钛合金表面磁控溅射TiB2-TiN复合薄膜的摩擦磨损性能

采用室温磁控溅射技术在钛合金(Ti6Al4V)表面制备SiC/TiB2-TiN双层薄膜,SiC为中间层,研究了TiB2-TiN复合薄膜的组织结构和摩擦磨损性能.结果表明,TiB2-TiN复合薄膜具有纳米尺度颗粒(畴)的微结构特征,SiC薄膜与基材和TiB2-TiN复合薄膜间都具有明显且呈梯度的元素扩散;在载荷200g、室温Kokubo人体模拟体液条件下,与氮化硅(Si3N4)球(直径4mm)对摩,其平均摩擦系数约为0.22,磨损速率在10-6mm3/(m·N)级;并且TiB2-TiN复合薄膜对Kokubo人体模拟体液中的Ca、P元素具有很强的黏附能力.     

Texture and sheet resistance of Al alloy thin films on Ti and TiN thin films

Ti films prepared by ionized physical vapor deposition (I-PVD) and TiN films prepared by metalorganic chemical vapor deposition (MOCVD) were examined as the underlayers of the Al interconnect films. The crystallographic texture of the Al films and the sheet resistance of the thin-film stacks were investigated at various thicknesses of the Ti or TiN thin film. The sheet resistance of the thin-film stacks was also measured after annealing at 400 °C in an N₂ ambient. For the I-PVD Ti underlayer, the excellent texture of the Al (1 1 1) was obtained even on a 5-nm thick Ti film. However, the sheet resistance of the multilayer structure increased after the annealing due to the reaction between Al and Ti. MOCVD TiN layers between the Ti film and the Al film could suppress the Al–Ti reaction without severe degradation of the Al (1 1 1) texture. Excellent texture of the Al film was obtained with thin MOCVD TiN films below 5 nm.     

Interfacial reaction mode and its influence on tensile strength in laser joining Al alloy to Ti alloy

Abstract

In order to obtain a robust dissimilar joint of Al/Ti alloys, a filler wire of Al–12 wt-%Si and 45° V shape groove on the base metal were used during CO₂ laser welding. Heat input had evident influence on the interfacial reaction mode. It was found that a dissolution mode for low heat input and a melting mode for high heat input exist at the joint interface, which was analysed from thermodynamic point of view. Tensile strength of the joints in the dissolution mode reached as high as 296 MPa, which was significantly higher than that in the melting mode.     

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.     

Ag衬底层对FePt薄膜结构和性能的影响

采用磁控溅射方法在自然氧化的单晶Si(100)衬底上制备了双层结构的FePt-X/Ag(X=Ag或Pt)薄膜.以20nm厚的Ag做衬底,可以制备出易磁化轴垂直基片的FePt合金薄膜;Ag在FePt薄膜中优先团聚,不利于控制FePt晶粒的长大,调整Pt的含量可以控制热处理过程中FePt薄膜的晶粒尺度;通过XRD、TEM、VSM对薄膜样品的结构、晶粒尺寸的观察和磁性检测,我们认为FePt合金薄膜有序化转变的最佳热处理温度在400℃;经过500℃热处理,薄膜软硬磁耦合较好,晶粒尺寸约为100nm,有最大的矫顽力1.04×106A/m.     

The influence of the substrate and the substrate temperature on the crystallinity of tin films

Thin films of tin were prepared on various substrates (NaCl, KCl, KBr and KI) and at various substrate temperatures (28–90°C) and were studied using transmission electron microscopy and selected area electron diffraction techniques. To determine the dependence on cleanness, tin was deposited on single-crystal surfaces prepared by vacuum cleaving. Films were prepared on substrate surfaces to which a parallel d.c. electric field (0–1000 V cm⁻¹) was applied. It was observed that the crystallites of tin films deposited on KBr were more preferentially oriented than those deposited on NaCl, KCl or KI. The effects of vacuum cleaving and of d.c. electric fields are discussed.     

Photo-induced properties of anodic oxide films on Ti6Al4V

Photocatalytic activity and wettability of the anodic oxide layer on Ti6Al4V prepared by anodization in a sulfuric acid electrolyte are explored. The oxide is composed mainly of TiO₂ with V₂O₅, VO₂ and Al₂O₃. The crystal structure of the TiO₂ varies from anatase to rutile with the sulfuric acid concentration in the electrolyte. Anatase exhibits better photocatalytic activity compared with rutile, which is different from those on Ti and Ti-Nb-Sn alloy. Contact angles of the oxides decrease with ultraviolet light illumination, and hydrophilicity is observed in the rutile oxide. Both photocatalytic activity and hydrophilicity are inferior to the corresponding Ti and Ti-Nb-Sn alloy, which is explained by the presence of Al₂O₃ in the anodic oxide.     

Influence of Ti/TiN bilayered and multilayered films on the axial fatigue performance of Ti46Al8Nb alloy

The effects of Ti/TiN bi- and multilayered films on the fatigue performance of the Ti46Al8Nb alloy were investigated. Ti/TiN films with a total thickness of 1 μm were deposited on the Ti46Al8Nb alloy substrate by the hollow cathode deposition method. The samples were examined with various analytical techniques including nanoindentation, scratch test, stripping layer substrate curvature test and scanning electron microscopy. The results show that multilayered Ti/TiN films can enhance the fatigue strength of the Ti46Al8Nb alloy, whereas bilayered films have no obvious effect. Compared with the bilayer, the multilayer exhibits higher hardness, higher residual compressive stress and higher adhesion strength to the substrate. It is also demonstrated that the multilayer is responsible for retarding fatigue crack growth. All the superior properties make the hard Ti/TiN multilayer to be an effective protection coating for the enhanced fatigue strength of the brittle substrate.     

An improved process for grain refinement of large 2219 Al alloy rings and its influence on mechanical properties

The large 2219 Al alloy rings used to connect propellant tank components of a satellite launch vehicle to each other are conventionally manufactured by radial-axial ring rolling at 460°C with 50% deformation,but often suffer from coarse elongated grain and low ductility. An improved process(hot ring rolling at460°C with 30% deformation, then air cooling to 240°C, followed by ring rolling at 240°C with 20% deformation) was tested for ring manufacturing. The corresponding microstructure evolution and mechanical properties of the produced rings were studied. The results show that the improved process can successfully be applied to manufacture the large 2219 Al alloy rings without formation of macroscopic defects,resulting in a product with fine and uniform grains after heat treatment. The fracture mechanism of both rings was mainly intergranular fracture. With the resulting grain size refinement due to the improved process, more homogeneous slip occured and the crack propagation path became more tortuous during the tensile testing process. Thus, the elongation in all three orthogonal directions was greatly improved,and the axial elongation increased from 3.5% to 10.0%.     

Effects of bias voltage on the microstructure and mechanical properties of (Ti,Al,Cr)N hard films with N-gradient distributions

(Ti,Al,Cr)N hard reactive films were deposited on high speed steel substrates by multi-arc ion plating (MAIP) technology using pure Cr and Ti-50Al(at.%) alloy targets. The partial pressure of N₂ was raised step by step in each deposition process. The surface morphology, the cross-sectional morphology of fracture sample, the surface compositions and the phase structure of the (Ti,Al,Cr)N films were investigated by scanning electronic microscope (SEM) and X-ray diffraction (XRD). The dense columnar microstructure was obtained in all of the (Ti,Al,Cr)N films, though micro-droplets evidently existed on the surface of the films. The micro-hardness of the film surface, the adhesive strength of the film/substrate and the thermal shock resistance were investigated. The results revealed the effects of bias voltage on the composition, phase structure, and mechanical properties. The improved balanced properties of a micro-hardness of about 50 GPa, an adhesive strength larger than 200 N and a thermal shock resistance of 7-8 cycles were reached at a bias voltage of 150 V. The present super-hard (Ti,Al,Cr)N films with N-gradient distribution may be an actual substitution of TiN, (Ti,Al)N, (Ti,Cr)N and single-layer (Ti,Al,Cr)N hard films.     

铸造Ti46Al8Nb合金拉伸过程中的损伤

研究了热等静压处理后铸态Ti46Al8Nb合金拉伸过程中的损伤.结果表明:1)消除了疏松后,Ti46Al8Nb合金拉伸强度的数据分散性仍然很大,表明疏松不是导致数据分散的唯一原因.在拉伸过程中不同强度试样的声发射行为有很大差异,说明其具有不同的损伤特征.断口分析和预拉伸着色实验结果证明,拉伸强度的数据分散性是合金晶粒粗大及其片层结构拉伸行为明显的各向异性所致;2)将预拉伸后样品表面去除约300 μm,在随后的第二次拉伸过程中声发射Kaiser效应不再出现,说明在拉伸加载初期(低应力下)该合金的损伤主要集中于近表面.     

Structural characteristics and mechanical properties of Ti(Cr) films produced on Si substrate

A series of nanogranular Ti₉₀Cr₁₀ thin films have been fabricated by pulsed-laser deposition on Si substrates at different temperatures. The crystal structure and mechanical properties of these films were investigated. The X-ray diffraction and transmission electron microscope images with selected area diffraction showed that the structure of as-prepared films is dependent on film thickness and deposition temperature. It was found that the Ti₉₀Cr₁₀ films consisted of fine hexagonal close packed microstructure with columnar grains, while body close-packed cubic structure of Cr films are composed of irregular grains, meanwhile, a chromium disilicide (CrSi₂) layer formed in the interface between the substrate and Cr films which deposited at temperature of greater than 600 °C. The crystalline and columnar grains improved with an increase of the thickness of the films and an optimum microstructure is obtained under the present experimental condition of about 50 nm thickness and deposited temperature of 500 °C for Ti₉₀Cr₁₀ films. Deposited at 300 °C, the Ti₉₀Cr₁₀ films have hardness of 12.7 GPa and elastic modulus of 174.6 GPa. Improved to 600 °C the sample shows higher hardness of 13.1 GPa and higher elastic modulus of 183.2 GPa. Using Benjamin-Weaver model, adhesion shearing force can be calculated as 34.9 MPa for 300 °C Ti₉₀Cr₁₀ film while higher value of 44.4 MPa for higher temperature of 600 °C.     

Surface characterization and influence of anodizing process on fatigue life of Al 7050 alloy

The present study investigates the influence of anodizing process on fatigue life of aluminium alloy 7050-T7451 by performing axial fatigue tests at stress ratio ‘R’ of 0.1. Effects of pre-treatments like degreasing and pickling employed prior to anodizing on fatigue life were studied. The post-exposure surface observations were made by scanning electron microscope (SEM) to characterize the effect of each treatment before fatigue testing. The surface observations have revealed that degreasing did not change the surface topography while pickling solution resulted in the formation of pits at the surface. Energy dispersive spectroscopy (EDS) was used to identify those constituent particles which were responsible for the pits formation. These pits are of primary concern with respect to accelerated fatigue crack initiation and subsequent anodic coating formation. The fatigue test results have shown that pickling process was detrimental in reducing the fatigue life significantly while less decrease has been observed for anodized specimens. Analyses of fracture surfaces of pickled specimens have revealed that the process completely changed the crack initiation mechanisms as compared to non-treated specimens and the crack initiation started at the pits. For most of the anodized specimens, fatigue cracks still initiated at the pits with very few cracks initiated from anodic coating. The decrease in fatigue life for pickled and anodized specimens as compared to bare condition has been attributed to decrease in initiation period and multi-site crack initiations. Multi-site crack initiation has resulted in rougher fractured surfaces for the pickled and anodized specimens as compare to bare specimens tested at same stress levels.     

UBMS合成的SiNO/Ti6Al4V薄膜的性能研究

利用非平衡磁控溅射技术在Ti6Al4V合金表面制备SiNO薄膜,对不同氮气流量下SiNO薄膜样品的耐磨性和耐蚀性进行研究.结果表明,SiNO薄膜样品具有优异的耐磨性和耐蚀性能.研究认为影响SiNO薄膜性能的主要因素为薄膜中的氮原子百分含量及化合物存在状态.     

Effect of substrate bias on properties of silicon nitride films prepared by activated reactive evaporation

Substrate biasing was explored to improve the quality of activated reactive evaporation processed (ARE) silicon nitride films. The samples were prepared at various r.f. (radio frequency) substrate bias power for a given electron beam current, pressure, and r.f. discharge powet. The quality of the ARE silicon nitride deposited at over 150 W of substrate bias was comparable with high temperature processed CVD films. These films showed a refractive index of 2.00, an absorption edge of 4.9 eV, a dielectric constant of 7.2–7.7 and hydrogen and oxygen concentrations far less than 1 at.%.     

Mechanical and corrosion properties of Al/Ti film on magnesium alloy AZ31B

Preparation of titanium film on magnesium substrate faces a challenge due to non-Fickian inter-diffusion between titanium and magnesium. Aluminum can build a bridge between titanium and magnesium. Al/Ti duplex coatings were deposited on magnesium alloy AZ31B using magnetron sputtering (MS). The low temperature diffusion bonding behavior of the Mg/Al/Ti coating was investigated through SEM and its affiliated EDS. The phase structure and critical load of the coatings were examined by means of XRD and scratch tests, respectively. The results demonstrated that the bonding strength was significantly improved after a post heat treatment (HT) at a temperature of 210°C. The diffusion mechanism of the interfaces of Mg/Al and Al/Ti in the coating was discussed based on the analysis of formation energy of vacancies and diffusion rates. The Al/Ti dual layer enhanced the corrosion resistance of the alloy. And the HT process further increased the corrosion resistance of the coated alloy. This result implies that a post HT at a lower temperature after MS is an effective approach to enhance the bonding strength and corrosion resistance of the Al/Ti film on Mg alloys.     

The substrate influence on the magnetization of nickel electrodeposited thin films

The effects of diffusion of substrate copper atoms into the film as well as substrate stresses on both saturation magnetization and coercive force of annealed electrodeposited Ni films have been investigated.     

Dielectric properties of anodized Al-Ta alloy films with high Al content

At 1 mA cm^-2 the anodization voltage of sputtered Al-Ta alloy films with about 7 at.% Ta content rises linearly with time at a rate of 0.45 V s^-1. The Al-Ta thickness-anodization voltage ratio and the oxide growth constant have been determined, for 7–14 at.% Ta in the films with 1% citric acid electrolyte, to be 1.03-0.94 nm V^-1 and 1.42–1.5 nm V^-1, respectively. The permittivity was found to range from 10.0–11.4, corresponding to a capacitance density of about 330 pF mm^-2 for an anodization voltage of 200 V. The temperature coefficient of capacitance (t.c.c.) was 500 ppm K^-1. The capacitance between 400 Hz and 1 MHz remained constant within ±1%. At 1 kHz the disspation factor tan δ was 0.6%.Nearly all leakage currents were between 0.1 and 0.5 nA using 5.6 nF test capacitors and 50 V as the test voltage. This corresponds to an insulation resistance R of 10¹¹ Ω or more, or a time constant τ ( = RC) of approximately 1000 s. For the 50 V test the yield was about 90% and at least 80% of the capacitors had no short circuits after step stress tests up to 90 V.The current-voltage characteristics of capacitors made from Al-Ta (7 at.% Ta) films showed non-destructive breakdown voltages greater than 100 V. Only a slight deviation from symmetry was noticed whether the Al-Ta electrode was positive or negative, indicating that the capacitors were virtually non-polar. In some cases non-shorting breakdown was observed.     

The influence of porous silica substrate on the properties of alumina films studied by X-ray reflection spectroscopy

The structure of alumina (Al₂O₃) films of various thicknesses grown by the atomic layer deposition method on porous silica (por-SiO₂) substrates has been studied using soft X-ray reflection spectroscopy. It is established that the synthesized films are amorphous and that the ratio of Al atoms with tetrahedral and octahedral coordinations in a film depends on its thickness. It can be suggested that thicker Al₂O₃ films contain a greater proportion of Al atoms with tetrahedral coordination.