Force‐deflection behaviour of NiTi archwires in a polytetrafluoroethylene (Teflon) bracket system

In orthodontic treatment, archwire forces for tooth movement is influenced by the magnitude of friction encountered during the sliding motion of archwire along the bracket slot. Friction will reduce the archwire force, and subsequently modify the constant force delivery trend into a slope. The aim of this work is to investigate the force‐deflection behaviour of nickel‐titanium (NiTi) shape memory alloy archwire on polytetrafluoroethylene (Teflon) as the bracket. Sliding tests was performed to determine the coefficient of friction of polytetrafluoroethylene‐NiTi material combinations. The force‐deflection behaviour was evaluated from a modified bending tests, at two different configurations; commercial stainless‐steel bracket and hand‐made polytetrafluoroethylene bracket. During test, wires were deflected into different deflections (2 mm, 3 mm and 4 mm) by using four commercial NiTi archwires at different sizes and geometry. From the test; coefficient of friction for polytetrafluoroethylene‐NiTi wire was recorded as small as 0.07. On force‐deflection graphs, bending load on 3 mm and 4 mm deflection were observed higher on stainless steel (SS) bracket compared with polytetrafluoroethylene bracket. Due to small coefficient of friction on polytetrafluoroethylene‐NiTi configuration, the NiTi archwire exhibited the activation and deactivation force within the plateau limit. Greater friction on stainless steel‐nickel‐titanium bracket configuration causes wire to release force in a slope trend. This finding highlights the potential of polytetrafluoroethylene as a material in the bracket slot to minimize friction during orthodontic treatment.     

High‐Temperature Corrosion of NiTi‐Shape‐Memory Alloys

Semi‐finished products and components made of NiTi‐shape‐memory alloys (NiTi‐SMA) are often subjected to heat treatment after their fabrication. During this heat treatment, oxide layers begin to form which contain a high amount of titanium. In this investigation special attention was drawn to the selective oxidation of Ti because a TiO_X‐layer can represent a Ni‐barrier and may therefore be of special use for medical applications. A comparison of the following three samples was carried out: A sample oxidised at room temperature, another that was heat‐treated in ambient air (600 °C/1min) and a third sample that was subjected to a heat treatment (600 °C/1min) in an atmosphere that oxidises titanium but reduces NiO in order to achieve a selective oxidation of the titanium. The analysis of the oxide layers was carried out by means of x‐ray photoelectron spectroscopy (XPS). It was shown that the ratio of titanium to nickel in the oxide layer can be substantially increased when performing the annealing treatments in a partial reducing atmosphere. Furthermore, a thermo‐gravimetric investigation of the material was carried out at 600 °C in dry air in order to estimate the growth of the oxide layers.     

Powder Metallurgical Near‐Net‐Shape Fabrication of Porous NiTi Shape Memory Alloys for Use as Long‐Term Implants by the Combination of the Metal Injection Molding Process with the Space‐Holder Technique

A new method was developed for producing highly porous NiTi for use as an implant material. The combination of the space‐holder technique with the metal injection molding process allows a net‐shape fabrication of geometrically complex samples and the possibility of mass production for porous NiTi. Further, the porosity can be easily adjusted with respect to pore size, pore shape, and total porosity. The influence of the surface properties of powder metallurgical NiTi on the biocompatibility was first examined using human mesenchymal stem cells (hMSCs). It was found that pre‐alloyed NiTi powders with an average particle size smaller than 45 μm led to the surface properties most suitable for the adhesion and proliferation of hMSCs. For the production of highly porous NiTi, different space‐holder materials were investigated regarding low C‐ and O‐impurity contents and the reproducibility of the process. NaCl was the most promising space‐holder material compared to PMMA and saccharose and was used in subsequent studies. In these studies, the influence of the total porosity on the mechanical properties of NiTi is investigated in detail. As a result, bone‐like mechanical properties were achieved by the choice of Ni‐rich NiTi powder and a space‐holder content of 50 vol% with a particle size fraction of 355–500 μm. Pseudoelasticity of up to 6% was achieved in compression tests at 37 °C as well as a bone‐like loading stiffness of 6.5 GPa, a sufficient plateau stress σ₂₅ of 261 MPa and a value for σ₅₀ of 415 MPa. The first biological tests of the porous NiTi samples produced by this method showed promising results regarding proliferation and ingrowth of mesenchymal stem cells, also in the pores of the implant material.     

Alternating current scanning electrochemical microscopy (AC‐SECM) studies on the surface of electrochemically polished NiTi shape memory alloys

Aiming at imaging local differences in electrochemical activity and related corrosion effects, the surface of electropolished NiTi was investigated using alternating current scanning electrochemical microscopy (AC‐SECM). Segregation‐related spatial variations in the rates of the anodic dissolution that are responsible for the formation of wavy surfaces during electropolishing could not be identified with AC‐SECM. Instead, the surface appeared rather uniform and did not reflect any (patterned) corrosion activity. Obviously, the anodically grown oxide film is highly isolating and passivating. This rationalizes the absence of the evolution of surface irregularities at the solid/liquid interface of NiTi‐shape‐memory alloys.     

NiTi shape memory alloys coated with calcium phosphate by plasma‐spraying. Chemical and biological properties

Plates of superelastic nickel‐titanium shape memory alloy (NiTi) were coated with calcium phosphate (hydroxyapatite) by high‐temperature plasma‐spraying. The porous layer of about 100 μm thickness showed a good adhesion to the metallic substrate that withstood bending of the plate but detached upon cutting the plate. The biocompatibility was tested by cultivation of blood cells (whole blood and isolated granulocytes [a subpopulation of blood leukocytes]). As substrates, pure NiTi, plasma‐spray‐coated NiTi and calcium phosphate‐coated NiTi prepared by a dip‐coating process were used. The adhesion of whole blood cells to all materials was not significantly different. In contrast, isolated granulocytes showed an increased adhesion to both calcium phosphate‐coated NiTi samples. However, compared to non‐coated NiTi or dip‐coated NiTi, the number of dead granulocytes adherent to plasma‐sprayed surfaces was significantly increased for isolated granulocytes (p<0.01).     

Determination of corrosion rate of orthodontic wires based on nickel‐titanium alloy in artificial saliva

The goal of this study was to determine corrosion behavior of three orthodontic wires based on nickel‐titanium alloy (NiTi) in artificial saliva at temperature of 37 °C as function of immersion time. Following orthodontic wires were used: uncoated (NiTi), rhodium coated (Rh NiTi) and nitrified (N NiTi) orthodontic wires. Corrosion of investigated orthodontic wires were monitored by measuring of Ni²⁺ and Ti⁴⁺ ions released in artificial saliva by inductively coupled plasma‐optical emission spectroscopy (ICP‐OES) after 3, 7, 14, 21 and 28 days of immersion. Obtained results indicate that corrosion reaction of the NiTi wires in artificial saliva follows the parabolic rate law. According to the obtained values of parabolic corrosion rate constants, corrosion susceptibility of orthodontic wires decreases in the following order: Rh NiTi wire (K_p = 2.48 μg²/cm⁴ h) > NiTi wire (K_p = 1.6 × 10^–3 μg²/cm⁴ h) > N NiTi wire (K_p = 6.0 × 10^–4 μg²/cm⁴ h). These results indicate that in comparison with uncoated NiTi wire, rhodium coating significantly increases corrosion susceptibility, while nitrification effectively suppresses the release of Ni²⁺ and Ti⁴⁺ ions.     

Fabrication and characteristics of porous NiTi shape memory alloy synthesized by microwave sintering

Porous nickel titanium (NiTi) shape memory alloy (SMA) was successfully fabricated by microwave sintering method. This method allows formation of porous structures without using any pore-forming agents. Moreover, microwave sintering of NiTi SMA can be successfully performed at a relatively low sintering temperature of 850 °C and a short sintering time of 15 min. The pore characteristics, microstructure, phase transformation and stress-strain behavior of the porous NiTi SMA were investigated. The porous NiTi SMA exhibited porosity ratios from 27% to 48% and pore sizes range from 50 to 200 μm when using different sintering temperatures and holding times. The predominant B2 (NiTi) and B19′ (NiTi) phases were identified in the porous NiTi SMA. A multi-step phase transformation took place on heating and a two-step phase transformation took place on cooling of the porous NiTi SMA. The irrecoverable strains decreased with increasing sintering temperature, but the holding time had little effect on the stress-strain behavior at 60 °C.     

High temperature creep measurements in equiatomic Ni‐Ti shape memory alloy

High temperatures creep rates in equiatomic NiTi alloys at three different stress levels and at different temperatures have been measured. It was obtained that the creep rate can be well described by the Dorn equation with n=3. The activation energy of the effective diffusion coefficient, D_c (characterizing the Herring‐Nabarro bulk creep) is Q_c= 226 kJmole^‐1. From comparison of this value with the activation energy of Ni tracer diffusion (155 kJmol^‐1) it was concluded that the Ti is the slower component with high diffusion activation energy close to Q_c.     

Influence of Ti Powder Characteristics on Combustion Synthesis of Porous NiTi Alloy

Porous NiTi shape memory alloy (SMA) is a novel biomedical material used for human hard tissue implant .The influence of elemental titanium powder characteristics such as powder morphology, particle size and specific surface area( SSA) on the minimal ignition temperature ,combustion temperature and final product of porous Ni-Ti SMA fabricated by combustion synthesis method was investigated in this paper by scanning electron microscopy (SEM) and laser diffraction.The preliminary data indicated that the titanium powder characteristics had a strong effect on combustion synthesis of porous NiTi SMA.     

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.     

Extremely high pitting resistance of NiTi shape memory alloy thin film in simulated body fluids

In this paper the corrosion behavior of NiTi thin films fabricated by sputtering from Ni and Ti targets has been studied by cyclic potentiodynamic polarization tests in Hank's and Ringer's solution at 310 K. For comparison, bulk NiTi Shape Memory Alloy (SMA) has also been studied to elucidate the different corrosion behavior of bulk and thin film material. The electrochemical experiments reveal that thin film NiTi SMA has comparable corrosion current density (i_corr), much higher pitting corrosion potentials and wider passive range than the bulk NiTi. We show that NiTi SMA vapour deposited thin films are less susceptible to pitting corrosion than the bulk.     

Damping Factors and Fatigue Notch Factors of Pseudoelastic NiTi‐Shape Memory Alloys

Pseudoelastic NiTi‐ shape memory alloys (SMAs) provide a high damping capacity and can be used in order to achieve a reduction of peak loads being caused by unexpected shock loading. These “pseudoelastic” properties are related to the formation of martensite M from austenite A, which has been induced by stress; they allow to refer to SMAs as functional materials. Furthermore, these functional materials can operate at high stresses and thus, have to withstand severe mechanical loadings like classical structural materials. In combination, these characteristics provide opportunities for technical applications, e.g., to reduce vibrations or to reduce peak loads caused by shock loading. An extensive knowledge of the functional and structural fatigue behaviour of the material is required to design SMA components. NiTi hollow shaft samples and solid shaft samples have been tested under cyclic torsional loading conditions in a load‐controlled mode. By using these two geometries the influence of the sample geometry on the fatigue behaviour can be investigated. In addition, a test programme has been elaborated in order to investigate the behaviour of the material when subjected to bending. The experimental data have been evaluated describing the transformation behaviour induced by stress concerning transformation stress, apparent shear modulus of the austenite G_A and apparent stiffness τ_Ms (describing the slope of the shear stress‐strain‐curve in the transformation range G_A‐M). These parameters naturally depend on the cycle number, the load amplitude as well as the temperature. Engineering failures are often associated with the presence of notches. In this context, torsion tests on notched samples are planned to be carried out in order to assess the resulting data based on the results obtained from the notch free samples. This will allow to derive simple design rules based on fatigue notch factors, which are needed for engineering design.     

The effect of grain orientation on the tensile‐compressive asymmetry of polycrystalline NiTi shape memory alloy

The purpose of the present study is to thoroughly understand the influence of crystallographic texture on the stress‐strain asymmetric behavior of polycrystalline NiTi shape memory alloy under tension and compression. To do this, a 3D thermo‐mechanical model has been implemented in a finite element program and textured and untextured polycrystalline NiTi have been considered. In our polycrystalline finite element model, each element represents one grain and a set of crystal orientations which approximate the initial crystallographic texture of the NiTi are assigned to the elements. From the calculated results, it is found that the crystallographic texture is the important reason for the tension‐compression asymmetry. For the textured polycrystal, the tension‐compression asymmetry can be observed clearly, but for the polycrystal containing randomly oriented grains, the stress‐strain curves show low levers of asymmetry between tensile and compressive loading, and the evolutions of martensite volume fractions are similar under two stress states.     

Bending rotation HCF testing of pseudoelastic Ni‐Ti shape memory alloys

In the present work, a computer‐controlled test rig for simultaneous fatigue testing of several pseudoelastic NiTi wires through bending rotation is described. Bending rotation fatigue (BRF) testing represents a displacement‐controlled experiment where a straight wire is bent into a semi‐circle und forced to rotate around its axis. Thus, each point on the wire surface is subjected to alternating tension and compression. A test rig, which allows to control loading amplitudes, rotation frequencies and temperatures is described. We report preliminary results of an experimental program, which aims for a better understanding of fatigue lives, crack initiation, and crack growth in pseudoelastic NiTi wires. It was found that a good surface quality is of utmost importance to avoid early crack initiation. Wöhler curves of pseudoelastic NiTi wires typically show two different regimes depending on the maximum imposed surface strain during bending rotation fatigue testing. Larger strain amplitudes, which are associated with macroscopic formation of stress‐induced martensite, result in relatively low fatigue lives (LCF regime). In contrast, cycle numbers exceeding 10⁷ were obtained for strain amplitudes where no large scale stress‐induced formation of martensite occurred (HCF regime).     

Effects of anodic oxidation in H2SO4 electrolyte on the biocompatibility of NiTi shape memory alloy

Effects of anodic oxidation in H₂SO₄ electrolyte on the biocompatibility of NiTi shape memory alloy (SMA) were investigated by characterizing surface structure, blood compatibility, wettability, release of harmful Ni ions of anodized NiTi SMA. Although titania film resulting from anodic oxidation in H₂SO₄ electrolyte has a porous structure, it can effectively block out-diffusion of Ni from NiTi SMA to simulated body fluid (SBF). Comparing with chemical polishing, anodic oxidation in H₂SO₄ electrolyte can also improve the wettability, blood compatibility, thromboresistance of NiTi SMA.     

NiTi形状记忆合金薄膜的制备及形变特性

研究了适用于微器件的溅射态NiTi形状记忆合金薄膜.讨论了溅射工艺及织构对薄膜结构和相变特征的影响.利用薄膜热相变特性制成了微驱动器,观察并分析了该器件的形变特性.结果表明:原位加热溅射可以获得具有织构的晶化薄膜;用该薄膜制备的驱动器回复率为0.76%.     

PZT基体沉积条形分布NiTiSMA薄膜复合材料的介电性能

使用模具并采用磁控溅射法在铁电陶瓷PZT基体上沉积具有条形分布结构的Ni Ti SMA薄膜。显微组织结构观察发现,以条形分布结构方式沉积的Ni Ti SMA薄膜晶化处理后具有等轴晶结构。比较所制备PZT/Ni-Ti SMA薄膜复合材料与纯PZT的介电常数及介电损耗发现,两者的介电损耗水平接近;复合材料的介电常数比纯PZT的提高约18%。Ni Ti SMA的沉积使基体中靠近薄膜区域的Zr/Ti物质的量比恰好落在准同型相界区内,致使所制备复合材料的介电性能优于纯PZT。     

Processing and property assessment of NiTi and NiTiCu shape memory actuator springs

Among the multifarious engineering applications of NiTi shape memory alloys (SMAs), their use in actuator applications stands out. In actuator applications, where the one‐way effect (1WE) of NiTi SMAs is exploited, SM components are often applied as helical coil springs. Ingots are generally used as starting materials for the production of springs. But before SM actuator springs can be manufactured, the processing of appropriate wires from NiTi ingots poses a challenge because cold and hot working of NiTi SMAs strongly affect microstructure, and it is well known that the functional properties of NiTi SMAs are strongly dependent on their microstructure. The objective of the present paper is therefore to produce binary Ni₅₀Ti₅₀ and ternary Ni₄₀Ti₅₀Cu₁₀ SMA actuator springs, starting from ingots produced by vacuum induction melting. From these ingots springs are produced using swaging, rolling, wire drawing and a shape‐constraining procedure in combination with appropriate heat treatments. The evolution of microstructure during processing is characterized and the mechanical properties of the wires prior to spring‐making are documented. The mechanical and functional characteristics of the wires are investigated in the stress‐strain‐temperature space. Finally, functional fatigue testing of actuator springs is briefly described and preliminary results for NiTi and NiTiCu actuator springs are reported.     

多孔NiTi形状记忆合金的制备及性能

采用球磨后的NiTi合金粉末为原料,添加尿素作为造孔剂,利用粉末烧结法制备多孔NiTi形状记忆合金.研究烧结温度、保温时间和预成型压力等条件对制备的多孔NiTi合金组织结构和力学性能的影响.结果表明:相对于传统的Ni粉和Ti粉近等原子比混合烧结方法,此方法制备的多孔NiTi合金的相组成更加纯净.且随烧结温度升高,多孔N...     

Superelasticity of free‐standing NiTi films depending on the oxygen impurity of the used targets

Off‐stoichiometric NiTi sputter targets were manufactured by ingot metallurgy in order to produce Ni‐rich NiTi thin films. Crystalline samples, which undergo a martensitic transformation, were fabricated by magnetron sputtering and subsequent thermal treatment. The sacrificial layer technique was applied to obtain free‐standing NiTi films. The stoichiometry of the sputtered film is different to the stoichiometry of the target material. Sputtering targets with a Ti content higher than 49.5 at.% have a typical Ti‐loss rate in the order of 4.3 at.%, whereas at more Ni‐rich targets a Ti loss rate of only 0.5–1.5 at.% is observed. Due to this Ti loss rate target composites of Ti‐53.1Ni‐46.9 at.% and Ti‐53.2Ni‐46.8 at.% were taken. The NiTi films obtained from these two targets were compared. The main difference between the two targets is the impurity content of oxygen and carbon. Auger electron spectroscopy measurements were performed to determine qualitatively the content of oxygen in the free‐standing NiTi films. Transformation temperatures and hysteresis properties of the martensitic transformation were characterised by differential scanning calorimetry. Free‐standing films obtained from the Ti‐53.1Ni‐46.9 at.% and Ti‐53.2Ni‐46.8 at.% sputtering targets revealed superelastic properties at 45 °C as demonstrated by tensile testing. Tensile tests were taken at various temperatures of 40 °C, 45 °C, 50 °C, 55 °C and 60 °C, revealing e.g. a maximum superelastic strain of approximately 5 % at 45 °C.