Thin-film X-ray Diffractometry Research Articles

Quantitative evaluation of biaxial compressive strain and its impact on proton conduction and diffusion in yttrium-doped barium zirconate epitaxial thin films

Proton-conducting oxides, including 20 mol% yttrium-doped BaZrO3 (BZY20), have attracted considerable attention as electrolytes for environmentally friendly electrochemical cells, such as proton ceramic fuel cells (PCFCs) and proton-conducting solid oxide cells. These oxides exhibit fast proton conduction due to the complex physicochemical phenomena of hydration, chemical lattice expansion, proton migration, proton trapping, and local distortion. Using a proton-conducting oxide as an electrolyte film in electrochemical devices introduces an interface, which thermally and chemically generates mechanical strain. Here, we briefly review the current state of research into proton-conducting oxides in bulk samples and films used in electrochemical devices. We fabricated 18 and 500 nm thick 20 mol% BZY20 epitaxial films on (001) Nb-doped SrTiO3 single-crystal substrates to form a model interface between proton-conductive and non-proton-conductive materials, using pulsed laser deposition, and quantified the mechanical strain, proton concentration, proton conductivity, and diffusivity using thin-film x-ray diffractometry, thermogravimetry, secondary ion mass spectrometry, and AC impedance spectroscopy. Compressive strains of −2.1% and −0.85% were measured for the 18 and 500 nm thick films, respectively, and these strains reduced both the proton conduction and diffusion by five and one orders of magnitude, respectively, at 375 °C. Analysis based on a simple trapping model revealed that the decrease in proton conduction results from the slower diffusion of mobile protons with a negligible change in the proton trapping contribution. The model shows that the high ohmic resistance reported for a high-performance PCFC with a power density of 740 mW cm−2 at 600 °C can be solely explained by the estimated compressive strain in the cells. This study shows that minimizing biaxial compressive strain by appropriate choices of the electrolyte–electrode combination and fabrication process is important for maximizing the performance of electrochemical cells.

Surface modification of Ti6Al4 V implants by heat, H2O2 and alkali treatments

In the present research we have applied three types of surface modifications on Ti6Al4 V alloy including heat treatment, H2O2 treatment and alkali treatment. Scanning electron microscope and thin-film X-ray diffractometry (TF-XRD) were used to analyse the surface structure and the formed phases on the surface modified specimens. In vitro bioactivity evaluations were carried out and the cytocompatibility assay was performed using the evaluation of viability and attachment of L-929 fibroblast cells. The results revealed more bioactivity of the alkali-treated Ti6Al4 V alloy compared to other surface modifications. Better cellular response was also observed on the alkali-treated specimens. According to the results of our study, alkali treatment enhanced the in vitro bioactivity and cytocompatibility of Ti6Al4 V alloy more effectively than H2O2 treatment and heat treatment.

Comparative evaluation of the effect of different types of surface modifiers on bioactivity of porous titanium implants

By surface modification of titanium foams, the bioactivity and bone bonding ability of the implants can be increased. The aim of the present research is to compare the effect of two different types of surface modifiers on the bioactivity of porous titanium implants. Two different types of surface modifiers (alkali and hydrogen peroxide) were performed on the surface of rigid and porous titanium implants. Scanning electron microscope (SEM) was employed to study the effect of performed modifiers on the outer and inner pores of the titanium foams. Thin film x-ray diffractometry (TF-XRD) was also used to identify the formed phase. Further, soaking of the titanium foams in simulated body fluids (SBF) was performed to compare the bioactivity of surface modified titanium foams. Inductively coupled plasma (ICP) atomic emission spectroscopy was employed to measure the changes of the calcium and phosphorus ions concentration of the SBF during the soaking times. Contact angle measurement was utilized to compare the wettability of surfaces modified rigid titanium implants. The results revealed that the surface treatment using alkali modifier was more effective than hydrogen peroxide (H2O2) modifier from the view of enhancement of bioactivity and increasing the surface wettability.

Enhanced osteoblast response to electrical discharge machining surface

The purpose of this study is to investigate the surface characteristics and biocompatibility of titanium (Ti) surfaces modified by wire electrical discharge machining (EDM). EDM surface characteristics were evaluated by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), thin-film X-ray diffractometry (XRD) and contact angle measurements. MC3T3-E1 cell morphology, attachment and proliferation, as well as analysis of osteoblastic gene expressions, on machined surfaces and EDM surfaces were also evaluated. EDM surfaces exhibited high super hydrophilicity, due to high surface energy. XPS and XRD revealed that a passive oxide layer with certain developing thickness onto. EDM surfaces promoted cell attachment, but restrained proliferation. Counted cell numbers increased significantly on the machined surfaces as compared to the EDM surfaces. Real-time PCR analyses showed significantly higher relative mRNA expression levels of osteoblastic genes (ALP, osteocalcin, Runx2, Osterix) in cells cultured on the EDM surfaces as compared to cells cultured on the machined surfaces.

Surface characteristics and in vitro biocompatibility of a manganese-containing titanium oxide surface

This study investigated the surface characteristics and in vitro biocompatibility of a titanium (Ti) oxide layer incorporating the manganese ions (Mn) obtained by hydrothermal treatment with the expectation of utilizing potent integrin–ligand binding enhancement effect of Mn for future applications as an endosseous implant surface. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, optical profilometry and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The in vitro biocompatibility of the Mn-containing Ti oxide surface was evaluated in comparison with untreated bare Ti using a mouse calvaria-derived osteoblastic cell line (MC3T3-E1). The hydrothermal treatment produced a nanostructured Mn-incorporated Ti oxide layer approximately 0.6μm thick. ICP-AES analysis demonstrated that the Mn ions were released from the hydrothermally treated surface into the solution. Mn incorporation notably decreased cellular attachment, spreading, proliferation, alkaline phosphatase activity, and osteoblast phenotype gene expression compared with the bare Ti surface (p<0.05). The results indicate that the Mn-incorporation into the surface Ti oxide layer has no evident beneficial effects on osteoblastic cell function, but instead, actually impaired cell behavior.

Surface structures and osteoblast response of hydrothermally produced CaTiO 3 thin film on Ti–13Nb–13Zr alloy

This study investigated the surface characteristics and in vitro biocompatibility of a titanium (Ti) oxide layer incorporating calcium ions (Ca) obtained by hydrothermal treatment with or without post heat-treatment in the Ti–13Nb–13Zr alloy. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, atomic force microscopy and contact angle measurements. In vitro biocompatibility of the Ca-containing surfaces was assessed in comparison with untreated surfaces using a pre-osteoblast cell line. Hydrothermal treatment produced a crystalline CaTiO 3 layer. Post heat-treatment at 400 °C for 2 h in air significantly decreased water contact angles in the CaTiO 3 layer ( p < 0.001). The Ca-incorporated alloy surfaces displayed markedly increased cell viability and ALP activity compared with untreated surfaces ( p < 0.001), and also an upregulated expression of various integrin genes (α1, α2, α5, αv, β1 and β3) at an early incubation time-point. Post heat-treatment further increased attachment and ALP activity in cells grown on Ca-incorporated Ti–13Nb–13Zr alloy surfaces. The results indicate that the Ca-incorporated oxide layer produced by hydrothermal treatment and a simple post heat-treatment may be effective in improving bone healing in Ti–13Nb–13Zr alloy implants by enhancing the viability and differentiation of osteoblastic cells.

Increased bone apposition on a titanium oxide surface incorporating phosphate and strontium

This study investigated the osteoconductivity of titanium (Ti) implants with a phosphate (P)- and strontium (Sr) ion-incorporated oxide surface, produced by hydrothermal treatment in the rabbit cortical and cancellous bone, for future biomedical applications as a biocompatible endosseous implant surface. The P- and Sr ion-incorporated Ti implants (P/Sr implant) were produced by hydrothermal treatment using a P- and Sr-containing solution. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy and optical profilometry. Forty screw implants (20 control and 20 experimental) were placed in the tibiae and femoral condyles of 10 New Zealand White rabbits. The surface in vivo osteoconductivity of the P/Sr implants was compared with micro-arc oxidized (TO) implants with surface calcium and P chemistry by histomorphometric analysis in the cortical and cancellous bone after 4 weeks of implantation. The P/Sr implants showed moderately rough surface features and had lower R(a) values than the TO implants. Histologically, more direct bone apposition was observed on the surface of the P/Sr implants. The P/Sr implants displayed significantly higher bone-to-implant contact percentages compared with the TO implant in both the tibiae and the femoral condyles (P<0.01). The results indicate that the hydrothermally produced P- and Sr ion-incorporated Ti oxide surface may be effective in improving implant osseointegration in both cortical and cancellous bone by increasing bone apposition, due to its surface properties combining micro-topography, P/Sr chemistry and superior wettability.

In vitro biocompatibility of magnesium-incorporated submicro-porous titanium oxide surface produced by hydrothermal treatment

This study investigated the surface characteristics and in vitro biocompatibility of titanium (Ti) oxide surface incorporating magnesium ions (Mg), produced by hydrothermal treatment using an alkaline Mg-containing solution, for future biomedical applications. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and optical profilometry. Mouse calvaria-derived osteoblastic cell (MC3T3-E1) attachment, spreading, proliferation, alkaline phosphatase (ALP) activity, and osteoblastic gene expression on Mg-containing surfaces were compared with untreated Ti surfaces. Hydrothermal treatment resulted in Mg-incorporated Ti oxide layer with submicro-porous surface structures approximately 2 μm in thickness. ICP-AES analysis revealed Mg ions release from treated surfaces into the solution. The Mg-incorporated surface displayed significantly increased cellular attachment and ALP activity compared with untreated surface ( p < 0.05), and supported better cell spreading. Real-time polymerase chain reaction analysis showed notably higher mRNA expression of the osteoblast transcription factor genes (Dlx5, Runx2) and the osteoblast phenotype genes (ALP, bone sialoprotein and osteocalcin) in cells grown on the Mg-incorporated surfaces than untreated surfaces. These results demonstrate that the Mg-incorporated submicro-porous Ti oxide surface produced by hydrothermal treatment may improve implant osseointegration by enhancing the attachment, spreading and differentiation of osteoblastic cells.

Characterization on titanium surfaces and its effect on photocatalytic bactericidal activity

Many studies have been published on the use of TiO 2 as a photocatalyst, which decomposes various organic compounds under UV illumination by generating various radicals. The purpose of the present study was to evaluate the photocatalytic bactericidal effects of variously treated titanium surfaces on Escherichia coli K-12. The specimens were fabricated from grade 4 commercially pure titanium, 12 mm in diameter and 1 mm in thickness. Five different surfaces were prepared (MA: machined surface; AO: anodized at 300 V; NO: NaOH-treated; NW: NaOH- and water-treated; and HT: heat-treated). Surface analysis was performed using scanning electron microscopy, optical interferometer, and thin-film X-ray diffractometry. Photocatalytic activity of each group was confirmed by degradation of methylene blue (MB). The antibacterial activity was assessed by calculating the survival ratio in a drop of a culture of E. coli placed on the surface under UV illumination. Significant photocatalytic activity and bactericidal effects were observed on the titanium surfaces of AO and NW, regardless of the surface roughness ( P < 0.01). The group with anatase was the most susceptible to the photocatalytic effect, while the surface without anatase showed the least susceptibility. Based on this in vitro study, the crystallography of the oxide layer on its titanium surfaces is an important factor affecting the photocatalytic bactericidal activity.

Osteoblast response to magnesium ion‐incorporated nanoporous titanium oxide surfaces

This study investigated the surface characteristics and in vitro osteoconductivity of a titanium (Ti) surface incorporated with the magnesium ions (Mg) produced by hydrothermal treatment for future application as an endosseous implant surface. Mg-incorporated Ti oxide surfaces were produced by hydrothermal treatment using Mg-containing solution on two different microstructured surfaces--abraded minimally rough (Ma) or grit-blasted moderately rough (RBM) samples. The surface characteristics were evaluated using scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, optical profilometry, and inductively coupled plasma atomic emission spectroscopy (ICP-AES). MC3T3-E1 pre-osteoblast cell attachment, proliferation, alkaline phosphatase (ALP) activity, and quantitative analysis of osteoblastic gene expression on Ma, RBM, Mg-incorporated Ma (Mg), and Mg-incorporated grit-blasted (RBM/Mg) Ti surfaces were evaluated. Hydrothermal treatment produced an Mg-incorporated Ti oxide layer with nanoporous surface structures. Mg-incorporated surfaces showed surface morphologies and surface roughness values almost identical to those of untreated smooth or micro-rough surfaces at the micron scale. ICP-AES analysis showed Mg ions released from treated surfaces into the solution. Mg incorporation significantly increased cellular attachment (P=0 at 0.5 h, P=0.01 at 1 h) on smooth surfaces, but no differences were found on micro-rough surfaces. Mg incorporation further increased ALP activity in cells grown on both smooth and micro-rough surfaces at 7 and 14 days of culture (P=0). Real-time polymerase chain reaction analysis showed higher mRNA expressions of the osteoblast transcription factor gene (Dlx5), various integrins, and the osteoblast phenotype genes (ALP, bone sialoprotein and osteocalcin) in cells grown on micro-rough (RBM) and Mg-incorporated (Mg and RBM/Mg) surfaces than those on Ma surfaces. Mg incorporation further increased the mRNA expressions of key osteoblast genes and integrins (α1, α2, α5, and β1) in cells grown on both the smooth and the micro-rough surfaces. These results indicate that an Mg-incorporated nanoporous Ti oxide surface produced by hydrothermal treatment may improve implant bone healing by enhancing the attachment and differentiation of osteoblastic cells.

Enhanced osteoblast response to hydrophilic strontium and/or phosphate ions‐incorporated titanium oxide surfaces

This study investigated the surface characteristics and in vitro biocompatibility of titanium (Ti) surfaces incorporated with strontium ions (Sr) and/or phosphate ions (P) produced by hydrothermal treatment for future applications as endosseous implant surfaces. Sr and/or P-incorporated Ti oxide surfaces were produced by hydrothermal treatment. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, contact angle and surface energy measurements, inductively coupled plasma atomic emission spectroscopy, and profilometry. MC3T3-E1 pre-osteoblast cell attachment, morphology of spread cells, viability, and quantitative analysis of osteoblastic gene expression on grit-blasted microrough (RBM), P-incorporated (P), and P- and Sr-incorporated (SrP) Ti surfaces were evaluated. Microstructured P and SrP surfaces showed significantly higher wettability and surface energy compared with RBM surfaces (P<0.01). After immersion in Hank's balanced salt solution, considerable apatite deposition was observed on the P and SrP surfaces. Sr incorporation significantly increased cellular attachment and viability compared with other surfaces (P<0.05). Real-time polymerase chain reaction analysis showed markedly higher mRNA expressions of the osteoblast transcription factor gene (Runx2) and the osteoblast phenotype genes (alkaline phosphatase, osteopontin, bone sialoprotein, and osteocalcin) in cells grown on the P and SrP surfaces compared with those on the RBM surface. These results demonstrate that Sr- and P-incorporated Ti oxide surfaces may improve implant bone healing by enhancing attachment, viability, and differentiation of osteoblastic cells.

Osteoblast response and osseointegration of a Ti–6Al–4V alloy implant incorporating strontium

This study investigated the surface characteristics, in vitro and in vivo biocompatibility of Ti–6Al–4V alloy implants incorporating strontium ions (Sr), produced by hydrothermal treatment using a Sr-containing solution, for future biomedical applications. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, optical profilometry, contact angle and surface energy measurement and inductively coupled plasma-mass spectroscopy (ICP-MS). Human osteoblast-like cell (MG63) attachment, proliferation, alkaline phosphatase (ALP) activity, and quantitative analysis of osteoblastic gene expression on Sr-containing Ti–6Al–4V surfaces were compared with untreated Ti–6Al–4V surfaces. Fifty-six screw implants (28 control and 28 experimental) were placed in the tibiae and femoral condyles of seven New Zealand White rabbits. The osteoconductivity of Sr-containing Ti–6Al–4V implants was evaluated by removal torque testing and histomorphometric analysis after 4 weeks implantation. Hydrothermal treatment produced a crystalline SrTiO 3 layer. ICP-MS analysis showed that Sr ions were released from treated surfaces into the solution. Significant increases in ALP activity ( P = 0.000), mRNA expressions of key osteoblast genes (osterix, bone sialoprotein, and osteocalcin), removal torque values ( P < 0.05) and bone–implant contact percentages ( P < 0.05) in both cortical and cancellous bone were observed for Sr-containing Ti–6Al–4V surfaces. The results indicate that the Sr-containing oxide layer produced by hydrothermal treatment may be effective in improving the osseointegration of Ti–6Al–4V alloy implants by enhancing differentiation of osteoblastic cells, removal torque forces and bone apposition in both cortical and cancellous bone.

In vitro investigation of anodization and CaP deposited titanium surface using MG63 osteoblast-like cells

The aim of the present study was to investigate surface characteristics in four different titanium surfaces (AN: anodized at 270 V; AN-CaP: anodic oxidation and CaP deposited; SLA: sandblasted and acid etched; MA: machined) and to evaluate biological behaviors such as cell adhesion, cell proliferation, cytoskeletal organization, and osteogenic protein expression of MG63 osteoblast-like cells at the early stage. Surface analysis was performed using scanning electron microscopy, thin-film X-ray diffractometry, and a confocal laser scanning microscope. In order to evaluate cellular responses, MG63 osteoblast-like cells were used. The cell viability was evaluated by MTT assay. Immunofluorescent analyses of actin, type I collagen, osteonectin and osteocalcin were performed. The anodized and CaP deposited specimen showed homogeneously distributed CaP particles around micropores and exhibited anatase type oxides, titanium, and HA crystalline structures. This experiment suggests that CaP particles on the anodic oxidation surface affect cellular attachment and spreading. When designing an in vitro biological study for CaP coated titanium, it must be taken into account that preincubation in medium prior to cell seeding and the cell culture medium may affect the CaP coatings. All these observations illustrate the importance of the experimental conditions and the physicochemical parameters of the CaP coating. It is considered that further evaluations such as long-term in vitro cellular assays and in vivo experiments should be necessary to figure out the effect of CaP deposition to biological responses.

Effects of phosphoric acid treatment of titanium surfaces on surface properties, osteoblast response and removal of torque forces

This study investigated the surface characteristics and biocompatibility of phosphate ion (P)-incorporated titanium (Ti) surfaces hydrothermally treated with various concentrations of phosphoric acid (H 3PO 4). The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, optical profilometry, contact angle and surface energy measurement and inductively coupled plasma mass spectroscopy (ICP-MS). MC3T3-E1 cell attachment, spreading, proliferation and osteoblastic gene expression on different surfaces were evaluated. The degree of bony integration was biomechanically evaluated by removal torque testing after 4 weeks of healing in rabbit tibiae. The H 3PO 4 treatment produced micro-rough Ti surfaces with crystalline P-incorporated Ti oxide layers. High concentration H 3PO 4 treatment (1% and 2%) produced significantly higher hydrophilic surfaces compared with low H 3PO 4 treatment (0.5%) and untreated surfaces ( P < 0.01). ICP-MS analysis showed P ions were released from P-incorporated surfaces. Significant increased cell attachment ( P < 0.05) and notably higher mRNA expressions of Runx2, alkaline phosphatase, osteopontin and osteocalcin were observed in cells grown on P-incorporated surfaces compared with cells on untreated machined surfaces. P-incorporated surfaces showed significantly higher removal torque forces compared with untreated machined implants ( P < 0.05). Ti surfaces treated with 2% H 3PO 4 showed increasing tendencies in osteoblastic gene expression and removal torque forces compared with those treated with lower H 3PO 4 concentrations or untreated surfaces. These results demonstrate that H 3PO 4 treatment may improve the biocompatibility of Ti implants by enhancing osteoblast attachment, differentiation and biomechanical anchorage.

Osteoconductivity of hydrophilic microstructured titanium implants with phosphate ion chemistry

This study investigated the surface characteristics and bone response of titanium implants produced by hydrothermal treatment using H 3PO 4, and compared them with those of implants produced by commercial surface treatment methods – machining, acid etching, grit blasting, grit blasting/acid etching or spark anodization. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, X-ray photoelectron spectroscopy, contact angle measurement and stylus profilometry. The osteoconductivity of experimental implants was evaluated by removal torque testing and histomorphometric analysis after 6 weeks of implantation in rabbit tibiae. Hydrothermal treatment with H 3PO 4 and subsequent heat treatment produced a crystalline phosphate ion-incorporated oxide (titanium oxide phosphate hydrate, Ti 2O(PO 4) 2(H 2O) 2; TiP) surface approximately 5 μm in thickness, which had needle-like surface microstructures and superior wettability compared with the control surfaces. Significant increases in removal torque forces and bone-to-implant contact values were observed for TiP implants compared with those of the control implants ( p < 0.001). After thorough cleaning of the implants removed during the removal torque testing, a considerable quantity of attached bone was observed on the surfaces of the TiP implants.

Ultraviolet photodetectors made from SnO 2 nanowires

SnO 2 nanowires can be synthesized on alumina substrates and formed into an ultraviolet (UV) photodetector. The photoelectric current of the SnO 2 nanowires exhibited a rapid photo-response as a UV lamp was switched on and off. The ratio of UV-exposed current to dark current has been investigated. The SnO 2 nanowires were synthesized by a vapor–liquid–solid process at a temperature of 900 °C. It was found that the nanowires were around 70–100 nm in diameter and several hundred microns in length. High-resolution transmission electron microscopy (HRTEM) image indicated that the nanowires grew along the [200] axis as a single crystallinity. Cathodoluminescence (CL), thin-film X-ray diffractometry, and X-ray photoelectron spectroscopy (XPS) were used to characterize the as-synthesized nanowires.

Preparation and characterization of 2,3-dialdehyde bacterial cellulose for potential biodegradable tissue engineering scaffolds

Bacterial cellulose (BC) is suitable for applications as scaffolds in tissue engineering due to its unique properties. However, BC is not enzymatically degradable in vivo and this has become an essential limiting factor in its potential applications. In this work, BC was modified by periodate oxidation to give rise to a biodegradable 2,3-dialdehyde bacterial cellulose (DABC). After characterization by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), attenuated total reflectance–Fourier transform infrared (ATR–FTIR) spectroscopy, thin-film X-ray diffractometry (XRD) and X-ray photoelectron spectroscopy (XPS), we demonstrated that the modified DABC nano-network was able to degrade into porous scaffold with micro-sized pores in water, phosphate buffered saline (PBS) and the simulated body fluid (SBF). The degradation process began from the oxidized amorphous part of the network and concurrently hydroxyapatite formed on the scaffold surface during the process in SBF. Our data also demonstrated that the tensile mechanical properties of the DABC nano-network were suitable for its use in tissue engineering scaffolds.

Effect of Oxide Film Containing Fluorine Ion on Enhancing the Initial Osseointegration of Titanium-Based Alloy

The effects of nano-γ-TiH phase on formation of nanoporous titanium oxide by anodization with HF pretreatment have been investigated by optical microscopy, x-ray photoelectron spectroscopy, thin film x-ray diffractometry, scanning electron microscopy, transmission electron microscopy and secondary ion mass spectroscopy. Furthermore, nanostructural titanium oxide was formed after anodization under various current densities. The γ-TiH is formed by HF pretreatments before anodization. The nano-γ-TiH phase is directly dissolved after anodization. Furthermore, the nanoporous Ti formed by dissolution of nano-titanium hydrides was changed to nanoporous TiO2. The nano-γ-TiH phase plays an important role in forming nanoporous TiO2. The anodization with HF pretreatment not only produces titanium hydride layer, but also results in formation of nanostructural titanium oxide. The bioactive nanoporous titanium oxide film presented in the prese nt study is believed to result in enhancing cell differentiation, thereby providing stable fixation to bone and rapid osseointegration.

Characterization and corrosion studies of fluoride conversion coating on degradable Mg implants

Fluoride conversion coating was synthesized on magnesium (Mg) by immersion treatment in hydrofluoric acid (HF) at room temperature, with the aim of improving the corrosion resistance of Mg in applications as degradable implant material. After an immersion period of 24 h in 48% HF, the samples carried a bronze color, and the conversion coating was dense and free of cracks. Field-emission scanning-electron microscopy (FE-SEM) of the cross-section revealed a coating thickness of about 1.5 μm. Atomic-force microscopy (AFM) recorded an average surface roughness of ∼ 21 nm for the coated sample, similar to that of the untreated one (∼ 17 nm). The coating was mainly composed of magnesium fluoride (MgF 2) as identified by thin-film X-ray diffractometry (TF-XRD), consistent with compositional analysis using X-ray photoelectron spectroscopy (XPS). The MgF 2 was in the form of crystallites of a few nm. A small amount of oxygen was present inside the coating, suggesting that some F − ions are replaced by hydroxyl (OH −) ions in the MgF 2 structure, or that a small amount of Mg(OH) 2 was present. The corrosion resistance of untreated and conversion coated Mg in Hanks' solution was studied using electrochemical impedance spectroscopy (EIS), potentiodynamic polarization tests, and immersion tests. EIS results showed a polarization resistance of 0.18 kΩ cm 2 for the untreated Mg and 5.2 kΩ cm 2 for the coated sample, giving an improvement of about 30 times. Polarization tests also recorded a reduction in corrosion current density from 400 μA/cm 2 to 10 μA/cm 2, showing an improvement of about 40 times. The galvanic effect between untreated and fluoride-coated Mg samples was small. Immersion tests in Hanks' solution also resulted in a much milder and more uniform corrosion damage on the fluoride-coated samples. The results of the present study showed that fluoride coating by conversion treatment is a simple and promising way of enhancing the corrosion resistance of Mg in Hanks' solution, or that it may be employed as a pretreatment step for subsequent coating.

Effects of calcium ion incorporation on bone healing of Ti6Al4V alloy implants in rabbit tibiae

The biocompatibility of calcium ion (Ca)-incorporated Ti6Al4V alloy implants, produced by hydrothermal treatment using a Ca-containing solution, was investigated. The surface characteristics were evaluated by scanning electron microscopy, thin-film X-ray diffractometry, Auger electron spectroscopy, and stylus profilometry. The viability of MC3T3-E1 cells on Ca-incorporated machined Ti6Al4V surfaces with different oxide thicknesses was compared with that on untreated machined Ti6Al4V surfaces with MTT assay. The osteoconductivity of the Ca-incorporated Ti6Al4V implants was evaluated by removal torque testing and histomorphometric analysis after 6 weeks of implantation in rabbit tibiae. Our results show that hydrothermal treatment with a Ca-containing solution produced a crystalline CaTiO 3 layer on Ti6Al4V surfaces, and calcium ions were gradually incorporated throughout the oxide layer. After immersion in Hank's balanced salt solution, a considerable apatite deposition was observed on all surfaces of the Ca-incorporated samples. Significant increases in cell viability ( p<0.001), removal torque forces, and bone-to-implant contact values ( p<0.05) were observed for Ca-incorporated Ti6Al4V implants compared with those for untreated Ti6Al4V implants.