New Ni-free superelastic alloy for orthodontic applications

A potential new Ni-free Ti alloy for biomedical applications was assessed in order to investigate the superelastic behavior, corrosion resistance and the biocompatibility. The alloy studied was Ti19.1Nb8.8Zr. The chemical composition was determined by X-ray microanalysis, the thermoelastic martensitic transformation was characterized by high sensitivity calorimeter. The critical stresses were determined by electromechanical testing machine and the corrosion behavior was analyzed by potentiostatic equipment in artificial saliva immersion at 37 °C. The results were compared with six different NiTi orthodontic archwire brands. The biocompatibility was studied by means of cultures of MG63 cells. Ni-free Ti alloy exhibits thermoelastic martensitic transformation with M_s = 45 °C. The phase present at 37 °C was austenite which under stress can induce martensite. The stress–strain curves show a superelastic effect with physiological critical stress (low and continuous) and a minimal lost of the recovery around 150 mechanical cycles. The corrosion resistance improves the values obtained by different NiTi alloys avoiding the problem of the Ni adverse reactions caused by Ni ion release. Cell culture results showed that adhered cell number in new substrate was comparable to that obtained in a commercially pure Ti grade II or beta-titanium alloy evaluated in the same conditions. Consequently, the new alloy presents an excellent in-vitro response.     

Investigation on microstructure and properties of dissimilar joint between SA553 and SUS304 made by laser welding with filler wire

The dissimilar joints between SA553 and SUS304 were produced by CO₂ laser welding with the ERNiMo-8 and ER308L filler wire. After welding parameters were optimized, qualified weld formations were made. Investigation on the microstructure showed that there were dual phases (martensite and austenite) in the ER308L weld, but only austenite in the ERNiMo-8 weld. For both joints, not only the microstructure gradient, but also the element gradient was observed near interfaces between weld metals and base metals. The Charpy impact and tensile test at room (25 °C) and low temperature (− 196 °C) was implemented. The cryogenic impact energy of the ER308L weldment was 51 J, lower than the value (84 J) of the ERNiMo-8 weldment. The corresponding cryogenic tensile strength of the two weldments was 1070 MPa and 960 MPa, respectively. The cryogenic tensile properties of both weldments were rather higher than requirements in the relevant standards. The ERNiMo-8 weldment showed relatively better comprehensive performance when the cryogenic toughness was considered.     

Osteoblast interaction with laser cladded HA and SiO2-HA coatings on Ti–6Al–4V

In order to improve the bioactivity and biocompatibility of titanium endosseous implants, the morphology and composition of the surfaces were modified. Polished Ti–6Al–4V substrates were coated by a laser cladding process with different precursors: 100 wt.% HA and 25 wt.% SiO₂-HA. X-ray diffraction of the laser processed samples showed the presence of CaTiO₃, Ca₃(PO₄)₂, and Ca₂SiO₄ phases within the coatings. From in vitro studies, it was observed that compared to the unmodified substrate all laser cladded samples presented improved cellular interactions and bioactivity. The samples processed with 25 wt.% SiO₂-HA precursor showed a significantly higher HA precipitation after immersion in simulated body fluid than 100 wt.% HA precursor and titanium substrates. The in vitro biocompatibility of the laser cladded coatings and titanium substrate was investigated by culturing of mouse MC3T3-E1 pre-osteoblast cell line and analyzing the cell viability, cell proliferation, and cell morphology. A significantly higher cell attachment and proliferation rate were observed for both laser cladded 100 wt.% HA and 25 wt.% SiO₂-HA samples. Compared to 100 wt.% HA sample, 25 wt.% SiO₂-HA samples presented a slightly improved cellular interaction due to the addition of SiO₂. The staining of the actin filaments showed that the laser cladded samples induced a normal cytoskeleton and well-developed focal adhesion contacts. Scanning electron microscopic image of the cell cultured samples revealed better cell attachment and spreading for 25 wt.% SiO₂-HA and 100 wt.% HA coatings than titanium substrate. These results suggest that the laser cladding process improves the bioactivity and biocompatibility of titanium. The observed biological improvements are mainly due to the coating induced changes in surface chemistry and surface morphology.     

Influence of the microstructure on electrochemical corrosion and nickel release in NiTi orthodontic archwires

The aim of this work was to determine the influence of the present phases and the chemical composition on the corrosion behavior and the nickel ion release of the NiTi orthodontic archwires. Eight Ni–Ti archwires from six commercial brands, in the as-received condition, were studied. The chemical composition, roughness, microstructure and the proportion of the phases as well as the corrosion behavior were analyzed for each archwire. The nickel ion release was characterized in artificial saliva immersion settings ranging up to 4 weeks. The results show that the presence of the martensitic phase improves corrosion resistance and significantly decreases Ni release into exterior medium in comparison with the austenitic specimens. In spite of the partial loss of superelasticity produced in the martensitic phase, it could be of great interest for biomedical applications, as it could minimize sensitization and allergies and improve biocompatibility and corrosion resistance of NiTi shape memory alloys.     

The location of atomic hydrogen in NiTi alloy: A first principles study

A first principles density functional theory study to investigate the H defect in NiTi alloy is presented. We have determined the interstitial H atom position in bulk B2 phase NiTi alloy. H positions on both the Ti and Ni terminated NiTi surfaces are calculated. Surface adsorptions of H atom on Ni/Ti terminated surfaces are calculated for a low surface coverage of 1.96 × 10¹⁴ cm^?2. We have also calculated the penetration barrier energy for an H atom from the surface site to the bulk lattice site.     

High strain and long duration cycling behavior of laser welded NiTi sheets

The use of NiTi in complex shaped components for structural applications is limited by the material cost and machinability and adequate joining techniques have been investigated to minimize the thermal cycle effect on the superelastic and shape memory effects exhibited by NiTi. Laser welding is the most used joining process for this material. However, existing studies mainly address the functional properties of laser welded NiTi wires, and the superelastic cycling tests are limited to either a low number of cycles (maximum 100) or to low strains (below 6%). This paper discusses the results of the cycling behavior exhibited by laser butt welded 1 mm thick NiTi plates, when tested to high strains (up to 10%) and for a large number of cycles (600). The superelastic effect was observed and the microstructural changes induced by the laser welding procedure, namely the extension of the thermal affected regions, were seen to influence the evolution of the accumulated irrecoverable strain. Thus, it is possible, by controlling the heat input introduced during welding, to tune the maximum superelastic recovery presented by NiTi laser welds.     

Microstructure evolution in a single crystal nickel-based superalloy joint by linear friction welding

Linear friction welding (LFW) was used with a single crystal nickel-based superalloy to produce sound welds. Microstructural examination shows that the joint has a distinct weld zone (WZ) and thermomechanically affected zone (TMAZ). In the WZ, the microstructure has recrystallized polycrystals instead of a single crystal. In the TMAZ, the amount of γ′ phase increased from the TMAZ/WZ interface to the parent material (PM) and decreased from the periphery to the centre along the weld creating a U-shaped microhardness profile in the TMAZ. The microhardness is however lower than that in the WZ. The average tensile strength was found to be 837.5 ± 50 MPa, comparable to the PM (880 MPa [26]).     

Surface characteristics and electrochemical corrosion behavior of NiTi alloy coated with IrO2

The aim of this work is to investigate the surface characteristics and corrosion behavior of NiTi (50.6 at.% Ni) shape memory alloy coated by a ceramic-like and highly biocompatible material, iridium oxide (IrO₂). IrO₂ coatings were prepared by thermal decomposition of H₂IrCl₆ · 6H₂O precursor solution at the temperature of 300 °C, 400 °C and 500 °C, respectively. The surface morphology and microstructure of the coatings were investigated by scanning electron microscope (SEM) and glancing angle X-ray diffraction (GAXRD). X-ray photoelectron spectroscopy (XPS) was employed to determine the surface elemental composition. Corrosion resistance property of the coated samples was studied in a simulated body fluid at 37 ± 1 °C by electrochemical method. It was found that the morphology and microstructure of the coatings were closely related to the oxidizing temperatures. A relatively smooth, intact and amorphous coating was obtained when the H₂IrCl₆·6H₂O precursor solution (0.03 mol/L) was thermally decomposed at 300 °C for 0.5 h. Compared with the bare NiTi alloy, IrO₂ coated samples exhibited better corrosion resistance behavior to some extent.     

Silk fibroin immobilization on poly(ethylene terephthalate) films: Comparison of two surface modification methods and their effect on mesenchymal stem cells culture

Silk fibroin (SF) has played a curial role for the surface modification of conventional materials to improve the biocompatibility, and SF modified poly(ethylene terephthalate) (PET) materials have potential applications on tissue engineering such as artificial ligament, artificial vessel, artificial heart valve sewing cuffs dacron and surgical mesh engineering. In this work, SF was immobilized onto PET film via two different methods: 1) plasma pretreatment followed by SF dip coating (PET-SF) and 2) plasma-induce acrylic acid graft polymerization and subsequent covalent immobilization of SF on PET film (PET-PAA-SF). It could be found that plasma treatment provided higher surface roughness which was suitable for further SF dip coating, while grafted poly(acrylic acid) (PAA) promised the covalent bonding between SF and PAA. ATR-FTIR adsorption band at 3284 cm^? 1, 1623 cm^? 1 and 1520 cm^? 1 suggested the successful introduction of SF onto PET surface, while the amount of immobilized SF of PET-SF was higher than PET-PAA-SF according to XPS investigation (0.29 vs 0.23 for N/C ratio). Surface modified PET film was used as substrate for mesenchymal stem cells (MSCs) culture, the cells on PET-SF surface exhibited optimum density compared to PET-PAA-SF according to CCK-8 assays, which indicated that plasma pretreatment followed by SF dip coating was a simple and effective way to prepare biocompatible PET surface.     

The biocompatibility of dense and porous Nickel–Titanium produced by selective laser melting

Nickel–Titanium shape memory alloys (NiTi-SMA) are of biomedical interest due to their unusual range of pure elastic deformability and their elastic modulus, which is closer to that of bone than any other metallic or ceramic material. Newly developed porous NiTi, produced by Selective Laser Melting (SLM), is currently under investigation as a potential carrier material for human mesenchymal stem cells (hMSC). SLM enables the production of highly complex and tailor-made implants for patients on the basis of CT data. Such implants could be used for the reconstruction of the skull, face, or pelvis. hMSC are a promising cell type for regenerative medicine and tissue engineering due to their ability to support the regeneration of critical size bone defects. Loading porous SLM-NiTi implants with autologous hMSC may enhance bone growth and healing for critical bone defects. The purpose of this study was to assess whether porous SLM-NiTi is a suitable carrier for hMSC. Specimens of varying porosity and surface structure were fabricated via SLM. hMSC were cultured for 8 days on NiTi specimens, and cell viability was analyzed using two-color fluorescence staining. Viable cells were detected on all specimens after 8 days of cell culture. Cell morphology and surface topography were analyzed by scanning electron microscopy (SEM). Cell morphology and surface topology were dependent on the orientation of the specimens during SLM production. The Nickel ion release can be reduced significantly by aligned laser processing conditions. The presented results clearly attest that both dense SLM-NiTi and porous SLM-NiTi are suitable carriers for hMSC. Nevertheless, before carrying out in vivo studies, some work on optimization of the manufacturing process and post-processing is required.     

Surface characterization and wear behavior of ion implanted NiTi shape memory alloy

The aim of this study was investigation of changes in the modified near-surface layer on the NiTi shape memory alloy, caused by ion implantation as well as their influence on the mechanical and shape memory properties of this material. Surface of NiTi has been modified by nitrogen ion beam at several fluences 1 × 10¹⁷ cm^?2, 1 × 10¹⁸ cm^?2 and 2 × 10¹⁸ cm^?2 at the energy 50 keV. The effect of implantation parameters on surface characteristics and wear properties was investigated using dry-sliding-wear test, depth sensing indentation test and scanning profilometry method. The experimental results have shown how the ion implantation treatment can change the original surface: reducing Ni content in the surface, increasing the surface hardness (furthermore, the hardness improvement extended to the regions much deeper than the implanted layer), and improving the sliding wear resistance. The experimental results of surface treatment conditions and mechanical properties of the modified NiTi alloys are compared, analyzed and discussed in this paper.     

Characteristics and in vitro biological assessment of (Ti, O, N)/Ti composite coating formed on NiTi shape memory alloy

In this investigation, plasma immersion ion implantation and deposition (PIIID) was used to fabricate a (Ti, O, N)/Ti coating on NiTi shape memory alloy (SMA) to improve its long-term biocompatibility and wear resistance. The surface morphology, composition and roughness of uncoated and coated NiTi SMA samples were examined. Energy dispersive X-ray elemental mapping of cross-sections of (Ti, O, N)/Ti coated NiTi SMA revealed that Ni was depleted from the surface of coated samples. No Ni was detected by X-ray photoelectron spectroscopy on the surface of coated samples. Furthermore, three-point bending tests showed that the composite coating could undergo large deformation without cracking or delamination. After 1 day cell culture, SaOS-2 cells on coated samples spread better than those on uncoated NiTi SMA samples. The proliferation of SaOS-2 cells on coated samples was significantly higher at day 3 and day 7 of cell culture.     

Attachment and proliferation of human osteoblast-like cells (MG-63) on laser-ablated titanium implant material

Demand is increasing for shortening the long (3–6 months) osseointegration period to rehabilitate patients' damaged chewing apparatus in as short a time as possible. For dental implants, as for biomaterials in general, the bio- and osseointegration processes can be controlled at molecular and cellular levels by modification of the implant surface. One of the most promising of such surface modifications is laser ablation, as demonstrated by our previous results [46]. Commercially pure (CP4) sand-blasted, acid-etched titanium disks (Denti® System Ltd., Hungary) were irradiated with a KrF excimer laser (248 nm, fluence 0.4 J/cm², FWHM 18 ns, 2000 pulses), or with a Nd:YAG laser (532 nm, 1.3 J/cm², 10 ns, 200 pulses) then examined by SEM, AFM, and XPS. In vitro attachment (24 h) and proliferation (72 h) of MG-63 osteoblast cells were investigated via dimethylthiazol-diphenyl tetrazolium bromide (MTT), alamarBlue (AB) assays alkaline phosphatase quantification (ALP) and SEM. SEM and AFM revealed significant changes in morphology and roughness. XPS confirmed the presence of TiO₂ on each sample; after Nd:YAG treatment a reduced state of Ti (Ti^3 +) was also observed. MTT, AB and ALP measurements detected an increase in the number of cells between the 24- and 72 hour observations; however, laser treatment did not affect cell attachment and proliferation significantly.     

Experimental investigations on welding behaviour of sintered and forged Fe–0.3%C–3%Mo low alloy steel

Tungsten Inert Gas (TIG) welding is considered as one of the cleanest welding methods. It is generally adopted for thinner materials with moderate weld joint strengths. Welding of sintered porous materials continues to be a challenge due to the inherent porosity of the parent metals. The present research work attempts to address some of the issues relating to the welding behaviour of sintered and forged Fe–0.3%C–3%Mo low alloy steels under TIG welding. Rectangular strips of size 70 mm × 15 mm × 5 mm, obtained by blending, compacting and sintering of elemental powders of iron, graphite and molybdenum, were upset forged – both hot and cold in order to obtain alloy steel strips of various porosities. Two identical alloy steel strips of equal density were then welded both along longitudinal and transverse directions, by TIG welding, employing filler metal of suitable composition. The welded strips were then subjected to tensile test, hardness test, microstructural and Scanning Electron Microscope (SEM) fractography studies. Cold/hot upsetting of the sintered alloy preforms has led to enhanced density. As a result of improved density, their tensile strength and hardness values were also found to be enhanced. The welded alloy exhibited higher tensile strength compared to the un-welded base metal, due to strengthening by residual stress. Similarly, the strength and hardness of the welded alloy strips were found to be enhanced with increase in density. The tensile strength of welded joint is found to be higher compared to that of the base metal due to alloy metals segregation, rapid cooling and formation of acicular ferrite at the weldment of welded joint. No porosity was observed in the weld metal or Heat Affected Zone (HAZ) of the weld joint. However, the base metal had numerous micro pores, though pore migration towards weldment has not been observed.     

Tribological behavior of NiTi alloy against 52100 steel and WC at elevated temperatures

The dry tribological behavior of a Ti–50.3 at.% Ni alloy at temperatures of 25 °C, 50 °C and 200 °C was studied. The wear tests were performed on a high temperature pin-on-disk tribometer using 52100 steel and tungsten carbide pins. The worn surfaces of the NiTi alloy were examined by scanning electron microscope. The results showed that in the wear tests involving steel pins, the wear rate of the NiTi decreased as the wear testing temperature was increased. However, for the NiTi/WC contact, a reverse trend was observed. There was also a large decrease in the coefficient of friction for the NiTi/steel contact with increasing wear testing temperature. The formation of compact tribological layers could be the main reason for the reduction of the wear rate and coefficient of friction of the NiTi/steel contact at higher wear testing temperatures.     

Improvement in the morphology of micro-arc oxidised titanium surfaces: A new process to increase osteoblast response

This study describes a method for combining sandblast-acid etching and micro-arc oxidation to optimise titanium implant surfaces, and examines the effects of these surfaces on osteoblast response. Titanium discs were grouped as: micro-arc oxidised (MAO), sandblast-acid etched and micro-arc oxidised (MAO-SA), micro-arc oxidised and heated (MAO-HT), and untreated smooth surface. The combination of sandblast-acid etching and micro-arc oxidation in the MAO-SA group created an average surface roughness of 2.02 ± 0.15 μm compared to the untreated machined surface of 0.31 ± 0.06 μm. Scanning electron microscopy observations of the surface structures showed that the irregularly ordered valleys created by sandblast-acid etching remained after micro-arc oxidation and that micropores had also formed. These microstructures provided a better place for osteoblasts to spread compared with the other surfaces. In addition, our results indicated that adherent osteoblasts expressed greater alkaline phosphatase (ALP) activity and osteocalcin (OC) production on MAO-SA surfaces compared with MAO, MAO-HT, and smooth surfaces. The overall results clearly indicate that combining sandblast-acid etching and micro-arc oxidation techniques improves the titanium surface morphology and increases the roughness, which provides an optimal surface for cell differentiation and osseointegration.     

Tuning exchange bias in epitaxial Ni/MgO/TiN heterostructures integrated on Si(1 0 0)

Epitaxial Ni thin films are integrated with tunneling barrier MgO on Si(1 0 0) substrate. During pulsed laser deposition, early island-like structure transformed into uniform thin film with increasing number of laser pulses. This led to transitions in exchange bias from positive to negative and back to positive, which is ascribed to morphology associated residual strain. The Ni island structure has a coercive field as high as 3 times of that of the continuous film. The current work holds a tremendous promise in the realization of magnetic devices integrated with the Si-platform.     

Cavitation erosion resistance of heat-treated NiTi

NiTi (Ti–50.8 at.% Ni) specimens were solution-treated at 1000 °C, followed by aging between 200 and 600 °C. The cavitation erosion resistance of all the aged specimens in deionized water was improved relative to the solution-treated specimen, with a maximum increase of about 8.7 times, which was achieved by aging at 500 °C. The results also indicate that both austenite and martensite contribute to the high cavitation erosion resistance of NiTi. It is also shown that a simple macro-indentation test employing a Rockwell indenter may be used for preliminary screening of heat-treated NiTi with respect to cavitation erosion resistance.     

Microstructure of selective laser melted nickel–titanium

In selective laser melting, the layer-wise local melting of metallic powder by means of a scanning focused laser beam leads to anisotropic microstructures, which reflect the pathway of the laser beam. We studied the impact of laser power, scanning speed, and laser path onto the microstructure of NiTi cylinders. Here, we varied the laser power from 56 to 100 W and the scanning speed from about 100 to 300 mm/s. In increasing the laser power, the grain width and length increased from (33 ± 7) to (90 ± 15) μm and from (60 ± 20) to (600 ± 200) μm, respectively. Also, the grain size distribution changed from uni- to bimodal. Ostwald-ripening of the crystallites explains the distinct bimodal size distributions. Decreasing the scanning speed did not alter the microstructure but led to increased phase transformation temperatures of up to 40 K. This was experimentally determined using differential scanning calorimetry and explained as a result of preferential nickel evaporation during the fabrication process. During selective laser melting of the NiTi shape memory alloy, the control of scanning speed allows restricted changes of the transformation temperatures, whereas controlling the laser power and scanning path enables us to tailor the microstructure, i.e. the crystallite shapes and arrangement, the extent of the preferred crystallographic orientation and the grain size distribution.     

Optimization of deep penetration laser welding of thick stainless steel with a 10 kW fiber laser

Deep penetration laser welding of 12 mm thick stainless steel plates was conducted using a 10 kW high-power fiber laser. The effect of the processing parameters on the weld bead geometry was examined, and the microstructure and mechanical properties of the optimal joint were investigated. The results show that the focal position is a key parameter in high-power fiber laser welding of thick plates. There is a critical range of welding speed for achieving good full penetration joint. The type of top shielding gas influences the weld depth. The application of a bottom shielding gas improves the stability of the entire welding process and yields good weld appearances at both the top and bottom surfaces. The maximum tensile stress of the joint is 809 MPa. The joint fails at the base metal far from the weld seam with a typical cup–cone-shaped fracture surface. The excellent welding appearance and mechanical properties indicate that high-power fiber laser welding of a 304 stainless steel thick plate is feasible.