NiTi合金低压等离子渗氮研究

采用低压等离子渗氮工艺对NiTi合金进行了渗氮处理.氮化处理后NiTi合金表面硬度升高.XRD测试结果表明在合金表面形成了一层TiN涂层,在TiN涂层下为Ni3Ti相.电化学腐蚀测试表明经氮化处理后合金的耐腐蚀能力大为提高.     

NiTi合金表面液相阴极等离子体沉积氧化铝陶瓷涂层的研究

在NiTi合金表面通过液相阴极等离子体技术制备了氧化铝(Al2O3)陶瓷涂层。采用X射线衍射和扫描电镜对涂层的相组成以及表面形貌进行了表征和分析,证实在材料表面形成了由α-Al2O3和γ-Al2O3组成的涂层,发现涂层具有粗糙多孔结构。在模拟体液中对NiTi合金的Ni离子释放情况进行了检测,发现液相阴极等离子体改性后显著降低了Ni离子的释放。为NiTi合金植入体的表面改性提供了一条新途径。     

脉冲真空弧源沉积类金刚石薄膜耐磨特性研究

本文利用脉冲真空弧源沉积技术在Cr17Ni14Cu4不锈钢和Si(100)基体上制备了类金刚石(DLC)薄膜,研究在不同基体偏压下,DLC薄膜的结构与性能.采用拉曼光谱和X射线光电子能谱(XPS)研究DLC薄膜的原子结合状态,利用CSEM销盘摩擦磨损试验机研究其耐磨性,利用HXD1000B显微硬度仪测试其显微硬度,并采用压痕法评价其结合力.研究结果表明:DLC薄膜与基体结合牢固.随着基体偏压的提高,DLC薄膜内sp3键含量增大,薄膜硬度提高.Cr17Ni14Cu4不锈钢表面沉积DLC薄膜后,耐磨性大幅度提高,本文探讨了DLC薄膜的耐磨机理.     

超声处理对建筑用EVM表面离子镀DLC涂层组织和摩擦性的影响

通过超声方法处理聚氨基甲酸酯表面,选择脉冲碳离子源,结合阴极放电等离子方法在EVM表面完成DLC涂层的沉积过程,对超声处理过程中温度与时间参数引起的DLC涂层摩擦特性改变进行分析.实验测试研究结果表明:当超声处理的时间延长或者温度升高后,在试样表面形成了更深的条纹,能够显著增强EVM表面发生溶解的能力.DLC涂层在拉曼...     

表面氧化及离子注氮对NiTi形状记忆合金耐腐蚀性能的影响

采用电化学测试的方法，研究了表面氧化以及表面氧化-离子注氮两种表面改性方式对NiTi形状记忆合金在人体生理模拟液(Hank′s溶液)中腐蚀行为的影响。腐蚀电位和极化曲线的测量结果表明表面氧化-离子注氮的方法使NiTi合金材料的腐蚀电位正移。雏钝电流密度下降，钝化电位区间扩大，合金表面耐蚀性明显提高。尤其是NiTi合金在进行氮离子注入后，测得击穿电位显著上升．增强了表面膜的抗局部腐蚀能力。因而表面氧化-离子注氮的改性方法可使材料的耐蚀性达到最佳。通过XPS的分析发现，离子注氮后合金表面形成氮化钛相以及富含羟基的化学效应，使NiTi基体的电化学性能得到提高。     

多元氮化物薄膜及其沉积工艺对NiTi记忆合金性能和组织的影响

采用真空阴极电弧沉积技术,在NiTi记忆合金表面沉积了TiAlBN和TiAlCrFeSiBN多元膜和TiN薄膜,研究了薄膜成份及沉积工艺对NiTi合金性能和组织的影响.结果表明,在NiTi合金表面沉积TiAlBN和TiAlCrFeSiBN多元膜和TiN薄膜均可降低合金在Hank溶液中的Ni溶出速率,其中多元膜的Ni溶出速率最小;提高偏压对沉积了TiAlBN多元膜的NiTi合金的Ni溶出速率无明显影响,但使沉积了TiAlCrFeSiBN膜的NiTi合金的Ni溶出速率降低.在TiAlBN和TiAlCrFeSiBN多元膜表面存在较多细小的钛滴和孔隙,钛滴与薄膜基体之间的融合良好;在TiN薄膜表面存在一些大钛滴和孔隙,钛滴与薄膜基体之间的融合不好.镀膜后,NiTi基体的加热相变点移向低温区,其幅度与薄膜成份及沉积工艺有关,提高偏压使沉积了两种多元膜的NiTi基体的相变点移动幅度增大,但却使沉积了TiN膜的NiTi基体的相变点的移动幅度减小.镀膜过程均使NiTi中的M体尺寸增大.     

工业纯铁等离子体氮化及Ti/TiN多层薄膜沉积复合处理研究

为改善工业纯铁的耐磨抗腐蚀性能,本文采用低偏压高频等离子浸没离子注入及氮化技术(HLPⅢ)对工业纯铁进行表面改性,然后利用非平衡磁控溅射技术(UBMS)在低压高频等离子浸没离子注入及氮化处理样品表面制备Ti/TiN多层膜.研究发现,工业纯铁在3.5kV脉冲电压(频率15.15kHz,占空比25%)下等离子注入及氮化3h后,表面形成了深度达4μm的氮化层,其相结构以ε-Fe_3N和γ-Fe_4N结构为主.等离子氮化及Ti/TiN多层薄膜沉积复合处理后,工业纯铁的硬度、耐磨损性能以及抗腐蚀性能均得到大大提高,等离子注入及氮化形成的氮化层有利于提高Ti/TiN多层薄膜与工业纯铁基体之间的结合力和耐磨性.     

NiTi 合金表面激光原位反应合成TiN增强金属基复合材料涂层

采用连续高功率固体Nd-YA G激光辐照, 使预置于NiTi 合金表面的Ti 粉在N₂ 环境中形成TiN 增强Ti 基复合材料涂层。选择适当的激光辐照工艺参数, 获得致密的TiN 增强金属基复合材料激光改性层。SEM 观察及EDAX 成分分析结果表明, TiN/ Ti 金属基复合材料表面改性层与基体NiTi 合金存在良好的冶金结合, 界面处成分均匀过渡, 表面Ni 含量极低。显微硬度测试及磨损实验表明, TiN/ Ti 金属基复合材料改性层显著提高了NiTi 合金的表面硬度和耐磨性, 激光表面改性层可有效地改善NiTi 合金作为生物医学材料使用的表面成分和性能。      

医用多孔NiTi合金表面微弧氧化改性研究

为解决多孔Ni Ti合金耐蚀性降低和Ni离子释放量增大而引起的使用安全性问题.本文采用微弧氧化技术对医用多孔Ni Ti合金进行表面改性处理,研究结果表明,微弧氧化处理并未改变多孔Ni Ti合金原有的孔隙结构和孔隙率,只在其外表面和孔隙内表面均形成了典型的微弧氧化多孔涂层.该涂层主要由氧化铝相组成,并含有少量的Ti和Ni元素,且外表面涂层的Ti和Ni含量要略低于孔隙内表面涂层.微弧氧化涂层提高了多孔Ni Ti合金的表面接触角,将原有的亲水表面转变成了疏水表面.经微弧处理后,多孔Ni Ti合金的耐蚀性较基体提高了1个数量级以上,Ni离子释放量也较基体降低了1个数量级以上.     

激光表面重熔NiTi合金Hanks''''溶液中腐蚀及Ni离子溶出行为

近等原子比NiTi合金以其独特的形状记忆效应、超弹性和射线不透性等性能而成为制备植入体的理想材料.本文利用光学显微镜、电子显微镜、X射线衍射、电化学极化测试、原子吸收光谱等研究了激光重熔NiTi合金的显微组织、表面特征、在人体模拟液中的耐腐蚀性能和Ni离子溶出行为;结果表明激光表面重熔可以显著改善NiTi合金在Hanks'溶液中的耐腐蚀能力,重熔层显微组织致密,夹杂物极少.重熔层外表面TiO2含量明显提高,试样在Hanks'溶液中浸泡15天后表面有Ca-P层生成.     

Electrochemical Corrosion Behavior of the DLC Coated and Uncoated NiTi Alloys

A dense and well-adhered diamond-like carbon （DLC） coating was prepared on the nickel-titanium （NiTi） alloys by plasma immersion ion implantation and deposition （PIIID）. Potentiodynamic polarization tests indicated the corrosion resistance of the NiTi alloys was markedly improved by the DLC coating. The Ni ions release of the NiTi alloys was effectively blocked by the DLC coating.     

Dissolution effect and cytotoxicity of diamond-like carbon coatings on orthodontic archwires

Nickel–titanium (NiTi) has been used for implants in orthodontics due to the unique properties such as shape memory effect and superelasticity. However, NiTi alloys are eroded in the oral cavity because they are immersed by saliva with enzymolysis. Their reactions lead corrosion and nickel release into the body. The higher concentrations of Ni release may generate harmful reactions. Ni release causes allergenic, toxic and carcinogenic reactions. It is well known that diamond-like carbon (DLC) films have excellent properties, such as extreme hardness, low friction coefficients, high wear resistance. In addition, DLC film has many other superior properties as a protective coating for biomedical applications such as biocompatibility and chemical inertness. Therefore, DLC film has received enormous attention as a biocompatible coating. In this study, DLC film coated NiTi orthodontic archwires to protect Ni release into the oral cavity. Each wire was immersed in physiological saline at the temperature 37 °C for 6 months. The release concentration of Ni ions was detected using microwave induced plasma mass spectrometry (MIP-MS) with the resolution of ppb level. The toxic effect of Ni release was studied the cell growth using squamous carcinoma cells. These cells were seeded in 24 well culture plates and materials were immersed in each well directly. The concentration of Ni ions in the solutions had been reduced one-sixth by DLC films when compared with non-coated wire. This study indicated that DLC films have the protective effect of the diffusion and the non-cytotoxicity in corrosive environment.     

PIIID-formed (Ti,O)/Ti, (Ti,N)/Ti and (Ti,O, N)/Ti coatings on NiTi shape memory alloy for medical applications

(Ti, O)/Ti, (Ti, N)/Ti and (Ti, O, N)/Ti composite coatings were fabricated on NiTi shape memory alloy via plasma immersion ion implantation and deposition (PIIID). Surface morphology of samples was investigated using atomic force microscopy (AFM) and scanning electron microscopy (SEM). Cross-sectional morphology indicated that the PIIID-formed coatings were dense and uniform. X-ray diffraction (XRD) was used to characterize the phase composition of samples. X-ray photoelectron spectroscopy (XPS) results showed that the surface of coated NiTi SMA samples was Ni-free. Nanoindentation measurements and pin-on-disc tests were carried out to evaluate mechanical properties and wear resistance of coated NiTi SMA, respectively. For the in vitro biological assessment of the composite coatings in terms of cell morphology and cell viability, osteoblast-like SaOS-2 cells and breast cancer MCF-7 cells were cultured on NiTi SMA samples, respectively. SaOS-2 cells attached and spread better on coated NiTi SMA. Viability of MCF-7 cells showed that the PIIID-formed composite coatings were noncytotoxic and coated samples were more biocompatible than uncoated samples.     

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.     

Fabrication and biocompatibility of polyethyleneimine/heparin self-assembly coating on NiTi alloy

NiTi alloy has been used widely as biomaterials. But because of toxic effects possibly caused by excess Ni ions released during the corrosion process in the physiological environment, it is still a controversial material. Fabricating medicine-loaded coating, which is expected to decrease the release of Ni ions and improve the biocompatibility of the materials, is a potential way to solve the problem. In this paper, NiTi alloy is coated by polyethyleneimine/heparin films via layer-by-layer (LBL) self-assembly method. UV-Vis, FT-IR, atomic force microscopy (AFM) and contact angle measurements are used to characterize the microstructure of coatings and select the best fabrication conditions. Potentiodynamic polarization researches in sodium chloride and dynamic clotting time experiment are utilized to study its corrosion resistance capability and biocompatibility of coatings, respectively. The results indicate that PEI/heparin multilayer coating can improve the biocompatibility of NiTi alloy surface.     

Surface Composition and Corrosion Property of TiNi Alloys Coated with Tantalum Films

Multi-arc ion plating method was employed to coat TiNi alloys with Ta in order to improve radiopacity and corrosion resistance property. The surface composition, corrosion resistance property and Ni ions release amount of TiNi alloys coated with Ta films compared with TiNi alloys, are investigated by means of X-ray photoelectron spectrometry (XPS), electrochemical measurements and atomic absorption spectrophotometry (AAS), respectively. The results show that the coated surface composition is composed of Ta and 0 and the corrosion resistance is improved, whereas the Ni ions release amount of the coated sample is lower than that of the uncoated samples in the whole immersion period, indicating that Ta coating can improve the biocompatibility of TiNi alloys.     

Structure and properties of TiC/Ti coatings fabricated on NiTi by plasma immersion ion implantation and deposition

A titanium carbide (TiC) nanostructured coating and Ti intermediate layer are fabricated on NiTi by plasma immersion ion implantation and deposition (PIII&D) to improve the surface properties. The chemical composition and structure are determined by X-ray diffraction, Auger electron spectroscopy, scanning electron microscopy, and atomic force microscopy. Nano-indentation is used to evaluate the mechanical properties of the thin film and the biological characteristics are assessed by electrochemical measurement and soaking tests in simulated body fluids. Based on the potentiodynamic polarization and Ni release data after the polarization test, the Ti/TiC nanostructure coating has better corrosion resistance compared to the NiTi substrate and there is significantly less Ni ion release from the NiTi substrate into the simulated body fluids than the uncoated NiTi alloy.     

Carbon plasma immersion ion implantation and DLC deposition on Ni−Ti alloy

Carbon plasma immersion ion implantation (PIII-C) has been performed on Ni?Ti alloy surface using methane as a precursor gas at low temperature and it has been followed by deposition of diamond-like carbon (DLC) coating. Untreated and coated alloys are characterized with field emission scanning electron microscopy, atomic force microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. Electrochemical impedance spectroscopy, and corrosion testing in Hanks’ solution which is simulated body fluid show that corrosion resistance has been enhanced in PIII-C?+?DLC-coated alloy compared to untreated alloy. The in vitro studies of untreated and PIII-C?+?DLC-coated alloys have been evaluated using osteoblast-like cells (MG-63). Cellular behavior in terms of cell morphology along with the viability and cell spreading has been evaluated using scanning electron microscopy and in vitro cell culture assay, respectively. In comparison to Ni–Ti alloy, the coated alloy exhibits better cell viability indicating their biocompatibility.