Enhanced in vitro immersion behavior and antibacterial activity of NiTi orthopedic biomaterial by HAp-Nb2O5 composite deposits.

NiTi is a class of metallic biomaterials, benefit from superelastic behavior, high biocompatibility, and favorable mechanical properties close to that of bone. However, the Ni ion leaching, poor bioactivity, and antibacterial activity limit its clinical applications. In this study, HAp-Nb2O5 composite layers were PC electrodeposited from aqueous electrolytes containing different concentrations of the Nb2O5 particles, i.e., 0-1 g/L, to evaluate the influence of the applied surface engineering strategy on in vitro immersion behavior, Ni2+ ion leaching level, and antibacterial activity of the bare NiTi. Surface characteristics of the electrodeposited layers were analyzed using SEM, TEM, XPS, and AFM. The immersion behavior of the samples was comprehensively investigated through SBF and long-term PBS soaking. Gram-negative Escherichia coli (E. coli) and Gram-positive Staphylococcus aureus (S. aureus) infective reference bacteria were employed to address the antibacterial activity of the samples. The results illustrated that the included particles led to more compact and smoother layers. Unlike bare NiTi, composite layers stimulated apatite formation upon immersion in both SBF and PBS media. The concentration of the released Ni2+ ion from the composite layer, containing 0.50 g/L Nb2O5 was ≈ 60% less than that of bare NiTi within 30 days of immersion in the corrosive PBS solution. The Nb2O5-reinforced layers exhibited high anti-adhesive activity against both types of pathogenic bacteria. The hybrid metallic-ceramic system comprising HAp-Nb2O5-coated NiTi offers the prospect of a potential solution for clinical challenges facing the orthopedic application of NiTi.

Improved osteogenic activity of NiTi orthopedic implant by HAp-Nb2O5 composite coatings: Materials and biological points of view.

The surface properties of NiTi, as an interface between the synthetic implant and living tissue, play a vital role in guaranteeing implantation success, especially during the initial stage. This contribution endeavors to enhance the surface features of NiTi orthopedic implants through the application of HAp-based coatings, placing emphasis on assessing the influence of Nb2O5 particles concentration in the electrolyte on resultant properties of HAp-Nb2O5 composite electrodeposits. The coatings were electrodeposited via pulse current mode under galvanostatic current control from an electrolyte containing 0-1 g/L of Nb2O5 particles. Surface morphology, topography, and phase composition were evaluated using FESEM, AFM, and XRD, respectively. EDS was employed to study surface chemistry. In vitro biomineralization and osteogenic activity of the samples were studied by immersing the samples in SBF and incubating them with osteoblastic SAOS-2 cells, respectively. The added Nb2O5 particles, at the optimum concentration, stimulated biomineralization, suppressed the Ni ion leaching, and improved SAOS-2 cell adhesion and proliferation. NiTi implant coated by HAp-0.50 g/L Nb2O5 layer showed tremendous osteogenic properties. Overall, the HAp-Nb2O5 composite layers bring forth fascinating coating in vitro biological performance, reducing Ni leaching, and promoting osteogenic activity, which are fundamental for the successful use of NiTi in vivo.

Progress in Niobium Oxide-Containing Coatings for Biomedical Applications: A Critical Review.

Typically, pure niobium oxide coatings are deposited on metallic substrates, such as commercially pure Ti, Ti6Al4 V alloys, stainless steels, niobium, TiNb alloy, and Mg alloys using techniques such as sputter deposition, sol-gel deposition, anodizing, and wet plasma electrolytic oxidation. The relative advantages and limitations of these coating techniques are considered, with particular emphasis on biomedical applications. The properties of a wide range of pure and modified niobium oxide coatings are illustrated, including their thickness, morphology, microstructure, elemental composition, phase composition, surface roughness and hardness. The corrosion resistance, tribological characteristics and cell viability/proliferation of the coatings are illustrated using data from electrochemical, wear resistance and biological cell culture measurements. Critical R&D needs for the development of improved future niobium oxide coatings, in the laboratory and in practice, are highlighted.

The effect of annealing temperature on microstructure and mechanical properties of dissimilar laser welded superelastic NiTi to austenitic stainless steels orthodontic archwires.

Annealing after welding is a common operational process to improve the mechanical properties of metallic joints through releasing residual stresses in the weld zone. In this study, the effect of post weld annealing on the microstructure and mechanical properties of dissimilar laser-welds for orthodontic archwires of NiTi alloy to austenitic stainless steel has been investigated. In order to do this, the laser-welded wires were annealed at temperatures of 100, 200, and 300 °C for 1 h and then they were quenched in water. Results show that annealing at 100 °C does not affect the microstructure and mechanical properties of joints but post weld heat treatment at 200 °C ends in an increase in the tensile strength to an order of 1.91 times of the strength of as welded (non-heat-treated) joints. Also, precipitation and increase of intermetallic compounds, such as Cr2Ti, and Fe2Ti, at the weld zone during heat treatment at 300 °C, results in a reduction in the mechanical properties of joints. Therefore, post-weld annealing is an effective process on improving mechanical properties of dissimilar joints of these two alloys. However, a suitable heat-treatment temperature is needed in order to achieve desired results.

Structural characterization, mechanical, and electrochemical studies of hydroxyapatite-titanium composite coating fabricated using electrophoretic deposition and reaction bonding process.

In the present work, hydroxyapatite (HA)-titanium (Ti, 20 wt%) composite coating was coated on NiTi alloy substrate by EPD (electrophoretic deposition) process. Before applying the coating, the HA powder was composed with Ti powder using a ball milling process. Influence of the ball milling time on morphology and phase structure of HA-Ti powder was evaluated using TEM and XRD analysis. After composing the HA particles with Ti, the HA-Ti composite powders were coated on the NiTi substrate by the EPD process in an n-butanol medium for 2 min, with the applied voltage of 60 V. XRD and SEM analysis were utilized to evaluate the phase analysis and morphology of the coatings. Mechanical and electrochemical characteristic of the coatings were also assessed using the micro-indentation, micro-scratch, and polarization tests, respectively. The results revealed that the milling process time had a significant influence on reaction bonds and optimum mixing time was 4 hr. Micro-hardness of the HA-Ti composite coating (304 HV) was substantially higher than the HA coating (72 HV). Also, as the HA coating was composed with Ti particles, the amount of force (in the micro-scratch test) required for detaching the coating from the NiTi substrate increased from 7.1 to 17.8 N. The polarization results showed that the HA-Ti composite coating had a higher electrochemical resistance compared with the HA coating. Corrosion resistance of the NiTi alloy coated with HA increased from 133 kΩ.cm2 to 2,720 kΩ.cm2 after composed with the Ti particles.

Effect of Ta2O5 content on the osseointegration and cytotoxicity behaviors in hydroxyapatite-Ta2O5 coatings applied by EPD on superelastic NiTi alloys.

In the present study, the different contents of tantalum pentoxide (Ta2O5: 10, 15, 20 and 30 wt%) nanoparticles were introduced into the natural hydroxyapatite (nHA) coating structure on NiTi substrate through electrophoretic deposition (EPD) method. The phase compositions of coatings were perused before and after the sintering at 800 °C for 1 h by XRD. The incorporation of 30wt%Ta2O5 into nHA matrix induced the formation of undesirable soluble Ca3(PO4)2 phase in composite coating. The FESEM images showed that the density of continuous nHA coating increased by compositing with Ta2O5. The maximum adhesion strength of 28.3 ±â€¯0.7 MPa accomplished from the nHA-20 wt%Ta2O5 composite coating. The Ni ions concentration measurement results from the passivated-NiTi with nHA and nHA-(10, 15 and 20)wt%Ta2O5 coatings during 30 days of immersion in PBS clarified the positive role of Ta2O5 in decreasing the Ni leaching due to the lowering the open porosities of nHA structure. The biological response of the coating surfaces was assessed in vitro by cell culturing and MTS assay. By considering the morphology and density of adsorbed cells on each coating, the improved biocompatibility of nHA coating in the presence of Ta2O5 was justified by scrutinizing the surface roughness, wettability and charge. The highest cell attachment and proliferation on nHA-20 wt%Ta2O5 coating was related to owning the lowest roughness, wetting angle of 34o ±â€¯0.5 and the highest negative surface charge density. Also, the concentration of the highest negative charge density on nHA-20 wt%Ta2O5 coating surface in the SBF solution caused to the enhancement of the amount of the apatite nuclei through providing more sites to calcium absorption.

Development of graphene oxide/calcium phosphate coating by pulse electrodeposition on anodized titanium: Biocorrosion and mechanical behavior.

In this work, graphene oxide (GO) reinforcement was used to improve the strength and fracture toughness of the calcium phosphate (CaP) coating applied on the anodized titanium using pulse electrodeposition. Based on the results, the CaP coating consisted of mixed phases of octa-calcium phosphate (OCP), dicalcium phosphate dehydrate (DCPD) and hydroxyapatite (HAp); however, compositing of this coating with GO caused deposition of the pure HAp phase. Moreover, the nanohardness and Young's modulus of the CaP-GO coating increased over 52% and 41%, respectively, as compared to those measured for the GO-free coating. An improvement of about 16% in the adhesion strength of the CaP coating composited with GO to the anodized titanium was also arisen from improving integrity, crystallinity and decreasing the Young's modulus mismatch of this coating with titanium substrate. Finally, uniformity in the microstructure and more biostability of the CaP-GO coating led to its better protection against the corrosion of anodized titanium.

Biocompatibility assessment of graphene oxide-hydroxyapatite coating applied on TiO2 nanotubes by ultrasound-assisted pulse electrodeposition.

In this study, the ultrasound-assisted pulse electrodeposition was introduced to fabricate the graphene oxide (GO)-hydroxyapatite (HA) coating on TiO2 nanotubes. The results of the X-ray diffraction (XRD), Fourier Transform Infrared spectroscope (FTIR), Transmission Electron Microscope (TEM) and micro-Raman spectroscopy showed the successful synthesis of GO. The Scanning Electron Microscope (SEM) images revealed that in the presence of ultrasonic waves and GO sheets a more compact HA-based coating with refined microstructure could be formed on the pretreated titanium. The results of micro-Raman analysis confirmed the successful incorporation of the reinforcement filler of GO into the coating electrodeposited by the ultrasound-assisted method. The FTIR analysis showed that the GO-HA coating was consisted predominantly of the B-type carbonated HA (CHA) phase. The pretreatment of the substrate and incorporation of the GO sheets into the HA coating had a significant effect on improving the bonding strength at the coating-substrate interface. Moreover, the results of the fibroblast cell culture and 3­(4,5­dimethylthiazolyl­2)­2, 5­diphenyltetrazolium bromide (MTT) assay after 2 days demonstrated a higher percentage of cell activity for the GO-HA coated sample. Finally, the 7-day exposure to simulated body fluid (SBF) showed a faster rate of apatite precipitation on the GO-HA coating, as compared to the HA coating and pretreated titanium.

Effect of employing ultrasonic waves during pulse electrochemical deposition on the characteristics and biocompatibility of calcium phosphate coatings.

In the present work, we investigated the effect of employing ultrasonic waves during pulse electrochemical deposition on surface topography, chemical composition and biocompatibility of calcium phosphate (Ca-P) coatings. The SEM and 3D AFM images showed that the anodized titanium surface was covered with the uniform and refined size of plate-like Ca-P crystals, when the ultrasonic treatment of the electrolyte with power of 60 W was carried out during deposition. In contrast, for the Ca-P; 0 W coating applied under only the magnetic stirring of the electrolyte, the microstructure was non-uniform and some Ca-P crystals with the larger size were randomly observed in different regions, causing a rougher surface. The FTIR results also revealed that employing the ultrasound increases the deposition of a coating involved in only the most stable Ca-P phase of carbonated hydroxyapatite (CHA). However, in the absence of ultrasound, besides the prominent phase of CHA, some less stable Ca-P phases like octa calcium phosphate (OCP) and brushite were also formed in the Ca-P; 0 W coating. The Ca-P; 60 W coating showed the higher ability for apatite biomineralization after a 7-day immersion in the simulated body fluid (SBF). This coating also provided a better surface for the cellular activity, as compared to the Ca-P; 0 W coating.

Characterization of mechanical properties of hydroxyapatite-silicon-multi walled carbon nano tubes composite coatings synthesized by EPD on NiTi alloys for biomedical application.

Release of Ni(1+) ions from NiTi alloy into tissue environment, biological response on the surface of NiTi and the allergic reaction of atopic people towards Ni are challengeable issues for biomedical application. In this study, composite coatings of hydroxyapatite-silicon multi walled carbon nano-tubes with 20wt% Silicon and 1wt% multi walled carbon nano-tubes of HA were deposited on a NiTi substrate using electrophoretic methods. The SEM images of coated samples exhibit a continuous and compact morphology for hydroxyapatite-silicon and hydroxyapatite-silicon-multi walled carbon nano-tubes coatings. Nano-indentation analysis on different locations of coatings represents the highest elastic modulus (45.8GPa) for HA-Si-MWCNTs which is between the elastic modulus of NiTi substrate (66.5GPa) and bone tissue (≈30GPa). This results in decrease of stress gradient on coating-substrate-bone interfaces during performance. The results of nano-scratch analysis show the highest critical distance of delamination (2.5mm) and normal load before failure (837mN) as well as highest critical contact pressure for hydroxyapatite-silicon-multi walled carbon nano-tubes coating. The cell culture results show that human mesenchymal stem cells are able to adhere and proliferate on the pure hydroxyapatite and composite coatings. The presence of both silicon and multi walled carbon nano-tubes (CS3) in the hydroxyapatite coating induce more adherence of viable human mesenchymal stem cells in contrast to the HA coated samples with only silicon (CS2). These results make hydroxyapatite-silicon-multi walled carbon nano-tubes a promising composite coating for future bone implant application.

Electrophoretic deposition of double-layer HA/Al composite coating on NiTi.

In order to improve the bioactivity of NiTi alloys, which are being known as the suitable materials for biomedical applications, numerous NiTi disks were electrophoretically coated by hetero-coagulated hydroxyapatite/aluminum composite coatings in three main voltages from suspensions with different Al concentrations. In this paper, the amount of Ni ions release and bioactivity of prepared samples as well as bonding strength of the coating to substrate were investigated. The surface characterization of the coating by XRD, EDX, SEM, and FTIR showed that HA particles bonded by Al particles. It caused the formation of a free crack coating on NiTi disks. Moreover, the bonding strength of HA/Al coatings to NiTi substrate were improved by two times as compared to that of the pure HA coatings. Immersing of coated samples in SBF for 1 week showed that apatite formation ability was improved on HA/Al composite coating and Ni ions release from the surface of composite coating decreased. These results induce the appropriate bioactivity and biocompatibility of the deposited HA/Al composite coatings on NiTi disks.

Tensile properties and interfacial bonding of multi-layered, high-purity titanium strips fabricated by ARB process.

Severe plastic deformation (SPD) processing has shown very effective in promotion of mechanical properties of metals and alloys. In this study, the results of investigating mechanical properties and also inter-layer bond performance of accumulative roll bonded high purity titanium (HP-Ti) strips are presented. High purity titanium plates were severely deformed by use of a combination of cold rolling (CR) to a thickness reduction of approximately 87% and then accumulative roll bonding (ARB) for three cycles (N=3) at ambient temperature. Optical and scanning electron microscopy, tensile testing, and hardness measurements were conducted. The ARB strips exhibited lower tensile strength and ductility in comparison to cold rolled one which can basically be attributed to the poor function of the latest bonds established in the centerlines of the strips. Fractographic examinations revealed the interfacial de-bonding along the centerline between the layers having undergone roll bonding for just one cycle. It was while the interfaces having experienced roll bonding for more cycles showed much higher resistance against delaminating.