Bogdanski et al. [193] coated NiTi with CP by dipping in oversaturated CP solution. Since polymorphonuclear neutrophil grannucytes (PMN) belong to the first cells which will adhere to implant materials, the apoptosis of isolated human PMN after cell culture on non-coated and CP-coated SME NiTi was analyzed by light and scanning electron microscopy and flow cytometry. It was found that (i) in contrast to PMN adherent to non-coated TiNi, the apoptosis of PMN adherent CP-coated samples was inhibited, and (ii) cell culture media obtained from cultured leukocytes with CP-coated were able to transfer the apoptosis inhibiting activities to freshly isolated PMN [193]. The compositions of the surface and the interface of calcium phosphate ceramic (CP) coatings electrophoretically deposited and sintered on CpTi and Ti-6Al-4V were evaluated before and after four weeks immersion in a simulated physiological solution. In the CP coating-metal interface, it was mentioned that (i) the phosphorus diffused beyond the Ti oxide layer, resulting in the depleted phosphorus in the ceramic adjacent to the metal, and (ii) the surface of the ceramic, however, was substantially unchanged [194].\nThe possible mechanisms of minimization of prosthesis-derived bone growth inhibitors by shielding of the metal and reduction of the associated metal dissolution was investigated by Ducheyne et al. [195]. Ti, Al, and V release rates were determined in vitro for Ti-6Al-4V alloy both with and without a CP coating. Surfaces were passivated in 40% HNO3 at 55 °C for 20 min. Calcium phosphate ceramic was electrophoretically deposited and subsequently vacuum sintered at 925 °C for 2 h. Immersion for 1, 2, 4, 8, and 16 weeks in Hank’s balanced salt solution, simulated physiological solution with 1.5 mM DS-EDTA. It was found that (i) the CP-coated specimens contained no measurable amounts of Ti, (ii) the Al ion solution around the CP-coated specimen was significantly greater than the concentration around the non-coated specimens; however (iii) Al did not increase significantly with time, at least up to 4 weeks immersion. The CP coating produced a significant increase of biological fixation, yet at the same time a greater Al release into solution, calling into question the value of calcium phosphate ceramic coating in shielding adverse metal passive dissolution to enhance bone growth [195].\nSimilarly to HA coating, there are various (chemical, electrochemical, and physical) processes for Ca-P coating available. The ions were implanted in sequence, first Ca and then P, both at a dose of 1017 ions/cm2 at beam energy of 25 keV on CpTi (grade 2). The corrosion tests were done in SBF at 37 °C. It was concluded that (i) the CpTi surface subjected to two-step implantation of Ca+P at a dose of 1017 ions/cm2 becomes amorphous, (ii) the implantation of Ca+P ions increases the corrosion resistance in SBF exposure at 37 °C for up to 3,200 h, (iii) during exposures to SBF, CP precipitates form the implanted as well as non-implanted samples, (iv) the CP precipitates have no effect on the corrosion resistance, and (v) under the conditions of the applied examination, the biocompatibility of Ti subjected to the two-step implantation of Ca+P ions was similar to that of untreated sample [196]. CpTi (grade 2) were surface-modified by anodic spark discharge anodization and a thin layer (ca. 5 μm) of amorphous TiO2 containing Ca and P - Ti/AM. Some of the Ti/AM samples were further modified by hydrothermal treatment to produce a thin outermost (ca. 1 μm) of HA (Ti/AM/HA). It was reported that (i) non-anodized vacuum annealed and hydrofluoric acid etched samples, used as control material, showed good bone adsorption producing Ti excellent surface properties, (ii) anodization at a voltage of 275 V that produced a crack free amorphous TiO2 film containing Ca and P (Ti/AM) provided good results for cytocompatibility, important morphological characteristics (micropores without crack development) but presented the lowest bone apposition probably due to the degradation of amorphous TiO2 film, and (iii) hydrothermal treatment at 300 °C for 2 h that produced a sub-micrometer layer of HA crystals (ca. 1 μm) upon the amorphous TiO2 film (Ti/AM/HA) gave rise to the highest bone apposition only at 8 weeks [81].\nCoating by a RF magnetron sputter technique for the production of thin Ca-P coatings can be produced that vary in Ca/P ratio as well as structural appearance. Jansen et al. [197] studied the effect of non-coated titanium and three different Ca-P sputtered surfaces on the proliferation and differentiation (morphology and matrix production) of osteoblast-like cells. It was found that (i) proliferation of the osteoblast-like cells was significantly higher on non-coated than on Ca-P coated samples, (ii) on the other hand, more mineralized extracellular matrix was formed on the coated surfaces, and (iii) TEM confirmed that the cells on the coated substrates were surrounded by extracellular matrix with collagen fibres embedded in crystallized needle shaped structures. On the basis of these findings, it was concluded that (i) the investigated Ca-P sputter coatings possess the capacity to activate the differentiation and expression of osteogenic cells, and (ii) bone formation proceeds faster on Ca-P surfaces than on Ti substrates. Further, it was noticed that this bone stimulating effect appeared to be independent of the Ca-P ratio of the deposited coatings [197].\nHayakawa et al. [198] prepared four types of Ti implants: (1) as-blasted with titania (\u003c150 μm), (2) sintered with Ti beads with 50–150 μm diameter, (3) blasted with IBDM (ion beam dynamic mixing) Ca-P coating, and (4) multilayered sintered implants with IBDM Ca-P coating. The Ca-P coating was rapid heat-treated with infrared radiation at 700 °C. The implants were inserted into the trabecular bone of the left and right femoral condyles of 16 rabbits, for 2, 3, 4, and 12 weeks. It was reported that (i) histological evaluation revealed new bone formation around different implant materials after already 3 weeks of implantation, (ii) after 12 weeks, mature trabecular bone surrounded all implants, and (iii) the combination of surface geometry and Ca-P coating benefits the implant-bone response during the healing phase [198].\nBiomimetic deposition and electrochemical deposition in solution were used for CP deposition on sintered CpTi bead-cylinders (1,300 °C for 2 h under vacuum). The supersaturated solution for CP deposition was prepared by dissolving NaCl, CaCl2, Na2HPO4·2H2O in distilled water buffered to pH 7.4. Biomimetic deposition was done by immersing samples in solution at 37 °C for 1, 2, 4, and 6 days, while electrochemical deposition was performed at −1.8 V (vs. Hg2SO4/Hg reference) for 2 h at 37 °C. It was reported that (i) a pre-coating alkaline treatment (5 mol/L NaOH at 60 °C for 5 h) is necessary to obtain a uniform coating layer on the inner pore surfaces when the biomimetric deposition is used, (ii) electrochemical deposition is more efficient and less sensitive to the conditions of the Ti surfaces compared to the biomimetric depositions; however (iii) the electrochemical deposition produces less uniform and thinner coating layers on the inner pore surfaces compared with the biomimetric deposition, and (iv) the crystal structure of the deposited Ca-P is octacalcium phosphate regardless of the deposition methods [199]. Heimann et al. [200] deposited hydroxyapatite and duplex hydroxyapatite + titania bond coat layers onto Ti-6Al-4V substrates by atmospheric plasma spraying at moderate plasma enthalpies. From as-sprayed coatings and coatings incubated in simulated body fluid, electron-transparent samples were generated by focused ion beam excavation. It was found that (i) adjacent to the metal surface a thin layer of amorphous calcium phosphate (CP) was deposited, (ii) after in vitro incubation of duplex coatings for 24 weeks, Ca-deficient defect apatite needles precipitated from amorphous CP, and (iii) during incubation of hydroxyapatite without a bond coat for 1 week diffusion bands were formed within the amorphous CP of 1–2 μm width parallel to the interface metal/coating, presumably by a dissolution-precipitation sequence [200]. Aluminoborosilicate glass + HA powder were coated on CpTi at 800–900 °C. It was found that (i) the precipitates were Ca-deficient carbonate with low crystallinity, (ii) both morphologies and composition of the precipitates in vivo were similar to those in vitro, and (iii) the HA particles on the surface of the composite act as nucleation sites for precipitation in physiologic environments, whereas the glass matrix is independent of it [201].\nFor the same purpose as done for the HA-coating, a Ca-P coated layer is needed to post-coating heat treatment. Lucas et al. [202] investigated the post-deposition heat treatments of ion beam as-sputtered coatings by varying the time and temperature. Ca-P coatings, deposited using a hydroxyapatite-fluorapatite target, received the post-deposition heat treatments as follows: 150, 300, 400, 500, and 600 °C for either 30 min or 60 min, followed by furnace cooling to room temperature. It was found that (i) the average bond strengths for the coatings heated to 500 °C (30 min), 600 °C (30 min) and 600 °C (1 h) were 40.1 MPa, 13.8 MPa and 9.1 MPa, respectively. The 500 °C heat treatment for 30 minute resulted in an HA-type coating without reducing the tensile bond strength of the coating. Thus, temperature and time are critical parameters in optimizing coating properties [202], suggesting that the diffusion process must be significantly involved.\nGan et al. [203] evaluated the interface shear strength of Ca-P thin films applied to Ti-6Al-4V substrates using a substrate straining method - a shear lag model. The Ca-P films were synthesized using sol-gel methods from either an inorganic or organic precursor solution. Strong interface bonding was demonstrated for both film types. It was reported that (i) the films were identified as non-stoichiometric hydroxyapatite, but with different Ca/P ratios, (ii) the Ca-P films were 1–1.5 μm thick, and (iii) the shear strength was approximately 347 and 280 MPa for inorganic and organic route-formed films, respectively [203]. NiTi was coated with CP by dipping in oversaturated CP solution, with layer thickness (5–20 μm). The porous nature of the layer makes it mechanically stable enough to withstand both the shape memory transition upon cooling and heating and also strong bending of materials (superelasticity). The adhence of human leukocytes and platelets to the AP layer was analyzed in vivo. By comparison, in non-coated SME-NiTi, it was reported that leukocytes and platelets showed a significantly increased adhesion to the coated NiTi [204]. Fend et al. [205] pre-treated CpTi: by immersing in boiling Ca(OH)2 solution for 30–40 min to have only Ca-added pre-calcification, immersing in 20% H3PO4 solution at 85–95 °C for 30 min to have only P-added pre-phosphatization, and immersed these pre-calcified CpTi in supersaturated CP solution at 37 °C for 1 week. It was found that (i) the osteoblast amount and activity on the surfaces containing Ca are higher than those on the surface containing sole P ions, (ii) Ca2+ ion sites on the material surfaces favor protein adsorption, such as fibronectin or vitronectin as ligands of osteoblast, onto the surface due to positive electricity, chemical, and biological function, and (iii) on the AP surfaces, Ca2+ ions are the active sites of the osteoblast adhesion and also promote the cell adhesion on PO43– ion sites [205].\nAs we have seen above, there are many evidence indicating that, in vitro tests, calcium phosphate is precipitated on such surfaces when they are immersed in a simulated physiological solution, suggesting a main reason for excellent biocompatibility (e.g., [181]). On the other hand, there are evidence suggesting that, in vivo, after even seven day implantation of such modified Ti in rat bone, it was found that Ca/P ratio reduced less than 1 (i.e., Ca-depletion) 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